[Federal Register Volume 62, Number 115 (Monday, June 16, 1997)]
[Rules and Regulations]
[Pages 32500-32536]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 97-15374]


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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 51

[FRL-5836-1]
RIN 2060-AF02


Preparation, Adoption, and Submittal of State Implementation 
Plans; Appendix M, Test Methods 204, 204A-204F

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: This rule adds seven methods to Appendix M of 40 CFR Part 51 
for capture efficiency (CE) testing to assist States in adopting 
enforceable CE measurement protocols into their State implementation 
plans (SIP's) for ozone. These final methods, in conjunction with the 
protocols, would also improve EPA's ability to enforce State 
regulations to reduce volatile organic compounds (VOC) emissions in 
ozone nonattainment areas.

EFFECTIVE DATE: These methods are effective June 16, 1997.

ADDRESSES: Docket. A Docket A-91-70, containing materials relevant to 
this rulemaking, is available for public inspection and copying between 
8:00 a.m.-5:30 p.m., Monday through Friday, at the EPA's Air Docket 
Section Mail Code: 6102, Room M-1500, Waterside Mall (ground floor), 
401 M Street, S.W., Washington D.C. 20460. A reasonable fee may be 
charged for copying.

FOR FURTHER INFORMATION CONTACT: Candace Sorrell, Source 
Characterization Group A (MD-19), Emissions, Monitoring, and Analysis 
Division, U.S. Environmental Protection Agency, Research Triangle Park, 
North Carolina 27711, telephone (919) 541-1064.

SUPPLEMENTARY INFORMATION:

I. The Rulemaking

    This rulemaking adds seven methods for measuring CE to Appendix M 
of 40 CFR Part 51 to provide methods that States can use in their 
SIP's.

II. Public Participation

    The proposed rulemaking was published in the Federal Register (FR) 
on August 2, 1995 (60 FR 39297).
    The opportunity to hold a public hearing on August 30, 1995 at 10 
a.m. was presented in the proposal notice, but no one desired to make 
an oral presentation. The public comment period was from August 2, 1995 
to October 2, 1995.

III. Electronic Access

    The background information document for the promulgated test 
methods is available on the Technology Transfer Network (TTN) on the 
EPA's electronic bulletin boards. The document is entitled ``Summary of 
Comments and Responses for Methods 204, 204A-F.'' If necessary, a 
limited number of copies are available from Candace Sorrell, MD-19, 
U.S. EPA, Research Triangle Park, North Carolina 27711, telephone 
number (919) 541-1064.

IV. Significant Comments and Changes to the Proposed Rulemaking

    Six comment letters were received from the proposal rulemaking. A 
detailed discussion of these comments is contained in the background 
document entitled ``Summary of Comments and Responses for Methods 204, 
204A-F,'' which is referred to in the SUPPLEMENTARY INFORMATION section 
of this preamble. The major comments raised in these letters and the 
Agency's responses follow.
    One commenter points out that even though Methods 204B and 204C 
measure the same parameter, captured VOC stream, the applicability 
sections of the methods were not consistent with respect to what type 
of material balance is permissible.
    The EPA reviewed the applicability section for both methods and 
determined that there was an error in Method 204B. Method 204B is 
intended to be used only in a gas/gas protocol, not in a liquid/gas 
protocol. The method has been revised to correct this error.
    One commenter suggests for Method 204D, section 8.2.4, and Method 
204E, section 8.4, that EPA make it explicit that if on site gas 
chromatography (GC) is used as an alternative to flame ionization 
analyzers (FIA) than GC must also be used to measure the VOC 
concentration of the other gas or liquid steams.
    The Agency agrees that further explanation is needed to explain 
that if a facility is conducting a gas/gas test and chooses to use the 
alternative GC procedure, it must use the GC procedure for both the 
captured and fugitive stream. If a facility wishes to conduct a liquid/
gas test using GC, the facility must use Method 204F for the liquid 
steam. A GC is not an acceptable alternative to the FIA in Method 204A.
    Another commenter suggests that Figure 204-1 of Method 204 be 
expanded to address capture efficiencies less than 80 percent since 
lower values are allowed in the current Reasonably Available Control 
Technology (RACT) rules.
    The EPA agrees that further guidance is needed and has added an 
equation to section 7.2 to help in estimating the ventilation rate at 
different capture efficiencies.
    Three commenters mention that Method 204A, section 11, the 
estimated uncertainty of 12 percent for the VOC fraction seemed too 
high.
    The EPA went back and reviewed the method evaluation report and 
discovered that the 12 percent is an error. The estimated uncertainty 
for this method is 4.0 percent. The method has been revised to correct 
this error.
    Two commenters note that several references in Method 204, sections 
5.5 and 6.1, were incorrect.
    The EPA agrees that several references in those sections are 
incorrect. The method has been revised to correct these errors.

[[Page 32501]]

    A commenter suggests that section 8.4 of Method 204 be revised to 
be consistent with the Aerospace NESHAP concerning the verification of 
air flow direction.
    The EPA agrees with the comment and the method has been revised to 
reflect these changes.
    One commenter feels that dilutions systems calibrated using Method 
205 should be allowed without approval of the Administrator in Methods 
204A-E, section 5.1 and Method 204F, section 5.3.
    The EPA agrees that calibration gas can be prepared using dilution 
systems calibrated using Method 205 without approval of the 
Administrator and the methods have been revised.
    A commenter requested that Methods 204A-204F be revised to not 
automatically invalidate the CE results if the drift check is in excess 
of the proposed 3 percent calibration drift requirement. In such 
situations the method should allow the FIA to be recalibrated and 
whichever calibration results in the ``worst case'' results be 
reported.
    The EPA agrees with the comment and the methods have been revised.
    One commenter suggests that Methods 204A-E, section 5.1.1 and 
Method 204F, section 5.3.1, be revised to allow for the use of hydrogen 
in air if appropriate adjustments are made to eliminate the oxygen 
synergism effect.
    The Agency agrees that alternative mixtures should be allowed if 
the user can demonstrate to the Administrator that there is no oxygen 
synergism effect. The method has been revised to allow alternative 
mixtures.
    One commenter notes that in Methods 204, 204A-F the term ``fugitive 
emissions'' is used in a manner inconsistent with the definition 
contained in 40 CFR 51.165(a)(1)(ix). The commenter suggests the word 
``fugitive'' should be changed to ``uncaptured.''
    The Agency agrees and the methods have been revised to change 
``fugitive'' to ``uncaptured.''
    A commenter feels that in Method 204A and 204F the required 
accuracy of the input weight determinations should be changed to allow 
the balance/digital scales to weigh within 2 lbs instead of the 
proposed 0.2 lb.
    The Agency believes that it is very important to get an accurate 
measurement of the amount of coating used during a test and that scales 
that read to within 2 lbs are not accurate enough in most test 
situations. However, after reviewing this issue, the Agency also feels 
that the 0.2 lb limit may be too restrictive in some situations. 
Therefore, the method has been revised to read ``within 0.2 lb or 1.0 
percent of the total weight of VOC liquid used.''
    The EPA has recently discovered that the pressure drop specified in 
section 8.3 of Method 204, which is suppose to correspond to the 
minimum required face velocity of 3,600 m/hr (200 fpm), is too low. 
According to the twenty first edition of the ``Industrial Ventilation'' 
handbook dated 1992 the required pressure drop is 0.013 mm Hg (0.007 
in. H2O). Therefore, Method 204 has been revised to reflect 
this finding.

IV. Administrative Requirements

A. Docket

    The docket is an organized and complete file for all information 
submitted or otherwise considered by EPA in the development of this 
promulgated rulemaking. The principal purposes of the docket are: (1) 
To allow interested parties to identify and locate documents so that 
they can effectively participate in the rulemaking process, and
    (2) To serve as the record in case of judicial review (except for 
interagency review materials) [Clean Air Act Section 307(d)(7)(A)].

B. Office of Management and Budget Review

    Under Executive Order 12866 (58 FR 51735 October 4, 1993), the EPA 
is required to judge whether a regulation is ``significant'' and 
therefore subject to Office of Management and Budget (OMB) review and 
the requirements of this Executive Order to prepare a regulatory impact 
analysis (RIA). The Order defines ``significant regulatory action'' as 
one that is likely to result in a rule that may: (1) Have an annual 
effect on the economy of $100 million or more or adversely affect in a 
material way the economy, a sector of the economy, productivity, 
competition, jobs, the environment, public health or safety, or State, 
local, or tribal governments or communities; (2) create a serious 
inconsistency or otherwise interfere with an action taken or planned by 
another agency; (3) materially alter the budgetary impact of 
entitlements, grants, user fees, or loan programs, or the rights and 
obligation of recipients thereof; or (4) raise novel legal or policy 
issues arising out of legal mandates, the President's priorities, or 
the principles set forth in the Executive Order. Pursuant to the terms 
of the Executive Order, this action has been determined to be ``not 
significant.''

