[Federal Register Volume 63, Number 56 (Tuesday, March 24, 1998)]
[Proposed Rules]
[Pages 14182-14248]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 98-6678]



[[Page 14181]]

_______________________________________________________________________

Part II





Environmental Protection Agency





_______________________________________________________________________



40 CFR Part 63



National Emission Standards for Hazardous Air Pollutants; Proposed 
Standards for Hazardous Air Pollutants Emissions for the Portland 
Cement Manufacturing Industry; Proposed Rule

  Federal Register / Vol. 63, No. 56 / Tuesday, March 24, 1998 / 
Proposed Rules  

[[Page 14182]]



ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 63

[IL-64-2-5807; FRL-5978-2]
RIN 2060-AE78


National Emission Standards for Hazardous Air Pollutants; 
Proposed Standards for Hazardous Air Pollutants Emissions for the 
Portland Cement Manufacturing Industry

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule and notice of public hearing.

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SUMMARY: This action proposes national emission standards for hazardous 
air pollutants (NESHAP) for new and existing sources in portland cement 
manufacturing plants. Exposure to the hazardous air pollutants (HAPs) 
in these emissions may be associated with a wide variety of effects, 
including carcinogenic, respiratory, nervous system, dermal, 
developmental, and/or reproductive health effects. Implementation of 
the proposed requirements would reduce emissions of several HAPs.
    The standards are proposed under the authority of section 112(d) of 
the Clean Air Act as amended (the Act) and are based on the 
Administrator's determination that portland cement manufacturing plants 
may reasonably be anticipated to emit several of the HAPs listed in 
section 112(b) of the Act from the various process operations found 
within the industry. The proposed NESHAP would provide protection to 
the public by requiring all portland cement plants which are major 
sources to meet emission standards reflecting the application of the 
maximum achievable control technology (MACT).

DATES: Comments. The EPA will accept comments on the proposed rule 
until May 26, 1998.
    Public Hearing. If anyone contacts the Agency requesting to speak 
at a public hearing, the hearing will be held at the Agency's Office of 
Administration Auditorium, Research Triangle Park, North Carolina on 
April 23, 1998 beginning at 10:00 a.m. Persons wishing to present oral 
testimony must contact the Agency by April 14, 1998.

ADDRESSES: Comments. Comments should be submitted (in duplicate) to: 
Air and Radiation Docket and Information Center (6102), Attention: 
Docket No. A-92-53, U.S. Environmental Protection Agency, 401 M Street 
SW., Washington, DC 20460. The Agency requests that a separate copy 
also be sent to the contact person listed below (Mr. Joseph Wood). 
Comments and data may also be submitted electronically by following the 
instructions provided in the SUPPLEMENTARY INFORMATION section. No 
confidential business information (CBI) should be submitted through 
electronic mail.
    Public Hearing. Persons wishing to present oral testimony or to 
inquire as to whether or not a hearing is to be held should notify Ms. 
Cathy Coats, Minerals and Inorganic Chemicals Group (MD-13), U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711, 
telephone number (919) 541-5422. Additional information regarding the 
public hearing is given in the SUPPLEMENTARY INFORMATION section.
    Docket. The official record for this rulemaking, as well as the 
public version, has been established under Docket No. A-92-53 
(including comments and data submitted electronically as described 
below). A public version of this record, including printed, paper 
versions of electronic comments and data, which does not include any 
information claimed as CBI, is available for inspection from 8 a.m. to 
4 p.m., Monday through Friday, excluding legal holidays. The official 
rulemaking docket is located at the address in the ADDRESSES section 
above. Alternatively, a docket index, as well as individual items 
contained within the docket, may be obtained by calling (202) 260-7548. 
A reasonable fee may be charged for copying.

FOR FURTHER INFORMATION CONTACT: For information about this proposed 
rule, contact Mr. Joseph Wood, P.E., Minerals and Inorganic Chemicals 
Group, Emission Standards Division (MD-13), U.S. Environmental 
Protection Agency, Research Triangle Park, NC 27711, telephone number 
(919) 541-5446; electronic mail address [email protected]. For 
information about the proposed test methods contact Ms. Rima 
Dishakjian, Emission Measurement Center, Emissions, Monitoring and 
Analysis Division (MD-19), U.S. Environmental Protection Agency, 
Research Triangle Park, NC 27711, telephone number (919) 541-0443.

SUPPLEMENTARY INFORMATION: Electronic filing. Electronic comments can 
be sent directly to the EPA at [email protected]. 
Electronic comments and data must be submitted as an ASCII file 
avoiding the use of special characters and any form of encryption. 
Comments and data will also be accepted on disks in Wordperfect 5.1 or 
6.1 file format or ASCII file format. All comments and data in 
electronic form must be identified by the docket number A-92-53. 
Electronic comments may be filed online at many Federal Depository 
Libraries.
    Implementation of the proposed requirements would achieve an 
emission reduction from existing and projected new sources estimated at 
82 megagrams per year (Mg/yr) (90 tons per year [tpy]) of HAPs and 
4,900 Mg/yr (5,400 tpy) of other pollutants (volatile organic compounds 
[VOC] and particulate matter [PM]). The EPA is also proposing to 
require portland cement plants that are area sources to meet emission 
standards for dioxins and furans reflecting the application of MACT.
    The EPA is also proposing Methods 320, 321, and 322 with the 
standards for addition to 40 CFR part 63, appendix A. These methods may 
be used to assist in determining the applicability of the proposed 
emission limitations.
    Public Hearing. If a public hearing is requested and held, EPA will 
ask clarifying questions during the oral presentation but will not 
respond to the presentations or comments. Written statements and 
supporting information will be considered with equivalent weight as any 
oral statement and supporting information subsequently presented at a 
public hearing, if held.
    Confidential Business Information. Commenters wishing to submit 
proprietary information for consideration should clearly distinguish 
such information from other comments and clearly label it 
``Confidential Business Information.'' Submissions containing such 
proprietary information should be sent directly to the following 
address, and not to the public docket, to ensure that proprietary 
information is not inadvertently placed in the docket: Attention: Mr. 
Joseph Wood, c/o Ms. Melva Toomer, U.S. EPA Confidential Business 
Information Manager, OAQPS (MD-13); Research Triangle Park, NC 27711. 
Information covered by such claim of confidentiality will be disclosed 
by the EPA only to the extent allowed and by the procedures set forth 
in 40 CFR part 2. If no claim of confidentiality accompanies a 
submission when it is received by the EPA, the submission may be made 
available to the public without further notice to the commenter.
    Regulated entities. Entities potentially regulated by this action 
are those who have the potential to emit HAPs listed in section 112(b) 
of the Act in the regulated categories and entities shown in Table 1.

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    This table is not intended to be exhaustive, but rather provides a 
guide for readers regarding entities likely to be regulated by this 
action. This table lists the types of entities that the EPA is now 
aware could potentially be regulated by this action. Other types of 
entities not listed in this table could also be regulated. To determine 
whether your facility is regulated by this action, you should carefully 
examine the applicability criteria in Sec. 63.1340 of the proposed 
rule. If you have questions regarding the applicability of this action 
to a particular entity, consult the person listed in the preceding FOR 
FURTHER INFORMATION CONTACT section of this preamble.

                      Table 1.--Regulated Entities                      
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                Category                  Examples of regulated entities
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Industry...............................  Owners or operators of portland
                                          cement manufacturing plants.  
State..................................  Owners or operators of portland
                                          cement manufacturing plants.  
Tribal associations....................  Owners or operators of portland
                                          cement manufacturing plants.  
Federal agencies.......................  None.                          
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    Technology Transfer Network. The proposed regulatory text is also 
available on the Technology Transfer Network (TTN), one of EPA's 
electronic bulletin boards. The TTN provides information and technology 
exchange in various areas of air pollution control. The service is 
free, except for the cost of a phone call. Dial (919) 541-5742 for up 
to a 14,400 BPS modem. The TTN is also accessible through the Internet 
(world wide web) at http://www.epa.gov/ttn/. If more information on the 
TTN is needed, call the HELP line at (919) 541-5384. The help desk is 
staffed from 11 a.m. to 5 p.m.; a voice menu is available at other 
times.
    Outline. The information in this preamble is organized as shown 
below.

I. Statutory Authority
II. Introduction
    A. Background
    B. NESHAP for Source Categories
    C. Health Effects of Pollutants
    D. Portland Cement Manufacturing Industry Profile
III. Summary of Proposed Standards
    A. Applicability
    B. Emission Limits and Requirements
    C. Performance Test and Compliance Provisions
    D. Monitoring Requirements
    E. Notification, Recordkeeping, and Reporting Requirements
IV. Impacts of Proposed Standards
    A. Applicability
    B. Air Quality Impacts
    C. Water Impacts
    D. Solid Waste Impacts
    E. Energy Impacts
    F. Nonair Health and Environmental Impacts
    G. Cost Impacts
    H. Economic Impacts
V. Selection of Proposed Standards
    A. Selection of Source Category
    B. Selection of Emission Sources
    1. Feed Preparation Processes (Grinding, Conveying)
    2. Feed Preparation Processes (Drying, Blending, Storage)
    3. Kiln
    4. Clinker Cooler
    5. Finish Grinding/Conversion of Clinker to Portland Cement
    C. Selection of Pollutants
    D. Selection of Proposed Standards for Existing and New Sources
    1. Background
    2. MACT Floor Technology, Emission Limits, and Format
    E. Selection of Testing and Monitoring Requirements
    1. Kiln and In-line Kiln Raw Mill PM Emissions
    2. Kiln D/F Emissions
    3. Kiln and Raw Material Dryer THC Emissions
    4. Clinker Cooler PM Emissions
    5. Raw and Finish Mill PM Emissions
    6. Raw Material Dryer and Materials Handling Processes PM 
Emissions
    7. General Monitoring Requirements
    F. Selection of Notification, Recordkeeping, and Reporting 
Requirements
VI. Public Participation
VII. Administrative Requirements
    A. Docket
    B. Public Hearing
    C. Executive Order 12866
    D. Enhancing the Intergovernmental Partnership Under Executive 
Order 12875
    E. Unfunded Mandates Reform Act
    F. Regulatory Flexibility Act
    G. Paperwork Reduction Act
    H. Clean Air Act

I. Statutory Authority

    The statutory authority for this proposal is provided by sections 
101, 112, 114, 116, 183(f) and 301 of the Clean Air Act, as amended (42 
U.S.C. 7401, 7411, 7414, 7416, 7511(f) and 7601).

II. Introduction

A. Background

    Nationwide baseline HAP emissions from portland cement 
manufacturing plants are estimated to be 260 Mg/yr (290 tpy) at the 
current level of control. The HAPs released from kiln systems include 
acetaldehyde, arsenic, benzene, cadmium, chromium, chlorobenzene, 
dibenzofurans, formaldehyde, hexane, hydrogen chloride, lead, 
manganese, mercury, naphthalene, nickel, phenol, polycyclic organic 
matter, selenium, styrene, 2,3,7,8-tetrachlorodibenzo-p-dioxin, 
toluene, and xylenes. The HAPs released from raw material dryers should 
be similar to those from the kiln. The HAPs released from clinker 
coolers, raw mills, finish mills, storage bins, conveying system 
transfer points, bagging systems and bulk loading and unloading systems 
include arsenic, cadmium, chromium, lead, manganese, mercury, nickel, 
and selenium. Implementing MACT-level controls is expected to decrease 
emissions of these HAPs from existing and projected new sources by 
approximately 82 Mg/yr (90 tpy). Plants can achieve this reduction by 
upgrading or installing fabric filters (FF), also known as baghouses, 
and electrostatic precipitators (ESP) to decrease HAP metals; limiting 
temperatures at the particulate matter control device (PMCD) inlet to 
decrease dioxin and furan (D/F) emissions; and selecting suitable feed 
materials to decrease organic HAP emissions.
    The overall effect of these standards would be to improve the 
control performance of the industry to the level achieved by the best 
performing plants. In addition to the health and environmental benefits 
associated with HAP emission reductions, benefits of this action 
include a decrease in site-specific emission levels of PM and VOC and 
lowered occupational exposure levels for employees.
    The nationwide capital and annualized costs of the proposed NESHAP, 
including emission controls and associated monitoring equipment, are 
estimated at $88 million and $27 million/yr, respectively. The economic 
impacts are predicted to increase prices of portland cement by an 
average of 1.1 percent.
    To minimize adverse impacts, the Agency has proposed controls at 
the MACT-floor level, tailored the requirements to allow less-costly 
testing and monitoring by using surrogates for HAP emissions and 
provided choice in methods of control. The proposed rule

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is ``user friendly,'' with language that is easy to understand by all 
of the regulated community. The EPA also proposes to allow existing 
facilities up to 3 years to comply. And, as allowed under section 
112(i)(3)(B) of the Act, the Administrator or delegated regulatory 
authority also may grant 1 additional year if necessary for the 
installation of controls.

B. NESHAP for Source Categories

    Section 112 of the Act as amended specifically directs the EPA to 
develop a list of all categories of major sources and such area sources 
as appropriate that emit one or more of the HAPs listed in the Act. The 
EPA is further directed to develop NESHAP to control emissions of HAPs 
from both existing and new major sources, where a major source is 
defined as a source that emits or has the potential to emit 9.1 Mg/yr 
(10 tpy) or more of any one HAP or 22.7 Mg/yr (25 tpy) of any 
combination of HAPs. The statute requires the standards to reflect the 
maximum degree of reduction in HAP emissions that is achievable, taking 
into consideration the cost of achieving the emission reduction, any 
nonair quality health and environmental impacts, and energy 
requirements. This level of control is commonly referred to as MACT.
    The control of HAPs is achieved through the promulgation of 
technology-based emission standards under sections 112(d) and 112(f) 
and work practice standards under 112(h) for categories of sources that 
emit HAPs. Emission reductions may be accomplished through the 
application of measures, processes, methods, systems, or techniques 
including, but not limited to: (1) Reducing the volume of, or 
eliminating emissions of, such pollutants through process changes, 
substitution of materials, or other modifications; (2) enclosing 
systems or processes to eliminate emissions; (3) collecting, capturing, 
or treating such pollutants when released from a process, stack, 
storage or fugitive emissions point; (4) design, equipment, work 
practice, or operational standards (including requirements for operator 
training or certification) as provided in subsection (h); or (5) a 
combination of the above. [See section 112(d)(2) of the Act.] The EPA 
may promulgate more stringent regulations to address residual risk that 
remains after the imposition of controls at a later date.

C. Health Effects of Pollutants

    The Clean Air Act was created in part to protect and enhance the 
quality of the Nation's air resources so as to promote the public 
health and welfare and the productive capacity of its population. [See 
section 101(b)(1).] In the 1990 Amendments to the Clean Air Act, 
Congress specified that each standard for major sources must require 
the maximum reduction in emissions of HAPs that EPA determines is 
achievable considering cost, health and environmental impacts, and 
energy requirements. Title III of the Act establishes a control 
technology-based program to reduce stationary source emissions of HAPs. 
The goal of section 112(d) (in Title III) is to apply such control 
technology to reduce emissions and thereby reduce the hazard of HAPs 
emitted from stationary sources.
    Section 112(b) of the Act lists HAPs believed to cause adverse 
health or environmental effects. The EPA recognizes that the degree of 
adverse effects to health can range from mild to severe. The extent and 
degree to which the health effects may be experienced is dependent 
upon: (1) The ambient concentrations observed in the area (e.g., as 
influenced by emission rates, meteorological conditions, and terrain); 
(2) the frequency of and duration of exposures; (3) characteristics of 
exposed individuals (e.g., genetics, age, pre-existing health 
conditions, and lifestyle) which vary significantly with the 
population; and (4) pollutant-specific characteristics (e.g., toxicity, 
half-life in the environment, bioaccumulation, and persistence). In 
essence, these MACT standards would ensure that all major sources of 
air toxic emissions achieve the level of control already being achieved 
by the better controlled and lower emitting sources in each category. 
This approach provides assurance to citizens that each major source of 
toxic air pollution will be required to effectively control its 
emissions. At the same time, this approach provides a level economic 
playing field, ensuring that facilities that employ cleaner processes 
and good emissions controls are not disadvantaged relative to 
competitors with poorer controls.
    Available emission data, collected in conjunction with the 
development of this NESHAP, show that non-volatile HAP metals, mercury, 
organic HAPs and hydrogen chloride are the predominant HAPs emitted 
from portland cement manufacturing plants. These pollutants (except 
mercury and hydrogen chloride) have the potential to be reduced by 
implementation of the proposed emission limits. In addition to the 
HAPs, the portland cement manufacturing NESHAP would also control some 
of the pollutants whose emissions are controlled under the National 
Ambient Air Quality Standards (NAAQS). These pollutants include PM, 
VOC, and lead. The following is a summary of the potential health 
effects associated with exposures, at some level, to pollutants that 
would be reduced by the standard.
    Almost all metals appearing on the section 112(b) list are emitted 
from portland cement manufacturing affected sources. There is a wide 
range of targets of toxicity for these metals. Effects include skin 
irritation, mucous membrane irritation (e.g., lung irritation), 
gastrointestinal effects, nervous system effects (including cognitive 
effects, tremor, and numbness), increased blood pressure, and 
reproductive and developmental effects. Additionally, several of the 
metals accumulate in the environment and in the human body. Cadmium, 
for example, is a cumulative pollutant which causes kidney effects 
after the cessation of exposure. Similarly, the onset of effects from 
beryllium exposure may be delayed by months to years. Many of the metal 
compounds are also known (arsenic, chromium (VI)) or probable (cadmium, 
nickel carbonyl, lead, and beryllium) human carcinogens.
    Organic compounds which will potentially be decreased by the 
proposed standard include but are not limited to acetaldehyde, benzene, 
chlorobenzene, formaldehyde, D/F, hexane, naphthalene, phenol, 
polycyclic organic matter, styrene, toluene, and xylenes. Each of these 
organic compounds has a range of potential health effects associated 
with exposure at some level. Some of the effects associated with short-
term inhalation exposure to these pollutants are similar and include 
irritation of the eyes, skin, and respiratory tract in humans; central 
nervous system effects (e.g., drowsiness, dizziness, headaches, 
depression, nausea, irregular heartbeat); reproductive and 
developmental effects; and, neurological effects. Exposure to benzene 
at extremely high concentrations may even lead to respiratory 
paralysis, coma, or death.
    Health effects associated with long-term inhalation exposure in 
humans to the organic compounds which will potentially be decreased by 
the proposed standard may include mild symptoms such as nausea, 
headache, weakness, insomnia, intestinal pain, and burning eyes; 
effects on the central nervous system; disorders of the blood; toxicity 
to the immune system; reproductive disorders in women (e.g., increased 
risk of spontaneous abortion); developmental effects; gastrointestinal 
irritation; liver injury; and muscular effects.

[[Page 14185]]

    In addition to the non-cancer effects described above, some of the 
organic HAPs that would be controlled under this proposed standard are 
either known (benzene) or probable (formaldehyde and D/F) human 
carcinogens.
    Hydrogen chloride (HCl) is highly corrosive to the eyes, skin, and 
mucous membranes. Short-term inhalation of HCl by humans may cause 
coughing, hoarseness, inflammation and ulceration of the respiratory 
tract, as well as chest pain and pulmonary edema. Long-term 
occupational exposure of humans to HCl has been reported to cause 
inflammation of the stomach, skin, and lungs, and photosensitization.
    The health effects of PM, lead, and VOC that would be reduced by 
this standard are described in EPA's Criteria Documents, which support 
the NAAQS. Briefly, PM emissions have been associated with aggravation 
of existing respiratory and cardiovascular disease and increased risk 
of premature death. Depending on the degree of exposure, lead can cause 
subtle effects on behavior and cognition, increased blood pressure, 
reproductive effects, seizures, and even death.
    Volatile organic compounds are precursors to the formation of ozone 
in the ambient air. At ambient levels, ozone has been shown in human 
laboratory and community studies to be responsible for the reduction of 
lung function, respiratory symptoms (e.g., cough, chest pain, throat 
and nose irritation), increased hospital admissions for respiratory 
causes, and increased lung inflammation. Animal studies have shown 
increased susceptibility to respiratory infection and lung structure 
changes. Exposure to ozone has also been linked to harmful effects on 
agricultural crops and forests.

D. Portland Cement Manufacturing Industry Profile

    Portland cement is a fine powder, usually gray in color, that 
consists of a mixture of the minerals dicalcium silicate, tricalcium 
silicate, tricalcium aluminate, and tetracalcium aluminoferrite, to 
which one or more forms of calcium sulfate have been added (docket item 
II-I-43, p. 746). The primary end use of portland cement is as the key 
ingredient in portland cement concrete, which is used in almost all 
construction applications.
    In 1993, 44 companies operated 118 portland cement plants located 
in 37 states. The manufacture of portland cement is covered by SIC code 
3241 for hydraulic cements. According to U.S. Small Business 
Administration size standards, companies owning portland cement plants 
are categorized as small if the total number of employees at the 
company is less than 750. Otherwise the company is classified as large. 
A total of 7 companies are categorized as small, while the remaining 37 
companies are in the large category (docket item II-D-200).
    Few new plants are predicted to be constructed during the next 5 
years. The EPA estimates that two to four existing plants will undergo 
reconstruction in the next 5 years.
    All existing kilns and alkali bypasses have PM control devices. 
Some existing cement manufacturing plants are required to meet new 
source performance standards (NSPS) for PM (40 CFR part 60, subpart F). 
The affected facilities to which the NSPS apply are the kiln, kiln gas 
alkali bypass, clinker cooler, raw material dryer, and materials 
handling processes.

III. Summary of Proposed Standards

A. Applicability

    The proposed standards apply to each existing, reconstructed, and 
newly constructed portland cement manufacturing plant at any facility 
which is a major source or an area source, with the following 
exception. Some portland cement plants fire hazardous wastes in the 
kiln to provide part or all of the fuel requirement for clinker 
production. Portland cement kilns and in-line kiln/raw mills subject to 
the NESHAP for hazardous waste combustors 1 (HWC) are not 
subject to this standard; however other affected sources at portland 
cement plants where hazardous waste is burned in the kiln are subject 
to this standard.
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    \1\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
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    For portland cement plants with on-site non-metallic minerals 
processing facilities, the first affected source in the sequence of 
materials handling operations subject to this proposed NESHAP is the 
raw material storage, which is just prior to the raw mill. The primary 
and secondary crushers and any other equipment in the non-metallic 
minerals processing plant, which precede the raw material storage are 
not affected sources under the proposed NESHAP. Furthermore, the first 
conveyor system transfer point subject to the proposed NESHAP is the 
transfer point associated with the conveyor transferring material from 
the raw material storage to the raw mill. Conveyor system transfer 
points prior to this conveyor are not affected sources under this 
proposed NESHAP (docket item II-B-53).
    This regulation does not apply to the emissions from cement kiln 
dust (CKD) storage facilities (i.e., CKD piles or landfills). A 
separate rulemaking will be forthcoming from EPA's Office of Solid 
Waste (OSW) that will apply to air emissions associated with CKD 
management and disposal facilities.
    Except for hazardous waste burning (HW) cement kilns and HW in-line 
kiln/raw mills, EPA is proposing to apply these standards to all cement 
kilns and in-line kiln/raw mills regardless of the material being 
combusted in the kiln. This proposal, however, does not preclude EPA 
from determining that cement kilns combusting solid waste materials 
should be regulated under section 129 of the Clean Air Act, 42 U.S.C. 
7429, and to revise the applicability section of these regulations 
accordingly at the time section 129 regulations applicable to cement 
kilns are promulgated.
    The EPA believes that applying this regulation to all non-hazardous 
waste burning (NHW) cement kilns regardless of the material combusted 
in the kiln is necessary at this time due to the Court of Appeals for 
the District of Columbia's recent decision in Davis County Solid Waste 
Management District v. Environmental Protection Agency, 101 F.3d 1395 
(D.C. Cir. 1996) (petition to review municipal waste combustor 
(``MWC'') regulations promulgated on December 19, 1995 pursuant to 
section 129 of the Act, 60 FR 65387). In the applicability section of 
the MWC regulations, EPA applied the standards to all solid waste 
incineration units combusting more than 30-percent municipal solid 
waste. Two owners and operators of MWC units with capacity less than 
250 tons/day filed petitions for review on the grounds that EPA 
improperly had included their units in the large category. The Cement 
Kiln Recycling Coalition (``CKRC'') also filed a petition for review on 
the grounds that the standards should not apply to cement kilns. In its 
opinion dated December 6, 1996, the Court indicated its intent to 
vacate the standards in their entirety on the grounds raised by the two 
petitioners who own and operate MWC units; as a result, the Court did 
not reach the issue raised by CKRC. Accordingly, EPA believes that it 
is appropriate to apply these regulations as a gap-filling measure to 
control emissions from NHW cement kilns and in-line kiln/raw mills 
regardless of the material combusted in the kiln (except for hazardous 
waste) until EPA determines whether regulations applicable to cement 
kilns combusting solid waste materials should be re-promulgated under 
section 129. To

[[Page 14186]]

decide otherwise would have the potential effect of allowing cement 
kiln owners and operators to avoid regulation by adding some solid 
waste material to the cement kiln.
    As background, section 129(a)(1)(A) requires the Administrator to 
establish performance standards and other requirements pursuant to 
section 111 and section 129 of the Act for each category of solid waste 
incineration units [42 U.S.C. 7429(a)(1)(A)]. Whereas section 112(c) of 
the Act requires EPA to determine major and area sources of the 188 
hazardous air pollutants (HAPs) listed in section 112(b), Congress 
specifically listed in section 129 various categories of solid waste 
incineration units that EPA must regulate, including solid waste 
incineration units combusting municipal solid waste [sections 
129(a)(1)(B) and (C)], solid waste incineration units combusting 
hospital waste, medical waste, and infectious waste [section 
129(a)(1)(C)], solid waste incineration units combusting commercial or 
industrial waste [section 129(a)(1)(D)], and ``other categories of 
solid waste incineration units'' which are to be defined by EPA [42 
U.S.C. 7429(a)(1)].
    Section 129(g)(1) of the Act broadly defines a solid waste 
incineration unit (``SWIU'') as ``a distinct operating unit of any 
facility which combusts any solid waste material from commercial or 
industrial establishments or the general public * * *.'' 42 U.S.C. 
7429(g)(1) (emphasis added). Section 129(g)(1) expressly states that 
``incinerators or other units required to have a permit under section 
3005 of the Solid Waste Disposal Act, 42 U.S.C. 6925'' shall not be 
considered a SWIU. That section also expressly excludes from the 
definition of SWIU the following units:

    (A) materials recovery facilities (including primary or 
secondary smelters) which combust waste for the primary purpose of 
recovering metals, (B) qualifying small power production facilities, 
as defined in section 769(17)(C) of Title 16, or qualifying 
cogeneration facilities as defined in section 796(18)(B) of Title 
16, which burn homogeneous waste (such as units which burn tires or 
used oil, but not including refuse-derived fuel) for the production 
of electric energy or in the case of qualifying cogeneration 
facilities which burn homogenous waste for the production of 
electric energy (such as heat) which are used for industrial, 
commercial, heating or cooling purposes, or (C) air curtain 
incinerators provided that such incinerators only burn wood wastes, 
yard wastes and clean lumber and that such air curtain incinerators 
comply with opacity limitations to be established by the 
Administrator by rule.

42 U.S.C. 7429(g)(1). Accordingly, with the exception of those solid 
waste incineration units that are expressly excluded from regulation by 
section 129(g)(1), Congress intended EPA to establish regulations for 
all SWIU's under section 129. This includes cement kilns that combust 
solid waste materials, including refuse-derived fuel.
    Section 129 is similar to section 112 of the Act in that both 
require EPA to establish performance standards that are based upon the 
performance of maximum achievable control technology (MACT). Section 
112(b), however, lists 188 hazardous air pollutants (HAPs) for 
potential regulation, and section 112(c)(6) requires EPA to establish 
performance standards under section 112(d) for categories of sources 
emitting seven specific pollutants, including the following HAPs 
emitted by cement kilns: mercury and dioxins/dibenzofurans [42 U.S.C. 
7412]. By comparison, section 129 expressly requires EPA to regulate 
emissions of the following criteria pollutants and HAPs--particulate 
matter, opacity (as appropriate), sulfur dioxide, hydrogen chloride, 
nitrogen oxides, carbon monoxide, lead, cadmium, mercury, and dioxins 
and dibenzofurans [42 U.S.C. 7429(a)(4)]. Section 129 also gives EPA 
the discretion to promulgate emission limitations or provide for the 
monitoring of postcombustion concentrations of surrogate substances or 
any other pollutant not expressly listed for regulation in section 
129(a)(4). [See 42 U.S.C. 7429(a)(4).] In addition, section 129 
contains other requirements not contained in section 112, such as 
operator training requirements. [See 42 U.S.C. 7429(d).]
    As stated previously, the regulations being proposed today are 
pursuant to section 112 of the Act and apply to all cement kilns except 
portland cement kilns and in-line kiln/raw mills that would be subject 
to the NESHAP for hazardous waste combustors. In today's notice, the 
EPA is proposing to establish emission limitations for particulate 
matter (as a surrogate for metals, except mercury), dioxins/furans, and 
total hydrocarbons (as a surrogate for organic HAPs) regardless of the 
material being combusted in the cement kiln. If EPA determines that 
additional regulations are required under section 129 for cement kilns 
that combust solid waste materials (e.g., cement kilns combusting 
materials containing more than 30-percent municipal solid waste or 
cement kilns combusting medical waste), then such regulations will be 
promulgated under section 129 and EPA will state clearly in the 
applicability section of those regulations when those standards apply 
and revise the applicability section of these regulations accordingly.
    At no time, will a cement kiln be expected to comply simultaneously 
with regulations promulgated pursuant to section 112 and regulations 
promulgated pursuant to section 129. Section 129(h)(1) expressly states 
that no solid waste incineration unit subject to performance standards 
under section 129 and section 111 shall be subject to standards under 
section 112(d) of the Act [42 U.S.C. 7429(h)(1)]. The EPA reads this 
provision to mean that for emissions potentially subject to section 
129, the Agency must elect whether to cover such emissions under that 
section, or under section 112. If EPA elects to cover emissions under 
section 129, those emissions must be excluded from regulation under 
section 112. For example, if a cement kiln combusts only fossil fuels, 
it would have to comply with the regulations being proposed today. If 
the kiln combusts a mixture of 50% coal and 50% non-hazardous solid 
waste, it would continue to comply with the regulations being proposed 
today until EPA promulgates regulations applicable to such kilns under 
section 129 of the Act. At that time, if the kiln is burning the 50% 
coal and 50% solid waste mixture, it would have to comply with the 
section 129 regulations as long as it continued to combust solid waste 
material. Thus, in the same way that installation of a particular type 
of combustion device determines which regulation is applicable, 
combustion of certain materials in that combustion device would 
determine whether the section 112 regulation or section 129 regulation 
is applicable.
    The EPA does not believe that this approach will subject cement 
kiln owners to duplicative regulations. As noted earlier, regulations 
under section 112 and section 129 are based on MACT. If EPA determines 
that additional regulations under section 129 are appropriate because 
cement kilns are combusting solid waste material, EPA would be required 
to promulgate additional MACT standards for the following pollutants 
pursuant to section 129(a)(4): opacity, sulfur dioxide, hydrogen 
chloride, nitrogen oxides, carbon monoxide, lead, cadmium, and mercury. 
The EPA also would determine whether the standards for particulate 
matter, total hydrocarbon, and dioxins/furans should be revised for 
kilns combusting solid waste materials [42 U.S.C. 7429(a)(4)].

B. Emission Limits and Requirements

    The proposed NESHAP for portland cement manufacturing would apply 
to both major and area sources of HAPs.

[[Page 14187]]

The affected sources for which emission limits are proposed include the 
kiln, in-line kiln/raw mill, clinker cooler, raw material dryer, and 
materials handling processes that include the raw mill, finish mill, 
raw material storage, clinker storage, finished product storage, 
conveyor transfer points, bagging and bulk loading and unloading 
systems (hereafter referred to as materials handling processes).
    The proposed NESHAP would limit emissions of HAPs from non-
hazardous waste (NHW) portland cement kilns, NHW in-line kiln/raw 
mills, and NHW kiln alkali bypasses. Kiln emission limits would not 
apply to kilns or in-line kiln/raw mills that will be subject to the 
NESHAP for various hazardous waste combustor (HWC) types, including 
cement kilns which burn hazardous waste.2
---------------------------------------------------------------------------

    \2\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    The kiln emission limits would apply to the kiln and in-line kiln/
raw mill gases and to kiln alkali bypass gases (which may or may not be 
discharged through a separate stack).
    The proposed rule would limit emissions of HAPs from raw material 
dryers, clinker coolers and materials handling processes, regardless of 
the type of fuel burned in the kiln. The proposed rule would limit PM 
(surrogate for non-volatile HAP metals) emissions from new and existing 
NHW kilns, NHW in-line kiln/raw mills, and clinker coolers at portland 
cement plants which are major sources. Particulate matter emitted from 
portland cement manufacturing contains quantities of metal HAPs such as 
compounds of arsenic, cadmium, chromium, lead, manganese, mercury, 
nickel, and selenium. Controlling PM emissions would also control 
emissions of HAP metals. A surrogate approach is used for particulate 
metal HAPs in the proposed NESHAP to allow easier and less expensive 
measurement, analysis, and monitoring requirements, and because the 
control techniques for non-volatile metal HAPs are the same as the 
control techniques for PM. Although trace amounts of mercury may be 
found in the particulate matter, it is generally considered a volatile 
metal, and appreciable reductions of mercury emissions are not expected 
through the use of PM controls. Opacity limits would also apply to NHW 
kilns, NHW in-line kiln/raw mills, clinker coolers, raw material 
dryers, and materials handling processes.
    The  proposed  rule  also  would  limit D/F emissions from new and 
existing NHW kilns and NHW in-line kiln/raw mills located at portland 
cement plants which are major or area sources of HAPs. In addition, the 
rule would limit total hydrocarbon (THC) as a surrogate for organic HAP 
emissions from new NHW kilns, new NHW in-line kiln/raw mills, and new 
raw material dryers at portland cement plants which are major sources. 
Kiln, in-line kiln/raw mill, and raw material dryer organic emissions 
contain various organic HAPs including, but not limited to, 
acetaldehyde, benzene, formaldehyde, hexane, naphthalene, styrene, 
toluene, and xylenes. Tables 2 and 3 present a summary of the proposed 
emission limits for new and existing portland cement affected sources.

 Table 2.--Summary of Proposed Emission Limitsa for Affected Sources at 
                         Portland Cement Plants                         
                             [Metric units]                             
------------------------------------------------------------------------
     Affected source and       Emission limit for    Emission limit for 
          pollutant             existing sources         new sources    
------------------------------------------------------------------------
NHW kiln and NHW in-line      0.15 kg/Mg dry feedd  0.15 kg/Mg dry feedd
 kiln/raw mill b PM.           and opacity levelb    and opacity levelb 
                               no greater than 20    no greater than 20 
                               percent.              percent.           
NHW kiln and NHW in-line      0.2 ng TEQ/dscm or    0.2 ng TEQ/dscm or  
 kiln/raw mill D/F b, c.       0.4 ng TEQ/dscm       0.4 ng TEQ/dscm    
                               with PM control       with PM control    
                               device operated at    device operated at 
                               204 deg.   204 deg.
                               C.                    C.                 
NHW kiln and NHW in-line      None................  50 ppmvd (as        
 kiln/raw mill THC.                                  propane).          
Clinker cooler PM...........  0.05 kg/Mg dry feed   0.05 kg/Mg dry feed 
                               and opacity level     and opacity level  
                               no greater than 10    no greater than 10 
                               percent.              percent.           
Raw material dryer and        10 percent opacity..  10 percent opacity. 
 materials handling                                                     
 processes (raw mill system,                                            
 finish mill system, raw                                                
 material storage, clinker                                              
 storage, finished product                                              
 storage, conveyor transfer                                             
 points, bagging, and bulk                                              
 loading and unloading                                                  
 systems) PM.                                                           
Raw material dryer THC......  None................  50 ppmvd (as        
                                                     propane).          
------------------------------------------------------------------------
a All concentration limits at 7 percent oxygen.                         
b Includes main and alkali bypass stacks.                               
c Applies to both major and area source portland cement plants.         
d If there is an alkali bypass stack associated with the kiln or in-line
  kiln/raw mill, the combined PM emission from the kiln or in-line kiln/
  raw mill and the alkali bypass must be less than 0.15 kg/Mg dry feed. 


 Table 3.--Summary of Proposed Emission Limits a for Affected Sources at
                         Portland Cement Plants                         
                             [English Units]                            
------------------------------------------------------------------------
     Affected source and       Emission limit for    Emission limit for 
          pollutant             existing sources         new sources    
------------------------------------------------------------------------
NHW kiln and NHW in-line      0.30 lb/ton dry feed  0.30 lb/ton dry feed
 kiln/raw mill b PM.           d and opacity level   d and opacity level
                               b no greater than     b no greater than  
                               20 percent.           20 percent.        
NHW kiln and NHW in-line      8.7 x 10-11 gr TEQ/   8.7 x 10-11 gr TEQ/ 
 kiln/raw mill D/F b, c.       dscf or 1.7 x 10-10   dscf or 1.7 x 10-10
                               gr TEQ/dscf with PM   gr TEQ/dscf with PM
                               control device        control device     
                               operated at 400  deg.F.        eq>400  deg.F.     
NHW kiln and NHW in-line      None................  50 ppmvd (as        
 kiln/raw mill THC.                                  propane).          
Clinker cooler PM...........  0.10 lb/ton dry feed  0.10 lb/ton dry feed
                               and opacity level     and opacity level  
                               no greater than 10    no greater than 10 
                               percent.              percent.           

[[Page 14188]]

                                                                        
Raw material dryer and        10 percent opacity..  10 percent opacity. 
 materials handling                                                     
 processes (raw mill system,                                            
 finish mill system, raw                                                
 material storage, clinker                                              
 storage, finished product                                              
 storage, conveyor transfer                                             
 points, bagging, and bulk                                              
 loading and unloading                                                  
 systems) PM.                                                           
Raw material dryer THC......  None................  50 ppmvd (as        
                                                     propane).          
------------------------------------------------------------------------
a All concentration limits at 7 percent oxygen.                         
b Includes main and alkali bypass stacks.                               
c Applies to both major and area source portland cement plants.         
d If there is an alkali bypass stack associated with the kiln or in-line
  kiln/raw mill, the combined PM emission from the kiln or in-line kiln/
  raw mill and the alkali bypass must be less than 0.30 lb/ton dry feed.

C. Performance Test and Compliance Provisions

    A performance test would be required to demonstrate initial 
compliance with each applicable numerical limit. Under the proposed 
standard, the owner or operator would use EPA Method 5, ``Determination 
of Particulate Emissions from Stationary Sources'' to measure PM 
emissions from kilns, in-line kiln/raw mills and clinker coolers. These 
tests would be repeated every 5 years. Kilns and in-line kiln/raw mills 
equipped with alkali bypasses would be required to meet the particulate 
standard based on combined emissions from the kiln exhaust and the 
alkali bypass. Owners or operators of in-line kiln/raw mills would be 
required to conduct a Method 5 performance test while the raw mill is 
operating and a separate Method 5 performance test while the raw mill 
is not operating. In conducting the Method 5 tests, a determination of 
the particulate matter collected in the impingers (``back half'') of 
the particulate sampling train would not be required.
    The opacity exhibited during the period of the initial Method 5 
performance test would be determined, if feasible, through the use of a 
continuous opacity monitor (COM). Where the control device exhausts 
through a monovent or where the use of a COM in accordance with the 
installation specifications of EPA Performance Specification (PS)-1 of 
appendix B to 40 CFR part 60, is not feasible, EPA Method 9, ``Visual 
Determination of the Opacity of Emissions from Stationary Sources'' 
would be used. Where the control device discharges through a FF with 
multiple stacks or an ESP with multiple stacks, the owner or operator 
would have the option of conducting an opacity test in accordance with 
Method 9, in lieu of installing a COM.
    Under the proposed standard, the owner or operator would use EPA 
Method 23, ``Determination of Polychlorinated Dibenzo-p-dioxins and 
Polychlorinated Dibenzofurans from Stationary Sources'' to measure D/F 
emissions from kilns and in-line kiln/raw mills. These tests would be 
repeated every 5 years. The temperature at the inlet to the PMCD during 
the period of the Method 23 performance test would be continuously 
recorded. If carbon injection is used for D/F control the carbon 
injection rate during the period of the Method 23 performance test 
would be monitored. Owners or operators of in-line kiln/raw mills would 
be required to conduct a Method 23 performance test, and monitor the 
temperature at the inlet to the PMCD while the raw mill is operating, 
and a separate Method 23 performance test and inlet temperature 
monitoring while the raw mill is not operating. If applicable, the 
carbon injection rate would be monitored during both performance tests. 
Where applicable, the exhausts from both the kiln or in-line kiln/raw 
mill and the alkali bypass would be required to meet the D/F standard.
    Under the proposed standard, the owner or operator would use a THC 
continuous emission monitor (CEM) to continuously measure THC emissions 
from new or reconstructed kilns, new or reconstructed in-line kiln/raw 
mills, and new raw material dryers. Owners or operators of new or 
reconstructed in-line kiln/raw mills would be required to demonstrate 
initial compliance by measuring THC emissions while the raw mill is 
operating and while the raw mill is not operating. The proposed 
standard for THC does not apply to the exhaust from the alkali bypass 
of kilns or in-line kiln/raw mills. Each THC CEM would be required to 
be designed, installed, and operated in accordance with EPA Performance 
Specification (PS)-8A of 40 CFR part 60, appendix B. 3
---------------------------------------------------------------------------

    \3\ The EPA proposed amendments to appendix B of 40 CFR part 60 
on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    Under the proposed standard, the owner or operator would use EPA 
Method 9, ``Visual Determination of the Opacity of Emissions from 
Stationary Sources'' to measure the opacity of gases discharged from 
raw mills, finish mills, raw material dryers and materials handling 
processes. These tests would be repeated every five years. A summary of 
proposed compliance and monitoring options is given in Table 4.

  Table 4.--Summary of Proposed Compliance Demonstration and Monitoring 
                              Requirements                              
------------------------------------------------------------------------
     Affected source and           Compliance            Monitoring     
          pollutant               demonstration          requirement    
------------------------------------------------------------------------
New and existing NHW kiln     EPA Method 5 a......  COM if feasible d, e
 and NHW in-line kiln/raw                            or daily EPA Method
 mill b, c PM.                                       9 visual opacity   
                                                     readings.          
New and existing NHW kiln     EPA Method 23 a.....  Monitor temperature 
 and NHW in-line kiln/raw                            at inlet to PM     
 mill b, c, h, i D/F.                                control device f   
                                                     and minimum carbon 
                                                     injection rate if  
                                                     activated carbon   
                                                     injection is used. 

[[Page 14189]]

                                                                        
New NHW kiln and NHW in-line  THC CEM (EPA PS-8A)   THC CEM (EPA PS-8A) 
 kiln/raw mill THC.            j.                    j                  
New and existing clinker      EPA Method 5 a......  COM d, g or daily   
 cooler PM.                                          EPA Method 9 visual
                                                     opacity readings.  
New and existing raw and      EPA Method 9 a, g...  Daily EPA Method 22 
 finish mill PM.                                     visual opacity     
                                                     readings or        
                                                     operation of bag   
                                                     break detectors.   
New and existing raw          EPA Method 9 a, g...  None.               
 material dryer and                                                     
 materials handling                                                     
 processes (raw mill system,                                            
 finish mill system, raw                                                
 material storage, clinker                                              
 storage, finished product                                              
 storage, conveyor transfer                                             
 points, bagging, and bulk                                              
 loading and unloading                                                  
 systems) PM.                                                           
New raw material dryer THC..  THC CEM (EPA PS-8A)   THC CEM (EPA PS-8A) 
                               j.                    j                  
------------------------------------------------------------------------
a Required initially and every 5 years thereafter.                      
b Includes main exhaust and alkali bypass.                              
c In-line kiln/raw mill to be tested with and without raw mill in       
  operation.                                                            
d Must meet COM performance specification criteria. If the fabric filter
  or electrostatic precipitator has multiple stacks, daily EPA Method 9 
  visual opacity readings may be taken instead of using a COM.          
e Opacity limit is 20 percent. Corrective action trigger is 15 percent. 
f Site-specific temperature limit at APCD inlet is established during   
  successful D/F emissions testing.                                     
g Opacity limit is 10 percent.                                          
h Alkali bypass is tested with the raw mill on.                         
i Temperature parameters determined separately with and without the raw 
  mill operating.                                                       
j EPA Performance Specification (PS)-8A. Proposed on April 19, 1996 at  
  61 FR 17358.                                                          

D. Monitoring Requirements

    The proposed rule requires owners or operators to monitor the 
opacity of gases discharged from kilns, in-line kiln/raw mills, alkali 
bypasses and clinker coolers using a COM, if a COM can be feasibly 
installed in accordance with PS-1 of appendix B to 40 CFR part 60. 
Where it is not feasible to install a COM, e.g., where the control 
device discharges through a monovent, the owner or operator would be 
required to monitor emissions by conducting daily Method 9 tests. Where 
the control device discharges through an FF with multiple stacks or an 
ESP with multiple stacks, the owner or operator would have the option 
of conducting daily tests in accordance with Method 9, in lieu of 
installing a COM. The duration of the Method 9 tests would be 30 
minutes. Owners or operators would also be required to determine kiln 
or in-line kiln/raw mill feed rate.
    The opacity limit for kilns and in-line kiln/raw mills would be 20 
percent. Any 30-minute average opacity reading greater than 20 percent 
determined by the COM or daily Method 9 test would be a violation of 
the standard. Any ten consecutive 30-minute average COM readings 
exceeding 15 percent, or any single 30-minute average Method 9 reading 
exceeding 15 percent would trigger a site-specific operating and 
maintenance plan, incorporated within the owner or operator's part 70 
permit. The owner or operator would be required to initiate the site-
specific operating and maintenance plan within one hour. If the opacity 
exceeds 15 percent for five percent of the operating time as determined 
by 30-minute average COM readings, or if the 30-minute average readings 
exceed 15 percent during five percent of the daily Method 9 tests, 
during any 180 day reporting period, the owner or operator would be 
required to develop and implement a quality improvement plan (QIP) 
consistent with subpart D of the draft approach to compliance assurance 
monitoring.4 The owner or operator would be required to 
implement the QIP as expeditiously as possible but in no case would the 
period for completing the implementation of the plan exceed 180 days. 
If the owner or operator determined that more than 180 days was 
required to complete the appropriate improvements, the owner or 
operator would be required to notify the permitting authority and 
obtain a site-specific resolution subject to the approval of the 
permitting authority.
---------------------------------------------------------------------------

    \4\ The EPA announced its intention to propose subpart D of 40 
CFR part 64 on August 13, 1996 at 61 FR 41991.
---------------------------------------------------------------------------

    The opacity limit for clinker coolers would be 10 percent, based on 
any 30-minute average COM or Method 9 reading.
    The proposed rule requires the owner or operator to monitor D/F 
emissions from kilns and in-line kiln/raw mill systems and to maintain 
the temperature at the inlet to the PMCD at a level no greater than 
either: (1) the higher of 400  deg.F or the level established during 
the successful Method 23 performance test plus five percent (not to 
exceed 25  deg.F) of the temperature measured in  deg.F during the 
successful compliance test, if D/F emissions were determined to be no 
greater than 0.15 ng toxic equivalent (TEQ)/dscm (6.5  x  
10-11 gr/dscf); (2) the higher of 400  deg.F or the level 
established during the successful Method 23 performance test, if D/F 
emissions were determined to be greater than 0.15 ng TEQ/dscm (6.5  x  
10-11 gr/dscf) but less than 0.2 ng TEQ/dscm (8.7  x  
10-11 gr/dscf); or (3) 400  deg.F if D/F emissions were 
greater than 0.2 ng TEQ/dscm (8.7  x  10-11 gr/dscf) but 
less than or equal to 0.4 ng TEQ/dscm (1.7  x  10-10 gr/
dscf).
    Owners or operators of in-line kiln/raw mills would be required to 
establish separate PMCD inlet temperatures applicable to periods when 
the raw mill is operating and periods when the raw mill is not 
operating. The appropriate ``raw mill operating status dependent'' PMCD 
inlet temperature could not be exceeded. Owners or operators of kilns 
or in-line kiln/raw mills equipped with alkali bypasses would be 
required to establish separate temperatures for the inlet to the kiln 
or in-line kiln raw mill exhaust PMCD and the kiln or in-line kiln 
alkali bypass PMCD.
    If carbon injection is used for D/F control, the carbon injection 
rate would be monitored, and maintained at a level equaling or 
exceeding the rate which existed during the successful Method 23 
performance test.
    The proposed rule requires the owner or operator to monitor THC 
emissions from the main exhaust of new and reconstructed kilns; the 
main exhaust of new and reconstructed in-line kiln/raw mills; and new 
and reconstructed raw

[[Page 14190]]

material dryers using a CEM installed in accordance with PS-8A in 40 
CFR part 60, appendix B.5
---------------------------------------------------------------------------

    \5\ The EPA proposed amendments to appendix B of 40 CFR part 60 
on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    The proposed rule requires the owner or operator to monitor the 
opacity from raw mills and finish mills either by conducting a daily 
six-minute test in accordance with Method 22, ``Visual Determination of 
Fugitive Emissions from Material Sources and Smoke Emissions from 
Flares'', or by installing, calibrating, operating and maintaining a 
bag break detection system. In the event that fugitive emissions are 
observed during the Method 22 test, the owner or operator would be 
required to conduct a 30-minute Method 9 test commencing within 24 
hours of the end of the Method 22 test. In addition, the owner or 
operator would be required to initiate, within one hour, a site-
specific operating and maintenance plan developed as part of the 
application for a part 70 permit.
    In the event that the bag break detection system alarm were 
triggered, the owner or operator would be required to initiate, within 
one hour, a site-specific operating and maintenance plan developed as 
part of the application for a part 70 permit.
    As required by the NESHAP general provisions (40 CFR part 63, 
subpart A), the owner or operator also must develop and implement a 
startup, shutdown, and malfunction plan.

E. Notification, Recordkeeping, and Reporting Requirements

    All notification, recordkeeping, and reporting requirements in the 
general provisions (40 CFR part 63, subpart A) would apply to portland 
cement manufacturing plants. These include: (1) Initial notification(s) 
of applicability, notification of performance test, and notification of 
compliance status; (2) a report of performance test results; (3) a 
startup, shutdown, and malfunction plan with semiannual reports of 
reportable events (if they occur); and (4) semiannual reports of excess 
emissions. If excess emissions are reported, the owner or operator 
would report quarterly until a request to return the reporting 
frequency to semiannual is approved.
    Owners and operators would also be required to prepare an operation 
and maintenance plan for kiln, in-line kiln/raw mill, raw mill and 
finish mill APCDs consistent with subpart D of the draft approach to 
compliance assurance monitoring (CAM).6 The operation and 
maintenance plan would become part of their operating permit required 
by 40 CFR part 70.
---------------------------------------------------------------------------

    \6\ The EPA announced its intention to propose subpart D of 40 
CFR part 64 on August 13, 1996 at 61 FR 41991.
---------------------------------------------------------------------------

    Under circumstances described in section III. D. of this preamble, 
kiln and in-line kiln/raw mill monitoring may trigger a requirement to 
prepare and implement a site-specific Quality Improvement Program 
(QIP), that will also be consistent with the draft CAM 
rule.7 Owners or operators would be required to report if a 
QIP were required, and to notify the permitting authority if a required 
QIP would take more than 180 days to implement.
---------------------------------------------------------------------------

    \7\ The EPA announced its intention to propose subpart D of 40 
CFR 64 on August 13, 1996 at 61 FR 41991.
---------------------------------------------------------------------------

    The NESHAP general provisions (40 CFR part 63, subpart A) require 
that records be maintained for at least 5 years from the date of each 
record. The owner or operator must retain the records onsite for at 
least 2 years but may retain the records offsite the remaining 3 years. 
The files may be retained on microfilm, microfiche, on a computer disk, 
or on magnetic tape. Reports may be made on paper or on a labeled 
computer disk using commonly available and compatible computer 
software.

