[Federal Register Volume 64, Number 113 (Monday, June 14, 1999)]
[Rules and Regulations]
[Pages 31898-31962]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 99-12893]



[[Page 31897]]

_______________________________________________________________________

Part II





Environmental Protection Agency





_______________________________________________________________________



40 CFR Part 63



National Emission Standards for Hazardous Air Pollutants for Source 
Categories; Portland Cement Manufacturing Industry; Final Rule

  Federal Register / Vol. 64, No. 113 / Monday, June 14, 1999 / Rules 
and Regulations  

[[Page 31898]]


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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 63

[FRL-6347-2]
RIN 2060-AE78


National Emission Standards for Hazardous Air Pollutants for 
Source Categories; Portland Cement Manufacturing Industry

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

-----------------------------------------------------------------------

SUMMARY: This action promulgates national emission standards for 
hazardous air pollutants (NESHAP) for new and existing sources in the 
portland cement manufacturing industry. This action also adds Method 
320 for the measurement of vapor phase organic and inorganic emissions 
by extractive Fourier Transform Infrared (FTIR) spectroscopy and Method 
321 for the measurement of gaseous hydrogen chloride emissions from 
portland cement kilns by FTIR spectroscopy to appendix A of part 63.
    Some of the hazardous air pollutants (HAPs) released from portland 
cement manufacturing facilities include, but are not limited to, 
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. Exposure to these HAPs can cause reversible or 
irreversible health effects including carcinogenic, respiratory, 
nervous system, developmental, reproductive and/or dermal health 
effects. The EPA estimates that this final rule will reduce nationwide 
emissions of HAPs from portland cement manufacturing facilities by 
approximately 82 megagrams per year (Mg/yr) [90 tons per year (tpy)], 
and particulate matter (PM) by approximately 4,700 Mg/yr (5,200 tpy).
    These standards implement section 112(d) of the Clean Air Act (CAA) 
and are based on the Administrator's determination that portland cement 
manufacturing facilities may reasonably be anticipated to emit several 
of the 188 HAPs listed in section 112(b) of the CAA from the various 
process operations found within the industry. The final rule provides 
protection to the public by requiring portland cement manufacturing 
plants to meet emission standards reflecting the application of the 
maximum achievable control technology (MACT).

EFFECTIVE DATE: June 14, 1999. See the SUPPLEMENTARY INFORMATION 
section concerning judicial review.

ADDRESSES: Docket. Docket No. A-92-53, containing information 
considered by the EPA in development of the promulgated standards, is 
available for public inspection between 8:00 a.m. to 5:30 p.m., Monday 
through Friday, except Federal holidays, at the following address: U.S. 
Environmental Protection Agency, Air and Radiation Docket and 
Information Center (6102), 401 M Street S.W., Washington, DC 20460, 
telephone number (202) 260-7548. The docket is located at the above 
address in room M-1500, Waterside Mall (ground floor). A reasonable fee 
may be charged for copying docket materials.

FOR FURTHER INFORMATION CONTACT: For further information concerning 
applicability and rule determinations, contact the appropriate State or 
local agency representative. If no State or local representative is 
available, contact the EPA Regional Office staff listed in the 
Supplementary Information section of this preamble. For information 
concerning the analyses performed in developing this rule, contact Mr. 
Joseph Wood, P. E., Minerals and Inorganic Chemicals Group, Emission 
Standards Division (MD-13), Office of Air Quality Planning and 
Standards, U.S. EPA, Research Triangle Park, North Carolina 27711, 
telephone number (919) 541-5446, facsimile number (919) 541-5600, 
electronic mail address ``[email protected]''. For information 
regarding Methods 320 and 321 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:
    Regulated entities. Entities potentially regulated by this action 
are those that manufacture portland cement. Regulated categories and 
entities shown in Table 1.

                                          Table 1.--Regulated Entities
----------------------------------------------------------------------------------------------------------------
                                                                                       Examples of Regulated
                        Category                          NAICS Code    SIC Code              Entities
----------------------------------------------------------------------------------------------------------------
Industry...............................................        32731         3241  Owners or operators of
                                                                                    portland cement
                                                                                    manufacturing plants.
State..................................................        32731         3241  Owners or operators of
                                                                                    portland cement
                                                                                    manufacturing plants.
Tribal associations....................................        32731         3241  Owners or operators of
                                                                                    portland cement
                                                                                    manufacturing plants.
Federal agencies.......................................        (\1\)        (\1\)  None.
----------------------------------------------------------------------------------------------------------------
\1\ None.

    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. To determine 
whether your facility, company, business organization, etc. is 
regulated by this action, you should carefully examine the 
applicability criteria in Sec. 63.1340 of the rule. If you have 
questions regarding the applicability of this action to a particular 
entity, consult the appropriate regional representative:
    Region 1--Janet Bowen, Office of Ecosystem Protection, U.S. EPA, 
Region I, CAP, JFK Federal Building, Boston, MA 02203, (617) 565-3595.
    Region II--Kenneth Eng, Air Compliance Branch Chief, U.S. EPA, 
Region II, 290 Broadway, New York, NY 10007-1866 (212) 637-4000.
    Region III--Bernard Turlinski, Air Enforcement Branch Chief, U.S. 
EPA, Region III (3AT10), 841 Chestnut Building, Philadelphia, PA 19107, 
(215) 566-2110.
    Region IV--Lee Page, Air Enforcement Branch, U.S. EPA, Region IV, 
Atlanta Federal Center, 61 Forsyth Street, Atlanta, GA 30303-3104, 
(404) 562-9131.
    Region V--George T. Czerniak, Jr., Air Enforcement Branch Chief, 
U.S. EPA, Region V (5AE-26), 77 West Jackson Street, Chicago, IL 60604, 
(312) 353-2088.
    Region VI--John R. Hepola, Air Enforcement Branch Chief, U.S. EPA,

[[Page 31899]]

Region VI, 1445 Ross Avenue, Suite 1200, Dallas, TX 75202-2733, (214) 
665-7220.
    Region VII--Donald Toensing, Chief, Air Permitting and Compliance 
Branch, U.S. EPA, Region VII, 726 Minnesota Avenue, Kansas City, KS 
66101, (913) 551-7446.
    Region VIII--Douglas M. Skie, Air and Technical Operations Branch 
Chief, U.S. EPA, Region VIII, 999 18th Street, Suite 500, Denver, CO 
80202-2466, (303) 312-6432.
    Region IX--Barbara Gross, Air Compliance Branch Chief, U.S. EPA, 
Region IX, 75 Hawthorne Street, San Francisco, CA 94105, (415) 744-
1138.
    Region X--Anita Frankel, Air and Radiation Branch Chief, U.S. EPA, 
Region X (AT-092), 1200 Sixth Avenue, Seattle, WA 98101-1128, (206) 
553-1757.
    Judicial Review. The NESHAP for portland cement manufacturing was 
proposed on March 24, 1998 (63 FR 14182). Today's Federal Register 
action announces the EPA's final decision on the rule. Under section 
307(b)(1) of the Act, judicial review of the final rule is available by 
filing a petition for review in the U.S. Court of Appeals for the 
District of Columbia Circuit within 60 days of today's publication of 
this final rule. Under section 307(b)(2) of the Act, the requirements 
that are the subject of today's notice may not be challenged later in 
civil or criminal proceedings brought by the EPA to enforce these 
requirements.
    Technology Transfer Network. In addition to being available in the 
docket, an electronic copy of today's document, which includes the 
regulatory text, is available through the Technology Transfer Network 
(TTN) at the Office of Air and Radiation Policy and Guidance website. 
Following promulgation, a copy of the rule will be posted at the TTN's 
policy and guidance page for newly proposed or promulgated rules 
(http://www.epa.gov/ttn/oarpg/t3pfpr.html). A copy of the Response to 
Comments document for this rule will be posted on the TTN at http://
www.epa.gov/ttn/oarpg/t3bid.html. The TTN provides information from EPA 
in various areas of air pollution technology or policy. If more 
information on the TTN is needed, call the TTN help line at (919) 541-
5384.
    Outline. The following outline is provided to aid in reading this 
preamble to the final rule.

I. Statutory Authority
II. Background and Public Participation
III. Summary of Final Rule
    A. Applicability
    B. Emission Limits and Operating Limits
    C. Performance Test Provisions
    D. Monitoring Requirements
    E. Notification, Recordkeeping, and Reporting Requirements
IV. Summary of Changes Since Proposal
    A. Designation of Affected Sources
    B. Definitions
    C. Emission Standards and Operating Limits
    D. Performance Test Requirements
    E. Monitoring Requirements
    F. Additional Test Methods
    G. Reporting
    H. Exemption from New Source Performance Standards
    I. Delegation of Authority
    J. Test Methods 320, 321, and 322
V. Summary of Impacts
    A. Air Quality Impacts
    B. Water Impacts
    C. Solid Waste Impacts
    D. Energy Impacts
    E. Nonair Health and Environmental Impacts
    F. Cost Impacts
    G. Economic Impacts
VI. Summary of Responses to Major Comments
VII. Administrative Requirements
    A. Docket
    B. Executive Order 12866
    C. Executive Order 12875: Enhancing Intergovernmental 
Partnerships
    D. Unfunded Mandates Reform Act
    E. Regulatory Flexibility Act
    F. Submission to Congress and the General Accounting Office
    G. Paperwork Reduction Act
    H. Pollution Prevention Act
    I. National Technology Transfer and Advancement Act
    J. Executive Order 13045
    K. Executive Order 13084: Consultation and Coordination with 
Indian Tribal Governments

I. Statutory Authority

    The statutory authority for this rule is provided by sections 101, 
112, 113, 114, 116, and 301 of the Clean Air Act, as amended (42 U.S.C. 
7401, 7412, 7413, 7414, 7416, and 7601). This rule is also subject to 
section 307(d) of the CAA (42 U.S.C. 7407(d)).

II. Background and Public Participation

    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.'' 
(Clean Air Act, section 101(b)(1)) Section 112(b), as revised in 61 FR 
30816 (June 18, 1996), lists 188 HAPs believed to cause adverse health 
or environmental effects. Section 112(d) requires that emission 
standards be promulgated for all categories and subcategories of 
``major'' sources of these HAP and for ``area'' sources listed for 
regulation, pursuant to section 112(c). Major sources are defined as 
those that emit or have the potential to emit (from all emission points 
in all source categories within the facility) at least 10 tons per year 
of any single HAP or 25 tons per year of any combination of HAP. Area 
sources are stationary sources of HAP that are not major sources.
    On July 16, 1992 (57 FR 31576), the EPA published a list of 
categories of sources slated for regulation. This list included the 
portland cement source category regulated by the standards being 
promulgated today. The statute requires emissions standards for the 
listed source categories to be promulgated between November 1992 and 
November 2000. On June 4, 1996, the EPA published a schedule for 
promulgating these standards (61 FR 28197). Standards for the portland 
cement manufacturing source category covered by this rule were proposed 
on March 24, 1998 (63 FR 14182).
    As in the proposal, the final standards give existing sources 3 
years from the date of promulgation to comply. New sources are required 
to comply with the standard upon initial startup. The EPA believes 
these standards to be achievable for affected sources within the time 
provided.
    Operating limits, methods for determining initial compliance, as 
well as monitoring, recordkeeping, and reporting requirements are 
included in the final rule. All of these components are necessary to 
ensure that sources will comply with the standards both initially and 
over time. However, the EPA has made every effort to simplify the 
requirements in the rule.
    The amended Clean Air Act requires the EPA to promulgate national 
emission standards for sources of HAPs. Section 112(d) provides that 
these standards must reflect:
    ``* * * the maximum degree of reduction in emissions of the HAP * * 
* that the Administrator, taking into consideration the cost of 
achieving such emission reduction, and any nonair quality health and 
environmental impacts and energy requirements, determines is achievable 
for new or existing sources in the category or subcategory to which 
such emission standard applies * * *'' [42 U.S.C. 7412(d)(2)].
    This level of control is referred to as MACT. The Clean Air Act 
goes on to establish the least stringent level of control for MACT; 
this level is termed the ``MACT floor.''
    For new sources, the standards for a source category or subcategory 
``shall not be less stringent than the emission control that is 
achieved in practice by the best controlled similar source, as 
determined by the Administrator'' [section 112(d)(3)]. Existing source

[[Page 31900]]

standards shall be no less stringent than the average emission 
limitation achieved by the best performing 12 percent of the existing 
sources for source categories and subcategories with 30 or more 
sources, or the average emission limitation achieved by the best 
performing 5 sources for sources or subcategories with fewer than 30 
sources [section 112(d)(3)]. These two minimum levels of control define 
the MACT floor for new and existing sources.
    The standards were proposed in the Federal Register on March 24, 
1998 (63 FR 14182). The preamble for the proposed standards described 
the rationale for the proposed standards. Public comments were 
solicited at the time of proposal. To provide interested individuals 
the opportunity for oral presentation of data, views, or arguments 
concerning the proposed standards, a public hearing was offered at 
proposal. However, the public did not request a hearing and, therefore, 
one was not held. The public comment period, which was extended by 
thirty days in response to requests from commenters, was from March 24, 
1998 to June 26, 1998. A total of 28 comment letters were received. 
Commenters included industry representatives, State and local agencies, 
and environmental groups. Today's final rule reflects the EPA's full 
consideration of all of the comments. These public comments along with 
the EPA's responses to comments on the proposed rule are summarized in 
this preamble. A more detailed discussion of public comments and the 
EPA's responses can be found in the Response to Comment Document 
(Docket No. A-92-53, Item V-C-1).

III. Summary of Final Rule

A. Applicability

    The standards apply to each 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 (HWC), 40 CFR 63, subpart 
EEE, 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. HW kilns and HW in-line kiln/raw mills 
that temporarily or permanently stop burning hazardous waste may be 
subject to the emission standards, notification, testing, and 
monitoring requirements of today's rule, as provided by subpart EEE of 
this part.
    Except for hazardous waste burning (HW) cement kilns and HW in-line 
kiln/raw mills, these standards apply to all cement kilns and in-line 
kiln/raw mills regardless of the material being combusted in the kiln. 
Currently, cement kilns which combust municipal solid waste, medical 
waste, or other waste materials (other than HW) are subject to today's 
rule. Since these devices currently are not subject to section 129 
standards, EPA is including them in this rule to avoid a situation 
where they aren't regulated at all. This measure, however, is 
potentially an interim step. EPA could determine that cement kilns 
combusting solid waste materials should be regulated under section 129 
of the Clean Air Act, 42 U.S.C. Sec. 7429, and if so, EPA would revise 
the applicability section of these regulations accordingly at the time 
section 129 regulations applicable to cement kilns are promulgated.
    EPA also considered but rejected the possibility of subcategorizing 
cement kilns based on the nature of feed preparation for the kiln. As 
discussed in the proposal preamble, there are two types of portland 
cement manufacturing processes differentiated on the basis of feed 
preparation: wet process, and dry process (which includes the 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 air pollution controls. 
Therefore, if subcategories were defined based on process type, the 
MACT floor technology would be identical (docket item II-B-73). For 
this reason, the EPA is not promulgating separate rules based on 
process (kiln) type.
    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 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 this NESHAP. The first conveyor system transfer 
point subject to this NESHAP is the transfer point associated with the 
conveyor transferring material from the raw material storage to the raw 
mill.
    This regulation does not apply to the emissions from cement kiln 
dust (CKD) storage facilities (e.g., CKD piles or landfills). A 
separate rulemaking will be forthcoming utilizing RCRA authority that 
will apply to air emissions associated with CKD management and disposal 
facilities.

B. Emission Limits and Operating Limits

    In today's notice, the EPA is establishing emission limitations for 
particulate matter (as a surrogate for HAP metals), dioxins/furans (D/
F), and total hydrocarbons (as a surrogate for organic HAPs, including 
polycyclic organic matter). The NESHAP for portland cement 
manufacturing applies to both major and area sources of HAPs. The 
affected sources for which emission limits are established include the 
non-hazardous waste (NHW) kiln, NHW 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 NESHAP limits PM (surrogate for HAP metals) emissions, as well 
as opacity, from new and existing NHW kilns, NHW in-line kiln/raw 
mills, and clinker coolers, and limits opacity from raw material dryers 
and materials handling processes, at portland cement plants which are 
major sources. The rule also limits 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 
limits total hydrocarbon (THC) as a surrogate for organic HAP emissions 
from new greenfield NHW kilns, new greenfield NHW in-line kiln/raw 
mills, and new greenfield raw material dryers at portland cement plants 
which are major or area sources. Tables 2 and 3 present a summary of 
the emission limits for new and existing portland cement affected 
sources.

[[Page 31901]]



            Table 2.--Summary of Emission Limits a,\b for Affected Sources at Portland Cement Plants
                                                 (Metric units)
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                                                        Emission limit for existing     Emission limit for new
            Affected source and pollutant                         sources                      sources
----------------------------------------------------------------------------------------------------------------
NHW kiln and NHW in-line kiln/raw mill c PM..........  0.15 kg/Mg dry feed e and     0.15 kg/Mg dry feed e and
                                                        opacity level cc no greater   opacity level cc no
                                                        than 20 percent               greater than 20 percent
NHW kiln and NHW in-line kiln/raw mill D/F c,\d......  0.2 ng TEQ/dscm or 0.4 ng     0.2 ng TEQ/dscm or 0.4 ng
                                                        TEQ/dscm with PM control      TEQ/dscm with PM control
                                                        device operated at 204 deg.C g                eq>204 deg.C g
NHW kiln and NHW in-line kiln/raw mill THC d.........  none........................  50 ppmvd f (as propane)
Clinker cooler PM....................................  0.05 kg/Mg dry feed and       0.05 kg/Mg dry feed and
                                                        opacity level no greater      opacity level no greater
                                                        than 10 percent               than 10 percent
Raw material dryer and materials handling processes    10 percent opacity            10 percent opacity
 (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 d.............................  none........................  50 ppmvd f (as propane)
----------------------------------------------------------------------------------------------------------------
a All concentration limits at 7 percent oxygen.
b Applies to major sources only, except as noted.
c Includes main and alkali bypass stacks.
d Applies to both major and area source portland cement plants.
e 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.
f Applies only to new greenfield affected sources.
g The average temperature of the test run averages during performance test must be less than or equal to 204
  degrees C.


            Table 3.--Summary of Emission Limits a,\b for Affected Sources at Portland Cement Plants
                                                 (English units)
----------------------------------------------------------------------------------------------------------------
                                                        Emission limit for existing     Emission limit for new
            Affected source and pollutant                         sources                      sources
----------------------------------------------------------------------------------------------------------------
NHW kiln and NHW in-line kiln/raw mill c PM..........  0.30 lb/ton dry feed e and    0.30 lb/ton dry feed e and
                                                        opacity level c no greater    opacity level c no greater
                                                        than 20 percent               than 20 percent
NHW kiln and NHW in-line kiln/raw mill D/F c,\d......  8.7 x 10 -11 gr TEQ/dscf or   8.7 x 10 -11 gr TEQ/dscf or
                                                        1.7 x 10 -10 gr TEQ/dscf      1.7 x 10 -10 gr TEQ/dscf
                                                        with PM control device        with PM control device
                                                        operated at 400    operated at 400
                                                        deg.F g                       deg.F g
NHW kiln and NHW in-line kiln/raw mill THC d.........  none........................  50 ppmvd f (as propane)
Clinker cooler PM....................................  0.10 lb/ton dry feed and      0.10 lb/ton dry feed and
                                                        opacity level no greater      opacity level no greater
                                                        than 10 percent               than 10 percent
Raw material dryer and materials handling processes    10 percent opacity            10 percent opacity
 (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 d.............................  none........................  50 ppmvd f (as propane)
----------------------------------------------------------------------------------------------------------------
a All concentration limits at 7 percent oxygen.
b Applies to major sources only, except as noted.
c Includes main and alkali bypass stacks.
d Applies to both major and area source portland cement plants.
e 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.
f Applies only to new greenfield affected sources.
g The average temperature of the test run averages during performance test must be less than or equal to 400
  degrees F.

    The NESHAP imposes operating limits on affected sources that are 
subject to D/F emission limits. These operating limits are summarized 
in Table 4.

[[Page 31902]]



 Table 4.--Summary of Operating Limits for Affected Sources at Portland
                              Cement Plants
------------------------------------------------------------------------
  Affected Source/Pollutant     Pollutant         Operating Limits
------------------------------------------------------------------------
All kilns and in-line kiln     D/F         Operate such that the 3-hour
 raw mills at major and area                rolling average particulate
 sources (including alkali                  matter control device (PMCD)
 bypasses).                                 inlet temperature is no
                                            greater than temperature
                                            established at performance
                                            test.
                               ..........  Operate such that the three-
                                            hour rolling average
                                            activated carbon injection
                                            rate is no less than the
                                            rate established at
                                            performance test (if
                                            applicable).
                               ..........  Operate such that the three-
                                            hour rolling average
                                            activated carbon injection
                                            nozzle pressure drop or
                                            carrier fluid flow rate is
                                            no less than that specified
                                            by manufacturer (if
                                            applicable).
------------------------------------------------------------------------

    The rule requires the owner or operator to operate such that the 
temperature at the inlet to the kiln or in-line kiln raw mill 
particulate matter control device (PMCD) is at a level no greater than 
the level established during the successful Method 23 performance test. 
The three-hour rolling average temperature limit is established by 
taking the average of the one-minute average temperatures for each test 
run conducted during the successful Method 23 performance test, then 
averaging each test run average. Further, sources may petition the 
Administrator for an alternate averaging period or method for 
establishing operating parameter limits.
    Owners or operators of in-line kiln/raw mills are 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 shall not be exceeded. Owners or operators of kilns 
or in-line kiln/raw mills equipped with alkali bypasses are required to 
establish a separate temperatures for the inlet to the kiln or in-line 
kiln raw mill PMCD and the kiln or in-line kiln/raw mill alkali bypass 
PMCD. The applicable temperature limit for the alkali bypass is 
established during the performance test in which the raw mill is 
operating.
    After a transition period in which the status of the raw mill was 
changed from ``off'' to ``on'' or from ``on'' to ``off'', compliance 
with the operating limits for the new mode of operation begins, and the 
three-hour rolling average is established anew, i.e., without 
considering previous recordings.
    If carbon injection is used for D/F control, the carbon injection 
system must be operated such that the carbon injection rate shall be 
maintained at a level equaling or exceeding the rate which existed 
during the successful Method 23 performance test. The three-hour 
rolling average carbon injection rate limit is established in the same 
way as the temperature limit, as described above. The injection nozzle 
pressure drop or carrier fluid flow rate must also be monitored, and 
the minimum levels for these parameters are established based on 
manufacturers specifications. The nozzle pressure drop or carrier fluid 
flow rate is monitored with a 3-hour rolling averaging period.

C. Performance Test Provisions

    A performance test is required to demonstrate initial compliance 
with each applicable numerical limit. The rule requires the owner or 
operator to 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 will be repeated every 
5 years. Kilns and in-line kiln/raw mills equipped with alkali bypasses 
are 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 are 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 is 
not required to demonstrate initial compliance with the standard, 
however the permitting authority may require a ``back half'' for 
permitting, determination of emission fees, particulate matter 
monitoring or other purposes. Owners or operators are also required to 
determine the kiln or in-line kiln/raw mill dry feed rate, because the 
PM emission standards for kilns, in-line kiln/raw mills and clinker 
coolers are expressed as lb PM/ton (kg PM/Mg) dry feed.
    The opacity exhibited during the period of the initial Method 5 
performance test shall 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'' 
shall be used. Where the control device discharges through a fabric 
filter (FF) with multiple stacks or an electrostatic precipitator (ESP) 
with multiple stacks, the owner or operator has the option of 
conducting an opacity test in accordance with Method 9, in lieu of 
installing a COM.
    The rule requires the owner or operator to 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 D/F tests shall 
be repeated every 2 and one-half years. The temperature at the inlet to 
the particulate matter control device (PMCD) during the period of the 
Method 23 performance test shall be continuously recorded. One minute 
average temperatures must be calculated for each minute of each run of 
the test. The average of the one-minute averages must be calculated for 
each test run and included in the performance test report. The average 
of one-minute averages for each test run is averaged for all test runs, 
and this is the operating temperature limit not-to-be-exceeded by any 
3-hour rolling average temperature during subsequent operations of the 
affected source. If carbon injection is used for D/F control, the 
carbon injection rate and other associated operating parameters must be 
measured during the period of each run of the Method 23 performance 
tests. The average carbon injection rate and other associated operating 
parameters measured for the three runs must be determined and included 
in the test report.
    Owners or operators of in-line kiln/raw mills are required to 
conduct a Method 23 performance test, and record the temperature at the 
inlet to the PMCD

[[Page 31903]]

while the raw mill is operating, and a separate Method 23 performance 
test with PMCD inlet temperature recording while the raw mill is not 
operating. If applicable, the carbon injection rate shall be determined 
during both performance tests. Where applicable, the exhausts from both 
the kiln or in-line kiln/raw mill and the alkali bypass are required to 
meet the D/F standard.
    The owner or operator is required to repeat the performance tests 
for opacity, PM, and D/F emissions from kilns and in-line kiln/raw 
mills within 90 days of any significant change in the raw material 
components or fuels fed to the kiln (e.g, when there is an increase in 
the input rate of municipal solid waste, tire-derived fuel, medical 
waste, or other solid wastes to the kiln or in-line kiln/raw mill, 
above the rate used in the previous performance test.) Under the 
standard, the owner or operator shall use a THC continuous emission 
monitor (CEM) to conduct a performance test of THC emissions from new 
greenfield kilns, new greenfield in-line kiln/raw mills, and new 
greenfield raw material dryers. Owners or operators of new greenfield 
in-line kiln/raw mills are required to demonstrate initial compliance 
by measuring THC emissions while the raw mill is operating and while 
the raw mill is not operating. The standard for THC does not apply to 
the exhaust from the alkali bypass of kilns or the alkali bypass of in-
line kiln/raw mills, and these streams are not subject to a performance 
test for THC. Each THC CEM is required to be designed, installed, and 
operated in accordance with EPA Performance Specification (PS)-8A of 40 
CFR part 60, appendix B.
    Under the standard, the owner or operator shall 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 
performance test requirements is given in Table 5.