C. Regulatory Flexibility Act Compliance

    The EPA has determined that it is not necessary to prepare a 
regulatory flexibility analysis in connection with this final rule. The 
EPA has also determined that this rule will not have a significant 
adverse impact on a substantial number of small businesses. This 
rulemaking does not impose emission measurement requirements beyond 
those specified in the current regulations, nor does it change any 
emission standard. As such, it will not present a significant economic 
impact on a substantial number of small businesses.

D. Paperwork Reduction Act

    The rule does not change any information collection requirements 
subject of Office of Management and Budget review under the Paperwork 
Reduction Act of 1980, 44 U.S.C. 3501 et seq.

E. Unfunded Mandates

    Under Section 202 of the Unfunded Mandates Reform Act of 1995 
(``Unfunded Mandates Act''), signed into law on March 22, 1995, EPA 
must prepare a budgetary impact statement to accompany any proposed or 
final rule that includes a Federal mandate that may result in estimated 
costs to State, local, or tribal governments in the aggregate; or to 
the private sector, of $100 million or more. Under Section 205, EPA 
must select the most cost-effective and least burdensome alternative 
that achieves the objectives of the rule and is consistent with 
statutory requirements. Section 203 requires EPA to establish a plan 
for significantly or uniquely impacted by the rule.
    EPA has determined that this final action does not include a 
Federal mandate that may result in estimated costs of $100 million or 
more to either State, local, or tribal governments in the aggregate, or 
to the private sector, nor does this action significantly or uniquely 
impact small governments, because this action contains no requirements 
that apply to such governments or impose obligations upon them. 
Therefore, the requirements of the Unfunded Mandates Act do not apply 
to this action.

F. Submission to Congress and the General Accounting Office

    Under 5 U.S.C. 801(a)(1)(A) of the Administrative Procedures Act 
(APA), as added by the Small Business Regulatory Enforcement Fairness 
Act of 1996, the EPA submitted a report containing this rule and other 
required

[[Page 32502]]

information to the U.S. Senate, the U.S. House of Representatives and 
the Comptroller General of the General Accounting Office prior to 
publication of the rule in today's Federal Register. This rule is not a 
``major rule'' as defined by 5 U.S.C. 804(2).

List of Subjects in 40 CFR Part 51

    Environmental protection, Administrative practice and procedure, 
Air pollution control, Capture efficiency, Carbon monoxide, 
Intergovernmental relations, Lead, Nitrogen dioxide, Ozone, Particulate 
matter, Printing operations, Reporting and recordkeeping requirements, 
Surface coating operations, Sulfur oxides, Volatile organic compounds.

    Dated: May 30, 1997.
Carol M. Browner,
Administrator.

    For the reasons set out in the preamble, Appendix M of 40 CFR Part 
51 is amended as follows:
    1. The authority citation for part 51 continues to read as follows:

    Authority: 42 U.S.C. 7410.

    2. Appendix M, Table of Contents is amended by adding seven entries 
to read as follows:

Appendix M to Part 51--Recommended Test Methods for State 
Implementation Plans

* * * * *
    Method 204--Criteria for and Verification of a Permanent or 
Temporary Total Enclosure.
    Method 204A--Volatile Organic Compounds Content in Liquid Input 
Stream.
    Method 204B--Volatile Organic Compounds Emissions in Captured 
Stream.
    Method 204C--Volatile Organic Compounds Emissions in Captured 
Stream (Dilution Technique).
    Method 204D--Volatile Organic Compounds Emissions in Uncaptured 
Stream from Temporary Total Enclosure.
    Method 204E--Volatile Organic Compounds Emissions in Uncaptured 
Stream from Building Enclosure.
    Method 204F--Volatile Organic Compounds Content in Liquid Input 
Stream (Distillation Approach).
* * * * *
    3. By adding Method 204 to read as follows:

Method 204--Criteria for and Verification of a Permanent or Temporary 
Total Enclosure

1. Scope and Application

    This procedure is used to determine whether a permanent or 
temporary enclosure meets the criteria for a total enclosure. An 
existing building may be used as a temporary or permanent enclosure as 
long as it meets the appropriate criteria described in this method.

2. Summary of Method

    An enclosure is evaluated against a set of criteria. If the 
criteria are met and if all the exhaust gases from the enclosure are 
ducted to a control device, then the volatile organic compounds (VOC) 
capture efficiency (CE) is assumed to be 100 percent, and CE need not 
be measured. However, if part of the exhaust gas stream is not ducted 
to a control device, CE must be determined.

3. Definitions

     3.1  Natural Draft Opening (NDO). Any permanent opening in the 
enclosure that remains open during operation of the facility and is not 
connected to a duct in which a fan is installed.
    3.2  Permanent Total Enclosure (PE). A permanently installed 
enclosure that completely surrounds a source of emissions such that all 
VOC emissions are captured and contained for discharge to a control 
device.
    3.3  Temporary Total Enclosure (TTE). A temporarily installed 
enclosure that completely surrounds a source of emissions such that all 
VOC emissions that are not directed through the control device (i.e. 
uncaptured) are captured by the enclosure and contained for discharge 
through ducts that allow for the accurate measurement of the uncaptured 
VOC emissions.
    3.4  Building Enclosure (BE). An existing building that is used as 
a TTE.

4. Safety

    An evaluation of the proposed building materials and the design for 
the enclosure is recommended to minimize any potential hazards.

5. Criteria for Temporary Total Enclosure

    5.1  Any NDO shall be at least four equivalent opening diameters 
from each VOC emitting point unless otherwise specified by the 
Administrator.
    5.2  Any exhaust point from the enclosure shall be at least four 
equivalent duct or hood diameters from each NDO.
    5.3  The total area of all NDO's shall not exceed 5 percent of the 
surface area of the enclosure's four walls, floor, and ceiling.
    5.4  The average facial velocity (FV) of air through all NDO's 
shall be at least 3,600 m/hr (200 fpm). The direction of air flow 
through all NDO's shall be into the enclosure.
    5.5  All access doors and windows whose areas are not included in 
section 5.3 and are not included in the calculation in section 5.4 
shall be closed during routine operation of the process.

6. Criteria for a Permanent Total Enclosure

    6.1  Same as sections 5.1 and 5.3 through 5.5.
    6.2  All VOC emissions must be captured and contained for discharge 
through a control device.

7. Quality Control

    7.1  The success of this method lies in designing the TTE to 
simulate the conditions that exist without the TTE (i.e., the effect of 
the TTE on the normal flow patterns around the affected facility or the 
amount of uncaptured VOC emissions should be minimal). The TTE must 
enclose the application stations, coating reservoirs, and all areas 
from the application station to the oven. The oven does not have to be 
enclosed if it is under negative pressure. The NDO's of the temporary 
enclosure and an exhaust fan must be properly sized and placed.
    7.2  Estimate the ventilation rate of the TTE that best simulates 
the conditions that exist without the TTE (i.e., the effect of the TTE 
on the normal flow patterns around the affected facility or the amount 
of uncaptured VOC emissions should be minimal). Figure 204-1 or the 
following equation may be used as an aid.
[GRAPHIC] [TIFF OMITTED] TR16JN97.000

Measure the concentration (CG) and flow rate (QG) 
of the captured gas stream, specify a safe concentration 
(CF) for the uncaptured gas stream, estimate the CE, and 
then use the plot in Figure 204-1 or Equation 204-1 to determine the 
volumetric flow rate of the uncaptured gas stream (QF). An exhaust fan 
that has a variable flow control is desirable.
    7.3  Monitor the VOC concentration of the captured gas steam in the 
duct before the capture device without the TTE. To minimize the effect 
of temporal variation on the captured emissions, the baseline 
measurement should be made over as long a time period as practical. 
However, the process conditions must be the same for the measurement in 
section 7.5 as they are for this baseline measurement. This may require 
short measuring times for this quality control check before and after 
the construction of the TTE.
    7.4  After the TTE is constructed, monitor the VOC concentration 
inside the TTE. This concentration should not continue to increase, and 
must not exceed the safe level according to

[[Page 32503]]

Occupational Safety and Health Administration requirements for 
permissible exposure limits. An increase in VOC concentration indicates 
poor TTE design.
    7.5  Monitor the VOC concentration of the captured gas stream in 
the duct before the capture device with the TTE. To limit the effect of 
the TTE on the process, the VOC concentration with and without the TTE 
must be within 10 percent. If the measurements do not agree, adjust the 
ventilation rate from the TTE until they agree within 10 percent.