IV. Impacts of Proposed Standards

A. Applicability

    The EPA estimates that there are currently 118 portland cement 
plants in the United States. All portland cement plants would be 
subject to the proposed standards. The following sources would be 
affected when located at a portland cement plant that is a major 
source:
    (1) New, reconstructed, and existing NHW kilns and NHW in-line 
kiln/raw mills including alkali bypasses that are not subject to the 
HWC NESHAP 8 would be subject to emission limits for PM, D/
F, and opacity;
---------------------------------------------------------------------------

    \8\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    (2) New and reconstructed NHW kiln main exhausts and new and 
reconstructed NHW in-line kiln/raw mills main exhausts, that are not 
subject to the HWC NESHAP,9 would be subject to an emission 
limit for THC;
---------------------------------------------------------------------------

    \9\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    (3) New and reconstructed raw material dryers would be subject to 
an emission limit for THC;
    (4) New, reconstructed, and existing clinker coolers would be 
subject to emission limits for PM and opacity; and
    (5) New, reconstructed, and existing raw material dryers, raw and 
finish mills, and material handling processes would be subject to an 
opacity limit.
    The following sources would be affected when located at a portland 
cement plant that is an area source: new, reconstructed, and existing 
NHW kilns and NHW in-line kiln/raw mills, including alkali bypasses, 
that are not subject to the HWC NESHAP,10 would be subject 
to emission limits for D/F.
---------------------------------------------------------------------------

    \10\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

B. Air Quality Impacts

    Nationwide baseline HAP emissions from portland cement 
manufacturing plants are estimated to be 260 Mg/yr (290 tpy) at the 
current level of control. The proposed standards would reduce emissions 
of HAPs by 82 Mg/yr (90 tpy) from baseline levels. Estimates of annual 
emissions of HAPs and expected reductions from implementation of the 
proposed standards are given in metric and English units in Tables 5 
and 6 (docket item II-B-76, docket item II-B-77). The following text 
reviews the information provided in Tables 5 and 6.

  Table 5.--Nationwide Annual Emissions of HAPS and Other Pollutants From Portland Cement Manufacturing Plants  
                                                 [Metric units]                                                 
----------------------------------------------------------------------------------------------------------------
                                                                  Baseline emissions (Mg/   Emission reduction  
               Source                         Pollutant                     yr)                   (Mg/yr)       
----------------------------------------------------------------------------------------------------------------
Kilns, in-line kiln/raw mills, and   HAP Metals a...............  150...................  35.                   
 alkali bypasses.                                                                                               
                                     PM a.......................  14,000................  3,400.                
                                     D/F (TEQ) b................  44 g/yr...............  16 g/yr.              
                                     Organic HAPs c.............  120...................  47.                   
                                     THC c......................  530...................  200.                  

[[Page 14191]]

                                                                                                                
Clinker coolers....................  HAP Metals a...............  1.1...................  0.18.                 
                                     PM a.......................  8,100.................  1,300.                
----------------------------------------------------------------------------------------------------------------
a These numbers pertain to existing sources only.                                                               
b These numbers pertain to both new and existing NHW kilns.                                                     
c These numbers pertain to new NHW kilns only.                                                                  


  Table 6.--Nationwide Annual Emissions of HAPS and Other Pollutants From Portland Cement Manufacturing Plants  
                                                 [English units]                                                
----------------------------------------------------------------------------------------------------------------
                                                                    Baseline emissions      Emission reduction  
               Source                         Pollutant                    (tpy)                   (tpy)        
----------------------------------------------------------------------------------------------------------------
Kilns, in-line kiln/raw mills, and   HAP Metalsa................  160...................  38.                   
 alkali bypasses.                                                                                               
                                     PMa........................  16,000................  3,800.                
                                     D/F (TEQ)b.................  0.096 lbs/yr..........  0.035 lbs/yr.         
                                     Organic HAPsc..............  130...................  52.                   
                                     THCc.......................  580...................  220.                  
Clinker coolers....................  HAP Metalsa................  1.2...................  0.2.                  
                                     PMa........................  8,800.................  1,400.                
----------------------------------------------------------------------------------------------------------------
a These numbers pertain to existing sources only.                                                               
b These numbers pertain to both new and existing NHW kilns.                                                     
c These numbers pertain to new NHW kilns only.                                                                  

    The proposed MACT standards would reduce PM emissions from the 
existing NHW cement kilns and in-line kiln/raw mills by 3,400 Mg/yr 
(3,800 tpy) from the baseline level, a reduction of 24 percent. 
Emissions of HAP metals from the affected existing NHW cement kilns and 
in-line kiln/raw mills would be reduced by 35 Mg/yr (38 tpy), a 
reduction of 24 percent from the baseline level. Emissions of D/F TEQ 
would be reduced by 15 grams (g)/yr (0.033 lb/yr), a reduction of 36 
percent from the baseline level, at existing NHW cement kiln and in-
line kiln/raw mills.
    For new NHW cement kilns and in-line kiln/raw mills, the MACT 
standards are projected to reduce emissions of D/F TEQ by an average of 
0.6 g/yr (0.001 lb/yr) over the next 5 years (from major and area 
sources), a 36 percent reduction from projected baseline emissions. For 
new kilns, the proposed standards would also reduce projected emissions 
of THC by an average of 200 Mg/yr (220 tpy) and organic HAPs by an 
average of 47 Mg/yr (52 tpy) over the next 5 years, an emissions 
reduction for each of 39 percent from corresponding estimated 
nationwide baseline emissions (docket item II-B-76).
    The proposed MACT standards would reduce PM emissions from 35 
percent of the existing clinker coolers by 1,300 Mg/yr (1,400 tpy) from 
the baseline level, a reduction of 16 percent. Emissions of HAP metals 
from the affected existing clinker coolers would be decreased by 0.18 
Mg/yr (0.2 tpy), a reduction of 16 percent from the baseline level.
    Additional reductions of THC and organic HAPs will result from the 
MACT standards for new raw material dryers. However, information on THC 
emission rates from raw material dryers and the number of such affected 
sources is not currently available, so nationwide reductions cannot be 
estimated.
    The MACT standards would also reduce PM emissions from raw material 
dryers, and other material handling processes. However, no impacts were 
estimated for these affected sources because there is no available 
information on typical PM emissions from the affected sources that do 
not meet the NSPS, and no information on the number of sources 
potentially affected by this MACT standard.

C. Water Impacts

    Control of D/F emissions using water injection for temperature 
reduction would result in an estimated increased water consumption 
(evaporated into the kiln exhaust gas for cooling) of 190 million 
gallons per year for existing NHW kilns and NHW in-line kiln/raw mills 
of 8 million gallons per year for new NHW kilns and NHW in-line kiln/
raw mills (docket item II-B-77).

D. Solid Waste Impacts

    The amount of solid waste from existing NHW kilns, in-line kiln/raw 
mills, and clinker coolers (located at major sources) would increase by 
an estimated 4,700 Mg/yr (5,200 tpy) due to the proposed standard for 
PM control (docket item II-B-77).

E. Energy Impacts

    For existing NHW kilns and NHW in-line kiln/raw mills the proposed 
MACT standards for PM and D/F would increase energy consumption by an 
estimated 11 million kilowatt hours (KWh)/yr [38 billion British 
thermal units (Btu)/yr]. For new NHW kilns and NHW in-line kiln/raw 
mills the proposed MACT standards for D/F would increase energy 
consumption by an estimated (docket item II-B-77) 10,600 KWh/yr (36 
million Btu/yr).

F. Nonair Health and Environmental Impacts

    The reduction in HAP emissions would have a beneficial effect on 
nonair health and environment impacts. D/F and HAP metals have been 
found in the Great Lakes and have been listed as pollutants of concern 
due to their persistence in the environment, potential to 
bioaccumulate, and toxicity to humans and the environment (docket item 
II-A-31, pp. 18 to 21). Implementation of the proposed

[[Page 14192]]

NESHAP would aid in reducing aerial deposition of these emissions.
    Occupational exposure limits under 29 CFR part 1910 are in place 
for some of the regulated HAPs (and surrogates) except D/F. The 
National Institute for Occupational Safety and Health recommends an 
exposure level for D/F at the lowest feasible concentration (docket 
item II-I-45, p. 124). The proposed NESHAP would reduce emissions, and 
consequently, occupational exposure levels for plant employees.

G. Cost Impacts

    For existing NHW kilns, NHW in-line kilns/raw mills, clinker 
coolers, raw and finish mills, and materials handling facilities, the 
projected total capital costs (including estimated monitoring costs) of 
the proposed standard for controlling emissions of PM and D/F are $87 
million. The projected annual costs (including monitoring costs) for 
these controls are $27 million. For new NHW kilns and NHW in-line kiln/
raw mills, the projected total capital and annual costs of the MACT 
standard for D/F are $390,000 and $89,000, respectively. No capital and 
annual costs are projected for new and reconstructed NHW kilns, NHW in-
line kilns/raw mills, and clinker coolers as a result of the proposed 
standard for PM because these sources will be required to comply with 
the existing NSPS for portland cement plants (40 CFR part 60, subpart 
F). The proposed THC emissions limit for new NHW kilns and NHW in-line 
kiln/raw mills can be met by processing materials with typical levels 
of organic content, without installing and operating add-on pollution 
control systems that would be relatively costly. Feed materials that 
have sufficiently low levels of organic matter are widespread across 
the U.S., and the siting of new kilns is not expected to be 
significantly limited by the proposed emission limit. Information is 
not available to quantify the costs of excluding deposits of feed 
materials with the highest levels of organic constituents as the 
primary feed for new kilns. Owners/operators of the few existing cement 
plants that process feed materials containing relatively high levels of 
organic material, and who desire to expand production through the 
addition of a new kiln, would need to blend their existing feed 
materials with lower THC materials from offsite, or selectively process 
lower organic portions of the feed materials from the onsite mine or 
quarry in the new kiln. Regarding the costs of monitoring, for new NHW 
kilns and in-line kiln/raw mills, the projected fifth-year national 
capital and annual costs of monitoring THC with a continuous emission 
monitor at an estimated four new kilns are $576,000 and $340,000, 
respectively (docket item II-B-77).

H. Economic Impacts

    An economic analysis of the proposed NESHAP was conducted. The EPA 
estimates that regional market price increases would be between 0.6 and 
2.0 percent. The national average price increase is estimated to be 1.1 
percent. The related decreases in quantity demanded are estimated to 
range from 0.5 to 1.8 percent, with a national average of 0.9 percent. 
Domestic production is estimated to decrease more than consumption (1.7 
percent compared to 0.9 percent nationally because imports are 
estimated to increase by 6.3 percent). The decreases in domestic 
production may lead to the loss of approximately 230 jobs. No plants 
are expected to close; two kilns are expected to cease operating 
(docket item II-A-46).

V. Selection of Proposed Standards

A. Selection of Source Category

    Section 112(c) of the Act directs the Agency to list each category 
of major and area sources, as appropriate, that emits one or more of 
the HAPs listed in section 112(b) of the Act. The EPA published an 
initial list of source categories on July 16, 1992 (57 FR 31576), and 
revised the list on June 4, 1996 (61 FR 28197). ``Portland Cement 
Manufacturing'' is one of the 174 categories of sources on the initial 
list. As defined in the EPA report, ``Documentation for Developing the 
Initial Source Category List'' (docket item II-A-18), the Portland 
Cement Manufacturing source category includes any facility engaged in 
manufacturing portland cement by either the wet or dry process. The 
category as described for the listing includes but is not limited to 
the following process facilities: kiln, clinker cooler, raw mill 
system, finish mill system, raw material dryer, raw material storage, 
clinker storage, finished product storage, conveyor transfer points, 
bagging, and bulk loading and unloading systems.
    The term ``major source'' is defined under section 112(a)(1) of the 
Act and in the EPA general provisions (40 CFR 63.2) as:

    * * * any stationary source or group of stationary sources 
located within a contiguous area under common control that emits or 
has the potential to emit considering controls, in the aggregate, 10 
tons per year or more of any hazardous air pollutant or 25 tons per 
year or more of any combination of hazardous air pollutants * * *

This definition of major source has been upheld in a recent decision, 
National Mining Ass'n v. EPA, 59 F.3d 1351 (D.C. Cir. 1995). In this 
case, the Court also concluded that ``EPA may require the inclusion of 
fugitive emissions in a site's aggregate emissions without conducting 
any special rule making'' for the purpose of determining whether a 
source is major.
    The listing of the portland cement major source category was based 
on the Administrator's determination that some portland cement plants 
would be major sources of particulate HAPs, including but not limited 
to compounds of arsenic, cadmium, chromium, lead, manganese, mercury, 
nickel, and selenium. Information and data have been compiled by the 
EPA characterizing the portland cement manufacturing process and its 
associated emission sources. There are three main steps to 
manufacturing portland cement: (1) kiln feed preparation (i.e., 
crushing and grinding), (2) firing the raw mix in a rotary kiln to 
produce clinker (including fuel handling), and (3) clinker grinding to 
produce cement. The responses received from the information collection 
request (ICR) that was sent to every company in the industry indicated 
that HAP emissions have been identified from all steps in the 
manufacturing process. The kiln feed preparation and clinker grinding 
operations all produce particulate emissions, a fraction of which are 
metal HAPs. The responses also showed that HAPs are emitted from the 
clinker production step; the kiln exhaust gases contain metal HAPs, 
organic HAPs, and HCl.
    All kiln exhaust gases are controlled at the existing plants by 
either FFs or ESPs to limit PM emissions. Based on currently available 
data, there are no plants that would be defined as major sources 
according to section 112(a) of the Act on the basis of the mass of 
metal HAPs emitted from kilns. That is, the reported emissions, 
considering controls, did not exceed 9.1 Mg/yr (10 tpy) of a single 
metal HAP or greater than 22.7 Mg/yr (25 tpy) of a combination of metal 
HAPs from a cement kiln. However, operators of portland cement plants 
must include HAP emissions from fugitive sources in determining whether 
their facility is a major source of HAP emissions. Fugitive sources may 
emit enough HAP metals to make a plant a major source (when fugitive 
emissions are combined with all other HAP emissions at the site).
    ICR responses for individual plants did show quantities of hydrogen 
chloride (HCl) and chlorine each being emitted in excess of 9.1 Mg/yr 
(10 tpy).

[[Page 14193]]

Most HCl emissions (reported in the ICR responses) were measured by EPA 
Method 26, a method that may underestimate HCl emissions by a factor of 
2 to 25 (docket item II-I-121). Results of Fourier Transform Infrared 
(FTIR) spectroscopy emissions tests suggest that most plants may be 
major sources of HCl. Hydrochloric acid concentrations of two wet 
process portland cement kiln exhaust gases (docket item II-A-20, docket 
item II-A-40) determined by FTIR spectroscopy ranged from 11 parts per 
million by volume (ppmv) to 110 ppmv (dry basis corrected to 7 percent 
oxygen). Assuming an average HCl emission of 50 ppmv (dry basis, 
corrected to 7 percent oxygen), a wet kiln producing 600,000 tpy of 
clinker would emit approximately 150 tpy of HCl.
    Some plants reported formaldehyde, benzene, and toluene emissions 
each to be in excess of 9.1 Mg/yr (10 tpy). One plant injects activated 
carbon into the kiln exhaust to reduce the plume opacity thought to be 
caused by hydrocarbons in the feed (docket item II-B-35). Various 
organic HAPs were detected in its kiln exhaust using FTIR spectroscopy 
(docket item II-A-41). Based on the kiln operating 330 d/yr, 24 hr/d, 
kiln emissions were estimated at 331 Mg/yr (365 tpy) of hexane, 29 Mg/
yr (32 tpy) of benzene, 27 Mg/yr (30 tpy) of toluene, 15 Mg/yr (16 tpy) 
of naphthalene, and 12 Mg/yr (13 tpy) chlorobenzene (docket item II-A-
41, docket item II-B-76).
    Based on ICR responses, acetaldehyde, acrylonitrile, arsenic 
compounds, lead compounds, manganese compounds, mercury compounds, 
naphthalene, phosphorus, styrene, and xylenes were emitted at rates of 
one tpy or greater from at least one portland cement kiln (docket item 
II-B-69). The analysis of HAP emissions data from portland cement 
manufacturing plants summarized above indicates that most if not all 
cement plants are major sources of HAP emissions.
    Consideration of subcategories or classes. Section 112(d)(1) of the 
Act provides that the Administrator may distinguish among classes, 
types and sizes of sources within a category or subcategory in 
establishing standards. The EPA reviewed the listed source category to 
determine if different classes were warranted. All portland cement is 
manufactured in direct-fired, rotating kilns. In 1993, 210 kilns at 118 
plants were in operation throughout the nation and Puerto Rico (docket 
item II-I-101).
    There are two main portland cement manufacturing processes 
differentiated on the basis of feed preparation: wet process and dry 
process. Approximately one-third of the kilns in operation use a wet 
process; the other two-thirds use a dry process. The trend in the 
industry for new kilns is toward the dry process because it is more 
energy efficient than the wet process. Within the dry process there are 
three variations: long kiln dry process, preheater process, and 
preheater/precalciner process. The wet process kilns and all variations 
of the dry process kilns use the same raw materials and use the same 
types of pollution controls for PM emissions (docket item II-C-94, 
attachment chapters 2 and 3). Based on ICR responses and test data the 
use of these pollution controls to meet the NSPS for PM is feasible for 
wet kilns and all types of dry kilns. Likewise test data show that 
lowering kiln exhaust gas temperature to 400 deg. F at the APCD inlet, 
MACT for reducing D/F concentrations, is feasible for wet and all types 
of dry kilns. In any event, if classes were defined based on process 
type, the MACT floor technology would be identical (docket item II-B-
73). For this reason, the EPA does not propose classes based on process 
type.
    The EPA OSW has recently proposed NESHAPs for various HWC types, 
including cement kilns which burn hazardous waste.11 The 
proposal is consistent with the terms of the 1993 settlement agreement 
between the Agency and a number of groups that challenged EPA's final 
RCRA rule entitled ``Burning of Hazardous Waste in Boilers and 
Industrial Furnaces'' (56 FR 7134, February 21, 1991) and with the 
Agency's Hazardous Waste Minimization and Combustion Strategy that was 
first announced in May 1993. Hazardous waste burning cement kilns are 
included in the portland cement manufacturing source category, but are 
subject to different regulations than the NHW kilns. This proposed 
NESHAP for portland cement manufacturing covers only NHW kilns and NHW 
in-line kiln/raw mills. However, this proposed NESHAP does cover the 
other affected sources (including clinker coolers, raw material dryers, 
and materials handling processes) located at manufacturing plants 
regardless of whether the plant has hazardous waste-burning cement 
kilns.
---------------------------------------------------------------------------

    \11\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    Decision to regulate portland cement area sources. Section 
112(c)(6) of the Act states that by November 15, 2000, EPA must list 
and promulgate section 112(d)(2) or (d)(4) standards (i.e., standards 
reflecting MACT) for categories (and subcategories) of sources emitting 
seven specific pollutants, including the following HAPs emitted by 
cement kilns: mercury, 2,3,7-8 tetrachlorodibenzofuran, and 2,3,7-8 
tetrachlorodibenzo-p-dioxin. (Although other 112(c)(6) HAPs have been 
found in cement kiln exhaust, the majority of the emissions data and 
concern for NHW cement kiln 112(c)(6) HAPs is for mercury and dioxin/
furans.) The EPA must assure that source categories accounting for not 
less than 90 percent of the aggregated emissions of each enumerated 
pollutant are subject to MACT standards. Congress (docket item II-I-13, 
p. 155 to 156) singled out the HAPs enumerated in section 112(c)(6) as 
being of ``specific concern'' not just because of their toxicity but 
because of their propensity to cause substantial harm to human health 
and the environment via indirect exposure pathways (i.e., from the air 
through other media, such as water, soil, food uptake, etc.). 
Furthermore, these pollutants have exhibited special potential to 
bioaccumulate, causing pervasive environmental harm in biota (and, 
ultimately, human health risks).
    The EPA estimates that approximately five tons of mercury are 
emitted annually in aggregate from NHW cement kilns at portland cement 
plants in the U.S. (docket item II-B-65). Also, it is estimated that 
NHW kilns emit in aggregate approximately 22 lb of D/F (or about 0.10 
lb TEQ per year (docket item II-B-57, docket item II-B-76). To assure 
that these pollutants are subject to MACT, EPA is proposing to add the 
portland cement manufacturing area source category to the list of 
source categories and subcategories listed pursuant to section 
112(c)(6). [See 62 FR 33625, 33637-38; June 20, 1997.] The EPA is doing 
so because area and major source cement kilns emit these HAPs in 
roughly equal quantities, because the dioxins and furans emitted by 
area sources are equally toxic as those emitted by major sources (i.e., 
the distribution of dioxin and furan isomers is the same for both area 
and major sources), and because these are particularly toxic HAPs. In 
addition, EPA is already counting on control of these pollutants from 
cement kiln area sources through the MACT process in assuring that 
sources accounting for at least 90 percent of the emissions of these 
HAPs are subject to standards under section 112(c)(6). [See 62 FR at 
33635, 33636; June 20, 1997.]
    The EPA notes, however, as it did in the June 20th notice, that 
although the section 112(c)(6) listing process makes sources subject to 
standards under subsection (d)(2) or (d)(4), the language of section 
112(c)(6) does not specify

[[Page 14194]]

either a particular degree of emissions control or a reduction in these 
specific pollutants emissions to be achieved by such regulations. 
Rather, the specific control requirements will result from determining 
the appropriate level of control under MACT [section 112(d)(2), or 
section 112(d)(4)], and this interpretation will be made during the 
section 112(d) rulemakings affecting the particular source category, 
not as part of the section 112(c)(6) listing process. [See 62 FR at 
33631; June 20, 1997.]
    As noted above, EPA is interpreting section 112(c)(6) to require 
the Agency to establish standards under section 112(d)(2) or 112(d)(4) 
for all sources listed pursuant to section 112(c)(6), whether such 
sources are major or area sources. This interpretation reflects the 
express language of section 112(c)(6) that sources * * * of each such 
pollutant are subject to standards under subsection (d)(2) or (d)(4) 
and is in accord with the function of section 112(c)(6):

    To assure that sources emitting significant amounts of the most 
dangerous HAPs are subject to the rigorous MACT standard-setting 
process.

[See S. Rep. No. 228, 101st Cong. 1st Sess., pp. 155, 166.]
    The EPA has in fact already adopted this interpretation in the 
proposed rule for hazardous waste combustion sources.
[See 61 FR at 17365; April 19, 1996.]
    Under an alternative interpretation of section 112(c)(6), the 
Agency might also establish standards pursuant to section 112(d)(5)--
based on generally available control technology (GACT)--for area 
sources listed under section 112(c)(6). Section 112(d)(5) states that 
for categories and subcategories of area sources listed pursuant to 
subsection 112(c), the Administrator may establish standards pursuant 
to GACT rather than MACT. Although the reference to listing area 
sources may have been intended to refer to the area source listing 
process in section 112(c)(3), it arguably extends to listing under 
section 112(c)(6) as well. The Agency requests comment on the use of 
this alternative approach to standard-setting for area sources listed 
under section 112(c)(6).
    In addition, the EPA is interpreting section 112(c)(6) to require 
that, for sources listed under section 112(c)(6), MACT [or section 
112(d)(4)] controls apply only to the section 112(c)(6) HAPs emitted by 
the source. Thus, in this proposed rule, only mercury, D/F, and POM 
(using THC as a surrogate) emitted by cement kiln area sources would be 
subject to the MACT standards. The EPA is aware that it proposed a 
different interpretation in the hazardous waste combustion NESHAP (see 
61 FR at 17365-66), but now believes that section 112(c)(6) is better 
read to apply only to particular HAPs rather than to the entire source. 
(Since the language of section 112(c)(6) is ambiguous as to whether the 
entire source must comply with MACT, or just for the HAPs enumerated in 
section 112(c)(6), [see 61 FR at 17365 n. 12], either interpretation is 
legally permissible.) Applying the provision to the entire source could 
result in applying MACT to all HAPs emitted by area sources under 
circumstances where control would not otherwise be warranted.

B. Selection of Emission Sources

    The portland cement manufacturing process consists of the following 
unit operations:
    (1) Grinding the carefully proportioned raw materials to a high 
degree of fineness;
    (2) firing the raw mix in a rotary kiln to produce clinker;
    (3) grinding the resulting clinker to a fine powder and mixing with 
gypsum to produce cement; and
    (4) raw and finished materials handling.
    The following sections include descriptions of the affected sources 
in the portland cement manufacturing source category, the origin of 
emissions from these affected sources, and factors affecting the 
emissions. The affected sources for which MACT standards are being 
proposed include the kiln, in-line kiln/raw mills, clinker cooler, raw 
and finish mills, raw material dryer, and materials handling processes.
1. Feed Preparation Processes (Grinding, Conveying)
    Oxides of calcium, silicon, aluminum, and iron comprise the basic 
ingredients of cement. The calcareous raw materials include limestone, 
chalk, marl, sea shells, aragonite, and an impure limestone known in 
the industry as natural cement rock. The requisite silica and alumina 
may be derived from clay or shale from a limestone quarry. Such 
materials usually contain some of the required iron oxide, but many 
plants need to supplement the iron with mill scale, pyrite cinders, or 
iron ore. Silica is supplemented, if necessary by adding sand to the 
raw mix; alumina may be supplemented by adding bauxite or alumina-rich 
flint clays to the raw mix (docket item II-I-5, p. 180).
    Industrial by-products and wastes are becoming more widely used as 
feed materials for cement production, e.g., slags contain carbonate-
free lime, as well as substantial levels of silica and alumina. Fly ash 
from coal-fired boilers can often be a suitable feed component, since 
it is already finely dispersed and provides silica and alumina (docket 
item II-I-5, p. 180).
    Ball mills are used to grind the feed material to the required 
fineness for both the wet and dry processes. In the wet-kiln process, 
the raw materials are ground with water to produce a well-homogenized 
slurry. In the dry-kiln process, raw materials are ground in closed-
circuit ball mills with air separators.
    Emissions from the grinding and conveying operations are 
essentially particulate emissions (e.g., dust from limestone, clay, 
bauxite ore) which contain HAP metals. Particulate matter control 
devices (FFs and ESPs) serve as HAP control devices. The quantity of 
emissions of HAP metals from raw materials handling processes are site 
specific and depend on dust control practices and weather conditions.
2. Feed Preparation Processes (Drying, Blending, Storage)
    Drying of kiln feed materials can be carried out in separate units 
that are gas-or coal-fired. However, to improve the process energy 
efficiency, waste heat can be utilized directly in the mill by routing 
the kiln gases through the raw mill. The catch from the APCDs that 
follow the raw mill is returned to the process and therefore, the APCD 
is also part of the process (docket item II-I-109, chapter 11.6). Where 
kiln gases are routed through the raw mill, emissions from the combined 
in-line kiln/raw mills must be controlled for the same pollutants and 
to the same extent as kiln gases.
    The more energy efficient preheater and preheater/ precalciner 
kilns usually route the exhaust gas from the preheater to a raw mill to 
dry the material in suspension in the mill. The gas stream exits the 
raw mill heavily laden with kiln raw material and is exhausted to an 
APCD to recover the raw material and any material entrained from the 
kiln preheater system. The raw material is collected and fed to a 
blending system to provide the kiln with a homogenous raw feed. Dry 
process blending is usually accomplished in a silo with compressed air 
(docket item II-I-5, p. 183).
    If the raw material dryer uses heat from a separate combustion 
source (fuel-fired raw material dryer), exhaust gases may contain trace 
quantities of products of incomplete combustion (PICs), HCl, and metals 
from the fuel. In addition, if the feed materials contain organic 
matter, this material may volatilize in the raw material dryer 
(regardless of the

[[Page 14195]]

source of the heat) and the dryer exhaust may contain organic HAPs. 
Under the NSPS, emissions from the raw material dryer and the feed 
preparation materials handling processes (raw mill system, raw material 
storage, and conveyor transfer points) are currently subject to a limit 
of 10 percent opacity.
3. Kiln
    The high temperature processing required to produce portland cement 
takes place in the rotary kiln. The rotary kiln consists of a 
refractory-brick-lined cylindrical steel shell that is rotated by an 
electrical drive. It is a countercurrent heating device slightly 
inclined so that material fed into the cooler, upper end travels slowly 
by gravity to be discharged onto the clinker cooler from the hotter, 
lower discharge end. The burners at the firing end, i.e., the lower or 
discharge end, produce a current of hot gases that heats the clinker 
and the calcined and raw materials in succession as the gases pass 
toward the feed end. As has been mentioned, a kiln can be classified as 
wet (in which the kiln feed is a slurry) or dry. Dry process kilns 
include the older-style, long dry process kiln with a single firing 
point; the preheater/kiln system; and the preheater/precalciner kiln 
system. In the preheater/precalciner system, a second burner is used to 
carry out calcination in a separate vessel interposed between the 
preheater and the kiln. The precalciner uses preheated combustion air 
drawn from the clinker cooler and the kiln exit gases and is equipped 
with an oil or coal burner that burns 50 to 60 percent of the total 
kiln fuel input. The precalciner system permits the use of smaller 
kilns since only the actual clinkering process is carried out in the 
rotary kiln.
    The kiln exhaust contains a wide variety of HAPs and other air 
pollutants that originate from the fuel combustion and from the feed 
material. In 1991, about 87 percent of the total U.S. kiln capacity 
used coal, coke, or a combination of coal and coke as the primary fuel 
(docket item II-I-42, p. 20). Only 3.5 percent of the kiln capacity is 
fired with natural gas alone (not in combination with other fuels) and 
oil as a primary fuel represented an insignificant fraction of the 
total kiln capacity. Plants firing waste-derived fuels account for the 
balance of the total capacity. The most common waste fuels used in 
cement kilns are RCRA hazardous waste, tires and tire-derived fuel. To 
a lesser extent, MSW, medical waste, and used motor oil are fired.
    Feed materials are a source of gaseous organic HAP emissions. Some 
feed materials contain organic carbon such as petroleum or kerogens. 
The organic carbon can volatilize in the kiln and appear at the stack 
exit as a ``blue haze'' which may contain organic HAPs. During one EPA-
sponsored test at a cement kiln using feed material with a high organic 
matter content, significant levels of benzene (32 tpy) were detected in 
the kiln exhaust (docket item II-A-41, docket item II-B-76). Organic 
HAP emissions were found to vary with THC emissions during this test.
    Chlorine entering the kiln system (from raw materials and also from 
fuels) may react with the organic compounds present in the raw 
materials or with PICs, to form chlorinated hydrocarbons or D/F in the 
kiln stack exhaust. Approximately 20 percent of the HAPs listed in 
section 112 of the Act are chlorinated organic compounds.
    In the wet process and in the long kiln dry process, the emission 
point for the kiln gases is typically the APCD discharge stack. In the 
more complex preheater and precalciner process designs, the kiln gases 
are routed through other pieces of process equipment, such as the raw 
mill. In-line kiln/raw mills vent kiln gases through the raw mill. In 
these systems the gases discharged from the APCD on the raw mill, are 
in fact kiln exhaust gases.
    The kiln alkali bypass stack is an additional emission point for 
kiln gases which is sometimes found with preheater and precalciner 
processes. The alkali bypass gas streams are kiln gases that have not 
contacted the incoming feed material. The kiln gases that are drawn out 
of the kiln prior to contact with the precalciner and preheater 
sections pass through a separate APCD and may be discharged to the 
atmosphere through a separate stack. In other process arrangements, the 
treated alkali bypass gases are combined with the main kiln exhaust 
gases and are discharged through a common stack. It is expected that 
the same HAPs found in the main kiln stack are found in the alkali 
bypass stack.
    Kiln PM/HAP metals. All HAP metals have been identified in kiln 
exhaust PM at various levels. Based on analysis of emissions test 
reports, the total average HAP metal content of kiln exhaust PM is 
approximately one weight percent (docket item II-B-36). Mass emission 
rates of metal HAPs from the kiln depend on the concentration of metals 
in the PM and the emission rates of PM. Analyses of emissions data 
(docket item II-B-62) have shown that ESP-controlled PM emissions for 
six NHW kilns ranged from 0.009 to 0.20 gr/dscf (corrected to seven 
percent oxygen), with an average of 0.045 gr/dscf for 14 data points. 
Fabric filter-controlled PM emissions for five NHW kilns ranged from 
0.002 to 0.29 gr/dscf (corrected to seven percent oxygen), with an 
average of 0.014 gr/dscf for 10 data points. For a 600,000 ton of 
clinker/year kiln (this represents the capacity of a mid-sized kiln), 
the range of kiln PM emissions (0.002 gr/dscf to 0.29 gr/dscf) 
corresponds to 9 tpy to 1,360 tpy (docket item II-B-76). Based on an 
average kiln PM emission of 0.03 gr/dscf, and assuming HAP metal 
emissions are one percent by weight of PM emissions, HAP metal 
emissions are approximately 1.4 tpy for a 600,000 ton of clinker/year 
kiln (docket item II-B-76). Based on ICR responses, at least one plant 
reported kiln emissions of over one tpy for one or more of the 
following metal HAPs: chromium, lead, arsenic, mercury, antimony, and 
manganese. However, no plant reported kiln emissions of more than 10 
tpy of any single metal HAP (docket item II-B-69).
    Kiln mercury. Mercury may be emitted in the kiln exhaust as either 
a particulate or a gas. A summary was compiled of all currently 
available mercury emission data for HW and NHW kilns (docket item II-B-
65). There are 8 data points for 7 NHW kilns, and 19 data points from 
21 HW kilns (two sets of kilns shared a stack). The HW kiln data were 
adjusted to remove mercury in the HW fuel and any mercury spikes. By 
removing the portion of emissions attributed to test method spiking and 
HW fuel mercury inputs, corrected emission data that are comparable 
with data from NHW kilns were developed.
    For a 600,000 ton of clinker/year kiln, the range of the mercury 
emissions data [0.6 to 83 micrograms (g)/dscm at 7 percent 
oxygen] corresponds to 0.0012 tpy to 0.17 tpy (docket item II-B-76), 
while the average mercury emission (24 g/dscm) corresponds to 
approximately 0.05 tpy (docket item II-B-76). One plant responding to 
the ICR reported mercury emissions of over one ton per year.
    Kiln D/F. For the purposes of analysis of the data, concentrations 
of dioxin and furan congeners (specifically the tetra, hepta, hexa, and 
octa congeners) were converted to a concentration that was equivalent 
to the toxicity of 2,3,7,8-tetrachlorodibenzo-p-dioxin. Determination 
of TEQ concentrations was performed according to the international 
method (docket item II-A-8).
    An analysis of all available D/F emission data from 15 NHW kilns 
showed that concentrations of D/F TEQ emitted in the kiln exhaust gas 
measured downstream of the PMCD

[[Page 14196]]

ranged from 0.001 ng TEQ/dscm to over 1.2 TEQ ng/dscm with an average 
of 0.20 ng TEQ/dscm (all concentrations at 7 percent oxygen)[D/F test 
data are shown in Table 8 in Section V.D.2]. For a 600,000 ton of 
clinker/year kiln, the range of the D/F TEQ concentrations (0.001 to 
1.2 ng/dscm) corresponds to 0.0018 g/yr to 2.2 g/yr (docket item II-B-
76), while the average concentration (0.20 ng TEQ/dscm) corresponds to 
an emission of 0.4 g TEQ/year (docket item II-B-76).
    The predominant factor affecting D/F emissions is the temperature 
of gases at the inlet to the PMCD (docket item II-I-81, docket item II-
I-82). Test data collected from both HW and NHW kilns show a trend of 
decreasing D/F gas stream concentrations with decreasing temperature at 
the inlet to the PMCD. In tests conducted on individual cement kilns 
where the gas stream temperature was varied in the range of 350 to 
500 deg.F, reductions in D/F TEQ concentrations by factors of 5 to 10 
were observed when gas temperatures entering the PMCD were lowered from 
the upper to lower end of the temperature range (docket item II-I-81, 
docket item II-I-82).
    Kiln THC/organic HAPs. The THC and organic HAP concentrations and 
emission levels from kilns vary widely, depending primarily on the feed 
materials (docket item II-I-66, docket item II-I-67, docket item II-I-
68). Some feed materials contain organic carbon such as petroleum or 
kerogens. One kiln operator has conducted an extensive study of the 
source of high THC and carbon monoxide (CO) emissions from the kiln 
(docket item II-I-107). Higher than normal emissions from this kiln 
were attributed to the shale used in the raw materials. Replacing the 
shale with fire clay in the raw mix resulted in a dramatic reduction of 
THC and CO emissions.
    Another NHW kiln operator has determined that the raw materials are 
the source of the majority of the observed benzene emissions (docket 
item II-D-112). Kiln stack gas and preheater gas stream analyses before 
and after switching fuel from a combination of coal and petroleum coke 
to 100 percent natural gas showed little effect on benzene emissions. 
These test data suggest that benzene emissions derived from the raw 
materials (docket item II-I-41).
    Fourier transform infrared spectroscopy was used to determine 
organic HAP emissions at a NHW kiln. Estimated organic HAP emissions 
(based on average concentrations measured in the kiln exhaust and 7,920 
hr/yr of operation) showed that the kiln was a major source based on 
organic HAP emissions. Organic HAP emission rates were estimated at 331 
Mg/yr (365 tpy) hexane, 27 Mg/yr (30 tpy) toluene, 29 Mg/yr (32 tpy) 
benzene, 14.5 Mg/yr (16 tpy) naphthalene, and 12 Mg/yr (13.2 tpy) 
chlorobenzene (docket item II-A-41, docket item II-B-76).
    In the ICR responses, many organic HAPs were reported as being 
emitted in the kiln exhaust gas. Organic HAPs for which there was at 
least one report of emissions of at least 0.91 Mg/yr (1.0 tpy) include 
benzene, naphthalene, toluene, formaldehyde, xylenes, styrene, and 
acetaldehyde. One facility reported more than 9.1 Mg/yr (10 tpy) each 
of benzene and toluene emissions (docket item II-B-69).
    Stack concentrations of THC were available for 16 NHW kilns (docket 
item II-B-75). The concentrations were expressed in ppmv as propane on 
a dry basis (ppmvd) at seven percent oxygen. For a 600,000 ton of 
clinker/year kiln, the range of kiln THC emissions (0.4 ppmvd to 224 
ppmvd as propane) corresponds to 1.5 tpy to 840 tpy (docket item II-B-
76), while the average kiln THC emissions (35 ppmvd as propane) 
corresponds to 131 tpy (docket item II-B-76). Organic HAP 
concentrations, as a percentage of THC for these data, ranged from 0 to 
98 percent (docket item II-B-75). With an average of 23 percent of the 
THC emissions being organic HAPs a 600,000 ton of clinker/year kiln 
would emit from 0.3 tpy to 190 tpy of organic HAPs, based on the range 
of THC stack concentrations.
    The emissions from kiln alkali bypasses are expected to be the 
result of incomplete combustion of fuel in the kiln, since this exhaust 
gas stream does not contact incoming kiln feed materials. Alkali bypass 
concentrations of THC were available for two kilns operating under NHW 
conditions. The concentrations were expressed as ppmvd (as propane) at 
seven percent oxygen, and averaged 3.4 ppmvd and 27 ppmvd, respectively 
(docket item II-B-75). For typical alkali bypass gas flow rates at a 
600,000 ton of clinker/year kiln, this range corresponds to 
approximately 2.4 tpy to 19 tpy of THC, while the average kiln bypass 
THC concentration (15 ppmvd) corresponds to 10.5 tpy of THC (docket 
item II-B-76). Assuming that 5 percent of the THC emissions from alkali 
bypasses are organic HAPs (docket item II-B-75), a 600,000 ton of 
clinker/year kiln would emit from 0.3 tpy to 6 tpy of organic HAPs, 
based on the range of THC alkali bypass stack concentrations.
    Kiln HCl. The currently available HCl emission data obtained from a 
total of 46 NHW and HW kilns range from 0.2 ppmvd to 157 ppmvd and the 
average is 27 ppmvd for 72 data points (docket item II-B-62). (All 
concentrations were corrected to seven percent oxygen.) For a 600,000 
ton of clinker/year kiln, the range of kiln HCl emissions corresponds 
to 0.6 tpy to 490 tpy, while the average HCl emission (27 ppmvd) 
corresponds to 84 tpy (docket item II-B-76). Based on analyses of test 
reports and ICR responses, HCl emissions range from less than 0.91 Mg/
yr (1 tpy) to over 272 Mg/yr (300 tpy). Ten plants responding to the 
ICR reported emissions of HCl greater than 9.1 Mg/yr (10 tpy) from each 
of 15 different kilns (docket item II-B-69).
    The EPA notes that with the exception of three kilns that were 
measured by FTIR, all of the HCl emission measurements included in the 
analysis were obtained using EPA Method 26. A recently completed study 
that compared the results of a draft test protocol using the gas filter 
correlation infrared (GFCIR) instrumental method (proposed EPA Method 
322) and EPA Method 26 found that HCl measured by GFCIR was typically 
much higher than that measured by Method 26 (docket item II-I-121). 
Concentrations of HCl measured by GFCIR ranged from 1.5 to 4.5 times 
the concentrations measured by Method 26 for wet kilns and up to 30 
times the concentrations measured by Method 26 for a dry kiln. 
Subsequent laboratory recovery efficiency analyses suggested that 
Method 26 is biased significantly low due to a scrubbing effect in the 
front half of the sampling train. Therefore, it is likely that 
currently available HCl emission data are understated.
4. Clinker Cooler
    It is desirable to cool the clinker rapidly as it leaves the 
burning zone of the kiln. Heat recovery, preheating of kiln combustion 
air, and fast clinker cooling are achieved by clinker coolers of the 
traveling-grate, planetary, rotary, or shaft type. Most commonly used 
are grate coolers where the clinker is conveyed along the grate and 
subjected to cooling by ambient air, which passes through the clinker 
bed in cross-current heat exchange.
    A portion of the clinker cooler exhaust serves as secondary 
combustion air in the kiln. The remainder of the clinker cooler exhaust 
is discharged to the atmosphere separately from the kiln exhaust gas 
through a PM emission control device. Clinker cooler gases are also 
sometimes routed through other pieces of process equipment, such as the 
coal or raw mill, as a source of warm,

[[Page 14197]]

dry air prior to being reused as combustion air.
    Since clinker coolers are not combustion devices, the only HAP 
expected to be emitted are the metal HAPs associated with the clinker 
cooler particulate, i.e., clinker dust. HAP metals that have been 
detected in clinker include chromium, lead, nickel, arsenic, beryllium, 
antimony, selenium, and mercury. In one study conducted by the Portland 
Cement Association (docket item II-I-44, p. 4), the average 
concentration of metal HAPs that has been detected in clinker is 555 
parts per million by weight (ppmw). In an earlier study, cited by EPA 
OSW the average HAP metal content in clinker was found to be 138 ppmw 
(docket item II-A-24, pp. 3-62 to 3-65). Under the existing NSPS, 
emissions of PM from clinker cooler gases are limited to 0.05 kg/Mg 
feed (dry basis) (0.10 lb/ton). A plant producing 600,000 tpy of 
clinker, emitting PM from the clinker cooler at the NSPS limit, would 
emit 6 kg (14 lb) of HAP metals per year, assuming a 140 ppmw HAP metal 
content in the PM (docket item II-B-76).
5. Finish Grinding/Conversion of Clinker to Portland Cement
    The cooled clinker is conveyed to clinker storage or mixed with 
gypsum and introduced directly into the finish mills. The finish mills 
are large, rotating steel cylinders containing a charge of steel balls. 
The clinker and gypsum are ground to a fine, homogeneous powder. Two 
different types of mill systems may be used. In open-circuit milling, 
the material passes directly through the mill without any separation of 
fine and coarse particles. In closed-circuit grinding, the mill product 
is carried to a cyclonic air separator in which the coarse particles 
are rejected from the product and returned to the mill for further 
grinding.
    The finished portland cement is conveyed to bulk storage silos from 
which it is dispensed for shipping. Portland cement is often loaded in 
bulk into hopper trucks or rail cars. It may also be packaged in ``tote 
bins'' or in 80 lb or 94 lb kraft paper bags. The bags are loaded onto 
pallets for handling, warehousing, and shipping.
    The only HAPs expected to be emitted from clinker/cement handling 
processes are the metal HAPs associated with clinker and cement dust. 
As was noted above, clinker dust is estimated to contain 555 ppmw of 
metal HAPs. The HAP metals that have been identified in portland cement 
include chromium, nickel, arsenic, lead, antimony, selenium, beryllium, 
cadmium, and mercury. In cement (as opposed to clinker), the 
concentrations of individual HAP metals range from an average of 0.014 
ppmw mercury to an average of 76 ppmw chromium. The total average 
concentration of metal HAPs in portland cement is 143 ppmw (docket item 
II-I-44).
    Total nationwide emissions of HAPs, PM, and VOCs from the above 
emission sources in portland cement plants are estimated at 23,300 Mg/
yr (25,700 tpy). Over 260 Mg/yr (290 tpy) of these emissions are HAPs. 
Emissions of PM and VOCs are estimated at 23,000 Mg/yr (25,400 tpy).
    Given that these processes release significant quantities of HAPs 
and the availability of emission control systems, the Agency selected 
to develop and propose NESHAP for the following emission sources: NHW 
kilns and NHW in-line kiln/raw mills; NHW kiln alkali bypasses; clinker 
coolers; raw material dryers; feed preparation and materials handling 
processes including raw mills, finish mills, storage bins (raw 
material, clinker, finished product), conveying system transfer points, 
bagging system, and bulk loading and unloading systems. Additional 
information on the operations in portland cement plants selected for 
regulation, and other operations, is included in the docket.

C. Selection of Pollutants

    The proposed standards would limit emissions of metal HAPs [almost 
all metals appearing in section 112(b) have been detected in portland 
cement plant emissions] and organic HAPs (including D/F) from portland 
cement manufacturing facilities. (Pollutant health effects were 
discussed in section II.C.) These HAPs are emitted in significant 
quantities from portland cement plant sources. The standards being 
proposed to address metal and organic HAP emissions establish limits 
for surrogate pollutants rather than for individual HAP compounds (a 
separate emission limit is established for D/F). The reasons for using 
surrogate pollutants are discussed below.
    Controlling PM emissions will control the emissions of non-volatile 
metal HAPs (and also the condensed organic HAPs including D/F which are 
adsorbed on particulates). The available technologies used in the 
cement manufacturing industry for the control of non-volatile HAP 
metals are the same technologies (FFs and ESPs) as the proposed MACT 
floor technologies for control of PM. Metal HAPs are estimated to 
constitute about 1 percent by weight of kiln PM emissions from portland 
cement manufacturing and about 0.06 percent by weight of clinker cooler 
PM emissions. In addition, the use of PM as a surrogate for non-
volatile metal HAP emissions reduces the costs associated with 
compliance testing and monitoring.
    The proposed standards establish an emission limit for THC as a 
surrogate for organic HAPs from new or reconstructed NHW kilns for the 
following reasons. Methods used in the cement manufacturing industry 
for the control of organic HAP emissions would be the same methods used 
to control THC emissions. These emission control methods include using 
feed materials with relatively low levels of organic matter and 
achieving good combustion (docket item II-B-47, docket item II-B-48). 
Standards limiting emissions of THC will also result in decreases in 
organic HAP emissions (with the additional benefit of decreasing VOC 
emissions).
    Establishing emission limits for specific organic HAPs (with the 
exception of D/F) would be impractical and costly. Total hydrocarbon, 
which is less expensive to test for and monitor, can be used as a 
surrogate for organic HAPs. Based on available data, organic HAPs range 
from 0 to 98 percent of THC and are estimated to account for 
approximately 23 percent on average of THC emissions from portland 
cement manufacturing (docket item II-B-75). The Agency recognizes that 
the level and distribution of organic HAPs associated with THC 
emissions from cement kilns will vary from kiln to kiln. Limiting THC 
as a surrogate for organic HAPs will eliminate costs associated with 
speciating numerous compounds.
    The proposed standards establish separate emission limits for D/F 
because of the high toxicity associated with even low masses of these 
compounds. In addition, data available to EPA establish the existence 
of a separate MACT floor technology for D/F control.
    The proposed regulation does not establish a limit for HCl 
emissions from cement kilns because no MACT floor technology has been 
identified. An HCl emission limit based on a beyond-the-floor control 
option was determined not to be justified as discussed in section V.D.2 
of this document.
    The proposed regulation does not establish limits for mercury 
emissions from cement kilns because no MACT floor control technology 
has been identified. A mercury emission limit based on a beyond-the-
floor control option was determined not to be justified as discussed in 
section V.D.2.

[[Page 14198]]

D. Selection of Proposed Standards for Existing and New Sources

1. Background
    After the EPA has identified the specific source categories or 
subcategories of sources to regulate under section 112, it must develop 
MACT standards for each category or subcategory. Section 112 
establishes a minimum baseline or ``floor'' for standards. For new 
sources, the standards for a source category or subcategory cannot be 
less stringent than the emission control that is achieved in practice 
by the best-controlled similar source. [See section 112(d)(3)]. The 
standards for existing sources may be less stringent than standards for 
new sources, but they cannot be less stringent than the average 
emission limitation achieved by the best-performing 12 percent of 
existing sources for categories and subcategories with 30 or more 
sources, or the average of the best-performing 5 sources for categories 
or subcategories with fewer than 30 sources.
    After the floor has been determined for a new or existing source in 
a source category or subcategory, the Administrator must set MACT 
standards that are technically achievable and no less stringent than 
the floor. Such standards must then be met by all sources within the 
category or subcategory. The regulatory alternatives selected for new 
and existing sources may be different because of different MACT floors, 
and separate emission limits may be established for new and existing 
sources.
    The EPA also may consider an alternative ``beyond the floor.'' 
Here, EPA considers the achievable reductions in emissions of HAPs (and 
possibly other pollutants that are co-controlled), cost and economic 
impacts, energy impacts, and other nonair environmental impacts. The 
objective is to achieve the maximum degree of emission reduction 
without unreasonable economic, energy or secondary environmental 
impacts.
2. MACT Floor Technology, Emission Limits, and Format
    The EPA conducted separate MACT determinations for PM (the 
surrogate for HAP metals), D/F, mercury, THC (the surrogate for organic 
HAPs), and HCl emissions from kilns and inline kiln/raw mills; for PM 
emissions from clinker coolers; for PM and THC emissions from raw 
material dryers; and for PM emissions from materials handling 
facilities. For each combination of pollutant and affected source, MACT 
floor technologies and beyond-the-floor control options were evaluated.
    Several formats are available for establishing the emission limits 
based on MACT. These include mass concentration (mass per unit volume), 
volume concentration (volume per unit volume), mass emission rate (mass 
per unit time), process emission rate (mass per unit of production or 
other process parameter), and percent reduction.
    For the portland cement manufacturing source category, EPA is 
proposing numerical emission standards expressed as a process emission 
rate and opacity limits for PM emissions from kilns; as mass per volume 
of exhaust gas for D/F emissions from kilns; as volume per volume of 
exhaust gas for THC emissions from kilns and raw material dryers; as a 
process emission rate and opacity limit for clinker cooler PM 
emissions; and as an opacity limit for materials handling facilities PM 
emissions.
    The following sections present a discussion of the rationale for 
selecting the MACT technologies, emission limits, and format of the 
standard for each affected source and associated pollutant.
    Kiln and in-line kiln/raw mill PM HAP emissions. Well-designed and 
properly operated FFs or ESPs are the PM control technologies presently 
in use by the best performing 12 percent of existing kilns and in-line 
kiln/raw mills. In the portland cement manufacturing industry, it is 
estimated that at least 30 percent (docket item II-A-4) of existing 
kilns are subject to the requirements of the NSPS for cement plants (40 
CFR part 60, subpart F).
    Table 7 lists the type of control device used with, and available 
PM emissions data from, kilns and in-line kiln/raw mills subject to the 
NSPS. The emission levels shown in Table 7 all meet the NSPS emission 
limit and were all achieved with FFs and ESPs designed to meet the 
NSPS. This represents the MACT floor technology for control of PM from 
kilns and in-line kiln/raw mills.