           Table 5.--Summary of Performance Test Requirements
------------------------------------------------------------------------
          Affected source and pollutant              Performance Test
------------------------------------------------------------------------
New and existing NHW kiln and NHW in-line kiln/   EPA Method 5 a
 raw mill b c PM.
New and existing NHW kiln and NHW in-line kiln/   COM if feasible d e or
 raw mill b c Opacity.                             EPA Method 9 visual
                                                   opacity readings.
New and existing NHW kiln and NHW in-line kiln/   EPA Method 23 j
 raw mill b c f g D/F.
New greenfield NHW kiln and NHW in-line kiln/raw  THC CEM (EPA PS-8A) h
 mill THC.
New and existing clinker cooler PM..............  EPA Method 5 a
New and existing clinker cooler opacity.........  COM d i or EPA Method
                                                   9 visual opacity
                                                   readings
New and existing raw and finish mill PM.........  EPA Method 9 a i
New and existing raw material dryer and           EPA Method 9 a i
 materials handling processes (raw material
 storage, clinker storage, finished product
 storage, conveyor transfer points, bagging, and
 bulk loading and unloading systems) PM.
New greenfield raw material dryer THC...........  THC CEM (EPA PS-8A) h
------------------------------------------------------------------------
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.
f Alkali bypass is tested with the raw mill on.
g Temperature parameters determined separately with and without the raw
  mill operating.
h EPA Performance Specification (PS)-8A of appendix B to 40 CFR part 60.
 
i Opacity limit is 10 percent.
j Required initially and every 2.5 years thereafter.

D. Monitoring Requirements

    The owner or operator of each portland cement manufacturing plant 
shall prepare for each affected source subject to the rule, a written 
operations and maintenance plan. The plan shall be submitted to the 
Administrator for review and approval as part of the application for a 
part 70 permit. The operations and maintenance plan shall include 
procedures for proper operation and maintenance of the affected source 
and air pollution control devices in order to meet the emission limits 
of the rule. The operations and maintenance plan shall also include 
procedures to be used during an inspection of the components of the 
combustion system of each kiln and each in-line kiln/raw mill. This 
inspection must be conducted at least once per year. Additionally, the 
operations and maintenance plan shall include corrective action 
procedures for the raw mill and finish mill, and associated particulate 
matter control devices (PMCDs), which must be implemented when required 
by the rule. The operations and maintenance plan shall also include 
provisions for monitoring opacity from materials handling sources, and 
to conduct M. 9 tests if visible emissions are observed. (Further 
details of this are discussed in the preamble section ``Summary of 
Changes Since Proposal''.) Finally, failure to implement procedures 
consistent with the operations and maintenance plan will be a violation 
of this subpart.
    The 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 is required to monitor 
emissions by conducting daily Method 9 tests. Where the control device 
discharges through a FF with multiple stacks or an ESP with multiple 
stacks, the owner or operator has the option of conducting daily tests 
in accordance with Method 9, in lieu of installing a COM. The duration 
of the Method 9 tests is 30 minutes.
    The rule requires that kilns and in-line kiln raw mills subject to 
the particulate matter (PM) standards must install, correlate, and 
operate PM continuous emission monitors (CEMs). However, the compliance 
date for

[[Page 31904]]

installing PM CEMs is deferred pending further rulemaking. Further 
discussion of this issue is found in the preamble sections ``Summary of 
Changes Since Proposal'' and ``Summary of Responses to Major 
Comments.''
    The owner or operator of a kiln or in-line kiln raw mill must 
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/or alkali bypass (if applicable), at the 
inlet to or upstream of the kiln, in-line kiln/raw mill, and alkali 
bypass PMCD. The calibration of the thermocouple or other temperature 
sensor must be verified at least once every three months.
    If activated carbon injection is used for D/F control, the owner or 
operator must install, operate, calibrate and maintain a device to 
continuously monitor and record the weight of activated carbon injected 
and record the weight in 1 minute rolling averages. The accuracy of the 
weight measurement device must be  1 percent of the weight 
being measured. The calibration of the device must be verified at least 
once every three months. The owner or operator must record the feeder 
setting at least once per day and determine the mass of carbon injected 
for every three-hour rolling average period. In addition, the carbon 
injection nozzle pressure drop or activated carbon carrier fluid flow 
rate must be monitored and recorded. Further, the activated carbon 
specifications must be the same as or better than the specifications of 
the carbon used during the previous performance test.
    To clarify how the three-hour rolling average is calculated at 
initial start-up, operating parameter limits will not become effective 
on the compliance date until enough data have been accumulated to 
calculate the rolling average for the limit. For example, given that 
compliance with the standards begins nominally at 12:01 am on the 
compliance date, the three-hour rolling average temperature limit does 
not become effective as a practical matter until 3:01 am on the 
compliance date. This approach is adopted for all continuous monitoring 
systems, including CEMs.
    During intermittent operations, however, periods of time when 
operating parameters are not recorded for any reason (e.g., source 
shutdown) are to be ignored when calculating rolling averages. For 
example, consider how the three-hour rolling average for a parameter 
would be calculated if a source shuts down for yearly maintenance for a 
three week period. The first one-minute average value recorded for the 
parameter for the first minute of renewed operations is added to the 
last 179 one-minute averages before the source shut down, to calculate 
the three-hour rolling average. This approach is adopted for all 
continuous monitoring systems, including CEMs. This approach would 
inhibit a source from intentionally interrupting the monitoring system 
to avoid unwanted parameter values.
    The rule requires the owner or operator to monitor THC emissions 
from the main exhaust of greenfield kilns; the main exhaust of 
greenfield in-line kiln/raw mills; and greenfield raw material dryers 
using a CEM installed in accordance with PS-8A in 40 CFR part 60, 
appendix B.
    The rule requires the owner or operator to monitor the opacity from 
raw mills and finish mills 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.''
    Owners or operators of raw mills and finish mills are required to 
initiate corrective action within one hour of a Method 22 test during 
which visible emissions are observed. A 30-minute Method 9 opacity test 
must be started within 24 hours of observing visible emissions.
    A summary of monitoring requirements is given in Table 6.

              Table 6.--Summary of Monitoring Requirements
------------------------------------------------------------------------
 Affected source and pollutant    Monitor/Type/          Monitoring
          or opacity            Operation/Process       requirement
------------------------------------------------------------------------
All affected sources..........  Operations and     Prepare written plan
                                 maintenance plan.  for all affected
                                                    sources and control
                                                    devices.
All kilns and in-line kiln raw  COM, if            Install, calibrate,
 mills at major sources          applicable.        maintain and operate
 (including alkali bypass)/                         in accordance with
 opacity.                                           general provisions
                                                    and with PS-1.
                                Method 9 opacity   Daily test of at
                                 test, if           least 30-minutes,
                                 applicable.        while kiln is at
                                                    highest load or
                                                    capacity level.
All kilns and in-line kiln raw  PM CEM...........  The compliance date
 mills at major sources                             is deferred until a
 (including alkali bypass)/PM.                      future rulemaking,
                                                    at which time EPA
                                                    will consider what
                                                    performance
                                                    specification
                                                    requirements should
                                                    be established.
All kilns and in-line kiln raw  Combustion system  Conduct annual
 mills at major and area         inspection.        inspection of
 sources (including alkali                          components of
 bypass)/D/F.                                       combustion system.
                                Continuous         Install, operate,
                                 temperature        calibrate and
                                 monitoring at      maintain continuous
                                 PMCD inlet.        temperature
                                                    monitoring and
                                                    recording system;
                                                    calculate 3-hour
                                                    rolling average;
                                                    verify temperature
                                                    sensor calibration
                                                    at least quarterly.
                                Activated carbon   Install, operate,
                                 injection rate,    calibrate and
                                 nozzle pressure    maintain continuous
                                 drop or carrier    activated carbon
                                 fluid flow rate,   injection rate
                                 and carbon type/   monitor; verify
                                 brand, if          calibration at least
                                 applicable.        quarterly; record
                                                    feeder setting
                                                    daily; calculate
                                                    average injection
                                                    rate for each 3-hour
                                                    rolling average.
                                                    Monitor nozzle
                                                    pressure drop or
                                                    carrier fluid flow
                                                    rate according to
                                                    manufacturers
                                                    specifications, and
                                                    calculate rolling 3-
                                                    hour averages.
New greenfield kilns and in-    THC CEM..........  Install, operate, and
 line raw mills at major and                        maintain THC CEM in
 area sources/THC.                                  accordance with PS-
                                                    8A; calculate 30-day
                                                    block average THC
                                                    concentration.
All clinker coolers at major    COM, if            Install, calibrate,
 sources/opacity.                applicable.        maintain and operate
                                                    in accordance with
                                                    general provisions
                                                    and with PS-1.
                                Method 9 opacity   Daily test of at
                                 test, if           least 30-minutes,
                                 applicable.        while kiln is at
                                                    highest load or
                                                    capacity level.

[[Page 31905]]

 
All materials handling          M. 22 visible      For each MHO, conduct
 operations (MHO) at major       emissions test     monthly 1-minute
 sources/opacity.                as part of         Method 22 visible
                                 operations and     emissions test; if
                                 maintenance plan.  visible emissions
                                                    are observed,
                                                    initiate corrective
                                                    action within one
                                                    hour and conduct 30-
                                                    minute Method 9 test
                                                    within 10 minutes.
                                                    For each MHO, if no
                                                    visible emissions
                                                    are observed after
                                                    first 6 months,
                                                    reduce monitoring to
                                                    semi-annual. If no
                                                    VE are observed
                                                    thereafter, reduce
                                                    monitoring to annual
                                                    basis. If VE are
                                                    observed for a MHO,
                                                    revert back to
                                                    conducting VE tests
                                                    on a monthly basis.
All raw mills and finish mills  Method 22 visible  Conduct daily 6-
 at major sources/opacity.       emissions test.    minute Method 22
                                                    visible emissions
                                                    test while mill is
                                                    operating at highest
                                                    load or capacity
                                                    level; if visible
                                                    emissions are
                                                    observed, initiate
                                                    corrective action
                                                    within one hour and
                                                    conduct 30-minute
                                                    Method 9 test within
                                                    24 hours.
New greenfield raw material     THC CEM..........  Install, operate, and
 dryers at major and area                           maintain THC CEM in
 sources/THC.                                       accordance with PS-
                                                    8A; calculate 30-day
                                                    block average THC
                                                    concentration.
------------------------------------------------------------------------

E. Notification, Recordkeeping, and Reporting Requirements

    All notification, recordkeeping, and reporting requirements in the 
general provisions (40 CFR part 63, subpart A) 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 
shall report quarterly until a request to return the reporting 
frequency to semiannual is approved.
    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. Summary of Changes Since Proposal

    In response to comments received on the proposed standards, changes 
have been made to the final standards. These changes include 
clarifications designed to make the EPA's intent clearer as well as 
changes to the requirements of the proposed standards. A summary of the 
substantive changes made since the proposal is given in the following 
sections, along with the rationales for these changes. Further details 
on the rationales for these changes can be found in Section VI of the 
preamble: Summary of Responses to Major Comments.

A. Designation of Affected Sources

    The section of the rule on designated affected sources is being 
clarified to include new greenfield raw material dryers that are 
located at facilities that are area sources. The EPA is clarifying 
today that these affected sources are subject to limitations on THC. 
The preamble for the proposed rule stated that polycyclic organic 
matter (POM) emissions (using THC as a surrogate) from portland cement 
NHW kiln area sources would be subject to MACT standards under EPA's 
interpretation of section 112(c)(6). The EPA proposed to use THC as a 
surrogate for organic HAPs, and today it is clarifying that POM is an 
organic HAP for which THC is a surrogate. Since POM was a listed HAP 
from portland cement NHW cement kilns (at both area and major source 
portland cement plants) in the section 112(c)(6) listing (63 FR 17838, 
April 10, 1998), the EPA is clarifying that the limitation of emissions 
of THC applies to new greenfield cement kilns, in-line kiln raw mills 
and raw material dryers at major and area source cement plants in the 
portland cement industry. Further discussion of this change is found 
below in the discussion of standards.

B. Definitions

    The definitions of ``alkali bypass'' and ``feed'' have been 
expanded to reflect cement industry practices. Definitions of 
``greenfield'' and new ``brownfield'' affected sources have been added 
to the final rule to clarify the applicability of the final THC 
standards to specific affected sources. A definition of ``one-minute 
average'' has been added to clarify the monitoring provisions of the 
final rule. A definition of rolling average has been added to clarify 
and maintain consistency with the requirements for HW kilns.

C. Emission Standards and Operating Limits

    Based on comments received, the EPA is clarifying today that the 
THC limitation applicable to new kilns, new in-line kiln/raw mills, and 
new raw material dryers is restricted to greenfield sources, in 
recognition of the difficulty that owners or operators of reconstructed 
and new brownfield affected sources might have in obtaining suitable 
kiln feed materials while remaining competitive. The selection of a 
site tied to feed materials with relatively low levels of naturally 
occurring organic matter is the basis for the MACT standard and is an 
option only available to greenfield sources. Further, as discussed 
above, the EPA is clarifying that this THC limitation applies to new 
greenfield kilns, new greenfield in-line kiln/raw mills, and greenfield 
raw material dryers located at facilities that are area, as well as 
major, sources.
    The requirements in the proposal for initiating a site-specific 
operating and maintenance plan, and implementation of a quality 
improvement plan, due to stipulated exceedences of a 15 percent kiln 
opacity limit, have been removed. The EPA agrees with commenters who 
questioned this tiered approach, and so the final rule will retain only 
a 20 percent opacity limit for the kiln and in-line kiln/raw mill.
    In response to a comment, the EPA is clarifying that the opacity 
limitation on gases discharged from raw mills and finish mills is 
restricted to the mill sweep and air separator air pollution control 
devices. This is consistent with the MACT floor technology for control 
of gases from these affected sources.
    The final rule has been reformatted to provide a separate section 
for operating

[[Page 31906]]

limits. Control of temperature at the inlet to kiln and in-line kiln/
raw mill PMCDs and control of the activated carbon injection parameters 
(if applied as a D/F control technique) are provisions promulgated as 
operating limits.
    The averaging period for the operating limit for the inlet kiln and 
in-line kiln/raw mill PM control device temperature (to demonstrate 
compliance with the D/F emission limits) has been changed from a 9-hour 
block average period to a three-hour rolling average period. Comments 
were received that the averaging period should be shorter. In addition, 
the rule has been clarified to include data reduction procedures to be 
followed to demonstrate compliance. Furthermore, sources may petition 
the Administrator for an alternate averaging period or method for 
establishing operating parameter limits.
    The provisions for establishing the PM control device inlet 
temperature limit based on the D/F performance test have been changed 
to correct an error in drafting the proposal. A commenter pointed out 
that the proposal would allow a source to conduct its D/F performance 
test with an inlet PM control device temperature below 400 degrees F, 
but after the performance test, the source would be allowed to operate 
its PM control device with an inlet temperature up to 400 degrees F. In 
drafting the proposal, the EPA did not intend to allow a source to 
operate its PM control device at a temperature higher than the 
temperature during the performance test, and so the EPA is clarifying 
today that the inlet temperature limit is established as and capped at 
the average temperature during the D/F performance test. To further 
achieve consistency with the D/F temperature requirements for HW kilns 
and to better assure that the standard reflects MACT, the EPA is 
dropping the proposed provision which would have allowed the 
temperature limit to be established as the average temperature during 
the performance test plus 25 degrees F if the D/F level was below 0.15 
ng/dscm. To clarify and maintain consistency with the requirements for 
HW kilns (and to best implement standards representing MACT), if the 
source complies with the O.4 ng TEQ/dscm D/F limit, the average 
temperature of the test run averages during the performance test must 
be below 400 degrees F. To further achieve consistency with the 
requirements for HW kilns, additional operating parameter limits 
associated with the use of activated carbon injection must be 
established and these parameters must be monitored continuously. The 
averaging period for the activated carbon injection rate and other 
operating parameters has been changed from a 9-hour period to a 3-hour 
rolling average period. Further details on the establishment of the 
temperature and other operating parameter limits are discussed in 
section VI. of this preamble.

D. Performance Test Requirements

    In response to comment, the EPA is clarifying that both during the 
performance test and to demonstrate continuous compliance, opacity 
limitations for the kiln and clinker cooler must be met for each 6-
minute block period. (The proposal incorrectly required a 30-minute 
averaging time.) This is consistent with the requirements of the NSPS, 
which is the basis for the MACT floor for PM/metals and opacity.
    Based on comments received that there should be consistency with 
the requirements for HW kilns, the performance tests for D/F must be 
conducted every 2 and one-half years. (The proposal would have required 
that the D/F emissions tests be conducted every 5 years.) To further 
achieve consistency, and to assure that the kiln continues to achieve 
the requisite emissions reductions reflected in the standard, the EPA 
is also clarifying today that in addition to repeating performance 
tests every five years (or 2.5 years for the D/F performance tests), 
performance tests for kilns or in-line kiln/raw mills must be repeated 
within 90 days of initiating any significant change in the feed 
materials or fuels fed to the kilns (e.g., an increase in the input 
rate of municipal solid waste, tire-derived fuel, or medical waste to 
the kiln or in-line kiln/raw mill above the rate used in the previous 
performance test; or a switch from burning natural gas to coal). Such 
changes in fuel or feeds could result in changes to emissions.

E. Monitoring Requirements

    In response to a comment, clarification has been added to the final 
rule to establish that any required Method 9 and Method 22 tests must 
be conducted while the affected source is operating at the highest load 
or capacity level reasonably expected to occur within the day that the 
test is performed.
    The option for use of triboelectric bag leak detection systems for 
monitoring raw mill and finish mill fabric filter performance is not 
being promulgated at this time. Numerous commenters expressed concern 
regarding installation, operation, calibration and maintenance, and 
that the lack of clear-cut specifications would lead to open-ended 
liability for owners/operators. Those owners or operators who want to 
use bag leak detection systems may petition the Administrator for 
approval of alternative monitoring requirements under the General 
Provisions.
    Requirements for temperature monitoring devices (including range 
and reference standard) have been added to the final rule. In response 
to a comment, monitoring requirements for activated carbon injection 
system accuracy, calibration frequency, and data recording and 
reduction have also been added to the final rule. To achieve 
consistency with the requirements for HW kilns, activated carbon 
injection nozzle pressure drop or carrier fluid flow rate, and carbon 
specifications, must also be monitored and recorded.
    An explicit monitoring requirement for an inspection of the 
components of the combustion system of each kiln or in-line kiln/raw 
mill has been added to the rule. This inspection must be conducted at 
least once per year, in accordance with the procedures specified in the 
operation and maintenance plan for the affected source. This change was 
made in response to several comments that were received suggesting that 
provisions (such as limitations on and monitoring of carbon monoxide) 
be added to the final rule to ensure good combustion and thus minimize 
formation of D/F.
    The operations and maintenance plan requirement has been changed to 
explain that the plan must also include provisions for observing 
opacity from materials handling sources, and for conducting a M. 9 test 
if visible emissions (VE) are observed. Specifically, materials 
handling sources' VE shall be monitored via M. 22 once per month. After 
6 months without VE for each individual source, the monitoring 
frequency would be reduced to a semi-annual basis. If there are no VE 
in the next 6 month period for a particular source, the monitoring 
frequency would be reduced to an annual basis. If VE occurs during the 
annual inspection, the frequency would revert back to once per month. 
If VE are observed during one of these inspections, a Method 9 test is 
required. This change was made to provide greater assurance that these 
units are in compliance with the opacity limit and to meet the Agency's 
commitment to incorporate enhanced monitoring in all MACT standards.
    Finally, the final rule is being clarified that failure to 
implement procedures consistent with the operations and maintenance 
plan will be a violation of this subpart.

[[Page 31907]]

    In the preamble to the proposal, the EPA noted its intent to 
include a requirement for PM continuous emission monitors (CEMs) in the 
final rule, unless the analyses of new information and data showed that 
it is not appropriate. (See 63 FR at 14205). Based on successful 
testing on an incinerator, as well as extensive use of these monitors 
in Europe, EPA believes there is sound evidence the PM CEMs should work 
at cement kilns. Accordingly, the final rule contains a requirement to 
install PM CEMs. However, we are deferring the effective date of this 
requirement pending further testing and additional rulemaking. Please 
see the preamble section ``Summary of Responses to Major Comments'' for 
further details on this issue.

F. Additional Test Methods

    The final rule has been changed to permit the use of either Method 
320 or Method 321 for the determination of hydrogen chloride (HCl) for 
the purpose of making an applicability determination. These methods are 
being promulgated as part of this rulemaking.
    Since proposal of Method 322 for the measurement of HCl along with 
the portland cement NESHAP, the EPA attempted to utilize Method 322 to 
gather data from lime kilns (which have a matrix similar to portland 
cement sources) and encountered technical problems with the gas filter 
correlation infrared spectroscopy (GFCIR). Many of these problems were 
adequately identified by the data quality indicators in the method. 
However, as a backup option, the Agency collected data sets at lime 
kilns using both GFCIR and Fourier transform infrared spectroscopy 
(FTIR). These paired data sets provide unexpected contradictory 
results.
    The dynamic spiking results of the GFCIR would indicate that Method 
322 results should be biased by overpredicting the true value (the 
spike recovery consistently showed greater than 100 percent recovery). 
However, FTIR data collected nearly simultaneously with the GFCIR data 
show that the GFCIR results were significantly lower than FTIR results. 
Since the Agency applied statistical methods to analyze the FTIR data 
and concluded that the FTIR method did not have a significant bias, the 
Agency is confident in the values reported by the FTIR instrument. 
Therefore, this leads to a paradox with the GFCIR data; the results are 
contradictory for the GFCIR. At this point, the Agency has not 
determined the cause of the paradox, which has led to the decision to 
postpone promulgation of Method 322 as an alternative method for 
measurement of HCl from portland cement kilns.
    The EPA will continue to investigate the reasons for the 
differences in the two methods, and if a satisfactory solution is found 
to correct the problem, may consider further action on this method if 
additional evaluation data are available. For this reason proposed 
Method 322 is not being promulgated at this time and may not be used in 
applicability determinations for portland cement plants. (A more 
detailed discussion of this can be found in comment 2.5.1 in the 
Response to Comment Document.)
    In the proposal, we stated that Methods 26 and 26A may be used in 
applicability determinations provided that these methods are validated 
concurrently using M. 321 or 322. Several comments were received 
stating that EPA is restricting M. 26 and M. 26A use by requiring that 
they be validated each time they are used, and that Method 26 has long 
been an approved EPA test method. Based on these comments, this 
requirement has been changed such that Methods 26 and 26A may be used 
to confirm a source is a major source without concurrent validation 
with M. 321 or M. 322. However, M. 26 or 26A may not be used to make 
the assertion that the source is an area source. Only the FTIR methods 
may be used for the measurement of HCl if the source wishes to claim it 
is not a major source. See the preamble section ``Summary of Responses 
to Major Comments'' for further discussion of this issue about how a 
source should determine whether it is a major or area source.

G. Reporting

    A provision has been added to the final rule requiring that the 
semi-annual summary report for the period in which the annual 
combustion system component inspection was conducted include the 
results of the inspection.

H. Exemption from New Source Performance Standards

    To eliminate overlap or duplicate coverage of NSPS and MACT 
standards for portland cement facilities, affected sources subject to 
requirements under this NESHAP are exempted from requirements under 40 
CFR 60, subpart F, the New Source Performance Standards. However, there 
are two exceptions to this: kiln and in-line kiln/raw mills, and 
greenfield raw material dryers, that are new or reconstructed sources 
under the definition in Subpart F, and are located at area source 
cement plants, would still be subject to applicable PM limits, opacity 
limits, and recordkeeping and reporting requirements of the NSPS. The 
reason for this is that these ``NSPS'' kilns and in-line kiln/raw 
mills, and greenfield raw material dryers that are located at area 
source cement plants would be subject to the NESHAP's D/F and/or THC 
limits, but would not be subject to the NESHAP's PM limits, because 
they are located at area source cement plants.

I. Delegation of Authority

    The final rule reserves authority for approval of alternate 
emission standards, major alternatives to test methods, major 
alternatives to monitoring procedures and waivers of recordkeeping.