8. Procedure

    8.1  Determine the equivalent diameters of the NDO's and determine 
the distances from each VOC emitting point to all NDO's. Determine the 
equivalent diameter of each exhaust duct or hood and its distance to 
all NDO's. Calculate the distances in terms of equivalent diameters. 
The number of equivalent diameters shall be at least four.
    8.2  Measure the total surface area (AT) of the 
enclosure and the total area (AN) of all NDO's in the 
enclosure. Calculate the NDO to enclosure area ratio (NEAR) as follows:
[GRAPHIC] [TIFF OMITTED] TR16JN97.001

The NEAR must be 10.05.
    8.3  Measure the volumetric flow rate, corrected to standard 
conditions, of each gas stream exiting the enclosure through an exhaust 
duct or hood using EPA Method 2. In some cases (e.g., when the building 
is the enclosure), it may be necessary to measure the volumetric flow 
rate, corrected to standard conditions, of each gas stream entering the 
enclosure through a forced makeup air duct using Method 2. Calculate FV 
using the following equation:
[GRAPHIC] [TIFF OMITTED] TR16JN97.002

where:
QO = the sum of the volumetric flow from all gas streams 
exiting the enclosure through an exhaust duct or hood.
QI = the sum of the volumetric flow from all gas streams 
into the enclosure through a forced makeup air duct; zero, if there is 
no forced makeup air into the enclosure.
AN = total area of all NDO's in enclosure.

    The FV shall be at least 3,600 m/hr (200 fpm). Alternatively, 
measure the pressure differential across the enclosure. A pressure drop 
of 0.013 mm Hg (0.007 in. H2O) corresponds to an FV of 3,600 
m/hr (200 fpm).
    8.4  Verify that the direction of air flow through all NDO's is 
inward. If FV is less than 9,000 m/hr (500 fpm), the continuous inward 
flow of air shall be verified using streamers, smoke tubes, or tracer 
gases. Monitor the direction of air flow for at least 1 hour, with 
checks made no more than 10 minutes apart. If FV is greater than 9,000 
m/hr (500 fpm), the direction of air flow through the NDOs shall be 
presumed to be inward at all times without verification.

9. Diagrams

BILLING CODE 6560-50-P

[[Page 32504]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.026



BILLING CODE 6560-50-C

[[Page 32505]]

Method 204A--Volatile Organic Compounds Content in Liquid Input Stream

1. Scope and Application

    1.1  Applicability. This procedure is applicable for determining 
the input of volatile organic compounds (VOC). It is intended to be 
used in the development of liquid/gas protocols for determining VOC 
capture efficiency (CE) for surface coating and printing operations.
    1.2  Principle. The amount of VOC introduced to the process (L) is 
the sum of the products of the weight (W) of each VOC containing liquid 
(ink, paint, solvent, etc.) used and its VOC content (V).
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    The amount of VOC containing liquid introduced to the process is 
determined as the weight difference of the feed material before and 
after each sampling run. The VOC content of the liquid input material 
is determined by volatilizing a small aliquot of the material and 
analyzing the volatile material using a flame ionization analyzer 
(FIA). A sample of each VOC containing liquid is analyzed with an FIA 
to determine V.

3. Safety

    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.

4. Equipment and Supplies

    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Liquid Weight.
    4.1.1  Balances/Digital Scales. To weigh drums of VOC containing 
liquids to within 0.2 lb or 1.0 percent of the total weight of VOC 
liquid used.
    4.1.2  Volume Measurement Apparatus (Alternative). Volume meters, 
flow meters, density measurement equipment, etc., as needed to achieve 
the same accuracy as direct weight measurements.
    4.2  VOC Content (FIA Technique). The liquid sample analysis system 
is shown in Figures 204A-1 and 204A-2. The following equipment is 
required:
    4.2.1  Sample Collection Can. An appropriately-sized metal can to 
be used to collect VOC containing materials. The can must be 
constructed in such a way that it can be grounded to the coating 
container.
    4.2.2  Needle Valves. To control gas flow.
    4.2.3  Regulators. For carrier gas and calibration gas cylinders.
    4.2.4  Tubing. Teflon or stainless steel tubing with diameters and 
lengths determined by connection requirements of equipment. The tubing 
between the sample oven outlet and the FIA shall be heated to maintain 
a temperature of 1205  deg.C.
    4.2.5  Atmospheric Vent. A tee and 0- to 0.5-liter/min rotameter 
placed in the sampling line between the carrier gas cylinder and the 
VOC sample vessel to release the excess carrier gas. A toggle valve 
placed between the tee and the rotameter facilitates leak tests of the 
analysis system.
    4.2.6  Thermometer. Capable of measuring the temperature of the hot 
water bath to within 1  deg.C.
    4.2.7  Sample Oven. Heated enclosure, containing calibration gas 
coil heaters, critical orifice, aspirator, and other liquid sample 
analysis components, capable of maintaining a temperature of 
1205  deg.C.
    4.2.8  Gas Coil Heaters. Sufficient lengths of stainless steel or 
Teflon tubing to allow zero and calibration gases to be heated to the 
sample oven temperature before entering the critical orifice or 
aspirator.
    4.2.9  Water Bath. Capable of heating and maintaining a sample 
vessel temperature of 1005  deg.C.
    4.2.10  Analytical Balance. To measure 0.001 g.
    4.2.11  Disposable Syringes. 2-cc or 5-cc.
    4.2.12  Sample Vessel. Glass, 40-ml septum vial. A separate vessel 
is needed for each sample.
    4.2.13  Rubber Stopper. Two-hole stopper to accommodate 3.2-mm (\1/
8\-in.) Teflon tubing, appropriately sized to fit the opening of the 
sample vessel. The rubber stopper should be wrapped in Teflon tape to 
provide a tighter seal and to prevent any reaction of the sample with 
the rubber stopper. Alternatively, any leak-free closure fabricated of 
nonreactive materials and accommodating the necessary tubing fittings 
may be used.
    4.2.14  Critical Orifices. Calibrated critical orifices capable of 
providing constant flow rates from 50 to 250 ml/min at known pressure 
drops. Sapphire orifice assemblies (available from O'Keefe Controls 
Company) and glass capillary tubing have been found to be adequate for 
this application.
    4.2.15  Vacuum Gauge. Zero to 760-mm (0- to 30-in.) Hg U-Tube 
manometer or vacuum gauge.
    4.2.16  Pressure Gauge. Bourdon gauge capable of measuring the 
maximum air pressure at the aspirator inlet (e.g., 100 psig).
    4.2.17  Aspirator. A device capable of generating sufficient vacuum 
at the sample vessel to create critical flow through the calibrated 
orifice when sufficient air pressure is present at the aspirator inlet. 
The aspirator must also provide sufficient sample pressure to operate 
the FIA. The sample is also mixed with the dilution gas within the 
aspirator.
    4.2.18  Soap Bubble Meter. Of an appropriate size to calibrate the 
critical orifices in the system.
    4.2.19  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated that they would provide 
more accurate measurements. The FIA instrument should be the same 
instrument used in the gaseous analyses adjusted with the same fuel, 
combustion air, and sample back-pressure (flow rate) settings. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.2.19.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.2.19.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.2.19.3  Calibration Error. Less than 5.0 percent of 
the calibration gas value.
    4.2.20  Integrator/Data Acquisition System. An analog or digital 
device or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated values is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2.21  Chart Recorder (Optional). A chart recorder or similar 
device is recommended to provide a continuous analog display of the 
measurement results during the liquid sample analysis.

5. Reagents and Standards

    5.1  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be

[[Page 32506]]

certified by the manufacturer to 1 percent of the tag 
value. Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing calibration gas mixtures may be used with the 
approval of the Administrator.
    5.1.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He or 40 percent H2/60 
percent N2 gas mixture is recommended to avoid an oxygen 
synergism effect that reportedly occurs when oxygen concentration 
varies significantly from a mean value. Other mixtures may be used 
provided the tester can demonstrate to the Administrator that there is 
no oxygen synergism effect.
    5.1.2  Carrier Gas. High purity air with less than 1 ppm of organic 
material (as propane) or less than 0.1 percent of the span value, 
whichever is greater.
    5.1.3  FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentrations of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
to the Administrator's satisfaction that equally accurate measurements 
would be achieved.
    5.1.4  System Calibration Gas. Gas mixture standard containing 
propane in air, approximating the undiluted VOC concentration expected 
for the liquid samples.

6. Sample Collection, Preservation and Storage

    6.1  Samples must be collected in a manner that prevents or 
minimizes loss of volatile components and that does not contaminate the 
coating reservoir.
    6.2  Collect a 100-ml or larger sample of the VOC containing liquid 
mixture at each application location at the beginning and end of each 
test run. A separate sample should be taken of each VOC containing 
liquid added to the application mixture during the test run. If a fresh 
drum is needed during the sampling run, then obtain a sample from the 
fresh drum.
    6.3  When collecting the sample, ground the sample container to the 
coating drum. Fill the sample container as close to the rim as possible 
to minimize the amount of headspace.
    6.4  After the sample is collected, seal the container so the 
sample cannot leak out or evaporate.
    6.5  Label the container to clearly identify the contents.