                                 Table 7.--Particulate Emissions From NSPS Kilns                                
                         [Docket Item II-A-4, Docket Item II-A-43, Docket Item II-B-62]                         
----------------------------------------------------------------------------------------------------------------
                                                                           PM (kg/Mg dry                        
             Kiln type                            APCD type                    feed)             Location       
----------------------------------------------------------------------------------------------------------------
PH.................................  FF                                           0.0011  Southdown--Kosmosdale,
                                                                                           KY.                  
PC.................................  FF                                         a 0.0039  Boxcrow Cement--      
                                                                                           Midlothian, TX.      
PH.................................  ESP                                        b 0.0075  Ash Grove--Durkee, OR.
DRY................................  FF                                         a 0.0090  Southdown #1--        
                                                                                           Fairborn, OH.        
PC.................................  ESP                                        c 0.015   RMC Lone Star--       
                                                                                           Davenport, CA.       
PC.................................  FF                                           0.015   Kaiser Cement--       
                                                                                           Cupertino, CA.       
PH.................................  ESP                                          0.015   Roanoke Cement--      
                                                                                           Cloverdale, VA.      
PC.................................  FF                                           0.020   Moore McCormack--     
                                                                                           Knoxville, TN.       
PH.................................  FF                                           0.029   Moore McCormack--     
                                                                                           Brooksville, FL.     
PC.................................  FF                                           0.033   Kaiser Cement--Lucerne
                                                                                           Valley, CA.          
PC.................................  FF                                           0.035   Calif Portland--      
                                                                                           Mojave, CA.          
PC.................................  FF                                           0.04    Martin Marietta--     
                                                                                           Leamington, UT.      
PC.................................  ESP                                          0.044   Kaiser--San Antonio,  
                                                                                           TX.                  
PC.................................  FF                                           0.048   Martin Marietta--     
                                                                                           Lyons, CO.           
PH/PC..............................  ESP                                        b 0.051   Lone Star--Cape       
                                                                                           Girardeau, MO.       
WET................................  ESP                                          0.056   Monolith Portland--   
                                                                                           Laramie, WY.         
DRY................................  FF                                           0.056   Lone Star--Pryor, OK. 
DRY................................  ESP                                        d 0.058   Ash Grove #2--        
                                                                                           Louisville, NE.      
PC.................................  ESP                                          0.065   General Portland--New 
                                                                                           Braunfels, TX.       
PC.................................  FF                                           0.068   Davenport Industries--
                                                                                           Buffalo, IA.         
PH.................................  FF                                           0.070   Ideal Basic--La Porte,
                                                                                           CO.                  
PH.................................  FF                                           0.074   Southwestern Portland--
                                                                                           Odessa, TX.          
DRY................................  ESP                                          0.11    Ash Grove #1--        
                                                                                           Louisville, NE.      

[[Page 14199]]

                                                                                                                
PC.................................  ESP                                          0.12    Texas Industries--    
                                                                                           Hunter, TX.          
PC.................................  ESP                                          0.13    Lehigh--Mason City,   
                                                                                           IA.                  
WET................................  ESP                                          0.15    Genstar--San Andreas, 
                                                                                           CA.                  
WET................................  FF                                           0.15    Lone Star--Salt Lake  
                                                                                           City, UT.            
----------------------------------------------------------------------------------------------------------------
PC = precalciner.                                                                                               
PH = preheater.                                                                                                 
a = average of four tests.                                                                                      
b = average of three tests.                                                                                     
c = average of two tests.                                                                                       
d = average of five tests.                                                                                      

    The data in Table 7 were obtained from EPA Method 5 compliance 
tests on new kilns subject to the NSPS [0.15 kg/Mg dry feed (0.30 lb/
ton dry feed)]. These tests measure the performance of PM APCDs 
associated with new kilns over a relatively short period (typically 
three 1-hour test runs). These data show that PM emissions from ESPs 
and FFs designed to meet the NSPS and operated and maintained to 
demonstrate initial compliance with the NSPS under Method 5 test 
conditions varied within a range of 0.0011 kg/Mg dry feed (0.0022 lb/
ton dry feed) to 0.15 kg/Mg dry feed (0.3 lb/ton dry feed). The data in 
Table 7 show equivalent performance can be expected from FFs and ESPs, 
and that neither technology offers a clear advantage. Due to the fact 
that the best performing kilns and in-line kiln/raw mills use FFs and 
ESPs designed to meet the NSPS and because of the variability in 
performance of well-designed, well-maintained and properly operated FFs 
and ESPs, the emission limit represented by the MACT floor technology 
is equivalent to the NSPS of 0.15 kg/Mg dry feed (0.30 lb/ton dry 
feed).
    No technologies were identified for existing or new kilns or in-
line kilns/raw mills that would consistently achieve lower emission 
levels of PM than the NSPS limit. Consequently, there is no beyond-the-
floor technology that has been shown to consistently achieve lower 
emissions. Therefore the PM emission limit proposed for new and 
existing kilns and in-line kiln/raw mills is 0.15 kg/Mg dry feed (0.30 
lb/ton dry feed), which is equivalent to the NSPS limit.
    The NSPS establishes an opacity limit, and an opacity limit is also 
being proposed under this standard. The maximum 6-minute average 
opacity level may not exceed 20 percent opacity, as is the case for the 
NSPS.
    The production-based emission limit format was chosen for kiln and 
in-line kiln/raw mill PM emissions. The units for this emission 
standard are kg of PM per Mg of dry feed (lb PM per ton of dry feed). 
This format (mass per unit of production) and associated opacity limit 
are consistent with the format of the portland cement plant NSPS (40 
CFR part 60, subpart F). At least 30 percent of the kilns in the 
industry are subject to the NSPS (docket item II-A-4) and these plants 
are already monitoring the production-based emission rate and the 
opacity.
    A concentration format (e.g., g/dscm [gr/dscf]) was considered for 
the kiln and in-line kiln/raw mill PM emission limit. One reason that 
this format was not chosen was that it would be inconsistent with the 
NSPS PM emission limit format. However, there are other considerations. 
A concentration format would penalize more energy efficient kilns, 
which burn less fuel and produce less kiln exhaust gas per megagram of 
dry feed. This is because with a concentration based standard the more 
energy-efficient kilns would be restricted to a lower level of PM 
emitted per unit of production.
    Kiln and in-line kiln/raw mill D/F emissions. The EPA has 
identified two technologies for control of D/F emissions. One 
technology achieves low D/F emissions by a combination of proper kiln 
operation, proper combustion, proper control device operation, and a 
reduction in the kiln gas temperature at the inlet to the PMCD. The 
other technology is activated carbon injected into the kiln exhaust 
gas.
    The discussion in this section refers to D/F emissions in units of 
TEQ. Toxic equivalent refers to the international method of expressing 
toxicity equivalents for dioxins and furans as defined in EPA report, 
``Interim Procedures for Estimating Risks Associated with Exposures to 
Mixtures of Chlorinated Dibenzo-p-dioxins and -dibenzofurans (CDDs and 
CDFs) and 1989 Update'' (docket item II-A-8).
    Dioxin/furan emissions data were obtained from testing that was 
conducted at NHW kilns, with NHW fuels at kilns that normally burn HW, 
and under worst-case conditions at kilns that burn HW (as part of 
Certificate of Compliance [COC] testing). Based on the test results for 
both NHW and HW kilns, the predominant factor affecting D/F emissions 
is the temperature of gases at the inlet to the PMCD (docket item II-A-
42; docket item II-B-78; docket item II-I-81, pp. 127 to 133; docket 
item II-I-82, pp. 135 to 175). The highest D/F emissions (near 40 ng 
TEQ/dscm) occurred at the highest gas temperatures (between 500  deg.F 
and 700  deg.F) while the lowest emissions (near 0.02 ng TEQ/dscm) 
occurred at the lowest temperature (at approximately 210  deg.F). [The 
emission 0.02 ng TEQ/dscm is the average of the four NHW D/F test 
results that were measured at gas temperatures less than 230  deg.F, as 
shown in Table 8.]
    Dioxin/furan TEQ emissions data and stack temperatures from kilns 
firing NHW fuels are listed in Table 8. The data are listed in order of 
ascending stack temperature. Fourteen NHW data points were obtained 
during normal kiln operation, three points were obtained as NHW 
baseline runs prior to HW COC testing, one data point (at the 518  
deg.F stack temperature) was obtained at maximum combustion 
temperature, and one point was obtained under unknown test conditions. 
Stack temperatures are presented, since inlet PMCD temperature data are 
not typically recorded during stack emissions testing. It is 
acknowledged that stack temperatures will be lower than inlet PMCD 
temperatures.

[[Page 14200]]



Table 8.--Average Dioxin/Furan Toxic Equivalent Emissions (at 7 Percent Oxygen) and Average Stack Gas Temperatures for NHW Cement Kilns and Kilns Tested
                                                                  Under NHW Conditions                                                                  
                                                                  [Docket Item II-B-78]                                                                 
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                               Avg TEQ ng/                              
         Kiln type                    APCD type                    Kiln fuel            Avg Gas T ( deg.F)        dscm              Kiln location       
--------------------------------------------------------------------------------------------------------------------------------------------------------
PH/PC......................  FF                           Natural gas; main stack      183                         0.011     Capital Aggregates--San    
                                                           tested.                                                            Antonio TX.               
PC.........................  FF                           Coal,tires, pulp/paper mill  220                0.0063    Calaveras Cement--Redding  
                                                           sludge.                                                            CA.                       
PH/PC......................  FF                           Natural gas; raw mill on...  221                         0.042     Ash Grove--Seattle WA (kiln/
                                                                                                                              in-line mill).            
PH/PC......................  ESP                          Not reported...............  226                         0.00087   RMC Lonestar--Davenport CA.
PC.........................  FF                           Coal & tires...............  233                0.21      Calaveras Cement--Redding, 
                                                                                                                              CA.                       
PH/PC......................  FF                           Natural gas; bypass stack    299                         0.054     Capital Aggregates--San    
                                                           tested.                                                            Antonio TX.               
WET........................  ESP                          Coal.......................  305                         0.0024    Holnam--Florence CO.       
WET........................  ESP                          Coal & natural gas.........  315                         0.072     Ash Grove--Montana City MT.
WET........................  ESP                          Coal.......................  346 q                       0.37      Lehigh--Union Bridge MD.   
WET........................  ESP                          coal & tires...............  358 q                       1.2       Lehigh--Union Bridge MD.   
WET........................  ESP                          Coal/coke..................  366                         0.032     Holnam kiln #1--Holly Hill 
                                                                                                                              SC.                       
DRY........................  FF                           Coal, gas, tire derived      396                         0.0035    Riverside--Oro Grande CA.  
                                                           fuel.                                                                                        
WET........................  ESP                          Natural gas................  397                         0.020     Capital Aggregates--San    
                                                                                                                              Antonio TX.               
DRY........................  FF                           Coal & natural gas.........  403                         0.0084    Riverside--Oro Grande CA.  
WET........................  ESP                          Coal.......................  417                         0.12      Lone Star--Greencastle IN. 
WET........................  ESP                          Coal/coke..................  418                         0.04      Holnam kiln #2--Holly Hill 
                                                                                                                              SC.                       
DRY........................  ESP                          Coal, coke, & tires........  450                         0.074     Lone Star--Oglesby IL.     
WET........................  ESP                          Coal.......................  482                         0.55      Continental Cement--       
                                                                                                                              Hannibal MO.              
WET........................  ESP                          Coal.......................  518                         1.0       Holnam--Clarksville MO.    
--------------------------------------------------------------------------------------------------------------------------------------------------------
 Abbreviations:                                                                                                                                         
   PH/PC = preheater/precalciner.                                                                                                                       
   ESP = electrostatic precipitator.                                                                                                                    
   PC = precalciner.                                                                                                                                    
   FF = fabric filter.                                                                                                                                  
Note: Entries flagged with  and q are listed in Table 9 and discussed in the text.                                                             

    The data in Table 8 show that all NHW D/F emissions were less than 
0.2 ng TEQ/dscm at stack temperatures below 340  deg.F, except for one 
data point which is discussed below. The stack temperature of 340 
deg.F corresponds to an estimated inlet PMCD temperature of 
approximately 400  deg.F after accounting for cooling in the ductwork. 
The EPA estimates that approximately 50 percent of existing PMCDs used 
at both wet-and dry-type NHW kilns operate with a maximum inlet PMCD 
temperature of approximately 400  deg.F (docket item II-B-73). Since 
the MACT floor is based on the technology in use by the best performing 
12 percent of the affected sources, the MACT floor for existing kilns 
corresponds to reduction of kiln exhaust gas stream temperature at the 
PMCD inlet to 400  deg.F.
    One demonstrated method of temperature reduction is injection of 
water to provide rapid cooling of kiln exhaust gases upstream of the 
inlet to the PMCD. Rapid cooling reduces D/F formation that occurs 
within the temperature window 232  deg.C (450  deg.F) to 343  deg.C 
(650  deg.F).
    As shown in Table 8, D/F emissions from 3 of the 13 tests conducted 
at stack temperatures below 400  deg.F exceeded 0.2 ng TEQ/dscm. For 
discussion purposes, the three data points are listed in Table 9 with 
the corresponding stack temperature. The Calaveras kiln that emitted 
0.21 ng TEQ/dscm when tested at a stack temperature of 233  deg.F 
emitted 97 percent less D/F at a slightly lower stack temperature and 
with a different mixture of fuels, demonstrating that the kiln could 
achieve 0.2 ng/dscm through proper kiln combustion.

 Table 9.--Data from KILNS at Which Dioxin/Furan TEQ Emissions Exceeded 
                               0.2 ng/dscm                              
------------------------------------------------------------------------
                                        Average                         
                                        D/F TEQ                         
  Average stack gas temperature (*F)   (ng/dscm       Kiln location     
                                         at 7%                          
                                          O2)                           
------------------------------------------------------------------------
233..................................      0.21  Calaveras--Redding CA. 
346..................................      0.37  Lehigh--Union Bridge   
                                                  MD.                   
358..................................      1.2   Lehigh--Union Bridge   
                                                  MD.                   
------------------------------------------------------------------------

    The Lehigh kiln emitted 0.37 ng TEQ/dscm at a stack temperature of 
346  deg.F during coal combustion and 1.2 ng TEQ/dscm at a stack 
temperature of 358  deg.F during coal and tire combustion. The EPA 
concluded that the high emission (of 1.2 ng TEQ/dscm) resulted from 
poorly controlled tire combustion/kiln operation, since (as shown in 
Table 8) three other NHW kilns emitted less than 0.2 ng TEQ/dscm when 
tested while burning tires. In the absence of detailed information on 
kiln and APCD operating conditions, fuel firing and combustion control, 
the Lehigh emission level of 0.37 ng TEQ/dscm at a stack temperature of 
346  deg.F cannot be explained.
    Temperature reduction to 400  deg.F, in conjunction with proper 
control of kiln and PMCD operation and efficient combustion will limit 
D/F emissions to 0.2 ng TEQ/dscm in most (if not all) cases, and the 
proposed D/F standard for existing kilns is set at this level. The EPA 
recognizes that the available emissions data show that one kiln (as 
illustrated by the Lehigh data in Table 9) cannot achieve 0.2 ng TEQ/
dscm at an inlet temperature to the PMCD below 400  deg.F, and that 
parameters consistent with proper equipment operation have not been 
precisely specified. The proposed standards therefore provide that 
kilns that cannot meet the 0.2 ng TEQ/dscm limit would be required to 
maintain the temperature at the inlet to the PMCD at no more than 400 
deg.F and to limit the D/F emissions to 0.4 ng

[[Page 14201]]

TEQ/dscm. This limit of 0.4 ng TEQ/dscm is consistent with the 
emissions from the Lehigh kiln during coal combustion with an estimated 
PMCD inlet gas temperature of 400  deg.F.
    The Agency has considered whether and how to account for emissions 
variability in establishing the alternative TEQ limit of 0.4 ng/dscm in 
conjunction with the 400  deg.F temperature limit at the PMCD. As 
discussed in this section, available emissions data indicate that most 
kilns will be able to achieve an emission level of 0.2 ng TEQ/dscm or 
lower when operating the PMCD at or below 400  deg.F. Even though the 
Lehigh kiln's emissions were 0.37 ng TEQ/dscm at 346  deg.F (when not 
burning tires), we believe that a TEQ limit of 0.4 ng/dscm is 
appropriate given the preponderance of emissions data at or below 0.2 
ng TEQ/dscm. These data (given the strong indications that all units 
will meet the 0.4 ng TEQ/dscm limit at temperatures of 400  deg.F or 
below) suggest that using a more specific approach for variability is 
not needed for this proposed standard. The Agency invites comments on 
other approaches for accommodating variability in D/F emissions for NHW 
cement kilns.
    Thus, the proposed standard requires that the temperature at the 
inlet to the PMCD be maintained at a level no greater than either: (1) 
the higher of 400  deg.F or the temperature established during the 
successful Method 23 performance test plus five percent (not to exceed 
25  deg.F) of the temperature measured in  deg.F during the successful 
compliance test, if D/F emissions were determined to be no greater than 
0.15 ng toxic equivalent (TEQ)/dscm (6.5 x 10-11 gr/dscf); 
(2) the higher of 400  deg.F or the temperature established during the 
successful Method 23 performance test, if D/F emissions were determined 
to be greater than 0.15 ng toxic equivalent (TEQ)/dscm (6.5 x 
10-11 gr/dscf) but less than 0.2 ng toxic equivalent (TEQ)/
dscm (8.7 x 10-11 gr/dscf);, or (3) 400  deg.F if D/F 
emissions were greater than 0.2 ng TEQ/dscm (8.7 x 10-11 gr/
dscf) but less than or equal to 0.4 ng TEQ/dscm (1.7 x 10-10 
gr/dscf).
    Activated carbon injection (ACI) was investigated as a potential 
beyond-the-MACT-floor option for existing cement kilns. Activated 
carbon injection is used at one cement plant on two NHW kilns for the 
purpose of reducing plume opacity. The total capital cost of an ACI 
system is estimated to range from $680,000 to $4.9 million per kiln. 
The total annual costs of an ACI system are estimated to range from 
$426,000 to $3.3 million per kiln. These costs include the carbon 
injection system and an additional baghouse to collect the carbon 
separately from the existing primary particulate collector (docket item 
II-B-67). Based on these costs, and considering the level of D/F 
emissions achievable at the floor level of control, the Administrator 
has determined that this beyond-the-floor (BTF) option for D/F MACT for 
existing kilns may not be justified. Therefore the Agency is not 
proposing a BTF standard. Notwithstanding these costs and the limited 
emissions reductions that a BTF standard would achieve, the Agency 
solicits comment on whether a BTF standard would be appropriate given 
the Agency's and the Congress' special concern about D/F. D/F are some 
of the most toxic compounds known due to their bioaccumulation 
potential and wide range of health effects at exceedingly low doses, 
including carcinogenesis. Exposure via indirect pathways was in fact a 
chief reason that Congress singled out D/F for priority MACT control in 
section 112(c)(6) of the Act [see S. Rep. No. 128, 101st Cong. 1st 
Sess. at 154-155 (1989)]. Thus costs to reduce dioxin emissions are 
frequently justified by the benefits of removing this very toxic HAP. 
[See 61 FR at 17382, 17392, and 17403 (April 19, 1996) (The EPA 
proposes BTF standards for D/F emissions from hazardous waste 
combustion sources).] The EPA is influenced here by the fact that most 
sources appear to be able to achieve the 0.2 ng TEQ/dscm BTF option 
through the use of the floor technology alone, i.e. solely through the 
use of temperature control. Thus, the floor standard (which facially 
allows the option of 0.4 ng TEQ/dscm) in reality may be virtually 
equivalent to the BTF level.
    Activated carbon injection was also considered as a candidate MACT 
for new cement kilns. Since no D/F performance data are available on 
the existing cement kiln ACI system installed to reduce opacity, EPA 
considered the performance of ACI on other potentially similar sources. 
Experience with ACI on municipal waste combustors (MWCs) and medical 
waste incinerators (MWIs) has led EPA to develop emission limits for D/
F for these sources in the range of 0.26 to 2.5 ng TEQ/dscm (docket 
item II-J-3, docket item II-J-7). Assuming the performance level of ACI 
on MWIs or MWCs to be similar to that of a cement kiln, the D/F 
emissions levels achieved with ACI are expected to be about the same 
level that can be achieved with temperature reduction. Therefore, 
considering the level of D/F emissions achievable by PMCD inlet 
temperature reduction alone, the Administrator has determined that the 
temperature reduction plus ACI option for D/F MACT for new kilns may 
not be justified, and the Agency is not proposing a standard based on 
ACI. Notwithstanding the limited emissions reduction that such a 
standard would achieve, the Agency solicits comment on whether or not 
such a standard would be appropriate, given the Agency's and the 
Congress' special concern about D/F. The EPA is influenced here, 
similarly to the situation for existing kilns, by the fact that most 
new sources appear to be able to achieve a 0.2 ng TEQ/dscm emission 
level solely through the use of temperature control. Thus the proposed 
standards (which facially allow a 0.4 ng TEQ/dscm emission level where 
the implementation of temperature reduction may not achieve a 0.2 ng 
TEQ/dscm emission level) in reality may be virtually equivalent to a 
0.2 ng TEQ/dscm emission level.
    For the kiln and in-line kiln/raw mill D/F emission standard, a 
mass per volume concentration emission limit format was chosen. The 
specific units of the emission limit are ng of D/F TEQ/dscm, referenced 
to seven percent oxygen. This emission limit format has historically 
been used by EPA for many air emission standards. This format is 
consistent with the format of the OSW MACT standard for HW cement 
kilns.12 The concentration is corrected to seven percent 
oxygen to put concentrations measured in stacks with different oxygen 
concentrations on a common basis. Also, the typical range of oxygen 
concentrations in cement kiln stack gas is from five to 10 percent 
oxygen; therefore, seven percent is representative.
---------------------------------------------------------------------------

    \12\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    A mass per volume concentration emission limit based on total D/F 
congeners rather than TEQ was also considered. However, the TEQ format 
was chosen in order to maintain consistency with the rule for cement 
kilns which burn hazardous waste.
    Kiln and in-line kiln/raw mill mercury emissions. Activated carbon 
injection (ACI) was considered a potential control technology for 
mercury MACT for cement kilns, since a form of this technology has been 
demonstrated on medical waste incinerators and municipal waste 
combustors (docket item II-A-36, pp. 98 to 99 and B-7 to B-8; docket 
item II-A-11; docket item II-A-19; docket item II-A-23), and is being 
used at one cement plant on two NHW kilns to reduce the opacity (docket 
item II-B-35). In these

[[Page 14202]]

applications, the activated carbon (AC) is injected into the 
uncontrolled exhaust gas stream ahead of the kiln PMCD.
    In cement kiln applications for mercury control, the AC would need 
to be injected downstream from the kiln PMCD and subsequently collected 
in a separate PMCD, e.g., a baghouse. This is because the PM collected 
from the kiln exhaust, i.e., cement kiln dust (CKD), is typically 
recycled from the kiln PMCD back to the kiln, and in some cases may 
constitute as much as 50 percent of the feed material input to the 
kiln. If the AC is not injected downstream of the kiln PMCD, and then 
collected in a separate PMCD downstream of the kiln PMCD, the AC would 
also be recycled back to the kiln along with the adsorbed mercury. This 
recycling of mercury back to the cement kiln via the AC would result in 
the revaporization of the mercury in the kiln gas and ultimately the 
mercury would be emitted to the atmosphere. The two cement kiln ACI 
systems cannot be considered as controls for mercury for cement kilns 
because they do not include provisions for injecting the AC downstream 
of the kiln PMCD nor do they have the additional PMCD necessary to 
remove the injected carbon from the exhaust gas stream for disposal, 
but instead include the AC with the CKD that is recycled to the kiln. 
Therefore there is no mercury MACT floor for new or existing kilns.
    Activated carbon injection (with an additional PMCD) was 
investigated as a potential beyond-the-MACT-floor option for mercury 
for new and existing cement kilns. The total capital cost of an ACI 
system is estimated to range from $680,000 to $4.9 million per kiln. 
The total annual costs of an ACI system are estimated to range from 
$430,000 to $3.3 million per kiln. These costs include the carbon 
injection system and an additional baghouse necessary to collect the 
carbon separately from the CKD (docket item II-B-67). The cost-
effectiveness of ACI applied to cement kilns ranges from $20,000,000 to 
$50,000,000 per ton of mercury.
    It is noted that the Agency has proposed a mercury emissions limit 
for hazardous waste burning (HW) cement kilns (61 FR 17358), based on 
the beyond-the-MACT-floor option of ACI. However, mercury levels in 
hazardous waste fuels per million BTU of heat input are generally 
higher than mercury levels in coal that is fired in non-hazardous waste 
burning (NHW) cement kilns. Thus, HW cement kilns generally have higher 
mercury emissions than NWH cement kilns. Further, the available data 
indicate that existing mercury emissions from essentially all 
individual NHW cement kilns are lower than the beyond-the-MACT-floor 
emission limit that is now being considered by the Agency to be 
promulgated for HW cement kilns. Based on the relatively low levels of 
existing mercury emissions from individual NHW cement kilns, and the 
costs of reducing these emissions by ACI, the Administrator has 
determined that this beyond-the-MACT-floor option for reducing mercury 
from new and existing NHW kilns may not be justified. Thus, the Agency 
is not proposing a mercury standard for new and existing NHW cement 
kilns.
    Notwithstanding the reasons for not proposing a mercury standard 
for NHW cement kilns, the Agency solicits comment on whether a BTF 
standard would be appropriate given the Agency's and Congress' special 
concern about mercury. Mercury is one of the more toxic metals known 
due to its bioaccumulation potential and the adverse neurological 
health effects at low concentrations especially to the most sensitive 
populations at risk (i.e. unborn children, infants and young children). 
In addition, as with D/F, Congress has singled out mercury in section 
112(c)(6) of the Act for prioritized control. Furthermore, the amount 
of mercury emitted by these sources is not inconsequential, roughly 
10,000 pounds annually (or about 60 pounds per kiln annually) making 
NHW cement kilns a significant source of mercury emissions that may 
warrant attention under section 112(c)(6) of the Act depending on what 
other opportunities for controlling mercury from other significant 
sources are available.
    It is EPA's tentative conclusion, however, that concerns as to 
health risks from mercury emissions from these sources may be 
appropriately addressed pursuant to the timetable set out in the Act, 
namely through the residual risk determination process set out in 
section 112(f) of the Act. A more accelerated determination may be 
warranted, however, for other mercury-emitting sources, in particular 
hazardous waste combustion sources, where there are special 
considerations of immediately protective rules imposed by the Resource 
Conservation and Recovery Act. [See 61 FR at 17369-17370 (April 19, 
1996).]
    Kiln and in-line kiln/raw mill THC main exhaust emissions. Based on 
data from 31 tests conducted at 16 NHW kilns (docket item II-B-75), THC 
emissions varied between 0.4 ppmvd and 224 ppmvd (as propane, corrected 
to seven percent oxygen). With the exception of two kilns which employ 
a precalciner system with no preheater, no add-on air pollution control 
technologies are presently in use that decrease emissions of THC (the 
surrogate for organic HAPs) from NHW cement kilns. On this basis the 
MACT floor for THC emissions from existing kilns and in-line kiln/raw 
mills is no control.
    The precalciner/no preheater system was considered as a possible 
beyond-the-floor technology for existing kilns and as a possible MACT 
floor for new kilns (docket item II-B-47, docket item II-B-48). The 
precalciner/no preheater technology acts like an afterburner to combust 
organic material in the feed. However, it was found to increase fuel 
consumption 79 percent relative to the preheater/precalciner designs 
(docket item II-B-48, docket item II-D-199). The EPA estimates that 
precalciner/no preheater kilns would emit six times as much 
SO2 (at 3.7 lb SO2/ton clinker), two and one half 
times as much NOX (at 9.8 lb NOX/ton clinker), 
and 1.2 times as much CO2 (at 2,086 lb CO2/ton 
clinker) as a preheater/precalciner kiln of equivalent clinker capacity 
(docket item II-B-48). For a 600,000 ton clinker/year kiln, increased 
emissions for a flash precalciner relative to a preheater/precalciner 
are: 930 tpy SO2, 1,740 tpy NOX, and 109,000 tpy 
CO2 (docket item II-B-76, docket item II-D-199).
    One THC control method available is feed material selection. Total 
hydrocarbon emissions from kilns can be limited by avoiding feed 
materials which have excessive organic contents (docket item II-I-66, 
docket item II-I-67, docket item II-I-68). A few existing kilns have 
employed this method, but not enough to constitute a MACT floor for 
existing kilns. Also, this method is not available for existing kilns 
in that facilities are generally tied to existing raw materials sources 
in close proximity to the facility. Raw material proximity 
(transportation cost) is usually a major factor in plant site 
selection. Feed material selection can be employed in the siting 
process for new kilns, and to a limited extent at existing kilns.
    The precalciner/no preheater technology was also considered as a 
MACT floor for new sources but, when NOX, SO2, 
and CO2 emissions and energy penalties are considered, the 
Administrator has determined that it does not represent the MACT floor 
for new sources, since the kilns employing this technology cannot be 
considered to be the best controlled similar source. The combination of 
feed material selection, site location and feed material blending was 
determined to be MACT for new sources, in that this method has been 
used at some existing sources and that site selection based on 
availability

[[Page 14203]]

of acceptable raw material hydrocarbon content is feasible.
    The numerical emission limit proposed for THC from the main exhaust 
of new kilns and new in-line kiln/raw mills is 50 ppmvd (as propane, 
corrected to seven percent oxygen). This represents a level which is 
consistently achievable, as shown by tests across a broad spectrum of 
feed material compositions, when feeds with high organic contents are 
avoided. Based on the available THC main exhaust concentration data for 
existing NHW kilns, approximately 62 percent of the tested NHW kilns 
could meet the 50 ppmvd limit (docket item II-B-75).
    For the new kiln and in-line kiln/raw mill main exhaust THC 
emission standard, a volume per volume concentration emission limit 
format was chosen. The specific units of the emission limit are ppmvd 
(as propane, corrected to seven percent oxygen). This emission limit 
format has historically been used by EPA for many air emission 
standards. This format is consistent with the format of the OSW MACT 
standard for HW cement kilns.13 The concentration is 
corrected to seven percent oxygen to put concentrations measured in 
stacks with different oxygen concentrations on a common basis, and 
because the typical range of oxygen concentrations in cement kiln stack 
gas is from five to 10 percent oxygen; therefore, seven percent is 
representative. The THC concentration can be monitored directly with 
the CEM required by this standard. The reference or calibration gas for 
the THC CEM is propane, and the data analyzed in the development of 
this standard were referenced to propane, therefore propane is the 
appropriate reference compound for concentration data.
---------------------------------------------------------------------------

    \13\ The EPA proposed regulations for subpart EEE of 40 CFR Part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    Kiln and in-line kiln/raw mill HCl emissions. No technologies that 
control HCl emissions have been identified that are currently being 
used by more than six percent of the cement kilns in the U.S. For this 
reason, there is no MACT floor for existing kilns. One technology 
considered as potential MACT for new kilns was an alkaline scrubber, 
since two kilns in the U.S. operate scrubbers to control SO2 
emissions. However, these SO2 scrubbers are operated only 
intermittently (docket item II-D-196) and thus cannot be considered 
best controlled similar source. For this reason there is no MACT floor 
for new kilns.
    Alkaline scrubbers were considered as a beyond-the-floor option for 
HCl control. Based on engineering assessment of HCl scrubbers used in 
MWC and MWI applications and transfer of similar technology to the 
cement industry and on vendor design information (docket item II-D-36), 
an alkaline scrubber could achieve 15 ppmv HCl outlet concentration at 
low inlet HCl loadings or at least 90 percent removal with an inlet HCl 
level of 100 ppmv or greater. Based on this estimated performance, 
annual emission reduction estimates range from 12 tpy of HCl and 27 tpy 
of SO2 to 200 tpy of HCl and 600 tpy of SO2 per 
kiln (docket item II-B-67). The total capital cost of installing an 
alkaline scrubber on an existing kiln is estimated to range from 
$980,000 to $4.6 million. The total annual cost is estimated to range 
from $300,000 to $1.5 million per kiln (docket item II-B-67).
    Based on the costs of control and the emissions reductions that 
would be achieved, the Administrator has determined that beyond-the-
floor controls are not warranted. Therefore, there is no proposed 
emission limit for HCl from new and existing NHW kilns and NHW in-line 
kiln/raw mills. Analyses indicate that the ambient concentrations of 
HCl produced by emissions from existing NHW kilns and in-line kiln/raw 
mills are below the health effects reference concentration for HCl 
(docket item II-B-71).
    Clinker cooler PM HAP emissions. Particulate emissions from clinker 
coolers are typically controlled by FFs (docket item II-B-69). In the 
portland cement manufacturing industry, it is estimated that at least 
54 existing clinker coolers (docket item II-A-4) are subject to the 
requirements of the NSPS for cement plants (40 CFR part 60, subpart F). 
This number represents about 25 percent of clinker coolers and, 
therefore, the NSPS represents the MACT floor. The NSPS level of 
control is being achieved through the use of well-designed and well-
operated FFs. Typical design parameters for pulse jet cleaned fabric 
filters applied to clinker coolers are air-to-cloth ratios in the range 
of 0.02 cubic meters per second per square meter (m3/sec)/
m2 [4 actual cubic feet per minute per square foot (acfm/
ft2)] to 0.046 (m3/sec)/m2 (9 acfm/
ft2).
    Table 10 lists plants and the results of emission tests performed 
on FFs applied to clinker coolers from the May 1985 NSPS review report 
(docket item II-A-4).

     Table 10.--Fabric Filter Controlled Clinker Cooler Test Results    
                          [Docket Item II-A-4]                          
------------------------------------------------------------------------
  PM stack emissions (kg/Mg dry feed)           Plant and location      
------------------------------------------------------------------------
0.0041.................................  Kaiser Cement--Cupertino, CA.  
0.004..................................  Moore McCormack--Knoxville, TN.
0.022..................................  Moore McCormack--Brooksville,  
                                          FL.                           
0.003 a................................  Kaiser Cement--Lucerne Valley, 
                                          CA.                           
0.02...................................  California Portland--Mojave,   
                                          CA.                           
0.017..................................  Martin Marietta--Leamington, UT
0.025..................................  Kaiser--San Antonio, TX.       
0.03 b.................................  Lone Star--Cape Girardeau, MO. 
0.002..................................  Monolith Portland--Laramie, WY.
0.024..................................  Ash Grove--Louisville, NE.     
0.09552 b..............................  Ideal Basic--La Porte, CO.     
0.0117.................................  Texas Industries--Hunter, TX   
0.0245.................................  Lone Star--Salt Lake City, UT. 
------------------------------------------------------------------------
a Includes alkali bypass emissions.                                     
b Include raw mill emissions.                                           

    The data shown are short-term performance measurements at cement 
plants that became subject to the NSPS subsequent to the 1979 NSPS 
review. The data in Table 10 served as the basis for the decision on 
the 1985 NSPS review to keep the emission limit established by the 
original NSPS for clinker cooler PM emissions at 0.05 kg/Mg of dry feed 
(.1 lb/ton of dry feed). Because no other PM data on clinker coolers 
became available as a result of this rule development, the Agency is 
relying on these same data (and interpretation thereof) in establishing 
the MACT floor for clinker coolers. The results for FFs serving only 
clinker coolers ranged from 0.002 to 0.025 kg/Mg of dry feed, all of 
which were in compliance with the NSPS. These data represent the 
performance level achieved by FFs designed to meet the NSPS level of 
control. No technologies were identified for existing or new sources 
that would achieve significant additional reductions in PM or metal HAP 
emissions; consequently, there is no beyond-the-floor technology and 
the MACT for new clinker coolers is also the NSPS level. Therefore the 
PM emission limit proposed for new and existing clinker coolers is 0.05 
kg/Mg dry feed (0.10 lb/ton dry feed), which is equivalent to the NSPS 
limit. An opacity limit of 10 percent (which is required under the 
NSPS) is also being proposed.
    The production-based emission limit format was chosen for clinker 
cooler PM emissions. The units for this emission standard are kg of PM 
per Mg of dry feed (lb PM per ton of dry feed). This

[[Page 14204]]

format (mass per unit of production) and associated opacity limit is 
consistent with the format of the portland cement plant NSPS (40 CFR 
part 60, subpart F).
    Raw material dryer and materials handling processes opacity. 
Particulate matter emissions from raw material dryers and materials 
handling processes at portland cement plants are typically captured by 
enclosures (total or partial) and/or hooding of transfer points. In 
most cases, the exhaust gases are directed to FF systems. At least 31 
portland cement plants (docket item II-A-4) have some affected sources 
that are subject to the requirements of the NSPS for portland cement 
plants (40 CFR part 60, subpart F). No technologies which are more 
efficient than FFs are in use for these affected sources. State agency 
personnel indicated that none of the facilities had problems meeting 
the NSPS opacity limit of 10 percent (docket item II-A-4, docket item 
II-B-71). The design characteristics of FFs applied to these emission 
sources include air-to-cloth ratios ranging from 0.02 (m 3/
sec) /m 2 (4 acfm/ft 2) to 0.041 (m 3/ 
sec) /m 2 (8 acfm/ft2) at pulse-jet and pulsed-
plenum cleaning systems in installations subject to the NSPS since the 
1979 NSPS review (docket item II-A-4, II-I-43). Therefore, the MACT 
floor technology for control of PM emissions from portland cement 
materials handling processes and raw material dryers is a combination 
of total enclosures, partial enclosures, or hooding with FF systems. No 
beyond-the-floor technologies for control of PM from raw material 
dryers and materials handling processes were identified.
    The emission limit established by the NSPS for raw material dryers 
and materials handling process PM emissions (surrogate for HAP metals) 
is an opacity limit of 10 percent. Given that no more effective 
technologies were identified, the emission limit corresponding to the 
MACT floor, which is the NSPS, is being proposed as MACT for PM 
emissions from new and existing portland cement materials handling 
processes and raw material dryers.
    The proposed standard for PM emissions from new and existing 
materials handling systems and raw material dryers is an opacity limit 
of 10 percent. An opacity limit format was chosen for these affected 
sources because it is consistent with the NSPS format for these 
facilities.
    Raw material dryer THC. Some plants may dry their raw materials in 
separate dryers prior to or during grinding (docket item II-I-43, 
p.750). This drying process can potentially lead to organic HAP and THC 
emissions in a manner analogous to the release of organic HAPs and THC 
emissions from kilns when hot kiln gas contacts incoming feed 
materials. The method available for reducing THC emissions (and organic 
HAPs) is the same technology described for reducing THC emissions from 
kilns and in-line kiln/raw mills. Therefore, the combination of feed 
material selection, site location and feed material blending was 
determined to be MACT for new sources. The numerical emission limit 
proposed for THC from new raw material dryers is 50 ppmvd reported as 
propane, corrected to seven percent oxygen. This represents a level 
which is consistently achievable when feeds with high organic contents 
are avoided.

E. Selection of Testing and Monitoring Requirements

    Testing requirements are being proposed for demonstrating 
compliance with all standards. Initial performance tests for all 
affected sources/pollutant combinations would demonstrate compliance 
with emission limits. These tests would be repeated every 5 years for 
PM from NHW kilns (including alkali bypasses), NHW in-line kiln/raw 
mills (including alkali bypasses), clinker coolers, raw material dryers 
and materials handling processes, and for D/F from kilns and in-line 
kiln/raw mills. Site-specific monitoring parameters would be 
established during the initial and subsequent performance tests for D/F 
from kilns and in-line kiln/raw mill systems. A PMCD inlet temperature 
parameter would be used to ensure continuous compliance with the D/F 
emission limit. The following paragraphs present the rationale for the 
selection of the proposed testing, test methods, and monitoring 
requirements for each affected source and associated pollutant.
1. Kiln and In-line Kiln Raw Mill PM Emissions
    The proposed standards would require the owner or operator of an 
affected NHW kiln or NHW in-line kiln/raw mill to conduct initial and 
periodic (every 5 years) performance tests using appropriate existing 
EPA reference methods in 40 CFR part 60, appendix A. Method 5 would be 
used to demonstrate compliance with the NHW kiln and NHW in-line kiln/
raw mill PM emission limits. (A determination of the particulate matter 
collected in the impingers [the ``back half''] of the Method 5 
particulate sampling train would not be required.) Method 5 is the 
long-standing EPA method for making PM determinations from stationary 
sources. Each performance test would consist of three runs conducted 
under representative operating conditions. Each run would have a 
minimum sampling volume of 0.85 dscm (30 dscf) and a minimum duration 
of 1 hour. The average of the three runs would be used to determine 
compliance. Method 5, as proposed, is currently required to demonstrate 
compliance with the NSPS.
    If the kiln is equipped with a separate alkali bypass, PM emissions 
from the alkali bypass would be determined by a simultaneous Method 5 
test and the combined emissions from the main exhaust and the alkali 
bypass would be subject to the PM emission limit.
    Owners or operators of in-line kiln/raw mills would be required to 
conduct a compliance demonstration with the raw mill in operation and a 
separate compliance demonstration when the raw mill is not in 
operation, since emissions may vary depending on the operating status 
of the raw mill.
    A COM would be required to ensure continuous compliance with the 
standard. During the initial Method 5 performance test, the owner or 
operator would use a COM to demonstrate compliance with the kiln and 
in-line kiln/raw mill opacity limit. If there is an alkali bypass, a 
COM would be required for the alkali bypass and compliance with the 
opacity limit would also be demonstrated for the alkali bypass during 
the initial Method 5 performance test.
    If the PM control device exhausts through a monovent, or if the use 
of a COM in accordance with the installation specifications of PS-1 of 
40 CFR part 60, appendix B were not feasible, a test in accordance with 
Method 9 of appendix A to 40 CFR part 60 would be conducted at the same 
time as the Method 5 performance test. If the control device exhausts 
through multiple stacks, the owner or operator would have the option of 
conducting a Method 9 test in lieu of installing COMs.
    The opacity limit would be 20 percent and would apply to both main 
and alkali bypass stacks. Exceedance of the kiln or in-line kiln/raw 
mill opacity limit, or the alkali bypass opacity limit, for any 30-
minute average would constitute a violation of the kiln or in-line 
kiln/raw mill PM emission limit. Owners or operators of in-line kiln/
raw mills would demonstrate compliance with the opacity limits during 
initial performance tests to be conducted while the raw mill is 
operating and while the raw mill is not operating.
    If the 30-minute average opacity exceeded 15 percent for any ten 
consecutive 30-minute periods as

[[Page 14205]]

determined by the COM, or if any 30-minute average opacity exceeded 15 
percent as determined by a daily Method 9 test, the owner or operator 
would be required to initiate a site-specific operating and maintenance 
(O and M) plan within one hour. The O and M plan would be required as 
part of the permit application submitted in accordance with part 70 of 
this chapter, and would address procedures for proper operation and 
maintenance of the affected source and the APCD and the corrective 
action to be taken.
    If the 30-minute average opacity exceeded 15 percent for five 
percent or more of the kiln operating time as determined by COM, or if 
the 30-minute average opacity reading exceeded 15 percent during five 
percent or more of the daily Method 9 readings in any 6-month reporting 
period, the owner or operator would be required to notify the 
permitting authority within 48 hours and to develop and implement a 
quality improvement plan (QIP) within 180 days. The QIP would address 
improved maintenance practices, process operation changes, appropriate 
improvements in control methods, other appropriate steps to improve 
performance and more frequent or improved monitoring. If the owner or 
operator determined that more than 180 days will be necessary to 
complete the appropriate improvements, the owner or operator would be 
required to notify the permitting authority and obtain a site-specific 
resolution subject to the approval of the permitting authority.
    Each COM would be required to be designed, installed, and operated 
in accordance with PS-1. The use of COMs would provide a timely and 
direct indication of increased emissions. A COM gives an immediate 
indication of an exceedance, and provides for timely action that will 
minimize the duration and, therefore, the emissions of an upset. A COM 
can also signal the long-term gradual deterioration of performance of a 
control device. Failure of any 30-minute average reading to meet the 
opacity limit would constitute a violation of the NHW kiln and NHW in-
line kiln/raw mill PM emission limit.
    Where the use of a COM is not feasible (or at the option of the 
owner or operator when the exhaust is discharged through multiple 
stacks), the proposed standards would require daily visual observations 
using Method 9. The duration of the Method 9 test would be 30 minutes. 
Method 9 is the established EPA method for visual determinations of 
opacity from stationary sources. Method 9 procedures for making visual 
observations and reducing the data would be followed. Failure of any 
30-minute average reading during the daily test to meet the opacity 
limit would constitute a violation of the NHW kiln and NHW in-line 
kiln/raw mill PM emission limit.
    The EPA proposed that HW cement kilns [and other hazardous waste 
combusters (HWCs)] maintain continuous compliance with the PM standard 
through the use of a PM continuous emissions monitoring system (CEMS). 
[See 61 FR at 17358 (April 19, 1996).] As discussed in the proposed HWC 
rule 14 PM CEMS are commercially available and currently in 
use in Europe. For example, PM CEMS are installed for compliance 
assurance purposes in the European Union (EU) for the EU HWC PM 
standard.
---------------------------------------------------------------------------

    \14\The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    The proposal to require HWCs to install a PM CEMS is predicated on 
a successful vendor (with EPA oversight) demonstration test program on 
a hazardous waste incinerator. The purpose of the demonstration test 
program is to verify that at least one PM CEMS can meet the proposed 
performance specifications. The testing program consists of a 
demonstration test and a long term endurance test. The demonstration 
test involves installing the CEMS and carrying out all of the tests 
prescribed in the performance specifications. The long term endurance 
test will involve evaluating (at least one) CEMS for a minimum of six 
months. The purpose of this test is to evaluate the PM CEMS for 
accuracy, daily drift, availability (i. e. up time), ruggedness, and 
maintenance over an extended period. The demonstration test program 
began in 1996 and it is anticipated that the program will conclude in 
1997. The Agency will notice the results and conclusions of the 
demonstration test program in the docket for the hazardous waste 
combustor rule. Considering the outcome of the demonstration test 
program and other relevant information received or developed by EPA, 
the Agency will reevaluate the monitoring requirements for NHW cement 
kilns. The EPA intends to include a requirement for PM CEMs in the 
final rule, unless the analysis of existing or newly acquired data and 
information shows this type of monitoring is not appropriate. The 
Agency will notice the results of this reevaluation in the docket for 
the NHW cement kiln rule.
2. Kiln D/F Emissions
    The proposed standards would require the owner or operator of an 
affected kiln or in-line kiln/raw mill to conduct initial and periodic 
(every five years) performance tests using appropriate existing EPA 
methods in 40 CFR part 60, appendix A. Method 23 is the established 
method for determining D/F concentration. Each performance test would 
consist of three runs conducted under representative operating 
conditions. Each run must be at least 3 hours duration with a minimum 
sampling volume of 2.5 dscm. The average of the three runs would be 
used to determine compliance.
    If the kiln is equipped with an alkali bypass, D/F emissions from 
the alkali bypass would also be subject to Method 23 testing 
requirements and the emissions from the alkali bypass would be subject 
to the D/F emission limit. Furthermore, in-line kiln/raw mills would be 
required to conduct a compliance demonstration with the raw mill in 
operation and a separate compliance demonstration when the raw mill is 
not in operation. However, if an in-line kiln/raw mill has an alkali 
bypass, a compliance demonstration for the alkali bypass would only be 
required when the raw mill is operating.
    There is no CEM available for D/F emissions and no suitable 
surrogate pollutant that could be monitored continuously. Therefore, 
for D/F emissions from an affected NHW kiln or NHW in-line kiln/raw 
mill, the proposed standards would require continuous monitoring and 
recording of the kiln exhaust gas temperature at the inlet to the kiln 
PMCD. If the kiln is equipped with an alkali bypass the proposed 
standards would also require continuous monitoring and recording of the 
gas temperature at the inlet to the alkali bypass PMCD.
    A kiln-specific maximum temperature limit would be established 
during the performance test. The temperature would be continually 
measured during the D/F performance test. The average temperature for 
each of the three runs would be determined, and the average of these 
three averages would, in some cases, be used to establish the kiln-
specific temperature limit. When the D/F performance test emissions 
were 0.15 ng TEQ/dscm or less (corrected to seven percent oxygen), the 
kiln-specific maximum temperature would be the higher of 400 deg. F or 
the average temperature of the performance test plus five percent (not 
to exceed 25 deg. F) of the temperature measured in  deg.F. When the D/
F performance test emissions (corrected to seven percent oxygen) were 
greater than 0.15 ng TEQ/dscm but did not exceed 0.20 ng TEQ/dscm, the 
kiln-specific maximum temperature would be the higher of 400 deg. F or 
the average temperature of the performance test. If D/F emissions 
(corrected to seven

[[Page 14206]]

percent oxygen) are greater than 0.2 ng/dscm TEQ but less than 0.4 ng/
dscm TEQ during the performance test, then the kiln specific 
temperature limit would be set at 400 deg. F. (If D/F emissions exceed 
0.4 ng/dscm, corrected to seven percent oxygen, the performance test 
would be unsuccessful and the kiln or in-line kiln/raw mill would not 
be in compliance with the standard.) The temperature would provide a 
direct indication of D/F emissions from the kiln or in-line kiln/raw 
mill and would be directly enforceable for compliance determinations.
    Owners or operators of kilns and in-line kiln/raw mills equipped 
with alkali bypasses would establish a separate alkali bypass PMCD 
inlet temperature limit for the alkali bypass during the performance 
test. This limit would be based on the temperature at the inlet to the 
alkali bypass PMCD and would be established in the same manner as the 
kiln specific temperature limit. Owners or operators of in-line kiln/
raw mills equipped with alkali bypasses would establish the temperature 
limit for the alkali bypass PMCD inlet during the performance test with 
the raw mill operating.
    The proposed averaging period for inlet temperature to the PMCD is 
9 hours, because the compliance test for D/F consists of 3-three hour 
manual tests which are averaged. Thus the inlet temperature limit is 
established as the average temperature level achieved over the three D/
F runs in a performance test.
    The Agency specifically requests comment on whether a 9-hour block 
average site-specific temperature limit is sufficient to ensure 
compliance with the D/F standard. Because EPA is concerned that D/F 
emissions emitted during high temperature episodes may not 
correspondingly be offset by low emissions during lower temperature 
episodes due to the non-linear relationship between dioxin formation 
and temperature, a 9-hour block average may not be adequate to ensure 
compliance with the D/F standard in some instances. The Agency 
addressed this concern in the proposal for HW combustion sources 
(cement kilns) [61 FR at 17424, (April 19, 1996)]. There, EPA proposed 
a site-specific ten-minute rolling average to control perturbations in 
temperature and a site-specific, one-hour rolling average to control 
average inlet PMCD temperatures. The ten-minute average was proposed to 
address the concern that short-term perturbations above the limit may 
result in D/F emissions that may not be offset by lower emissions at 
lower temperatures. The one-hour averaging period was proposed to limit 
average temperatures. Thus, in today's proposal, the Agency requests 
comment on whether a shorter-term block or rolling average limit (i. 
e., less than 9 hours) is more appropriate than the one proposed, or 
whether a short-term limit in conjunction with the proposed 9-hour 
block average is needed to properly ensure compliance with the D/F 
standard. The EPA further notes that it may also take these comments 
into account in considering what averaging time to adopt for hazardous 
waste combustion sources.
    If carbon injection is used for D/F control, a kiln-specific (and 
where applicable, an alkali bypass-specific) carbon injection rate for 
each run would be established during the performance test. The average 
carbon injection rate for the three runs would be calculated. This 
carbon injection rate would serve as an additional monitoring limit and 
would be required to be maintained or exceeded for every 9-hour period 
of kiln operation. The carbon injection rate would provide a direct 
indication of D/F emissions from the kiln and would be directly 
enforceable for compliance determinations.
3. Kiln and Raw Material Dryer THC Emissions
    The proposed standards applicable to new NHW kiln main exhausts, 
new NHW in-line kiln/raw mill main exhausts and new raw material dryers 
would require the owner or operator to conduct an initial performance 
test of THC emissions from an affected source using a THC CEM and to 
demonstrate continuous compliance with the THC concentration limit of 
50 ppmvd reported as propane (corrected to 7 percent oxygen), through 
operation of a THC CEM. The use of THC CEMs was selected as the 
monitoring method because these instruments are available, accurate and 
reliable, and when calibrated with propane provide an output which is 
consistent with the THC standard. Each THC CEM would be required to be 
designed, installed, and operated in accordance with PS-8A of 40 CFR 
part 60, appendix B 15. The performance test would be of 3 
hours duration. To determine compliance with the THC emission 
concentration limit, a 30-day block averaging period would be used. Any 
exceedance of the THC emission concentration limit over any 30-day 
block averaging period would constitute a violation of the new NHW kiln 
and in-line kiln/raw mill THC standard, or the new raw material dryer 
THC standard.
---------------------------------------------------------------------------

    \15\ The EPA proposed amendments to appendix B of 40 CFR part 60 
on April 19, 1996, at 61 FR 17358.
---------------------------------------------------------------------------

    The rationale for the 30-day block averaging time is that the 
organic content of the feed material may vary with quarry or mine 
location. Once raw material storage bins are filled with high organic 
content feed material and an excursion is experienced, it may take a 
considerable amount of time to consume these already stored feed 
materials and locate/obtain feed materials with lower organic content.
4. Clinker Cooler PM Emissions
    As in the case with NHW kiln and NHW in-line kiln/raw mill PM 
emissions, the proposed standards would require the owner or operator 
of an affected clinker cooler to conduct initial and periodic (every 5 
years) performance tests using EPA Method 5 of 40 CFR part 60, appendix 
A. Method 5 is the long-standing method for making PM determinations 
from stationary sources. (A determination of the particulate matter 
collected in the impingers [``back half''] of the Method 5 particulate 
sampling train would not be required.) Each performance test would 
consist of three runs conducted under representative operating 
conditions. Each run would have a minimum sampling volume of 0.85 dscm 
(30 dscf) and a minimum duration of 1-hour. The average of the three 
runs would be used to determine compliance with the PM limit. Method 5 
is currently required to demonstrate compliance with the NSPS.
    The opacity limit for clinker coolers is 10 percent. The proposed 
clinker cooler emissions monitoring requirements are the same as the 
proposed requirements for affected NHW kilns and NHW in-line kilns/raw 
mills. A COM would be required to ensure continuous compliance with the 
standard. During the initial Method 5 performance test, the owner or 
operator would use a COM to demonstrate initial compliance with the 
opacity limit.
    If the control device exhausts through a monovent, or if the use of 
a COM in accordance with the installation specifications of PS-1 of 40 
CFR part 60, appendix B were not feasible, a Method 9 test would be 
conducted at the same time as the Method 5 performance test. If the 
control device exhausts through multiple stacks, the owner or operator 
would have the option of conducting a Method 9 test in lieu of 
installing COMs. Exceedance of the clinker cooler opacity limit for any 
30-minute average would constitute a violation of the clinker cooler PM 
emission standard.
    Each COM would be required to be designed, installed, and operated 
in accordance with PS-1. The use of COMs

[[Page 14207]]

would provide a timely and direct indication of increased emissions. A 
COM gives an immediate indication of an exceedance, and provides for 
timely action that will minimize the duration and, therefore, the 
emissions of an upset. A COM can also signal the long-term gradual 
deterioration of performance of a control device. Failure of any 30-
minute average reading to meet the clinker cooler opacity limit would 
constitute a violation of the clinker cooler PM emission standard.
    Where the use of a COM is not feasible (or at the option of the 
owner or operator when the exhaust is discharged through multiple 
stacks), the proposed standards would require daily visual observations 
using Method 9. The duration of the Method 9 test would be 30 minutes. 
Method 9 is the established EPA method for visual determinations of 
opacity from stationary sources. Method 9 procedures for making visual 
observations and reducing the data would be followed. Failure of any 
daily reading to meet the 10 percent opacity limit would constitute a 
violation of the clinker cooler PM emission limit.
5. Raw and Finish Mill PM Emissions
    The proposed standards would require the owner or operator of raw 
and finish mills to conduct initial and periodic (every five years) 
compliance tests using Method 9, and to either install, calibrate, 
maintain and operate a bag leak detection system or to conduct daily 
visual observations using Method 22 to ensure compliance with the 
opacity standard. The opacity limit for raw and finish mills is 10 
percent. The duration of the Method 9 tests is 3-hours and the duration 
of the daily Method 22 tests is six minutes. The duration of the Method 
9 test can be reduced to one hour if during the first hour of the test, 
there are no individual readings greater than 10 percent and there are 
no more than three individual readings of 10 percent.
    If visible emissions are detected during any daily Method 22 test, 
the owner or operator must begin a 30-minute Method 9 test within 24 
hours and initiate a site specific operating and maintenance plan 
within one hour. If the bag leak detection system alarm is triggered, 
the owner or operator must initiate a site specific operating and 
maintenance plan within one hour. Failure to conduct a Method 9 test as 
required, failure to initiate a site-specific operating and maintenance 
plan as required, or observation of any 30-minute average opacity in 
excess of 10 percent during the Method 9 test shall constitute a 
violation of the raw mill and finish mill opacity standard.
6. Raw Material Dryer and Materials Handling Processes PM Emissions
    The proposed standards would require the owner or operator of raw 
material dryers and materials handling processes to conduct initial and 
periodic (every five years) performance tests of visual emissions. 
Particulate matter emissions from these sources are much lower than 
those from kilns, clinker coolers, and raw and finish mills, therefore, 
continuous opacity monitoring, and more frequent visual opacity 
measurements are not being proposed. Method 9 of 40 CFR part 60, 
appendix A is the proposed method for the visual opacity measurements. 
As previously noted, Method 9 is the established method for opacity 
determinations for stationary sources, and provides a directly 
enforceable opacity reading for compliance determinations.
    Section 63.6(h)(5)(ii) of the NESHAP general provisions (40 CFR 
part 63, subpart A) requires 3 hours (30 6-minute averages) of Method 9 
observations for determining compliance for fugitive emission sources. 
However, due to the potentially large number of affected materials 
handling sources at portland cement plants, the costs for observations 
from these sources are considered overly burdensome. Furthermore, data 
from similar facilities in non-metallic mineral processing plants 
(docket item II-J-10) show that the opacity readings for the first hour 
are typically the same as the readings for the second and third hours. 
Therefore EPA is proposing a reduction in Method 9 testing duration for 
these facilities to one hour (ten 6-minute averages), provided that no 
individual reading exceeds 10 percent and that no more than three 
individual readings of ten percent are observed during the first hour 
of the test. Exceedance of the 10-percent opacity limit for any 30-
minute average reading would constitute a violation of the proposed 
opacity standard.
7. General Monitoring Requirements
    The general provisions in 40 CFR part 63, subpart A require each 
owner or operator to develop and implement a startup, shutdown, and 
malfunction plan. The proposed NESHAP requires the owner or operator to 
include procedures to be followed in the event that a CEM, COM or 
temperature monitor indicates that emissions exceed the applicable 
standards. Block averages are proposed for opacity, D/F, and THC 
monitoring required by the standard.
    Owners or operators are also required to develop site specific 
operating and maintenance plans as part of the part 70 permit 
application process. Such plans are applicable to the operation and 
maintenance of kilns, in-line kiln/raw mills, raw mills and finish 
mills and the PM APCDs associated with these affected sources.