J. Test Methods 320, 321, and 322

    Test Methods 320 and 321 are being promulgated with minor 
corrections to clarify and improve test procedures, and correct 
equations incorrectly stated in the proposal notice. Proposed Test 
Method 322 is not being promulgated at this time as noted in Section F 
above.

V. Summary of Impacts

A. Air Quality Impacts

    The air quality impacts of the final rule are identical to those of 
the proposed rule. Nationwide baseline HAP emissions from portland 
cement manufacturing plants are estimated to be 260 Mg/yr (290 tpy) at 
the current level of control. This rule will 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 this 
rule are given in metric and English units in Tables 7 and 8. The 
following text reviews the information provided in Tables 7 and 8.

[[Page 31908]]



 Table 7.--Nationwide Annual Emission Reductions of HAPS and Other Pollutants From Portland Cement Manufacturing
                                                     Plants
                                                 (Metric units)
----------------------------------------------------------------------------------------------------------------
                                                           Baseline emissions  (Mg/    Emission reduction  [Mg/
           Source                      Pollutant                      yr)                         yr]
----------------------------------------------------------------------------------------------------------------
Kilns, in-line kiln/raw       HAP Metals a..............  150.......................  35
 mills, and 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
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 greenfield NHW kilns only.


 Table 8.--Nationwide Annual Emission Reductions of HAPS and Other Pollutants From Portland Cement Manufacturing
                                                     Plants
                                                 [English units]
----------------------------------------------------------------------------------------------------------------
           Source                      Pollutant           Baseline emissions (tpy)    Emission reduction (tpy)
----------------------------------------------------------------------------------------------------------------
Kilns, in-line kiln/raw       HAP Metals a..............  160.......................  38
 mills, and alkali bypasses.  PM a......................  16,000....................  3,800
                              D/F (TEQ) b...............  0.096 lbs/yr..............  0.035 lbs/yr
                              Organic HAPs c............  130.......................  52
                              THC c.....................  580.......................  220
Clinker coolers.............  HAP Metals a..............  1.2.......................  0.2
                              PM a......................  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 greenfield NHW kilns only.

    This rule will 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 will 
be reduced by 35 Mg/yr (38 tpy), a reduction of 24 percent from the 
baseline level. Emissions of D/F TEQ will be reduced by 15 grams (g)/yr 
(0.033 lb/yr), a reduction of 36 percent from the baseline level, at 
existing NHW cement kilns and in-line kiln/raw mills located at major 
source and area source facilities.
    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 MACT standards will 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.
    The MACT standards will 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 affected 
existing clinker coolers will 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 greenfield raw material dryers. However, 
information on THC emission rates from raw material dryers and a 
projection of the number of such affected sources is not currently 
available, so nationwide reductions cannot be estimated.

B. Water Impacts

    The impacts of the final rule are identical to those of the 
proposed rule. Control of D/F emissions using water injection for 
temperature reduction will 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 and 8 million gallons per year for new NHW kilns and NHW in-
line kiln/raw mills.

C. Solid Waste Impacts

    The impacts of the final rule are identical to those of the 
proposed rule. The amount of solid waste from existing NHW kilns, in-
line kiln/raw mills, and clinker coolers (located at major sources) 
will increase by an estimated 4,700 Mg/yr (5,200 tpy) due to the 
requirements for PM control in the final rule.

D. Energy Impacts

    The impacts of the final rule are identical to those of the 
proposed rule. For existing NHW kilns and NHW in-line kiln/raw mills 
the MACT standards for PM and D/F will 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 MACT standards for D/F will increase energy consumption by an 
estimated 10,600 KWh/yr (36 million Btu/yr).

E. Nonair Health and Environmental Impacts

    The reduction in HAP emissions will have a beneficial effect on 
nonair health and environment impacts. Dioxin/furan and HAP metals have 
been found in the Great Lakes and other water bodies and

[[Page 31909]]

have been listed as pollutants of concern due to their persistence in 
the environment, potential to bioaccumulate, and toxicity to humans and 
the environment. Implementation of the NESHAP will 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) not including D/F. The 
National Institute for Occupational Safety and Health recommends an 
exposure level for D/F at the lowest feasible concentration. The final 
rule will reduce emissions, and consequently, occupational exposure 
levels for plant employees.

F. Cost Impacts

    For new and existing NHW kilns, NHW in-line kilns/raw mills, 
clinker coolers, raw and finish mills, and materials handling 
facilities, the projected overall total capital costs of the final rule 
for controlling and monitoring emissions of D/F, PM (includes opacity), 
and THC are $108 million. The overall projected annual costs of the 
rule, for controlling and monitoring for D/F, PM (includes opacity), 
and THC, are $37 million. For new and existing NHW kilns and NHW in-
line kiln/raw mills, the projected total capital and annual costs of 
complying with the MACT standard for D/F (includes controls and 
monitoring) are $15 million and $3.6 million, respectively. For new and 
existing sources subject to PM and/or opacity limits, the projected 
total capital and annual costs of complying with the MACT standards for 
PM and opacity (including PM controls, PM CEMs, and continuous opacity 
monitors) are $92 million and $33 million, respectively. With respect 
to PM CEMs costs only, the projected total capital and annual costs of 
PM CEMs are $15 million and 7.6 million, respectively. The THC 
emissions limit for new greenfield NHW kilns, NHW in-line kiln/raw 
mills and raw material dryers 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 greenfield kilns is 
not expected to be significantly limited by the emission limit. The 
projected fifth-year national capital and annual costs of monitoring 
THC with a continuous emission monitor for new greenfield NHW kilns, 
in-line kiln/raw mills and raw material dryers are $0.75 million and 
$0.45 million, respectively (based on an estimated four new affected 
sources).

G. Economic Impacts

    EPA conducted an economic analysis of the proposed NESHAP, and has 
reconducted its analysis to include the costs of PM CEMs and the 
monitoring of materials handling sources. The economic impacts of the 
final rule are slightly greater than those of the rule as proposed. 
Because the final standards may potentially include costs associated 
with PM CEMs and the monitoring of materials handling sources, EPA 
reconducted its economic analysis. This revised analysis evaluates a 
regulatory option that is more stringent than the final standards. 
Analyzing this more stringent option, which overstates the expected 
compliance costs, causes the economic impacts presented here to over 
estimate the expected impacts of the final standards. However, these 
economic impacts are only slightly greater than those of the proposal 
analysis.
    The EPA estimates that regional market price increases of portland 
cement will be between 0.3 and 2.6 percent. The national average price 
increase is estimated to be 1.1 percent. The related decreases in 
quantity demanded of portland cement are estimated to range from 0.3 to 
2.3 percent, with a national average of 1.0 percent. Domestic 
production of portland cement is estimated to decrease more than 
consumption (2.2 percent compared to 1.0 percent nationally because 
imports are estimated to increase by 5.5 percent). The decreases in 
domestic production may lead to the loss of approximately 334 jobs in 
the United States. No plants are expected to close; four kilns are 
expected to cease operating.

VI. Summary of Responses to Major Comments

    A complete summary of all of the public comments on the proposal, 
and responses to these comments is provided in the ``Response to 
Comments'' document available in the docket and from EPA's Technology 
Transfer Network. The responses to major comments are given in this 
section.

Portland Cement Source Category

    Comment: Commenters raised objections to splitting the portland 
cement category for cement kilns by the type of fuel (hazardous waste 
vs. fossil fuels) burned in the kiln. The commenters stated that 
splitting the industry by fuel type deviates from EPA's original source 
category list (July 16, 1992 FR) which included only a portland cement 
manufacturing category, and that no distinction is made regarding fuel 
type under the New Source Performance Standards (NSPS) for portland 
cement plants. The commenters were concerned that EPA's decision not to 
use the NSPS category will result in what Congress hoped to avoid 
(through section 112(c)(1)) by causing unnecessary costs and 
dislocations in the cement industry.
    Response: Section 112(d)(1) of the Clean Air Act specifically 
provides that ``the Administrator may distinguish among classes, types 
and sizes of sources within a category or subcategory in establishing 
standards. . . .''. With regard to having separate categories/
subcategories, the EPA believes that there can be significant 
differences in emissions due to hazardous waste burning that warrant 
separate classes for these devices. The types of HAPs found in 
emissions from hazardous waste-burning kilns are different from, and 
more numerous than, those from NHW kilns. Hazardous wastes can contain 
virtually any HAP, which in turn can be in stack emissions. The fact 
that hazardous waste-burning kilns are dealt with separately under a 
different statute (RCRA section 3004(q)(special standards for 
industrial furnaces which burn hazardous waste fuels)) likewise 
indicates that hazardous waste-burning cement kilns can be dealt with 
legitimately as a separate class. Indeed, this existing RCRA regulatory 
regime has created a different data base, and system of existing 
controls, which can result in different analyses, different floor 
controls and standards under the section 112 MACT process, again 
indicating that these sources can reasonably be classified as a 
distinct class. To summarize, this NESHAP for portland cement 
manufacturing covers NHW kilns and NHW in-line kiln raw mills; it does 
not apply to HW cement kilns which are subject to subpart EEE of this 
part. This NESHAP also covers affected sources located at portland 
cement manufacturing plants (such as clinker coolers, raw material 
dryers, and materials handling processes), regardless of whether the 
plant operates HW kilns.
    Comment: Two commenters stated that EPA has not met its legal 
burden to be consistent when regulating HW and NHW cement kilns. The 
commenters stated that the EPA has not used consistent rationales and 
approaches to develop emission limitations for the same pollutants.
    Response: There are a number of differences between kilns that burn 
hazardous waste and those that do not

[[Page 31910]]

in terms of process feed/fuel, process operation, pollutants and 
pollutant quantities generated, existing regulations that impact MACT 
floor determinations, and the economics of their operations. These 
differences provide the bases for differences in determinations of MACT 
floors, emission limits, and other regulatory requirements. When there 
is no rational reason for differences between the two standards, EPA 
has changed the two sets of rules (see section IV. of this preamble for 
a discussion of changes made to this rule since proposal) to make them 
more consistent.

Regulation of Cement Kilns Under Section 129

    Comment: According to one commenter, the EPA is required to 
regulate any facility that combusts any solid waste under section 129 
of the Clean Air Act. However, EPA's current section 129 regulations 
either: (1) Exempt portland cement kilns that burn any amount of 
hospital waste, medical waste, and infectious waste from the medical 
waste incinerator (MWI) rule, (2) exempt cement kilns that burn less 
than thirty percent waste from the municipal waste combustor (MWC) 
rule, or (3) have yet to be promulgated as the commercial and 
industrial waste rule. The commenter asserts that the EPA cannot fail 
to promulgate section 129 regulations for cement kilns that burn non-
hazardous solid waste by suggesting that it may promulgate section 129 
regulations in the future. Cement kilns would then be permitted to 
combust any of these wastes without complying with section 129, despite 
the fact that the Clean Air Act expressly mandates that any unit 
burning any solid waste must comply with section 129. Therefore, the 
commenter asserts that the EPA must promulgate section 129 standards 
for cement kilns that burn any solid waste now. If EPA cannot 
promulgate section 129 standards immediately, the commenter asserts 
that EPA must, at a minimum, include numerical emission standards for 
the pollutants listed in section 129 (including mercury, cadmium, and 
lead) in its proposed regulations under section 112.
    Response: EPA does not read section 129 as precluding EPA from 
promulgating an interim section 112 (d) standard for portland cement 
kilns which burn non-hazardous solid waste. The interim alternative is 
to have no regulation at all for HAP emissions. This is because the 
only rules implementing section 129 explicitly do not apply to waste-
burning cement kilns (see 40 CFR sections 60.50b(p), 60.32b(m), 
60.50c(g) and 60.32e(g)) and the explanation for these provisions in 62 
FR at 45117 (Aug. 25, 1997) and 62 FR at 48538 (Sept. 15, 1997)). 
Neither the commenter or any other person challenged these provisions, 
and EPA is not reopening the section 129 rules for consideration here.
    EPA does not regard interim non-regulation of non-hazardous waste 
burning cement kilns as a reasonable alternative to including them 
within the scope of these portland cement MACT regulations. Indeed, 
were the Agency to exempt waste burning cement kilns from these MACT 
standards, it would create a strong incentive for cement kilns to burn 
waste to escape MACT regulation. EPA emphasizes, however, as we did at 
proposal, that the standards in today's rule do not represent EPA's 
final determination that only section 112 (d) standards are appropriate 
or required for solid non-hazardous waste-burning cement kilns. Today's 
action does not in any way foreclose an eventual section 129 
standard.1
---------------------------------------------------------------------------

    \1\ Any waste burning cement kiln subject to a section 129 
standard would no longer be subject to these section 112 (d) MACT 
standards. See CAA section 129 (h) (2).
---------------------------------------------------------------------------

    With regard to the commenter's suggestion that EPA adopt specific 
emission limits in this MACT rule for mercury, lead, and cadmium--which 
are pollutants identified in Section 129 for regulation--as EPA 
discussed at proposal, emission limits were considered in the MACT rule 
for these pollutants. As discussed at proposal, EPA was unable to 
identify a MACT floor for mercury. As a result, there is no mercury 
emission limit which can be associated with a MACT floor. The use of 
activated carbon injection (ACI) was considered by EPA as a ``beyond 
the floor'' alternative. However, as also discussed at proposal, based 
on the relatively low levels of existing mercury emissions from 
individual NHW cement kilns and the costs of reducing these emissions 
by ACI, EPA does not consider this beyond the floor alternative 
justified. Thus, no mercury emission limit is included in the final 
MACT rule, and thus would not be included even if this was a section 
129 rule. Finally, as also discussed at proposal, EPA considers PM a 
surrogate for semi-volatile metals (e.g., lead, cadmium, etc.). The 
proposed rule and the final rule include a PM emission limit based on 
the use of MACT. As a result, the final rule achieves reductions in 
emissions of these pollutants consistent with MACT. Furthermore, 
sufficient data do not exist to identify emission limits for lead and/
or cadmium associated with MACT and EPA is unable to establish emission 
limits for these pollutants in this rule. See Sierra Club v. EPA, no. 
97-1686 (D.C. Cir. 1999) slip op. at 15 (EPA is not obliged to 
establish a MACT standard for HAPs for which the Agency is unable to 
quantify emission reductions). Even if such emission limits could be 
developed, however, they would not result in any further reduction in 
emissions beyond that achieved by the MACT rule, given the PM standard.
    Comment: Other commenters believe that cement kilns, irrespective 
of their fuel or raw material mix, should be regulated under the 
portland cement NESHAP and not under section 129 of the Clean Air Act. 
Commenters stated that the EPA's discussion of its authority under 
section 129 is irrelevant to, and inappropriate in, the proposed 
portland cement NESHAP. They said that if EPA intends to regulate 
cement kilns that burn solid waste materials under section 129, the 
proper venue would be in a proposal pursuant to section 129. Commenters 
stated that, based on the discussion of section 129, EPA has apparently 
already determined how it intends to treat solid waste burning cement 
kilns in the section 129 rulemaking. Ten commenters were concerned that 
cement kilns could be subject to different regulations from year-to-
year (or day-to-day) depending on whether they trigger the section 129 
applicability thresholds. The commenters believe that such a regulatory 
structure is confusing, burdensome, inappropriate, and raises serious 
legal issues. Commenters noted that the EPA's proposed regulation of 
solid waste burning cement kilns under section 129 could lead to 
increased fuel consumption and emissions of greenhouse gases as cement 
kilns try to avoid triggering section 129 regulation by not burning 
alternative fuels like solid waste.
    Response: The EPA acknowledges all the comments dealing with the 
potential future regulation under section 129 of the CAA of air 
emissions from cement kilns that burn solid waste (other than hazardous 
waste). Both the proposed and final promulgated portland cement NESHAP 
apply to cement kilns which burn solid waste (other than hazardous 
waste). If the EPA decides in the future that emission standards 
developed under the authority of section 129 of the CAA are warranted 
for cement kilns that burn solid waste, a separate rule will be 
proposed to allow for public comment. The commenters' concerns 
regarding duplicative regulations are misplaced, however. See CAA 
section 129(h)(2)

[[Page 31911]]

(units can't be regulated simultaneously under both sections 129 and 
112(d)(2)).

Regulation Under 112(c)(6)

    Comment: Commenters stated that the EPA should not exercise its 
authority under section 112(c)(6) to regulate dioxin/furan emissions 
from area sources since the area sources have de minimis dioxin/furan 
emissions and regulating them under section 112 will impose significant 
burdens (for reporting, recordkeeping, monitoring, and control 
technology) while providing negligible environmental benefits. These 
commenters further state that EPA's own estimates indicate D/F 
emissions from NHW kilns contribute only 0.8 percent of total 
nationwide D/F emissions. The commenters do not believe that Congress 
intended such a result in drafting section 112(c)(6).
    Response: Regarding the above comments about regulation of D/F 
under section 112(c)(6), the EPA is required by section 112(c)(6) to 
``list categories and subcategories of sources assuring that sources 
accounting for not less than 90 per centum of the aggregate emissions 
of each such pollutant are subject to standards under subsection (d)(2) 
or (d)(4) of this section.'' The method for identifying and selecting 
sources for listing and regulation under these subsections was 
discussed at length in Federal Register notices published on June 20, 
1997 (62 FR 33625) and April 10, 1998 (63 FR 17838). Section 112(c)(6) 
does not provide for de minimis exemptions for source categories, but 
rather directs EPA to make findings on the basis of what is necessary 
to meet the requirement to assure that sources accounting for 90 
percent of the emissions of these pollutants are subject to standards. 
Moreover, because the pollutants addressed by section 112(c)(6) are 
persistent, that is, they remain in the environment for extremely long 
periods of time without breaking down, the EPA believes that any claims 
of de minimis contributions should be considered with great caution, 
and granted in only very exceptional circumstances. Consequently, the 
EPA believes that its decisions in response to section 112(c)(6) 
represent a reasonable exercise of its discretion within the 
constraints of that subsection.
    Comment: Several commenters stated that EPA's proposed action to 
regulate cement kiln ``area sources'' under CAA section 112(c)(6) 
violates the CAA and is arbitrary and capricious. They stated that the 
EPA has improperly proposed to apply the MACT standards to area source 
cement kilns and other HWCs before deciding upon listing criteria and 
preparing the overall list or lists of sources required by that 
provision. In referring to EPA's proposal to regulate area sources of 
112(c)(6) pollutants, they stated their view that only those 112(c)(6) 
pollutants for which a source category is listed under 112(c)(6) should 
be regulated.
    Response: Regarding the initial portion of the above comment, the 
notice of the final source category listing for section 112(d)(2) 
rulemaking pursuant section 112(c)(6) requirements was published April 
10, 1998, in 63 FR 17838-17855. The referenced notice provides the 
required listing of area sources, and therefore the commenter's point 
is moot.
    The proposed rules for NHW kiln portland cement manufacturing would 
only have regulated area sources for
D/F emissions, which is one of the pollutants for which these plants 
are listed as area sources. The pollutants for which portland cement 
NHW kilns were listed under 112(c)(6) are polycyclic organic matter 
(POM), D/F, and mercury. At proposal, the EPA had conducted an analysis 
under section 112(d)(2) for D/F and mercury with respect to 
establishing emission standards, and concluded that area sources of D/F 
should be regulated. The analysis for mercury showed that the MACT 
floor for new and existing sources was no control. The BTF technology, 
use of activated carbon injection, was determined not to be cost-
effective. Therefore, no emission standard was proposed for mercury.
    The preamble for the proposed rule stated that POM emissions (using 
THC as a surrogate) from portland cement NHW kiln area sources would be 
subject to MACT standards under EPA's interpretation of section 
112(c)(6). A THC emission standard was proposed for new raw material 
dryers and new NHW in-line kiln/raw mill main exhausts at cement plants 
that are major sources. At proposal, THC was identified as a surrogate 
for organic HAP emissions, which would include POM. The final rule's 
limits on THC emissions are applicable only to new greenfield kilns, 
in-line kiln raw mills, and raw material dryers, for reasons discussed 
in section IV.C. of this preamble. EPA is clarifying today that since 
THC is a surrogate for POM, the THC emission limits are applicable to 
new greenfield kilns and raw material dryers at cement plants that are 
major and area sources.
    Comment: Several commenters stated their support for an alternative 
interpretation of regulating area sources emitting HAPs listed under 
112(c)(6). They stated that section 112(d)(5) does not exclude area 
source categories listed pursuant to section 112(c)(6) from the 
Agency's discretionary authority to apply GACT standards nor does 
section 112(c)(6) prohibit EPA from exercising its discretionary 
authority under section 112(d)(5). According to the commenters, section 
112(d)(5) grants the Administrator authority to establish GACT 
standards for any area sources listed pursuant to section 112(c), 
whether such sources are listed pursuant to section 112(c)(3) or 
(c)(6). They contended that had Congress intended to exclude section 
112(c)(6) area sources from the GACT standards under section 112(d)(5), 
Congress would have stated this exclusion in section 112(d)(5).
    Another commenter argued against the alternative interpretation 
owing to the bioaccumulation potential of the 112(c)(6) pollutants and 
the fact that the GACT approach would include no floor analysis or 
residual risk assessment.
    Response: Section 112(c)(6) specifically states that EPA is to 
assure that sources of the pollutants to which this subsection applies 
be subject to standards under subsections (d)(2) or (d)(4). These 
subsections refer, respectively, to MACT and standards for pollutants 
for which a health threshold has been established (a null set of 
purposes for this rule). The natural reading of the provision (and at 
the least, a permissible one) is to say that MACT standards apply to 
emissions of 112(c)(6) HAPs from all sources. The alternative reading, 
that GACT requirements could apply because GACT requirements apply in 
lieu of section 112d(2) MACT requirements reads language into section 
112c(6) not apparent on its face. Moreover, where Congress wished to 
reference subsection (d) without limitation, it omitted references to 
specific paragraphs. Compare the language of section 112(c)(6), which 
refers to standards under subsection (d)(2) or (d)(4), with the 
language of section 112(k)(3)(B)(ii), which refers to standards under 
subsection (d). In addition, the reading suggested by the industry 
commenters goes against the natural purpose of section 112c(6), namely, 
to assure that the maximum available control technology is applied to 
control the emission of the most dangerous HAPs. (This is also the 
thrust of the comment summarized above criticizing the reading 
suggested by industry commenters. EPA agrees with this comment.) The 
Agency has therefore concluded that none of the comments provided 
compelling facts or arguments to overcome the interpretation that 
section 112(d)(2) specifically refers to MACT standards.