7. Quality Control

    7.1  Required instrument quality control parameters are found in 
the following sections:
    7.1.1  The FIA system must be calibrated as specified in section 
8.1.
    7.1.2  The system drift check must be performed as specified in 
section 8.2.
    7.2  Audits.
    7.2.1  Audit Procedure. Concurrently, analyze the audit sample and 
a set of compliance samples in the same manner to evaluate the 
technique of the analyst and the standards preparation. The same 
analyst, analytical reagents, and analytical system shall be used both 
for compliance samples and the EPA audit sample. If this condition is 
met, auditing of subsequent compliance analyses for the same 
enforcement agency within 30 days is not required. An audit sample set 
may not be used to validate different sets of compliance samples under 
the jurisdiction of different enforcement agencies, unless prior 
arrangements are made with both enforcement agencies.
    7.2.2  Audit Samples and Audit Sample Availability. Audit samples 
will be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B), Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Laboratory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    7.2.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

8. Calibration and Standardization

    8.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system and 
adjust the back-pressure regulator to the value required to achieve the 
flow rates specified by the manufacturer. Inject the zero- and the 
high-range calibration gases and adjust the analyzer calibration to 
provide the proper responses. Inject the low- and mid-range gases and 
record the responses of the measurement system. The calibration and 
linearity of the system are acceptable if the responses for all four 
gases are within 5 percent of the respective gas values. If the 
performance of the system is not acceptable, repair or adjust the 
system and repeat the linearity check. Conduct a calibration and 
linearity check after assembling the analysis system and after a major 
change is made to the system.
    8.2  Systems Drift Checks. After each sample, repeat the system 
calibration checks in section 9.2.7 before any adjustments to the FIA 
or measurement system are made. If the zero or calibration drift 
exceeds 3 percent of the span value, discard the result and 
repeat the analysis.
    Alternatively, recalibrate the FIA as in section 8.1 and report the 
results using both sets of calibration data (i.e., data determined 
prior to the test period and data determined following the test 
period). The data that results in the lowest CE value shall be reported 
as the results for the test run.
    8.3  Critical Orifice Calibration.
    8.3.1  Each critical orifice must be calibrated at the specific 
operating conditions under which it will be used. Therefore, assemble 
all components of the liquid sample analysis system as shown in Figure 
204A-3. A stopwatch is also required.
    8.3.2  Turn on the sample oven, sample line, and water bath 
heaters, and allow the system to reach the proper operating 
temperature. Adjust the aspirator to a vacuum of 380 mm (15 in.) Hg 
vacuum. Measure the time required for one soap bubble to move a known 
distance and record barometric pressure.
    8.3.3  Repeat the calibration procedure at a vacuum of 406 mm (16 
in.) Hg and at 25-mm (1-in.) Hg intervals until three consecutive 
determinations provide the same flow rate. Calculate the critical flow 
rate for the orifice in ml/min at standard conditions. Record the 
vacuum necessary to achieve critical flow.

[[Page 32507]]

9. Procedure

    9.1  Determination of Liquid Input Weight.
    9.1.1  Weight Difference. Determine the amount of material 
introduced to the process as the weight difference of the feed material 
before and after each sampling run. In determining the total VOC 
containing liquid usage, account for:
    (a) The initial (beginning) VOC containing liquid mixture.
    (b) Any solvent added during the test run.
    (c) Any coating added during the test run.
    (d) Any residual VOC containing liquid mixture remaining at the end 
of the sample run.
    9.1.1.1  Identify all points where VOC containing liquids are 
introduced to the process. To obtain an accurate measurement of VOC 
containing liquids, start with an empty fountain (if applicable). After 
completing the run, drain the liquid in the fountain back into the 
liquid drum (if possible) and weigh the drum again. Weigh the VOC 
containing liquids to 0.5 percent of the total weight 
(full) or 1.0 percent of the total weight of VOC containing 
liquid used during the sample run, whichever is less. If the residual 
liquid cannot be returned to the drum, drain the fountain into a 
preweighed empty drum to determine the final weight of the liquid.
    9.1.1.2  If it is not possible to measure a single representative 
mixture, then weigh the various components separately (e.g., if solvent 
is added during the sampling run, weigh the solvent before it is added 
to the mixture). If a fresh drum of VOC containing liquid is needed 
during the run, then weigh both the empty drum and fresh drum.
    9.1.2  Volume Measurement (Alternative). If direct weight 
measurements are not feasible, the tester may use volume meters or flow 
rate meters and density measurements to determine the weight of liquids 
used if it can be demonstrated that the technique produces results 
equivalent to the direct weight measurements. If a single 
representative mixture cannot be measured, measure the components 
separately.
    9.2  Determination of VOC Content in Input Liquids
    9.2.1 Assemble the liquid VOC content analysis system as shown in 
Figure 204A-1.
    9.2.2  Permanently identify all of the critical orifices that may 
be used. Calibrate each critical orifice under the expected operating 
conditions (i.e., sample vacuum and temperature) against a volume meter 
as described in section 8.3.
    9.2.3  Label and tare the sample vessels (including the stoppers 
and caps) and the syringes.
    9.2.4  Install an empty sample vessel and perform a leak test of 
the system. Close the carrier gas valve and atmospheric vent and 
evacuate the sample vessel to 250 mm (10 in.) Hg absolute or less using 
the aspirator. Close the toggle valve at the inlet to the aspirator and 
observe the vacuum for at least 1 minute. If there is any change in the 
sample pressure, release the vacuum, adjust or repair the apparatus as 
necessary, and repeat the leak test.
    9.2.5  Perform the analyzer calibration and linearity checks 
according to the procedure in section 5.1. Record the responses to each 
of the calibration gases and the back-pressure setting of the FIA.
    9.2.6  Establish the appropriate dilution ratio by adjusting the 
aspirator air supply or substituting critical orifices. Operate the 
aspirator at a vacuum of at least 25 mm (1 in.) Hg greater than the 
vacuum necessary to achieve critical flow. Select the dilution ratio so 
that the maximum response of the FIA to the sample does not exceed the 
high-range calibration gas.
    9.2.7  Perform system calibration checks at two levels by 
introducing compressed gases at the inlet to the sample vessel while 
the aspirator and dilution devices are operating. Perform these checks 
using the carrier gas (zero concentration) and the system calibration 
gas. If the response to the carrier gas exceeds 0.5 percent 
of span, clean or repair the apparatus and repeat the check. Adjust the 
dilution ratio as necessary to achieve the correct response to the 
upscale check, but do not adjust the analyzer calibration. Record the 
identification of the orifice, aspirator air supply pressure, FIA back-
pressure, and the responses of the FIA to the carrier and system 
calibration gases.
    9.2.8  After completing the above checks, inject the system 
calibration gas for approximately 10 minutes. Time the exact duration 
of the gas injection using a stopwatch. Determine the area under the 
FIA response curve and calculate the system response factor based on 
the sample gas flow rate, gas concentration, and the duration of the 
injection as compared to the integrated response using Equations 204A-2 
and 204A-3.
    9.2.9  Verify that the sample oven and sample line temperatures are 
120 5 deg.C and that the water bath temperature is 
100 5 deg.C.
    9.2.10  Fill a tared syringe with approximately 1 g of the VOC 
containing liquid and weigh it. Transfer the liquid to a tared sample 
vessel. Plug the sample vessel to minimize sample loss. Weigh the 
sample vessel containing the liquid to determine the amount of sample 
actually received. Also, as a quality control check, weigh the empty 
syringe to determine the amount of material delivered. The two coating 
sample weights should agree within 0.02 g. If not, repeat the procedure 
until an acceptable sample is obtained.
    9.2.11  Connect the vessel to the analysis system. Adjust the 
aspirator supply pressure to the correct value. Open the valve on the 
carrier gas supply to the sample vessel and adjust it to provide a 
slight excess flow to the atmospheric vent. As soon as the initial 
response of the FIA begins to decrease, immerse the sample vessel in 
the water bath. (Applying heat to the sample vessel too soon may cause 
the FIA response to exceed the calibrated range of the instrument and, 
thus, invalidate the analysis.)
    9.2.12  Continuously measure and record the response of the FIA 
until all of the volatile material has been evaporated from the sample 
and the instrument response has returned to the baseline (i.e., 
response less than 0.5 percent of the span value). Observe the 
aspirator supply pressure, FIA back-pressure, atmospheric vent, and 
other system operating parameters during the run; repeat the analysis 
procedure if any of these parameters deviate from the values 
established during the system calibration checks in section 9.2.7. 
After each sample, perform the drift check described in section 8.2. If 
the drift check results are acceptable, calculate the VOC content of 
the sample using the equations in section 11.2. Alternatively, 
recalibrate the FIA as in section 8.1 and report the results using both 
sets of calibration data (i.e., data determined prior to the test 
period and data determined following the test period). The data that 
results in the lowest CE value shall be reported as the results for the 
test run. Integrate the area under the FIA response curve, or determine 
the average concentration response and the duration of sample analysis.