F. Selection of Notification, Recordkeeping, and Reporting Requirements

    The proposed NESHAP would require portland cement manufacturing 
plants to comply with all applicable requirements in the NESHAP general 
provisions (40 CFR part 63, subpart A), including recordkeeping, 
notification, and reporting requirements. General recordkeeping 
requirements would include relevant records for each affected source 
of: (1) The occurrence and duration of each startup, shutdown, or 
malfunction of operation of process equipment, (2) the occurrence and 
duration of each malfunction of the air pollution control equipment, 
(3) all maintenance performed on the air pollution control equipment, 
(4) actions taken during startup, shutdown and malfunction that are 
different from the procedures specified in the source's startup, 
shutdown, and malfunction plan, (5) all information necessary to 
demonstrate conformance with the affected source's startup, shutdown, 
and malfunction plan when the plan procedures are followed, (6) each 
period during which a CMS is malfunctioning or inoperative (including 
out-of-control periods), (7) all required measurements needed to 
demonstrate compliance with the standards, (8) all results of 
performance tests, CMS performance evaluations, and opacity and visible 
emissions observations, (9) all measurements as may be necessary to 
determine the conditions of performance tests and performance 
evaluations, (10) all CMS calibration checks, (11) all adjustments and 
maintenance performed on CMS, (12) any information demonstrating 
whether a source is meeting the requirements for a waiver of record 
keeping or reporting requirements, (13) all emission levels relative to 
the criterion for obtaining permission to use an alternative to the 
relative accuracy test, (14) all records or any bag leak detection 
system alarm, and (15) all documentation supporting initial 
notifications and notifications of compliance status. Records would 
also be required of applicability determinations that the source is not 
subject to the requirements of the NESHAP and of CMS measurements, 
operation, and malfunctions.
    General Provisions notification requirements would include: (1) 
initial

[[Page 14208]]

notifications, (2) notification of performance test, (3) notification 
of opacity and visible emission observations, (4) additional 
notifications required for sources with CMS and (5) notification of 
compliance status. Notifications of the requirement to develop and 
implement a QIP, and if applicable, notifications of the inability to 
implement a required QIP within 180 days would also be required by this 
subpart. Reporting requirements would include (1) a report of 
performance test results, (2) a report of results of opacity or visible 
emission observations done concurrently with performance test, (3) 
progress reports if required as a condition of receiving an extension 
of compliance, (4) periodic and immediate startup, shutdown, and 
malfunction reports, and (5) summary excess emissions and performance 
monitoring reports.

VI. Public Participation

    The EPA seeks full public participation in arriving at its final 
decisions and encourages comments on all aspects of this proposal from 
all interested parties. Full supporting data and detailed analyses 
should be submitted with comments to allow EPA to make maximum use of 
the comments. All comments should be directed to the Air and Radiation 
Docket and Information Center, Docket No. A-92-53 (see ADDRESSES). 
Comments on this notice must be submitted on or before the date 
specified in DATES.
    Commenters wishing to submit proprietary information for 
consideration should clearly distinguish such information from other 
comments and clearly label it ``Confidential Business Information'' 
(CBI). Submissions containing such proprietary information should be 
sent directly to the Emission Standards Division CBI Office, U.S. 
Environmental Protection Agency (MD-13), Research Triangle Park, North 
Carolina 27711, with a copy of the cover letter directed to the contact 
person listed above. Confidential business information should not be 
sent to the public docket. Information covered by such a claim of 
confidentiality will be disclosed by EPA only to the extent allowed and 
by the procedures set forth in 40 CFR part 2. If no claim of 
confidentiality accompanies the submission when it is received by EPA, 
it may be made available to the public without further notice to the 
commenter.

VII. Administrative Requirements

A. Docket

    The docket is an organized and complete file of all the information 
considered by EPA in the development of this rulemaking. The docket is 
a dynamic file, because material is added throughout the rulemaking 
development. The docketing system is intended to allow members of the 
public and industries involved to readily identify and locate documents 
so that they can effectively participate in the rulemaking process. 
Along with the proposed and promulgated standards and their preambles, 
the contents of the docket will serve as the record in the case of 
judicial review. [See section 307(d)(7)(A) of the Act.]

B. Public Hearing

    A public hearing will be held, if requested, to discuss the 
proposed standards in accordance with section 307(d)(5) of the Act. 
Persons wishing to make oral presentations on the proposed standards 
should contact EPA (see ADDRESSES). If a public hearing is requested 
and held, EPA will ask clarifying questions during the oral 
presentation but will not respond to the presentations or comments. To 
provide an opportunity for all who may wish to speak, oral 
presentations will be limited to 15 minutes each. Any member of the 
public may file a written statement on or before May 26, 1998. Written 
statements should be addressed to the Air and Radiation Docket and 
Information Center (see ADDRESSES), and refer to Docket No. A-92-53. 
Written statements and supporting information will be considered with 
equivalent weight as any oral statement and supporting information 
subsequently presented at a public hearing, if held. A verbatim 
transcript of the hearing and written statements will be placed in the 
docket and be available for public inspection and copying, or mailed 
upon request, at the Air and Radiation Docket and Information Center 
(see ADDRESSES).

C. Executive Order 12866

    Under Executive Order 12866 (58 FR 51735, October 4, 1993), EPA 
must determine whether the regulatory action is ``significant'' and 
therefore subject to review by the Office of Management and Budget 
(OMB), and the requirements of the Executive Order. The Executive Order 
defines ``significant regulatory action'' as one that is likely to 
result in a rule that may:
    (1) Have an annual effect on the economy of $100 million or more or 
adversely affect in a material way the economy, a sector of the 
economy, productivity, competition, jobs, the environment, public 
health or safety, or State, local, or tribal governments or 
communities;
    (2) Create a serious inconsistency or otherwise interfere with an 
action taken or planned by another agency;
    (3) Materially alter the budgetary impact of entitlements, grants, 
user fees, or loan programs, or the rights and obligation of recipients 
thereof; or
    (4) Raise novel legal or policy issues arising out of legal 
mandates, the President's priorities, or the principles set forth in 
the Executive Order.
    Because the projected annual costs (including monitoring) for this 
NESHAP are $27 million a regulatory impact analysis has not been 
prepared. However this action is considered a ``significant regulatory 
action'' within the meaning of Executive Order 12866, and the proposed 
regulation presented in this notice was submitted to the OMB for 
review. Any written comments are included in the docket listed at the 
beginning of today's notice under ADDRESSES. The docket is available 
for public inspection at the EPA's Air Docket Section, which is listed 
in the ADDRESSES section of this preamble.

D. Enhancing the Intergovernmental Partnership Under Executive Order 
12875

    In compliance with Executive Order 12875, EPA has involved State 
and local regulatory experts in the development of this proposed rule. 
One tribal government and one State government is believed to be 
affected by this proposed rule. Local governments, and State 
governments other than the one State which operates a portland cement 
plant are not directly impacted by the rule, i.e., they are not 
required to purchase control systems to meet the requirements of the 
rule. However, they will be required to implement the rule; e.g., 
incorporate the rule into permits and enforce the rule. They will 
collect permit fees that will be used to offset the burden of 
implementing the rule. Comments have been solicited from States and 
from local air pollution control agency representatives and these 
comments have been carefully considered in the rule development 
process. In addition, all States are encouraged to comment on this 
proposed rule during the public comment period, and the EPA intends to 
fully consider these comments in the development of the final rule.

E. Unfunded Mandates Reform Act

    Section 202 of the Unfunded Mandates Reform Act of 1995 (UMRA), 
signed into law on March 22, 1995 (109

[[Page 14209]]

Stat. 48), requires that the Agency prepare a budgetary impact 
statement before promulgating a rule that includes a Federal mandate 
that may result in expenditure by State, local, and tribal governments, 
in aggregate, or by the private sector, of $100 million or more in any 
one year. Section 203 requires the Agency to establish a plan for 
obtaining input from and informing, educating, and advising any small 
governments that may be significantly or uniquely affected by the rule.
    Under section 205 of the UMRA, the Agency must identify and 
consider a reasonable number of regulatory alternatives before 
promulgating a rule for which a budgetary impact statement must be 
prepared. The Agency must select from those alternatives the least 
costly, most cost-effective, or least burdensome alternative for State, 
local, and tribal governments and the private sector that achieves the 
objectives of the rule, unless the Agency explains why this alternative 
is not selected or unless the selection of this alternative is 
inconsistent with law.
    Because this proposed rule, if promulgated, is estimated to result 
in the expenditure by State, local, and tribal governments or the 
private sector of less than $100 million in any one year, the Agency 
has not prepared a budgetary impact statement or specifically addressed 
the selection of the least costly, most cost-effective, or least 
burdensome alternative. Because small governments will not be 
significantly or uniquely affected by this rule, the Agency is not 
required to develop a plan with regard to small governments. Therefore, 
the requirements of the UMRA do not apply to this action.

F. Regulatory Flexibility Act

    Under section 605 of the Regulatory Flexibility Act of 1980, 5 
U.S.C. 601 et seq., Federal agencies are required to assess the 
economic impact of Federal regulations on small entities. The 
Regulatory Flexibility Act specifies that Federal agencies must prepare 
an initial Regulatory Flexibility Analysis (RFA) if a proposed 
regulation will have a significant economic impact on a substantial 
number of small entities. For the purposes of the Agency's 
implementation of the Act, the EPA's guidelines define a ``substantial 
number'' as 100 or more firms.
    The manufacture of portland cement is covered by SIC code 3241 for 
hydraulic cements. According to Small Business Administration size 
standards, firms owning portland cement plants are categorized as small 
if the total number of employees at the firm is less than 750. 
Otherwise the firm is classified as large. A total of 7 firms are 
categorized as small, while the remaining 37 firms are large. Because a 
substantial number of small firms are not affected, and the EPA does 
not project a significant impact on small firms, the rule does not 
require an RFA.
    I certify that the rule will not have a significant economic impact 
on a substantial number of small entities. This is because the rule has 
a control cost share of revenue of less than one percent for all of the 
seven cement plants which are considered small entities. [Refer to 
section IV.H. (Economic Impacts) for more details on the cost and 
estimated price increases.]
    Although the rule will not have a significant impact on a 
substantial number of small entities, nevertheless the Agency has 
worked with portland cement small entities throughout the rulemaking 
process. Meetings were held on a regular basis with the Portland Cement 
Association (PCA) and industry representatives, including both small 
and large firms, to discuss the development of the rule, exchange 
information and data, solicit comments on draft rule requirements, and 
provide a list of the small firms. In addition, some cement industry 
representatives formed a group called the ``Small Cement Company MACT 
Coalition'', which was represented by counsel during meetings held with 
the PCA and industry representatives during the later stages of the 
proposal development process. Finally, the Small Cement Company MACT 
Coalition designated the PCA as its representative in future meetings 
with the EPA concerning the rulemaking for the portland cement 
industry.
    To minimize adverse impacts on the small entities, the Agency has 
proposed controls at the MACT-floor level and tailored the requirements 
to permit less costly testing and monitoring by using surrogates for 
HAP emissions and provided choice in methods of demonstrating 
compliance. The Agency has also tried to make the rule ``user 
friendly,'' with language that is easy to understand by all of the 
regulated community. To minimize capital availability problems EPA also 
proposes to allow affected firms up to 3 years from the effective date 
of the final rule to comply. An extra year may be granted by the 
Administrator or delegated regulatory authority if necessary to install 
controls.

G. Paperwork Reduction Act

    The information collection requirements in this proposed rule have 
been submitted for approval to OMB under the requirements of the 
Paperwork Reduction Act, 44 U.S.C. 3501 et seq. An Information 
Collection Request (ICR) document has been prepared by EPA (ICR No. 
1801.01), and a copy may be obtained from Sandy Farmer, OPPE Regulatory 
Information Division, U.S. Environmental Protection Agency (2137), 401 
M Street SW., Washington, DC 20460, or by calling (202) 260-2740.
    The proposed information requirements include the notification, 
recordkeeping, and reporting requirements of the NESHAP general 
provisions (40 CFR part 63, subpart A), authorized under section 114 of 
the Act, which are mandatory for all owners or operators subject to 
national emission standards. All information submitted to EPA for which 
a claim of confidentiality is made is safeguarded according to Agency 
policies in 40 CFR part 2, subpart B. The proposed rule does not 
require any notifications or reports beyond those required by the 
general provisions. These information requirements are necessary to 
determine compliance with the standard.
    The annual public reporting and recordkeeping burden for this 
collection is estimated at 77,000 labor hours per year at a total 
annual cost of $2,470,000 over the three-year period. This corresponds 
to an estimated burden of approximately 2000 hours per year for an 
estimated 39 respondents. This estimate includes performance tests and 
reports (with repeat tests where needed); one-time preparation of a 
startup, shutdown, and malfunction plan with semiannual reports of any 
event where the procedures in the plan were not followed; semiannual 
excess emissions reports; notifications; and recordkeeping. Total 
annualized capital costs associated with monitoring requirements over 
the three-year period of the ICR is estimated at $194,000; this 
estimate includes the capital and startup costs associated with 
installation of required continuous monitoring equipment for those 
affected subject to the standard. The total operation and maintenance 
cost is estimated at $191,000 per year.
    Burden means the total time, effort, or financial resources 
expended by persons to generate, maintain, retain, or disclose or 
provide information to or for a Federal agency. This includes the time 
needed to review instructions; develop, acquire, install, and utilize 
technology and systems for the purpose of collecting, validating, and 
verifying information; processing and maintaining information, and 
disclosing and providing information; adjust the existing ways to 
comply with any

[[Page 14210]]

previously applicable instructions and requirements; train personnel to 
respond to a collection of information; search existing data sources; 
complete and review the collection of information; and transmit or 
otherwise disclose the information.
    An Agency may not conduct or sponsor, and a person is not required 
to respond to a collection of information unless it displays a 
currently valid OMB control number. The OMB control numbers for EPA's 
regulations are listed in 40 CFR part 9 and 48 CFR chapter 15.
    Send comments on the Agency's need for this information, the 
accuracy of the provided burden estimates, and any suggested methods 
for minimizing respondent burden, including through the use of 
automated collection techniques to the Director, OPPE Regulatory 
Information Division; U.S. Environmental Protection Agency (2137), 401 
M Street SW., Washington, DC 20460; and to the Office of Information 
and Regulatory Affairs, Office of Management and Budget, 725 17th 
Street, NW, Washington, D.C. 20503, marked ``Attention: Desk Officer 
for EPA.'' Include the ICR number in any correspondence. Since OMB is 
required to make a decision concerning the ICR between 30 and 60 days 
after March 24, 1998, a comment to OMB is best assured of having its 
full effect if OMB receives it by April 23, 1998. The final rule will 
respond to any OMB or public comments on the information collection 
requirements contained in this proposal.

H. Clean Air Act

    In accordance with section 117 of the Act, publication of this 
proposal was preceded by consultation with appropriate advisory 
committees, independent experts, and Federal departments and agencies. 
This regulation will be reviewed eight years from the date of 
promulgation. This review will include an assessment of such factors as 
evaluation of the residual health risks, any overlap with other 
programs, the existence of alternative methods, enforceability, 
improvements in emission control technology and health data, and the 
recordkeeping and reporting requirements.

List of Subjects in 40 CFR Part 63

    Environmental protection, Air pollution control, Hazardous 
substances, Portland cement manufacturing, Reporting and recordkeeping 
requirements.

    Dated: March 9, 1998.
Carol M. Browner,
Administrator.

    For the reasons set out in the preamble, part 63 of title 40, 
chapter 1 of the Code of Federal Regulations is proposed to be amended 
as follows:

PART 63--NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS 
FOR SOURCE CATEGORIES

    1. The authority citation for part 63 continues to read as follows:

    Authority: Secs. 101, 112, 114, 116, 183(f) and 301 of the Clean 
Air Act as amended (42 U.S.C. et seq).

    2. Part 63 is amended by adding a new subpart LLL consisting of 
Secs. 63.1340 through 63.1359 to read as follows:

Subpart LLL--National Emission Standards for the Portland Cement 
Manufacturing Industry

Sec.
63.1340  Applicability and designation of affected sources.
63.1341  Definitions.
63.1342  Standards: General.
63.1343  Standards for kilns and in-line kiln/raw mills.
63.1344  Standards for clinker coolers.
63.1345  Standards for new and reconstructed raw material dryers.
63.1346  Standards for affected sources other than kilns, in-line 
kiln raw mills, clinker coolers, and new and reconstructed raw 
material dryers.
63.1347  Compliance dates.
63.1348  Initial compliance demonstration.
63.1349  Monitoring requirements.
63.1350  Additional test methods.
63.1351  Notification requirements.
63.1352  Reporting requirements.
63.1353  Recordkeeping requirements.
63.1354  Delegation of authority.
63.1355-63.1359  [Reserved]

Table 1 to Subpart LLL--Applicability of General Provisions

Subpart LLL--National Emission Standards for the Portland Cement 
Manufacturing Industry


Sec. 63.1340  Applicability and designation of affected sources.

    (a) Except as specified in paragraphs (b) and (c) of this section, 
the provisions of this subpart apply to each new and existing portland 
cement plant which is a major source or an area source as defined in 
Sec. 63.2 of this part.
    (b) The affected sources subject to this subpart are:
    (1) Each kiln and each in-line kiln/raw mill at any major or area 
source, including alkali bypasses, except for kilns and in-line kiln/
raw mills that burn hazardous waste and are subject to and regulated 
under subpart EEE of this part.1
---------------------------------------------------------------------------

    \1\ The EPA proposed regulations for subpart EEE of 40 CFR part 
63 on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    (2) Each clinker cooler at any portland cement plant which is a 
major source;
    (3) Each raw mill at any portland cement plant which is a major 
source;
    (4) Each finish mill at any portland cement plant which is a major 
source;
    (5) Each raw material dryer at any portland cement plant which is a 
major source;
    (6) Each raw material, clinker, or finished product storage bin at 
any portland cement plant which is a major source;
    (7) Each conveying system transfer point at any portland cement 
plant which is a major source;
    (8) Each bagging system at any portland cement plant which is a 
major source; and
    (9) Each bulk loading or unloading system at any portland cement 
plant which is a major source.
    (c) For portland cement plants with on-site nonmetallic mineral 
processing facilities, the first affected source in the sequence of 
materials handling operations subject to this subpart is the raw 
material storage, which is just prior to the raw mill. The primary and 
secondary crushers and any other equipment of the on-site nonmetallic 
mineral processing plant which precedes the raw material storage are 
not subject to this subpart. Furthermore, the first conveyor transfer 
point subject to this subpart is the transfer point associated with the 
conveyor transferring material from the raw material storage to the raw 
mill.
    (d) The owner or operator of any affected source subject to the 
provisions of this subpart is subject to title V permitting 
requirements.


Sec. 63.1341  Definitions.

    All terms used in this subpart that are not defined below have the 
meaning given to them in the CAA and in subpart A of this part.
    Alkali bypass means a duct between the feed end of the kiln and the 
preheater tower through which a portion of the kiln exit gas stream is 
withdrawn and quickly cooled by air or water to avoid excessive buildup 
of alkali and sulfur on the raw feed.
    Bag leak detection system means a monitoring system for a fabric 
filter that identifies an increase in particulate emissions resulting 
from a broken filter bag or other malfunction and sounds an alarm.
    Bagging system means the equipment which fills bags with portland 
cement.

[[Page 14211]]

    Clinker cooler means equipment into which clinker product leaving 
the kiln is placed to be cooled by air supplied by a forced draft or 
natural draft supply system.
    Conveying system means a device for transporting materials from one 
piece of equipment or location to another location within a facility. 
Conveying systems include but are not limited to the following: 
feeders, belt conveyors, bucket elevators and pneumatic systems.
    Conveying system transfer point means a point where any material 
including but not limited to feed material, fuel, clinker or product, 
is transferred to or from a conveying system, or between separate parts 
of a conveying system.
    Dioxins and furans (D/F) means
tetra-, penta-, hexa-, hepta-, and octa-chlorinated dibenzo dioxins and 
furans.
    Facility means all contiguous or adjoining property that is under 
common ownership or control, including properties that are separated 
only by a road or other public right-of-way.
    Feed means the prepared and mixed materials, which include but are 
not limited to materials such as limestone, clay, shale, sand, iron 
ore, mill scale, and flyash, that are fed to the kiln and become part 
of the clinker product. Feed does not include the fuels used in the 
kiln to produce heat to form the clinker product.
    Finish mill means a roll crusher, ball and tube mill or other size 
reduction equipment used to grind clinker to a fine powder. Gypsum and 
other materials may be added to and blended with clinker in a finish 
mill. The finish mill also includes the air separator associated with 
the finish mill.
    Hazardous waste is defined in Sec. 261.3 of this chapter.
    In-line kiln/raw mill means a system in a portland cement 
production process where a dry kiln system is integrated with the raw 
mill so that all or a portion of the kiln exhaust gases are used to 
perform the drying operation of the raw mill, with no auxiliary heat 
source used. In this system the kiln is capable of operating without 
the raw mill operating, but the raw mill cannot operate without the 
kiln gases, and consequently, the raw mill does not generate a separate 
exhaust gas stream.
    Kiln means a device, including any associated preheater or 
precalciner devices, that produces clinker by heating limestone and 
other materials for subsequent production of cement.
    Monovent means an exhaust configuration of a building or emission 
control device (e. g. positive pressure fabric filter) that extends the 
length of the structure and has a width very small in relation to its 
length (i.e., length to width ratio is typically greater than 5:1). The 
exhaust may be an open vent with or without a roof, louvered vents, or 
a combination of such features.
    Portland cement plant means any facility manufacturing portland 
cement.
    Raw material dryer means an impact dryer, drum dryer, paddle-
equipped rapid dryer, air separator, or other equipment used to reduce 
the moisture content of feed materials.
    Raw mill means a ball and tube mill, vertical roller mill or other 
size reduction equipment, that is not part of an in-line kiln/raw mill, 
used to grind feed to the appropriate size. Moisture may be added or 
removed from the feed during the grinding operation. If the raw mill is 
used to remove moisture from feed materials, it is also, by definition, 
a raw material dryer. The raw mill also includes the air separator 
associated with the raw mill.
    TEO means the international method of expressing toxicity 
equivalents for dioxins and furans as defined in U.S. EPA, Interim 
Procedures for Estimating Risks Associated with Exposures to Mixtures 
of Chlorinated Dibenzo-p-dioxins and -dibenzofurans (CDDs and CDFs) and 
1989 Update, March 1989.


Sec. 63.1342  Standards: General.

    Table 1 to this subpart provides cross references to the 40 CFR 
part 63, subpart A, general provisions, indicating the applicability of 
the general provisions requirements to subpart LLL.


Sec. 63.1343  Standards for kilns and in-line kiln/raw mills.

    (a) The provisions in this section apply to each kiln, each in-line 
kiln/raw mill, and any alkali bypass associated with that kiln or in-
line kiln/raw mill.
    (b) No owner or operator of an existing kiln or in-line kiln/raw 
mill at a facility that is a major source subject to the provisions of 
this subpart shall cause to be discharged into the atmosphere from 
these affected sources, any gases which:
    (1) Contain particulate matter in excess of 0.15 kg per Mg (0.30 lb 
per ton) of feed (dry basis) to the kiln. When there is an alkali 
bypass associated with a kiln or in-line kiln/raw mill, the combined 
particulate matter emissions from the kiln or in-line kiln/raw mill and 
the alkali bypass are subject to this emission limit.
    (2) Exhibit opacity greater than 20 percent.
    (3) Contain D/F in excess of
    (i) 0.20 ng per dscm (8.7  x  10-11 gr per dscf)(TEQ) 
corrected to seven percent oxygen; or
    (ii) 0.40 ng per dscm (1.7  x  10-10 gr per dscf)(TEQ) 
corrected to seven percent oxygen, when the temperature at the inlet to 
the particulate matter air pollution control device is 204  deg.C 
(400 deg.(F) or less.
    (c) No owner or operator that commences construction of a new kiln 
or new inline kiln/raw mill, or commences reconstruction of a kiln or 
in-line kiln/raw mill at a facility which is a major source subject to 
the provisions of this subpart shall cause to be discharged into the 
atmosphere from these affected sources any gases which:
    (1) Contain particulate matter in excess of 0.15 kg per Mg (0.30 lb 
per ton) of feed (dry basis) to the kiln. When there is an alkali 
bypass associated with a kiln or in-line kiln/raw mill, the combined 
particulate matter emissions from the kiln or in-line kiln/raw mill and 
the bypass stack are subject to this emission limit.
    (2) Exhibit opacity greater than 20 percent.
    (3) Contain D/F in excess of
    (i) 0.20 ng per dscm (8.7  x  10-11 gr per dscf) (TEQ) 
corrected to seven percent oxygen; or
    (ii) 0.40 ng per dscm (1.7  x  10-10 gr per dscf) (TEQ) 
corrected to seven percent oxygen, when the temperature at the inlet to 
the particulate matter air pollution control device is 204  deg.C (400 
deg.F) or less.
    (4) Contain total hydrocarbon (THC), from the main exhaust of the 
kiln or in-line kiln/raw mill, in excess of 50 ppmvd as propane, 
corrected to seven percent oxygen.
    (d) No owner or operator of a new or existing kiln or in-line kiln/
raw mill at a facility that is an area source subject to the provisions 
of this subpart shall cause to be discharged into the atmosphere from 
these affected sources any gases which contain D/F in excess of:
    (1) 0.20 ng per dscm (8.7  x  10-11 gr per dscf) (TEQ) 
corrected to seven percent oxygen; or
    (2) 0.40 ng per dscm (1.7  x  10-10 gr per dscf) (TEQ) 
corrected to seven percent oxygen, when the temperature at the inlet to 
the particulate matter air pollution control device is 204  deg.C (400 
deg.F) or less.


Sec. 63.1344  Standards for clinker coolers.

    (a) No owner or operator of a new or existing clinker cooler at a 
facility which is a major source subject to the provisions of this 
subpart shall cause to be discharged into the atmosphere from the 
clinker cooler any gases which:
    (1) Contain particulate matter in excess of 0.050 kg per Mg (0.10 
lb per ton) of feed (dry basis) to the kiln.

[[Page 14212]]

    (2) Exhibit opacity greater than ten percent.
    (b) [Reserved]


Sec. 63.1345  Standards for new and reconstructed raw material dryers.

    (a) No owner or operator of a new or reconstructed raw material 
dryer at a facility which is a major source subject to this subpart 
shall cause to be discharged into the atmosphere from the new or 
reconstructed raw material dryer any gases which:
    (1) Contain THC in excess of 50 ppmvd, reported as propane, 
corrected to seven percent oxygen.
    (2) Exhibit opacity greater than ten percent.
    (b) [Reserved]


Sec. 63.1346  Standards for affected sources other than kilns, in-line 
kiln/raw mills, clinker coolers, and new and reconstructed raw material 
dryers.

    The owner or operator of each new or existing raw mill; finish 
mill; raw material, clinker, or finished product storage bin; conveying 
system transfer point; bagging system; and bulk loading or unloading 
system; and each existing raw material dryer, at a facility which is a 
major source subject to the provisions of this subpart shall not cause 
to be discharged any gases from these affected sources which exhibit 
opacity in excess of ten percent.


Sec. 63.1347  Compliance dates.

    (a) The compliance date for an owner or operator of an existing 
affected source subject to the provisions of this subpart is no later 
than 36 months after publication of the final rule.
    (b) The compliance date for an owner or operator of an affected 
source subject to the provisions of this subpart that commences new 
construction or reconstruction after March 24, 1998 is the date of 
publication of the final rule or immediately upon startup of 
operations, whichever is later.


Sec. 63.1348  Initial compliance demonstration.

    (a) The owner or operator of an affected source subject to this 
subpart shall demonstrate initial compliance with the emission limits 
of Secs. 63.1343-63.1346 using the test methods and procedures in 
paragraph (b) of this section and Sec. 63.7. Performance test results 
shall be documented in complete test reports that contain the 
information required by paragraphs (a)(1) through (a)(10) of this 
section, as well as all other relevant information. The plan to be 
followed during testing shall be made available to the Administrator 
prior to testing, if requested.
    (1) A brief description of the process and the air pollution 
control system;
    (2) Sampling location description(s);
    (3) A description of sampling and analytical procedures and any 
modifications to standard procedures;
    (4) Test results;
    (5) Quality assurance procedures and results;
    (6) Records of operating conditions during the test, preparation of 
standards, and calibration procedures;
    (7) Raw data sheets for field sampling and field and laboratory 
analyses;
    (8) Documentation of calculations;
    (9) All data recorded and used to establish parameters for 
compliance monitoring; and
    (10) Any other information required by the test method.
    (b) Performance tests to demonstrate initial compliance with this 
subpart shall be conducted as specified in paragraphs (b)(1) through 
(b)(5) of this section.
    (1) The owner or operator of a kiln subject to limitations on 
particulate matter emissions shall demonstrate initial compliance by 
conducting a performance test as specified in paragraphs (b)(1)(i) 
through (b)(1)(iv) of this section. The owner or operator of an in-line 
kiln/raw mill shall demonstrate initial compliance by conducting 
separate performance tests as specified in paragraphs (b)(1)(i) through 
(b)(1)(iv) of this section while the raw mill of the in-line kiln/raw 
mill is under normal operating conditions and while the raw mill of the 
in-line kiln/raw mill is not operating. The owner or operator of a 
clinker cooler subject to limitations on particulate matter emissions 
shall demonstrate initial compliance by conducting a performance test 
as specified in paragraphs (b)(1)(i) through (b)(1)(iii) of this 
section. The opacity exhibited during the period of the Method 5 
performance tests required by paragraph (b)(1)(i) of this section shall 
be determined as required in paragraphs (b)(1)(v) through (vi) of this 
section.
    (i) EPA Method 5 of appendix A to part 60 of this chapter shall be 
used to determine PM emissions. Each performance test shall consist of 
three separate runs under the conditions that exist when the affected 
source is operating at the highest load or capacity level reasonably 
expected to occur. Each run shall be conducted for at least one hour, 
and the minimum sample volume shall be 0.85 dscm (30 dscf). The average 
of the three runs shall be used to determine compliance. A 
determination of the particulate matter collected in the impingers 
(``back half'') of the Method 5 particulate sampling train is not 
required.
    (ii) Suitable methods shall be used to determine the kiln or inline 
kiln/raw mill feed rate, except for fuels, for each run.
    (iii) The emission rate, E, of PM shall be computed for each run 
using equation 1:

E = (cs Qsd) / P

Where:

E = emission rate of particulate matter, kg/Mg of kiln feed.
cs = concentration of PM, kg/dscm.
Qsd = volumetric flow rate of effluent gas, dscm/hr.
P = total kiln feed (dry basis), Mg/hr.

    (iv) When there is an alkali bypass associated with a kiln or in-
line kiln/raw mill, the main exhaust and alkali bypass of the kiln or 
in-line kiln/raw mill shall be tested simultaneously and the combined 
emission rate of particulate matter from the kiln or in-line kiln/raw 
mill and alkali bypass shall be computed for each run using equation 2,

Ec = (cskQsdk + 
csbQsdb)/P  

Where:

Ec = the combined emission rate of particulate matter from 
the kiln or in-line kiln/raw mill and bypass stack, kg/Mg of kiln feed,
csk = concentration of particulate matter in the kiln or in-
line kiln/raw mill effluent, kg/dscm,
Qsdk = volumetric flow rate of kiln or in-line kiln/raw mill 
effluent, dscm/hr,
csb = concentration of particulate matter in the alkali 
bypass gas, kg/dscm,
Qsdb = volumetric flow rate of alkali bypass gas, dscm/hr, 
and P = total kiln feed (dry basis), Mg/hr.

    (v) Except as provided in paragraph (b)(1)(vi) of this section the 
opacity exhibited during the period of the Method 5 performance tests 
required by paragraph (b)(1)(i) of this section shall be determined 
through the use of a continuous opacity monitor (COM). The maximum six-
minute average opacity during the three Method 5 test runs shall be 
determined during each Method 5 test run, and used to demonstrate 
initial compliance with the applicable opacity limits of 
Secs. 63.1343(b)(2), 63.1343(c)(2), or 63.1344(a)(2) of this subpart.
    (vi) Each owner or operator of a kiln, in-line kiln/raw mill, or 
clinker cooler subject to the provisions of this subpart using a fabric 
filter with multiple stacks or an electrostatic precipitator with 
multiple stacks may, in lieu of installing the continuous opacity 
monitoring system required by paragraph (b)(1)(v) of this section, 
conduct an opacity test in accordance with Method 9 of appendix A to 
part 60 of this chapter

[[Page 14213]]

during each Method 5 performance test required by paragraph (b)(1)(i) 
of this section. If the control device exhausts through a monovent, or 
if the use of a COM in accordance with the installation specifications 
of Performance Specification 1 (PS-1) of appendix B to part 60 of this 
chapter is not feasible, a test shall be conducted in accordance with 
Method 9 of appendix A to part 60 of this chapter during each Method 5 
performance test required by paragraph (b)(1)(i) of this section. The 
maximum six-minute average opacity shall be determined during the three 
Method 5 test runs, and used to demonstrate initial compliance with the 
applicable opacity limits of Secs. 63.1343(b)(2), 63.1343(c)(2), or 
63.1344(a)(2) of this subpart.
    (2) The owner or operator of a raw mill or finish mill subject to 
limitations on opacity under this subpart shall demonstrate initial 
compliance with the raw mill and finish mill opacity limit by 
conducting a performance test in accordance with Method 9 of appendix A 
to part 60 of this chapter. The performance test shall be conducted 
under the conditions that exist when the affected source is operating 
at the highest load or capacity level reasonably expected to occur. The 
maximum six-minute average opacity exhibited during the performance 
test shall be used to determine whether the affected source is in 
initial compliance with the standard. The duration of the Method 9 
performance test shall be 3-hours (30 6-minute averages), except that 
the duration of the Method 9 performance test may be reduced to 1-hour 
if the conditions of paragraphs (b)(2)(i) through (ii) of the section 
apply:
    (i) There are no individual readings greater than 10 percent 
opacity;
    (ii) There are no more than three readings of 10 percent for the 
first 1-hour period.
    (3) The owner or operator of any affected source subject to 
limitations on opacity under this subpart that is not subject to 
Sec. 63.1348(b)(1) through (2) shall demonstrate initial compliance 
with the affected source opacity limit by conducting a test in 
accordance with Method 9 of appendix A to part 60 of this chapter. The 
maximum six-minute average opacity exhibited during the test period 
shall be used to determine whether the affected source is in initial 
compliance with the standard. The duration of the Method 9 performance 
test shall be 3-hours (30 6-minute averages), except that the duration 
of the Method 9 performance test may be reduced to 1-hour if the 
conditions of paragraphs (b)(3)(i) through (ii) of the section apply:
    (i) There are no individual readings greater than 10 percent 
opacity;
    (ii) There are no more than three readings of 10 percent for the 
first 1-hour period.
    (4) The owner or operator of an affected source subject to 
limitations on D/F emissions shall demonstrate initial compliance with 
the D/F emission limit by conducting a performance test using Method 23 
of appendix A to part 60 of this chapter. The owner or operator of an 
in-line kiln/raw mill shall demonstrate initial compliance by 
conducting separate performance tests while the raw mill of the in-line 
kiln/raw mill is under normal operating conditions and while the raw 
mill of the in-line kiln/raw mill is not operating. The owner or 
operator of a kiln or in-line kiln/raw mill equipped with an alkali 
bypass shall conduct simultaneous performance tests of the kiln or in-
line kiln/raw mill exhaust and the alkali bypass, however the owner or 
operator of an in-line kiln/raw mill is not required to conduct a 
performance test of the alkali bypass exhaust when the raw mill of the 
in-line kiln/raw mill is not operating.
    (i) Each performance test shall consist of three separate runs; 
each run shall be conducted under the conditions that exist when the 
affected source is operating at the highest load or capacity level 
reasonably expected to occur. The duration of each run shall be at 
least three hours and the sample volume for each run shall be at least 
2.5 dscm (90 dscf). The arithmetic average concentration measured 
during each of the three runs shall be used to determine compliance.
    (ii) The temperature at the inlet to the kiln or in-line kiln/raw 
mill PM APCD, and where applicable, the temperature at the inlet to the 
alkali bypass PM APCD, must be continuously recorded during the period 
of the Method 23 test, and the continuous temperature record(s) must be 
included in the performance test report. The arithmetic average 
temperature must be determined for each run. The arithmetic average of 
the averages for the three runs must be calculated and included in the 
performance test report and will determine the applicable temperature 
limit in accordance with Sec. 63.1349(d)(4) of this subpart.
    (iii) If carbon injection is used for D/F control, the carbon 
injection rate must be measured during the period of each run. The 
average carbon injection rate measured for the three runs shall be 
determined and included in the test report, and shall be used for 
compliance purposes in accordance with Sec. 63.1349(e) of this subpart.
    (5) The owner or operator of an affected source subject to 
limitations on emissions of THC shall demonstrate initial compliance 
with the THC limit by operating a continuous emission monitor in 
accordance with Performance Specification 8A of appendix B to part 60 
of this chapter.2 The duration of the performance test shall 
be three hours, and the average THC concentration during the three hour 
performance test shall be calculated. The owner or operator of an in-
line kiln/raw mill shall demonstrate initial compliance by conducting 
separate performance tests while the raw mill of the in-line kiln/raw 
mill is under normal operating conditions and while the raw mill of the 
in-line kiln/raw mill is not operating.
---------------------------------------------------------------------------

    \2\ The EPA proposed amendments to appendix B to 40 CFR part 60 
on April 19, 1996 at 61 FR 17358.
---------------------------------------------------------------------------

    (c) Performance tests required under paragraphs (b)(1) through (4) 
of this section shall be repeated every five years, except that the 
owner or operator of a kiln, in-line kiln/raw mill or clinker cooler is 
not required to repeat the initial performance test of opacity.


Sec. 63.1349  Monitoring requirements.