[[Page 31912]]

Regulatory Flexibility Act and the Small Business Regulatory 
Enforcement Fairness Act

    Comment: Several commenters stated or supported the belief that the 
proposed rulemaking was incorrectly certified, contending that no 
factual basis was provided for the Agency's certification of no 
significant impact on a substantial number of small entities, and thus, 
EPA is not in compliance with provisions of the Regulatory Flexibility 
Act (RFA), 5 U.S.C. 601 et seq. They stated that EPA needs to review 
its certification and provide a factual basis for it or complete an 
initial regulatory flexibility analysis, as required by the RFA.
    The commenters contended the certification was deficient in that 
the Agency's guidance allows regulators to bypass a regulatory 
flexibility analysis if the industry has fewer than 100 firms. 
Furthermore, the seven small companies, representing 16 percent of the 
total number of affected companies, constitutes a ``substantial 
number.'' Some commenters also stated their concern that even at a less 
than one percent cost-to-sales ratio effect on small businesses there 
could be a significant economic impact. Another commenter stated that 
EPA had not evaluated ``reasonable worst case'' impacts for any single 
plant. Several commenters requested more information regarding EPA's 
assessment of small business impacts and steps taken to minimize the 
impacts.
    Response: The following discussion responds to the small business 
impact issues raised by the commenters. In accordance with the RFA, the 
Agency conducted a small business assessment and based its finding of 
``no significant impact on a substantial number of small entities'' on 
the reported impacts of the proposed NESHAP on small businesses within 
the cement industry (Docket Item II-A-46, Table 4-7; Docket Item IV-C-
15). The Agency did not intend to suggest that this certification was 
based solely upon the number of small businesses potentially affected 
by the rule, nor that the Agency sets thresholds for determining 
whether a particular number of businesses is a substantial number or a 
particular impact is a significant impact. The EPA did not certify that 
the rule would have no significant impact on a substantial number of 
small firms based solely on there being less than 100 firms subject to 
the rulemaking (Docket Item II-C-14). To clarify the factual basis of 
EPA's determination and address subsequent comments, a summary of the 
Agency's small business assessment is provided below.
    Based on SBA-defined small business criteria, the Agency originally 
identified nine of the 44 companies within the U.S. cement industry as 
small businesses, or roughly 20 percent of total. However, based on 
updated information and changes in ownership since 1993, the Agency 
determined that four of these companies should not be considered small 
businesses. The APCA indicated that there are currently seven small 
businesses within this industry. This list includes the remaining five 
identified by the Agency plus Dacotah Cement and Royal Cement Company. 
Dacotah Cement is owned by the State of South Dakota and, thus, was not 
considered a small business by the Agency. Royal Cement Company began 
operations in 1995 after the Agency had completed its small business 
assessment and, thus, was not included in the Agency's small business 
assessment because EPA's engineering and economic data base did not 
contain information on this relatively new facility.
    The Agency typically uses the cost-to-sales ratio as a measure of 
impact on small businesses. This ratio refers to the change in the 
annual control cost divided by the annual revenue generated from sales 
of the particular good or goods being produced in the process for which 
additional pollution control is required. It can be estimated for 
either individual firms or as an average for some set of firms such as 
affected small companies. While it has different significance for 
different market situations, it is a good rough gage of potential 
impact. In this case, to develop the cost-to-sales ratios, the Agency 
used the estimated control costs specific to the kilns operating at 
each manufacturing plant owned by a small business divided by their 
baseline cement sales. Contrary to industry's comments, the cost-to-
sales measure of impact used by the Agency is a conservative approach 
and may, in fact, overstate the regulatory burden on small businesses 
for two reasons: (1) The Agency's sales estimate understates company 
sales because it only reflects cement operations and most companies 
have other vertical or horizontal business lines; and (2) this measure 
does not account for the expected market adjustments, i.e., increase in 
market prices that can potentially offset a portion of the regulatory 
costs.
    For the economic impact analyses, the regulatory control costs were 
input to an economic model to predict outcomes at the market and plant 
level, including the impacts for markets served by manufacturing plants 
owned by small businesses. As shown in Table 4-7 of the EIA report 
(Docket Item II-A-46), the Agency did not project any plants or kilns 
owned by the original nine small businesses to close as a result of the 
proposed NESHAP.
    As summarized in the Agency's June 10, 1998, letter to industry 
(Docket Item IV-C-15), a second small business assessment was conducted 
for the small businesses identified by the APCA. The weighted average 
cost-to-sales ratio for these small businesses was 0.93 percent with no 
plants or kilns projected to cease operations (Docket Item IV-B-5).
    A third small business assessment was conducted to include the cost 
of PM CEMs and the monitoring of materials handling operations. (The 
promulgated rule requires the installation of PM CEMs, and more 
frequent monitoring of materials handling operations than included in 
the proposed rule. See Section IV and this section for further 
discussion of these requirements). The new weighted average cost-to-
sales ratio for the small businesses was 1.4 percent with no plants or 
kilns projected to cease operations. See Docket Item IV-B-11 for the 
resulting company-specific cost-to-sales ratios for this third 
analysis. Further, to measure the relative regulatory burden on small 
businesses, these impacts at small businesses can be compared to those 
for the whole industry. See Docket Item IV-A-4 for this comparison.
    As discussed above, based on the Agency's revised small business 
impacts assessments, which now include the cost of PM CEMs and other 
monitoring costs not considered at proposal, the Agency concludes that 
this NESHAP as promulgated today will not have a significant impact on 
a substantial number of small businesses. Nevertheless, EPA will 
reassess, as appropriate, small business impacts in the future proposed 
rulemaking that will establish the date that PM CEMs must be installed 
on NHW cement kilns.
    Comment: One commenter stated that EPA must have objective, 
reasonable certainty that there will be no pertinent impacts on small 
entities or it cannot validly certify. The EPA must create a testable 
record against which the validity of certifications could be judicially 
reviewed. 5 U.S.C. 611(a) and (b). The commenter further claimed that 
EPA's SBREFA Guidance states that when EPA ``cannot or does not certify 
that a proposed rule will not have a significant impact on a 
substantial number of small entities, it must prepare a regulatory 
flexibility analysis for the proposed rule.'' The commenter

[[Page 31913]]

does not believe EPA has met this burden for the proposed rule.
    Response: Section 605(b) provides an exemption from the 
requirements in sections 603 and 604 to conduct a regulatory 
flexibility analysis when the Agency ``certifies that the rule will 
not, if promulgated, have a significant economic impact on a 
substantial number of small entities.'' The EPA has made this 
certification for the rulemaking. The EPA believes its interpretation 
of the requirements of the RFA is reasonable and that its factual basis 
for certification is also reasonable.
    To the extent that the commenter is suggesting that the RFA 
requires more than a reasonable basis for its decision to certify, the 
EPA disagrees. Courts review compliance with the RFA in accordance with 
Chapter 7 of the Administrative Procedure Act (APA), 5 U.S.C. 701, et 
seq. See 5 U.S.C. 611(a)(1) and (2). Under the APA, courts generally 
provide substantial deference to agency decisionmaking and will only 
set aside administrative actions or findings if the court concludes 
that the agency's action or finding was arbitrary, capricious, or 
otherwise contrary to law. 5 U.S.C. 706(2)(A). The Supreme Court has 
explained, ``To make this finding the court must consider whether the 
decision was based on consideration of the relevant factors and whether 
there has been a clear error of judgement.'' Citizens to Preserve 
Overton Park v. Volpe, 401 U.S. 415 (1971). The EPA believes that its 
detailed economic analysis more than adequately supports its conclusion 
that the rule will not result in a significant impact on a substantial 
number of small entities.
    Comment: The same commenter believes SBREFA can only be interpreted 
to allow numerical cutoffs based on the percentage of all small 
entities in the regulated universe that experience any impact. The 
commenter contends that when a rule impacts all the small entities in 
an industry, the statute a fortiori requires an analysis of whether 
those impacts are significant, and precludes a certification based 
solely on any absolute number of small entities impacted. By the same 
token, if the percentage of small entities experiencing any impact is 
more than de minimis, a similar analysis appears required. The 
commenter contends that this concept has been repeatedly recognized by 
EPA findings that impacts on more than 20 percent of the small entities 
within a universe proposed to be regulated constitute a ``significant 
number.'' 61 FR 48206, 48228 (September 12, 1996); 59 FR 62585, 62588 
(December 6, 1994). It also lies at the heart of the ``impacts'' matrix 
in EPA's SBREFA Guidance. The commenter notes that under that matrix, 
greater ``impact'' priority is assigned to rules that will impact a 
larger percentage of small entities, even if the impacts are relatively 
low.
    Response: Other than small entities, the RFA does not define the 
term, or any part of the term, ``significant impact on a substantial 
number of small entities.'' Thus, the statute does not specify whether 
an agency may properly certify a rule either because there is not a 
significant impact on small entities, or because, even if the impact is 
significant, there are not a substantial number of small entities 
affected. In any event, the EPA has chosen not to establish any 
mechanistic approach for determining when an impact is significant or 
when the number of small entities is substantial. Instead the EPA 
considers a variety of approaches depending on the particular 
circumstances of the rulemaking. In general, the EPA looks at both the 
extent of the potential impact and the number of small entities 
impacted to decide whether a more detailed regulatory flexibility 
analysis pursuant to sections 603 and 604 of the RFA is warranted. The 
EPA's Guidance repeatedly explains that the criteria offered in the 
Guidance cannot be applied mechanistically and that rule writers should 
consider other relevant information in deciding whether or not to 
certify a rule.
    EPA's analysis of both the number of small entities impacted and 
the extent of that impact are described in previous responses in this 
section of this preamble, and as indicated above, the EPA has not 
certified this rulemaking based solely on the number (or percentage) of 
small entities.

Economic Impact Analysis

    Comment: Several commenters believe that the final EPA economic 
analysis at proposal was inaccurate and should be either revised to 
reflect industry's comments (in Attachment G to docket item IV-D-26) or 
withdrawn. Another commenter stated that EPA's model economic impacts 
data are seriously flawed because:
    1. The model would not detect company-level impacts.
    2. The economic analysis is not based on any estimate or analysis 
of actual small-entity impacts but is based on an aggregated industry 
wide economic model based on theoretically constructed model kilns.
    3. The model predicts that older smaller dry kilns will close, 
which is counterintuitive because wet kilns are substantially more 
costly to operate per unit of product.
    4. Flaws in the market-specific part of the model which lead 
directly to the modeled conclusion that profits will increase with more 
stringent control.
    Response: The EPA disagrees with the preceding comments suggesting 
the analysis is inaccurate and should be withdrawn. The Agency 
developed its economic analysis based on the best available information 
using an accepted approach firmly rooted in economic theory to provide 
the necessary impact results to satisfy legislative and administrative 
requirements. Furthermore, the Agency conducted a revised economic 
impact analysis in response to the additional monitoring requirements 
for cement kilns and materials handling operations at major source 
cement plants (as fully described in Appendix G recently added to the 
July 1996 EIA report, Docket Item II-A-46). In conducting this revised 
analysis, the Agency also updated the original 1993 baseline 
information that supported the economic analysis for proposal to 1995 
and is thereby consistent with the baseline used by the Agency for the 
Cement Kiln Dust (CKD) rulemaking and Hazardous Waste Combustion MACT 
Standards. This adjustment to the baseline characterization results in 
some differences in the projected economic impacts from the proposal 
analysis. In particular, under 1995 baseline conditions, the model 
predicts an aggregate loss in industry profits because of the sharp 
reduction in excess U.S. cement capacity from 1993 to 1995. This 
increase in capacity utilization to roughly 94 percent in 1995 severely 
limits the ability of unaffected (and slightly affected) domestic 
producers to offset production declines at affected cement plants. As a 
result, the potential profit gains to these producers from offsetting 
these reductions is no longer present in 1995 as in 1993 and the 
economic model predicts an aggregate loss in pre-tax earning of the 
U.S. industry, which is consistent with the expectations of the 
commenter. However, this occurs through the difference in baseline 
characterization rather than flaws in the Agency economic model and 
approach.
    The following responses address the above comments that are 
specific to the economic analysis conducted for the regulation as 
originally proposed. First, the comments are specific to a draft 
version of the EIA report that has been revised. Comments were 
addressed in changes to the analysis prior to proposal as follows:

[[Page 31914]]

    1. As the commenter suggested, the economic model incorporated a 
more realistic assumption for the elasticity of supply from foreign 
imports.
    2. According to the commenter the draft EIA report did not 
adequately describe the basis for defining the regional markets used in 
the economic analysis and led to some confusion and/or 
misinterpretation by the industry as reflected in its comments. 
Contrary to assertions, the Agency's economic model does not omit any 
market areas as all U.S. production and consumption of cement is 
accounted for within the 20 regional markets as defined by the Agency. 
The Agency utilized the best available information in defining regional 
markets to better account for the regional competition within the 
industry.
    3. The commenter claimed the draft EIA report did not adequately 
describe the basis for selecting the imperfectly competitive market 
structure for the cement industry and the implications of this 
selection of the economic impact results. The Agency's selection of 
market structure was not an attempt to distort the economic impact 
results or to infer that the industry is collusive and lacks any 
competition. Rather it was selected to provide better estimates given 
well-known characteristics of the industry. The Agency has 
appropriately modeled the competitive interaction between domestic 
producers of cement as well as foreign imports (where applicable) 
within each regional market in a manner that is consistent with the 
empirical evidence for cement markets and economic theory.
    In regard to the statement that the economic impact data are flawed 
and accompanying reasons, the Agency responds as follows:
    1. The economic impact analysis does allow the Agency to detect 
company-level impacts by aggregating the estimated control costs and 
related economic impacts at all manufacturing plants owned by each 
company, both large and small. Although the issue of capital 
availability is an important consideration for small businesses, it is 
not typically addressed in EPA economic analyses of regulatory actions 
as it requires company-specific information not available to the Agency 
and, moreover, there is not a generally accepted method with which to 
model and analyze this complex issue in the context of environmental 
regulation.
    2. The Agency's characterization of costs at individual kilns was 
based on the econometric estimation of cost functions for cement kilns 
by Das (1991 and 1992). Using the best information available, the EPA 
made adjustments to these cost functions to better reflect the 
operating costs of kilns by process type and capacity (as fully 
described in Appendix C, Docket Item II-A-46). However, in accounting 
for size or economies of scale in estimating baseline operating costs, 
the Agency was limited by the two capacity size classifications of less 
than and greater than 500,000 short tons per year for which labor 
productivity and fuel consumption were reported by the Portland Cement 
Association. This data limitation prevents the EPA from developing 
baseline cost functions for very small kilns and, effectively, ``lumps 
smaller kilns in with mid-size kilns into a larger class'' of all kilns 
as stated by industry. Therefore, it is possible that the EPA's 
economic model understates the baseline operating costs at very small 
kilns. However, the Agency is able to estimate the incremental 
compliance costs for many categories of kiln capacity below 500,000 
short tons per year ranging from 55,000 to 450,000 short tons per year. 
This more detailed classification scheme for estimating the regulatory 
compliance costs reduces the uncertainty related to the Agency's 
estimates of kiln closures.
    3. The Agency agrees with the industry comment that wet kilns are 
generally more costly to operate, which has contributed to their use of 
hazardous waste to reduce their fuel costs and remain competitive with 
the dry process kilns, especially those using precalciner and/or 
preheater technologies. However, the economic impacts of the proposed 
NESHAP depend not only on the baseline costs of cement production but 
also on the incremental costs of compliance for each kiln. The proposed 
NESHAP largely impacts non-hazardous waste burning kilns as opposed to 
hazardous waste kilns that are most often wet process kilns. As stated 
in the EIA report, it is the higher relative incremental cost impact 
compared to that for its competitors that causes the Agency's model to 
project closure for two dry process kilns under the proposed NESHAP. 
Furthermore, the baseline costs of cement production were high for 
these kilns because they were each older and smaller than average. 
Thus, the projected closures are actually consistent with the 
commenter's statement that older and smaller kilns are more vulnerable 
to closure with regulation. Moreover, in the final EIA report, the 
Agency provides closure estimates for additional regulatory 
alternatives and, for more stringent ``above-the-floor'' alternatives, 
the economic model projects up to 10 kilns to close including 5 wet 
process kilns. Thus, the Agency believes that its economic model 
produces closure estimates that are consistent with the commenter's 
characterizations.
    4. Although the Agency projects a net increase in profits for the 
cement industry as a whole in response to regulation, there is a 
``social cost'' to reducing hazardous air emissions from the 
manufacture of cement. As shown in the final report, the Agency 
estimates that society must give up $34.5 million per year for the 
expected environmental benefits (as compared to the $28.8 million in 
regulatory compliance costs incurred by industry after market 
adjustments). Furthermore, factors cited by industry are not the reason 
for the model's prediction of a net increase in profits for the 
industry as a whole. The Agency believes that it has appropriately 
modeled the competitive interaction between domestic producers of 
cement as well as foreign imports (where applicable) within each 
regional market in a manner that is consistent with the empirical 
evidence for cement markets and economic theory.
    Related to the net increase in profits for the industry as a whole, 
several commenters were surprised that the economic analysis predicts 
an increase in cement plants' pretax earnings. They interpreted this as 
applying to individual plants, which is a misinterpretation. The 
economic analysis projects a net increase in the U.S. cement industry's 
pre-tax earnings, which reflects profit gains at unaffected or 
relatively less affected cement plants and profit losses at affected 
plants that incur higher relative compliance costs. Thus, the 
commenter's statement that each cement plant's pre-tax earnings will 
increase by X dollars for every dollar spent on compliance is incorrect 
as these impacts are distributed across different plants. Also, the 
estimated price increase applies to all cement produced by U.S. 
manufacturing plants whereas the MACT compliance costs apply only to 
cement produced at affected plants. Therefore, the commenter's 
calculation of the projected price increase as a share of MACT 
compliance costs is also incorrect as the commenter is understating the 
relevant change in cost by dividing the MACT compliance costs by all 
cement produced rather than only the affected share of cement 
production. The projected increase in pre-tax earnings is a net result 
for the industry that results from losses at some cement plants that 
are offset by gains at other cement plants.

[[Page 31915]]

PM CEMs

    Comment: Numerous comments were received stating that the EPA has 
not fully considered the impacts of a potential requirement for PM CEMS 
applied to NHW kilns, and that PM CEMs have not been adequately 
demonstrated on cement kilns.
    Response: In the preamble to the proposal, EPA noted its intent to 
include a requirement for PM continuous emission monitoring system 
(CEMS) in the final rule, unless the analysis of existing or newly 
acquired data and information showed that it is not appropriate (see 63 
FR at 14205). Based on successful testing on an incinerator conducted 
in the interim, as well as extensive use of these monitors in Europe, 
EPA believes there is sound evidence that PM CEMS should work at cement 
kilns. In addition, preliminary analyses of the cost of PM CEMS applied 
to cement kilns (docket items IV-C-1 and IV-C-21) and hazardous waste 
combustors (HWC) suggest that these costs are reasonable. Accordingly, 
the final rule contains a requirement to install PM CEMS. However, we 
agree with comments that indicate a need to develop cement kiln-
specific performance requirements for CEMS and to resolve other 
outstanding technical issues. These issues include all questions 
related to implementation of the CEM requirement (i.e. relation to all 
other testing, monitoring, notification, and recordkeeping), relation 
of the CEM requirement to the PM emission standard, as well as 
technical issues involving performance, maintenance and correlation of 
the CEM itself. These issues will be addressed in a subsequent 
rulemaking. Therefore, we are deferring the effective date of this 
requirement pending further testing and additional rulemaking. As a 
result, in today's final rule, EPA is requiring that particulate matter 
continuous emission monitoring systems (PM CEMS) be installed at cement 
kilns. However, since the Agency has not finalized the performance 
specifications for the use of these instruments at cement kilns or 
resolved some of the technical issues noted above, we are deferring the 
effective date of the requirement to install, correlate, maintain and 
operate PM CEMS until these actions can be completed. The PM CEMS 
installation deadline will be established through future rulemaking, 
along with other pertinent requirements, such as final Performance 
Specification 11, Appendix F Procedure 2. It should finally be noted 
that EPA has a concurrent rulemaking process underway for hazardous 
waste combustors (HWC) and plans to adopt the same approach in that 
rule.
    EPA also is taking action now to avoid facilities being in 
violation of the PM standard during CEM correlation testing. Commenters 
properly observed that CEM correlation testing would require sources to 
manipulate their PM control device during correlation tests to obtain 
higher PM emissions levels than the emission limit. It is necessary to 
do so because a good PM CEMS correlation must include CEMS and manual 
method data above the stated emission standard in order to have a wide 
enough range of data to meet the correlation coefficiency statistical 
requirement and to assure that calibrated readings above the level of 
the emission standard can be properly interpreted. Such data, however, 
could be misconstrued by state or local enforcement authorities or 
citizens as violations of the PM standard. It is important to address 
this issue now to encourage the development of additional PM CEMS data, 
and not to discourage facilities from choosing to install a CEM before 
the deferred effective date.
    We are addressing this concern here in the same manner we plan to 
address it in the HWC MACT rule by providing that the particulate 
matter and opacity standards of parts 60, 61, 63 (i.e., all applicable 
Parts of Title 40) do not apply during particulate matter CEMS 
correlation testing, provided that you comply with certain provisions 
discussed below that ensure that the provision is not abused. EPA is 
also making this provision effective immediately, so that sources need 
not wait for the compliance date to take advantage of this particulate 
matter CEMS correlation test provision. We believe this approach 
adequately addresses commenters' concerns.
    The temporary exemption from particulate matter and opacity 
standards is conditioned on several requirements. Sources are required 
to develop and submit to permitting officials a PM CEMS correlation 
test plan along with a statement of when and how any excess emissions 
will occur during the correlation tests (i.e., how you will modify 
operating conditions to ensure a wide range of particulate emissions, 
and thus a valid correlation test). If the permitting officials fail to 
respond to the test plan in 30 days, the source may proceed with the 
tests as described in the test plan. If the permitting officials 
comment on the plan, the source must address those comments and 
resubmit the plan for approval. In addition, runs that exceed any PM or 
opacity emission standard are limited to no more than a total of 96 
hours per correlation test. This 96 hours is sufficient time for a 
source to increase emissions to the desired level and reach system 
equilibrium, conduct testing at the equilibrium condition followed by a 
return to normal settings indicative of compliance with emissions 
standard(s) after those higher emissions data have been obtained, and 
return to equilibrium at normal conditions. Finally, to ensure these 
periods of high emissions are due to the bona fide need described here, 
a manual method test crew must be on-site and making measurements (or 
in the event some unforeseen problem develops, prepared to make 
measurements) at least 24 hours after you make equipment or workplace 
modifications to increase PM emissions to levels of the high 
correlation runs.

Selection of Emission Limits in General

    Comment: One commenter stated that according to section 112(d) EPA 
may not base the floors of its emission standards on a particular 
technology. Instead, emission standards for existing sources must be no 
less stringent than ``the average emission limitation achieved by the 
best performing twelve percent of the existing sources'' (for which EPA 
has data). The commenter further stated that for new sources, standards 
must be based on the emission control that is achieved in practice by 
the best controlled similar source. Thus, the standards proposed for 
emissions of dioxins, mercury, total hydrocarbons, and hydrogen 
chloride are not valid.
    Response: First, it should be noted most of the commenter's points 
were recently rejected by the DC Circuit in Sierra Club v. EPA (March 
2, 1999). That case holds that because MACT standards must be 
achievable in practice, EPA must assure that the standards are 
achievable ``under most adverse circumstances which can reasonably be 
expected to recur'' (assuming proper design and operation of control 
technology). Slip op. p. 13. The case further holds that EPA can 
reasonably interpret the MACT floor methodology language so long as the 
Agency's methodology in a particular rule allows it to ``make a 
reasonable estimate of the performance of the top 12 percent of 
units'', slip op. p. 7; that evaluating how a given MACT technology 
performs is a permissible means estimating this performance, id. at 13; 
and that new source standards need not be based on performance of a 
single source, id.
    Second, the commenter provided no additional emissions data for any 
pollutant. The EPA has selected emission limits at the floor level of

[[Page 31916]]

control. Section 112(d) requires EPA to promulgate emission standards 
based on what is determined to be achievable through the application of 
techniques, methods, etc. The rule does not require the use of any 
specific technology to meet the emission standard. The emission 
standards are based on the emissions levels achieved through the 
application of MACT floor technologies and account for variation in the 
process and in the air pollution control device effectiveness.
    Although the commenter did not specifically mention PM, the 
following discussion using PM as an example will help clarify EPA's 
approach in setting MACT standards for this source category. The EPA 
evaluated the PM MACT floor technology for both existing and new 
sources at proposal and determined that the MACT floor technology is 
properly designed and operated FFs and ESPs. Commenters provided no 
data to suggest that a particular design or operating mode, or an 
alternative technology could achieve a lower level of PM emissions on a 
consistent basis. Nor did EPA identify other technologies for existing 
or new kilns or in-line kiln/raw mills that would consistently achieve 
lower emission levels of PM than the NSPS limit.
    As discussed in docket item number IV-B-10, the data upon which the 
MACT floor was based were obtained from EPA Method 5 compliance tests 
on kilns subject to the NSPS and represent performance of PMCDs 
associated with new kilns over a relatively short period (typically 
three 1-hour test runs). These test data were obtained at kilns 
equipped with well designed and operated ESPs and FFs representative of 
the MACT floor, which is also represented by the NSPS emission level. 
Method 5 testing of these cement kilns equipped with MACT floor 
technology showed a range of emissions up to the NSPS level. Additional 
Method 5 tests performed on some of the same kilns included in the MACT 
floor analysis showed PM variations after control as plotted in docket 
item IV-B-10. EPA believes that the data base--which shows cement kilns 
with properly designed and operated fabric filters and electrostatic 
precipitators achieving levels up to and including the NSPS level--
adequately accounts for the variability inherent in the air pollution 
control technologies, and indicates what PM levels are consistently 
achievable in practice. See Sierra Club, slip op. p. 13. In summary, 
the PM emission limit reflects an emission level consistently 
achievable with the use of well designed and operated MACT floor 
technology.
    The emission standard for dioxin is based on the emission level 
achievable through the application of the MACT floor control 
technology, which is exhaust gas temperature control at the inlet to 
the PM control device to less than 400 deg. F, and efficient 
combustion. Based on data evaluated at proposal, the technology can be 
represented by the dual standard of 0.2 ng TEQ/dscm or 0.4 ng TEQ/dscm 
with a PM control device inlet temperature of 400 deg. F or less. Since 
the commenter provided no additional data, the EPA has reviewed, in 
response to this comment, the existing test data and literature on D/F 
formation and concluded that the selected emission limits are 
consistently achievable and represent the MACT floor. Similar to the 
discussion above regarding the PM data, the D/F performance test data 
are based on short-term tests of facilities using the MACT floor 
technology. Thus the proposed emission limits are retained and account 
for normal, inherent process and air pollution control operating 
variability, including the use of various fuels.
    As discussed in the proposal preamble, there are no standards for 
THC emissions from existing sources because the MACT floor for control 
of THC for existing sources is no control. Further, the BTF control 
technique for existing sources, and a floor control for new sources, 
would be based on the performance of precalciner/no preheater 
technology. However, as discussed in the proposal, EPA rejected this 
technology as a basis for setting THC emission limits because of the 
technology's negative environmental and energy impacts. The basis for 
the THC limit for new greenfield kilns is site selection to ensure low 
hydrocarbon content in feed materials. (In the proposal, the THC limit 
applied to all new kilns, but based on comments received, the rule has 
been changed such that the THC limit will only apply to new greenfield 
kilns. See comment responses regarding this issue for more detail.) As 
discussed in the proposal, this option is not available to existing 
(and new brownfield) kilns, in that facilities are generally tied to 
existing raw material sources in close proximity to the facility, so 
that raw material proximity (i.e., transportation cost) is usually a 
major (indeed, critical) factor in plant site selection.
    As discussed in the proposal preamble, no standards are being 
adopted for Hg and HCl because the MACT floor has been determined to be 
no control and the BTF controls were not cost effective (docket item 
II-B-67).
    This standard was developed under section 112, not section 129, so 
there is no statutory requirement to establish standards for individual 
HAP metals. However, control of cadmium, lead, and other non-volatile 
and semi-volatile metal HAPs is achieved via the floor level-based 
emission limit for PM, which serves as a surrogate for the non-volatile 
and semi-volatile metals. This is supported by data from coal-fired 
electric utility boilers which show relatively high HAP metals (except 
mercury) removal with fabric filters and electrostatic precipitators. 
(Study of Hazardous Air Pollutant Emissions from Electric Utility Steam 
Generating Units--Final Report to Congress, volume 1, 453/R-98-004a, 
February 1998, p. 13-23 and 13-26).