10. Data Analysis and Calculations

    10.1  Nomenclature.
AL=area under the response curve of the liquid sample, area 
count.
AS=area under the response curve of the calibration gas, 
area count.
CS=actual concentration of system calibration gas, ppm 
propane.
K=1.830  x  10-9 g/(ml-ppm).
L=total VOC content of liquid input, kg.

[[Page 32508]]

ML=mass of liquid sample delivered to the sample vessel, g.
q = flow rate through critical orifice, ml/min.
RF=liquid analysis system response factor, g/area count.
    S=total gas injection time for system 
calibration gas during integrator calibration, min.
    VFj=final VOC fraction of VOC containing liquid j.
VIj=initial VOC fraction of VOC containing liquid j.
VAj=VOC fraction of VOC containing liquid j added during the 
run.
V=VOC fraction of liquid sample.
WFj=weight of VOC containing liquid j remaining at end of 
the run, kg.
WIj=weight of VOC containing liquid j at beginning of the 
run, kg.
WAj=weight of VOC containing liquid j added during the run, 
kg.
10.2  Calculations
    10.2.1  Total VOC Content of the Input VOC Containing Liquid.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.003
    
    10.2.2  Liquid Sample Analysis System Response Factor for Systems 
Using Integrators, Grams/Area Count.
[GRAPHIC] [TIFF OMITTED] TR16JN97.004

    10.2.3  VOC Content of the Liquid Sample.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.005
    
11. Method Performance

    The measurement uncertainties are estimated for each VOC containing 
liquid as follows: W = 2.0 percent and V = 4.0 
percent. Based on these numbers, the probable uncertainty for L is 
estimated at about 4.5 percent for each VOC containing 
liquid.

12. Diagrams

BILLING CODE 6560-50-P

[[Page 32509]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.036



[[Page 32510]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.037



[[Page 32511]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.038



BILLING CODE 6560-50-C

[[Page 32512]]

Method 204B--Volatile Organic Compounds Emissions in Captured Stream

1. Scope and Application

    1.1  Applicability. This procedure is applicable for determining 
the volatile organic compounds (VOC) content of captured gas streams. 
It is intended to be used in the development of a gas/gas protocol for 
determining VOC capture efficiency (CE) for surface coating and 
printing operations. The procedure may not be acceptable in certain 
site-specific situations [e.g., when: (1) direct-fired heaters or other 
circumstances affect the quantity of VOC at the control device inlet; 
and (2) particulate organic aerosols are formed in the process and are 
present in the captured emissions].
    1.2  Principle. The amount of VOC captured (G) is calculated as the 
sum of the products of the VOC content (CGj), the flow rate 
(QGj), and the sample time (C) from 
each captured emissions point.
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    A gas sample is extracted from the source though a heated sample 
line and, if necessary, a glass fiber filter to a flame ionization 
analyzer (FIA).

3. Safety

    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.

4. Equipment and Supplies

    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Gas VOC Concentration. A schematic of the measurement system 
is shown in Figure 204B-1. The main components are as follows:
    4.1.1  Sample Probe. Stainless steel or equivalent. The probe shall 
be heated to prevent VOC condensation.
    4.1.2  Calibration Valve Assembly. Three-way valve assembly at the 
outlet of the sample probe to direct the zero and calibration gases to 
the analyzer. Other methods, such as quick-connect lines, to route 
calibration gases to the outlet of the sample probe are acceptable.
    4.1.3  Sample Line. Stainless steel or Teflon tubing to transport 
the sample gas to the analyzer. The sample line must be heated to 
prevent condensation.
    4.1.4  Sample Pump. A leak-free pump, to pull the sample gas 
through the system at a flow rate sufficient to minimize the response 
time of the measurement system. The components of the pump that contact 
the gas stream shall be constructed of stainless steel or Teflon. The 
sample pump must be heated to prevent condensation.
    4.1.5  Sample Flow Rate Control. A sample flow rate control valve 
and rotameter, or equivalent, to maintain a constant sampling rate 
within 10 percent. The flow rate control valve and rotameter must be 
heated to prevent condensation. A control valve may also be located on 
the sample pump bypass loop to assist in controlling the sample 
pressure and flow rate.
    4.1.6  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated to the Administrator's 
satisfaction that they would provide equally accurate measurements. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.1.6.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.1.6.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.1.6.3  Calibration Error. Less than 5.0 percent of 
the calibration gas value.
    4.1.6.4  Response Time. Less than 30 seconds.
    4.1.7  Integrator/Data Acquisition System. An analog or digital 
device, or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated values is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2  Captured Emissions Volumetric Flow Rate.
    4.2.1  Method 2 or 2A Apparatus. For determining volumetric flow 
rate.
    4.2.2  Method 3 Apparatus and Reagents. For determining molecular 
weight of the gas stream. An estimate of the molecular weight of the 
gas stream may be used if approved by the Administrator.
    4.2.3  Method 4 Apparatus and Reagents. For determining moisture 
content, if necessary.

5. Reagents and Standards

    5.1  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be certified 
by the manufacturer to 1 percent of the tag value. 
Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing calibration gas mixtures may be used with the 
approval of the Administrator.
    5.1.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He or 40 percent 
H2/60 percent N2 gas mixture is recommended to 
avoid an oxygen synergism effect that reportedly occurs when oxygen 
concentration varies significantly from a mean value. Other mixtures 
may be used provided the tester can demonstrate to the Administrator 
that there is no oxygen synergism effect.
    5.1.2  Carrier Gas. High purity air with less than 1 ppm of organic 
material (as propane or carbon equivalent) or less than 0.1 percent of 
the span value, whichever is greater.
    5.1.3  FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentrations of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
to the Administrator's satisfaction that equally accurate measurements 
would be achieved.
    5.2  Particulate Filter. An in-stack or an out-of-stack glass fiber 
filter is recommended if exhaust gas particulate loading is 
significant. An out-of-stack filter must be heated to prevent any 
condensation unless it can be demonstrated that no condensation occurs.

6. Quality Control

    6.1  Required instrument quality control parameters are found in 
the following sections:
    6.1.1  The FIA system must be calibrated as specified in section 
7.1.
    6.1.2  The system drift check must be performed as specified in 
section 7.2.
    6.1.3  The system check must be conducted as specified in section 
7.3.

[[Page 32513]]

    6.2  Audits.
    6.2.1  Analysis Audit Procedure. Immediately before each test, 
analyze an audit cylinder as described in section 7.2. The analysis 
audit must agree with the audit cylinder concentration within 10 
percent.
    6.2.2  Audit Samples and Audit Sample Availability. Audit samples 
will be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B), Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Labortory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    6.2.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

7. Calibration and Standardization

    7.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system and 
adjust the back-pressure regulator to the value required to achieve the 
flow rates specified by the manufacturer. Inject the zero-and the high-
range calibration gases and adjust the analyzer calibration to provide 
the proper responses. Inject the low- and mid-range gases and record 
the responses of the measurement system. The calibration and linearity 
of the system are acceptable if the responses for all four gases are 
within 5 percent of the respective gas values. If the performance of 
the system is not acceptable, repair or adjust the system and repeat 
the linearity check. Conduct a calibration and linearity check after 
assembling the analysis system and after a major change is made to the 
system.
    7.2  Systems Drift Checks. Select the calibration gas that most 
closely approximates the concentration of the captured emissions for 
conducting the drift checks. Introduce the zero and calibration gases 
at the calibration valve assembly and verify that the appropriate gas 
flow rate and pressure are present at the FIA. Record the measurement 
system responses to the zero and calibration gases. The performance of 
the system is acceptable if the difference between the drift check 
measurement and the value obtained in section 7.1 is less than 3 
percent of the span value. Alternatively, recalibrate the FIA as in 
section 7.1 and report the results using both sets of calibration data 
(i.e., data determined prior to the test period and data determined 
following the test period). The data that results in the lowest CE 
value shall be reported as the results for the test run. Conduct the 
system drift checks at the end of each run.
    7.3  System Check. Inject the high-range calibration gas at the 
inlet of the sampling probe and record the response. The performance of 
the system is acceptable if the measurement system response is within 5 
percent of the value obtained in section 7.1 for the high-range 
calibration gas. Conduct a system check before and after each test run.