    (a) The owner or operator of a kiln or in-line kiln/raw mill shall 
demonstrate continuous compliance with the opacity standard at each 
point where emissions are vented from these affected sources including 
alkali bypasses in accordance with paragraphs (a)(1) through (a)(5) of 
this section.
    (1) Except as provided in paragraph (a)(2) of this section, the 
owner or operator shall install, calibrate, maintain, and continuously 
operate a continuous opacity monitor (COM) located at the outlet of the 
PM control device to continuously monitor the opacity. The COM shall be 
installed, maintained, calibrated, and operated as required by subpart 
A, general provisions of this part, and according to PS-1 of appendix B 
to part 60 of this chapter.
    (2) The owner or operator of a kiln or in-line kiln/raw mill 
subject to the provisions of this subpart using a fabric filter with 
multiple stacks or an electrostatic precipitator with multiple stacks 
may, in lieu of installing the continuous opacity monitoring system 
required by paragraph (a)(1) of this section, monitor opacity in 
accordance with paragraphs (a)(2)(i) through (ii) of this section. If 
the control device exhausts through a monovent, or if the use of a COM 
in accordance with the installation specifications of PS-1 of appendix 
B to part 60 of this chapter is not feasible, the owner or operator 
must

[[Page 14214]]

monitor opacity in accordance with paragraphs (a)(2)(i) through (ii) of 
this section.
    (i) Perform daily visual opacity observations of each stack in 
accordance with the procedures of Method 9 of appendix A of part 60 of 
this chapter. The duration of the Method 9 test shall be at least 30 
minutes each day.
    (ii) Use the Method 9 procedures to monitor and record the average 
opacity for each six-minute period during the test.
    (3) To remain in compliance, the opacity must be maintained such 
that the average of the 6-minute average opacities for any 30-minute 
period does not exceed 20 percent. If the average of the six-minute 
average opacities for any 30-minute period exceeds 20 percent, this 
shall constitute a violation of the standard.
    (4) If the average opacity as determined in accordance with 
paragraph (a)(1) of this section exceeds 15 percent for any ten 
consecutive 30-minute periods, or if the average opacity as determined 
in accordance with paragraphs (a)(2)(i) through (ii) of this section 
exceeds 15 percent for any 30-minute period, the owner or operator 
shall initiate a site-specific operating and maintenance plan within 
one hour. The site-specific operating and maintenance plan shall be 
developed in accordance with paragraph (g) of this section. Failure to 
initiate the site-specific operating and maintenance plan within one 
hour shall constitute a violation of the standard.
    (5) If the average 30-minute opacity as determined in accordance 
with paragraph (a)(1) of this section exceeds 15 percent for five 
percent or more of the kiln operating time in any six-month reporting 
period, or if the 30-minute average opacity reading as determined in 
accordance with paragraphs (a)(2)(i) through (ii) of this section 
exceeds 15 percent during five percent or more of the daily readings in 
any six-month reporting period, the owner or operator shall notify the 
permitting authority within 48 hours and shall develop and implement a 
quality improvement plan (QIP) within 180 days. The QIP shall be 
developed in accordance with paragraph (h) of this section. Failure to 
notify the permitting authority within 48 hours shall constitute a 
violation of the standard. Failure to develop and implement a QIP 
within 180 days shall constitute a violation of the standard.
    (b) The owner or operator of a clinker cooler shall demonstrate 
continuous compliance with the opacity standard at each point where 
emissions are vented from the clinker cooler in accordance with 
paragraphs (b)(1) through (b)(3) of this section.
    (1) Except as provided in paragraph (b)(2) of this section, the 
owner or operator shall install, calibrate, maintain, and continuously 
operate a COM located at the outlet of the clinker cooler PM control 
device to continuously monitor the opacity. The COM shall be installed, 
maintained, calibrated, and operated as required by subpart A, general 
provisions of this part, and according to PS-1 of appendix B to part 60 
of this chapter.
    (2) The owner or operator of a clinker cooler subject to the 
provisions of this subpart using a fabric filter with multiple stacks 
or an electrostatic precipitator with multiple stacks may, in lieu of 
installing the continuous opacity monitoring system required by 
paragraph (b)(1) of this section, monitor opacity in accordance with 
paragraphs (b)(2)(i) through (ii) of this section. If the control 
device exhausts through a monovent, or if the use of a COM in 
accordance with the installation specifications of PS-1 of appendix B 
to part 60 of this chapter is not feasible, the owner or operator must 
monitor opacity in accordance with paragraphs (b)(2)(i) through (ii) of 
this section.
    (i) Perform daily visual opacity observations of each stack in 
accordance with the procedures of Method 9 of appendix A of part 60 of 
this chapter. The duration of the Method 9 test shall be at least 30 
minutes each day.
    (ii) Use the Method 9 procedures to monitor and record the average 
opacity for each six-minute period during the test.
    (3) To remain in compliance, the opacity must be maintained such 
that the average of the 6-minute average opacities for any 30-minute 
period does not exceed 10 percent. If the average of the six-minute 
average opacities for any 30-minute period exceeds 10 percent, this 
shall constitute a violation of the standard.
    (c) The owner or operator of a raw mill or finish mill shall 
demonstrate continuous compliance with the opacity standard either by 
conducting visual emissions observations in accordance with paragraph 
(c)(1) of this section or through the use of a bag leak detection 
system in accordance with paragraphs (c)(2)(i) through (vii) of this 
section.
    (1) An owner or operator may demonstrate compliance by performing 
daily visual emissions observations in accordance with the procedures 
of Method 22 of appendix A of part 60 of this chapter. The duration of 
the Method 22 test shall be six-minutes. If no visual emissions are 
observed at any time within the six-minute test, the source is in 
compliance.
    (2) An owner or operator may demonstrate compliance by installing, 
calibrating, maintaining, and continuously operating a bag leak 
detection system in accordance with paragraphs (c)(2)(i) through (vii) 
of this section.
    (i) The bag leak detection system must be capable of detecting PM 
emissions at concentrations of 1.0 mg per actual cubic meter (0.00044 
grains per actual cubic foot) and greater.
    (ii) The bag leak detection system sensor must provide output of 
relative or absolute PM emissions.
    (iii) The bag leak detection system must be equipped with an alarm 
system that will sound when an increase in PM emissions is detected.
    (iv) For positive pressure baghouses, a bag leak detector must be 
installed in each baghouse compartment. If a negative pressure or 
induced air baghouse is used, the bag leak detector must be installed 
downstream of the baghouse. Where multiple detectors are required (for 
either type of baghouse), the system instrumentation and alarm may be 
shared among detectors.
    (v) The bag leak detection system shall be installed, operated, 
calibrated, and maintained in a manner consistent with available 
guidance from the U. S. Environmental Protection Agency or, in the 
absence of such guidance, the manufacturer's written specifications and 
recommendations.
    (vi) Calibration of the system shall, at minimum, consist of 
establishing the relative baseline output level by adjusting the 
sensitivity and averaging period of the device and establishing the 
alarm set points and the alarm delay time.
    (vii) The owner or operator shall not adjust the sensitivity, 
averaging period, alarm set points, or alarm delay time after the 
initial performance test unless a subsequent performance test is 
performed.
    (3) If, in accordance with paragraph (c)(1) of this section visual 
emissions are observed the owner or operator shall follow the 
procedures of paragraphs (c)(3)(i) through (ii) of this section. If, in 
accordance with paragraphs (c)(2)(i) through (vii) of this section, the 
bag leak detection system alarm is triggered, the owner or operator 
shall follow the procedure of paragraphs (c)(3)(i) of this section.
    (i) Initiate, within one-hour, a site specific operating and 
maintenance plan developed in accordance with paragraph (g) of this 
section. If a site specific operating and maintenance plan is not 
initiated within one hour, this

[[Page 14215]]

shall constitute a violation of the standard.
    (ii) Conduct a visual opacity observation of each stack from which 
visible emissions were observed in accordance with the procedures of 
Method 9 of appendix A of part 60 of this chapter. The owner or 
operator must begin the Method 9 test within 24 hours of the end of the 
Method 22 test in which visible emissions were observed. The duration 
of the Method 9 test shall be thirty-minutes. If the average of the 
six-minute average opacities recorded during the Method 9 test exceeds 
10 percent, this shall constitute a violation of the standard. If the 
owner or operator fails to begin the Method 9 test within 24 hours of 
the end of the Method 22 test in which visible emissions were observed, 
this shall constitute a violation of the standard.
    (d) The owner or operator of an affected source subject to a 
limitation on D/F emissions shall comply with the following monitoring 
requirements to demonstrate continuous compliance with the D/F emission 
standard:
    (1) The owner or operator shall install, calibrate, maintain, and 
continuously operate a device to monitor and record the temperature of 
the exhaust gases from the kiln, in-line kiln/raw mill and alkali 
bypass, if applicable, at the inlet to the kiln, in-line kiln/raw mill 
and/or alkali bypass PM control devices consistent with the 
requirements for continuous monitoring systems in subpart A, general 
provisions. The device shall have an accuracy of 2 degrees 
Fahrenheit or 1 percent of the temperature measured in 
degrees Fahrenheit.
    (2) The owner or operator shall monitor and continuously record the 
temperature of the exhaust gases from the kiln, in-line kiln/raw mill 
and alkali bypass, if applicable, at the inlet to the kiln, in-line 
kiln/raw mill and/or alkali bypass PM control device.
    (3) To remain in compliance with the D/F emission limit, the owner 
or operator of a kiln must maintain the temperature of the gas at the 
inlet to the kiln PM control device and alkali bypass PM control 
device, if applicable, such that the applicable temperature limits 
specified in paragraph (d)(4) of this section are never exceeded for 
any nine-hour block averaging period. If any nine-hour average 
temperature exceeds these temperature limits, this shall constitute a 
violation of the standard. To remain in compliance with the D/F 
emission limit, the owner or operator of an in-line kiln/raw mill must 
maintain the temperature of the gas at the inlet to the in-line kiln/
raw mill PM control device and in-line kiln/raw mill alkali bypass PM 
control device, if applicable, such that,
    (i) When the raw mill of the in-line kiln/raw mill is operating, 
the applicable temperature limit(s) specified in paragraph (d)(4) of 
this section and established during the performance test when the raw 
mill was operating is (are) never exceeded for any nine-hour average. 
If any nine-hour average temperature exceeds the applicable temperature 
limit, this shall constitute a violation of the standard, and
    (ii) When the raw mill of the in-line kiln/raw mill is not 
operating, the applicable temperature limit for the main in-line kiln/
raw mill exhaust, specified in paragraph (d)(4) of this section and 
established during the performance test when the raw mill was not 
operating, is never exceeded for any nine-hour block averaging period. 
If any nine-hour average temperature exceeds the applicable temperature 
limit, this shall constitute a violation of the standard, and
    (iii) If the in-line kiln/raw mill is equipped with an alkali 
bypass, the applicable temperature limit for the alkali bypass, 
specified in paragraph (d)(4) of this section and established during 
the performance test when the raw mill was operating, is never exceeded 
for any nine-hour block averaging period. If any nine-hour average 
temperature exceeds the applicable temperature limit, this shall 
constitute a violation of the standard.
    (4) The temperature limit for affected sources meeting the limits 
of Secs. 63.1343(b)(3)(ii), 63.1343(c)(3)(ii) and 63.1343(d)(2) of this 
subpart is 204 degrees C (400 degrees F). The temperature limits(s) for 
affected sources meeting the limits of Secs. 63.1343(b)(3)(i), 
63.1343(c)(3)(i) and 63.1343(d)(1) is (are) determined according to 
paragraphs (d)(4)(i) through (iii) of this section.
    (i) Except as provided in paragraph (d)(4)(iii) of this section, if 
the D/F emissions determined by the most recent performance test 
conducted in accordance with Sec. 63.1348(b)(4) of this subpart do not 
exceed 0.15 ng TEQ/dscm (6.5  x  10-11 gr/dscf), the 
temperature limit(s) is (are) the average temperature(s) recorded 
during the performance test plus five percent of the temperature 
expressed in degrees Fahrenheit, or the average temperature(s) recorded 
during the performance test plus 25 deg. F, whichever is lower.
    (ii) Except as provided in paragraph (d)(4)(iii) of this section, 
if the D/F emissions determined by the most recent performance test 
conducted in accordance with Sec. 63.1348(b)(4) of this subpart is 
(are) between 0.15 ng TEQ/dscm (6.5  x  10-11 gr TEQ/dscf) 
and 0.20 ng TEQ/dscm (8.7  x  10-11 gr TEQ/dscf), the 
temperature limit(s) is (are) the average temperature(s) recorded 
during the performance test.
    (iii) No temperature limit established under this section shall be 
less than 204  deg.C (400  deg.F).
    (5) The calibration of all thermocouples and other temperature 
sensors shall be verified every three months.
    (e) The owner or operator of an affected source subject to a 
limitation on D/F emissions that employs carbon injection as an 
emission control technique shall comply with the monitoring 
requirements of paragraphs (d)(1) through (d)(5) and (e)(1) through 
(e)(2) of this section to demonstrate continuous compliance with the D/
F emission standard:
    (1) Measure the mass of carbon injected for every nine-hour period.
    (2) If the carbon injection rate averaged over any nine-hour period 
is less than the average of the carbon injection rates for the three 
runs of the performance test conducted in accordance with 
Sec. 63.1348(b)(4) of this subpart, this shall constitute a violation 
of the standard.
    (f) The owner or operator of an affected source subject to a 
limitation on THC emissions under this subpart shall comply with the 
monitoring requirements of paragraphs (f)(1) and (f)(2) of this section 
to demonstrate continuous compliance with the THC emission standard:
    (1) The owner or operator shall install, operate and maintain a THC 
continuous emission monitoring system in accordance with Performance 
Specification 8A, of appendix B to part 60 of this chapter 3 
and comply with all of the requirements for continuous monitoring 
systems found in subpart A, general provisions of this part.
---------------------------------------------------------------------------

    \3\ Ibid.
---------------------------------------------------------------------------

    (2) Any thirty-day block average THC concentration in any gas 
discharged from a new or reconstructed raw material dryer, a new or 
reconstructed kiln, or a new or reconstructed in-line kiln/raw mill, 
exceeding 50 ppmvd, reported as propane, corrected to seven percent 
oxygen, is a violation of the standard.
    (g) The owner or operator of each portland cement plant shall 
prepare for each kiln, in-line kiln raw mill, raw mill and finish mill 
which is an affected source subject to the provisions of this subpart, 
a written operations and maintenance plan. The plan shall be

[[Page 14216]]

submitted to the Administrator for review and approval as part of the 
application for a part 70 permit and shall include the following 
information:
    (1) Procedures for proper operation and maintenance of the affected 
source and APCDs in order to meet the emission limits of Sec. 63.1343 
of this subpart for kilns and in-line kiln raw mills and Sec. 63.1346 
of this subpart for raw mills and finish mills, and
    (2) Corrective actions to be taken when required by paragraphs 
(a)(4) or (c)(3)(i) of this section.
    (h) If required under paragraph (a)(5) of this section, an owner or 
operator shall implement a QIP in accordance with paragraphs (h)(1) 
through (h)(4) of this section.
    (1) A QIP shall be a written plan.
    (2) An initial QIP shall include procedures that are adequate for 
evaluating the control performance problems monitored under paragraph 
(a)(5) of this section.
    (3) Based on the results of the evaluation procedures, the QIP 
shall be modified to include procedures for conducting one or more of 
the actions described in paragraphs (h)(3)(i) through (v) of this 
section:
    (i) Improved preventive maintenance practices,
    (ii) Process operation changes,
    (iii) Appropriate improvements in control methods,
    (iv) Other steps appropriate to correct control performance, and
    (v) More frequent or improved monitoring in conjunction with one or 
more steps under paragraphs (h)(3)(i) through (iv) of this section.
    (4) The owner or operator shall act to develop and implement a QIP 
as expeditiously as practicable but in no case shall the period for 
completing implementation of the QIP exceed 180 days from the date on 
which notice of the need to implement the QIP must be provided to the 
permitting authority under paragraph (a)(5) of this section. If the 
owner or operator determines that more than 180 days will be necessary 
to complete the appropriate improvements, the owner or operator shall 
notify the permitting authority and obtain a site-specific resolution 
subject to the approval of the permitting authority. Where appropriate, 
the QIP may rely on procedures and corrective actions specified in an 
existing plan developed to satisfy a separate applicable requirement 
(such as a startup, shutdown, and malfunction plan or an operations and 
maintenance plan).


63.1350   Additional test methods.

    (a) Owners or operators conducting tests to determine the rates of 
emission of hydrogen chloride (HCl) from kilns, in-line kiln/raw mills 
and associated bypass stacks at portland cement manufacturing 
facilities, for use in applicability determinations under Sec. 63.1340 
of this subpart are permitted to use Method 321 or Method 322 of 
appendix A to this part.
    (b) Owners or operators conducting tests to determine the rates of 
emission of HCl from kilns, in-line kiln/raw mills and associated 
bypass stacks at portland cement manufacturing facilities, for use in 
applicability determinations under Sec. 63.1340 of this subpart are 
permitted to use Method 26 of appendix A to part 60 of this chapter, 
provided that the conditions of paragraphs (b)(1) through (b)(3) of 
this section are met:
    (1) Method 321 or Method 322 of appendix A to this part is used to 
validate Method 26 of appendix A to part 60 of this chapter in 
accordance with section 6.1 of Method 301 of appendix A to this part.
    (2) If a dry kiln or in-line kiln/raw mill is tested by Method 26, 
the Method 301 validation is conducted on a dry kiln or in-line kiln/
raw mill.
    (3) If a wet kiln is tested by Method 26, the Method 301 validation 
is conducted on a wet kiln.
    (c) Owners or operators conducting tests to determine the rates of 
emission of HCl from kilns, in-line kiln/raw mills and associated 
bypass stacks at portland cement manufacturing facilities, for use in 
applicability determinations under Sec. 63.1340 of this subpart are 
permitted to use Method 26A of appendix A to part 60 of this chapter, 
provided that the conditions of paragraphs (c)(1) through (c)(3) of 
this section are met:
    (1) Method 321 or Method 322 of appendix A to this part is used to 
validate Method 26A of appendix A to part 60 of this chapter in 
accordance with section 6.1 of Method 301 of appendix A to this part.
    (2) If a dry kiln or in-line kiln/raw mill is tested by Method 26A, 
the Method 301 validation is conducted on a dry kiln or in-line kiln/
raw mill.
    (3) If a wet kiln is tested by Method 26A, the Method 301 
validation is conducted on a wet kiln.
    (d) Owners or operators conducting tests to determine the rates of 
emission of specific organic HAP from raw material dryers, kilns and 
in-line kiln/raw mills at portland cement manufacturing facilities, for 
use in applicability determinations under Sec. 63.1340 of this subpart 
are permitted to use Method 320 of appendix A to this part, or Method 
18 of appendix A to part 60 of this chapter.


Sec. 63.1351  Notification requirements.

    (a) The notification provisions of 40 CFR part 63, subpart A that 
apply and those that do not apply to owners and operators of affected 
sources subject to this subpart are listed in Table 1 of this subpart. 
If any State requires a notice that contains all of the information 
required in a notification listed in this section, the owner or 
operator may send the Administrator a copy of the notice sent to the 
State to satisfy the requirements of this section for that 
notification.
    (b) Each owner or operator subject to the requirements of this 
subpart shall comply with the notification requirements in Sec. 63.9 of 
this part as follows:
    (1) Initial notifications as required by Sec. 63.9(b) through (d) 
of this part. For the purposes of this subpart, a Title V or part 70 
permit application may be used in lieu of the initial notification 
required under Sec. 63.9(b), provided the same information is contained 
in the permit application as required by Sec. 63.9(b), and the State to 
which the permit application has been submitted has an approved 
operating permit program under part 70 of this chapter and has received 
delegation of authority from the EPA. Permit applications shall be 
submitted by the same due dates as those specified for the initial 
notification.
    (2) Notification of performance tests, as required by Secs. 63.7 
and 63.9(e) of this part.
    (3) Notification of opacity and visible emission observations 
required by Sec. 63.1348(b)(1) through (3) in accordance with 
Secs. 63.6(h)(5) and 63.9(f) of this part.
    (4) Notification, as required by Sec. 63.9(g) of this part, of the 
date that the continuous emission monitor performance evaluation 
required by Sec. 63.8(e) of this part is scheduled to begin.
    (5) Notification of compliance status, as required by Sec. 63.9(h) 
of this part.
    (c) Each owner or operator subject to the requirements of this 
subpart that is required to implement a QIP shall submit notifications 
as follows:
    (1) Notification, as required by Sec. 63.1349(a)(5) of this 
subpart, of the requirement to implement a QIP.
    (2) Notification, as required by Sec. 63.1349(h)(4) of this 
subpart, if applicable, that more than 180 days will be required to 
complete the appropriate improvements.


Sec. 63.1352  Reporting requirements.

    (a) The reporting provisions of 40 CFR part 63, subpart A that 
apply and those that do not apply to owners or operators

[[Page 14217]]

of affected sources subject to this subpart are listed in Table 1 of 
this subpart. If any State requires a report that contains all of the 
information required in a report listed in this section, the owner or 
operator may send the Administrator a copy of the report sent to the 
State to satisfy the requirements of this section for that report.
    (b) The owner or operator of an affected source shall comply with 
the reporting requirements specified in Sec. 63.10 of the general 
provisions to part 63, subpart A as follows:
    (1) As required by Sec. 63.10(d)(2) of this part, the owner or 
operator shall report the results of performance tests as part of the 
notification of compliance status.
    (2) As required by Sec. 63.10(d)(3) of this part, the owner or 
operator of an affected source shall report the opacity or visible 
emission results from tests required by Sec. 63.1348(b)(1)-(3) of this 
subpart along with the results of the performance test required under 
Sec. 63.7 of this part.
    (3) As required by Sec. 63.10(d)(4) of this part, the owner or 
operator of an affected source who is required to submit progress 
reports as a condition of receiving an extension of compliance under 
Sec. 63.6(i) of this part shall submit such reports by the dates 
specified in the written extension of compliance.
    (4) As required by Sec. 63.10(d)(5) of this part, if actions taken 
by an owner or operator during a startup, shutdown, or malfunction of 
an affected source (including actions taken to correct a malfunction) 
are consistent with the procedures specified in the source's startup, 
shutdown, and malfunction plan specified in Sec. 63.6(e)(3) of this 
part, the owner or operator shall state such information in a 
semiannual report. Reports shall only be required if a startup, 
shutdown, or malfunction occurred during the reporting period. The 
startup, shutdown, and malfunction report may be submitted 
simultaneously with the excess emissions and continuous monitoring 
system performance reports; and
    (5) Any time an action taken by an owner or operator during a 
startup, shutdown, or malfunction (including actions taken to correct a 
malfunction) is not consistent with the procedures in the startup, 
shutdown, and malfunction plan, the owner or operator shall make an 
immediate report of the actions taken for that event within 2 working 
days, by telephone call or facsimile (FAX) transmission. The immediate 
report shall be followed by a letter, certified by the owner or 
operator or other responsible official, explaining the circumstances of 
the event, the reasons for not following the startup, shutdown, and 
malfunction plan, and whether any excess emissions and/or parameter 
monitoring exceedances are believed to have occurred.
    (6) As required by Sec. 63.10(e)(2) of this part, the owner or 
operator shall submit a written report of the results of the 
performance evaluation for the continuous monitoring system required by 
Sec. 63.8(e) of this part. The owner or operator shall submit the 
report simultaneously with the results of the performance test.
    (7) As required by Sec. 63.10(e)(2) of this part, the owner or 
operator of an affected source using a continuous opacity monitoring 
system to determine opacity compliance during any performance test 
required under Sec. 63.7 of this part and described in Sec. 63.6(d)(6) 
of this part shall report the results of the continuous opacity 
monitoring system performance evaluation conducted under Sec. 63.8(e) 
of this part.
    (8) As required by Sec. 63.10(e)(3) of this part, the owner or 
operator of an affected source equipped with a continuous emission 
monitor shall submit an excess emissions and continuous monitoring 
system performance report for any event when the continuous monitoring 
system data indicate the source is not in compliance with the 
applicable emission limitation or operating parameter limit.
    (9) The owner or operator shall submit a summary report 
semiannually which contains the information specified in 
Sec. 63.10(e)(3)(vi) of this part. In addition, the summary report 
shall include:
    (i) All exceedences of maximum control device inlet gas temperature 
limits determined under Sec. 63.1349(d)(4) of this subpart,
    (ii) All failures to calibrate thermocouples and other temperature 
sensors as required under Sec. 63.1349(d)(5) of this subpart, and
    (iii) All exceedences in carbon injection rate as required under 
Sec. 63.1349(e)(2) of this subpart.
    (10) If the total continuous monitoring system downtime for any CEM 
or any continuous monitoring system (CMS) for the reporting period is 
five percent or greater of the total operating time for the reporting 
period, the owner or operator shall submit an excess emissions and 
continuous monitoring system performance report along with the summary 
report.


Sec. 63.1353  Recordkeeping requirements.

    (a) The owner or operator shall maintain files of all information 
(including all reports and notifications) required by this section 
recorded in a form suitable and readily available for inspection and 
review as required by Sec. 63.10(b)(1). The files shall be retained for 
at least five years following the date of each occurrence, measurement, 
maintenance, corrective action, report, or record. At a minimum, the 
most recent two years of data shall be retained on site. The remaining 
three years of data may be retained off site. The files may be 
maintained on microfilm, on a computer, on floppy disks, on magnetic 
tape, or on microfiche.
    (b) The owner or operator shall maintain records for each affected 
source as required by Sec. 63.10(b)(2) and (b)(3) of this part, and
    (1) All documentation supporting initial notifications and 
notifications of compliance status under Sec. 63.9 of this part.
    (2) All records of applicability determination, including 
supporting analyses, and
    (3) If the owner or operator has been granted a waiver under 
Sec. 63.8(f)(6) of this part, any information demonstrating whether a 
source is meeting the requirements for a waiver of recordkeeping or 
reporting requirements.
    (c) In addition to the recordkeeping requirements in paragraph (b) 
of this section, the owner or operator of an affected source equipped 
with a continuous monitoring system shall maintain all records required 
by Sec. 63.10(c) of this part.
    (d) In addition to the recordkeeping requirements in paragraph (b) 
of this section, the owner or operator of an affected source equipped 
with a bag leak detection system shall maintain records of any bag leak 
detection system alarm, including the date and time of the alarm and 
the date and time that corrective action was initiated, with a brief 
explanation of the cause of the alarm and the corrective action taken.


Sec. 63.1354  Delegation of authority.

    (a) In delegating implementation and enforcement authority to a 
State under subpart E of this part, the authorities contained in 
paragraph (b) of this section shall be retained by the Administrator 
and not transferred to a State.
    (b) Authority which will not be delegated to States: 
Sec. 63.1348(b), approval of alternate test methods for particulate 
matter determination; approval of alternate test methods for opacity; 
approval of alternate test methods for D/F; Sec. 63.1350, approval of 
alternate test methods for Hcl.


Secs. 63.1355-63.1359  [Reserved]

[[Page 14218]]



                          Table 1 To Subpart LLL.--Applicability of General Provisions                          
----------------------------------------------------------------------------------------------------------------
  General provisions citation        Requirement             Applies to subpart LLL               Comment       
----------------------------------------------------------------------------------------------------------------
63.1(a)(1)-(4)................  Applicability........  Yes                                                      
63.1(a)(5)....................  .....................  No................................  [Reserved].          
63.1(a)(6)-(a)(8).............  Applicability........  Yes                                                      
63.1(a)(9)....................  .....................  No................................  [Reserved].          
63.1(a)(10)-(14)..............  Applicability........  Yes                                                      
63.1(b)(1)....................  Initial Applicability  No................................  Sec.  63.1340        
                                 Determination.                                             specifies           
                                                                                            applicability.      
63.1(b)(2)-(3)................  Initial Applicability  Yes                                                      
                                 Determination.                                                                 
63.1(c)(1)....................  Applicability After    Yes                                                      
                                 Standard Established.                                                          
63.1(c)(2)....................  Permit Requirements..  Yes...............................  Area sources must    
                                                                                            obtain Title V      
                                                                                            permits.            
63.1(c)(3)....................  .....................  No................................  [Reserved].          
63.1(c)(4)-(5)................  Extensions,            Yes                                 .....................
                                 Notifications.                                                                 
63.1(d).......................  .....................  No................................  [Reserved].          
63.1(e).......................  Applicability of       Yes                                                      
                                 Permit Program.                                                                
63.2..........................  Definitions..........  Yes...............................  Additional           
                                                                                            definitions in Sec. 
                                                                                            63.1341.            
63.3(a)-(c)...................  Units and              Yes                                 .....................
                                 Abbreviations.                                                                 
63.4(a)(1)-(a)(3).............  Prohibited Activities  Yes                                 .....................
63.4(a)(4)....................  .....................  No................................  [Reserved].          
63.4(a)(5)....................  Compliance date......  Yes                                                      
63.4(b)-(c)...................  Circumvention,         Yes                                                      
                                 Severability.                                                                  
63.5(a)(1)-(2)................  Construction/          Yes                                                      
                                 Reconstruction.                                                                
63.5(b)(1)....................  Compliance Dates.....  Yes                                                      
63.5(b)(2)....................  .....................  No................................  [Reserved].          
63.5(b)(3)-(6)................  Construction           Yes                                                      
                                 Approval,                                                                      
                                 Applicability.                                                                 
63.5(c).......................  .....................  No................................  [Reserved].          
63.5(d)(1)-(4)................  Approval of            Yes                                                      
                                 Construction/                                                                  
                                 Reconstruction.                                                                
63.5(e).......................  Approval of            Yes                                                      
                                 Construction/                                                                  
                                 Reconstruction.                                                                
63.5(f)(1)-(2)................  Approval of            Yes                                 .....................
                                 Construction/                                                                  
                                 Reconstruction.                                                                
63.6(a).......................  Compliance for         Yes                                                      
                                 Standards and                                                                  
                                 Maintenance.                                                                   
63.6(b)(1)-(5)................  Compliance Dates.....  Yes                                                      
63.6(b)(6)....................  .....................  No................................  [Reserved].          
63.6(b)(7)....................  Compliance Dates.....  Yes                                                      
63.6(c)(1)-(2)................  Compliance Dates.....  Yes                                                      
63.6(c)(3)-(c)(4).............  .....................  No................................  [Reserved].          
63.6(c)(5)....................  Compliance Dates.....  Yes                                                      
63.6(d).......................  .....................  No................................  [Reserved].          
63.6(e)(1)-(e)(2).............  Operation &            Yes                                                      
                                 Maintenance.                                                                   
63.6(e)(3)....................  Startup, Shutdown      Yes                                                      
                                 Malfunction Plan.                                                              
63.6(f)(1)-(3)................  Compliance with        Yes                                                      
                                 Emission Standards.                                                            
63.6(g)(1)-(g)(3).............  Alternative Standard.  Yes                                                      
63.6(h)(1)-(2)................  Opacity/VE Standards.  Yes                                                      
63.6(h)(3)....................  .....................  No................................  Reserved             
63.6(h)(4)-(h)(5)(i)..........  Opacity/VE Standards.  Yes                                                      
63.6(h)(5)(ii)-(iv)...........  Opacity/VE Standards.  No................................  Test duration        
                                                                                            specified in Subpart
                                                                                            LLL                 
63.6(h)(6)....................  Opacity/VE Standards.  Yes                                                      
63.6(i)(1)-(i)(14)............  Extension of           Yes                                                      
                                 Compliance.                                                                    
63.6(i)(15)...................  .....................  No................................  [Reserved].          
63.6(i)(16)...................  Extension of           Yes                                                      
                                 Compliance.                                                                    
63.6(j).......................  Exemption from         Yes...............................                       
                                 Compliance                                                                     
63.7(a)(1)-(a)(3).............  Performance Testing    Yes...............................  Sec.  63.1348 has    
                                 Requirements.                                              specific            
                                                                                            requirements.       
63.7(b).......................  Notification.........  Yes                                                      
63.7(c).......................  Quality Assurance/     Yes                                                      
                                 Test Plan.                                                                     
63.7(d).......................  Testing Facilities...  Yes                                                      
63.7(e)(1)-(4)................  Conduct of Tests.....  Yes                                                      
63.7(f).......................  Alternative Test       Yes                                                      
                                 Method.                                                                        
63.7(g).......................  Data Analysis........  Yes                                                      
63.7(h).......................  Waiver of Tests......  Yes                                                      
63.8(a)(1)....................  Monitoring             Yes                                                      
                                 Requirements.                                                                  
63.8(a)(2)....................  Monitoring...........  No................................  Sec.  63.1349        
                                                                                            includes CEM        
                                                                                            requirements.       
63.8(a)(3)....................  .....................  No................................  [Reserved].          
63.8(a)(4)....................  Monitoring...........  No................................  Flares not           
                                                                                            applicable.         
63.8(b)(1)-(3)................  Conduct of Monitoring  Yes                                                      
63.8(c)(1)-(8)................  CMS Operation/         Yes                                                      
                                 Maintenance.                                                                   
63.8(d).......................  Quality Control......  Yes                                                      

[[Page 14219]]

                                                                                                                
63.8(e).......................  Performance            Yes                                                      
                                 Evaluation for CMS.                                                            
63.8(f)(1)-(f)(5).............  Alternative            Yes                                                      
                                 Monitoring Method.                                                             
63.8(f)(6)....................  Alternative to RATA    Yes                                                      
                                 Test.                                                                          
63.8(g).......................  Data Reduction.......  Yes                                                      
63.9(a).......................  Notification           Yes...............................  Additional           
                                 Requirements.                                              notification        
                                                                                            requirements in Sec.
                                                                                             363.1351 (c).      
63.9(b)(1)-(5)................  Initial Notifications  Yes                                                      
63.9(c).......................  Request for            Yes                                                      
                                 Compliance Extension.                                                          
63.9(d).......................  New Source             Yes                                                      
                                 Notification for                                                               
                                 Special Compliance                                                             
                                 Requirements.                                                                  
63.9(e).......................  Notification of        Yes                                                      
                                 Performance Test.                                                              
63.9(f).......................  Notification of VE/    Yes                                 Notification not     
                                 Opacity Test.                                              required for VE/    
                                                                                            opacity test under  
                                                                                            Sec.  63.1349.      
63.9(g).......................  Additional CMS         Yes                                                      
                                 Notifications.                                                                 
63.9(h)(1)-(h)(3).............  Notification of        Yes                                                      
                                 Compliance Status.                                                             
63.9(h)(4)....................  .....................  No................................  [Reserved].          
63.9(h)(5)-(h)(6).............  Notification of        Yes                                                      
                                 Compliance Status.                                                             
63.9(i).......................  Adjustment of          Yes                                                      
                                 Deadlines.                                                                     
63.9(j).......................  Change in Previous     Yes                                                      
                                 Information.                                                                   
63.10(a)......................  Recordkeeping/         Yes                                                      
                                 Reporting.                                                                     
63.10(b)......................  General Requirements.  Yes                                                      
63.10(c)(1)...................  Additional CMS         Yes                                                      
                                 Recordkeeping.                                                                 
63.10(c)(2)-(c)(4)............  .....................  No................................  [Reserved].          
63.10(c)(5)-(c)(8)............  Additional CMS         Yes                                                      
                                 Recordkeeping.                                                                 
63.10(c)(9)...................  .....................  No................................  [Reserved].          
63.10(c)(10)-(15).............   Additional CMS        Yes                                                      
                                 Recordkeeping.                                                                 
63.10(d)(1)...................  General Reporting      Yes                                                      
                                 Requirements.                                                                  
63.10(d)(2)...................  Performance Test       Yes                                                      
                                 Results.                                                                       
63.10(d)(3)...................  Opacity or VE          Yes                                                      
                                 Observations.                                                                  
63.10(d)(4)...................  Progress Reports.....  Yes                                                      
63.10(d)(5)...................  Startup, Shutdown,     Yes                                                      
                                 Malfunction Reports.                                                           
63.10(e)(1)-(e)(2)............  Additional CMS         Yes                                                      
                                 Reports.                                                                       
63.10(e)(3)...................  Excess Emissions and   Yes...............................  Exceedences are      
                                 CMS Performance                                            defined in Sec.     
                                 Reports.                                                   63.1349.            
63.10(f)......................  Waiver for             Yes                                                      
                                 Recordkeeping/                                                                 
                                 Reporting.                                                                     
63.11(a)-(b)..................  Control Device         No................................  Flares not           
                                 Requirements.                                              applicable.         
63.12(a)-(c)..................  State Authority and    Yes                                                      
                                 Delegations.                                                                   
63.13(a)-(c)..................  State/Regional         Yes                                                      
                                 Addresses.                                                                     
63.14(a)-(b)..................  Incorporation by       Yes                                                      
                                 Reference.                                                                     
63.15(a)-(b)..................  Availability of        Yes                                                      
                                 Information.                                                                   
----------------------------------------------------------------------------------------------------------------

    3. Appendix A of part 63 is amended by adding, in numerical order, 
Methods 320, 321, and 322 to read as follows:


Appendix A to Part 63-Test Methods

* * * * *

METHOD 320

Measurement of Vapor Phase Organic and Inorganic Emissions by 
Extractive Fourier Transform Infrared (FTIR) Spectroscopy

1.0  Introduction.

    Persons unfamiliar with basic elements of FTIR spectroscopy 
should not attempt to use this method. This method describes 
sampling and analytical procedures for extractive emission 
measurements using Fourier transform infrared (FTIR) spectroscopy. 
Detailed analytical procedures for interpreting infrared spectra are 
described in the ``Protocol for the Use of Extractive Fourier 
Transform Infrared (FTIR) Spectrometry in Analyses of Gaseous 
Emissions from Stationary Sources,'' hereafter referred to as the 
``Protocol.'' Definitions not given in this method are given in 
appendix A of the Protocol. References to specific sections in the 
Protocol are made throughout this Method. For additional information 
refer to references 1 and 2, and other EPA reports, which describe 
the use of FTIR spectrometry in specific field measurement 
applications and validation tests. The sampling procedure described 
here is extractive. Flue gas is extracted through a heated gas 
transport and handling system. For some sources, sample conditioning 
systems may be applicable. Some examples are given in this method. 
(Note: sample conditioning systems may be used providing the method 
validation requirements in Sections 9.2 and 13.0 of this method are 
met.)
    1.1  Scope and Applicability.
    1.1.1  Analytes. Analytes include hazardous air pollutants 
(HAPs) for which EPA reference spectra have been developed. Other 
compounds can also be measured with this method if reference spectra 
are prepared according to section 4.6 of the protocol.
    1.1.2  Applicability. This method applies to the analysis of 
vapor phase organic or inorganic compounds which absorb energy in 
the mid-infrared spectral region, about 400 to 4000 cm-1 
(25 to 2.5 m). This method is used to determine compound-
specific concentrations in a multi-component vapor phase sample, 
which is contained in a closed-path gas cell. Spectra of samples are 
collected using double beam infrared absorption spectroscopy. A 
computer program is used to analyze spectra and report compound 
concentrations.
    1.2  Method Range and Sensitivity. Analytical range and 
sensitivity depend on the frequency-dependent analyte absorptivity, 
instrument configuration, data collection parameters, and gas stream 
composition. Instrument factors include: (a) spectral resolution, 
(b) interferometer signal averaging time, (c) detector sensitivity 
and response, and (d) absorption path length.
    1.2.1  For any optical configuration the analytical range is 
between the absorbance values of about .01 (infrared transmittance 
relative to the background = 0.98) and 1.0 (T = 0.1). (For 
absorbance > 1.0 the relation between absorbance and concentration 
may not be linear.)
    1.2.2  The concentrations associated with this absorbance range 
depend primarily on the cell path length and the sample temperature. 
An analyte absorbance greater than 1.0, can be lowered by decreasing 
the

[[Page 14220]]

optical path length. Analyte absorbance increases with a longer path 
length. Analyte detection also depends on the presence of other 
species exhibiting absorbance in the same analytical region. 
Additionally, the estimated lower absorbance (A) limit (A = 0.01) 
depends on the root mean square deviation (RMSD) noise in the 
analytical region.
    1.2.3  The concentration range of this method is determined by 
the choice of optical configuration.
    1.2.3.1  The absorbance for a given concentration can be 
decreased by decreasing the path length or by diluting the sample. 
There is no practical upper limit to the measurement range.
    1.2.3.2  The analyte absorbance for a given concentration may be 
increased by increasing the cell path length or (to some extent) 
using a higher resolution. Both modifications also cause a 
corresponding increased absorbance for all compounds in the sample, 
and a decrease in the signal throughput. For this reason the 
practical lower detection range (quantitation limit) usually depends 
on sample characteristics such as moisture content of the gas, the 
presence of other interferants, and losses in the sampling system.
    1.3  Sensitivity. The limit of sensitivity for an optical 
configuration and integration time is determined using appendix D of 
the Protocol: Minimum Analyte Uncertainty, (MAU). The MAU depends on 
the RMSD noise in an analytical region, and on the absorptivity of 
the analyte in the same region.
    1.4  Data Quality. Data quality shall be determined by executing 
Protocol pre-test procedures in appendices B to H of the protocol 
and post-test procedures in appendices I and J of the protocol.
    1.4.1  Measurement objectives shall be established by the choice 
of detection limit (DLi) and analytical uncertainty 
(AUi) for each analyte.
    1.4.2  An instrumental configuration shall be selected. An 
estimate of gas composition shall be made based on previous test 
data, data from a similar source or information gathered in a pre-
test site survey. Spectral interferants shall be identified using 
the selected DLi and AUi and band areas from 
reference spectra and interferant spectra. The baseline noise of the 
system shall be measured in each analytical region to determine the 
MAU of the instrument configuration for each analyte and interferant 
(MIUi).
    1.4.3  Data quality for the application shall be determined, in 
part, by measuring the RMS (root mean square) noise level in each 
analytical spectral region (appendix C of the Protocol). The RMS 
noise is defined as the RMSD of the absorbance values in an 
analytical region from the mean absorbance value in the region.
    1.4.4  The MAU is the minimum analyte concentration for which 
the AUi can be maintained; if the measured analyte 
concentration is less than MAUi, then data quality are 
unacceptable.

2.0  Summary of Method.

    2.1  Principle. References 4 through 7 provide background 
material on infrared spectroscopy and quantitative analysis. A 
summary is given in this section.
    2.1.1  Infrared absorption spectroscopy is performed by 
directing an infrared beam through a sample to a detector. The 
frequency-dependent infrared absorbance of the sample is measured by 
comparing this detector signal (single beam spectrum) to a signal 
obtained without a sample in the beam path (background).
    2.1.2  Most molecules absorb infrared radiation and the 
absorbance occurs in a characteristic and reproducible pattern. The 
infrared spectrum measures fundamental molecular properties and a 
compound can be identified from its infrared spectrum alone.
    2.1.3  Within constraints, there is a linear relationship 
between infrared absorption and compound concentration. If this 
frequency dependent relationship (absorptivity) is known (measured), 
it can be used to determine compound concentration in a sample 
mixture.
    2.1.4  Absorptivity is measured by preparing, in the laboratory, 
standard samples of compounds at known concentrations and measuring 
the FTIR ``reference spectra'' of these standard samples. These 
``reference spectra'' are then used in sample analysis: (1) 
compounds are detected by matching sample absorbance bands with 
bands in reference spectra, and (2) concentrations are measured by 
comparing sample band intensities with reference band intensities.
    2.1.5  This method is self-validating provided that the results 
meet the performance requirement of the QA spike in sections 9.0 and 
8.6.2 of this method, and results from a previous method validation 
study support the use of this method in the application.
    2.2  Sampling and Analysis. In extractive sampling a probe 
assembly and pump are used to extract gas from the exhaust of the 
affected source and transport the sample to the FTIR gas cell. 
Typically, the sampling apparatus is similar to that used for 
single-component continuous emission monitor (CEM) measurements.
    2.2.1  The digitized infrared spectrum of the sample in the FTIR 
gas cell is measured and stored on a computer. Absorbance band 
intensities in the spectrum are related to sample concentrations by 
what is commonly referred to as Beer's Law.

Ai = aibci       (Eq. 320-1)

Where:
Ai = absorbance at a given frequency of the ith sample 
component.
ai = absorption coefficient (absorptivity) of the ith 
sample component.
b = path length of the cell.
ci = concentration of the ith sample component.

    2.2.2  Analyte spiking is used for quality assurance (QA). In 
this procedure (section 8.6.2 of this method) an analyte is spiked 
into the gas stream at the back end of the sample probe. Analyte 
concentrations in the spiked samples are compared to analyte 
concentrations in unspiked samples. Since the concentration of the 
spike is known, this procedure can be used to determine if the 
sampling system is removing the spiked analyte(s) from the sample 
stream.
    2.3  Reference Spectra Availability. Reference spectra of over 
100 HAPs are available in the EPA FTIR spectral library on the EMTIC 
(Emission Measurement Technical Information Center) computer 
bulletin board service and at internet address http://
info.arnold.af.mil/epa/welcome.htm. Reference spectra for HAPs, or 
other analytes, may also be prepared according to section 4.6 of the 
Protocol.
    2.4  Operator Requirements. The FTIR analyst shall be trained in 
setting up the instrumentation, verifying the instrument is 
functioning properly, and performing routine maintenance. The 
analyst must evaluate the initial sample spectra to determine if the 
sample matrix is consistent with pre-test assumptions and if the 
instrument configuration is suitable. The analyst must be able to 
modify the instrument configuration, if necessary.
    2.4.1  The spectral analysis shall be supervised by someone 
familiar with EPA FTIR Protocol procedures.
    2.4.2  A technician trained in CEM test methods is qualified to 
install and operate the sampling system. This includes installing 
the probe and heated line assembly, operating the analyte spike 
system, and performing moisture and flow measurements.

3.0  Definitions.

    See appendix A of the Protocol for definitions relating to 
infrared spectroscopy. Additional definitions are given below.
    3.1  Analyte. A compound that this method is used to measure. 
The term ``target analyte'' is also used. This method is multi-
component and a number of analytes can be targeted for a test.
    3.2  Reference Spectrum. Infrared spectrum of an analyte 
prepared under controlled, documented, and reproducible laboratory 
conditions according to procedures in section 4.6 of the Protocol. A 
library of reference spectra is used to measure analytes in gas 
samples.
    3.3  Standard Spectrum. A spectrum that has been prepared from a 
reference spectrum through a (documented) mathematical operation. A 
common example is de-resolving of reference spectra to lower-
resolution standard spectra (Protocol, appendix K). Standard 
spectra, prepared by approved, and documented, procedures can be 
used as reference spectra for analysis.
    3.4  Concentration. In this method concentration is expressed as 
a molar concentration, in ppm-meters, or in (ppm-meters)/K, where K 
is the absolute temperature (Kelvin). The latter units allow the 
direct comparison of concentrations from systems using different 
optical configurations or sampling temperatures.
    3.5  Interferant. A compound in the sample matrix whose infrared 
spectrum overlaps with part of an analyte spectrum. The most 
accurate analyte measurements are achieved when reference spectra of 
interferants are used in the quantitative analysis with the analyte 
reference spectra.
    The presence of an interferant can increase the analytical 
uncertainty in the measured analyte concentration.
    3.6  Gas Cell. A gas containment cell that can be evacuated. It 
is equipped with the

[[Page 14221]]

optical components to pass the infrared beam through the sample to 
the detector. Important cell features include: path length (or range 
if variable), temperature range, materials of construction, and 
total gas volume.
    3.7  Sampling System. Equipment used to extract the sample from 
the test location and transport the sample gas to the FTIR analyzer. 
This includes sample conditioning systems.
    3.8  Sample Analysis. The process of interpreting the infrared 
spectra to obtain sample analyte concentrations. This process is 
usually automated using a software routine employing a classical 
least squares (cls), partial least squares (pls), or K- or P- matrix 
method.
    3.9  One hundred percent line. A double beam transmittance 
spectrum obtained by combining two background single beam spectra. 
Ideally, this line is equal to 100 percent transmittance (or zero 
absorbance) at every frequency in the spectrum. Practically, a zero 
absorbance line is used to measure the baseline noise in the 
spectrum.
    3.10  Background Deviation. A deviation from 100 percent 
transmittance in any region of the 100 percent line. Deviations 
greater than 5 percent in an analytical region are 
unacceptable (absorbance of 0.021 to -0.022). Such deviations 
indicate a change in the instrument throughput relative to the 
background single beam.
    3.11  Batch Sampling. A procedure where spectra of discreet, 
static samples are collected. The gas cell is filled with sample and 
the cell is isolated. The spectrum is collected. Finally, the cell 
is evacuated to prepare for the next sample.
    3.12  Continuous Sampling. A procedure where spectra are 
collected while sample gas is flowing through the cell at a measured 
rate.
    3.13  Sampling resolution. The spectral resolution used to 
collect sample spectra.
    3.14  Truncation. Limiting the number of interferogram data 
points by deleting points farthest from the center burst (zero path 
difference, ZPD).
    3.15  Zero filling. The addition of points to the interferogram. 
The position of each added point is interpolated from neighboring 
real data points. Zero filling adds no information to the 
interferogram, but affects line shapes in the absorbance spectrum 
(and possibly analytical results).
    3.16  Reference CTS. Calibration Transfer Standard spectra that 
were collected with reference spectra.
    3.17  CTS Standard. CTS spectrum produced by applying a de-
resolution procedure to a reference CTS.
    3.18  Test CTS. CTS spectra collected at the sampling resolution 
using the same optical configuration as for sample spectra. Test 
spectra help verify the resolution, temperature and path length of 
the FTIR system.
    3.19  RMSD. Root Mean Square Difference, defined in EPA FTIR 
Protocol, appendix A.
    3.20  Sensitivity. The noise-limited compound-dependent 
detection limit for the FTIR system configuration. This is estimated 
by the MAU. It depends on the RMSD in an analytical region of a zero 
absorbance line.
    3.21  Quantitation Limit. The lower limit of detection for the 
FTIR system configuration in the sample spectra. This is estimated 
by mathematically subtracting scaled reference spectra of analytes 
and interferences from sample spectra, then measuring the RMSD in an 
analytical region of the subtracted spectrum. Since the noise in 
subtracted sample spectra may be much greater than in a zero 
absorbance spectrum, the quantitation limit is generally much higher 
than the sensitivity. Removing spectral interferences from the 
sample or improving the spectral subtraction can lower the 
quantitation limit toward (but not below) the sensitivity.
    3.22  Independent Sample. A unique volume of sample gas; there 
is no mixing of gas between two consecutive independent samples. In 
continuous sampling two independent samples are separated by at 
least 5 cell volumes. The interval between independent measurements 
depends on the cell volume and the sample flow rate (through the 
cell).
    3.23  Measurement. A single spectrum of flue gas contained in 
the FTIR cell.
    3.24  Run. A run consists of a series of measurements. At a 
minimum a run includes 8 independent measurements spaced over 1 
hour.
    3.25  Validation. Validation of FTIR measurements is described 
in sections 13.0 through 13.4 of this method. Validation is used to 
verify the test procedures for measuring specific analytes at a 
source. Validation provides proof that the method works under 
certain test conditions.
    3.26  Validation Run. A validation run consists of at least 24 
measurements of independent samples. Half of the samples are spiked 
and half are not spiked. The length of the run is determined by the 
interval between independent samples.
    3.27  Screening. Screening is used when there is little or no 
available information about a source. The purpose of screening is to 
determine what analytes are emitted and to obtain information about 
important sample characteristics such as moisture, temperature, and 
interferences. Screening results are semi-quantitative (estimated 
concentrations) or qualitative (identification only). Various 
optical and sampling configurations may be used. Sample conditioning 
systems may be evaluated for their effectiveness in removing 
interferences. It is unnecessary to perform a complete run under any 
set of sampling conditions. Spiking is not necessary, but spiking 
can be a useful screening tool for evaluating the sampling system, 
especially if a reactive or soluble analyte is used for the spike.
    3.28  Emissions Test. An FTIR emissions test is performed 
according specific sampling and analytical procedures. These 
procedures, for the target analytes and the source, are based on 
previous screening and validation results. Emission results are 
quantitative. A QA spike (sections 8.6.2 and 9.2 of this method) is 
performed under each set of sampling conditions using a 
representative analyte. Flow, gas temperature and diluent data are 
recorded concurrently with the FTIR measurements to provide mass 
emission rates for detected compounds.
    3.29  Surrogate. A surrogate is a compound that is used in a QA 
spike procedure (section 8.6.2 of this method) to represent other 
compounds. The chemical and physical properties of a surrogate shall 
be similar to the compounds it is chosen to represent. Under given 
sampling conditions, usually a single sampling factor is of primary 
concern for measuring the target analytes: for example, the 
surrogate spike results can be representative for analytes that are 
more reactive, more soluble, have a lower absorptivity, or have a 
lower vapor pressure than the surrogate itself.

4.0  Interferences.

    Interferences are divided into two classifications: analytical 
and sampling.
    4.1  Analytical Interferences. An analytical interference is a 
spectral feature that complicates (in extreme cases may prevent) the 
analysis of an analyte. Analytical interferences are classified as 
background or spectral interference.
    4.1.1  Background Interference. This results from a change in 
throughput relative to the single beam background. It is corrected 
by collecting a new background and proceeding with the test. In 
severe instances the cause must be identified and corrected. 
Potential causes include: (1) deposits on reflective surfaces or 
transmitting windows, (2) changes in detector sensitivity, (3) a 
change in the infrared source output, or (4) failure in the 
instrument electronics. In routine sampling throughput may degrade 
over several hours. Periodically a new background must be collected, 
but no other corrective action will be required.
    4.1.2  Spectral Interference. This results from the presence of 
interfering compound(s) (interferant) in the sample. Interferant 
spectral features overlap analyte spectral features. Any compound 
with an infrared spectrum, including analytes, can potentially be an 
interferant. The Protocol measures absorbance band overlap in each 
analytical region to determine if potential interferants shall be 
classified as known interferants (FTIR Protocol, section 4.9 and 
appendix B). Water vapor and CO2 are common spectral 
interferants. Both of these compounds have strong infrared spectra 
and are present in many sample matrices at high concentrations 
relative to analytes. The extent of interference depends on the (1) 
interferant concentration, (2) analyte concentration, and (3) the 
degree of band overlap. Choosing an alternate analytical region can 
minimize or avoid the spectral interference. For example, 
CO2 interferes with the analysis of the 670 
cm-1 benzene band. However, benzene can also be measured 
near 3000 cm-1 (with less sensitivity).
    4.2  Sampling System Interferences. These prevent analytes from 
reaching the instrument. The analyte spike procedure is designed to 
measure sampling system interference, if any.
    4.2.1  Temperature. A temperature that is too low causes 
condensation of analytes or water vapor. The materials of the 
sampling system and the FTIR gas cell usually set the upper limit of 
temperature.
    4.2.2  Reactive Species. Anything that reacts with analytes. 
Some analytes, like formaldehyde, polymerize at lower temperatures.

[[Page 14222]]

    4.2.3  Materials. Poor choice of material for probe, or sampling 
line may remove some analytes. For example, HF reacts with glass 
components.
    4.2.4  Moisture. In addition to being a spectral interferant, 
condensed moisture removes soluble compounds.

5.0  Safety.

    The hazards of performing this method are those associated with 
any stack sampling method and the same precautions shall be 
followed. Many HAPs are suspected carcinogens or present other 
serious health risks. Exposure to these compounds should be avoided 
in all circumstances. For instructions on the safe handling of any 
particular compound, refer to its material safety data sheet. When 
using analyte standards, always ensure that gases are properly 
vented and that the gas handling system is leak free. (Always 
perform a leak check with the system under maximum vacuum and, 
again, with the system at greater than ambient pressure.) Refer to 
section 8.2 of this method for leak check procedures. This method 
does not address all of the potential safety risks associated with 
its use. Anyone performing this method must follow safety and health 
practices consistent with applicable legal requirements and with 
prudent practice for each application.

6.0  Equipment and Supplies.

    Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.
    The equipment and supplies are based on the schematic of a 
sampling system shown in Figure 1. Either the batch or continuous 
sampling procedures may be used with this sampling system. 
Alternative sampling configurations may also be used, provided that 
the data quality objectives are met as determined in the post-
analysis evaluation. Other equipment or supplies may be necessary, 
depending on the design of the sampling system or the specific 
target analytes.
    6.1  Sampling Probe. Glass, stainless steel, or other 
appropriate material of sufficient length and physical integrity to 
sustain heating, prevent adsorption of analytes, and to transport 
analytes to the infrared gas cell. Special materials or 
configurations may be required in some applications. For instance, 
high stack sample temperatures may require special steel or cooling 
the probe. For very high moisture sources it may be desirable to use 
a dilution probe.
    6.2  Particulate Filters. A glass wool plug (optional) inserted 
at the probe tip (for large particulate removal) and a filter 
(required) rated for 99 percent removal efficiency at 1-micron 
(e.g., BalstonTM) connected at the outlet of the heated 
probe.
    6.3  Sampling Line/Heating System. Heated (sufficient to prevent 
condensation) stainless steel, polytetrafluoroethane, or other 
material inert to the analytes.
    6.4  Gas Distribution Manifold. A heated manifold allowing the 
operator to control flows of gas standards and samples directly to 
the FTIR system or through sample conditioning systems. Usually 
includes heated flow meter, heated valve for selecting and sending 
sample to the analyzer, and a by-pass vent. This is typically 
constructed of stainless steel tubing and fittings, and high-
temperature valves.
    6.5  Stainless Steel Tubing. Type 316, appropriate diameter 
(e.g., \3/8\ in.) and length for heated connections. Higher grade 
stainless may be desirable in some applications.
    6.6  Calibration/Analyte Spike Assembly. A three way valve 
assembly (or equivalent) to introduce analyte or surrogate spikes 
into the sampling system at the outlet of the probe upstream of the 
out-of-stack particulate filter and the FTIR analytical system.
    6.7  Mass Flow Meter (MFM). These are used for measuring analyte 
spike flow. The MFM shall be calibrated in the range of 0 to 5 L/min 
and be accurate to 2 percent (or better) of the flow 
meter span.
    6.8  Gas Regulators. Appropriate for individual gas standards.
    6.9  Polytetrafluoroethane Tubing. Diameter (e.g., \3/8\ in.) 
and length suitable to connect cylinder regulators to gas standard 
manifold.
    6.10  Sample Pump. A leak-free pump (e.g., KNFTM), 
with by-pass valve, capable of producing a sample flow rate of at 
least 10 L/min through 100 ft of sample line. If the pump is 
positioned upstream of the distribution manifold and FTIR system, 
use a heated pump that is constructed from materials non-reactive to 
the analytes. If the pump is located downstream of the FTIR system, 
the gas cell sample pressure will be lower than ambient pressure and 
it must be recorded at regular intervals.
    6.11  Gas Sample Manifold. Secondary manifold to control sample 
flow at the inlet to the FTIR manifold. This is optional, but 
includes a by-pass vent and heated rotameter.
    6.12  Rotameter. A 0 to 20 L/min rotameter. This meter need not 
be calibrated.
    6.13  FTIR Analytical System. Spectrometer and detector, capable 
of measuring the analytes to the chosen detection limit. The system 
shall include a personal computer with compatible software allowing 
automated collection of spectra.
    6.14  FTIR Cell Pump. Required for the batch sampling technique, 
capable of evacuating the FTIR cell volume within 2 minutes. The 
pumping speed shall allow the operator to obtain 8 sample spectra in 
1 hour.
    6.15  Absolute Pressure Gauge. Capable of measuring pressure 
from 0 to 1000 mmHg to within  2.5 mmHg (e.g., 
BaratronTM).
    6.16  Temperature Gauge. Capable of measuring the cell 
temperature to within  2 deg.C.
    6.17  Sample Conditioning. One option is a condenser system, 
which is used for moisture removal. This can be helpful in the 
measurement of some analytes. Other sample conditioning procedures 
may be devised for the removal of moisture or other interfering 
species.
    6.17.1  The analyte spike procedure of section 9.2 of this 
method, the QA spike procedure of section 8.6.2 of this method, and 
the validation procedure of section 13 of this method demonstrate 
whether the sample conditioning affects analyte concentrations. 
Alternatively, measurements can be made with two parallel FTIR 
systems; one measuring conditioned sample, the other measuring 
unconditioned sample.
    6.17.2  Another option is sample dilution. The dilution factor 
measurement must be documented and accounted for in the reported 
concentrations. An alternative to dilution is to lower the 
sensitivity of the FTIR system by decreasing the cell path length, 
or to use a short-path cell in conjunction with a long path cell to 
measure more than one concentration range.