PM Limits

    Comment: Numerous commenters supported the use of PM as a surrogate 
for non-volatile HAP metals. One commenter questioned the use of PM as 
a surrogate for HAP metals, and suggested that the EPA require stack 
testing for specific metal content.
    Response: The final rule retains the use of PM as a surrogate for 
HAP metals because the MACT floor equipment and level of control for 
HAP metals, i.e., properly designed and operated fabric filters (FFs) 
and electrostatic precipitators (ESPs), is identical to that for PM. 
Using PM as a surrogate for specific HAP metals eliminates the cost of 
performance testing to comply with numerous standards for individual 
metals, and achieves exactly the same level of HAP metal emissions 
limitation.
    Comment: Although many commenters were in favor of the MACT floor 
determination and associated emission limit for PM (see docket item, 
number to be assigned), several other commenters suggested that more 
stringent PM standards were required in recognition of the performance 
test data presented in the preamble showing that many affected sources 
achieved lower levels of PM emissions than the proposed standard.
    Response: The proposed PM standards have been retained in the final 
rule. EPA evaluated the MACT floor technology for both existing and new 
sources at proposal and determined that the MACT floor technology is 
properly designed and operated FFs and ESPs. Commenters provided no 
data to support that an alternative design or technology represents a 
floor that could achieve a lower level of PM emissions on a consistent 
basis. The EPA did not identify other technologies for existing or new 
kilns or in-line kiln/raw mills that would consistently achieve lower 
emission levels of PM than the NSPS limit.

[[Page 31917]]

    As discussed in the proposal preamble, the data upon which the MACT 
floor was based were obtained from EPA Method 5 compliance tests on 
kilns subject to the NSPS and represent performance of PMCDs associated 
with new kilns over a relatively short period (typically three 1-hour 
test runs). These test data were obtained at kilns equipped with well 
designed and operated ESPs and FFs representative of the MACT floor, 
which is also represented by the NSPS emission level. Method 5 testing 
of these cement kilns equipped with MACT floor technology showed a 
range of emissions up to the NSPS level. Additional Method 5 tests 
performed on some of the same kilns included in the MACT floor analysis 
showed PM variations after control as plotted in the reference, 
confirming that some operating variability is inherent. EPA believes 
that these data reasonably represent levels achievable in practice by 
the average of the best performing 12 percent of sources, and by 
accounting adequately for variability, further assure that the standard 
will be achievable under the worst forseeable circumstances consistent 
with proper design and operation. Sierra Club, slip. op. p. 13. In 
summary, the PM emission limit reflects an emission level consistently 
achievable with the use of well designed and operated MACT floor 
technology.
    Comment: One commenter stated that it is feasible, both technically 
and economically, for portland cement kilns to use fuels and raw 
materials with low metals content. Because feed limits are an 
achievable measure that would further reduce emissions, EPA must 
require them.
    Response: Feed and/or fossil-fuel switching has not been undertaken 
by any NHW kilns to reduce metals emissions, and therefore this is not 
a MACT floor option.
    The use of feed material selection and feed material blending to 
achieve lower metals emissions thus is a potential beyond-the-floor 
technology. Cost is a consideration in the decision to go beyond-the-
floor. The ability of a facility to remain cost competitive typically 
depends on the use of raw materials mined in close proximity to the 
facility. Several commenters described the economic difficulties in 
locating, purchasing, and transporting feed materials to existing 
sites; the comment to the contrary stated the opposite categorically, 
but provided no supporting cost, economic or technical data. See Sierra 
Club, slip op. p. 13 (rejecting argument that pollution prevention 
measures had to be included as part of a standard where costs were not 
adequately quantified). EPA disagrees with this comment. Cement kilns 
require enormous amounts of raw material, and the costs of transporting 
the raw material are enormous, given the volumes involved. Finding a 
new source of raw material will often (if not invariably) entail more 
costs because the source of the raw materials will be further from the 
facility. The Agency believes that in many cases a facility could not 
even remain economically viable were existing sources of raw material 
to become unavailable. In many cases, costs of the change in raw 
material would exceed air pollution benefits.2
---------------------------------------------------------------------------

    \2\ As discussed above, EPA considered control of feed materials 
as a potential beyond the floor technology. EPA is aware of the 
Conference Report to the 1990 amendments which state that controls 
on feed materials are not to be part of MACT for mineral processing 
facilities. H.R. Rep. No. 952, 101st Cong., 2d sess. 339. 
However, the text of the statute does not reflect this legislative 
history, stating unambiguously that MACT for all sources includes 
eliminating HAP emissions through ``substitution of materials''. 
Section 112 (d) (2) (A). EPA is following the explicit statutory 
text in considering (albeit rejecting) feed control as a potential 
beyond the floor technology in this rule. At the very least, this is 
a permissible interpretation of the statute, given the statutory 
goal of protecting and enhancing of the Nation's air resources. 
Section 101 (b)(1).
---------------------------------------------------------------------------

    In the case of NHW kilns, fuel switching is not a demonstrated 
metals control technology. There are no data available to EPA that 
indicate that this technology can or has achieved metals emission 
reductions from NHW kilns. A HW kiln operator can control metals via 
the hazardous waste fuel, but this is not an option available to NHW 
kiln operations.

D/F Limits

    Comment: Several comments were received regarding the D/F limits in 
the proposed rule, which were based on the MACT floor. Some commenters 
suggested that a lower D/F emission limit was appropriate for both new 
and existing sources, based on the performance test data reported in 
the proposal preamble. Other commenters felt that the proposed emission 
limit was too stringent and unjustified, and was not representative of 
the MACT floor technology. Many other commenters supported the proposed 
standards.
    Response: In response to these comments, the EPA has reviewed the 
existing test data and literature on D/F formation and concluded that 
the selected emissions limits represent the MACT floor and are 
consistently achievable. Again, EPA is influenced by the fact that 
cement kilns using the floor control technology achieved different D/F 
levels in their performance tests--indicating that different levels 
reflect normal variability of the process and control technology. 
Consequently, EPA is retaining the proposed standard for D/F emissions 
from kilns and in-line kiln/raw mills in the final rule.
    In order to establish a more stringent emission limit for new 
kilns, it is necessary to identify a different technology to which 
better performance is attributable. Since EPA could not identify a 
different technology for new kilns, the standard is based on the range 
of available data, considering process and control variability.
    The EPA determined that the MACT floor technology for both existing 
and new sources was inlet PM control device temperature control to 
400 deg. F accompanied by good combustion and process control. Based on 
data evaluated at proposal, the technology can be represented by the 
dual standard of 0.2 ng TEQ/dscm or 0.4 ng TEQ/dscm with a PM control 
device inlet temperature of 400 deg. F or less. The performance test 
data are based on short-term tests but do indicate that all kilns will 
achieve the numerical emission limit of 0.4 ng TEQ/dscm with the 
application of the floor technology. Thus the 0.4 ng TEQ/dscm emission 
limit is retained to account for normal inherent process and air 
pollution control operating variability, including the use of various 
fuels, such as tires.

THC Limit

    Comment: Several comments were received questioning the 
specification of a THC standard for reconstructed kilns or new kilns 
built at existing sites. Commenters asserted that these facilities 
could not economically locate, purchase and transport suitable feed 
materials to meet this standard.
    Response: In recognition of these comments, the final rule has been 
changed to make the THC limitation applicable only to greenfield kilns, 
greenfield in-line kiln/raw mills and greenfield raw material dryers. 
EPA agrees that only greenfield sources would be able to apply MACT, 
which is the site selection of feed materials with low levels of 
naturally occurring organic material. The EPA considered the use of 
precalciner/no preheater kilns for THC control, (docket items II-B-47, 
II-B-48, II-B-67, and II-B-76), but concluded that because of negative 
energy impacts and increased emissions of criteria pollutants these did 
not provide the maximum achievable control technology for either 
existing or new sources. Further discussion of this technology is 
provided in the response to the next comment.

[[Page 31918]]

    Comment: Commenters stated that the proposed rulemaking provides no 
justification or insufficient support for the selection of 50 ppmvd as 
the total hydrocarbon (THC) standard for new or modified kilns. Another 
commenter noted that EPA has recognized that portland cement kilns use 
a variety of methods and technologies to control their THC emissions, 
including precalciner/no preheater technology and a combination of feed 
material selection, site location, and feed material blending. All of 
these methods and technologies are reflected in existing sources' 
actual performance, on which EPA must base the floors for its THC 
standard. That commenter stated that under section 112(d) the THC 
emission standard would be much lower than 50 ppmvd.
    Response: First, with regard to the methods and technologies 
determined to be the MACT floor, the ``precalciner, no preheater'' kiln 
is not considered maximum achievable control technology when other 
considerations such as energy impacts and NOX emissions are 
taken into account. As explained in the preamble to the proposed rule, 
EPA believes that use of these technologies would not be MACT for new 
or existing sources because of the adverse environmental impacts 
associated with these technologies' use, in particular increased 
emissions of certain criteria pollutants. See Portland Cement Assn v. 
Ruckelshaus, 486 F. 2d 375, 385-96 (D.C. Cir. 1973) (if use of a 
particular technology results in other, adverse environmental 
consequences, that technology need not be considered the ``best''). The 
proposal preamble also addressed consideration of feed material 
selection for existing sources as a MACT floor technology and concluded 
that this option is not available to existing (and new brownfield) 
kilns, in that facilities are generally tied to existing raw material 
sources in close proximity to the facility, and that raw material 
proximity (i.e., transportation cost) is usually a major factor in 
plant site selection. This conclusion was supported by several 
commenters. The commenters described the economic difficulties in 
locating, purchasing, and transporting low organic feed materials to 
existing sites. However, for new ``greenfield'' kilns, feed material 
selection as achieved through appropriate site selection and feed 
material blending is considered new source MACT.
    With regard to the level of standard, it is based upon data 
available to the Administrator and no data were provided after proposal 
which would justify a different standard. Based on a review of 
available information (docket item II-B-62, docket item II-B-75, docket 
item II-D-195) the EPA believes that a THC concentration of 50 ppmvd 
represents a level that is achievable nationwide across a broad 
spectrum of feed materials. This level has been retained in the final 
rule.
    Comment: Comments were received concerning the suitability of THC 
as a surrogate for organic HAP, in light of the high variability in the 
ratio of organic HAP to THC in cement kiln exhaust gas.
    Response: The EPA recognizes the variability of the data but 
concludes that when speciated analyses of THC were undertaken organic 
HAPs were found to be present. No attempt was made to correlate organic 
HAP emissions with THC emissions. Because of the cost savings to 
industry in conducting performance tests to establish compliance with a 
THC standard, EPA has chosen not to set standards for individual 
speciated organic HAPs. Further, since the source of organic HAPs is 
the same source as for THC (feed materials), using MACT will also 
control organic HAP emissions. Adopting THC as a surrogate will result 
in cost savings to the cement industry and to the EPA during compliance 
testing and monitoring.
    The EPA notes further that the same issue was presented when EPA 
adopted standards for boilers and industrial furnaces burning hazardous 
waste, and in the course of that rulemaking, not only the Agency but 
the Science Advisory Board concluded that THC was indeed a reasonable 
surrogate for toxic organic emissions from cement kilns. [See 56 FR at 
7153-54 (Feb. 21, 1991).]
    The proposal preamble stated that POM, one of the seven pollutants 
listed in section 112(c)(6), would be regulated using THC as a 
surrogate. The final source category listing notice for section 112(d) 
rulemaking pursuant to section 112(c)(6) requirements shows the NHW 
kiln facilities portion of the portland cement source category to be a 
significant source of POM (63 FR 17838, April 10,1998). For this 
reason, and to control other THC HAPs, the final rule limits emissions 
of THC from new greenfield raw material dryers and new greenfield kilns 
and greenfield in-line kiln/raw mills at area sources as well as major 
sources.

Mercury Limit

    Comment: Comments were received concerning the need for an emission 
standard to limit the emissions of mercury from NHW cement kilns. Other 
commenters suggested that a mercury standard be established based on a 
presumed floor or beyond the floor basis of fuel and/or feed material 
control, referring to the proposed Hazardous Waste Combustor rules and 
research on clean coal to reduce mercury emissions in the electric 
utility industry. Other commenters agreed with EPA's determination for 
no mercury emission limit.
    Response: The EPA determined, at proposal, that the MACT floor for 
both new and existing sources was no control. The EPA evaluated 
activated carbon injection as a beyond the floor alternative for 
control of mercury emission from NHW kilns and in-line kiln/raw mills, 
and this technology was not found to be cost effective. Feed and/or 
fossil-fuel switching or cleaning has not been undertaken by any NHW 
kilns in order to reduce mercury emissions, and therefore these are not 
MACT floor options. For this reason feed and/or fossil-fuel switching 
or cleaning would be considered a beyond the MACT floor option but the 
EPA does not have data, nor did commenters provide data, that show that 
this option would consistently decrease mercury emissions. Moreover, as 
noted earlier, raw material feed control is prohibitively costly for 
this industry.
    The proposed rule for Hazardous Waste Combustors included a 
standard of mercury. However, control of mercury in that rule would be 
based on controlling the amount of mercury in the hazardous waste fuel, 
not controlling raw material or fossil fuel. This approach is thus not 
available to NHW kilns. In addition, based on the Electric Utility 
Report to Congress on HAP emissions, EPA believes that fuel switching 
among different coals and from coal to oil would not consistently 
reduce HAP metal emissions from cement manufacturing plants. (Study of 
Hazardous Air Pollutant Emissions from Electric Utility Steam 
Generating Units--Final Report to Congress, volume 1, 453/R-98-004a, 
February 1998, pp. 13-1 through 13-5.) Therefore, this final rule 
establishes MACT for mercury as no control. However, EPA will be 
performing research and development work with the objective of finding 
more cost effective methods to reduce mercury air emissions from 
fossil-fuel fired electric utilities, and EPA will in the future 
consider whether any more cost effective methods may be appropriate as 
a basis for reducing mercury emissions from NHW cement kilns.

Hydrogen Chloride Limit

    Comment: Comments were received stating the need for an emission 
standard for HCl emissions from kilns

[[Page 31919]]

because EPA did not provide data to show that HCl emissions pose no 
threat to public health and that HCl is emitted in large quantities 
from new and existing NHW kilns. Other commenters stated that EPA 
appropriately concluded that there is no basis for a MACT standard for 
HCl.
    Response: With regard to the threat to public health comment, the 
EPA is conducting this rulemaking under section 112(d)(2) and therefore 
the decision on an emission standard is not based on health risk. 
Impacts to public health will be studied and addressed later under 
section 112(f) of the Act. The EPA determined, at proposal, that the 
MACT floor for both new and existing sources was no control. Further, 
no cost effective beyond the floor alternatives were identified. The 
commenters provided no new information on the use of any control 
technologies to limit emissions of HCl from NHW kilns. For this reason 
no emission standard is being established for HCl.

Opacity Limit

    Comment: One commenter requested that EPA clarify the duration of 
both the performance test and continuous compliance demonstrations for 
opacity emissions.
    Response: The opacity requirements in the final rule have been 
changed to provide for compliance on the basis of average opacity for 
each and every 6-minute block of operating time. This is consistent 
with the NSPS which is the MACT floor level of PM control upon which 
the standard is based. (The proposed rule incorrectly required a 
thirty-minute averaging time for demonstrating continuous compliance.)
    Comment: Commenters expressed concern regarding the requirement to 
initiate a Quality Improvement Plan (QIP) and the need to track and 
statistically analyze opacities at levels below the standards. One 
commenter stated that a violation triggered by not initiating a QIP 
when the source was not violating an emission standard was extreme.
    Response: The requirements for developing and implementing a QIP in 
response to a 15 percent kiln and in-line kiln/raw mill opacity trigger 
have been removed from the final rule. The final rule retains the 
opacity limit of 20 percent which if exceeded during any 6-minute 
period is a violation.
    Comment: One commenter requested that EPA specify the scope of 
monitoring opacity from raw and finish mills.
    Response: The EPA has clarified that the opacity limitation on 
gases discharged from raw mills and finish mills is restricted to the 
mill sweep and air separator air pollution control devices. This is 
consistent with the MACT floor technology for control of gases from 
these affected sources.
    Comment: A commenter noted that the proposed rule did not specify 
under what conditions visual opacity monitoring should be conducted.
    Response: The final rule clarifies that Method 9 (and Method 22) 
tests must be conducted under the highest load or capacity level 
reasonably expected to occur.
    Comment: Numerous commenters expressed concern regarding 
installation, operation, calibration and maintenance of triboelectric 
bag leak detection systems, and that the lack of clear-cut 
specifications would lead to open-ended liability for owners/operators.
    Response: The option for use of triboelectric bag leak detection 
systems for monitoring fabric filter performance is not being 
promulgated at this time. The EPA is presently considering this issue 
and may propose revised bag leak detector requirements for some source 
categories. Those owners or operators who want to use bag leak 
detection systems may petition the Administrator for approval of 
alternative monitoring requirements under the General Provisions.
    The rule requires the owner or operator to monitor the opacity from 
raw mills and finish mills 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.''
    Owners or operators of raw mills and finish mills are required to 
initiate corrective action within one hour of a Method 22 test during 
which visible emissions are observed. A 30-minute Method 9 opacity test 
must be started within 24 hours of observing visible emissions.

D/F Monitoring

    Comment: Several commenters suggested averaging periods for 
temperature limits shorter than 9 hours as proposed. One commenter 
preferred one-hour rolling averages. Two commenters preferred ten-
minute averages as rationalized in the proposed Hazardous Waste 
Combustor Rule.
    Response: As noted in section IV. Summary of Changes Since 
Proposal, the final rule, in response to these comments, has been 
changed to a shorter averaging period. The nine-hour block average 
period used for the monitoring of temperature (as well as the activated 
carbon injection rate, if applicable) has been changed to a three-hour 
rolling average period. The three-hour averaging time will help to 
limit disproportionate increases in D/F emissions that could be caused 
by very short periods of higher temperatures. A three-hour averaging 
time is reasonable because it is within the range of values the Agency 
could have selected, ranging from an instantaneous limit (i.e., no 
averaging period) up to a nine-hour averaging period.
    The enforceable operating limit for gas stream temperature is 
derived from the temperature measured during 3 three-hour measurements 
of D/F emission. The three-hour rolling average temperature limit is 
established by taking the average of the one-minute average 
temperatures for each test run conducted during the successful Method 
23 performance test, then averaging each test run average. Further, 
sources may petition the Administrator for an alternative averaging 
period or an alternative method for establishing operating parameter 
limits.
    Comment: A commenter pointed out that the proposal would allow a 
source to conduct its D/F performance test with an inlet PM control 
device temperature below 400 degrees F, but after the performance test, 
the source would be allowed to operate its PM control device with an 
inlet temperature up to 400 degrees F.
    Response: In drafting the proposal, the EPA did not intend to allow 
a source to operate its PM control device at a temperature higher than 
the temperature during the performance test, and so the EPA has 
clarified that the inlet temperature limit is established as and capped 
at the average temperature during the D/F performance test.
    Comment: One commenter stated that the D/F standard should be 
coordinated with the rule for hazardous waste combustors.
    Response: As was previously noted, the EPA has adopted a shorter 
temperature averaging time. To further achieve consistency with the D/F 
temperature requirements for HW kilns, the EPA is dropping the proposed 
provision which would have allowed the temperature limit to be 
established as the average temperature during the performance test plus 
25 degrees F if the D/F level (during compliance testing) was below 
0.15 ng/dscm. Further, new activated carbon injection operating 
parameters (nozzle pressure drop or carrier fluid flow rate) and 
averaging time have been added and changed, respectively, to be 
consistent with the requirements for the HW kilns.
    Comment: A comment was received requesting a clarification of the

[[Page 31920]]

procedure for demonstrating compliance for in-line kiln/raw mills 
during time periods which span a change in raw mill operating status.
    Response: After a transition period in which the status of the raw 
mill was changed from ``off'' to ``on'' or from ``on'' to ``off'', 
compliance with the operating limits for the new mode of operation 
begins, and the three-hour rolling average is established anew, i.e., 
without considering previous recordings.
    Comment: Comments were received suggesting that combustion 
parameters (e.g., CO and THC) should be monitored to demonstrate 
compliance with the
D/F standard.
    Response: The final rule does not require monitoring of these 
parameters as a means of monitoring combustion because the EPA believes 
that THC and CO emissions from NHW cement kilns are largely due to 
formation outside of the combustion zone, i.e., due to the feed 
materials. Therefore THC and carbon monoxide emissions might not 
accurately reflect combustion conditions, therefore the EPA has not 
included CO monitoring requirements to ensure good combustion. However, 
the final rule has been changed to include a monitoring requirement for 
an inspection of combustion system components to be conducted at least 
annually.

THC Monitoring

    Comment: The EPA received comments related to the use of THC 
monitoring as a means of controlling combustion related pollutants and, 
therefore, organic HAPs (see comment 6.4.1 in the Response to Comments 
Document).
    Response: Stack THC emissions from kilns, in-line kiln raw mills, 
and raw material dryers result mainly from organic material within the 
feed and not from incomplete combustion. As a result, the suggested 
combustion monitoring alternatives are not relevant.

Performance Testing Frequency

    Comment: The EPA received a comment requesting that performance 
tests be required more frequently than once every five years, citing 
other rules with more frequent testing requirements.
    Response: The EPA selected the five year testing interval to 
synchronize the testing schedule with Title V permit renewals. The 
testing frequency for NHW cement kilns and other affected sources at 
portland cement manufacturing facilities has not been changed. The 
exception to this is the
D/F performance tests. To maintain consistency with the requirements 
for HW kilns, the D/F performance testing frequency has been changed to 
every 2 and one half years.

Definitions

    Comment: Commenters requested various changes to the definitions, 
including those of ``alkali bypass'' and ``feed'' to reflect cement 
industry practices.
    Response: The final rule expands the definition of ``alkali 
bypass'', and defines ``kiln exhaust gas bypass'' as a synonym for 
alkali bypass. The final rule clarifies the definition of ``feed'' to 
include recycled cement kiln dust, consistent with past practice in 
enforcement of the NSPS.