8. Procedure

    8.1.  Determination of Volumetric Flow Rate of Captured Emissions.
    8.1.1  Locate all points where emissions are captured from the 
affected facility. Using Method 1, determine the sampling points. Be 
sure to check each site for cyclonic or swirling flow.
    8.1.2  Measure the velocity at each sampling site at least once 
every hour during each sampling run using Method 2 or 2A.
    8.2  Determination of VOC Content of Captured Emissions.
    8.2.1  Analysis Duration. Measure the VOC responses at each 
captured emissions point during the entire test run or, if applicable, 
while the process is operating. If there are multiple captured emission 
locations, design a sampling system to allow a single FIA to be used to 
determine the VOC responses at all sampling locations.
    8.2.2  Gas VOC Concentration.
    8.2.2.1  Assemble the sample train as shown in Figure 204B-1. 
Calibrate the FIA according to the procedure in section 7.1.
    8.2.2.2  Conduct a system check according to the procedure in 
section 7.3.
    8.2.2.3  Install the sample probe so that the probe is centrally 
located in the stack, pipe, or duct, and is sealed tightly at the stack 
port connection.
    8.2.2.4  Inject zero gas at the calibration valve assembly. Allow 
the measurement system response to reach zero. Measure the system 
response time as the time required for the system to reach the effluent 
concentration after the calibration valve has been returned to the 
effluent sampling position.
    8.2.2.5  Conduct a system check before, and a system drift check 
after, each sampling run according to the procedures in sections 7.2 
and 7.3. If the drift check following a run indicates unacceptable 
performance (see section 7.3), the run is not valid. Alternatively, 
recalibrate the FIA as in section 7.1 and report the results using both 
sets of calibration data (i.e., data determined prior to the test 
period and data determined following the test period). The data that 
results in the lowest CE value shall be reported as the results for the 
test run. The tester may elect to perform system drift checks during 
the run not to exceed one drift check per hour.
    8.2.2.6  Verify that the sample lines, filter, and pump 
temperatures are 1205  deg.C.
    8.2.2.7  Begin sampling at the start of the test period and 
continue to sample during the entire run. Record the starting and 
ending times and any required process information as appropriate. If 
multiple captured emission locations are sampled using a single FIA, 
sample at each location for the same amount of time (e.g., 2 minutes) 
and continue to switch from one location to another for the entire test 
run. Be sure that total sampling time at each location is the same at 
the end of the test run. Collect at least four separate measurements 
from each sample point during each hour of testing. Disregard the 
measurements at each sampling location until two times the response 
time of the measurement system has elapsed. Continue sampling for at 
least 1 minute and record the concentration measurements.
    8.2.3  Background Concentration.

    Note: Not applicable when the building is used as the temporary 
total enclosure (TTE).

    8.2.3.1  Locate all natural draft openings (NDO's) of the TTE. A 
sampling point shall be at the center of each NDO, unless otherwise 
specified by the Administrator. If there are more than six NDO's, 
choose six sampling points evenly spaced among the NDO's.
    8.2.3.2  Assemble the sample train as shown in Figure 204B-2. 
Calibrate the FIA and conduct a system check according to the 
procedures in sections 7.1 and 7.3.


[[Page 32514]]


    Note: This sample train shall be separate from the sample train 
used to measure the captured emissions.

    8.2.3.3  Position the probe at the sampling location.
    8.2.3.4  Determine the response time, conduct the system check, and 
sample according to the procedures described in sections 8.2.2.4 
through 8.2.2.7.
    8.2.4  Alternative Procedure. The direct interface sampling and 
analysis procedure described in section 7.2 of Method 18 may be used to 
determine the gas VOC concentration. The system must be designed to 
collect and analyze at least one sample every 10 minutes. If the 
alternative procedure is used to determine the VOC concentration of the 
captured emissions, it must also be used to determine the VOC 
concentration of the uncaptured emissions.

9. Data Analysis and Calculations

    9.1  Nomenclature.

Ai=area of NDO i, ft\2\.
AN=total area of all NDO's in the enclosure, ft\2\.
CBi=corrected average VOC concentration of background 
emissions at point i, ppm propane.
CB=average background concentration, ppm propane.
CGj=corrected average VOC concentration of captured 
emissions at point j, ppm propane.
CDH=average measured concentration for the drift check 
calibration gas, ppm propane.
CDO=average system drift check concentration for zero 
concentration gas, ppm propane.
CH=actual concentration of the drift check calibration gas, 
ppm propane.
Ci=uncorrected average background VOC concentration measured 
at point i, ppm propane.
Cj=uncorrected average VOC concentration measured at point 
j, ppm propane.
G=total VOC content of captured emissions, kg.
K1=1.830 x 10-6 kg/(m\3\-ppm).
n=number of measurement points.
QGj=average effluent volumetric flow rate corrected to 
standard conditions at captured emissions point j, m\3\/min.
C=total duration of captured emissions.
    9.2  Calculations.
    9.2.1  Total VOC Captured Emissions.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.006
    
    9.2.2  VOC Concentration of the Captured Emissions at Point j.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.007
    
    9.2.3  Background VOC Concentration at Point i.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.008
    
    9.2.4  Average Background Concentration.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.009
    
    Note: If the concentration at each point is within 20 percent of 
the average concentration of all points, then use the arithmetic 
average.

10. Method Performance

    The measurement uncertainties are estimated for each captured or 
uncaptured emissions point as follows: QGj=5.5 
percent and CGj=5.0 percent. Based on these 
numbers, the probable uncertainty for G is estimated at about 
7.4 percent.

11. Diagrams

BILLING CODE 6560-50-P

[[Page 32515]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.027



[[Page 32516]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.028



BILLING CODE 6560-50-C

[[Page 32517]]

Method 204C--Volatile Organic Compounds Emissions in Captured Stream 
(Dilution Technique)

1. Scope and Application

    1.1  Applicability. This procedure is applicable for determining 
the volatile organic compounds (VOC) content of captured gas streams. 
It is intended to be used in the development of a gas/gas protocol in 
which uncaptured emissions are also measured for determining VOC 
capture efficiency (CE) for surface coating and printing operations. A 
dilution system is used to reduce the VOC concentration of the captured 
emissions to about the same concentration as the uncaptured emissions. 
The procedure may not be acceptable in certain site-specific situations 
[e.g., when: (1) direct-fired heaters or other circumstances affect the 
quantity of VOC at the control device inlet; and (2) particulate 
organic aerosols are formed in the process and are present in the 
captured emissions].
    1.2  Principle. The amount of VOC captured (G) is calculated as the 
sum of the products of the VOC content (CGj), the flow rate 
(QGj), and the sampling time (C) from 
each captured emissions point.
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    A gas sample is extracted from the source using an in-stack 
dilution probe through a heated sample line and, if necessary, a glass 
fiber filter to a flame ionization analyzer (FIA). The sample train 
contains a sample gas manifold which allows multiple points to be 
sampled using a single FIA.

3. Safety

    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.

4. Equipment and Supplies

    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Gas VOC Concentration. A schematic of the measurement system 
is shown in Figure 204C-1. The main components are as follows:
    4.1.1  Dilution System. A Kipp in-stack dilution probe and 
controller or similar device may be used. The dilution rate may be 
changed by substituting different critical orifices or adjustments of 
the aspirator supply pressure. The dilution system shall be heated to 
prevent VOC condensation. Note: An out-of-stack dilution device may be 
used.
    4.1.2  Calibration Valve Assembly. Three-way valve assembly at the 
outlet of the sample probe to direct the zero and calibration gases to 
the analyzer. Other methods, such as quick-connect lines, to route 
calibration gases to the outlet of the sample probe are acceptable.
    4.1.3  Sample Line. Stainless steel or Teflon tubing to transport 
the sample gas to the analyzer. The sample line must be heated to 
prevent condensation.
    4.1.4  Sample Pump. A leak-free pump, to pull the sample gas 
through the system at a flow rate sufficient to minimize the response 
time of the measurement system. The components of the pump that contact 
the gas stream shall be constructed of stainless steel or Teflon. The 
sample pump must be heated to prevent condensation.
    4.1.5  Sample Flow Rate Control. A sample flow rate control valve 
and rotameter, or equivalent, to maintain a constant sampling rate 
within 10 percent. The flow control valve and rotameter must be heated 
to prevent condensation. A control valve may also be located on the 
sample pump bypass loop to assist in controlling the sample pressure 
and flow rate.
    4.1.6  Sample Gas Manifold. Capable of diverting a portion of the 
sample gas stream to the FIA, and the remainder to the bypass discharge 
vent. The manifold components shall be constructed of stainless steel 
or Teflon. If captured or uncaptured emissions are to be measured at 
multiple locations, the measurement system shall be designed to use 
separate sampling probes, lines, and pumps for each measurement 
location and a common sample gas manifold and FIA. The sample gas 
manifold and connecting lines to the FIA must be heated to prevent 
condensation.