7.0  Reagents and Standards.

    7.1  Analyte(s) and Tracer Gas. Obtain a certified gas cylinder 
mixture containing all of the analyte(s) at concentrations within 
2 percent of the emission source levels (expressed in 
ppm-meter/K). If practical, the analyte standard cylinder shall also 
contain the tracer gas at a concentration which gives a measurable 
absorbance at a dilution factor of at least 10:1. Two ppm 
SF6 is sufficient for a path length of 22 meters at 250 
deg.F.
    7.2  Calibration Transfer Standard(s). Select the calibration 
transfer standards (CTS) according to section 4.5 of the FTIR 
Protocol. Obtain a National Institute of Standards and Technology 
(NIST) traceable gravimetric standard of the CTS (2 
percent).
    7.3  Reference Spectra. Obtain reference spectra for each 
analyte, interferant, surrogate, CTS, and tracer. If EPA reference 
spectra are not available, use reference spectra prepared according 
to procedures in section 4.6 of the EPA FTIR Protocol.

8.0  Sampling and Analysis Procedure.

    Three types of testing can be performed: (1) screening, (2) 
emissions test, and (3) validation. Each is defined in section 3 of 
this method. Determine the purpose(s) of the FTIR test. Test 
requirements include: (a) AUI, DLI, overall 
fractional uncertainty, OFUI, maximum expected 
concentration (CMAXI), and tAN for each, (b) 
potential interferants, (c) sampling system factors, e.g., minimum 
absolute cell pressure, (PMIN), FTIR cell volume 
(VSS), estimated sample absorption pathlength, 
LS', estimated sample pressure, PS', 
TS', signal integration time (tSS), minimum 
instrumental linewidth, MIL, fractional error, and (d) analytical 
regions, e.g., m = 1 to M, lower wavenumber position, 
FLM, center wavenumber position, FCM, and 
upper wavenumber position, FUM, plus interferants, upper 
wavenumber position of the CTS absorption band, FFUM, 
lower wavenumber position of the CTS absorption band, 
FFLM, wavenumber range FNU to FNL. If necessary, sample 
and acquire an initial spectrum. From analysis of this preliminary 
spectrum determine a suitable operational path length. Set up the 
sampling train as shown in Figure 1 or use an appropriate 
alternative configuration. Sections 8.1 through 8.11 of this method 
provide guidance on pre-test calculations in the EPA protocol, 
sampling and analytical procedures, and post-test protocol 
calculations.
    8.1  Pretest Preparations and Evaluations. Using the procedure 
in section 4.0 of the FTIR Protocol, determine the optimum sampling 
system configuration for measuring the target analytes. Use 
available information to make reasonable assumptions about moisture 
content and other interferences.

[[Page 14223]]

    8.1.1  Analytes. Select the required detection limit 
(DLi) and the maximum permissible analytical uncertainty 
(AUi) for each analyte (labeled from 1 to i). Estimate, 
if possible, the maximum expected concentration for each analyte, 
CMAXi. The expected measurement range is fixed by 
DLi and CMAXi for each analyte (i).
    8.1.2  Potential Interferants. List the potential interferants. 
This usually includes water vapor and CO2, but may also 
include some analytes and other compounds.
    8.1.3  Optical Configuration. Choose an optical configuration 
that can measure all of the analytes within the absorbance range of 
.01 to 1.0 (this may require more than one path length). Use 
Protocol sections 4.3 to 4.8 for guidance in choosing a 
configuration and measuring CTS.
    8.1.4  Fractional Reproducibility Uncertainty (FRUi). 
The FRU is determined for each analyte by comparing CTS spectra 
taken before and after the reference spectra were measured. The EPA 
para-xylene reference spectra were collected on 10/31/91 and 11/01/
91 with corresponding CTS spectra ``cts1031a,'' and ``cts1101b.'' 
The CTS spectra are used to estimate the reproducibility (FRU) in 
the system that was used to collect the references. The FRU must be 
< AU. Appendix E of the protocol is used to calculate the FRU from 
CTS spectra. Figure 2 plots results for 0.25 cm-1 CTS 
spectra in EPA reference library: S3 (cts1101b--
cts1031a), and S4 [(cts1101b + cts1031a)/2]. The RMSD 
(SRMS) is calculated in the subtracted baseline, S3, in 
the corresponding CTS region from 850 to 1065 cm-1. The 
area (BAV) is calculated in the same region of the averaged CTS 
spectrum, S4.
    8.1.5  Known Interferants. Use appendix B of the EPA FTIR 
Protocol.
    8.1.6  Calculate the Minimum Analyte Uncertainty, MAU (section 
1.3 of this method discusses MAU and protocol appendix D gives the 
MAU procedure). The MAU for each analyte, i, and each analytical 
region, m, depends on the RMS noise.
    8.1.7  Analytical Program. See FTIR Protocol, section 4.10. 
Prepare computer program based on the chosen analytical technique. 
Use as input reference spectra of all target analytes and expected 
interferants. Reference spectra of additional compounds shall also 
be included in the program if their presence (even if transient) in 
the samples is considered possible. The program output shall be in 
ppm (or ppb) and shall be corrected for differences between the 
reference path length, LR, temperature, TR, 
and pressure, PR, and the conditions used for collecting 
the sample spectra. If sampling is performed at ambient pressure, 
then any pressure correction is usually small relative to 
corrections for path length and temperature, and may be neglected.
    8.2  Leak-check.
    8.2.1  Sampling System. A typical FTIR extractive sampling train 
is shown in Figure 1. Leak check from the probe tip to pump outlet 
as follows: Connect a 0- to 250-mL/min rate meter (rotameter or 
bubble meter) to the outlet of the pump. Close off the inlet to the 
probe, and record the leak rate. The leak rate shall be  
200 mL/min.
    8.2.2  Analytical System Leak check. Leak check the FTIR cell 
under vacuum and under pressure (greater than ambient). Leak check 
connecting tubing and inlet manifold under pressure.
    8.2.2.1  For the evacuated sample technique, close the valve to 
the FTIR cell, and evacuate the absorption cell to the minimum 
absolute pressure Pmin. Close the valve to the pump, and 
determine the change in pressure Pv after 2 
minutes.
    8.2.2.2  For both the evacuated sample and purging techniques, 
pressurize the system to about 100 mmHg above atmospheric pressure. 
Isolate the pump and determine the change in pressure 
Pp after 2 minutes.
    8.2.2.3  Measure the barometric pressure, Pb in mmHg.
    8.2.2.4  Determine the percent leak volume %VL for 
the signal integration time tSS and for 
Pmax, i.e., the larger of Pv 
or Pp, as follows:
[GRAPHIC] [TIFF OMITTED] TP24MR98.004

Where 50=100% divided by the leak-check time of 2 minutes.

    8.2.2.5  Leak volumes in excess of 4 percent of the FTIR system 
volume VSS are unacceptable.
    8.3  Detector Linearity. Once an optical configuration is 
chosen, use one of the procedures of sections 8.3.1 through 8.3.3 to 
verify that the detector response is linear. If the detector 
response is not linear, decrease the aperture, or attenuate the 
infrared beam. After a change in the instrument configuration 
perform a linearity check until it is demonstrated that the detector 
response is linear.
    8.3.1  Vary the power incident on the detector by modifying the 
aperture setting. Measure the background and CTS at three instrument 
aperture settings: (1) at the aperture setting to be used in the 
testing, (2) at one half this aperture and (3) at twice the proposed 
testing aperture. Compare the three CTS spectra. CTS band areas 
shall agree to within the uncertainty of the cylinder standard and 
the RMSD noise in the system. If test aperture is the maximum 
aperture, collect CTS spectrum at maximum aperture, then close the 
aperture to reduce the IR throughput by half. Collect a second 
background and CTS at the smaller aperture setting and compare the 
spectra again.
    8.3.2  Use neutral density filters to attenuate the infrared 
beam. Set up the FTIR system as it will be used in the test 
measurements. Collect a CTS spectrum. Use a neutral density filter 
to attenuate the infrared beam (either immediately after the source 
or the interferometer) to approximately \1/2\ its original 
intensity. Collect a second CTS spectrum. Use another filter to 
attenuate the infrared beam to approximately \1/4\ its original 
intensity. Collect a third background and CTS spectrum. Compare the 
CTS spectra. CTS band areas shall agree to within the uncertainty of 
the cylinder standard and the RMSD noise in the system.
    8.3.3  Observe the single beam instrument response in a 
frequency region where the detector response is known to be zero. 
Verify that the detector response is ``flat'' and equal to zero in 
these regions.
    8.4  Data Storage Requirements. All field test spectra shall be 
stored on a computer disk and a second backup copy must stored on a 
separate disk. The stored information includes sample 
interferograms, processed absorbance spectra, background 
interferograms, CTS sample interferograms and CTS absorbance 
spectra. Additionally, documentation of all sample conditions, 
instrument settings, and test records must be recorded on hard copy 
or on computer medium. Table 1 to this method gives a sample 
presentation of documentation.
    8.5  Background Spectrum. Evacuate the gas cell to  5 
mmHg, and fill with dry nitrogen gas to ambient pressure (or purge 
the cell with 10 volumes of dry nitrogen). Verify that no 
significant amounts of absorbing species (for example water vapor 
and CO2) are present. Collect a background spectrum, 
using a signal averaging period equal to or greater than the 
averaging period for the sample spectra. Assign a unique file name 
to the background spectrum. Store two copies of the background 
interferogram and processed single-beam spectrum on separate 
computer disks (one copy is the back-up).
    8.5.1  Interference Spectra. If possible, collect spectra of 
known and suspected major interferences using the same optical 
system that will be used in the field measurements. This can be done 
on-site or earlier. A number of gases, e.g. CO2, 
SO2, CO, NH3, are readily available from 
cylinder gas suppliers.
    8.5.2  Water vapor spectra can be prepared by the following 
procedure. Fill a sample tube with distilled water. Evacuate above 
the sample and remove dissolved gasses by alternately freezing and 
thawing the water while evacuating. Allow water vapor into the FTIR 
cell, then dilute to atmospheric pressure with nitrogen or dry air. 
If quantitative water spectra are required, follow the reference 
spectrum procedure for neat samples (protocol, section 4.6). Often, 
interference spectra need not be quantitative, but for best results 
the absorbance must be comparable to the interference absorbance in 
the sample spectra.
    8.6  Pre-Test Calibrations
    8.6.1  Calibration Transfer Standard. Evacuate the gas cell to 
 5 mmHg absolute pressure, and fill the FTIR cell to 
atmospheric pressure with the CTS gas. Alternatively, purge the cell 
with 10 cell volumes of CTS gas. (If purge is used, verify that the 
CTS concentration in the cell is stable by collecting two spectra 2 
minutes apart as the CTS gas continues to flow. If the absorbance in 
the second spectrum is no greater than in the first, within the 
uncertainty of the gas standard, then this can be used as the CTS 
spectrum.) Record the spectrum.
    8.6.2  QA Spike. This procedure assumes that the method has been 
validated for at least some of the target analytes at the source. 
For emissions testing perform a QA spike. Use a certified standard, 
if possible, of an analyte, which has been validated at the source. 
One analyte standard can serve as a QA surrogate for other analytes 
which are less reactive or less soluble than the

[[Page 14224]]

standard. Perform the spike procedure of section 9.2 of this method. 
Record spectra of at least three independent (section 3.22 of this 
method) spiked samples. Calculate the spiked component of the 
analyte concentration. If the average spiked concentration is within 
0.7 to 1.3 times the expected concentration, then proceed with the 
testing. If applicable, apply the correction factor from the Method 
301 of this appendix validation test (not the result from the QA 
spike).
    8.7  Sampling. If analyte concentrations vary rapidly with time, 
CEM sampling is preferable using the smallest cell volume, fastest 
sampling rate and fastest spectra collection rate possible. CEM 
sampling requires the least operator intervention even without an 
automated sampling system. For continuous monitoring at one location 
over long periods, CEM sampling is preferred. Batch sampling and 
continuous static sampling are used for screening and performing 
test runs of finite duration. Either technique is preferred for 
sampling several locations in a matter of days. Batch sampling gives 
reasonably good time resolution and ensures that each spectrum 
measures a discreet (and unique) sample volume. Continuous static 
(and CEM) sampling provide a very stable background over long 
periods. Like batch sampling, continuous static sampling also 
ensures that each spectrum measures a unique sample volume. It is 
essential that the leak check procedure under vacuum (section 8.2 of 
this method) is passed if the batch sampling procedure is used. It 
is essential that the leak check procedure under positive pressure 
is passed if the continuous static or CEM sampling procedures are 
used. The sampling techniques are described in sections 8.7.1 
through 8.7.2 of this method.
    8.7.1  Batch Sampling. Evacuate the absorbance cell to 
 5 mmHg absolute pressure. Fill the cell with exhaust gas 
to ambient pressure, isolate the cell, and record the spectrum. 
Before taking the next sample, evacuate the cell until no spectral 
evidence of sample absorption remains. Repeat this procedure to 
collect eight spectra of separate samples in 1 hour.
    8.7.2  Continuous Static Sampling. Purge the FTIR cell with 10 
cell volumes of sample gas. Isolate the cell, collect the spectrum 
of the static sample and record the pressure. Before measuring the 
next sample, purge the cell with 10 more cell volumes of sample gas.
    8.8  Sampling QA and Reporting.
    8.8.1  Sample integration times shall be sufficient to achieve 
the required signal-to-noise ratio. Obtain an absorbance spectrum by 
filling the cell with N2. Measure the RMSD in each 
analytical region in this absorbance spectrum. Verify that the 
number of scans used is sufficient to achieve the target MAU.
    8.8.2  Assign a unique file name to each spectrum.
    8.8.3  Store two copies of sample interferograms and processed 
spectra on separate computer disks.
    8.8.4  For each sample spectrum, document the sampling 
conditions, the sampling time (while the cell was being filled), the 
time the spectrum was recorded, the instrumental conditions (path 
length, temperature, pressure, resolution, signal integration time), 
and the spectral file name. Keep a hard copy of these data sheets.
    8.9  Signal Transmittance. While sampling, monitor the signal 
transmittance. If signal transmittance (relative to the background) 
changes by 5 percent or more (absorbance = -.02 to .02) in any 
analytical spectral region, obtain a new background spectrum.
    8.10  Post-test CTS. After the sampling run, record another CTS 
spectrum.
    8.11  Post-test QA.
    8.11.1  Inspect the sample spectra immediately after the run to 
verify that the gas matrix composition was close to the expected 
(assumed) gas matrix.
    8.11.2  Verify that the sampling and instrumental parameters 
were appropriate for the conditions encountered. For example, if the 
moisture is much greater than anticipated, it may be necessary to 
use a shorter path length or dilute the sample.
    8.11.3  Compare the pre- and post-test CTS spectra. The peak 
absorbance in pre- and post-test CTS must be # 5 percent 
of the mean value. See appendix E of the FTIR Protocol.

9.0  Quality Control.

    Use analyte spiking (sections 8.6.2, 9.2 and 13.0 of this 
method) to verify that the sampling system can transport the 
analytes from the probe to the FTIR system.
    9.1  Spike Materials. Use a certified standard (accurate to 
 2 percent) of the target analyte, if one can be 
obtained. If a certified standard cannot be obtained, follow the 
procedures in section 4.6.2.2 of the FTIR Protocol.
    9.2  Spiking Procedure. QA spiking (section 8.6.2 of this 
method) is a calibration procedure used before testing. QA spiking 
involves following the spike procedure of sections 9.2.1 through 
9.2.3 of this method to obtain at least three spiked samples. The 
analyte concentrations in the spiked samples shall be compared to 
the expected spike concentration to verify that the sampling system 
is working properly. Usually, when QA spiking is used, the method 
has already been validated at a similar source for the analyte in 
question. The QA spike demonstrates that the validated sampling 
conditions are being duplicated. If the QA spike fails then the 
sampling system shall be repaired before testing proceeds. The 
method validation procedure (section 13.0 of this method) involves a 
more extensive use of the analyte spike procedure of sections 9.2.1 
through 9.2.3 of this method. Spectra of at least 12 independent 
spiked and 12 independent unspiked samples are recorded. The 
concentration results are analyzed statistically to determine if 
there is a systematic bias in the method for measuring a particular 
analyte. If there is a systematic bias, within the limits allowed by 
Method 301 of this appendix, then a correction factor shall be 
applied to the analytical results. If the systematic bias is greater 
than the allowed limits, this method is not valid and cannot be 
used.
    9.2.1  Introduce the spike/tracer gas at a constant flow rate of 
 10 percent of the total sample flow. (Note: Use the 
rotameter at the end of the sampling train to estimate the required 
spike/tracer gas flow rate.) Use a flow device, e.g., mass flow 
meter ( 2 percent), to monitor the spike flow rate. 
Record the spike flow rate every 10 minutes.
    9.2.2  Determine the response time (RT) of the system by 
continuously collecting spectra of the spiked effluent until the 
spectrum of the spiked component is constant for 5 minutes. The RT 
is the interval from the first measurement until the spike becomes 
constant. Wait for twice the duration of the RT, then collect 
spectra of two independent spiked gas samples. Duplicate analyses of 
the spiked concentration shall be within 5 percent of the mean of 
the two measurements.
    9.2.3  Calculate the dilution ratio using the tracer gas as 
follows:
[GRAPHIC] [TIFF OMITTED] TP24MR98.005

Where:
[GRAPHIC] [TIFF OMITTED] TP24MR98.006

DF = Dilution factor of the spike gas; this value shall be 
10.
SF6(dir) = SF6 (or tracer gas) concentration 
measured directly in undiluted spike gas.
SF6(spk) = Diluted SF6 (or tracer gas) 
concentration measured in a spiked sample.
Spikedir = Concentration of the analyte in the spike 
standard measured by filling the FTIR cell directly.
CS = Expected concentration of the spiked samples.

10.0  Calibration and Standardization.

    10.1  Signal-to-Noise Ratio (S/N). The RMSD in the noise must be 
less than one tenth of the minimum analyte peak absorbance in each 
analytical region. For example if the minimum peak absorbance is 
0.01 at the required DL, then RMSD measured over the entire 
analytical region must be  0.001.
    10.2  Absorbance Path length. Verify the absorbance path length 
by comparing reference CTS spectra to test CTS spectra. See appendix 
E of the FTIR Protocol.
    10.3  Instrument Resolution. Measure the line width of 
appropriate test CTS band(s) to verify instrument resolution. 
Alternatively, compare CTS spectra to a reference CTS spectrum, if 
available, measured at the nominal resolution.
    10.4  Apodization Function. In transforming the sample 
interferograms to absorbance spectra use the same apodization 
function that was used in transforming the reference spectra.
    10.5  FTIR Cell Volume. Evacuate the cell to  5 mmHg. 
Measure the initial absolute temperature (Ti) and 
absolute pressure (Pi). Connect a wet test meter (or a 
calibrated dry gas meter), and slowly draw room air into the cell. 
Measure the meter volume (Vm), meter absolute temperature 
(Tm), and meter absolute pressure (Pm); and 
the cell final absolute temperature (Tf) and absolute

[[Page 14225]]

pressure (Pf). Calculate the FTIR cell volume 
VSS, including that of the connecting tubing, as follows:
[GRAPHIC] [TIFF OMITTED] TP24MR98.007

11.0  Data Analysis and Calculations.

    Analyte concentrations shall be measured using reference spectra 
from the EPA FTIR spectral library. When EPA library spectra are not 
available, the procedures in section 4.6 of the Protocol shall be 
followed to prepare reference spectra of all the target analytes. 
11.1 Spectral De-resolution. Reference spectra can be converted to 
lower resolution standard spectra (section 3.3 of this method) by 
truncating the original reference sample and background 
interferograms. Appendix K of the FTIR Protocol gives specific 
deresolution procedures. Deresolved spectra shall be transformed 
using the same apodization function and level of zero filling as the 
sample spectra. Additionally, pre-test FTIR protocol calculations 
(e.g., FRU, MAU, FCU) shall be performed using the de-resolved 
standard spectra.
    11.2  Data Analysis. Various analytical programs are available 
for relating sample absorbance to a concentration standard. 
Calculated concentrations shall be verified by analyzing residual 
baselines after mathematically subtracting scaled reference spectra 
from the sample spectra. A full description of the data analysis and 
calculations is contained in the FTIR Protocol (sections 4.0, 5.0, 
6.0 and appendices). Correct the calculated concentrations in the 
sample spectra for differences in absorption path length and 
temperature between the reference and sample spectra using equation 
6,
[GRAPHIC] [TIFF OMITTED] TP24MR98.008

Where:

Ccorr = Concentration, corrected for path length.
    Ccalc = Concentration, initial calculation (output of 
the analytical program designed for the compound).
Lr = Reference spectra path length.
Ls = Sample spectra path length.
Ts = Absolute temperature of the sample gas, K.
Tr = Absolute gas temperature of reference spectra, K.

12.0  Method Performance.

    12.1  Spectral Quality. Refer to the FTIR Protocol appendices 
for analytical requirements, evaluation of data quality, and 
analysis of uncertainty.
    12.2  Sampling QA/QC. The analyte spike procedure of section 9 
of this method, the QA spike of section 8.6.2 of this method, and 
the validation procedure of section 13 of this method are used to 
evaluate the performance of the sampling system and to quantify 
sampling system effects, if any, on the measured concentrations. 
This method is self-validating provided that the results meet the 
performance requirement of the QA spike in sections 9.0 and 8.6.2 of 
this method and results from a previous method validation study 
support the use of this method in the application. Several factors 
can contribute to uncertainty in the measurement of spiked samples. 
Factors which can be controlled to provide better accuracy in the 
spiking procedure are listed in sections 12.2.1 through 12.2.4 of 
this method.
    12.2.1  Flow meter. An accurate mass flow meter is accurate to 
 1 percent of its span. If a flow of 1 L/min is 
monitored with such a MFM, which is calibrated in the range of 0-5 
L/min, the flow measurement has an uncertainty of 5 percent. This 
may be improved by re-calibrating the meter at the specific flow 
rate to be used.
    12.2.2  Calibration gas. Usually the calibration standard is 
certified to within  2 percent. With reactive analytes, 
such as HCl, the certified accuracy in a commercially available 
standard may be no better than  5 percent.
    12.2.3  Temperature. Temperature measurements of the cell shall 
be quite accurate. If practical, it is preferable to measure sample 
temperature directly, by inserting a thermocouple into the cell 
chamber instead of monitoring the cell outer wall temperature.
    12.2.4  Pressure. Accuracy depends on the accuracy of the 
barometer, but fluctuations in pressure throughout a day may be as 
much as 2.5 percent due to weather variations.

13.0  Method Validation Procedure.

    This validation procedure, which is based on EPA Method 301 (40 
CFR part 63, appendix A), may be used to validate this method for 
the analytes in a gas matrix. Validation at one source may also 
apply to another type of source, if it can be shown that the exhaust 
gas characteristics are similar at both sources.
    13.1  Section 5.3 of Method 301 (40 CFR part 63, appendix A), 
the Analyte Spike procedure, is used with these modifications. The 
statistical analysis of the results follows section 6.3 of EPA 
Method 301. Section 3 of this method defines terms that are not 
defined in Method 301.
    13.1.1  The analyte spike is performed dynamically. This means 
the spike flow is continuous and constant as spiked samples are 
measured.
    13.1.2  The spike gas is introduced at the back of the sample 
probe.
    13.1.3  Spiked effluent is carried through all sampling 
components downstream of the probe.
    13.1.4  A single FTIR system (or more) may be used to collect 
and analyze spectra (not quadruplicate integrated sampling trains).
    13.1.5  All of the validation measurements are performed 
sequentially in a single ``run'' (section 3.26 of this method).
    13.1.6  The measurements analyzed statistically are each 
independent (section 3.22 of this method).
    13.1.7  A validation data set can consist of more than 12 spiked 
and 12 unspiked measurements.
    13.2  Batch Sampling. The procedure in sections 13.2.1 through 
13.2.2 may be used for stable processes. If process emissions are 
highly variable, the procedure in section 13.2.3 shall be used.
    13.2.1  With a single FTIR instrument and sampling system, begin 
by collecting spectra of two unspiked samples. Introduce the spike 
flow into the sampling system and allow 10 cell volumes to purge the 
sampling system and FTIR cell. Collect spectra of two spiked 
samples. Turn off the spike and allow 10 cell volumes of unspiked 
sample to purge the FTIR cell. Repeat this procedure until the 24 
(or more) samples are collected.
    13.2.2  In batch sampling, collect spectra of 24 distinct 
samples. (Each distinct sample consists of filling the cell to 
ambient pressure after the cell has been evacuated.)
    13.2.3  Alternatively, a separate probe assembly, line, and 
sample pump can be used for spiked sample. Verify and document that 
sampling conditions are the same in both the spiked and the unspiked 
sampling systems. This can be done by wrapping both sample lines in 
the same heated bundle. Keep the same flow rate in both sample 
lines. Measure samples in sequence in pairs. After two spiked 
samples are measured, evacuate the FTIR cell, and turn the manifold 
valve so that spiked sample flows to the FTIR cell. Allow the 
connecting line from the manifold to the FTIR cell to purge 
thoroughly (the time depends on the line length and flow rate). 
Collect a pair of spiked samples. Repeat the procedure until at 
least 24 measurements are completed.
    13.3  Simultaneous Measurements With Two FTIR Systems. If 
unspiked effluent concentrations of the target analyte(s) vary 
significantly with time, it may be desirable to perform synchronized 
measurements of spiked and unspiked sample. Use two FTIR systems, 
each with its own cell and sampling system to perform simultaneous 
spiked and unspiked measurements. The optical configurations shall 
be similar, if possible. The sampling configurations shall be the 
same. One sampling system and FTIR analyzer shall be used to measure 
spiked effluent. The other sampling system and FTIR analyzer shall 
be used to measure unspiked flue gas. Both systems shall use the 
same sampling procedure (i.e., batch or continuous).
    13.3.1  If batch sampling is used, synchronize the cell 
evacuation, cell filling, and collection of spectra. Fill both cells 
at the same rate (in cell volumes per unit time).
    13.3.2  If continuous sampling is used, adjust the sample flow 
through each gas cell so that the same number of cell volumes pass 
through each cell in a given time (i.e. TC1 = 
TC2).
    13.4  Statistical Treatment. The statistical procedure of EPA 
Method 301 of this appendix, section 6.3 is used to evaluate the 
bias and precision. For FTIR testing a validation ``run'' is defined 
as spectra of 24 independent samples, 12 of which are spiked with 
the analyte(s) and 12 of which are not spiked.
    13.4.1  Bias. Determine the bias (defined by EPA Method 301 of 
this appendix, section 6.3.2) using equation 7:

B = Sm - Mm - CS  (Eq. 320-7)

Where:

B = Bias at spike level.

[[Page 14226]]

Sm = Mean concentration of the analyte spiked samples.
Mm = Mean concentration of the unspiked samples.
CS = Expected concentration of the spiked samples.

    13.4.2  Correction Factor. Use section 6.3.2.2 of Method 301 of 
this appendix to evaluate the statistical significance of the bias. 
If it is determined that the bias is significant, then use section 
6.3.3 of Method 301 to calculate a correction factor (CF). 
Analytical results of the test method are multiplied by the 
correction factor, if 0.7  CF  1.3. If it is 
determined that the bias is significant and CF >  30 
percent, then the test method is considered to be ``not valid.''
    13.4.3  If measurements do not pass validation, evaluate the 
sampling system, instrument configuration, and analytical system to 
determine if improper set-up or a malfunction was the cause. If so, 
repair the system and repeat the validation.

14.0  Pollution Prevention.

    The extracted sample gas is vented outside the enclosure 
containing the FTIR system and gas manifold after the analysis. In 
typical method applications the vented sample volume is a small 
fraction of the source volumetric flow and its composition is 
identical to that emitted from the source. When analyte spiking is 
used, spiked pollutants are vented with the extracted sample gas. 
Approximately 1.6  x  10-4 to 3.2  x  10-4 lbs 
of a single HAP may be vented to the atmosphere in a typical 
validation run of 3 hours. (This assumes a molar mass of 50 to 100 
g, spike rate of 1.0 L/min, and a standard concentration of 100 
ppm). Minimize emissions by keeping the spike flow off when not in 
use.
    15.0  Waste Management.
    Small volumes of laboratory gas standards can be vented through 
a laboratory hood. Neat samples must be packed and disposed 
according to applicable regulations. Surplus materials may be 
returned to supplier for disposal.
    16.0  References.
    1. ``Field Validation Test Using Fourier Transform Infrared 
(FTIR) Spectrometry To Measure Formaldehyde, Phenol and Methanol at 
a Wool Fiberglass Production Facility.'' Draft. U.S. Environmental 
Protection Agency Report, EPA Contract No. 68D20163, Work Assignment 
I-32, September 1994.
    2. ``FTIR Method Validation at a Coal-Fired Boiler''. Prepared 
for U.S. Environmental Protection Agency, Research Triangle Park, 
NC. Publication No.: EPA-454/R95-004, NTIS No.: PB95-193199. July, 
1993.
    3. ``Method 301--Field Validation of Pollutant Measurement 
Methods from Various Waste Media,'' 40 CFR part 63, appendix A.
    4. ``Molecular Vibrations; The Theory of Infrared and Raman 
Vibrational Spectra,'' E. Bright Wilson, J.C. Decius, and P.C. 
Cross, Dover Publications, Inc., 1980. For a less intensive 
treatment of molecular rotational-vibrational spectra see, for 
example, ``Physical Chemistry,'' G.M. Barrow, chapters 12, 13, and 
14, McGraw Hill, Inc., 1979.
    5. ``Fourier Transform Infrared Spectrometry,'' Peter R. 
Griffiths and James de Haseth, Chemical Analysis, 83, 16-25, (1986), 
P.J. Elving, J.D. Winefordner and I.M. Kolthoff (ed.), John Wiley 
and Sons.
    6. ``Computer-Assisted Quantitative Infrared Spectroscopy,'' 
Gregory L. McClure (ed.), ASTM Special Publication 934 (ASTM), 1987.
    7. ``Multivariate Least-Squares Methods Applied to the 
Quantitative Spectral Analysis of Multicomponent Mixtures,'' Applied 
Spectroscopy, 39(10), 73-84, 1985.

                            Table 1.--Example Presentation of Sampling Documentation                            
----------------------------------------------------------------------------------------------------------------
                                                        Background file         Sample                          
           Sample time            Spectrum file name         name            conditioning      Process condition
----------------------------------------------------------------------------------------------------------------
                                                                                                                
                                                                                                                
                                                                                                                
                                                                                                                
                                                                                                                
                                                                                                                
----------------------------------------------------------------------------------------------------------------


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         Sample time             Spectrum file     Interferogram      Resolution           Scans         Apodization          Gain         CTS spectrum 
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
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BILLING CODE 6560-50-P

[[Page 14227]]

[GRAPHIC] [TIFF OMITTED] TP24MR98.000



[[Page 14228]]

[GRAPHIC] [TIFF OMITTED] TP24MR98.001



BILLING CODE 6560-50-C

[[Page 14229]]

Addendum to Method 320--Protocol for the Use of Extractive Fourier 
Transform Infrared (FTIR) Spectrometry for the Analyses of Gaseous 
Emissions From Stationary Sources

1.0  Introduction

    The purpose of this addendum is to set general guidelines for 
the use of modern FTIR spectroscopic methods for the analysis of gas 
samples extracted from the effluent of stationary emission sources. 
This addendum outlines techniques for developing and evaluating such 
methods and sets basic requirements for reporting and quality 
assurance procedures.

1.1  Nomenclature

    1.1.1  Attachment A to this addendum lists definitions of the 
symbols and terms used in this Protocol, many of which have been 
taken directly from American Society for Testing and Materials 
(ASTM) publication E 131-90a, entitled ``Terminology Relating to 
Molecular Spectroscopy.''
    1.1.2  Except in the case of background spectra or where 
otherwise noted, the term ``spectrum'' refers to a double-beam 
spectrum in units of absorbance vs. wavenumber (cm-1).
    1.1.3  The term ``Study'' in this addendum refers to a 
publication that has been subjected to EPA- or peer-review.

2.0  Applicability and Analytical Principle

    2.1  Applicability. This Protocol applies to the determination 
of compound-specific concentrations in single- and multiple-
component gas phase samples using double-beam absorption 
spectroscopy in the mid-infrared band. It does not specifically 
address other FTIR applications, such as single-beam spectroscopy, 
analysis of open-path (non-enclosed) samples, and continuous 
measurement techniques. If multiple spectrometers, absorption cells, 
or instrumental linewidths are used in such analyses, each distinct 
operational configuration of the system must be evaluated separately 
according to this Protocol.
    2.2  Analytical Principle.
    2.2.1  In the mid-infrared band, most molecules exhibit 
characteristic gas phase absorption spectra that may be recorded by 
FTIR systems. Such systems consist of a source of mid-infrared 
radiation, an interferometer, an enclosed sample cell of known 
absorption pathlength, an infrared detector, optical elements for 
the transfer of infrared radiation between components, and gas flow 
control and measurement components. Adjunct and integral computer 
systems are used for controlling the instrument, processing the 
signal, and for performing both Fourier transforms and quantitative 
analyses of spectral data.
    2.2.2  The absorption spectra of pure gases and of mixtures of 
gases are described by a linear absorbance theory referred to as 
Beer's Law. Using this law, modern FTIR systems use computerized 
analytical programs to quantify compounds by comparing the 
absorption spectra of known (reference) gas samples to the 
absorption spectrum of the sample gas. Some standard mathematical 
techniques used for comparisons are classical least squares, inverse 
least squares, cross-correlation, factor analysis, and partial least 
squares. Reference A describes several of these techniques, as well 
as additional techniques, such as differentiation methods, linear 
baseline corrections, and non-linear absorbance corrections.

3.0  General Principles of Protocol Requirements

    The characteristics that distinguish FTIR systems from gas 
analyzers used in instrumental gas analysis methods (e.g., Methods 
6C and 7E of appendix A to part 60 of this chapter) are: (1) 
Computers are necessary to obtain and analyze data; (2) chemical 
concentrations can be quantified using previously recorded infrared 
reference spectra; and (3) analytical assumptions and results, 
including possible effects of interfering compounds, can be 
evaluated after the quantitative analysis. The following general 
principles and requirements of this Protocol are based on these 
characteristics.
    3.1  Verifiability and Reproducibility of Results. Store all 
data and document data analysis techniques sufficient to allow an 
independent agent to reproduce the analytical results from the raw 
interferometric data.
    3.2  Transfer of Reference Spectra. To determine whether 
reference spectra recorded under one set of conditions (e.g., 
optical bench, instrumental linewidth, absorption pathlength, 
detector performance, pressure, and temperature) can be used to 
analyze sample spectra taken under a different set of conditions, 
quantitatively compare ``calibration transfer standards'' (CTS) and 
reference spectra as described in this Protocol. (Note: The CTS may, 
but need not, include analytes of interest). To effect this, record 
the absorption spectra of the CTS (a) immediately before and 
immediately after recording reference spectra and (b) immediately 
after recording sample spectra.
    3.3  Evaluation of FTIR Analyses. The applicability, accuracy, 
and precision of FTIR measurements are influenced by a number of 
interrelated factors, which may be divided into two classes:
    3.3.1  Sample-Independent Factors. Examples are system 
configuration and performance (e.g., detector sensitivity and 
infrared source output), quality and applicability of reference 
absorption spectra, and type of mathematical analyses of the 
spectra. These factors define the fundamental limitations of FTIR 
measurements for a given system configuration. These limitations may 
be estimated from evaluations of the system before samples are 
available.
    For example, the detection limit for the absorbing compound 
under a given set of conditions may be estimated from the system 
noise level and the strength of a particular absorption band. 
Similarly, the accuracy of measurements may be estimated from the 
analysis of the reference spectra.
    3.3.2  Sample-Dependent Factors. Examples are spectral 
interferants (e.g., water vapor and CO2) or the overlap 
of spectral features of different compounds and contamination 
deposits on reflective surfaces or transmitting windows. To maximize 
the effectiveness of the mathematical techniques used in spectral 
analysis, identification of interferants (a standard initial step) 
and analysis of samples (includes effect of other analytical errors) 
are necessary. Thus, the Protocol requires post-analysis calculation 
of measurement concentration uncertainties for the detection of 
these potential sources of measurement error.

4.0  Pre-Test Preparations and Evaluations

    Before testing, demonstrate the suitability of FTIR spectrometry 
for the desired application according to the procedures of this 
section.
    4.1  Identify Test Requirements. Identify and record the test 
requirements described in sections 4.1.1 through 4.1.4 of this 
addendum. These values set the desired or required goals of the 
proposed analysis; the description of methods for determining 
whether these goals are actually met during the analysis comprises 
the majority of this Protocol.
    4.1.1  Analytes (specific chemical species) of interest. Label 
the analytes from i = 1 to I.
    4.1.2  Analytical uncertainty limit (AUi). The 
AUi is the maximum permissible fractional uncertainty of 
analysis for the ith analyte concentration, expressed as 
a fraction of the analyte concentration in the sample.
    4.1.3  Required detection limit for each analyte 
(DLi, ppm). The detection limit is the lowest 
concentration of an analyte for which its overall fractional 
uncertainty (OFUi) is required to be less than its 
analytical uncertainty limit (AUi).
    4.1.4  Maximum expected concentration of each analyte 
(CMAXi, ppm).
    4.2  Identify Potential Interferants. Considering the chemistry 
of the process or results of previous studies, identify potential 
interferants, i.e., the major effluent constituents and any 
relatively minor effluent constituents that possess either strong 
absorption characteristics or strong structural similarities to any 
analyte of interest. Label them 1 through Nj, where the 
subscript ``j'' pertains to potential interferants. Estimate the 
concentrations of these compounds in the effluent (CPOTj, 
ppm).
    4.3  Select and Evaluate the Sampling System. Considering the 
source, e.g., temperature and pressure profiles, moisture content, 
analyte characteristics, and particulate concentration, select the 
equipment for extracting gas samples. Recommended are a particulate 
filter, heating system to maintain sample temperature above the dew 
point for all sample constituents at all points within the sampling 
system (including the filter), and sample conditioning system (e.g., 
coolers, water-permeable membranes that remove water or other 
compounds from the sample, and dilution devices) to remove spectral 
interferants or to protect the sampling and analytical components. 
Determine the minimum absolute sample system pressure 
(Pmin, mmHg) and the infrared absorption cell volume 
(VSS, liter). Select the techniques and/or equipment for 
the measurement of sample pressures and temperatures.
    4.4  Select Spectroscopic System. Select a spectroscopic 
configuration for the

[[Page 14230]]

application. Approximate the absorption pathlength (LS', 
meter), sample pressure (PS', kPa), absolute sample 
temperature TS', and signal integration period 
(tSS, seconds) for the analysis. Specify the nominal 
minimum instrumental linewidth (MIL) of the system. Verify that the 
fractional error at the approximate values PS' and 
TS' is less than one half the smallest value 
AUi (see section 4.1.2 of this addendum).
    4.5  Select Calibration Transfer Standards (CTS's). Select CTS's 
that meet the criteria listed in sections 4.5.1, 4.5.2, and 4.5.3 of 
this addendum. (Note: It may be necessary to choose preliminary 
analytical regions (see section 4.7 of this addendum), identify the 
minimum analyte linewidths, or estimate the system noise level (see 
section 4.12 of this addendum) before selecting the CTS. More than 
one compound may be needed to meet the criteria; if so, obtain 
separate cylinders for each compound.)
    4.5.1  The central wavenumber position of each analytical region 
shall lie within 25 percent of the wavenumber position of at least 
one CTS absorption band.
    4.5.2  The absorption bands in section 4.5.1 of this addendum 
shall exhibit peak absorbances greater than ten times the value 
RMSEST (see section 4.12 of this addendum) but less than 
1.5 absorbance units.
    4.5.3  At least one absorption CTS band within the operating 
range of the FTIR instrument shall have an instrument-independent 
linewidth no greater than the narrowest analyte absorption band. 
Perform and document measurements or cite Studies to determine 
analyte and CTS compound linewidths.
    4.5.4  For each analytical region, specify the upper and lower 
wavenumber positions (FFUm and FFLm, 
respectively) that bracket the CTS absorption band or bands for the 
associated analytical region. Specify the wavenumber range, FNU to 
FNL, containing the absorption band that meets the criterion of 
section 4.5.3 of this addendum.
    4.5.5  Associate, whenever possible, a single set of CTS gas 
cylinders with a set of reference spectra.
    Replacement CTS gas cylinders shall contain the same compounds 
at concentrations within 5 percent of that of the original CTS 
cylinders; the entire absorption spectra (not individual spectral 
segments) of the replacement gas shall be scaled by a factor between 
0.95 and 1.05 to match the original CTS spectra.
    4.6  Prepare Reference Spectra. (Note: Reference spectra are 
available in a permanent soft copy from the EPA spectral library on 
the EMTIC (Emission Measurement Technical Information Center) 
computer bulletin board; they may be used if applicable.)
    4.6.1  Select the reference absorption pathlength 
(LR) of the cell.
    4.6.2  Obtain or prepare a set of chemical standards for each 
analyte, potential and known spectral interferants, and CTS. Select 
the concentrations of the chemical standards to correspond to the 
top of the desired range.
    4.6.2.1  Commercially-Prepared Chemical Standards. Chemical 
standards for many compounds may be obtained from independent 
sources, such as a specialty gas manufacturer, chemical company, or 
commercial laboratory. These standards (accurate to within 
 2 percent) shall be prepared according to EPA 
Traceability Protocol (see Reference D) or shall be traceable to 
NIST standards. Obtain from the supplier an estimate of the 
stability of the analyte concentration. Obtain and follow all of the 
supplier's recommendations for recertifying the analyte 
concentration.
    4.6.2.2  Self-Prepared Chemical Standards. Chemical standards 
may be prepared by diluting certified commercially prepared chemical 
gases or pure analytes with ultra-pure carrier (UPC) grade nitrogen 
according to the barometric and volumetric techniques generally 
described in Reference A, section A4.6.
    4.6.3  Record a set of the absorption spectra of the CTS {R1}, 
then a set of the reference spectra at two or more concentrations in 
duplicate over the desired range (the top of the range must be less 
than 10 times that of the bottom), followed by a second set of CTS 
spectra {R2}. (If self-prepared standards are used, see section 
4.6.5 of this addendum before disposing of any of the standards.) 
The maximum accepted standard concentration-pathlength product 
(ASCPP) for each compound shall be higher than the maximum estimated 
concentration-pathlength products for both analytes and known 
interferants in the effluent gas. For each analyte, the minimum 
ASCPP shall be no greater than ten times the concentration-
pathlength product of that analyte at its required detection limit.
    4.6.4  Permanently store the background and interferograms in 
digitized form. Document details of the mathematical process for 
generating the spectra from these interferograms. Record the sample 
pressure (PR), sample temperature (TR), 
reference absorption pathlength (LR), and interferogram 
signal integration period (tSR). Signal integration 
periods for the background interferograms shall be 
tSR. Values of PR, LR, 
and tSR shall not deviate by more than 1 
percent from the time of recording {R1} to that of recording {R2}.
    4.6.5  If self-prepared chemical standards are employed and 
spectra of only two concentrations are recorded for one or more 
compounds, verify the accuracy of the dilution technique by 
analyzing the prepared standards for those compounds with a 
secondary (non-FTIR) technique in accordance with sections 4.6.5.1 
through 4.6.5.4 of this addendum.
    4.6.5.1  Record the response of the secondary technique to each 
of the four standards prepared.
    4.6.5.2  Perform a linear regression of the response values 
(dependant variable) versus the accepted standard concentration 
(ASC) values (independent variable), with the regression constrained 
to pass through the zero-response, zero ASC point.
    4.6.5.3  Calculate the average fractional difference between the 
actual response values and the regression-predicted values (those 
calculated from the regression line using the four ASC values as the 
independent variable).
    4.6.5.4  If the average fractional difference value calculated 
in section 4.6.5.3 of this addendum is larger for any compound than 
the corresponding AUi, the dilution technique is not sufficiently 
accurate and the reference spectra prepared are not valid for the 
analysis.
    4.7  Select Analytical Regions. Using the general considerations 
in section 7 of Reference A and the spectral characteristics of the 
analytes and interferants, select the analytical regions for the 
application. Label them m = 1 to M. Specify the lower, center and 
upper wavenumber positions of each analytical region 
(FLm, FCm, and FUm, respectively). 
Specify the analytes and interferants which exhibit absorption in 
each region.
    4.8  Determine Fractional Reproducibility Uncertainties. Using 
attachement E of this addendum, calculate the fractional 
reproducibility uncertainty for each analyte (FRUi) from 
a comparison of {R1} and {R2}. If FRUi > AUi 
for any analyte, the reference spectra generated in accordance with 
section 4.6 of this addendum are not valid for the application.
    4.9  Identify Known Interferants. Using attachment B of this 
addendum, determine which potential interferants affect the analyte 
concentration determinations. Relabel these potential interferant as 
``known'' interferants, and designate these compounds from k = 1 to 
K. Attachment B to this addendum also provides criteria for 
determining whether the selected analytical regions are suitable.
    4.10  Prepare Computerized Analytical Programs.
    4.10.1  Choose or devise mathematical techniques (e.g, classical 
least squares, inverse least squares, cross-correlation, and factor 
analysis) based on equation 4 of Reference A that are appropriate 
for analyzing spectral data by comparison with reference spectra.
    4.10.2  Following the general recommendations of Reference A, 
prepare a computer program or set of programs that analyzes all of 
the analytes and known interferants, based on the selected 
analytical regions (section 4.7 of this addendum) and the prepared 
reference spectra (section 4.6 of this addendum). Specify the 
baseline correction technique (e.g., determining the slope and 
intercept of a linear baseline contribution in each analytical 
region) for each analytical region, including all relevant 
wavenumber positions.
    4.10.3  Use programs that provide as output [at the reference 
absorption pathlength (LR), reference gas temperature 
(TR), and reference gas pressure (PR)] the 
analyte concentrations, the known interferant concentrations, and 
the baseline slope and intercept values. If the sample absorption 
pathlength (LS), sample gas temperature (TS), 
or sample gas pressure (PS) during the actual sample 
analyses differ from LR, TR, and 
PR, use a program or set of programs that applies 
multiplicative corrections to the derived concentrations to account 
for these variations, and that provides as output both the corrected 
and uncorrected values. Include in the report of the analysis (see 
section 7.0 of this addendum) the details of any transformations 
applied to the original reference spectra (e.g., differentiation), 
in such a fashion that all analytical results may

[[Page 14231]]

be verified by an independent agent from the reference spectra and 
data spectra alone.
    4.11  Determine the Fractional Calibration Uncertainty. 
Calculate the fractional calibration uncertainty for each analyte 
(FCUi) according to attachment F of this addendum, and 
compare these values to the fractional uncertainty limits 
(AUi; see section 4.1.2 of this addendum). If 
FCUi > AUi, either the reference spectra or 
analytical programs for that analyte are unsuitable.
    4.12  Verify System Configuration Suitability. Using attachment 
C of this addendum, measure or obtain estimates of the noise level 
(RMSEST, absorbance) of the FTIR system. Alternatively, 
construct the complete spectrometer system and determine the values 
RMSSm using attachment G of this addendum. Estimate the 
minimum measurement uncertainty for each analyte (MAUi, 
ppm) and known interferant (MIUk, ppm) using attachment D 
of this addendum. Verify that (a) MAUi < (AUi) 
(DLi), FRUi < AUi, and 
FCUi < AUi for each analyte and that (b) the 
CTS chosen meets the requirements listed in sections 4.5.1 through 
4.5.5 of this addendum.

5.0  Sampling and Analysis Procedure

    5.1  Analysis System Assembly and Leak-Test. Assemble the 
analysis system. Allow sufficient time for all system components to 
reach the desired temperature. Then, determine the leak-rate 
(LR) and leak volume (VL), where VL 
= LR tSS. Leak volumes shall be 4 
percent of VSS.
    5.2  Verify Instrumental Performance. Measure the noise level of 
the system in each analytical region using the procedure of 
attachment G of this addendum. If any noise level is higher than 
that estimated for the system in section 4.12 of this addendum, 
repeat the calculations of attachment D of this addendum and verify 
that the requirements of section 4.12 of this addendum are met; if 
they are not, adjust or repair the instrument and repeat this 
section.
    5.3  Determine the Sample Absorption Pathlength. Record a 
background spectrum. Then, fill the absorption cell with CTS at the 
pressure PR and record a set of CTS spectra {R3}. Store 
the background and unscaled CTS single beam interferograms and 
spectra. Using attachment H of this addendum, calculate the sample 
absorption pathlength (LS) for each analytical region. 
The values LS shall not differ from the approximated 
sample pathlength LS' (see section 4.4 of this addendum) 
by more than 5 percent.
    5.4  Record Sample Spectrum. Connect the sample line to the 
source. Either evacuate the absorption cell to an absolute pressure 
below 5 mmHg before extracting a sample from the effluent stream 
into the absorption cell, or pump at least ten cell volumes of 
sample through the cell before obtaining a sample. Record the sample 
pressure PS. Generate the absorbance spectrum of the 
sample. Store the background and sample single beam interferograms, 
and document the process by which the absorbance spectra are 
generated from these data. (If necessary, apply the spectral 
transformations developed in section 5.6.2 of this addendum). The 
resulting sample spectrum is referred to below as SS. 
(Note: Multiple sample spectra may be recorded according to the 
procedures of section 5.4 of this addendum before performing 
sections 5.5 and 5.6 of this addendum.)
    5.5  Quantify Analyte Concentrations. Calculate the unscaled 
analyte concentrations RUAi and unscaled interferant 
concentrations RUIK using the programs developed in 
section 4 of this addendum. To correct for pathlength and pressure 
variations between the reference and sample spectra, calculate the 
scaling factor, RLPS using equation A.1,

RLPS = (LRPRTS)/
(LSPSTR)  ((Eq. 320-A.1)

Calculate the final analyte and interferant concentrations 
RSAi and RSIk using equations A.2 and A.3,

RSAi = RLPSRUAi  (Eq. 320-A.2)
RSIk = RLPSRUIk  (Eq. 320-A.3)

    5.6  Determine Fractional Analysis Uncertainty. Fill the 
absorption cell with CTS at the pressure PS. Record a set 
of CTS spectra {R4}. Store the background and CTS single beam 
interferograms. Using appendix H of this addendum, calculate the 
fractional analysis uncertainty (FAU) for each analytical region. If 
the FAU indicated for any analytical region is greater than the 
required accuracy requirements determined in sections 4.1.1 through 
4.1.4 of this addendum, then comparisons to previously recorded 
reference spectra are invalid in that analytical region, and the 
analyst shall perform one or both of the procedures of sections 
5.6.1 through 5.6.2 of this addendum.
    5.6.1  Perform instrumental checks and adjust the instrument to 
restore its performance to acceptable levels. If adjustments are 
made, repeat sections 5.3, 5.4 (except for the recording of a sample 
spectrum), and 5.5 of this addendum to demonstrate that acceptable 
uncertainties are obtained in all analytical regions.
    5.6.2  Apply appropriate mathematical transformations (e.g., 
frequency shifting, zero-filling, apodization, smoothing) to the 
spectra (or to the interferograms upon which the spectra are based) 
generated during the performance of the procedures of section 5.3 of 
this addendum. Document these transformations and their 
reproducibility. Do not apply multiplicative scaling of the spectra, 
or any set of transformations that is mathematically equivalent to 
multiplicative scaling. Different transformations may be applied to 
different analytical regions. Frequency shifts shall be less than 
one-half the minimum instrumental linewidth, and must be applied to 
all spectral data points in an analytical region. The mathematical 
transformations may be retained for the analysis if they are also 
applied to the appropriate analytical regions of all sample spectra 
recorded, and if all original sample spectra are digitally stored. 
Repeat sections 5.3, 5.4 (except the recording of a sample 
spectrum), and 5.5 of this addendum to demonstrate that these 
transformations lead to acceptable calculated concentration 
uncertainties in all analytical regions.