Major Source Determination

    Comment: Numerous comments were received regarding the use of 
emissions test data and emission factors (based on data provided in the 
proposal docket) in determining whether a source is major for hazardous 
air pollutants.
    Response: The need for HAP-specific test methods and the validity 
of data obtained by various means to determine major source status are 
closely related. Hence this discussion covers both aspects under the 
overall title of major source determination.
    Although emission standards are being promulgated for PM as a 
surrogate for semi-volatile and non-volatile HAP metals; THC as a 
surrogate for organic HAPs; and D/F, each facility owner/operator must 
make a major source determination that requires an estimate of the 
facility's potential to emit all HAPs from all emission sources. HCl 
and organic HAP emissions such as (but not limited to) benzene, 
toluene, hexane, formaldehyde, hexane, naphthalene, phenol, styrene, 
and xylenes are the main HAPs from the kiln that may cause facilities 
to be major sources, but HAPs emitted from all sources at the plant 
site should be accounted for in making a major source determination.
    Comment: Some commenters questioned the need for accurate HCl 
measurements, since there is no HCl emission standard. Others stated 
that EPA should provide industry the choice of conducting testing for 
HCl with either Method 26, 321, or 322. They objected to the 
restriction that Method 26 could be used only if validated by Method 
321 or 322. They also stated their belief that the Agency's decision 
regarding the negative bias of Method 26 was based on a limited set of 
test results and an insufficient investigation of the potential cause. 
Additional comments noted that Method 26 may actually give false 
positives due to inclusion of chloride salts in the calculation of 
measured results.
    Response: As discussed above, HCl and organic HAPs emissions are 
the main HAPs from the kiln that will cause a source to be a major 
source, but HAPs emitted from all sources at the plant site, including 
metals emissions (discussed below) should be accounted for in making a 
major source determination. Accurate measurements of HCl in the kiln 
exhaust gases are necessary for major source determination. The EPA 
agrees with commenters that Method 26 may have positive biases 
attributable to chloride salts rather than to HCl; and negative biases 
due to condensation and/or removal of HCl on the filter and/or in the 
sampling probe. Therefore, the Agency has decided that Method 26 and 
26A use without concurrent validation with M. 321 or M. 322 will only 
be acceptable for measuring HCl from NHW kilns to confirm that the 
portland cement plant is a major source. M. 26 or 26A may not be used 
to measure HCl in the determination that the source is an area source. 
Only the FTIR methods may be used in the measurement of HCl if the 
source claims it is not a major source.
    Further, as a result of technical problems encountered by the 
Agency with the use of draft Method 322 (based on gas filter 
correlation/infrared technology) in the emission testing of lime kilns 
(which have a matrix similar to portland cement sources) [See Section 
IV.F. on Additional Test Methods for a description of the technical 
problems], and in response to concerns expressed by the commenters, the 
EPA is modifying its position regarding HCl measurements using this 
method in promulgating the final rule.
    For the above reasons, the Agency has decided that only Methods 320 
and 321 will be acceptable for measuring HCl from NHW kilns if the 
owner/operator wishes to claim its portland cement facility is not a 
major source. These methods are being promulgated as part of this 
rulemaking.
    Comment: Commenters also requested that EPA allow cement 
manufacturers the option of using Method 25 (in addition to Method 18 
or Method 320) for testing emissions of organic HAPs. The commenters 
suggest that the relatively inexpensive Method 25 could be used by 
cement plants that have low concentrations of organic matter in the raw 
material mix to verify that the plant's THC emissions are less than 10 
tons/year.
    Response: The focus of these commenters' point is alternatives to

[[Page 31921]]

measurement of organic HAPs in the process of making a major source 
determination. However, all HAPs (organic, HCl, metals, etc.) from all 
sources must be included in that determination, so it is necessary to 
obtain data that will allow summation of all HAP emissions to compare 
to the 10/25 ton per year thresholds specified in section 112 of the 
Clean Air Act. Depending on site-specific circumstances, EPA Method 25 
may not provide sufficient information to make an accurate summation. 
For example, a source's determination that its THC emissions based on 
Method 25 or 25A are less than 10 tons per year does not necessarily 
signify that it is an area source; the source may be a major source 
based on the 25 ton per year criterion when all other HAP emissions are 
summed with the THC. If the source's THC emissions are over 10 tons per 
year, the source may choose to conduct emissions tests using EPA Method 
320 to make a determination of actual organic HAP emissions. However, 
in lieu of conducting Method 320 emissions tests, the source could use 
Method 25A, but the source would have to assume that the mass emission 
rate (as propane) from all combustion sources combined at the site is 
attributed to one organic HAP. This amount would then have to be 
compared to the 10 ton per year threshold for one HAP. To summarize, in 
addition to accounting for organic HAPs (either through Method 320 
testing or assuming all THC is one organic HAP), accurate measurements 
of HCl in the kiln exhaust gases would be necessary for major source 
determination, as well as measurements of HAP metals (see below), to 
obtain data that will allow summation of all HAP emissions to compare 
to the 10/25 ton per year thresholds.
    Comment: Another commenter requested that EPA allow the use of an 
alternative to what they perceived as an EPA-suggested emission factor 
for metal emissions, of one percent of PM emissions, to determine major 
source status.
    Response: If after the source determines that it is not major 
because it does not meet either the 10/25 ton per year thresholds based 
on the summation of HCl and organic HAP emissions from all sources at 
the plant, the source would need to determine its HAP metals emissions 
from all sources at the facility as well, to make a determination that 
it is not a major source. The use of a ``one percent HAP metals in PM'' 
emission factor assumption will not provide definitive evidence that 
the source is an area source. However, the Agency would allow sources 
to forego the speciated HAP metals emission tests (through the use of 
Method 29) if it is assumed that 1 percent of the total PM emissions 
from all sources at the site are metal HAPs. This assumed amount of 
metal HAPs emissions would be added to the amount of HCl and organic 
HAPs emitted (determined as described above), and this total amount 
would then be compared to the 25 ton per year threshold for all HAPs 
combined. To reiterate, each facility owner/operator must make a major 
source determination that requires an estimate of the facility's 
potential to emit all HAPs from all emission sources, accounting for 
HCl, organic HAPs (either through speciation of organic HAPs or 
assuming all THC is one organic HAP), and metals (either through 
speciation of metal HAPs or assuming 1 percent of PM is metal HAP), to 
allow summation of all HAP emissions to compare to the 10/25 ton per 
year thresholds.

Voluntary Consensus Standards

    Comment: One commenter (IV-D-17) stated that EPA's actions (in 
developing and proposing the precursor to EPA Fourier Transform 
Infrared Spectroscopy [FTIR] test method 320) directly conflict with 
the guidance of and directives of the 1995 National Technology Transfer 
and Advancement Act and the Office of Management and Budget (OMB) 
Circular A-119 because: (1) the American Society of Testing and 
Materials (ASTM) FTIR consensus based test method is available, and (2) 
the EPA Emission Measurement Center (EMC) representatives were made 
aware of the development of the ASTM method and chose duplicative 
measures in developing and proposing the precursor to EPA FTIR test 
method 320. (The OMB Circular states specifically that ``If a voluntary 
consensus standards body is in the process of developing or adopting a 
voluntary consensus standard that would likely be lawful and practical 
for an agency to use, and would be developed on a timely basis, an 
agency should not be developing its own government unique standard and 
instead should be participating in the activities of the voluntary 
consensus standards body.'')
    Response: The Agency has been actively developing extractive FTIR-
based methods for HAPs since 1992. Methods 320 and 321 are direct 
products of this long-term effort to apply an innovative approach to 
emissions measurement in the form of extractive FTIR. The Agency has 
tested these methods in the laboratory and in the field extensively 
(conducting testing at two portland cement facilities), and has 
conducted multiple validation tests of these methods. The Portland 
Cement Association (PCA), in representing various members of the 
regulated industry, has conducted its own series of validation tests of 
these methods. Actually, Method 321 was developed and validated by PCA, 
and has been adopted by the Agency as Method 321. Agency personnel 
informed ASTM in 1996 that the Agency methods were in active 
development, and an ASTM standard seemed redundant. Additionally, the 
ASTM standard has not undergone field validation, which is essential in 
establishing the precision and accuracy of any test method.
    The Agency has conducted a review of the ASTM method. While the 
ASTM method is in some ways similar to Method 320, the ASTM method is 
not sufficiently detailed to document proper application, and does not 
contain the quality assurance procedures the Agency requires in 
compliance methods. Specifically, the ASTM method does not address 
specific calibration transfer standards, nor does it address the 
preparation of reference spectra. Therefore, EPA has determined that it 
is impractical to adopt the ASTM method at this time and is 
promulgating Method 320.

Pollution Prevention

    Comment: Comments were received stating that the proposed rule did 
not contain measures that prevent pollution or reduce energy 
requirements, and suggested specific pollution prevention measures, 
including process modifications, taken by specific facilities.
    Response: The NESHAP is written in terms of emissions standards 
based on MACT floor technologies and allows pollution prevention 
techniques to achieve compliance. The EPA considered pollution 
prevention options available and the basis for the standard for THC for 
new greenfield sites, feed material selection, is a pollution 
prevention measure. In addition, the final standard includes a 
monitoring requirement for inspection of the combustion system 
components of kilns and in-line kiln raw mills (an energy efficiency 
and pollution prevention measure) and standards for PM from product 
handling affected sources (which leads to improved recovery of salable 
product and pollution prevention). Furthermore, the final standard 
clarifies that recovered cement kiln dust can be included in the 
calculation of kiln feed (encouraging recycling, improved PM control 
and pollution prevention).

[[Page 31922]]

Control Cost Impacts and Data Evaluation

    Comment: Comments were received concerning the EPA's control cost 
estimates, including the assumptions regarding the number of sources 
requiring upgrades to meet the standards for PM and D/F, and the 
capital expenditures necessary to meet the standard. In particular one 
commenter projected that capital costs would exceed the threshold which 
triggers Executive Order 12866. Another commenter questioned the lack 
of cost data on upgrades to PMCDs for material handling affected 
sources.
    Response: The costs to achieve compliance are expected to be highly 
site-specific and vary significantly. The commenters did not provide 
any details regarding their estimates of the cost to comply, so the EPA 
is unable to determine whether the commenters' cost estimates were 
limited to those costs necessary to comply with the provisions of the 
NESHAP.
    The EPA has reviewed cost data provided by the Portland Cement 
Association prior to proposal. The foundation for the cost estimates, 
and initial point of criticism of EPA's cost estimates, is the model 
plant characteristics. For example, the APCA report provided a review 
of the model plant characteristics and suggested that the design 
characteristics for each model be 20 to 25 percent higher than the 
annual average production rate basis for the model. In particular, the 
APCA report stated that the EPA model plant gas flows for wet process 
and long dry kilns were 25 to 30 percent too low, based on their 
consultant's design practice.
    The EPA developed design characteristics for the model plants based 
on data provided to the Agency in ICRs and test reports (docket items 
II-B-24 and II-B-37). For a kiln with a given nominal production rate 
that might be found in several different plants, variations in gas flow 
rates would be expected. The EPA used the flow rate and production data 
from actual installations to develop production rate versus gas flow 
graphs to establish the model plant characteristics. Owners may elect 
to design their upgrades or new equipment to accommodate higher 
production rates, but those costs and other impacts are not 
attributable to compliance with the MACT standards. EPA did not include 
costs associated with upgrading equipment used to control emissions 
from materials handling affected sources, as these affected sources 
have been subject to the NSPS for many years (a longer period than the 
expected life of these affected sources), and compliance with the 
NESHAP, which is equivalent to the NSPS for these affected sources 
would not impose additional costs.
    The basis of the control costs for model plants estimated in the 
docket memoranda and proposal preamble is the Office of Air Quality 
Planning and Standards Cost Manual. The cost algorithms in the manual 
were derived from control equipment vendor quotes, standard cost 
estimating factors, and contractor experience. Installation costs, 
utilities, maintenance, and other operating costs were estimated and 
included for impact estimation. The EPA maintains that the costs 
provided in the proposal preamble are a reasonable basis for projecting 
the national impacts of the these rules.

VII. Administrative Requirements

A. Docket

    A record has been established for this rulemaking under docket 
number A-92-53. This record includes information considered by the EPA 
in the development of the promulgated standards. A public version of 
this record, which does not include any information included as 
confidential business information, is available for inspection from 
8:00 a.m. to 5:30 p.m. Monday-Friday, excluding legal holidays. The 
public record is located in the Air & Radiation Docket & Information 
Center, Room M1500, 401 M Street S.W., Washington, D.C. 20460.
Response-to-Comment Document
    The response-to-comment document for the promulgated standards 
contains a summary of all public comments received following proposal 
of the rule and the EPA's response to these comments. This document is 
located in the docket (Docket Item No. V-C-1) and is available for 
downloading from the Technology Transfer Network (TTN). The TTN is one 
of the EPA's electronic bulletin boards. The TTN provides information 
from EPA in various areas of air pollution technology or policy. The 
service is free except for the cost of a phone call. Dial (919) 541-
5742 for up to a 14,400 bps modem, or connect through the internet to 
the following address: ``www.epa.gov/ttn/oarpg''. If more information 
on the Technology Transfer Network is needed, call the HELP line at 
(919) 541-5384.

B. Executive Order 12866

    Under Executive Order 12866 (58 FR 5173, October 4, 1993), the EPA 
must determine whether the regulatory action is ``significant'' and 
therefore subject to Office of Management and Budget (OMB) review and 
the requirements of the Executive Order. The Executive Order defines 
``significant regulatory action'' as one that is likely to result in 
standards 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 entitlement, grants, 
user fees, or loan programs or the rights and obligations 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 $37 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 (primarily due to 
this action's overlap with the Hazardous Waste Combustor MACT 
standard), and the promulgated 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 ADDRESSESS. 
The docket is available for public inspection at the EPA's Air Docket 
Section, which is listed in the ADDRESSES section of this preamble.

C. Executive Order 12875: Enhancing Intergovernmental Partnerships

    Under Executive Order 12875, the EPA may not issue a regulation 
that is not required by statute and that creates a mandate upon a 
State, local or tribal government, unless the Federal government 
provides the funds necessary to pay the direct compliance costs 
incurred by those governments, or EPA consults with those governments. 
If EPA complies by consulting, Executive Order 12875 requires EPA to 
provide to the Office of Management and Budget a description of the 
extent of EPA's prior consultation with representatives of affected 
State, local and tribal governments, the nature of their concerns, 
copies of any written communications from the governments, and a 
statement supporting the need to issue the regulation. In addition, 
Executive Order 12875 requires EPA to

[[Page 31923]]

develop an effective process permitting elected officials and other 
representatives of State, local and tribal governments ``to provide 
meaningful and timely input in the development of regulatory proposals 
containing significant unfunded mandates.''
    Today's rule does not create a mandate on State, local or tribal 
governments. The rule does not impose any enforceable duties on these 
entities. Accordingly, the requirements of section 1(a) of Executive 
Order 12875 do not apply to this rule.

D. Unfunded Mandates Reform Act

    Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Public 
Law 104-4, establishes requirements for Federal agencies to assess the 
effects of their regulatory actions on State, local, and tribal 
governments and the private sector. Under section 202 of the UMRA, the 
EPA generally must prepare a written statement, including a cost-
benefit analysis, for proposed and final rules with ``Federal 
mandates'' that may result in expenditures to State, local, and tribal 
governments, in the aggregate, or to the private sector, of $100 
million or more in any one year. Before promulgating an EPA rule for 
which a written statement is needed, section 205 of the UMRA generally 
requires the EPA to identify and consider a reasonable number of 
regulatory alternatives and adopt the least costly, most cost-effective 
or least burdensome alternative that achieves the objectives of the 
rule. The provisions of section 205 do not apply when they are 
inconsistent with applicable law. Moreover, section 205 allows the EPA 
to adopt an alternative other than the least costly, most cost-
effective, or least burdensome alternative if the Administrator 
publishes with the final rule an explanation why that alternative was 
not adopted. Before the EPA establishes any regulatory requirements 
that may significantly or uniquely affect small governments, including 
tribal governments, it must have developed under section 203 of the 
UMRA a small government agency plan. The plan must provide for 
notifying potentially affected small governments, enabling officials of 
affected small governments to have meaningful and timely input in the 
development of EPA regulatory proposals with significant Federal 
intergovernmental mandates, and informing, educating, and advising 
small governments on compliance with the regulatory requirements.
    The EPA has determined that this rule does not contain a Federal 
mandate that may result in expenditures of $100 million or more for 
State, local, and tribal governments, in aggregate, or the private 
sector in any one year, nor does the rule significantly or uniquely 
impact small governments, because it contains no requirements that 
apply to such governments or impose obligations upon them. Thus, the 
requirements of the UMRA do not apply to this rule.

E. Regulatory Flexibility Act

    The EPA has determined that it is not necessary to prepare a 
regulatory flexibility analysis in connection with this final rule. As 
discussed earlier in the response to comments section of the preamble, 
the EPA has determined that this rule will not have a significant 
economic impact on a substantial number of small entities.
    Although the rule will not have a significant impact on a 
substantial number of small entities, the EPA 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 
designated the PCA as its representative in meetings with the EPA 
concerning the rulemaking for the portland cement industry.
    The promulgated emission standards are representative of the floor 
level of emision control, which is the minimum level of control allowed 
under the Act. Further, the costs of required performance testing and 
monitoring have been minimized by specifying emission limits and 
monitoring parameters in terms of surrogates for HAP emissions, which 
are less costly to measure. The Agency has also tried to make the rule 
``user friendly,'' with language that is easy to understand by all of 
the regulated community. EPA is also allowing affected firms up to 3 
years from the effective date of the final rule to comply, which could 
lessen capital availability concerns. An extra year may be granted by 
the Administrator or delegated regulatory authority if necessary to 
install controls. Further, EPA has deferred the compliance date for 
installing PM CEMs pending a future proposed rulemaking.

F. Submission to Congress and the General Accounting Office

    The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the 
Small Business Regulatory Enforcement Fairness Act of 1996, generally 
provides that before a rule may take effect, the agency promulgating 
the rule must submit a rule report, which includes a copy of the rule, 
to each House of the Congress and to the Comptroller General of the 
United States. The EPA will submit a report containing this rule and 
other required information to the U.S. Senate, the U.S. House of 
Representatives, and the Comptroller General of the United States prior 
to publication of the rule in the Federal Register. This rule is not a 
``major rule'' as defined by 5 U.S.C. Sec. 804(2).

G. Paperwork Reduction Act

    The information collection requirements in this rule are being 
submitted for approval to the Office of Management and Budget (OMB) 
under the Paperwork Reduction Act, 44 U.S.C. 3501 et seq. An 
Information Collection Request (ICR) document has been prepared by EPA 
(ICR No. 1801.02) and a copy may be obtained from Sandy Farmer by mail 
at OP Regulatory Information Division; U.S. Environmental Protection 
Agency (2137); 401 M St., S.W.; Washington, DC 20460, by email at 
[email protected], or by calling (202) 260-2740. A copy may 
also be downloaded off the internet at http://www.epa.gov/icr. The 
information requirements are not effective until OMB approves them.
    The EPA is required under section 112 (d) of the Clean Air Act to 
regulate emissions of HAPs listed in section 112 (b). The requested 
information is needed as part of the overall compliance and enforcement 
program. The ICR requires that portland cement manufacturing plants 
retain records of parameter and emissions monitoring data at facilities 
for a period of 5 years, which is consistent with the General 
Provisions to 40 CFR part 63 and the permit requirements under 40 CFR 
part 70. All sources subject to this rule will be required to obtain 
operating permits either through the State-approved permitting program 
or, if one does not exist, in accordance with the provisions of 40 CFR 
part 71, when promulgated.
    The public reporting burden for this collection of information is 
estimated to average 2148 hours per respondent per year for an 
estimated 36 respondents. This estimate includes performance tests and 
reports (with repeat tests where needed); one-time preparation of an 
operation and maintenance plan with semiannual reports of any event 
where the procedures in the plan were not followed; semiannual excess 
emissions reports; notifications; and

[[Page 31924]]

recordkeeping. The total annualized capital costs associated with 
monitoring requirements over the three-year period of the ICR is 
estimated at $750,000. This estimate includes the capital and startup 
costs associated with installation of required continuous monitoring 
equipment for those affected sources subject to the standard. The total 
operation and maintenance cost is estimated at $682,000 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 purposes of collecting, validating, and 
verifying information, processing and maintaining information, and 
disclosing and providing information; adjust the existing ways to 
comply with any previously applicable instructions and requirements; 
train personnel to be able to respond to a collection of information; 
search 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.

H. Pollution Prevention Act

    During the development of this rule, the EPA explored opportunities 
to eliminate or reduce emissions through the application of new 
processes or work practices. This NESHAP includes a monitoring 
requirement for an inspection of the components of the combustion 
system of each kiln and in-line kiln raw mill to be conducted at least 
once per year. Such an inspection will promote fuel efficiency and 
decrease the formation of combustion related pollutants.

I. National Technology Transfer and Advancement Act

    Section 12(d) of the National Technology Transfer and Advancement 
Act (NTTAA) directs all Federal agencies to use voluntary consensus 
standards in regulatory and procurement activities unless to do so 
would be inconsistent with applicable law or otherwise impracticable. 
Voluntary consensus standards are technical standards (e.g., materials 
specifications, test methods, sampling procedures, and business 
practices) developed or adopted by one or more voluntary consensus 
bodies. The NTTAA requires Federal agencies to provide Congress, 
through annual reports to OMB, with explanations when an agency does 
not use available and applicable voluntary consensus standards.
    Consistent with the NTTAA, the EPA conducted a search to identify 
voluntary consensus standards. The search identified 21 voluntary 
consensus standards that appeared to have possible use in lieu of EPA 
standard reference methods. However, after reviewing available 
standards, EPA determined that 14 of the candidate consensus standards 
identified for measuring emissions of the HAPs or surrogates subject to 
emission standards in the rule would not be practical due to lack of 
equivalency, documentation, validation data and other important 
technical and policy considerations. Six of the remaining candidate 
consensus standards are new standards under development that EPA plans 
to follow, review and consider adopting at a later date.
    One consensus standard, ASTM D6216-98, appears to be practical for 
EPA use in lieu of EPA Performance Specification 1 (See 40 CFR Part 60, 
Appendix B). On September 23, 1998, EPA proposed incorporating by 
reference ASTM D6216-98 under a separate rulemaking (63 FR 50824) that 
would allow broader use and application of this consensus standard. EPA 
plans to complete this action in the near future. For these reasons, 
EPA defers taking action in this rulemaking that would adopt D6216-98 
in lieu of PS-1 requirements as it would be impractical for EPA to act 
independently from other rulemaking activity already undergoing notice 
and comment.
    Additionally, EPA received comments that ASTM FTIR Standard D6348 
should be used in lieu of EPA's proposed Fourier transform infrared 
spectroscopy (FTIR) emission test methods. EPA has determined for a 
number of reasons that the ASTM Standard D6348 is one of the 14 
standards determined to be impractical to adopt for the purposes of 
this rulemaking. EPA review comments on ASTM Standard D6348 are 
included in the docket for this rulemaking and summarized in the 
response to comments section of this preamble. ASTM has also been 
advised of the reasons for impracticality and ASTM Subcommittee D22-03 
is now undertaking a revision of the ASTM standard. Upon demonstration 
of technical equivalency with the EPA FTIR methods, the revised ASTM 
standard could be incorporated by reference for EPA regulatory 
applicability at a later date.
    This rule requires standard EPA methods known to the industry and 
States. Approved alternative methods also may be used with prior EPA 
approval.

J. Executive Order 13045

    Executive Order 13045 applies to any rule that EPA determines (1) 
is ``economically significant'' as defined under Executive Order 12866, 
and (2) the environmental health or safety risk addressed by the rule 
has a disproportionate effect on children. If the regulatory action 
meets both criteria, the Agency must evaluate the environmental health 
or safety effects of the planned rule on children and explain why the 
planned regulation is preferable to other potentially effective and 
reasonably feasible alternatives considered by the Agency.
    This final rule is not subject to E.O. 13045, entitled ``Protection 
of Children from Environmental Health Risks and Safety Risks'' (62 FR 
19885, April 23, 1997), because it is not an economically significant 
regulatory action as defined by Executive Order 12866, and it does not 
address an environmental health or safety risk that would have a 
disproportionate effect on children.

K. Executive Order 13084: Consultation and Coordination With Indian 
Tribal Governments

    Under Executive Order 13084, EPA may not issue a regulation that is 
not required by statute, that significantly or uniquely affects the 
communities of Indian tribal governments, and that imposes substantial 
direct compliance costs on those communities, unless the Federal 
government provides the funds necessary to pay the direct compliance 
costs incurred by the tribal governments, or EPA consults with those 
governments. If EPA complies by consulting, Executive Order 13084 
requires EPA to provide to the Office of Management and Budget, in a 
separately identified section of the preamble to the rule, a 
description of the extent of EPA's prior consultation with 
representatives of affected tribal governments, a summary of the nature 
of their concerns, and a statement supporting the need to issue the 
regulation. In addition, Executive Order 13084 requires EPA to develop 
an effective process permitting elected officials and other 
representatives of Indian tribal governments ``to provide meaningful 
and timely input in the development of regulatory policies on matters 
that

[[Page 31925]]

significantly or uniquely affect their communities.''
    Today's rule does not significantly or uniquely affect the 
communities of Indian tribal governments. Accordingly, the requirements 
of section 3(b) of Executive Order 13084 do not apply to this rule.

List of Subjects in 40 CFR Part 63

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

    Dated: May 14, 1999.
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 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: 42 U.S.C. 7401, 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 Hazardous Air Pollutants 
From the Portland Cement Manufacturing Industry

General

Sec.
63.1340  Applicability and designation of affected sources.
63.1341  Definitions.

Emission Standards and Operating Limits

63.1342  Standards: General.
63.1343  Standards for kilns and in-line kiln/raw mills.
63.1344  Operating limits for kilns and in-line kiln/raw mills.
63.1345  Standards for clinker coolers.
63.1346  Standards for new and reconstructed raw material dryers.
63.1347  Standards for raw and finish mills.
63.1348  Standards for affected sources other than kilns; in-line 
kiln raw mills; clinker coolers; new and reconstructed raw material 
dryers; and raw and finish mills.

Monitoring and Compliance Provisions

63.1349  Performance testing requirements.
63.1350  Monitoring requirements.
63.1351  Compliance dates.
63.1352  Additional test methods.

Notification, Reporting and Recordkeeping

63.1353  Notification requirements.
63.1354  Reporting requirements.
63.1355  Recordkeeping requirements.

Other

63.1356  Exemption from new source performance standards.
63.1357  Temporary, conditioned exemption from particulate and 
opacity standards.
63.1358  Delegation of authority.
63.1359  [Reserved]

Table 1 to Subpart LLL of Part 63--Applicability of General Provisions

Subpart LLL--National Emission Standards for Hazardous Air 
Pollutants From the Portland Cement Manufacturing Industry

General


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.
    (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;
    (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 and each greenfield raw material dryer at any portland 
cement plant which is a major or area 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 in this section 
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, chloride and/or sulfur on the raw feed. This may also be 
referred to as the ``kiln exhaust gas bypass''.
    Bagging system means the equipment which fills bags with portland 
cement.
    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.
    Continuous monitor means a device which continuously samples the 
regulated parameter specified in Sec. 63.1350 of this subpart without 
interruption, evaluates the detector response at least once every 15 
seconds, and computes and records the average value at least every 60 
seconds, except during allowable periods of calibration and except as 
defined otherwise by the continuous emission monitoring system 
performance specifications in appendix B to part 60 of this chapter.
    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.