    Note: Depending on the number of sampling points and their 
location, it may not be possible to use only one FIA. However to 
reduce the effect of calibration error, the number of FIA's used 
during a test should be keep as small as possible.

    4.1.7  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated to the Administrator's 
satisfaction that they would provide equally accurate measurements. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.1.7.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.1.7.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.1.7.3  Calibration Error. Less than 5.0 percent of 
the calibration gas value.
    4.1.7.4  Response Time. Less than 30 seconds.
    4.1.8  Integrator/Data Acquisition System. An analog or digital 
device or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated values is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2  Captured Emissions Volumetric Flow Rate.
    4.2.1  Method 2 or 2A Apparatus. For determining volumetric flow 
rate.
    4.2.2  Method 3 Apparatus and Reagents. For determining molecular 
weight of the gas stream. An estimate of the molecular weight of the 
gas stream may be used if approved by the Administrator.
    4.2.3  Method 4 Apparatus and Reagents. For determining moisture 
content, if necessary.

5. Reagents and Standards

    5.1  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be certified 
by the manufacturer to 1 percent of the tag value. 
Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing calibration gas mixtures may be used with the 
approval of the Administrator.
    5.1.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He or 40 percent 
H2/60 percent N2 gas mixture is recommended to 
avoid an oxygen synergism effect that reportedly occurs when oxygen 
concentration varies

[[Page 32518]]

significantly from a mean value. Other mixtures may be used provided 
the tester can demonstrate to the Administrator that there is no oxygen 
synergism effect
    5.1.2   Carrier Gas and Dilution Air Supply. High purity air with 
less than 1 ppm of organic material (as propane or carbon equivalent), 
or less than 0.1 percent of the span value, whichever is greater.
    5.1.3   FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentrations of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
to the Administrator's satisfaction that equally accurate measurements 
would be achieved.
    5.1.4  Dilution Check Gas. Gas mixture standard containing propane 
in air, approximately half the span value after dilution.
    5.2  Particulate Filter. An in-stack or an out-of-stack glass fiber 
filter is recommended if exhaust gas particulate loading is 
significant. An out-of-stack filter must be heated to prevent any 
condensation unless it can be demonstrated that no condensation occurs.

6. Quality Control

    6.1  Required instrument quality control parameters are found in 
the following sections:
    6.1.1  The FIA system must be calibrated as specified in section 
7.1.
    6.1.2  The system drift check must be performed as specified in 
section 7.2.
    6.1.3  The dilution factor must be determined as specified in 
section 7.3.
    6.1.4  The system check must be conducted as specified in section 
7.4.
    6.2  Audits.
    6.2.1  Analysis Audit Procedure. Immediately before each test, 
analyze an audit cylinder as described in section 7.2. The analysis 
audit must agree with the audit cylinder concentration within 10 
percent.
    6.2.2  Audit Samples and Audit Sample Availability. Audit samples 
will be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B), Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Laboratory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    6.2.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

7. Calibration and Standardization

    7.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system 
after the dilution system and adjust the back-pressure regulator to the 
value required to achieve the flow rates specified by the manufacturer. 
Inject the zero-and the high-range calibration gases and adjust the 
analyzer calibration to provide the proper responses. Inject the low-
and mid-range gases and record the responses of the measurement system. 
The calibration and linearity of the system are acceptable if the 
responses for all four gases are within 5 percent of the respective gas 
values. If the performance of the system is not acceptable, repair or 
adjust the system and repeat the linearity check. Conduct a calibration 
and linearity check after assembling the analysis system and after a 
major change is made to the system.
    7.2  Systems Drift Checks. Select the calibration gas that most 
closely approximates the concentration of the diluted captured 
emissions for conducting the drift checks. Introduce the zero and 
calibration gases at the calibration valve assembly, and verify that 
the appropriate gas flow rate and pressure are present at the FIA. 
Record the measurement system responses to the zero and calibration 
gases. The performance of the system is acceptable if the difference 
between the drift check measurement and the value obtained in section 
7.1 is less than 3 percent of the span value. Alternatively, 
recalibrate the FIA as in section 7.1 and report the results using both 
sets of calibration data (i.e., data determined prior to the test 
period and data determined following the test period). The data that 
results in the lowest CE value shall be reported as the results for the 
test run. Conduct the system drift check at the end of each run.
    7.3  Determination of Dilution Factor. Inject the dilution check 
gas into the measurement system before the dilution system and record 
the response. Calculate the dilution factor using Equation 204C-3.
    7.4  System Check. Inject the high-range calibration gas at the 
inlet to the sampling probe while the dilution air is turned off. 
Record the response. The performance of the system is acceptable if the 
measurement system response is within 5 percent of the value obtained 
in section 7.1 for the high-range calibration gas. Conduct a system 
check before and after each test run.

8. Procedure

    8.1  Determination of Volumetric Flow Rate of Captured Emissions
    8.1.1  Locate all points where emissions are captured from the 
affected facility. Using Method 1, determine the sampling points. Be 
sure to check each site for cyclonic or swirling flow.
    8.2.2  Measure the velocity at each sampling site at least once 
every hour during each sampling run using Method 2 or 2A.
    8.2  Determination of VOC Content of Captured Emissions
    8.2.1  Analysis Duration. Measure the VOC responses at each 
captured emissions point during the entire test run or, if applicable, 
while the process is operating. If there are multiple captured 
emissions locations, design a sampling system to allow a single FIA to 
be used to determine the VOC responses at all sampling locations.
    8.2.2  Gas VOC Concentration.
    8.2.2.1  Assemble the sample train as shown in Figure 204C-1. 
Calibrate the FIA according to the procedure in section 7.1.
    8.2.2.2  Set the dilution ratio and determine the dilution factor 
according to the procedure in section 7.3.
    8.2.2.3  Conduct a system check according to the procedure in 
section 7.4.
    8.2.2.4  Install the sample probe so that the probe is centrally 
located in the stack, pipe, or duct, and is sealed tightly at the stack 
port connection.
    8.2.2.5  Inject zero gas at the calibration valve assembly. Measure 
the system response time as the time required for the system to reach 
the effluent concentration after the calibration valve has been 
returned to the effluent sampling position.
    8.2.2.6  Conduct a system check before, and a system drift check 
after,

[[Page 32519]]

each sampling run according to the procedures in sections 7.2 and 7.4. 
If the drift check following a run indicates unacceptable performance 
(see section 7.4), the run is not valid. Alternatively, recalibrate the 
FIA as in section 7.1 and report the results using both sets of 
calibration data (i.e., data determined prior to the test period and 
data determined following the test period). The data that results in 
the lowest CE value shall be reported as the results for the test run. 
The tester may elect to perform system drift checks during the run not 
to exceed one drift check per hour.
    8.2.2.7  Verify that the sample lines, filter, and pump 
temperatures are 120 5  deg.C.
    8.2.2.8  Begin sampling at the start of the test period and 
continue to sample during the entire run. Record the starting and 
ending times and any required process information as appropriate. If 
multiple captured emission locations are sampled using a single FIA, 
sample at each location for the same amount of time (e.g., 2 min.) and 
continue to switch from one location to another for the entire test 
run. Be sure that total sampling time at each location is the same at 
the end of the test run. Collect at least four separate measurements 
from each sample point during each hour of testing. Disregard the 
measurements at each sampling location until two times the response 
time of the measurement system has elapsed. Continue sampling for at 
least 1 minute and record the concentration measurements.
    8.2.3   Background Concentration.

    Note: Not applicable when the building is used as the temporary 
total enclosure (TTE).

    8.2.3.1  Locate all natural draft openings (NDO's) of the TTE. A 
sampling point shall be at the center of each NDO, unless otherwise 
approved by the Administrator. If there are more than six NDO's, choose 
six sampling points evenly spaced among the NDO's.
    8.2.3.2  Assemble the sample train as shown in Figure 204C-2. 
Calibrate the FIA and conduct a system check according to the 
procedures in sections 7.1 and 7.4.
    8.2.3.3  Position the probe at the sampling location.
    8.2.3.4  Determine the response time, conduct the system check, and 
sample according to the procedures described in sections 8.2.2.4 
through 8.2.2.8.
    8.2.4  Alternative Procedure. The direct interface sampling and 
analysis procedure described in section 7.2 of Method 18 may be used to 
determine the gas VOC concentration. The system must be designed to 
collect and analyze at least one sample every 10 minutes. If the 
alternative procedure is used to determine the VOC concentration of the 
captured emissions, it must also be used to determine the VOC 
concentration of the uncaptured emissions.