6.0 Post-Analysis Evaluations

    Estimate the overall accuracy of the analyses performed in 
accordance with sections 5.1 through 5.6 of this addendum using the 
procedures of sections 6.1 through 6.3 of this addendum.
    6.1  Qualitatively Confirm the Assumed Matrix. Examine each 
analytical region of the sample spectrum for spectral evidence of 
unexpected or unidentified interferants. If found, identify the 
interfering compounds (see Reference C for guidance) and add them to 
the list of known interferants. Repeat the procedures of section 4 
of this addendum to include the interferants in the uncertainty 
calculations and analysis procedures. Verify that the MAU and FCU 
values do not increase beyond acceptable levels for the application 
requirements. Re-calculate the analyte concentrations (section 5.5 
of this addendum) in the affected analytical regions.
    6.2  Quantitatively Evaluate Fractional Model Uncertainty (FMU). 
Perform the procedures of either section 6.2.1 or 6.2.2 of this 
addendum:
    6.2.1  Using appendix I of this addendum, determine the 
fractional model error (FMU) for each analyte.
    6.2.2  Provide statistically determined uncertainties FMU for 
each analyte which are equivalent to two standard deviations at the 
95 percent confidence level. Such determinations, if employed, must 
be based on mathematical examinations of the pertinent sample 
spectra (not the reference spectra alone). Include in the report of 
the analysis (see section 7.0 of this addendum) a complete 
description of the determination of the concentration uncertainties.
    6.3  Estimate Overall Concentration Uncertainty (OCU). Using 
appendix J of this addendum, determine the overall concentration 
uncertainty (OCU) for each analyte. If the OCU is larger than the 
required accuracy for any analyte, repeat sections 4 and 6 of this 
addendum.

7.0  Reporting Requirements

[Documentation pertaining to virtually all the procedures of 
sections 4, 5, and 6 will be required. Software copies of reference 
spectra and sample spectra will be retained for some minimum time 
following the actual testing.]

8.0  References

    (A) Standard Practices for General Techniques of Infrared 
Quantitative Analysis (American Society for Testing and Materials, 
Designation E 168-88).
    (B) The Coblentz Society Specifications for Evaluation of 
Research Quality Analytical Infrared Reference Spectra (Class II); 
Anal. Chemistry 47, 945A (1975); Appl. Spectroscopy 444, pp. 211-
215, 1990.
    (C) Standard Practices for General Techniques for Qualitative 
Infrared Analysis, American Society for Testing and Materials, 
Designation E 1252-88.
    (D) ``EPA Traceability Protocol for Assay and Certification of 
Gaseous Calibration Standards,'' U.S. Environmental Protection 
Agency Publication No. EPA/600/R-93/224, December 1993.

Attachment A to Addendum to Method 320--Definitions of Terms and 
Symbols

    A.1  Definitions of Terms. All terms used in this method that 
are not defined below have the meaning given to them in the CAA and 
in subpart A of this part.

[[Page 14232]]

    Absorption band means a contiguous wavenumber region of a 
spectrum (equivalently, a contiguous set of absorbance spectrum data 
points) in which the absorbance passes through a maximum or a series 
of maxima.
    Absorption pathlength means the distance in a spectrophotometer, 
measured in the direction of propagation of the beam of radiant 
energy, between the surface of the specimen on which the radiant 
energy is incident and the surface of the specimen from which it is 
emergent.
    Analytical region means a contiguous wavenumber region 
(equivalently, a contiguous set of absorbance spectrum data points) 
used in the quantitative analysis for one or more analytes. (Note: 
The quantitative result for a single analyte may be based on data 
from more than one analytical region.)
    Apodization means modification of the ILS function by 
multiplying the interferogram by a weighing function whose magnitude 
varies with retardation.
    Background spectrum means the single beam spectrum obtained with 
all system components without sample present.
    Baseline means any line drawn on an absorption spectrum to 
establish a reference point that represents a function of the 
radiant power incident on a sample at a given wavelength.
    Beers's law means the direct proportionality of the absorbance 
of a compound in a homogeneous sample to its concentration.
    Calibration transfer standard (CTS) gas means a gas standard of 
a compound used to achieve and/or demonstrate suitable quantitative 
agreement between sample spectra and the reference spectra; see 
section 4.5.1 of this addendum.
    Compound means a substance possessing a distinct, unique 
molecular structure.
    Concentration (c) means the quantity of a compound contained in 
a unit quantity of sample. The unit ``ppm'' (number, or mole, basis) 
is recommended.
    Concentration-pathlength product means the mathematical product 
of concentration of the species and absorption pathlength. For 
reference spectra, this is a known quantity; for sample spectra, it 
is the quantity directly determined from Beer's law. The units 
``centimeters-ppm'' or ``meters-ppm'' are recommended.
    Derivative absorption spectrum means a plot of rate of change of 
absorbance or of any function of absorbance with respect to 
wavelength or any function of wavelength.
    Double beam spectrum means a transmission or absorbance spectrum 
derived by dividing the sample single beam spectrum by the 
background spectrum.(Note: The term ``double-beam'' is used 
elsewhere to denote a spectrum in which the sample and background 
interferograms are collected simultaneously along physically 
distinct absorption paths. Here, the term denotes a spectrum in 
which the sample and background interferograms are collected at 
different times along the same absorption path.)
    Fast Fourier transform (FFT) means a method of speeding up the 
computation of a discrete FT by factoring the data into sparse 
matrices containing mostly zeros.
    Flyback means interferometer motion during which no data are 
recorded.
    Fourier transform (FT) means the mathematical process for 
converting an amplitude-time spectrum to an amplitude-frequency 
spectrum, or vice versa.
    Fourier transform infrared (FTIR) spectrometer means an 
analytical system that employs a source of mid-infrared radiation, 
an interferometer, an enclosed sample cell of known absorption 
pathlength, an infrared detector, optical elements that transfer 
infrared radiation between components, and a computer system. The 
time-domain detector response (interferogram) is processed by a 
Fourier transform to yield a representation of the detector response 
vs. infrared frequency. (Note: When FTIR spectrometers are 
interfaced with other instruments, a slash should be used to denote 
the interface; e.g., GC/FTIR; HPCL/FTIR, and the use of FTIR should 
be explicit; i.e., FTIR not IR.)
    Frequency, v means the number of cycles per unit time.
    Infrared means the portion of the electromagnetic spectrum 
containing wavelengths from approximately 0.78 to 800 microns.
    Interferogram, I() means record of the modulated 
component of the interference signal measured as a function of 
retardation by the detector.
    Interferometer means device that divides a beam of radiant 
energy into two or more paths, generates an optical path difference 
between the beams, and recombines them in order to produce 
repetitive interference maxima and minima as the optical retardation 
is varied.
    Linewidth means the full width at half maximum of an absorption 
band in units of wavenumbers (cm-1).
    Mid-infrared means the region of the electromagnetic spectrum 
from approximately 400 to 5000 cm-1.
    Reference spectra means absorption spectra of gases with known 
chemical compositions, recorded at a known absorption pathlength, 
which are used in the quantitative analysis of gas samples.
    Retardation,  means optical path difference between two 
beams in an interferometer; also known as ``optical path 
difference'' or ``optical retardation.''
    Scan means digital representation of the detector output 
obtained during one complete motion of the interferometer's moving 
assembly or assemblies.
    Scaling means application of a multiplicative factor to the 
absorbance values in a spectrum.
    Single beam spectrum means Fourier-transformed interferogram, 
representing the detector response vs. wavenumber. (Note: The term 
``single-beam'' is used elsewhere to denote any spectrum in which 
the sample and background interferograms are recorded on the same 
physical absorption path; such usage differentiates such spectra 
from those generated using interferograms recorded along two 
physically distinct absorption paths (see ``double-beam spectrum'' 
above). Here, the term applies (for example) to the two spectra used 
directly in the calculation of transmission and absorbance spectra 
of a sample.)
    Standard reference material means a reference material, the 
composition or properties of which are certified by a recognized 
standardizing agency or group. (Note: The equivalent ISO term is 
``certified reference material.'')
    Transmittance, T means the ratio of radiant power transmitted by 
the sample to the radiant power incident on the sample. Estimated in 
FTIR spectroscopy by forming the ratio of the single-beam sample and 
background spectra.
    Wavenumber, v means the number of waves per unit length. (Note: 
The usual unit of wavenumber is the reciprocal centimeter, 
cm-1. The wavenumber is the reciprocal of the wavelength, 
, when  is expressed in centimeters.) Zero-filling 
means the addition of zero-valued points to the end of a measured 
interferogram. (Note: Performing the FT of a zero-filled 
interferogram results in correctly interpolated points in the 
computed spectrum.)
    A.2  Definitions of Mathematical Symbols. The symbols used in 
equations in this subpart are defined as follows:
    (1) A, absorbance = the logarithm to the base 10 of the 
reciprocal of the transmittance (T).
[GRAPHIC] [TIFF OMITTED] TP24MR98.009

    (2) AAIim = band area of the ith analyte 
in the mth analytical region, at the concentration 
(CLi) corresponding to the product of its required 
detection limit (DLi) and analytical uncertainty limit 
(AUi) .
    (3) AAVim = average absorbance of the ith 
analyte in the mth analytical region, at the 
concentration (CLi) corresponding to the product of its 
required detection limit (DLi) and analytical uncertainty 
limit (AUi) .
    (4) ASC, accepted standard concentration = the concentration 
value assigned to a chemical standard.
    (5) ASCPP, accepted standard concentration-pathlength product = 
for a chemical standard, the product of the ASC and the sample 
absorption pathlength. The units ``centimeters-ppm'' or ``meters-
ppm'' are recommended.
    (6) AUi, analytical uncertainty limit = the maximum 
permissible fractional uncertainty of analysis for the 
ith analyte concentration, expressed as a fraction of the 
analyte concentration determined in the analysis.
    (7) AVTm = average estimated total absorbance in the 
mth analytical region.
    (8) CKWNk = estimated concentration of the 
kth known interferant.
    (9) CMAXi = estimated maximum concentration of the 
ith analyte.
    (10) CPOTj = estimated concentration of the 
jth potential interferant.
    (11) DLi, required detection limit = for the 
ith analyte, the lowest concentration of the analyte for 
which its overall fractional uncertainty (OFUi) is 
required to be less than the analytical uncertainty limit 
(AUi).
    (12) FCm = center wavenumber position of the 
mth analytical region.
    (13) FAUi, fractional analytical uncertainty = 
calculated uncertainty in the measured concentration of the 
ith analyte because of errors in the mathematical 
comparison of reference and sample spectra.

[[Page 14233]]

    (14) FCUi, fractional calibration uncertainty = 
calculated uncertainty in the measured concentration of the 
ith analyte because of errors in Beer's law modeling of 
the reference spectra concentrations.
    (15) FFLm = lower wavenumber position of the CTS 
absorption band associated with the mth analytical 
region.
    (16) FFUm = upper wavenumber position of the CTS 
absorption band associated with the mth analytical 
region.
    (17) FLm = lower wavenumber position of the 
mth analytical region.
    (18) FMUi, fractional model uncertainty = calculated 
uncertainty in the measured concentration of the ith 
analyte because of errors in the absorption model employed.
    (19) FNL = lower wavenumber position of the CTS 
spectrum containing an absorption band at least as narrow as the 
analyte absorption bands.
    (20) FNU = upper wavenumber position of the CTS 
spectrum containing an absorption band at least as narrow as the 
analyte absorption bands.
    (21) FRUi, fractional reproducibility uncertainty = 
calculated uncertainty in the measured concentration of the 
ith analyte because of errors in the reproducibility of 
spectra from the FTIR system.
    (22) FUm = upper wavenumber position of the 
mth analytical region.
    (23) IAIjm = band area of the jth 
potential interferant in the mth analytical region, at 
its expected concentration (CPOTj).
    (24) IAVim = average absorbance of the ith 
analyte in the mth analytical region, at its expected 
concentration (CPOTj).
    (25) ISCi or k, indicated standard concentration = 
the concentration from the computerized analytical program for a 
single-compound reference spectrum for the ith analyte or 
kth known interferant.
    (26) kPa = kilo-Pascal (see Pascal).
    (27) LS' = estimated sample absorption pathlength.
    (28) LR = reference absorption pathlength.
    (29) LS = actual sample absorption pathlength.
    (30) MAUi = mean of the MAUim over the 
appropriate analytical regions.
    (31) MAUim, minimum analyte uncertainty = the 
calculated minimum concentration for which the analytical 
uncertainty limit (AUi) in the measurement of the 
ith analyte, based on spectral data in the mth 
analytical region, can be maintained.
    (32) MIUj = mean of the MIUjm over the 
appropriate analytical regions.
    (33) MIUjm, minimum interferant uncertainty = the 
calculated minimum concentration for which the analytical 
uncertainty limit CPOTj/20 in the measurement of the 
jth interferant, based on spectral data in the 
mth analytical region, can be maintained.
    (34) MIL, minimum instrumental linewidth = the minimum linewidth 
from the FTIR system, in wavenumbers. (Note: The MIL of a system may 
be determined by observing an absorption band known (through higher 
resolution examinations) to be narrower than indicated by the 
system. The MIL is fundamentally limited by the retardation of the 
interferometer, but is also affected by other operational parameters 
(e.g., the choice of apodization).)
    (35) Ni = number of analytes.
    (36) Nj = number of potential interferants.
    (37) Nk = number of known interferants.
    (38) Nscan = the number of scans averaged to obtain 
an interferogram.
    (39) OFUi = the overall fractional uncertainty in an 
analyte concentration determined in the analysis (OFUi = 
MAX {FRU, FCUi, FAUi, FMUi }).
    (40) Pascal (Pa) = metric unit of static pressure, equal to one 
Newton per square meter; one atmosphere is equal to 101,325 Pa; 1/
760 atmosphere (one Torr, or one millimeter Hg) is equal to 133.322 
Pa.
    (41) Pmin = minimum pressure of the sampling system 
during the sampling procedure.
    (42) PS' = estimated sample pressure.
    (43) PR = reference pressure.
    (44) PS = actual sample pressure.
    (45) RMSsm = measured noise level of the FTIR system 
in the mth analytical region.
    (46) RMSD, root mean square difference = a measure of accuracy 
determined by the following equation:
[GRAPHIC] [TIFF OMITTED] TP24MR98.010

Where:

n = the number of observations for which the accuracy is determined.
ei = the difference between a measured value of a 
property and its mean value over the n observations.

    Note: The RMSD value ``between a set of n contiguous absorbance 
values (Ai) and the mean of the values'' (AM) 
is defined as
[GRAPHIC] [TIFF OMITTED] TP24MR98.011

    (47) RSAi = the (calculated) final concentration of 
the ith analyte.
    (48) RSIk = the (calculated) final concentration of 
the kth known interferant.
    (49) tscan, scan time = time used to acquire a single 
scan, not including flyback.
    (50) tS, signal integration period = the period of 
time over which an interferogram is averaged by addition and scaling 
of individual scans. In terms of the number of scans 
Nscan and scan time tscan, tS = 
Nscantscan.
    (51) tSR = signal integration period used in 
recording reference spectra.
    (52) tSS = signal integration period used in 
recording sample spectra.
    (53) TR = absolute temperature of gases used in 
recording reference spectra.
    (54) TS = absolute temperature of sample gas as 
sample spectra are recorded.
    (55) TP, Throughput = manufacturer's estimate of the fraction of 
the total infrared power transmitted by the absorption cell and 
transfer optics from the interferometer to the detector.
    (56) VSS = volume of the infrared absorption cell, 
including parts of attached tubing.
    (57) Wik = weight used to average over analytical 
regions k for quantities related to the analyte i; see attachment D 
of this addendum.

Attachment B to Addendum to Method 320--Identifying Spectral 
Interferants

B.1  General

    B.1.1  Assume a fixed absorption pathlength equal to the value 
LS'.
    B.1.2  Use band area calculations to compare the relative 
absorption strengths of the analytes and potential interferants. In 
the mth analytical region (FLm to 
FUm), use either rectangular or trapezoidal 
approximations to determine the band areas described below (see 
Reference A, sections A.3.1 through A.3.3). Document any baseline 
corrections applied to the spectra.
    B.1.3  Use the average total absorbance of the analytes and 
potential interferants in each analytical region to determine 
whether the analytical region is suitable for analyte concentration 
determinations. (Note: The average absorbance in an analytical 
region is the band area divided by the width of the analytical 
region in wavenumbers. The average total absorbance in an analytical 
region is the sum of the average absorbances of all analytes and 
potential interferants.)

B.2  Calculations

    B.2.1  Prepare spectral representations of each analyte at the 
concentration CLi = (DLi)(AUi), 
where DLi is the required detection limit and 
AUi is the maximum permissible analytical uncertainty. 
For the mth analytical region, calculate the band area 
(AAIim) and average absorbance (AAVim) from 
these scaled analyte spectra.
    B.2.2  Prepare spectral representations of each potential 
interferant at its expected concentration (CPOTj). For 
the mth analytical region, calculate the band area 
(IAIjm) and average absorbance (IAVjm) from 
these scaled potential interferant spectra.
    B.2.3  Repeat the calculation for each analytical region, and 
record the band area results in matrix form as indicated in Figure 
B.1.
    B.2.4  If the band area of any potential interferant in an 
analytical region is greater than the one-half the band area of any 
analyte (i.e., IAIjm >0.5 AAIim for any pair 
ij and any m), classify the potential interferant as a known 
interferant. Label the known interferants k = 1 to K. Record the 
results in matrix form as indicated in Figure B.2.
    B.2.5  Calculate the average total absorbance (AVTm) 
for each analytical region and record the values in the last row of 
the matrix described in Figure B.2. Any analytical region where 
AVTm >2.0 is unsuitable.

     Figure B.1.--Presentation of Potential Interferant Calculations    
------------------------------------------------------------------------
                                             Analytical regions         
                                   -------------------------------------
                                            1                  M        
------------------------------------------------------------------------
          Analyte Labels                                                
                                                                        
1.................................  AAI11              AAI1M            
I.................................  AAII1              AAIIM            
                                                                        
   Potential Interferant Labels                                         
                                                                        
1.................................  IAI11              IAI1M            

[[Page 14234]]

                                                                        
J.................................  IAIJ1              IAIJM            
------------------------------------------------------------------------


       Figure B.2.--Presentation of Known Interferant Calculations      
------------------------------------------------------------------------
                                             Analytical regions         
                                   -------------------------------------
                                            1                  M        
------------------------------------------------------------------------
          Analyte Labels                                                
                                                                        
1.................................  AAI11              AAI1M            
I.................................  AAII1              AAIIM            
     Known Interferant Labels                                           
                                                                        
1.................................  IAI11              IAI1M            
K.................................  IAIK1              IAIKM            
                                   -------------------------------------
    Total Average Absorbance......  AVT1               AVTM             
------------------------------------------------------------------------

Attachment C to Addendum to Method 320--Estimating Noise Levels

C.1  General

    C.1.1  The root-mean-square (RMS) noise level is the standard 
measure of noise in this addendum. The RMS noise level of a 
contiguous segment of a spectrum is defined as the RMS difference 
(RMSD) between the absorbance values which form the segment and the 
mean value of that segment (see attachment A of this addendum).
    C.1.2  The RMS noise value in double-beam absorbance spectra is 
assumed to be inversely proportional to: (a) the square root of the 
signal integration period of the sample single beam spectra from 
which it is formed, and (b) the total infrared power transmitted 
through the interferometer and absorption cell.
    C.1.3  Practically, the assumption of C.1.2 allows the RMS noise 
level of a complete system to be estimated from the quantities 
described in sections C.1.3.1 through C.1.3.4:
    C.1.3.1  RMSMAN, the noise level of the system (in 
absorbance units), without the absorption cell and transfer optics, 
under those conditions necessary to yield the specified minimum 
instrumental linewidth, e.g., Jacquinot stop size.
    C.1.3.2  tMAN, the manufacturer's signal integration 
time used to determine RMSMAN.
    C.1.3.3  tSS, the signal integration time for the 
analyses.
    C.1.3.4  TP, the manufacturer's estimate of the fraction of the 
total infrared power transmitted by the absorption cell and transfer 
optics from the interferometer to the detector.

C.2  Calculations

    C.2.1  Obtain the values of RMSMAN, tMAN, 
and TP from the manufacturers of the equipment, or determine the 
noise level by direct measurements with the completely constructed 
system proposed in section 4 of this addendum.
    C.2.2  Calculate the noise value of the system 
(RMSEST) using equation C.1.
[GRAPHIC] [TIFF OMITTED] TP24MR98.012

Attachment D to Addendum to Method 320--Estimating Minimum 
Concentration Measurement Uncertainties (MAU and MIU)

D.1  General

    Estimate the minimum concentration measurement uncertainties for 
the ith analyte (MAUi) and jth 
interferant (MIUj) based on the spectral data in the 
mth analytical region by comparing the analyte band area 
in the analytical region (AAIim) and estimating or 
measuring the noise level of the system (RMSEST or 
RMSSm). (Note: For a single analytical region, the MAU or 
MIU value is the concentration of the analyte or interferant for 
which the band area is equal to the product of the analytical region 
width (in wavenumbers) and the noise level of the system (in 
absorbance units). If data from more than one analytical region are 
used in the determination of an analyte concentration, the MAU or 
MIU is the mean of the separate MAU or MIU values calculated for 
each analytical region.)

D.2  Calculations

    D.2.1  For each analytical region, set RMS = RMSSm if 
measured ( attachment G of this addendum), or set RMS = 
RMSEST if estimated ( attachment C of this addendum).
    D.2.2  For each analyte associated with the analytical region, 
calculate MAUim using equation D.1,
[GRAPHIC] [TIFF OMITTED] TP24MR98.013

    D.2.3  If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
MAUi = MAUim.
    D.2.4  If more than one analytical region is used to calculate 
the concentration of the ith analyte, set MAUi 
equal to the weighted mean of the appropriate MAUim 
values calculated above; the weight for each term in the mean is 
equal to the fraction of the total wavenumber range used for the 
calculation represented by each analytical region. Mathematically, 
if the set of analytical regions employed is {m'}, then the MAU for 
each analytical region is given by equation D.2.
[GRAPHIC] [TIFF OMITTED] TP24MR98.014

    Where the weight Wik is defined for each term in the sum as
    [GRAPHIC] [TIFF OMITTED] TP24MR98.015
    

[[Page 14235]]


    D.2.5  Repeat sections D.2.1 through D.2.4 of this to calculate 
the analogous values MIUj for the interferants j = 1 to 
J. Replace the value (AUi) (DLi) in equation 
D.1 with CPOTj/20; replace the value AAIim in 
equation D.1 with IAIjm.

Attachment E to Addendum to Method 320--Determining Fractional 
Reproducibility Uncertainties (FRU)

E.1  General

    To estimate the reproducibility of the spectroscopic results of 
the system, compare the CTS spectra recorded before and after 
preparing the reference spectra. Compare the difference between the 
spectra to their average band area. Perform the calculation for each 
analytical region on the portions of the CTS spectra associated with 
that analytical region.

E.2  Calculations

    E.2.1  The CTS spectra {R1} consist of N spectra, denoted by 
S1i, i=1, N. Similarly, the CTS spectra {R2} consist of N 
spectra, denoted by S2i, i=1, N. Each Ski is 
the spectrum of a single compound, where i denotes the compound and 
k denotes the set {Rk} of which Ski is a member. Form the 
spectra S3 according to S3i = 
S2i-S1i for each i. Form the spectra 
S4 according to S4i = 
[S2i+S1i]/2 for each i.
    E.2.2  Each analytical region m is associated with a portion of 
the CTS spectra S2i and S1i, for a particular 
i, with lower and upper wavenumber limits FFLm and 
FFUm, respectively.
    E.2.3  For each m and the associated i, calculate the band area 
of S4i in the wavenumber range FFUm to 
FFLm. Follow the guidelines of section B.1.2 of this 
addendum for this band area calculation. Denote the result by 
BAVm.
    E.2.4  For each m and the associated i, calculate the RMSD of 
S3i between the absorbance values and their mean in the 
wavenumber range FFUm to FFLm. Denote the 
result by SRMSm.
    E.2.5  For each analytical region m, calculate FMm 
using equation E.1,
[GRAPHIC] [TIFF OMITTED] TP24MR98.016

    E.2.6  If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
FRUi = FMm.
    E.2.7  If a number pi of analytical regions are used to 
calculate the concentration of the ith analyte, set 
FRUi equal to the weighted mean of the appropriate 
FMm values calculated according to section E.2.5. 
Mathematically, if the set of analytical regions employed is {m'}, 
then FRUi is given by equation E.2,
[GRAPHIC] [TIFF OMITTED] TP24MR98.017

    Where the Wik are calculated as described in 
Attachment D of this addendum.

Attachment F to Addendum to Method 320--Determining Fractional 
Calibration Uncertainties (FCU)

F.1  General

    F.1.1  The concentrations yielded by the computerized analytical 
program applied to each single-compound reference spectrum are 
defined as the indicated standard concentrations (ISC's). The ISC 
values for a single compound spectrum should ideally equal the 
accepted standard concentration (ASC) for one analyte or 
interferant, and should ideally be zero for all other compounds. 
Variations from these results are caused by errors in the ASC 
values, variations from the Beer's law (or modified Beer's law) 
model used to determine the concentrations, and noise in the 
spectra. When the first two effects dominate, the systematic nature 
of the errors is often apparent and the analyst shall take steps to 
correct them.
    F.1.2  When the calibration error appears non-systematic, apply 
the procedures of sections F.2.1 through F.2.3 of this appendix to 
estimate the fractional calibration uncertainty (FCU) for each 
compound. The FCU is defined as the mean fractional error between 
the ASC and the ISC for all reference spectra with non-zero ASC for 
that compound. The FCU for each compound shall be less than the 
required fractional uncertainty specified in section 4.1 of this 
addendum.
    F.1.3  The computerized analytical programs shall also be 
required to yield acceptably low concentrations for compounds with 
ISC = 0 when applied to the reference spectra. The ISC of each 
reference spectrum for each analyte or interferant shall not exceed 
that compound's minimum measurement uncertainty (MAU or MIU).

F.2  Calculations

    F.2.1  Apply each analytical program to each reference spectrum. 
Prepare a similar table to that in Figure F.1 to present the ISC and 
ASC values for each analyte and interferant in each reference 
spectrum. Maintain the order of reference file names and compounds 
employed in preparing Figure F.1.
    F.2.2  For all reference spectra in Figure F.1, verify that the 
absolute values of the ISC's are less than the compound's MAU (for 
analytes) or MIU (for interferants).
    F.2.3  For each analyte reference spectrum, calculate the 
quantity (ASC-ISC)/ASC. For each analyte, calculate the mean of 
these values (the FCUi for the ith analyte) 
over all reference spectra. Prepare a similar table to that in 
Figure F.2 to present the FCUi and analytical uncertainty 
limit (AUi) for each analyte.

                   Figure F.1.--Presentation of Accepted Standard Concentrations (ASC's) and Indicated Standard Concentrations (ISC's)                  
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                        
--------------------------------------------------------------------------------------------------------------------------------------------------------
            Compound name             Reference spectrum file   ASC (ppm)                                                                               
                                                name                                                                                                    
(5)ISC (ppm)                                                                                                                                            
                                                                                                                                                        
(5)Analytes    Interferants                                                                                                                             
                                                                                                                                                        
(5) i=1           I                                                                                                                                     
                                                                                                                                                        
(5) j=1           J                                                                                                                                     
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
                                                                                                                                                        
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 14236]]


    Figure F.2.--Presentation of Fractional Calibration Uncertainties   
               (FCU's) and Analytical Uncertainties (AU's)              
------------------------------------------------------------------------
              Analyte name                    FCU (%)         AU (%)    
------------------------------------------------------------------------
                                                                        
                                                                        
                                                                        
                                                                        
                                                                        
                                                                        
------------------------------------------------------------------------

Attachment G to Addendum to Method 320--Measuring Noise Levels

G.1  General

    The root-mean-square (RMS) noise level is the standard measure 
of noise. The RMS noise level of a contiguous segment of a spectrum 
is the RMSD between the absorbance values that form the segment and 
the mean value of the segment (see appendix A of this addendum).

G.2  Calculations

    G.2.1  Evacuate the absorption cell or fill it with UPC grade 
nitrogen at approximately one atmosphere total pressure.
    G.2.2  Record two single beam spectra of signal integration 
period tSS.
    G.2.3  Form the double beam absorption spectrum from these two 
single beam spectra, and calculate the noise level RMSSm 
in the M analytical regions.

Attachment H of Addendum to Method 320--Determining Sample Absorption 
Pathlength (LS) and Fractional Analytical Uncertainty (FAU)

H.1  General

    Reference spectra recorded at absorption pathlength 
(LR), gas pressure (PR), and gas absolute 
temperature (TR) may be used to determine analyte 
concentrations in samples whose spectra are recorded at conditions 
different from that of the reference spectra, i.e., at absorption 
pathlength (LS), absolute temperature (TS), 
and pressure (PS). This appendix describes the 
calculations for estimating the fractional uncertainty (FAU) of this 
practice. It also describes the calculations for determining the 
sample absorption pathlength from comparison of CTS spectra, and for 
preparing spectra for further instrumental and procedural checks.
    H.1.1  Before sampling, determine the sample absorption 
pathlength using least squares analysis. Determine the ratio 
LS/LR by comparing the spectral sets {R1} and 
{R3}, which are recorded using the same CTS at LS and 
LR, and TS and TR, but both at 
PR.
    H.1.2  Determine the fractional analysis uncertainty (FAU) for 
each analyte by comparing a scaled CTS spectral set, recorded at 
LS, TS, and PS, to the CTS 
reference spectra of the same gas, recorded at LR, 
TR, and PR. Perform the quantitative 
comparison after recording the sample spectra, based on band areas 
of the spectra in the CTS absorbance band associated with each 
analyte.

H.2  Calculations

    H.2.1   Absorption Pathlength Determination. Perform and 
document separate linear baseline corrections to each analytical 
region in the spectral sets {R1} and {R3}. Form a one-dimensional 
array AR containing the absorbance values from all 
segments of {R1} that are associated with the analytical regions; 
the members of the array are ARi, i = 1, n. Form a 
similar one-dimensional array AS from the absorbance 
values in the spectral set {R3}; the members of the array are 
ASi, i = 1, n. Based on the model AS = 
rAR + E, determine the least-squares estimate of r', the 
value of r which minimizes the square error E \2\. Calculate the 
sample absorption pathlength, LS, using equation H.1,

LS = r'(TS/TR)LR  (Eq. 
320-H.)

    H.2.2  Fractional Analysis Uncertainty. Perform and document 
separate linear baseline corrections to each analytical region in 
the spectral sets {R1} and {R4}. Form the arrays AS and 
AR as described in section H.2.1 of this appendix, using 
values from {R1} to form AR, and values from {R4} to form 
AS. Calculate NRMSE and IAAV using 
equations H.2 and H.3,
[GRAPHIC] [TIFF OMITTED] TP24MR98.018

[GRAPHIC] [TIFF OMITTED] TP24MR98.019

    The fractional analytical uncertainty, FAU, is given by equation 
H.4,
[GRAPHIC] [TIFF OMITTED] TP24MR98.020

Attachment I to Addendum to Method 320--Determining Fractional Model 
Uncertainties (FMU)

I.1  General

    To prepare analytical programs for FTIR analyses, the sample 
constituents must first be assumed. The calculations in this, 
appendix, based upon a simulation of the sample spectrum, shall be 
used to verify the appropriateness of these assumptions. The 
simulated spectra consist of the sum of single compound reference 
spectra scaled to represent their contributions to the sample 
absorbance spectrum; scaling factors are based on the indicated 
standard concentrations (ISC) and measured (sample) analyte and 
interferant concentrations, the sample and reference absorption 
pathlengths, and the sample and reference gas pressures. No band-
shape correction for differences in the temperature of the sample 
and reference spectra gases is made; such errors are included in the 
FMU estimate. The actual and simulated sample spectra are 
quantitatively compared to determine the fractional model 
uncertainty; this comparison uses the reference spectra band areas 
and residuals in the difference spectrum formed from the actual and 
simulated sample spectra.

I.2  Calculations

    I.2.1  For each analyte (with scaled concentration 
RSAi), select a reference spectrum SAi with 
indicated standard concentration ISCi. Calculate the 
scaling factors, RAi, using equation I.1,
[GRAPHIC] [TIFF OMITTED] TP24MR98.021

    Form the spectra SACi by scaling each SAi 
by the factor RAi.
    I.2.2  For each interferant, select a reference spectrum 
SIk with indicated standard concentration 
ISCk. Calculate the scaling factors, RIk, 
using equation I.2,

[[Page 14237]]

[GRAPHIC] [TIFF OMITTED] TP24MR98.022


    Form the spectra SICk by scaling each SIk 
by the factor RIk.
    I.2.3  For each analytical region, determine by visual 
inspection which of the spectra SACi and SICk 
exhibit absorbance bands within the analytical region. Subtract each 
spectrum SACi and SICk exhibiting absorbance 
from the sample spectrum SS to form the spectrum 
SUBS. To save analysis time and to avoid the introduction 
of unwanted noise into the subtracted spectrum, it is recommended 
that the calculation be made (1) only for those spectral data points 
within the analytical regions, and (2) for each analytical region 
separately using the original spectrum SS.
    I.2.4  For each analytical region m, calculate the RMSD of 
SUBS between the absorbance values and their mean in the 
region FFUm to FFLm. Denote the result by 
RMSSm.
    I.2.5  For each analyte i, calculate FMm, using equation I.3,
    [GRAPHIC] [TIFF OMITTED] TP24MR98.023
    
for each analytical region associated with the analyte.

    I.2.6  If only the mth analytical region is used to 
calculate the concentration of the ith analyte, set 
FMUi=FMm.
    I.2.7  If a number of analytical regions are used to calculate 
the concentration of the ith analyte, set FMi 
equal to the weighted mean of the appropriate FMm values 
calculated using equation I-3. Mathematically, if the set of 
analytical regions employed is {m'}, then the fractional model 
uncertainty, FMU, is given by equation I.4,
[GRAPHIC] [TIFF OMITTED] TP24MR98.024

    Where Wik is calculated as described in Attachment D 
of this addendum.

Attachment J to Addendum to Method 320--Determining Overall 
Concentration Uncertainties (OCU)

    The calculations in this addendum estimate the measurement 
uncertainties for various FTIR measurements. The lowest possible 
overall concentration uncertainty (OCU) for an analyte is its MAU 
value, which is an estimate of the absolute concentration 
uncertainty when spectral noise dominates the measurement error. 
However, if the product of the largest fractional concentration 
uncertainty (FRU, FCU, FAU, or FMU) and the measured concentration 
of an analyte exceeds the MAU for the analyte, then the OCU is this 
product. In mathematical terms, set OFUi = 
MAX{FRUi, FCUi, FAUi, 
FMUi} and OCUi = 
MAX{RSAi*OFUi, MAUi}.

Method 321--Measurement of Gaseous Hydrogen Chloride Emissions At 
Portland Cement Kilns by Fourier Transform Infrared (FTIR) Spectroscopy

1.0  Introduction

    This method should be performed by those persons familiar with 
the operation of Fourier Transform Infrared (FTIR) instrumentation 
in the application to source sampling. This document describes the 
sampling procedures for use in the application of FTIR spectrometry 
for the determination of vapor phase hydrogen chloride (HCl) 
concentrations both before and after particulate matter control 
devices installed at portland cement kilns. A procedure for analyte 
spiking is included for quality assurance. This method is considered 
to be self validating provided that the requirements listed in 
section 9 of this method are followed. The analytical procedures for 
interpreting infrared spectra from emission measurements are 
described in the ``Protocol For The Use of Extractive Fourier 
Transform Infrared (FTIR) Spectrometry in Analyses of Gaseous 
Emissions From Stationary Industrial Sources'', included as an 
addendum to proposed Method 320 of this appendix (hereafter referred 
to as the ``FTIR Protocol''). References 1 and 2 describe the use of 
FTIR spectrometry in field measurements. Sample transport presents 
the principal difficulty in directly measuring HCl emissions. This 
identical problem must be overcome by any extractive measurement 
method. HCl is reactive and water soluble. The sampling system must 
be adequately designed to prevent sample condensation in the system.
    1.1  Scope and Application.
    This method is specifically designed for the application of FTIR 
Spectrometry in extractive measurements of gaseous HCl 
concentrations in portland cement kiln emissions.
    1.2  Applicability. This method applies to the measurement of 
HCl [CAS No. 7647-01-0]. This method can be applied to the 
determination of HCl concentrations both before and after 
particulate matter control devices installed at portland cement 
manufacturing facilities. This method applies to either continuous 
flow through measurement (with isolated sample analysis) or grab 
sampling (batch analysis). HCl is measured using the mid-infrared 
spectral region for analysis (about 400 to 4000 cm-1 or 
25 to 2.5 m). Table 1 lists the suggested analytical region 
for quantification of HCl taking the interference from water vapor 
into consideration.

               Table 1.--Example Analytical Region for HCl              
------------------------------------------------------------------------
                                      Analytical          Potential     
             Compound                region (cm-1)      interferants    
------------------------------------------------------------------------
Hydrogen chloride.................       2679-2840  Water.              
------------------------------------------------------------------------

    1.3  Method Range and Sensitivity.
    1.3.1  The analytical range is determined by the instrumental 
design and the composition of the gas stream. For practical purposes 
there is no upper limit to the range because the pathlength may be 
reduced or the sample may be diluted. The lower detection range 
depends on (1) the absorption coefficient of the compound in the 
analytical frequency region, (2) the spectral resolution, (3) the 
interferometer sampling time, (4) the detector sensitivity and 
response, and (5) the absorption pathlength.
    1.3.2  The practical lower quantification range is usually 
higher than the instrument sensitivity allows and is dependent upon 
(1) the presence of interfering species in the exhaust gas including 
H2O, CO2, and SO2, (2) analyte 
losses in the sampling system, (3) the optical alignment of the gas 
cell and transfer optics, and (4) the quality of the reflective 
surfaces in the cell (cell throughput). Under typical test 
conditions (moisture content of up to 30% and CO2 
concentrations from 1 to 15 percent), a 22 meter path length cell 
with a suitable sampling system may achieve a lower quantification 
range of from 1 to 5 ppm for HCl.
    1.4  Data Quality Objectives.
    1.4.1  In designing or configuring the analytical system, data 
quality is determined by measuring of the root mean square deviation 
(RMSD) of the absorbance values within a chosen spectral 
(analytical) region. The RMSD provides an indication of the signal-
to-noise ratio (S/N) of the spectral baseline. Appendix D of the 
FTIR Protocol (the addendum to Method 320 of this appendix) presents 
a discussion of the relationship between the RMSD, lower detection 
limit, DLi, and analytical uncertainty, AUi. 
It is important to consider the target analyte quantification limit 
when performing testing with FTIR instrumentation, and to optimize 
the system to achieve the desired detection limit.
    1.4.2  Data quality is determined by measuring the root mean 
square (RMS) noise level in each analytical spectral region 
(appendix C of the FTIR Protocol). The RMS noise is defined as the 
root mean square deviation (RMSD) of the absorbance values in an 
analytical region from the mean absorbance value in the same region. 
Appendix D of the FTIR Protocol defines the minimum analyte 
uncertainty (MAU), and how the RMSD is used to calculate the MAU. 
The MAUim is the minimum concentration of the ith analyte 
in the mth analytical region for which the analytical uncertainty 
limit can be maintained. Table 2 to this method presents example 
values of AU and MAU using the analytical region presented in Table 
1 to this method.

[[Page 14238]]



 TABLE 2.--Example Pre-Test Protocol Calculations for Hydrogen Chloride 
------------------------------------------------------------------------
                                                                HCl     
------------------------------------------------------------------------
Reference concentration (ppm-meters)/K..................            11.2
Reference Band Area.....................................           2.881
DL (ppm-meters)/K.......................................          0.1117
AU......................................................             0.2
CL (DL x AU)............................................         0.02234
FL (cm-1)...............................................         2679.83
FU (cm-1)...............................................         2840.93
FC (cm-1)...............................................         2760.38
AAI (ppm-meters)/K......................................         0.06435
RMSD....................................................       2.28 E-03
MAU (ppm-meters)/K......................................        1.28E-01
MAU ppm at 22 meters and 250  deg.F.....................          0.2284
------------------------------------------------------------------------

2.0  Summary of Method

    2.1  Principle.
    See Method 320 of this appendix. HCl can also undergo rotation 
transitions by absorbing energy in the far-infrared spectral region. 
The rotational transitions are superimposed on the vibrational 
fundamental to give a series of lines centered at the fundamental 
vibrational frequency, 2885 cm-1. The frequencies of 
absorbance and the pattern of rotational/vibrational lines are 
unique to HCl. When this distinct pattern is observed in an infrared 
spectrum of an unknown sample, it unequivocally identifies HCl as a 
component of the mixture. The infrared spectrum of HCl is very 
distinctive and cannot be confused with the spectrum of any other 
compound. See Reference 6.
    2.2  Sampling and Analysis. See Method 320 of this appendix.
    2.3  Operator Requirements. The analyst must have knowledge of 
spectral patterns to choose an appropriate absorption path length or 
determine if sample dilution is necessary. The analyst should also 
understand FTIR instrument operation well enough to choose 
instrument settings that are consistent with the objectives of the 
analysis.

3.0  Definitions

    See A of the FTIR Protocol.

4.0  Interferences

    This method will not measure HCl under conditions: (1) where the 
sample gas stream can condense in the sampling system or the 
instrumentation, or (2) where a high moisture content sample 
relative to the analyte concentrations imparts spectral interference 
due to the water vapor absorbance bands. For measuring HCl the first 
(sampling) consideration is more critical. Spectral interference 
from water vapor is not a significant problem except at very high 
moisture levels and low HCl concentrations.
    4.1  Analytical Interferences. See Method 320 of this appendix.
    4.1.1  Background Interferences. See Method 320 of this 
appendix.
    4.1.2  Spectral interferences. Water vapor can present spectral 
interference for FTIR gas analysis of HCl. Therefore, the water 
vapor in the spectra of kiln gas samples must be accounted for. This 
means preparing at least one spectrum of a water vapor sample where 
the moisture concentration is close to that in the kiln gas.
    4.2  Sampling System Interferences. The principal sampling 
system interferant for measuring HCl is water vapor. Steps must be 
taken to ensure that no condensation forms anywhere in the probe 
assembly, sample lines, or analytical instrumentation. Cold spots 
anywhere in the sampling system must be avoided. The extent of 
sampling system bias in the FTIR analysis of HCl depends on 
concentrations of potential interferants, moisture content of the 
gas stream, temperature of the gas stream, temperature of sampling 
system components, sample flow rate, and reactivity of HCl with 
other species in the gas stream (e.g., ammonia). For measuring HCl 
in a wet gas stream the temperatures of the gas stream, sampling 
components, and the sample flow rate are of primary importance. 
Analyte spiking with HCl is performed to demonstrate the integrity 
of the sampling system for transporting HCl vapor in the flue gas to 
the FTIR instrument. See section 9 of this method for a complete 
description of analyte spiking.

5.0  Safety

    5.1  Hydrogen chloride vapor is corrosive and can cause 
irritation or severe damage to respiratory system, eyes and skin. 
Exposure to this compound should be avoided.
    5.2  This method may involve sampling at locations having high 
positive or negative pressures, or high concentrations of hazardous 
or toxic pollutants, and can not address all safety problems 
encountered under these diverse sampling conditions. It is the 
responsibility of the tester(s) to ensure proper safety and health 
practices, and to determine the applicability of regulatory 
limitations before performing this test method. Leak-check 
procedures are outlined in section 8.2 of Method 320 of this .

6.0  Equipment and Supplies.

    (Note: Mention of trade names or specific products does not 
constitute endorsement by the Environmental Protection Agency.)

    6.1  FTIR Spectrometer and Detector. An FTIR Spectrometer system 
(interferometer, transfer optics, gas cell and detector) having the 
capability of measuring HCl to the predetermined minimum detectable 
level required (see section 4.1.3 of the FTIR Protocol). The system 
must also include an accurate means to control and/or measure the 
temperature of the FTIR gas analysis cell, and a personal computer 
with compatible software that provides real-time updates of the 
spectral profile during sample and spectral collection.
    6.2  Pump. Capable of evacuating the FTIR cell volume to 1 Torr 
(133.3 Pascals) within two minutes (for batch sample analysis).
    6.3  Mass Flow Meters/Controllers. To accurately measure analyte 
spike flow rate, having the appropriate calibrated range and a 
stated accuracy of  2 percent of the absolute 
measurement value. This device must be calibrated with the major 
component of the calibration/spike gas (e.g., nitrogen) using an 
NIST traceable bubble meter or equivalent. Single point calibration 
checks should be performed daily in the field. When spiking HCl, the 
mass flow meter/controller should be thoroughly purged before and 
after introduction of the gas to prevent corrosion of the interior 
parts.
    6.4  Polytetrafluoroethane tubing. Diameter and length suitable 
to connect cylinder regulators.
    6.5  Stainless Steel tubing. Type 316 of appropriate length and 
diameter for heated connections.
    6.6  Gas Regulators. Purgeable HCl regulator.
    6.7  Pressure Gauge. Capable of measuring pressure from 0 to 
1000 Torr (133.3 Pa=1 Torr) within  5 percent.
    6.8  Sampling Probe. Glass, stainless steel or other appropriate 
material of sufficient length and physical integrity to sustain 
heating, prevent adsorption of analytes and capable of reaching gas 
sampling point.
    6.9  Sampling Line. Heated 180  deg.C (360  deg.F) and 
fabricated of either stainless steel, polytetrafluoroethane or other 
material that prevents adsorption of HCl and transports effluent to 
analytical instrumentation. The extractive sample line must have the 
capability to transport sample gas to the analytical components as 
well as direct heated calibration spike gas to the calibration 
assembly located at the sample probe. It is important to minimize 
the length of heated sample line.
    6.10  Particulate Filters. A sintered stainless steel filter 
rated at 20 microns or greater may be placed at the inlet of the 
probe (for removal of large particulate matter). A heated filter 
(Balston or equivalent) rated at 1 micron is necessary 
for primary particulate matter removal, and shall be placed 
immediately after the heated probe. The filter/filter holder 
temperature should be maintained at 180  deg.C (360  deg.F).
    6.11   Calibration/Analyte Spike Assembly. A heated three-way 
valve assembly (or equivalent) to introduce surrogate spikes into 
the sampling system at the outlet of the probe before the primary 
particulate filter.
    6.12  Sample Extraction Pump. A leak-free heated head pump 
(KNF Neuberger or equivalent) capable of extracting 
sample effluent through entire sampling system at a rate which 
prevents analyte losses and minimizes analyzer response time. The 
pump should have a heated by-pass and may be placed either before 
the FTIR instrument or after. If the sample pump is located upstream 
of the FTIR instrument, it must be fabricated from materials non-
reactive to HCl. The sampling system and FTIR measurement system 
shall allow the operator to obtain at least six sample spectra 
during a one-hour period.
    6.13  Barometer. For measurement of barometric pressure.
    6.14  Gas Sample Manifold. A distribution manifold having the 
capabilities listed in sections 6.14.1 through 6.14.4;
    6.14.1  Delivery of calibration gas directly to the analytical 
instrumentation;
    6.14.2  Delivery of calibration gas to the sample probe (system 
calibration or analyte spike) via a heated traced sample line;
    6.14.3  Delivery of sample gas (kiln gas, spiked kiln gas, or 
system calibrations) to the analytical instrumentation;
    6.14.4  Delivery (optional) of a humidified nitrogen sample 
stream.

[[Page 14239]]

    6.15  Flow Measurement Device. Type S Pitot tube (or equivalent) 
and Magnahelic set for measurement of volumetric flow 
rate.

7.0  Reagents and Standards

    HCl can be purchased in a standard compressed gas cylinder. The 
most stable HCl cylinder mixture available has a concentration 
certified at 5 percent. Such a cylinder is suitable for 
performing analyte spiking because it will provide reproducible 
samples. The stability of the cylinder can be monitored over time by 
periodically performing direct FTIR analysis of cylinder samples. It 
is recommended that a 10-50 ppm cylinder of HCl be prepared having 
from 2-5 ppm SF6 as a tracer compound. (See sections 7.1 through 7.3 
of Method 320 of this for a complete description of the use of 
existing HCl reference spectra. See section 9.1 of Method 320 of 
this for a complete discussion of standard concentration selection.)

8.0  Sample Collection, Preservation and Storage

    See also Method 320 of this appendix.
    8.1  Pretest. A screening test is ideal for obtaining proper 
data that can be used for preparing analytical program files. 
Information from literature surveys and source personnel is also 
acceptable. Information about the sampling location and gas stream 
composition is required to determine the optimum sampling system 
configuration for measuring HCl. Determine the percent moisture of 
the kiln gas by Method 4 of appendix A to part 60 of this chapter or 
by performing a wet bulb/dry bulb measurement. Perform a preliminary 
traverse of the sample duct or stack and select the sampling 
point(s). Acquire an initial spectrum and determine the optimum 
operational pathlength of the instrument.
    8.2  Leak-Check. See Method 320 of this appendix, section 8.2 
for direction on performing leak-checks.
    8.3  Background Spectrum. See Method 320 of this appendix, 
section 8.5 for direction in background spectral acquisition.
    8.4  Pre-Test Calibration Transfer Standard (Direct Instrument 
Calibration). See Method 320 of this appendix, section 8.3 for 
direction in CTS spectral acquisition.
    8.5  Pre-Test System Calibration. See Method 320 of this 
appendix, sections 8.6.1 through 8.6.2 for direction in performing 
system calibration.
    8.6  Sampling.
    8.6.1  Extractive System. An extractive system maintained at 180 
 deg.C (360  deg.F) or higher which is capable of directing a total 
flow of at least 12 L/min to the sample cell is required (References 
1 and 2). Insert the probe into the duct or stack at a point 
representing the average volumetric flow rate and 25 percent of the 
cross sectional area. Co-locate an appropriate flow monitoring 
device with the sample probe so that the flow rate is recorded at 
specified time intervals during emission testing (e.g., differential 
pressure measurements taken every 10 minutes during each run).
    8.6.2  Batch Samples. Evacuate the absorbance cell to 5 Torr (or 
less) absolute pressure before taking first sample. Fill the cell 
with kiln gas to ambient pressure and record the infrared spectrum, 
then evacuate the cell until there is no further evidence of 
infrared absorption. Repeat this procedure, collecting a total of 
six separate sample spectra within a 1-hour period.
    8.6.3  Continuous Flow Through Sampling. Purge the FTIR cell 
with kiln gas for a time period sufficient to equilibrate the entire 
sampling system and FTIR gas cell. The time required is a function 
of the mechanical response time of the system (determined by 
performing the system calibration with the CTS gas or equivalent), 
and by the chemical reactivity of the target analytes. If the 
effluent target analyte concentration is not variable, observation 
of the spectral up-date of the flowing gas sample should be 
performed until equilibration of the sample is achieved. Isolate the 
gas cell from the sample flow by directing the purge flow to vent. 
Record the spectrum and pressure of the sample gas. After spectral 
acquisition, allow the sample gas to purge the cell with at least 
three volumes of kiln gas. The time required to adequately purge the 
cell with the required volume of gas is a function of (1) cell 
volume, (2) flow rate through the cell, and (3) cell design. It is 
important that the gas introduction and vent for the FTIR cell 
provides a complete purge through the cell.
    8.6.4  Continuous Sampling. In some cases it is possible to 
collect spectra continuously while the FTIR cell is purged with 
sample gas. The sample integration time, tss, the sample 
flow rate through the gas cell, and the sample integration time must 
be chosen so that the collected data consist of at least 10 spectra 
with each spectrum being of a separate cell volume of flue gas. 
Sampling in this manner may only be performed if the native source 
analyte concentrations do not affect the test results.
    8.7  Sample Conditioning
    8.7.1  High Moisture Sampling. Kiln gas emitted from wet process 
cement kilns may contain 3- to 40 percent moisture. Zinc selenide 
windows or the equivalent should be used when attempting to analyze 
hot/wet kiln gas under these conditions to prevent dissolution of 
water soluble window materials (e.g., KBr).
    8.7.2  Sample Dilution. The sample may be diluted using an in-
stack dilution probe, or an external dilution device provided that 
the sample is not diluted below the instrument's quantification 
range. As an alternative to using a dilution probe, nitrogen may be 
dynamically spiked into the effluent stream in the same manner as 
analyte spiking. A constant dilution rate shall be maintained 
throughout the measurement process. It is critical to measure and 
verify the exact dilution ratio when using a dilution probe or the 
nitrogen spiking approach. Calibrating the system with a calibration 
gas containing an appropriate tracer compound will allow 
determination of the dilution ratio for most measurement systems. 
The tester shall specify the procedures used to determine the 
dilution ratio, and include these calibration results in the report.
    8.8  Sampling QA, Data Storage and Reporting. See the FTIR 
Protocol. Sample integration times shall be sufficient to achieve 
the required signal-to-noise ratio, and all sample spectra should 
have unique file names. Two copies of sample interferograms and 
processed spectra will be stored on separate computer media. For 
each sample spectrum the analyst must document the sampling 
conditions, the sampling time (while the cell was being filled), the 
time the spectrum was recorded, the instrumental conditions (path 
length, temperature, pressure, resolution, integration time), and 
the spectral file name. A hard copy of these data must be maintained 
until the test results are accepted.
    8.9   Signal Transmittance. Monitor the signal transmittance 
through the instrumental system. If signal transmittance (relative 
to the background) drops below 95 percent in any spectral region 
where the sample does not absorb infrared energy, then a new 
background spectrum must be obtained.
    8.10  Post-test CTS. After the sampling run completion, record 
the CTS spectrum. Analysis of the spectral band area used for 
quantification from pre-and post-test CTS spectra should agree to 
within 5 percent or corrective action must be taken.
    8.11  Post-test QA. The sample spectra shall be inspected 
immediately after the run to verify that the gas matrix composition 
was close to the assumed gas matrix, (this is necessary to account 
for the concentrations of the interferants for use in the analytical 
analysis programs), and to confirm that the sampling and 
instrumental parameters were appropriate for the conditions 
encountered.