[[Page 31926]]

    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, cement kiln dust and flyash, that are fed to the kiln. 
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.
    Greenfield kiln, in-line kiln/raw mill, or raw material dryer means 
a kiln, in-line kiln/raw mill, or raw material dryer for which 
construction is commenced at a plant site (where no kilns and no in-
line kiln/raw mills were in operation at any time prior to March 24, 
1998) after March 24, 1998.
    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 portland cement.
    Kiln exhaust gas bypass means alkali bypass.
    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.
    New brownfield kiln, in-line kiln raw mill, or raw material dryer 
means a kiln, in-line kiln/raw mill or raw material dryer for which 
construction is commenced at a plant site (where kilns and/or in-line 
kiln/raw mills were in operation prior to March 24, 1998) after March 
24, 1998.
    One-minute average means the average of thermocouple or other 
sensor responses calculated at least every 60 seconds from responses 
obtained at least once during each consecutive 15 second period.
    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.
    Rolling average means the average of all one-minute averages over 
the averaging period.
    Run average means the average of the one-minute parameter values 
for a run.
    TEQ 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.

Emission Standards and Operating Limits


Sec. 63.1342  Standards: General.

    (a) 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.
    (b) Table 1 of this section provides a summary of emission limits 
and operating limits of this subpart.

                         Table 1 to Sec.  63.1342.--Emission Limits and Operating Limits
----------------------------------------------------------------------------------------------------------------
            Affected source                        Pollutant or opacity            Emission and operating limit
----------------------------------------------------------------------------------------------------------------
All kilns and in-line kiln/raw mills at  PM.....................................  0.15 kg/Mg of feed (dry
 major sources (including alkali         Opacity................................   basis).
 bypass).                                                                         20 percent.
All kilns and in-line kiln/raw mills at  D/F....................................  0.20 ng TEQ/dscm
 major and area sources (including                                                or
 alkali bypass).                                                                  0.40 ng TEQ/dscm when the
                                                                                   average of the performance
                                                                                   test run average particulate
                                                                                   matter control device (PMCD)
                                                                                   inlet temperatures is 204
                                                                                   deg. C or less. [Corrected to
                                                                                   7 percent oxygen]
                                                                                  Operate such that the three-
                                                                                   hour rolling average PMCD
                                                                                   inlet temperature is no
                                                                                   greater than the temperature
                                                                                   established at performance
                                                                                   test.
                                                                                  If activated carbon injection
                                                                                   is used: Operate such that
                                                                                   the three-hour rolling
                                                                                   average activated carbon
                                                                                   injection rate is no less
                                                                                   than rate established at
                                                                                   performance test. Operate
                                                                                   such that either the carrier
                                                                                   gas flow rate or carrier gas
                                                                                   pressure drop exceeds the
                                                                                   value established at
                                                                                   performance test. Inject
                                                                                   carbon of equivalent
                                                                                   specifications to that used
                                                                                   at performance test.
New greenfield kilns and in-line kiln/   THC....................................  50 ppmvd, as propane,
 raw mills at major and area sources.                                              corrected to 7 percent
                                                                                   oxygen.
All clinker coolers at major sources...  PM.....................................  0.050 kg/Mg of feed (dry
                                         Opacity................................   basis)
                                                                                  10 percent.
All raw mills and finish mills at major  Opacity................................  10 percent.
 sources.
New greenfield raw material dryers at    THC....................................  50 ppmvd, as propane,
 major and area sources.                                                           corrected to 7 percent
                                                                                   oxygen.
All raw material dryers and material     Opacity................................  10 percent.
 handling points at major sources.
----------------------------------------------------------------------------------------------------------------


[[Page 31927]]

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

    (a) General. 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) Existing, reconstructed, or new brownfield/major sources. No 
owner or operator of an existing, reconstructed or new brownfield kiln 
or an existing, reconstructed or new brownfield 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 (PM) 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 average of the performance 
test run average temperatures at the inlet to the particulate matter 
control device is 204  deg.C (400  deg.F) or less.
    (c) Greenfield/major sources. No owner or operator that commences 
construction of a greenfield kiln or greenfield inline 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 average of the performance 
test run average temperatures at the inlet to the particulate matter 
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) Existing, reconstructed, or new brownfield/area sources. No 
owner or operator of an existing, reconstructed, or new brownfield kiln 
or an existing, reconstructed or new brownfield 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 average of the performance 
test run average temperatures at the inlet to the particulate matter 
control device is 204  deg.C (400  deg.F) or less.
    (e) Greenfield/area sources. No owner or operator of a greenfield 
kiln or a greenfield 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:
    (1) 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 10-11 gr per dscf) (TEQ) 
corrected to seven percent oxygen, when the average of the performance 
test run average temperatures at the inlet to the particulate matter 
control device is 204  deg.C (400  deg.F) or less.
    (2) Contain 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.


Sec. 63.1344  Operating limits for kilns and in-line kiln/raw mills.

    (a) The owner or operator of a kiln subject to a D/F emission 
limitation under Sec. 63.1343 must operate the kiln such that the 
temperature of the gas at the inlet to the kiln particulate matter 
control device (PMCD) and alkali bypass PMCD, if applicable, does not 
exceed the applicable temperature limit specified in paragraph (b) of 
this section. The owner or operator of an in-line kiln/raw mill subject 
to a D/F emission limitation under Sec. 63.1343 must operate the in-
line kiln/raw mill, such that:
    (1) When the raw mill of the in-line kiln/raw mill is operating, 
the applicable temperature limit for the main in-line kiln/raw mill 
exhaust, specified in paragraph (b) of this section and established 
during the performance test when the raw mill was operating is not 
exceeded.
    (2) 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 (b) of this section and 
established during the performance test when the raw mill was not 
operating, is not exceeded.
    (3) If the in-line kiln/raw mill is equipped with an alkali bypass, 
the applicable temperature limit for the alkali bypass, specified in 
paragraph (b) of this section and established during the performance 
test when the raw mill was operating, is not exceeded.
    (b) The temperature limit for affected sources meeting the limits 
of paragraph (a) of this section or paragraphs (a)(1) through (a)(3) of 
this section is determined in accordance with Sec. 63.1349(b)(3)(iv).
    (c) The owner or operator of an affected source subject to a D/F 
emission limitation under Sec. 63.1343 that employs carbon injection as 
an emission control technique must operate the carbon injection system 
in accordance with paragraphs (c)(1) and (c)(2) of this section.
    (1) The three-hour rolling average activated carbon injection rate 
shall be equal to or greater than the activated carbon injection rate 
determined in accordance with Sec. 63.1349(b)(3)(vi).
    (2) The owner or operator shall either:
    (i) Maintain the minimum activated carbon injection carrier gas 
flow rate, as a three-hour rolling average, based on the manufacturer's 
specifications. These specifications must be documented in the test 
plan developed in accordance with Sec. 63.7(c), or
    (ii) Maintain the minimum activated carbon injection carrier gas 
pressure drop, as a three-hour rolling average, based on the 
manufacturer's specifications. These specifications must be documented 
in the test plan developed in accordance with Sec. 63.7(c).
    (d) Except as provided in paragraph (e) of this section, the owner 
or operator of an affected source subject to a D/F emission limitation 
under Sec. 63.1343 that employs carbon injection as an emission control 
technique must specify and use the brand and type of activated carbon 
used during the performance test until a subsequent performance test is 
conducted, unless the site-specific performance test plan contains 
documentation of key parameters that

[[Page 31928]]

affect adsorption and the owner or operator establishes limits based on 
those parameters, and the limits on these parameters are maintained.
    (e) The owner or operator of an affected source subject to a D/F 
emission limitation under Sec. 63.1343 that employs carbon injection as 
an emission control technique may substitute, at any time, a different 
brand or type of activated carbon provided that the replacement has 
equivalent or improved properties compared to the activated carbon 
specified in the site-specific performance test plan and used in the 
performance test. The owner or operator must maintain documentation 
that the substitute activated carbon will provide the same or better 
level of control as the original activated carbon.


Sec. 63.1345  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.
    (2) Exhibit opacity greater than ten percent.
    (b) [Reserved].


Sec. 63.1346  Standards for new and reconstructed raw material dryers.

    (a) Brownfield/major sources. No owner or operator of a new or 
reconstructed brownfield 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 exhibit opacity greater than ten percent.
    (b) Greenfield/area sources. No owner or operator of a greenfield 
raw material dryer at a facility which is an area source subject to 
this subpart shall cause to be discharged into the atmosphere from the 
greenfield raw material dryer any gases which contain THC in excess of 
50 ppmvd, reported as propane, corrected to seven percent oxygen.
    (c) Greenfield/major sources. No owner or operator of a greenfield 
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 
greenfield 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.


Sec. 63.1347  Standards for raw and finish mills.

    The owner or operator of each new or existing raw mill or finish 
mill at a facility which is a major source subject to the provisions of 
this subpart shall not cause to be discharged from the mill sweep or 
air separator air pollution control devices of these affected sources 
any gases which exhibit opacity in excess of ten percent.


Sec. 63.1348  Standards for affected sources other than kilns; in-line 
kiln/raw mills; clinker coolers; new and reconstructed raw material 
dryers; and raw and finish mills.

    The owner or operator of each new or existing 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.

Monitoring and Compliance Provisions


Sec. 63.1349  Performance testing requirements.

    (a) The owner or operator of an affected source subject to this 
subpart shall demonstrate initial compliance with the emission limits 
of Sec. 63.1343 and Secs. 63.1345 through 63.1348 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)(4) 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 subject to limitations on particulate matter emissions 
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 of Appendix A 
to part 60 of this chapter 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 to demonstrate initial compliance with the PM standards of 
this subpart. However this shall not preclude the permitting authority 
from requiring a determination of the ``back half'' for other purposes.
    (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:
[GRAPHIC] [TIFF OMITTED] TR14JN99.001

Where:


[[Page 31929]]


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,
[GRAPHIC] [TIFF OMITTED] TR14JN99.002

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.
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 
Sec. 63.1343(b)(2), Sec. 63.1343(c)(2), or Sec. 63.1345(a)(2).
    (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 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 
Sec. 63.1343(b)(2), Sec. 63.1343(c)(2), or Sec. 63.1345(a)(2).
    (2) The owner or operator of any affected source subject to 
limitations on opacity under this subpart that is not subject to 
paragraph (b)(1) of this section 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 
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 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)(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 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 concentration shall be determined for each run 
and the arithmetic average of the concentrations measured for the three 
runs shall be calculated and used to determine compliance.
    (ii) The temperature at the inlet to the kiln or in-line kiln/raw 
mill PMCD, and where applicable, the temperature at the inlet to the 
alkali bypass PMCD, 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.
    (iii) One-minute average temperatures must be calculated for each 
minute of each run of the test.
    (iv) The run average temperature must be calculated for each run, 
and the average of the run average temperatures must be determined and 
included in the performance test report and will determine the 
applicable temperature limit in accordance with Sec. 63.1344(b).
    (v) If activated carbon injection is used for D/F control, the rate 
of activated carbon injection to the kiln or in-line kiln/raw mill 
exhaust, and where applicable, the rate of activated carbon injection 
to the alkali bypass exhaust, must be continuously recorded during the 
period of the Method 23 test, and the continuous injection rate 
record(s) must be included in the performance test report. In addition, 
the performance test report must include the brand and type of 
activated carbon used during the performance test and a continuous 
record of either the carrier gas flow rate or the carrier gas pressure 
drop for the duration of the test. Activated carbon injection rate 
parameters must be determined in accordance with paragraphs (b)(3)(vi) 
of this section.
    (vi) The run average injection rate must be calculated for each 
run, and the average of the run average injection rates must be 
determined and included in the performance test report and will 
determine the applicable injection rate limit in accordance with 
Sec. 63.1344(c)(1).
    (4) 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. The duration of the performance test shall be three 
hours, and the average THC concentration (as calculated from the one-
minute averages) during the three hour performance test shall be

[[Page 31930]]

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.
    (c) Except as provided in paragraph (e) of this section, 
performance tests required under paragraphs (b)(1) and (b)(2) 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 for the 
kiln, in-line kiln/raw mill or clinker cooler.
    (d) Performance tests required under paragraph (b)(3) of this 
section shall be repeated every 30 months.
    (e) The owner or operator is required to repeat the performance 
tests for kilns or in-line kiln/raw mills as specified in paragraphs 
(b)(1) and (b)(3) of this section within 90 days of initiating any 
significant change in the feed or fuel from that used in the previous 
performance test.
    (f) Table 1 of this section provides a summary of the performance 
test requirements of this subpart.

   Table 1 to Sec.  63.1349.--Summary of Performance Test Requirements
------------------------------------------------------------------------
  Affected source and pollutant               Performance test
------------------------------------------------------------------------
New and existing kiln and in-line  EPA Method 5.a
 kiln/raw mill b c PM.
New and existing kiln and in-line  COM if feasible d e or EPA Method 9
 kiln/raw mill b c Opacity.         visual opacity readings.
New and existing kiln and in-line  EPA Method 23h.
 kiln/raw mill b c f gD/F.
New greenfield kiln and in-line    THC CEM (EPA PS-8A) i.
 kiln/raw mill c THC.
New and existing clinker cooler    EPA Method 5 a.
 PM.
New and existing clinker cooler    COM d,j or EPA Method 9 visual
 opacity.                           opacity readings.
New and existing raw and finish    EPA Method 9.a j
 mill opacity.
New and existing raw material      EPA Method 9.a j
 dryer and materials handling
 processes (raw material storage,
 clinker storage, finished
 product storage, conveyor
 transfer points, bagging, and
 bulk loading and unloading
 systems) opacity.
New greenfield raw material dryer  THC CEM (EPA PS-8A).i
 THC.
------------------------------------------------------------------------
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.
f Alkali bypass is tested with the raw mill on.
g Temperature and (if applicable) activated carbon injection parameters
  determined separately with and without the raw mill operating.
h Required initially and every 30 months thereafter.
i EPA Performance Specification (PS)-8A of appendix B to 40 CFR part 60.
 
j Opacity limit is 10 percent.

Sec. 63.1350  Monitoring requirements.

    (a) The owner or operator of each portland cement plant shall 
prepare for each affected source subject to the provisions of this 
subpart, a written operations and maintenance plan. The plan shall be 
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 air pollution control devices in order to meet the emission 
limits and operating limits of Secs. 63.1343 through 63.1348;
    (2) Corrective actions to be taken when required by paragraph (e) 
of this section;
    (3) Procedures to be used during an inspection of the components of 
the combustion system of each kiln and each in-line kiln raw mill 
located at the facility at least once per year; and
    (4) Procedures to be used to periodically monitor affected sources 
subject to opacity standards under Secs. 63.1346 and 63.1348. Such 
procedures must include the provisions of paragraphs (a)(4)(i) through 
(a)(4)(iv) of this section.
    (i) The owner or operator must conduct a monthly 1-minute visible 
emissions test of each affected source in accordance with Method 22 of 
Appendix A to part 60 of this chapter. The test must be conducted while 
the affected source is in operation.
    (ii) If no visible emissions are observed in six consecutive 
monthly tests for any affected source, the owner or operator may 
decrease the frequency of testing from monthly to semi-annually for 
that affected source. If visible emissions are observed during any 
semi-annual test, the owner or operator must resume testing of that 
affected source on a monthly basis and maintain that schedule until no 
visible emissions are observed in six consecutive monthly tests.
    (iii) If no visible emissions are observed during the semi-annual 
test for any affected source, the owner or operator may decrease the 
frequency of testing from semi-annually to annually for that affected 
source. If visible emissions are observed during any annual test, the 
owner or operator must resume testing of that affected source on a 
monthly basis and maintain that schedule until no visible emissions are 
observed in six consecutive monthly tests.
    (iv) If visible emissions are observed during any Method 22 test, 
the owner or operator must conduct a 6-minute test of opacity in 
accordance with Method 9 of appendix A to part 60 of this chapter. The 
Method 9 test must begin within one hour of any observation of visible 
emissions.
    (b) Failure to comply with any provision of the operations and 
maintenance plan developed in accordance with paragraph (a) of this 
section shall be a violation of the standard.
    (c) The owner or operator of a kiln or in-line kiln/raw mill shall 
monitor opacity at each point where emissions are vented from these 
affected sources including alkali bypasses in accordance with 
paragraphs (c)(1) through (c)(3) of this section.
    (1) Except as provided in paragraph (c)(2) of this section, the 
owner or operator shall install, calibrate, maintain, and continuously 
operate a

[[Page 31931]]

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 (c)(1) of this section, monitor opacity in 
accordance with paragraphs (c)(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 (c)(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 Method 9 test shall be conducted while the affected 
source is operating at the highest load or capacity level reasonably 
expected to occur within the day. 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 6-minute average opacity for any 6-minute block period does 
not exceed 20 percent. If the average opacity for any 6-minute block 
period exceeds 20 percent, this shall constitute a violation of the 
standard.
    (d) The owner or operator of a clinker cooler shall monitor opacity 
at each point where emissions are vented from the clinker cooler in 
accordance with paragraphs (d)(1) through (d)(3) of this section.
    (1) Except as provided in paragraph (d)(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 (d)(1) of this section, monitor opacity in accordance with 
paragraphs (d)(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 (d)(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 Method 9 test shall be conducted while the affected 
source is operating at the highest load or capacity level reasonably 
expected to occur within the day. 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 6-minute average opacity for any 6-minute block period does 
not exceed 10 percent. If the average opacity for any 6-minute block 
period exceeds 10 percent, this shall constitute a violation of the 
standard.
    (e) The owner or operator of a raw mill or finish mill shall 
monitor opacity by conducting daily visual emissions observations of 
the mill sweep and air separator PMCDs of these affected sources, in 
accordance with the procedures of Method 22 of appendix A of part 60 of 
this chapter. The Method 22 test shall be conducted while the affected 
source is operating at the highest load or capacity level reasonably 
expected to occur within the day. The duration of the Method 22 test 
shall be six minutes. If visible emissions are observed during any 
Method 22 visible emissions test, the owner or operator must:
    (1) Initiate, within one-hour, the corrective actions specified in 
the site specific operating and maintenance plan developed in 
accordance with paragraphs (a)(1) and (a)(2) of this section; and
    (2) Within 24 hours of the end of the Method 22 test in which 
visible emissions were observed, conduct a visual opacity test of each 
stack from which visible emissions were observed in accordance with 
Method 9 of appendix A of part 60 of this chapter. The duration of the 
Method 9 test shall be thirty minutes.
    (f) The owner or operator of an affected source subject to a 
limitation on D/F emissions shall monitor D/F emissions in accordance 
with paragraphs (f)(1) through (f)(6) of this section.
    (1) The owner or operator shall install, calibrate, maintain, and 
continuously operate a continuous monitor to record the temperature of 
the exhaust gases from the kiln, in-line kiln/raw mill and alkali 
bypass, if applicable, at the inlet to, or upstream of, the kiln, in-
line kiln/raw mill and/or alkali bypass PM control devices.
    (i) The recorder response range must include zero and 1.5 times 
either of the average temperatures established according to the 
requirements in Sec. 63.1349(b)(3)(iv).
    (ii) The reference method must be a National Institute of Standards 
and Technology calibrated reference thermocouple-potentiometer system 
or alternate reference, subject to approval by the Administrator.
    (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 PMCD.
    (3) The three-hour rolling average temperature shall be calculated 
as the average of 180 successive one-minute average temperatures.
    (4) Periods of time when one-minute averages are not available 
shall be ignored when calculating three-hour rolling averages. When 
one-minute averages become available, the first one-minute average is 
added to the previous 179 values to calculate the three-hour rolling 
average.
    (5) When the operating status of the raw mill of the in-line kiln/
raw mill is changed from off to on, or from on to off the calculation 
of the three-hour rolling average temperature must begin anew, without 
considering previous recordings.
    (6) The calibration of all thermocouples and other temperature 
sensors shall be verified at least once every three months.
    (g) 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 (f)(1) through (f)(6) and (g)(1) through 
(g)(6) of this section to demonstrate continuous compliance with the D/
F emission standard.

[[Page 31932]]

    (1) Install, operate, calibrate and maintain a continuous monitor 
to record the rate of activated carbon injection. The accuracy of the 
rate measurement device must be 1 percent of the rate being 
measured.
    (2) Verify the calibration of the device at least once every three 
months.
    (3) The three-hour rolling average activated carbon injection rate 
shall be calculated as the average of 180 successive one-minute average 
activated carbon injection rates.
    (4) Periods of time when one-minute averages are not available 
shall be ignored when calculating three-hour rolling averages. When 
one-minute averages become available, the first one-minute average is 
added to the previous 179 values to calculate the three-hour rolling 
average.
    (5) When the operating status of the raw mill of the in-line kiln/
raw mill is changed from off to on, or from on to off the calculation 
of the three-hour rolling average activated carbon injection rate must 
begin anew, without considering previous recordings.
    (6) The owner or operator must install, operate, calibrate and 
maintain a continuous monitor to record the activated carbon injection 
system carrier gas parameter (either the carrier gas flow rate or the 
carrier gas pressure drop) established during the D/F performance test 
in accordance with paragraphs (g)(6)(i) through (g)(6)(iii) of this 
section.
    (i) The owner or operator shall install, calibrate, operate and 
maintain a device to continuously monitor and record the parameter 
value.
    (ii) The owner or operator must calculate and record three-hour 
rolling averages of the parameter value.
    (iii) Periods of time when one-minute averages are not available 
shall be ignored when calculating three-hour rolling averages. When 
one-minute averages become available, the first one-minute average 
shall be added to the previous 179 values to calculate the three-hour 
rolling average.
    (h) 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 (h)(1) through (h)(3) 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 and comply 
with all of the requirements for continuous monitoring systems found in 
the general provisions, subpart A of this part.
    (2) The owner or operator is not required to calculate hourly 
rolling averages in accordance with section 4.9 of Performance 
Specification 8A.
    (3) Any thirty-day block average THC concentration in any gas 
discharged from a greenfield raw material dryer, the main exhaust of a 
greenfield kiln, or the main exhaust of a greenfield in-line kiln/raw 
mill, exceeding 50 ppmvd, reported as propane, corrected to seven 
percent oxygen, is a violation of the standard.
    (i) The owner or operator of any kiln or in-line kiln/raw mill 
subject to a     D/F emission limit under this subpart shall conduct an 
inspection of the components of the combustion system of each kiln or 
in-line kiln raw mill at least once per year.
    (j) The owner or operator of an affected source subject to a 
limitation on opacity under Sec. 63.1346 or Sec. 63.1348 shall monitor 
opacity in accordance with the operation and maintenance plan developed 
in accordance with paragraph (a) of this section.
    (k) The owner or operator of an affected source subject to a 
particulate matter standard under Sec. 63.1343 shall install, 
calibrate, maintain and operate a particulate matter continuous 
emission monitoring system (PM CEMS) to measure the particulate matter 
discharged to the atmosphere. The compliance deadline for installing 
the PM CEMS and all requirements relating to performance of the PM CEMS 
and implementation of the PM CEMS requirement is deferred pending 
further rulemaking.
    (l) An owner or operator may submit an application to the 
Administrator for approval of alternate monitoring requirements to 
demonstrate compliance with the emission standards of this subpart, 
except for emission standards for THC, subject to the provisions of 
paragraphs (l)(1) through (l)(6) of this section.
    (1) The Administrator will not approve averaging periods other than 
those specified in this section, unless the owner or operator 
documents, using data or information, that the longer averaging period 
will ensure that emissions do not exceed levels achieved during the 
performance test over any increment of time equivalent to the time 
required to conduct three runs of the performance test.
    (2) If the application to use an alternate monitoring requirement 
is approved, the owner or operator must continue to use the original 
monitoring requirement until approval is received to use another 
monitoring requirement.
    (3) The owner or operator shall submit the application for approval 
of alternate monitoring requirements no later than the notification of 
performance test. The application must contain the information 
specified in paragraphs (l)(3)(i) through (l)(3)(iii) of this section:
    (i) Data or information justifying the request, such as the 
technical or economic infeasibility, or the impracticality of using the 
required approach;
    (ii) A description of the proposed alternative monitoring 
requirement, including the operating parameter to be monitored, the 
monitoring approach and technique, the averaging period for the limit, 
and how the limit is to be calculated; and
    (iii) Data or information documenting that the alternative 
monitoring requirement would provide equivalent or better assurance of 
compliance with the relevant emission standard.
    (4) The Administrator will notify the owner or operator of the 
approval or denial of the application within 90 calendar days after 
receipt of the original request, or within 60 calendar days of the 
receipt of any supplementary information, whichever is later. The 
Administrator will not approve an alternate monitoring application 
unless it would provide equivalent or better assurance of compliance 
with the relevant emission standard. Before disapproving any alternate 
monitoring application, the Administrator will provide:
    (i) Notice of the information and findings upon which the intended 
disapproval is based; and
    (ii) Notice of opportunity for the owner or operator to present 
additional supporting information before final action is taken on the 
application. This notice will specify how much additional time is 
allowed for the owner or operator to provide additional supporting 
information.
    (5) The owner or operator is responsible for submitting any 
supporting information in a timely manner to enable the Administrator 
to consider the application prior to the performance test. Neither 
submittal of an application, nor the Administrator's failure to approve 
or disapprove the application relieves the owner or operator of the 
responsibility to comply with any provision of this subpart.
    (6) The Administrator may decide at any time, on a case-by-case 
basis that additional or alternative operating limits, or alternative 
approaches to establishing operating limits, are necessary to 
demonstrate compliance with the emission standards of this subpart.

[[Page 31933]]

    (m) A summary of the monitoring requirements of this subpart is 
given in Table 1 to this section.

           Table 1 to Sec.  63.1350.--Monitoring Requirements
------------------------------------------------------------------------
Affected source/pollutant or      Monitor type/          Monitoring
           opacity              operation/process       requirements
------------------------------------------------------------------------
All affected sources........  Operations and        Prepare written plan
                               maintenance plan.     for all affected
                                                     sources and control
                                                     devices.
All kilns and in-line kiln    Continuous opacity    Install, calibrate,
 raw mills at major sources    monitor, if           maintain and
 (including alkali bypass)/    applicable.           operate in
 opacity.                                            accordance with
                                                     general provisions
                                                     and with PS-1.
                              Method 9 opacity      Daily test of at
                               test, if applicable.  least 30-minutes,
                                                     while kiln is at
                                                     highest load or
                                                     capacity level.
Kilns and in-line kiln raw    Particulate matter    Deferred.
 mills at major sources        continuous emission
 (including alkali bypass)/    monitoring system.
 particulate matter.
Kilns and in-line kiln raw    Combustion system     Conduct annual
 mills at major and area       inspection.           inspection of
 sources (including alkali                           components of
 bypass)/ D/F.                                       combustion system.
                              Continuous            Install, operate,
                               temperature           calibrate and
                               monitoring at PMCD    maintain continuous
                               inlet.                temperature
                                                     monitoring and
                                                     recording system;
                                                     calculate three-
                                                     hour rolling
                                                     averages; verify
                                                     temperature sensor
                                                     calibration at
                                                     least quarterly.
Kilns and in-line kiln raw    Activated carbon      Install, operate,
 mills at major and area       injection rate        calibrate and
 sources (including alkali     monitor, if           maintain continuous
 bypass)/ D/F (continued).     applicable.           activated carbon
                                                     injection rate
                                                     monitor; calculate
                                                     three-hour rolling
                                                     averages; verify
                                                     calibration at
                                                     least quarterly;
                                                     install, operate,
                                                     calibrate and
                                                     maintain carrier
                                                     gas flow rate
                                                     monitor or carrier
                                                     gas pressure drop
                                                     monitor; calculate
                                                     three-hour rolling
                                                     averages; document
                                                     carbon
                                                     specifications.
New greenfield kilns and in-  Total hydrocarbon     Install, operate,
 line kiln raw mills at        continuous emission   and maintain THC
 major and area sources/THC.   monitor.              CEM in accordance
                                                     with PS-8A;
                                                     calculate 30-day
                                                     block average THC
                                                     concentration.
Clinker coolers at major      Continuous opacity    Install, calibrate,
 sources/opacity.              monitor, if           maintain and
                               applicable.           operate in
                                                     accordance with
                                                     general provisions
                                                     and with PS-1.
                              Method 9 opacity      Daily test of at
                               test, if applicable.  least 30-minutes,
                                                     while kiln is at
                                                     highest load or
                                                     capacity level.
Raw mills and finish mills    Method 22 visible     Conduct daily 6-
 at major sources/opacity.     emissions test.       minute Method 22
                                                     visible emissions
                                                     test while mill is
                                                     operating at
                                                     highest load or
                                                     capacity level; if
                                                     visible emissions
                                                     are observed,
                                                     initiate corrective
                                                     action within one
                                                     hour and conduct 30-
                                                     minute Method 9
                                                     test within 24
                                                     hours.
New greenfield raw material   Total hydrocarbon     Install, operate,
 dryers at major and area      continuous emission   and maintain THC
 sources/THC.                  monitor.              CEM in accordance
                                                     with PS-8A;
                                                     calculate 30-day
                                                     block average THC
                                                     concentration.
Raw material dryers; raw      Method 22 visible     As specified in
 material, clinker, finished   emissions test.       operation and
 product storage bins;                               maintenance plan.
 conveying system transfer
 points; bagging systems;
 and bulk loading and
 unloading systems at major
 sources/opacity.
------------------------------------------------------------------------

Sec. 63.1351  Compliance dates.

    (a) The compliance date for an owner or operator of an existing 
affected source subject to the provisions of this subpart is June 10, 
2002.
    (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 June 9, 1999 or 
immediately upon startup of operations, whichever is later.


6Sec. 3.1352  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 
are permitted to use Method 320 or Method 321 of appendix A of this 
part.
    (b) 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 
are permitted to use Methods 26 or 26A of appendix A to part 60 of this 
chapter, except that the results of these tests shall not be used to 
establish status as an area source.
    (c) 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.

[[Page 31934]]

Notification, Reporting and Recordkeeping


Sec. 63.1353  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 as 
follows:
    (1) Initial notifications as required by Sec. 63.9(b) through (d). 
For the purposes of this subpart, a Title V or 40 CFR 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).
    (3) Notification of opacity and visible emission observations 
required by Sec. 63.1349 in accordance with Secs. 63.6(h)(5) and 
63.9(f).
    (4) Notification, as required by Sec. 63.9(g), of the date that the 
continuous emission monitor performance evaluation required by 
Sec. 63.8(e) is scheduled to begin.
    (5) Notification of compliance status, as required by Sec. 63.9(h).


Sec. 63.1354  Reporting requirements.

    (a) The reporting provisions of subpart A of this part that apply 
and those that do not apply to owners or operators 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 of this part 63, subpart A as follows:
    (1) As required by Sec. 63.10(d)(2), 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), the owner or operator of an 
affected source shall report the opacity results from tests required by 
Sec. 63.1349.
    (3) As required by Sec. 63.10(d)(4), 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) 
shall submit such reports by the dates specified in the written 
extension of compliance.
    (4) As required by Sec. 63.10(d)(5), 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), 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), 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). 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), 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 and described in Sec. 63.6(d)(6) shall report the results of 
the continuous opacity monitoring system performance evaluation 
conducted under Sec. 63.8(e).
    (8) As required by Sec. 63.10(e)(3), 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). In addition, the summary report shall include:
    (i) All exceedences of maximum control device inlet gas temperature 
limits specified in Sec. 63.1344(a) and (b);
    (ii) All failures to calibrate thermocouples and other temperature 
sensors as required under Sec. 63.1350(f)(7) of this subpart; and
    (iii) All failures to maintain the activated carbon injection rate, 
and the activated carbon injection carrier gas flow rate or pressure 
drop, as applicable, as required under Sec. 63.1344(c).
    (iv) The results of any combustion system component inspections 
conducted within the reporting period as required under 
Sec. 63.1350(i).
    (v) All failures to comply with any provision of the operation and 
maintenance plan developed in accordance with Sec. 63.1350(a).
    (10) If the total continuous monitoring system downtime for any CEM 
or any continuous monitoring system (CMS) for the reporting period is 
ten 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. 63.1355  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

[[Page 31935]]

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;
    (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), 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).

Other


Sec. 63.1356  Exemption from new source performance standards.

    (a) Except as provided in paragraphs (a)(1) and (a)(2) of this 
section, any affected source subject to the provisions of this subpart 
is exempted from any otherwise applicable new source performance 
standard contained in 40 CFR part 60, subpart F.
    (1) Kilns and in-line kiln/raw mills, as applicable under 40 CFR 
60.60(b), located at area sources are subject to PM and opacity limits 
and associated reporting and recordkeeping, under 40 CFR part 60, 
subpart F.
    (2) Greenfield raw material dryers, as applicable under 40 CFR 
60.60(b), located at area sources are subject to opacity limits and 
associated reporting and recordkeeping under 40 CFR part 60, subpart F.


Sec. 63.1357  Temporary, conditioned exemption from particulate matter 
and opacity standards.

    (a) Subject to the limitations of paragraphs (b) through (f) of 
this section, an owner or operator conducting PM CEMS correlation tests 
(that is, correlation with manual stack methods) is exempt from:
    (1) Any particulate matter and opacity standards of part 60 or part 
63 of this chapter that are applicable to cement kilns and in-line 
kiln/raw mills.
    (2) Any permit or other emissions or operating parameter or other 
limitation on workplace practices that are applicable to cement kilns 
and in-line kiln raw mills to ensure compliance with any particulate 
matter and opacity standards of this part or part 60 of this chapter.
    (b) The owner or operator must develop a PM CEMS correlation test 
plan. The plan must be submitted to the Administrator for approval at 
least 90 days before the correlation test is scheduled to be conducted. 
The plan must include:
    (1) The number of test conditions and the number of runs for each 
test condition;
    (2) The target particulate matter emission level for each test 
condition;
    (3) How the operation of the affected source will be modified to 
attain the desired particulate matter emission rate; and
    (4) The anticipated normal particulate matter emission level.
    (c) The Administrator will review and approve or disapprove the 
correlation test plan in accordance with Sec. 63.7(c)(3)(i) and (iii). 
If the Administrator fails to approve or disapprove the correlation 
test plan within the time period specified in Sec. 63.7(c)(3)(iii), the 
plan shall be considered approved, unless the Administrator has 
requested additional information.
    (d) The stack sampling team must be on-site and prepared to perform 
correlation testing no later than 24 hours after operations are 
modified to attain the desired particulate matter emissions 
concentrations, unless the correlation test plan documents that a 
longer period is appropriate.
    (e) The particulate matter and opacity standards and associated 
operating limits and conditions will not be waived for more than 96 
hours, in the aggregate, for a correlation test, including all runs and 
conditions.
    (f) The owner or operator must return the affected source to 
operating conditions indicative of compliance with the applicable 
particulate matter and opacity standards as soon as possible after 
correlation testing is completed.


Sec. 63.1358  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:
    (1) Approval of alternative non-opacity emission standards under 
Sec. 63.6(g).
    (2) Approval of alternative opacity standards under 
Sec. 63.6(h)(9).
    (3) Approval of major changes to test methods under 
Secs. 63.7(e)(2)(ii) and 63.7(f). A major change to a test method is a 
modification to a federally enforceable test method that uses unproven 
technology or procedures or is an entirely new method (sometimes 
necessary when the required test method is unsuitable).
    (4) Approval of major changes to monitoring under Sec. 63.8(f). A 
major change to monitoring is a modification to federally enforceable 
monitoring that uses unproven technology or procedures, is an entirely 
new method (sometimes necessary when the required monitoring is 
unsuitable), or is a change in the averaging period.
    (5) Waiver of recordkeeping under Sec. 63.10(f).


Sec. 63.1359  [Reserved]

                          Table 1 to Subpart LLL.--Applicability of General Provisions
----------------------------------------------------------------------------------------------------------------
 General Provisions 40 CFR Citation         Requirement         Applies to Subpart LLL           Comment
----------------------------------------------------------------------------------------------------------------
63.1(a)(1) through (4)..............  Applicability..........  Yes.                      .......................
63.1(a)(5)..........................                           No......................  [Reserved].
63.1(a)(6) through (a)(8)...........  Applicability..........  Yes.                      .......................
63.1(a)(9)..........................                           No......................  [Reserved].
63.1(a)(10) through (14)............  Applicability..........  Yes.                      .......................
63.1(b)(1)..........................  Initial Applicability    No......................  Sec.  63.1340 specifies
                                       Determination.                                     applicability.
63.1(b)(2) and (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.

[[Page 31936]]

 
63.1(c)(3)..........................                           No......................  [Reserved].
63.1(c)(4) and (5)..................  Extensions,              Yes.                      .......................
                                       Notifications.
63.1(d).............................                           No......................  [Reserved].
63.1(e).............................  Applicability of Permit  Yes.                      .......................
                                       Program.
63.2................................  Definitions............  Yes.                      Additional definitions
                                                                                          in Sec.  63.1341.
63.3(a) through (c).................  Units and Abbreviations  Yes.                      .......................
63.4(a)(1) through (a)(3)...........  Prohibited Activities..  Yes.                      .......................
63.4(a)(4)..........................                           No......................  [Reserved].
63.4(a)(5)..........................  Compliance date........  Yes.                      .......................
63.4(b) and (c).....................  Circumvention,           Yes.                      .......................
                                       Severability.
63.5(a)(1) and (2)..................  Construction/            Yes.                      .......................
                                       Reconstruction.
63.5(b)(1)..........................  Compliance Dates.......  Yes.                      .......................
63.5(b)(2)..........................                           No......................  [Reserved].
63.5(b)(3) through (6)..............  Construction Approval,   Yes.                      .......................
                                       Applicability.
63.5(c).............................                           No......................  [Reserved].
63.5(d)(1) through (4)..............  Approval of              Yes.                      .......................
                                       Construction/
                                       Reconstruction.
63.5(e).............................  Approval of              Yes.                      .......................
                                       Construction/
                                       Reconstruction.
63.5(f)(1) and (2)..................  Approval of              Yes.                      .......................
                                       Construction/
                                       Reconstruction.
63.6(a).............................  Compliance for           Yes.                      .......................
                                       Standards and
                                       Maintenance.
63.6(b)(1) through (5)..............  Compliance Dates.......  Yes.                      .......................
63.6(b)(6)..........................                           No......................  [Reserved].
63.6(b)(7)..........................  Compliance Dates.......  Yes.
63.6(c)(1) and (2)..................  Compliance Dates.......  Yes.
63.6(c)(3) and (c)(4)...............  .......................  No......................  [Reserved].
63.6(c)(5)..........................  Compliance Dates.......  Yes.
63.6(d).............................                           No......................  [Reserved].
63.6(e)(1) and (e)(2)...............  Operation & Maintenance  Yes.
63.6(e)(3)..........................  Startup, Shutdown        Yes.
                                       Malfunction Plan.
63.6(f)(1) through (3)..............  Compliance with          Yes.
                                       Emission Standards.
63.6(g)(1) through (g)(3)...........  Alternative Standard...  Yes.
63.6(h)(1) and (2)..................  Opacity/VE Standards...  Yes.
63.6(h)(3)..........................                           No......................  Reserved
63.6(h)(4) and (h)(5)(i)............  Opacity/VE Standards...  Yes.
63.6(h)(5)(ii) through (iv).........  Opacity/VE Standards...  No......................  Test duration specified
                                                                                          in Subpart LLL.
63.6(h)(6)..........................  Opacity/VE Standards...  Yes.
63.6(i)(1) through (i)(14)..........  Extension of Compliance  Yes.
63.6(i)(15).........................                           No......................  [Reserved].
63.6(i)(16).........................  Extension of Compliance  Yes.
63.6(j).............................  Exemption from           Yes.
                                       Compliance.
63.7(a)(1) through (a)(3)...........  Performance Testing      Yes.....................  Sec.  63.1349 has
                                       Requirements.                                      specific requirements.
63.7(b).............................  Notification...........  Yes.
63.7(c).............................  Quality Assurance/Test   Yes.
                                       Plan.
63.7(d).............................  Testing Facilities.....  Yes.
63.7(e)(1) through (4)..............  Conduct of Tests.......  Yes.
63.7(f).............................  Alternative Test Method  Yes.
63.7(g).............................  Data Analysis..........  Yes.
63.7(h).............................  Waiver of Tests........  Yes.
63.8(a)(1)..........................  Monitoring Requirements  Yes.
63.8(a)(2)..........................  Monitoring.............  No......................  Sec.  63.1350 includes
                                                                                          CEM requirements.
63.8(a)(3)..........................                           No......................  [Reserved].
63.8(a)(4)..........................  Monitoring.............  No......................  Flares not applicable.
63.8(b)(1) through (3)..............  Conduct of Monitoring..  Yes.
63.8(c)(1) through (8)..............  CMS Operation/           Yes.                      Performance
                                       Maintenance.                                       specification
                                                                                          supersedes
                                                                                          requirements for THC
                                                                                          CEM. Temperature and
                                                                                          activated carbon
                                                                                          injection monitoring
                                                                                          data reduction
                                                                                          requirements given in
                                                                                          subpart LLL.
63.8(d).............................  Quality Control........  Yes.
63.8(e).............................  Performance Evaluation   Yes.....................  Performance
                                       for CMS.                                           specification
                                                                                          supersedes
                                                                                          requirements for THC
                                                                                          CEM.
63.8(f)(1) through (f)(5)...........  Alternative Monitoring   Yes.....................  Additional requirements
                                       Method.                                            in Sec.  1350(l).
63.8(f)(6)..........................  Alternative to RATA      Yes.
                                       Test.
63.8(g).............................  Data Reduction.........  Yes.
63.9(a).............................  Notification             Yes.
                                       Requirements.
63.9(b)(1) through (5)..............  Initial Notifications..  Yes.
63.9(c).............................  Request for Compliance   Yes.
                                       Extension.
63.9(d).............................  New Source Notification  Yes.
                                       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.  63.1350(e) and
                                                                                          (j).

[[Page 31937]]

 
63.9(g).............................  Additional CMS           Yes.
                                       Notifications.
63.9(h)(1) through (h)(3)...........  Notification of          Yes.
                                       Compliance Status.
63.9(h)(4)..........................                           No......................  [Reserved].
63.9(h)(5) and (h)(6)...............  Notification of          Yes.
                                       Compliance Status.
63.9(i).............................  Adjustment of Deadlines  Yes.
63.9(j).............................  Change in Previous       Yes.
                                       Information.
63.10(a)............................  Recordkeeping/Reporting  Yes                       Yes.
63.10(b)............................  General Requirements...  Yes.
63.10(c)(1).........................  Additional CMS           Yes.....................  PS-8A applies.
                                       Recordkeeping.
63.10(c)(2) through (c)(4)..........                           No......................  Reserved]
63.10(c)(5) through (c)(8)..........  Additional CMS           Yes.....................  PS-8A applies instead
                                       Recordkeeping.                                     of requirements for
                                                                                          THC CEM.
63.10(c)(9).........................                           No......................  [Reserved]
63.10(c)(10) through (15)...........  Additional CMS           Yes.....................  PS-8A applies instead
                                       Recordkeeping.                                     of requirements for
                                                                                          THC CEM.
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) and (e)(2)..............  Additional CMS Reports.  Yes.
63.10(e)(3).........................  Excess Emissions and     Yes.....................  Exceedences are defined
                                       CMS Performance                                    in subpart LLL.
                                       Reports.
63.10(f)............................  Waiver for               Yes.
                                       Recordkeeping/
                                       Reporting.
63.11(a) and (b)....................  Control Device           No......................  Flares not applicable.
                                       Requirements.
63.12(a)-(c.........................  )State Authority and     Yes.
                                       Delegations.
63.13(a)-(c)........................  State/Regional           Yes.
                                       Addresses.
63.14(a) and (b)....................  Incorporation by         Yes.
                                       Reference.
63.15(a) and (b)....................  Availability of          Yes.
                                       Information.
----------------------------------------------------------------------------------------------------------------

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

Appendix A to Part 63--Test Methods

* * * * *

Test 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 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.

[[Page 31938]]

    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 8.6.2 
and 9.0 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.
[GRAPHIC] [TIFF OMITTED] TR14JN99.003

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 instrumental 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 in sections 
3.1 through 3.29.
    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 to the addendum of 
this method). 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 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

[[Page 31939]]

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.
    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

[[Page 31940]]

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., Balston'') 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.
    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

[[Page 31941]]

``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] TR14JN99.004

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 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 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, 
continuous sampling is preferable using the smallest cell volume, 
fastest sampling rate and fastest spectra collection rate possible. 
Continuous sampling requires the least operator intervention even 
without an automated sampling system. For continuous monitoring at 
one location over long periods, Continuous 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

[[Page 31942]]

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 continuous) 
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 continuous 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 
 
  
 
. 
 

    
 

.

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/
analytical 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/analytical conditions are being duplicated. If 
the QA spike fails then the sampling/analytical 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, when possible.
    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: where:
[GRAPHIC] [TIFF OMITTED] TR14JN99.005

      
Where:

[GRAPHIC] [TIFF OMITTED] TR14JN99.006

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.
Unspike=Native concentration of analytes in unspiked 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 
pressure (Pf). Calculate the FTIR cell volume VSS, 
including that of the connecting tubing, as follows:

[[Page 31943]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.007



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] TR14JN99.008

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.
Ps=Sample cell pressure.
Pr=Reference spectrum sample pressure.

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:

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Where:

B = Bias at spike level.
Sm = Mean concentration of the analyte spiked 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 is 
determined that the bias is significant and CF >  30 
percent, then the test method is considered to ``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.
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Sample time                   Spectrum file name          Background file name         Sample conditioning           Process condition
--------------------------------------------------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
--------------------------------------------------------------------------------------------------------------------------------------------------------


 
          Sample time              Spectrum file      Interferogram        Resolution        Scans        Apodization         Gain        CTS Spectrum
--------------------------------------------------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
--------------------------------------------------------------------------------------------------------------------------------------------------------

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[GRAPHIC] [TIFF OMITTED] TR14JN99.011



BILLING CODE 6560-50-O

Addendum to Test 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  Appendix 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

[[Page 31947]]

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 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.

[[Page 31948]]

    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 
appendix 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 appendix 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. Appendix 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 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 appendix 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 appendix 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 appendix G of this addendum. Estimate the 
minimum measurement uncertainty for each analyte (MAUi, 
ppm) and known interferant (MIUk, ppm) using appendix 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 appendix 
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 appendix 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 appendix 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,
[GRAPHIC] [TIFF OMITTED] TR14JN99.012


[[Page 31949]]


Calculate the final analyte and interferant concentrations 
RSAi and RSIk using equations A.2 and A.3,
[GRAPHIC] [TIFF OMITTED] TR14JN99.013

[GRAPHIC] [TIFF OMITTED] TR14JN99.014

    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.

Appendix 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.
    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

[[Page 31950]]

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 protocol are defined as follows:
    (1) A, absorbance = the logarithm to the base 10 of the 
reciprocal of the transmittance (T).
[GRAPHIC] [TIFF OMITTED] TR14JN99.015

    (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.
    (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).


[[Page 31951]]


    (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{FRUi, 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] TR14JN99.016

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] TR14JN99.017

    (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 appendix D of 
this addendum.

Appendix 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.

BILLING CODE 6560-50-P

[[Page 31952]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.018



BILLING CODE 6560-50-C

[[Page 31953]]

Appendix 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 appendix 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] TR14JN99.019

Appendix 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 (appendix G of this addendum), or 
set RMS = RMSEST 
if estimated (appendix C of this addendum).
    D.2.2  For each analyte associated with the analytical region, 
calculate MAUim using equation D.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.020

    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] TR14JN99.021

where the weight Wik is defined for each term in the sum 
as
[GRAPHIC] [TIFF OMITTED] TR14JN99.022

    D.2.5  Repeat sections D.2.1 through D.2.4 of this appendix 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.

Appendix 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,

[[Page 31954]]

[GRAPHIC] [TIFF OMITTED] TR14JN99.023


    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] TR14JN99.024

where the Wik are calculated as described in appendix D 
of this addendum.

Appendix F of 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)                                     ISC (ppm)
                                                name
                                                                                                       Analytes    Interferants
                                                                                                           i=1         I
                                                                                                           j=1         J
--------------------------------------------------------------------------------------------------------------------------------------------------------
 
 
 
 
 
 
--------------------------------------------------------------------------------------------------------------------------------------------------------


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

Appendix 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.

Appendix 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

[[Page 31955]]

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 E2. Calculate the sample 
absorption pathlength, LS, using equation H.1,
[GRAPHIC] [TIFF OMITTED] TR14JN99.025

    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] TR14JN99.026

[GRAPHIC] [TIFF OMITTED] TR14JN99.027

    The fractional analytical uncertainty, FAU, is given by equation 
H.4,
[GRAPHIC] [TIFF OMITTED] TR14JN99.028

Appendix 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] TR14JN99.029

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,
[GRAPHIC] [TIFF OMITTED] TR14JN99.030

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] TR14JN99.031

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] TR14JN99.032

where Wik is calculated as described in appendix D of 
this addendum.

[[Page 31956]]

Appendix J of 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}.

Test 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 presents example values of AU and 
MAU using the analytical region presented in Table 1.

 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.......................................................     2.28E-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.

[[Page 31957]]

    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 appendix 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 
appendix.

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.
    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 appendix for a complete description of the use 
of existing HCl reference spectra. See section 9.1 of Method 320 of 
this appendix 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

[[Page 31958]]

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). 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.

[[Page 31959]]

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.
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Sm = Mean concentration of the analyte spiked effluent 
samples (observed).
[GRAPHIC] [TIFF OMITTED] TR14JN99.034

Ce = Expected concentration of the spiked samples 
(theoretical).
Df = dilution Factor (Total flow/Spike 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
[GRAPHIC] [TIFF OMITTED] TR14JN99.035

[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 appendix (Reference 8) as,
[GRAPHIC] [TIFF OMITTED] TR14JN99.036

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 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.

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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
[GRAPHIC] [TIFF OMITTED] TR14JN99.037

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, appendix 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.

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