9.0  Quality Control

    Use analyte spiking to verify the effectiveness of the sampling 
system for the target compounds in the actual kiln gas matrix. QA 
spiking shall be performed before and after each sample run. QA 
spiking shall be performed after the pre-and post-test CTS direct 
and system calibrations. The system biases calculated from the pre-
and post-test dynamic analyte spiking shall be within 30 
percent for the spiked surrogate analytes for the measurements to be 
considered valid. See sections 9.3.1 through 9.3.2 for the requisite 
calculations. Measurement of the undiluted spike (direct-to-cell 
measurement) involves sending dry, spike gas to the FTIR cell, 
filling the cell to 1 atmosphere and obtaining the spectrum of this 
sample. The direct-to-cell measurement should be performed before 
each analyte spike so that the recovery of the dynamically spiked 
analytes may be calculated. Analyte spiking is only effective for 
assessing the integrity of the sampling system when the 
concentration of HCl in the source does not vary substantially. Any 
attempt to quantify an analyte recovery in a variable concentration 
matrix will result in errors in the expected concentration of the 
spiked sample. If the kiln gas target analyte concentrations vary by 
more than 5 percent (or 5 ppm, whichever is greater) in 
the time required to acquire a sample spectrum, it may be necessary 
to: (1) use a dual sample probe approach, (2) use two independent 
FTIR measurement systems, (3) use alternate QA/QC procedures, or (4) 
postpone testing until stable emission concentrations are achieved. 
(See section 9.2.3 of this method).

[[Page 14240]]

It is recommended that a laboratory evaluation be performed before 
attempting to employ this method under actual field conditions. The 
laboratory evaluation shall include (1) performance of all 
applicable calculations in section 4 of the FTIR Protocol; (2) 
simulated analyte spiking experiments in dry (ambient) and 
humidified sample matrices using HCl; and (3) performance of bias 
(recovery) calculations from analyte spiking experiments. It is not 
necessary to perform a laboratory evaluation before every field 
test. The purpose of the laboratory study is to demonstrate that the 
actual instrument and sampling system configuration used in field 
testing meets the requirements set forth in this method.
    9.1  Spike Materials. Perform analyte spiking with an HCl 
standard to demonstrate the integrity of the sampling system.
    9.1.1  An HCl standard of approximately 50 ppm in a balance of 
ultra pure nitrogen is recommended. The SF6 (tracer) 
concentration shall be 2 to 5 ppm depending upon the measurement 
pathlength. The spike ratio (spike flow/total flow) shall be no 
greater than 1:10, and an ideal spike concentration should 
approximate the native effluent concentration.
    9.1.2  The ideal spike concentration may not be achieved because 
the target concentration cannot be accurately predicted prior to the 
field test, and limited calibration standards will be available 
during testing. Therefore, practical constraints must be applied 
that allow the tester to spike at an anticipated concentration. For 
these tests, the analyte concentration contributed by the HCl 
standard spike should be 1 to 5 ppm or should more closely 
approximate the native concentration if it is greater.

9.2  Spike Procedure

    9.2.1  A spiking/sampling apparatus is shown in Figure 2. 
Introduce the spike/tracer gas mixture at a constant flow 
(2 percent) rate at approximately 10 percent of the 
total sample flow. (For example, introduce the surrogate spike at 1 
L/min 20 cc/min, into a total sample flow rate of 10 L/
min). The spike must be pre-heated before introduction into the 
sample matrix to prevent a localized condensation of the gas stream 
at the spike introduction point. A heated sample transport line(s) 
containing multiple transport tubes within the heated bundle may be 
used to spike gas up through the sampling system to the spike 
introduction point. Use a calibrated flow device (e.g., mass flow 
meter/controller), to monitor the spike flow as indicated by a 
calibrated flow meter or controller, or alternately, the 
SF6 tracer ratio may be calculated from the direct 
measurement and the diluted measurement. It is often desirable to 
use the tracer approach in calculating the spike/total flow ratio 
because of the difficulty in accurately measuring hot/wet total 
flow. The tracer technique has been successfully used in past 
validation efforts (Reference 1).
    9.2.2  Perform a direct-to-cell measurement of the dry, 
undiluted spike gas. Introduce the spike directly to the FTIR cell, 
bypassing the sampling system. Fill cell to 1 atmosphere and collect 
the spectrum of this sample. Ensure that the spike gas has 
equilibrated to the temperature of the measurement cell before 
acquisition of the spectra. Inspect the spectrum and verify that the 
gas is dry and contains negligible CO2. Repeat the 
process to obtain a second direct-to-cell measurement. Analysis of 
spectral band areas for HCl from these duplicate measurements should 
agree to within 5 percent of the mean.
    9.2.3  Analyte Spiking. Determine whether the kiln gas contains 
native concentrations of HCl by examination of preliminary spectra. 
Determine whether the concentration varies significantly with time 
by observing a continuously up-dated spectrum of sample gas in the 
flow-through sampling mode. If the concentration varies by more than 
5 percent during the period of time required to acquire 
a spectra, then an alternate approach should be used. One alternate 
approach uses two sampling lines to convey sample to the gas 
distribution manifold. One of the sample lines is used to 
continuously extract unspiked kiln gas from the source. The other 
sample line serves as the analyte spike line. One FTIR system can be 
used in this arrangement. Spiked or unspiked sample gas may be 
directed to the FTIR system from the gas distribution manifold, with 
the need to purge only the components between the manifold and the 
FTIR system. This approach minimizes the time required to acquire an 
equilibrated sample of spiked or unspiked kiln gas. If the source 
varies by more than 5 percent (or 5 ppm, whichever is 
greater) in the time it takes to switch from the unspiked sample 
line to the spiked sample line, then analyte spiking may not be a 
feasible means to determine the effectiveness of the sampling system 
for the HCl in the sample matrix. A second alternative is to use two 
completely independent FTIR measurement systems. One system would 
measure unspiked samples while the other system would measure the 
spiked samples. As a last option, (where no other alternatives can 
be used) a humidified nitrogen stream may be generated in the field 
which approximates the moisture content of the kiln gas. Analyte 
spiking into this humidified stream can be employed to assure that 
the sampling system is adequate for transporting the HCl to the FTIR 
instrumentation.
    9.2.3.1  Adjust the spike flow rate to approximately 10 percent 
of the total flow by metering spike gas through a calibrated mass 
flowmeter or controller. Allow spike flow to equilibrate within the 
sampling system before analyzing the first spiked kiln gas samples. 
A minimum of two consecutive spikes are required. Analysis of the 
spectral band area used for quantification should agree to within 
5 percent or corrective action must be taken.
    9.2.3.2  After QA spiking is completed, the sampling system 
components shall be purged with nitrogen or dry air to eliminate 
traces of the HCl compound from the sampling system components. 
Acquire a sample spectra of the nitrogen purge to verify the absence 
of the calibration mixture.
    9.2.3.3  Analyte spiking procedures must be carefully executed 
to ensure that meaningful measurements are achieved. The 
requirements of sections 9.2.3.3.1 through 9.2.3.3.4 shall be met.
    9.2.3.3.1  The spike must be in the vapor phase, dry, and heated 
to (or above) the kiln gas temperature before it is introduced to 
the kiln gas stream.
    9.2.3.3.2  The spike flow rate must be constant and accurately 
measured.
    9.2.3.3.3  The total flow must also be measured continuously and 
reliably or the dilution ratio must otherwise be verified before and 
after a run by introducing a spike of a non-reactive, stable 
compound (i.e., tracer).
    9.2.3.3.4  The tracer must be inert to the sampling system 
components, not contained in the effluent gas, and readily detected 
by the analytical instrumentation. Sulfur hexafluoride 
(SF6) has been used successfully (References 1 and 2) for 
this purpose.

9.3  Calculations

    9.3.1  Recovery. Calculate the percent recovery of the spiked 
analytes using equations 1 and 2.

%R = (Sm/Ce)  x  100  (Eq. 321-1).
Sm = Mean concentration of the analyte spiked effluent 
samples (observed).
Ce = Expected concentration of the spiked samples 
(theoretical).
Ce = DfCs + Su (1-
Df)   (Eq. 321-2)
Df = dilution Factor (Spike flow/Total flow). total flow 
= spike flow plus effluent flow.
Cs = cylinder concentration of spike gas.
Su = native concentration of analytes in unspiked 
samples.

    The spike dilution factor may be confirmed by measuring the 
total flow and the spike flow directly. Alternately, the spike 
dilution can be verified by comparing the concentration of the 
tracer compound in the spiked samples (diluted) to the tracer 
concentration in the direct (undiluted) measurement of the spike 
gas.
    If SF6 is the tracer gas, then

Df = [SF6]spike/ 
[SF6]direct  (Eq. 321-3)
[SF6]spike = the diluted SF6 concentration 
measured in a spiked sample.
[SF6]direct = the SF6 concentration 
measured directly.

    9.3.2   Bias. The bias may be determined by the difference 
between the observed spike value and the expected response (i.e., 
the equivalent concentration of the spiked material plus the analyte 
concentration adjusted for spike dilution). Bias is defined by 
section 6.3.1 of EPA Method 301 of this (Reference 8) as,

B = Sm -- Ce  (Eq. 321-4)

 where:

B = Bias at spike level.
Sm = Mean concentration of the analyte spiked samples.
Ce = Expected concentration of the analyte in spiked 
samples.

    Acceptable recoveries for analyte spiking are 30 
percent. Application of correction factors to the data based upon 
bias and recovery calculations is subject to the approval of the 
Administrator.

10.0  Calibration and Standardization

    10.1  Calibration transfer standards (CTS). The EPA Traceability 
Protocol gases or NIST traceable standards, with a minimum accuracy 
of 2 percent shall be used. For

[[Page 14241]]

other requirements of the CTS, see the FTIR Protocol section 4.5.
    10.2  Signal-to-Noise Ratio (S/N). The S/N shall be less than 
the minimum acceptable measurement uncertainty in the analytical 
regions to be used for measuring HCl.
    10.3  Absorbance Pathlength. Verify the absorbance path length 
by comparing CTS spectra to reference spectra of the calibration 
gas(es).
    10.4  Instrument Resolution. Measure the line width of 
appropriate CTS band(s) to verify instrumental resolution.
    10.5  Apodization Function. Choose the appropriate apodization 
function. Determine any appropriate mathematical transformations 
that are required to correct instrumental errors by measuring the 
CTS. Any mathematical transformations must be documented and 
reproducible. Reference 9 provides additional information about FTIR 
instrumentation.

11.0  Analytical Procedure

    A full description of the analytical procedures is given in 
sections 4.6--4.11, sections 5, 6, and 7, and the appendices of the 
FTIR Protocol. Additional description of quantitative spectral 
analysis is provided in References 10 and 11.

12.0  Data Analysis and Calculations

    Data analysis is performed using appropriate reference spectra 
whose concentrations can be verified using CTS spectra. Various 
analytical programs (References 10 and 11) are available to relate 
sample absorbance to a concentration standard. Calculated 
concentrations should be verified by analyzing spectral baselines 
after mathematically subtracting scaled reference spectra from the 
sample spectra. A full description of the data analysis and 
calculations may be found in the FTIR Protocol (sections 4.0, 5.0, 
6.0 and appendices).
    12.1  Calculated concentrations in sample spectra are corrected 
for differences in absorption pathlength between the reference and 
sample spectra by
Ccorr = (Lr/Ls)  x  (Ts/
Tr)  x  (Ccalc)  (Eq. 321-5)

Where:

Ccorr = The pathlength corrected concentration.
Ccalc = The initial calculated concentration (output of 
the multicomponent analysis program designed for the compound).
Lr = The pathlength associated with the reference 
spectra.
Ls = The pathlength associated with the sample spectra.
Ts = The absolute temperature (K) of the sample gas.
Tr = The absolute temperature (K) at which reference 
spectra were recorded.

    12.2  The temperature correction in equation 5 is a volumetric 
correction. It does not account for temperature dependence of 
rotational-vibrational relative line intensities. Whenever possible, 
the reference spectra used in the analysis should be collected at a 
temperature near the temperature of the FTIR cell used in the test 
to minimize the calculated error in the measurement (FTIR Protocol, 
appendix D). Additionally, the analytical region chosen for the 
analysis should be sufficiently broad to minimize errors caused by 
small differences in relative line intensities between reference 
spectra and the sample spectra.

13.0  Method Performance

    A description of the method performance may be found in the FTIR 
Protocol. This method is self validating provided the results meet 
the performance specification of the QA spike in sections 9.0 
through 9.3 of this method.

14.0  Pollution Prevention

    This is a gas phase measurement. Gas is extracted from the 
source, analyzed by the instrumentation, and discharged through the 
instrument vent.

15.0  Waste Management

    Gas standards of HCl are handled according to the instructions 
enclosed with the material safety data sheet.

16.0 References

    1.  ``Laboratory and Field Evaluation of a Methodology for 
Determination of Hydrogen Chloride Emissions From Municipal and 
Hazardous Waste Incinerators,'' S. C. Steinsberger and J. H. 
Margeson. Prepared for U.S. Environmental Protection Agency, 
Research Triangle Park, NC. NTIS Report No. PB89-220586. (1989).
    2. ``Evaluation of HCl Measurement Techniques at Municipal and 
Hazardous Waste Incinerators,'' S.A. Shanklin, S.C. Steinsberger, 
and L. Cone, Entropy, Inc. Prepared for U.S. Environmental 
Protection Agency, Research Triangle Park, NC. NTIS Report No. PB90-
221896. (1989).
    3. ``Fourier Transform Infrared (FTIR) Method Validation at a 
Coal Fired-Boiler,'' Entropy, Inc. Prepared for U.S. Environmental 
Protection Agency, Research Triangle Park, NC. EPA Publication No. 
EPA-454/R95-004. NTIS Report No. PB95-193199. (1993).
    4. ``Field Validation Test Using Fourier Transform Infrared 
(FTIR) Spectrometry To Measure Formaldehyde, Phenol and Methanol at 
a Wool Fiberglass Production Facility.'' Draft. U.S. Environmental 
Protection Agency Report, Entropy, Inc., EPA Contract No. 68D20163, 
Work Assignment I-32.
    5. Kinner, L.L., Geyer, T.G., Plummer, G.W., Dunder, T.A., 
Entropy, Inc. ``Application of FTIR as a Continuous Emission 
Monitoring System.'' Presentation at 1994 International Incineration 
Conference, Houston, Tx. May 10, 1994.
    6. ``Molecular Vibrations; The Theory of Infrared and Raman 
Vibrational Spectra,'' E. Bright Wilson, J.C. Decius, and P.C. 
Cross, Dover Publications, Inc., 1980. For a less intensive 
treatment of molecular rotational-vibrational spectra see, for 
example, ``Physical Chemistry,'' G.M. Barrow, chapters 12, 13, and 
14, McGraw Hill, Inc., 1979.
    7. ``Laboratory and Field Evaluations of Ammonium Chloride 
Interference in Method 26,'' U.S. Environmental Protection Agency 
Report, Entropy, Inc., EPA Contract No. 68D20163, Work Assignment 
No. I-45.
    8. 40 CFR 63, A. Method 301--Field Validation of Pollutant 
Measurement Methods from Various Waste Media.
    9. ``Fourier Transform Infrared Spectrometry,'' Peter R. 
Griffiths and James de Haseth, Chemical Analysis, 83, 16-25,(1986), 
P.J. Elving, J.D. Winefordner and I.M. Kolthoff (ed.), John Wiley 
and Sons.
    10. ``Computer-Assisted Quantitative Infrared Spectroscopy,'' 
Gregory L. McClure (ed.), ASTM Special Publication 934 (ASTM), 1987.
    11. ``Multivariate Least-Squares Methods Applied to the 
Quantitative Spectral Analysis of Multicomponent Mixtures,'' Applied 
Spectroscopy, 39(10), 73-84, 1985.

BILLING CODE 6560-50-P

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[GRAPHIC] [TIFF OMITTED] TP24MR98.002



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Method 322--Measurement of Hydrogen Chloride Emissions From Portland 
Cement Kilns by GFCIR

1.0  Applicability and Principle

    1.1  Applicability. This method is applicable to the 
determination of hydrogen chloride (HCl) concentrations in emissions 
from portland cement kilns. This is an instrumental method for the 
measurement of HCl using an extractive sampling system and an 
infrared (IR) gas-filter correlation (GFC) analyzer. This method is 
intended to provide the cement industry with a direct interface 
instrumental method. A procedure for analyte spiking is included for 
quality assurance. This method is considered to be self-validating 
provided that the requirements in section 9 of this method are 
followed.
    1.2  Principle. A gas sample is continuously extracted from a 
stack or duct over the test period using either a source-level hot/
wet extractive subsystem or a dilution extractive subsystem. A 
nondispersive infrared gas filter correlation (NDIR-GFC) analyzer is 
specified for the measurement of HCl in the sample. The total 
measurement system is comprised of the extractive subsystem, the 
analyzer, and the data acquisition subsystem. Test system 
performance specifications are included in this method to provide 
for the collection of accurate, reproducible data.
    1.3  Test System Operating Range. The measurement range (span) 
of the test system shall include the anticipated HCl concentrations 
of the effluent and spiked samples. The range should be selected so 
that the average of the effluent measurements is between 25 and 75 
percent of span. If at any time during a test run, the effluent 
concentration exceeds the span value of the test system, the run 
shall be considered invalid.

2.0  Summary of Method

    2.1  Sampling and Analysis. Kiln gas is continuously extracted 
from the stack or duct using either a source level, hot/wet 
extractive system, or an in-situ dilution probe or heated out-of-
stack dilution system. The sample is then directed by a heated 
sample line maintained above 350  deg.F to a GFC analyzer having a 
range appropriate to the type of sampling system. The gas filter 
correlation analyzer incorporates a gas cell filled with HCl. This 
gas cell is periodically moved into the path of an infrared 
measurement beam of the instrument to filter out essentially all of 
the HCl absorption wavelengths. Spectral filtering provides a 
reference from which the HCl concentration of the sample can be 
determined. Interferences are minimized in the analyzer by choosing 
a spectral band over which compounds such as CO2 and 
H2O either do not absorb significantly or do not match 
the spectral pattern of the HCl infrared absorption.
    2.2  Operator Requirements. The analyst must be familiar with 
the specifications and test procedures of this method and follow 
them in order to obtain reproducible and accurate data.

3.0  Definitions

    3.1  Measurement System. The total equipment required for the 
determination of gas concentration. The measurement system consists 
of the following major subsystems:
    3.1.1  Sample Interface. That portion of a system used for one 
or more of the following: sample acquisition, sample transport, 
sample conditioning, or protection of the analyzers from the effects 
of the stack gas.
    3.1.2  Gas Analyzer. That portion of the system that senses the 
gas to be measured and generates an output proportional to its 
concentration.
    3.1.3  Data Recorder. A strip chart recorder, analog computer, 
or digital recorder for recording measurement data from the analyzer 
output.
    3.2  Span. The upper limit of the gas concentration measurement 
range displayed on the data recorder.
    3.3  Calibration Gas. A known concentration of a gas in an 
appropriate diluent gas (i.e., N2).
    3.4  Analyzer Calibration Error. The difference between the gas 
concentration exhibited by the gas analyzer and the known 
concentration of the calibration gas when the calibration gas is 
introduced directly to the analyzer.
    3.5  Sampling System Bias. The sampling system bias is the 
difference between the gas concentrations exhibited by the 
measurement system when a known concentration gas is introduced at 
the outlet of the sampling probe and the known value of the 
calibration gas.
    3.6  Response Time. The amount of time required for the 
measurement system to display 95 percent of a step change in gas 
concentration on the data recorder.
    3.7  Calibration Curve. A graph or other systematic method of 
establishing the relationship between the analyzer response and the 
actual gas concentration introduced to the analyzer.
    3.8  Linearity. The linear response of the analyzer or test 
system to known calibration inputs covering the concentration range 
of the system.
    3.9  Interference Rejection. The ability of the system to reject 
the effect of interferences in the analytical measurement processes 
of the test system.

4.0  Interferences

    4.1  Sampling System Interferences. An important consideration 
in measuring HCl using an extractive measurement system is to ensure 
that a representative kiln gas sample is delivered to the gas 
analyzer. A sampling system interferant is a factor that inhibits an 
analyte from reaching the analytical instrumentation. Condensed 
water vapor is a strong sampling system interferant for HCl and 
other water soluble compounds. ``Cold spots'' in the sampling system 
can allow water vapor in the sample to condense resulting in removal 
of HCl from the sample stream. The extent of HCl sampling system 
bias depends on concentrations of potential interferants, moisture 
content of the gas stream, temperature of the gas stream, 
temperature of sampling system components, sample flow rate, and 
reactivity of HCl with other species in the gas stream. For 
measuring HCl in a wet gas stream, the temperatures of the gas 
stream and sampling system components and the sample flow rate are 
of primary importance. In order to prevent problems with 
condensation in the sampling system, these parameters must be 
closely monitored.
    4.1.1  System Calibration Checks. Performing these calibration 
checks where HCl calibration gas is injected through the entire 
system both before and after each test run demonstrates the 
integrity of the sampling system and capability of the analyzer for 
measuring this water soluble and otherwise unstable compound under 
ideal conditions (i.e., HCl in N2).
    4.1.2  Analyte Spiking Checks. For analyte spiking checks, HCl 
calibration gas is quantitatively added to the sample stream at a 
point upstream of the particulate filter and all other sample 
handling components both before and after each test run. The volume 
of HCl spike gas should not exceed 10 percent of the total sample 
volume so that the sample matrix is relatively unaffected. 
Successfully performing these checks demonstrates the integrity of 
the sampling system for measuring this water soluble and reactive 
compound under actual sample matrix conditions. Successfully 
performing these checks also demonstrates the adequacy of the 
interference rejection capability of the analyzer. (See section 9.3 
of this method.)
    4.2  Analytical Interferences. Analytical interferences are 
reduced by the GFC spectroscopic technique required by the method. 
The accuracy of HCl measurements provided by some GFC analyzers is 
known to be sensitive to the moisture content of the sample. This 
must be taken into account in order to acquire accurate results. 
These analyzers must be calibrated for the specific moisture content 
of the samples.

5.0  Safety

    This method may involve sampling at locations having high 
positive or negative pressures, or high concentrations of hazardous 
or toxic pollutants, and cannot address all safety problems 
encountered under these diverse sampling conditions. It is the 
responsibility of the tester(s) to ensure proper safety and health 
practices, and to determine the applicability of regulatory 
limitations before performing this test method. Because HCl is a 
respiratory irritant, it is advisable to limit exposure to this 
compound.

6.0  Equipment and Supplies.

    (Note: Mention of company or product names does not constitute 
endorsement by the U. S. Environmental Protection Agency.)

    6.1  Measurement System. Use any GFC measurement system for HCl 
that meets the specifications of this method. All sampling system 
components must be maintained above the kiln gas temperature, when 
possible, or at least 350  deg.F. The length of sample transport 
line should be minimized and sampling rate should be as high as 
possible to minimize adsorption of HCl. The essential components of 
the measurement system are described in sections 6.1.1 through 
6.1.12.
    6.1.1   Sample Probe. Glass, stainless steel, Hastalloy 
TM, or equivalent, of sufficient

[[Page 14245]]

length to traverse the sample points. The sampling probe shall be 
heated to a minimum of 350  deg.F to prevent condensation. Dilution 
extractive systems must use a dilution ratio such that the average 
diluted concentrations are between 25 to 75 percent of the selected 
measurement range of the analyzer.
    6.1.2  Calibration Valve Assembly. Use a heated, three-way valve 
assembly, or equivalent, for selecting either sample gas or 
introducing calibration gases to the measurement system or 
introducing analyte spikes into the measurement system at the outlet 
of the sampling probe before the primary particulate filter.
    6.1.3  Particulate Filter. A coarse filter or other device may 
be placed at the inlet of the probe for removal of large particulate 
(10 microns or greater). A heated (Balston or 
equivalent) filter rated at 1 micron is necessary for primary 
particulate removal, and shall be placed immediately after the 
heated probe. The filter/filter holder shall be maintained at 350 
deg.F or a higher temperature. Additional filters at the inlet of 
the gas analyzer may be used to prevent accumulation of particulate 
material in the measurement system and extend the useful life of 
components. All filters shall be fabricated of materials that are 
nonreactive with HCl. Some types of glass filters are known to react 
with HCl.
    6.1.4  Sample Transport Lines. Stainless steel or 
polytetrafluoroethylene (PTFE) tubing shall be heated to a minimum 
temperature of 350  deg.F (sufficient to prevent condensation and to 
prevent HCl and NH3 from combining into ammonium chloride 
in the sampling system) to transport the sample gas to the gas 
analyzer.
    6.1.5  Sample Pump. Use a leak-free pump to pull the sample gas 
through the system at a flow rate sufficient to minimize the 
response time of the measurement system. The pump components that 
contact the sample must be heated to a temperature greater than 350 
deg.F and must be constructed of a material that is nonreactive to 
HCl.
    6.1.6  Sample Flow Rate Control. A sample flow rate control 
valve and rotameter, or equivalent, must be used to maintain a 
constant sampling rate within 10 percent. These 
components must be heated to a temperature greater than 350  deg.F. 
(Note: The tester may elect to install a back-pressure regulator to 
maintain the sample gas manifold at a constant pressure in order to 
protect the analyzer(s) from over-pressurization, and to minimize 
the need for flow rate adjustments.)
    6.1.7  Sample Gas Manifold. A sample gas manifold, heated to a 
minimum of 350  deg.F, is used to divert a portion of the sample gas 
stream to the analyzer and the remainder to the by-pass discharge 
vent. The sample gas manifold should also include provisions for 
introducing calibration gases directly to the analyzer. The manifold 
must be constructed of material that is nonreactive to the gas being 
sampled.
    6.1.8  Gas Analyzer. Use a nondispersive infrared analyzer 
utilizing the gas filter correlation technique to determine HCl 
concentrations. The analyzer shall meet the applicable performance 
specifications of section 8.0 of this method. (Note: Housing the 
analyzer in a clean, thermally-stable, vibration free environment 
will minimize drift in the analyzer calibration.) The analyzer 
(system) shall be designed so that the response of a known 
calibration input shall not deviate by more than 3 
percent from the expected value. The analyzer or measurement system 
manufacturer may provide documentation that the instrument meets 
this design requirement. Alternatively, a known concentration gas 
standard and calibration dilution system meeting the requirements of 
Method 205 of appendix M to part 51 of this chapter, ``Verification 
of Gas Dilution Systems for Field Calibrations'' (or equivalent 
procedure), may be used to develop a multi-point calibration curve 
over the measurement range of the analyzer.
    6.1.9  Gas Regulators. Single stage regulator with cross purge 
assembly that is used to purge the CGA fitting and regulator before 
and after use. (This purge is necessary to clear the calibration gas 
delivery system of ambient water vapor after the initial connection 
is made, or after cylinder changeover, and will extend the life of 
the regulator.) Wetted parts are 316 stainless steel to handle 
corrosive gases.
    6.1.10  Data Recorder. A strip chart recorder, analog computer, 
or digital recorder, for recording measurement data. The data 
recorder resolution (i.e., readability) shall be 0.5 percent of 
span. Alternatively, a digital or analog meter having a resolution 
of 0.5 percent of span may be used to obtain the analyzer responses 
and the readings may be recorded manually. If this alternative is 
used, the readings shall be obtained at equally-spaced intervals 
over the duration of the sampling run. For sampling run durations of 
less than 1 hour, measurements at 1-minute intervals or a minimum of 
30 measurements, whichever is less restrictive, shall be obtained. 
For sampling run durations greater than 1 hour, measurements at 2-
minute intervals or a minimum of 96 measurements, whichever is less 
restrictive, shall be obtained.
    6.1.11  Mass Flow Meters/Controllers. A mass flow meter having 
the appropriate calibrated range and a stated accuracy of 
2 percent of the measurement range is used to measure 
the HCl spike flow rate. This device must be calibrated with the 
major component of the calibration spike gas (e.g., nitrogen) using 
an NIST traceable bubble meter or equivalent. When spiking HCl, the 
mass flow meter/controller should be thoroughly purged before and 
after introduction of the gas to prevent corrosion of the interior 
parts.
    6.1.12  System Flow Measurement. A measurement device or 
procedure to determine the total flow rate of sample gas within the 
measurement system. A rotameter, or mass flow meter calibrated 
relative to a laboratory standard to within 2 percent of 
the measurement value at the actual operating temperature, moisture 
content, and sample composition (molecular weight) is acceptable. A 
system which ensures that the total sample flow rate is constant 
within 2 percent and which relies on an intermittent 
measurement of the actual flow rate (e.g., calibrated gas meter) is 
also acceptable.
    6.2  HCl Calibration Gases. The calibration gases for the gas 
analyzer shall be HCl in N2. Use at least three 
calibration gases as specified below:
    6.2.1  High-Range Gas. Concentration equivalent to 80 to 100 
percent of the span.
    6.2.2  Mid-Range Gas. Concentration equivalent to 40 to 60 
percent of the span.
    6.2.3  Zero Gas. Concentration of less than 0.25 percent of the 
span. Purified ambient air may be used for the zero gas by passing 
air through a charcoal filter or through one or more impingers 
containing a solution of 3 percent H2O2.
    6.2.4  Spike Gas. A calibration gas of known concentration 
(typically 100 to 200 ppm) used for analyte spikes in accordance 
with the requirements of section 9.3 of this method.

7.0  Reagents and Standards

    7.1   Hydrogen Chloride. Hydrogen Chloride is a reactive gas and 
is available in steel cylinders from various commercial gas vendors. 
The stability is such that it is not possible to purchase a cylinder 
mixture whose HCl concentration can be certified at better than 
5 percent. The stability of the cylinder may be 
monitored over time by periodically analyzing cylinder samples. The 
cylinder gas concentration must be verified within 1 month prior to 
the use of the calibration gas. Due to the relatively high 
uncertainty of HCl calibration gas values, difficulties may develop 
in meeting the performance specifications if the mid-range and high-
range calibration gases are not consistent with each other. Where 
problems are encountered, the consistency of the test gas standards 
may be determined: (1) By comparing analyzer responses for the test 
gases with the responses to additional certified calibration gas 
standards, (2) by reanalysis of the calibration gases in accordance 
with sections 7.2.1 or 7.2.2 of this method, or (3) by other 
procedures subject to the approval of EPA.
    7.2  Calibration Gas Concentration Verification. There are two 
alternatives for establishing the concentrations of calibration 
gases. Alternative No. 1 is preferred.
    7.2.1  Alternative No. 1. The value of the calibration gases may 
be obtained from the vendor's certified analysis within 1 month 
prior to the test. Obtain a certification from the gas manufacturer 
that identifies the analytical procedures and date of certification.
    7.2.2  Alternative No. 2. Perform triplicate analyses of the 
gases using Method 26 of A to part 60 of this chapter. Obtain gas 
mixtures with a manufacturer's tolerance not to exceed 5 
percent of the tag value. Within 1 month of the field test, analyze 
each of the calibration gases in triplicate using Method 26 of 
appendix A to part 60 of this chapter. The tester must follow all of 
the procedures in Method 26 (e.g., use midget impingers, heated 
Pallflex TX40H175 filter (TFE-glass mat), etc. if this analysis is 
performed. Citation 3 in section 13 of this method describes 
procedures and techniques that may be used for this analysis. Record 
the results on a data sheet. Each of the individual HCl analytical 
results for each calibration gas shall be within 5 percent (or 5 
ppm, whichever is greater) of the triplicate set average; otherwise, 
discard the entire set and

[[Page 14246]]

repeat the triplicate analyses. If the average of the triplicate 
analyses is within 5 percent of the calibration gas manufacturer's 
cylinder tag value, use the tag value; otherwise, conduct at least 
three additional analyses until the results of six consecutive runs 
agree within 5 percent (or 5 ppm, whichever is greater) of the 
average. Then use this average for the cylinder value.
    7.3  Calibration Gas Dilution Systems. Sample flow rates of 
approximately 15 L/min are typical for extractive HCl measurement 
systems. These flow rates coupled with response times of 15 to 30 
minutes will result in consumption of large quantities of 
calibration gases. The number of cylinders and amount of calibration 
gas can be reduced by the use of a calibration gas dilution system 
in accordance with Method 205 of appendix M to part 51 of this 
chapter, ``Verification of Gas Dilution Systems for Field Instrument 
Calibrations.'' If this option is used, the tester shall also 
introduce an undiluted calibration gas approximating the effluent 
HCl concentration during the initial calibration error test of the 
measurement system as a quality assurance check.

8.0  Test System Performance Specifications

    8.1  Analyzer Calibration Error. This error shall be less than 
5 percent of the emission standard concentration or 
1 ppm, (whichever is greater) for zero, mid-, and high-
range gases.
    8.2  Sampling System Bias. This bias shall be less than 
7.5 percent of the emission standard concentration or 
1.5 ppm (whichever is greater) for zero and mid-range 
gases.
    8.3  Analyte Spike Recovery. This recovery shall be between 70 
to 130 percent of the expected concentration of spiked samples 
calculated with the average of the before and after run spikes.

9.0  Sample Collection, Preservation, and Storage

    9.1  Pretest. Perform the procedures of sections 9.1.1 through 
9.1.3.3 of this method before measurement of emissions (procedures 
in section 9.2 of this method). It is important to note that after a 
regulator is placed on an HCl gas cylinder valve, the regulator 
should be purged with dry N2 or dry compressed air for approximately 
10 minutes before initiating any HCl gas flow through the system. 
This purge is necessary to remove any ambient water vapor from 
within the regulator and calibration gas transport lines; the HCl in 
the calibration gas may react with this water vapor and increase 
system response time. A purge of the system should also be performed 
at the conclusion of a test day prior to removing the regulator from 
the gas cylinder. Although the regulator wetted parts are corrosion 
resistant, this will reduce the possibility of corrosion developing 
within the regulator and extend the life of the equipment.
    9.1.1  Measurement System Preparation. Assemble the measurement 
system by following the manufacturer's written instructions for 
preparing and preconditioning the gas analyzer and, as applicable, 
the other system components. Introduce the calibration gases in any 
sequence, and make all necessary adjustments to calibrate the 
analyzer and the data recorder. If necessary, adjust the instrument 
for the specific moisture content of the samples. Adjust system 
components to achieve correct sampling rates.
    9.1.2  Analyzer Calibration Error. Conduct the analyzer 
calibration error check in the field by introducing calibration 
gases to the measurement system at any point upstream of the gas 
analyzer in accordance with sections 9.1.2.1 and 9.1.2.2 of this 
method.
    9.1.2.1  After the measurement system has been prepared for use, 
introduce the zero, mid-range, and high-range gases to the analyzer. 
During this check, make no adjustments to the system except those 
necessary to achieve the correct calibration gas flow rate at the 
analyzer. Record the analyzer responses to each calibration gas. 
(Note: A calibration curve established prior to the analyzer 
calibration error check may be used to convert the analyzer response 
to the equivalent gas concentration introduced to the analyzer. 
However, the same correction procedure shall be used for all 
effluent and calibration measurements obtained during the test.
9.1.2.2  The analyzer calibration error check shall be considered 
invalid if the difference in gas concentration displayed by the 
analyzer and the concentration of the calibration gas exceeds 
5 percent of the emission standard concentration or 
1 ppm, (whichever is greater) for the zero, mid-, or 
high-range calibration gases. If an invalid calibration is 
exhibited, cross-check or recertify the calibration gases, take 
corrective action, and repeat the analyzer calibration error check 
until acceptable performance is achieved.
9.1.3  Sampling System Bias Check. For nondilution extractive 
systems, perform the sampling system bias check by introducing 
calibration gases either at the probe inlet or at a calibration 
valve installed at the outlet of the sampling probe. For dilution 
systems, calibration gases for both the analyzer calibration error 
check and the sampling system bias check must be introduced prior to 
the point of sample dilution. For dilution and nondilution systems, 
a zero gas and either a mid-range or high-range gas (whichever more 
closely approximates the effluent concentration) shall be used for 
the sampling system bias check.
    9.1.3.1  Introduce the upscale calibration gas, and record the 
gas concentration displayed by the analyzer. Then introduce zero 
gas, and record the gas concentration displayed by the analyzer. 
During the sampling system bias check, operate the system at the 
normal sampling rate, and make no adjustments to the measurement 
system other than those necessary to achieve proper calibration gas 
flow rates at the analyzer. Alternately introduce the zero and 
upscale gases until a stable response is achieved. The tester shall 
determine the measurement system response time by observing the 
times required to achieve a stable response for both the zero and 
upscale gases. Note the longer of the two times and note the time 
required for the measurement system to reach 95 percent of the step 
change in the effluent concentration as the response time.
    9.1.3.2  For nondilution systems, where the analyzer calibration 
error test is performed by introducing gases directly to the 
analyzer, the sampling system bias check shall be considered invalid 
if the difference between the gas concentrations displayed by the 
measurement system for the sampling system bias check and the known 
gas concentration standard exceeds 7.5 percent of the 
emission standard or 1.5 ppm, (whichever is greater) for 
either the zero or the upscale calibration gases. If an invalid 
calibration is exhibited, take corrective action, and repeat the 
sampling system bias check until acceptable performance is achieved. 
If adjustment to the analyzer is required, first repeat the analyzer 
calibration error check, then repeat the sampling system bias check.
    9.1.3.3  For dilution systems (and nondilution systems where all 
calibration gases are introduced at the probe), the comparison of 
the analyzer calibration error results and sampling system bias 
check results is not meaningful. For these systems, the sampling 
system bias check shall be considered invalid if the difference 
between the gas concentrations displayed by the analyzer and the 
actual gas concentrations exceed 7.5 percent of the 
emission standard or 1.5 ppm, (whichever is greater) for 
either the zero or the upscale calibration gases. If an invalid 
calibration is exhibited, take corrective action, and repeat the 
sampling system bias check until acceptable performance is achieved. 
If adjustment to the analyzer is required, first repeat the analyzer 
calibration error check.
    9.2  Emission Test Procedures
    9.2.1  Selection of Sampling Site and Sampling Points. Select a 
measurement site and sampling points using the same criteria that 
are applicable to Method 26 of A to part 60 of this chapter.
    9.2.2  Sample Collection. Position the sampling probe at the 
first measurement point, and begin sampling at the same rate as used 
during the sampling system bias check. Maintain constant rate 
sampling (i.e., 10 percent) during the entire run. Field 
test experience has shown that conditioning of the sample system is 
necessary for approximately 1-hour prior to conducting the first 
sample run. This conditioning period should be repeated after 
particulate filters are replaced and at the beginning of each new 
day or following any period when the sampling system is inoperative. 
Experience has also shown that prior to adequate conditioning of the 
system, the response to analyte spikes and/or the change from an 
upscale calibration gas to a representative effluent measurement may 
be delayed by more than twice the normal measurement system response 
time. It is recommended that the analyte spikes (see section 9.3 of 
this method) be performed to determine if the system is adequately 
conditioned. The sampling system is ready for use when the time 
required for the measurement system to equilibrate after a change 
from a representative effluent measurement to a representative 
spiked sample measurement approximates the calibration gas response 
time observed in section 9.1.3.1 of this method.

[[Page 14247]]

    9.2.3  Sample Duration. After completing the sampling system 
bias checks and analyte spikes prior to a test run, constant rate 
sampling of the effluent should begin. For each run, use only those 
measurements obtained after all residual response to calibration 
standards or spikes are eliminated and representative effluent 
measurements are displayed to determine the average effluent 
concentration. At a minimum, this requires that the response time of 
the measurement system has elapsed before data are recorded for 
calculation of the average effluent concentration. Sampling should 
be continuous for the duration of the test run. The length of data 
collection should be at least as long as required for sample 
collection by Method 26 of part 60 of this chapter. One hour 
sampling runs using this method have provided reliable data for 
cement kilns.
    9.2.4  Validation of Runs. Before and after each run, or if 
adjustments are necessary for the measurement system during the run, 
repeat the sampling system bias check procedure described in section 
9.1.3 of this method. (Make no adjustments to the measurement system 
until after the drift checks are completed.) Record the analyzer's 
responses.
    9.2.4.1  If the post-run sampling system bias for either the 
zero or upscale calibration gas exceeds the sampling system bias 
specification, then the run is considered invalid. Take corrective 
action, and repeat both the analyzer calibration error check 
procedure (section 9.1.2 of this method) and the sampling system 
bias check procedure (section 9.1.3 of this method) before repeating 
the run.
    9.2.4.2  If the post-run sampling system bias for both the zero 
and upscale calibration gas are within the sampling system bias 
specification, then construct two 2-point straight lines, one using 
the pre-run zero and upscale check values and the other using the 
post-run zero and upscale check values. Use the slopes and y-
intercepts of the two lines to calculate the gas concentration for 
the run in accordance with equation 1 of this method.
    9.3  Analyte Spiking--Self-Validating Procedure. Use analyte 
spiking to verify the effectiveness of the sampling system for the 
target compounds in the actual kiln gas matrix. Quality assurance 
(QA) spiking should be performed before and after each sample run. 
The spikes may be performed following the sampling system bias 
checks (zero and mid-range system calibrations) before each run in a 
series and also after the last run. The HCl spike recovery should be 
within 30 percent as calculated using equations 1 and 2 
of this method. Two general approaches are applicable for the use of 
analyte spiking to validate a GFC HCl measurement system: (1) Two 
independent measurement systems can be operated concurrently with 
analyte spikes introduced to one of the systems, or (2) a single 
measurement system can be used to analyze consecutively, spiked and 
unspiked samples in an alternating fashion. The two-system approach 
is similar to Method 301 of this appendix and the measurement bias 
is determined from the difference in the paired concurrent 
measurements relative to the amount of HCl spike added to the spiked 
system. The two-system approach must employ identical sampling 
systems and analyzers and both measurement systems should be 
calibrated using the same mid- and high-range calibration standards. 
The two-system approach should be largely unaffected by temporal 
variations in the effluent concentrations if both measurement 
systems achieve the same calibration responses and both systems have 
the same response times. (See Method 301 of this appendix for 
appropriate calculation procedures.) The single measurement system 
approach is applicable when the concentration of HCl in the source 
does not vary substantially during the period of the test. Since the 
approach depends on the comparison of consecutive spiked and 
unspiked samples, temporal variations in the effluent HCl 
concentrations will introduce errors in determining the expected 
concentration of the spiked samples. If the effluent HCl 
concentrations vary by more than 10 percent (or 
5 ppm, whichever is greater) during the time required to 
obtain and equilibrate a new sample (system response time), it may 
be necessary to: (1) Use a dual sampling system approach, (2) 
postpone testing until stable emission concentrations are achieved, 
(3) switch to the two-system approach [if possible] or, (4) rely on 
alternative QA/QC procedures. The dual-sampling system alternative 
uses two sampling lines to convey sample to the gas distribution 
manifold. One of the sample lines is used to continuously extract 
unspiked kiln gas from the source. The other sample line serves as 
the analyte spike line. One GFC analyzer can be used to alternately 
measure the HCl concentration from the two sampling systems with the 
need to purge only the components between the common manifold and 
the analyzer. This minimizes the time required to acquire an 
equilibrated sample of spiked or unspiked kiln gas. If the source 
varies by more than #10 percent or 5 ppm, 
(whichever is greater) during the time it takes to switch from the 
unspiked sample line to the spiked sample line, then the dual-
sampling system alternative approach is not applicable. As a last 
option, (where no other alternatives can be used) a humidified 
nitrogen stream may be generated in the field which approximates the 
moisture content of the kiln gas. Analyte spiking into this 
humidified stream can be employed to assure that the sampling system 
is adequate for transporting the HCl to the GFC analyzer and that 
the analyzer's water interference rejection is adequate.
    9.3.1  Spike Gas Concentration and Spike Ratio. The volume of 
HCl spike gas should not exceed 10 percent of the total sample 
volume (i.e., spike to total sample ratio of 1:10) to ensure that 
the sample matrix is relatively unaffected. An ideal spike 
concentration should approximate the native effluent concentration, 
thus the spiked sample concentrations would represent approximately 
twice the native effluent concentrations. The ideal spike 
concentration may not be achieved because the native HCl 
concentration cannot be accurately predicted prior to the field 
test, and limited calibration gas standards will be available during 
the field test. Some flexibility is available by varying the spike 
ratio over the range from 1:10 to 1:20. Practical constraints must 
be applied to allow the tester to spike at an anticipated 
concentration. Thus, the tester may use a 100 ppm calibration gas 
and a spike ratio of 1:10 as default values where information 
regarding the expected HCl effluent concentration is not available 
prior to the tests. Alternatively, the tester may select another 
calibration gas standard and/or lower spike ratio (e.g., 1:20) to 
more closely approximate the effluent HCl concentration.
    9.3.2  Spike Procedure. Introduce the HCl spike gas mixture at a 
constant flow rate (2 percent) at less than 10 percent 
of the total sample flow rate. (For example, introduce the HCl spike 
gas at 1 L/min (20 cc/min) into a total sample flow rate 
of 10 L/min). The spike gas must be preheated before introduction 
into the sample matrix to prevent a localized condensation of the 
gas stream at the spike introduction point. A heated sample 
transport line(s) containing multiple transport tubes within the 
heated bundle may be used to spike gas up through the sampling 
system to the spike introduction point. Use a calibrated flow device 
(e.g., mass flow meter/controller) to monitor the spike flow rate. 
Use a calibrated flow device (e.g., rotameter, mass flow meter, 
orifice meter, or other method) to monitor the total sample flow 
rate. Calculate the spike ratio from the measurements of spike flow 
and total flow. (See equation 2 and 3 in section 10.2 of this 
method.)
    9.3.3  Analyte Spiking. Determine the approximate effluent HCl 
concentrations by examination of preliminary samples. For single-
system approaches, determine whether the HCl concentration varies 
significantly with time by comparing consecutive samples for the 
period of time corresponding to at least twice the system response 
time. (For analyzers without sample averaging, estimate average 
values for two to five minute periods by observing the instrument 
display or data recorder output.) If the concentration of the 
individual samples varies by more than 10 percent 
relative to the mean value or 5 ppm, (whichever is 
greater), an alternate approach may be needed.
    9.3.3.1  Adjust the spike flow rate to the appropriate level 
relative to the total flow by metering spike gas through a 
calibrated mass flow meter or controller. Allow spike flow to 
equilibrate within the sampling system for at least the measurement 
system response time and a steady response to the spike gas is 
observed before recording response to the spiked gas sample. Next, 
terminate the spike gas flow and allow the measurement system to 
sample only the effluent. After the measurement system response time 
has elapsed and representative effluent measurements are obtained, 
record the effluent unspiked concentration. Immediately calculate 
the spike recovery.
    9.3.3.2  If the spike recovery is not within acceptable limits 
and a change in the effluent concentration is suspected as the cause 
for exceeding the recovery limit, repeat the analyte spike procedure 
without making any adjustments to the analyzer or sampling system. 
If the second spike recovery falls within the recovery limits, 
disregard the first

[[Page 14248]]

attempt and record the results of the second spike.
    9.3.3.3  Analyte spikes must be performed before and after each 
test run. Sampling system bias checks must also be performed before 
and after each test run. Depending on the particular sampling 
strategy and other constraints, it may be necessary to compare 
effluent data either immediately before or immediately after the 
spike sample to determine the spike recovery. Either method is 
acceptable provided a consistent approach is used for the test 
program. The average spike recovery for the pre-and post-run spikes 
shall be used to determine if spike recovery is between 70 and 130 
percent.

10.0  Data Analysis and Emission Calculations

    The average gas effluent concentration is determined from the 
average gas concentration displayed by the gas analyzer and is 
adjusted for the zero and upscale sampling system bias checks, as 
determined in accordance with section 9.2.3 of this method. The 
average gas concentration displayed by the analyzer may be 
determined by integration of the area under the curve for chart 
recorders, or by averaging all of the effluent measurements. 
Alternatively, the average may be calculated from measurements 
recorded at equally spaced intervals over the entire duration of the 
run. For sampling run durations of less than 1-hour, average 
measurements at 2-minute intervals or less, shall be used. For 
sampling run durations greater than 1-hour, measurements at 2-minute 
intervals or a minimum of 96 measurements, whichever is less 
restrictive, shall be used. Calculate the effluent gas concentration 
using equation 1.
[GRAPHIC] [TIFF OMITTED] TP24MR98.025

Where:

bc=Y-intercept of the calibration least-squares line.
bf=Y-intercept of the final bias check 2-point line.
bi=Y-intercept of the initial bias check 2-point line.
Cgas=Effluent gas concentration, as measured, ppm.
Cavg=Average gas concentration indicated by gas analyzer, 
as measured, ppm.
mc=Slope of the calibration least-squares line.
mf=Slope of the final bias check 2-point line.
mi=Slope of the initial bias check 2-point line.

    The following equations are used to determine the percent 
recovery (%R) for analyte spiking:

%R=(SM/CE) x 100 (Eq. 322-2)

Where:

SM=Mean concentration of duplicate analyte spiked samples 
(observed).
CE=Expected concentration of analyte spiked samples 
(theoretical).

CE=CS(QS/
QT)+SU(1-QS/QT) (Eq. 
322-3)

Where:

CS=Concentration of HCl spike gas (cylinder tag value).
QS=Spike gas flow rate.
QT=Total sample flow rate (effluent sample flow plus 
spike flow).
SU=Native concentration of HCl in unspiked effluent 
samples.

    Acceptable recoveries for analyte spiking are 30 
percent.

11.0  Pollution Prevention

    Gas extracted from the source and analyzed or vented from the 
system manifold shall be either scrubbed, exhausted back into the 
stack, or discharged into the atmosphere where suitable dilution can 
occur to prevent harm to personnel health and welfare or plant or 
personal property.

12.0  Waste Management

    Gas standards of HCl are handled as according to the 
instructions enclosed with the materials safety data sheets.

13.0  References

    1. Peeler, J.W., Summary Letter Report to Ann Dougherty, 
Portland Cement Association, June 20, 1996.
    2. Test Protocol, Determination of Hydrogen Chloride Emissions 
from Cement Kilns (Instrumental Analyzer Procedure) Revision 4; June 
20, 1996.
    3. Westlin, Peter R. and John W. Brown. Methods for Collecting 
and Analyzing Gas Cylinder Samples. Source Evaluation Society 
Newsletter. 3(3):5-15. September 1978.

[FR Doc. 98-6678 Filed 3-23-98; 8:45 am]
BILLING CODE 6560-50-P