9. Data Analysis and Calculations

    9.1  Nomenclature.

Ai=area of NDO i, ft2.
AN=total area of all NDO's in the enclosure, ft2.
CA = actual concentration of the dilution check gas, ppm 
propane.
CBi=corrected average VOC concentration of background 
emissions at point i, ppm propane.
CB=average background concentration, ppm propane.
CDH=average measured concentration for the drift check 
calibration gas, ppm propane.
CD0=average system drift check concentration for zero 
concentration gas, ppm propane.
CH=actual concentration of the drift check calibration gas, 
ppm propane.
Ci=uncorrected average background VOC concentration measured 
at point i, ppm propane.
Cj=uncorrected average VOC concentration measured at point 
j, ppm propane.
CM=measured concentration of the dilution check gas, ppm 
propane.
DF=dilution factor.
G=total VOC content of captured emissions, kg.
K1=1.830 x 10-6 kg/(m3-ppm).
n=number of measurement points.
QGj=average effluent volumetric flow rate corrected to 
standard conditions at captured emissions point j, m3/min.
C=total duration of CE sampling run, min.
    9.2  Calculations.
     9.2.1  Total VOC Captured Emissions.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.010
    
    9.2.2  VOC Concentration of the Captured Emissions at Point j.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.011
    
    9.2.3  Dilution Factor.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.012
    
    9.2.4  Background VOC Concentration at Point i.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.013
    
    9.2.5  Average Background Concentration.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.014
    
    Note: If the concentration at each point is within 20 percent of 
the average concentration of all points, then use the arithmetic 
average.

10. Method Performance

    The measurement uncertainties are estimated for each captured or 
uncaptured emissions point as follows: QGj=5.5 
percent and CGj= 5 percent. Based on these 
numbers, the probable uncertainty for G is estimated at about 
7.4 percent.

11. Diagrams

BILLING CODE 6560-SO-P

[[Page 32520]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.029



[[Page 32521]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.030



BILLIING CODE 6560-50-C

[[Page 32522]]

Method 204D--Volatile Organic Compounds Emissions in Uncaptured 
Stream From Temporary Total Enclosure

1. Scope and Application

    1.1  Applicability. This procedure is applicable for determining 
the uncaptured volatile organic compounds (VOC) emissions from a 
temporary total enclosure (TTE). It is intended to be used as a segment 
in the development of liquid/gas or gas/gas protocols for determining 
VOC capture efficiency (CE) for surface coating and printing 
operations.
    1.2  Principle. The amount of uncaptured VOC emissions (F) from the 
TTE is calculated as the sum of the products of the VOC content 
(CFj), the flow rate (QFj) from each uncaptured 
emissions point, and the sampling time (F).
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    A gas sample is extracted from the uncaptured exhaust duct of a TTE 
through a heated sample line and, if necessary, a glass fiber filter to 
a flame ionization analyzer (FIA).

3. Safety

    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.

4. Equipment and Supplies

    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Gas VOC Concentration. A schematic of the measurement system 
is shown in Figure 204D-1. The main components are as follows:
    4.1.1  Sample Probe. Stainless steel or equivalent. The probe shall 
be heated to prevent VOC condensation.
    4.1.2  Calibration Valve Assembly. Three-way valve assembly at the 
outlet of the sample probe to direct the zero and calibration gases to 
the analyzer. Other methods, such as quick-connect lines, to route 
calibration gases to the outlet of the sample probe are acceptable.
    4.1.3  Sample Line. Stainless steel or Teflon tubing to transport 
the sample gas to the analyzer. The sample line must be heated to 
prevent condensation.
    4.1.4  Sample Pump. A leak-free pump, to pull the sample gas 
through the system at a flow rate sufficient to minimize the response 
time of the measurement system. The components of the pump that contact 
the gas stream shall be constructed of stainless steel or Teflon. The 
sample pump must be heated to prevent condensation.
    4.1.5  Sample Flow Rate Control. A sample flow rate control valve 
and rotameter, or equivalent, to maintain a constant sampling rate 
within 10 percent. The flow control valve and rotameter must be heated 
to prevent condensation. A control valve may also be located on the 
sample pump bypass loop to assist in controlling the sample pressure 
and flow rate.
    4.1.6  Sample Gas Manifold. Capable of diverting a portion of the 
sample gas stream to the FIA, and the remainder to the bypass discharge 
vent. The manifold components shall be constructed of stainless steel 
or Teflon. If emissions are to be measured at multiple locations, the 
measurement system shall be designed to use separate sampling probes, 
lines, and pumps for each measurement location and a common sample gas 
manifold and FIA. The sample gas manifold and connecting lines to the 
FIA must be heated to prevent condensation.
    4.1.7  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated to the Administrator's 
satisfaction that they would provide more accurate measurements. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.1.7.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.1.7.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.1.7.3  Calibration Error. Less than 5.0 percent of 
the calibration gas value.
    4.1.7.4  Response Time. Less than 30 seconds.
    4.1.8  Integrator/Data Acquisition System. An analog or digital 
device or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated values is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2  Uncaptured Emissions Volumetric Flow Rate.
    4.2.1  Method 2 or 2A Apparatus. For determining volumetric flow 
rate.
    4.2.2  Method 3 Apparatus and Reagents. For determining molecular 
weight of the gas stream. An estimate of the molecular weight of the 
gas stream may be used if approved by the Administrator.
    4.2.3  Method 4 Apparatus and Reagents. For determining moisture 
content, if necessary.
    4.3  Temporary Total Enclosure. The criteria for designing an 
acceptable TTE are specified in Method 204.

5. Reagents and Standards

    5.1  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be certified 
by the manufacturer to 1 percent of the tag value. 
Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing calibration gas mixtures may be used with the 
approval of the Administrator.
    5.1.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He or 40 percent 
H2/60 percent N2 gas mixture is recommended to 
avoid an oxygen synergism effect that reportedly occurs when oxygen 
concentration varies significantly from a mean value. Other mixtures 
may be used provided the tester can demonstrate to the Administrator 
that there is no oxygen synergism effect.
    5.1.2  Carrier Gas. High purity air with less than 1 ppm of organic 
material (as propane or carbon equivalent) or less than 0.1 percent of 
the span value, whichever is greater.
    5.1.3  FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentrations of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
to the Administrator's satisfaction that equally accurate measurements 
would be achieved.
    5.2  Particulate Filter. An in-stack or an out-of-stack glass fiber 
filter is recommended if exhaust gas particulate

[[Page 32523]]

loading is significant. An out-of-stack filter must be heated to 
prevent any condensation unless it can be demonstrated that no 
condensation occurs.

6. Quality Control

    6.1  Required instrument quality control parameters are found in 
the following sections:
    6.1.1  The FIA system must be calibrated as specified in section 
7.1.
    6.1.2  The system drift check must be performed as specified in 
section 7.2.
    6.1.3  The system check must be conducted as specified in section 
7.3.
    6.2  Audits.
    6.2.1  Analysis Audit Procedure. Immediately before each test, 
analyze an audit cylinder as described in section 7.2. The analysis 
audit must agree with the audit cylinder concentration within 10 
percent.
    6.2.2  Audit Samples and Audit Sample Availability. Audit samples 
will be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B) Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Laboratory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    6.2.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

7. Calibration and Standardization

    7.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system and 
adjust the back-pressure regulator to the value required to achieve the 
flow rates specified by the manufacturer. Inject the zero-and the high-
range calibration gases and adjust the analyzer calibration to provide 
the proper responses. Inject the low-and mid-range gases and record the 
responses of the measurement system. The calibration and linearity of 
the system are acceptable if the responses for all four gases are 
within 5 percent of the respective gas values. If the performance of 
the system is not acceptable, repair or adjust the system and repeat 
the linearity check. Conduct a calibration and linearity check after 
assembling the analysis system and after a major change is made to the 
system.
    7.2  Systems Drift Checks. Select the calibration gas concentration 
that most closely approximates that of the uncaptured gas emissions 
concentration to conduct the drift checks. Introduce the zero and 
calibration gases at the calibration valve assembly and verify that the 
appropriate gas flow rate and pressure are present at the FIA. Record 
the measurement system responses to the zero and calibration gases. The 
performance of the system is acceptable if the difference between the 
drift check measurement and the value obtained in section 7.1 is less 
than 3 percent of the span value. Alternatively, recalibrate the FIA as 
in section 7.1 and report the results using both sets of calibration 
data (i.e., data determined prior to the test period and data 
determined following the test period). The data that results in the 
lowest CE value shall be reported as the results for the test run. 
Conduct a system drift check at the end of each run.
    7.3  System Check. Inject the high-range calibration gas at the 
inlet of the sampling probe and record the response. The performance of 
the system is acceptable if the measurement system response is within 5 
percent of the value obtained in section 7.1 for the high-range 
calibration gas. Conduct a system check before each test run.

8. Procedure

    8.1  Determination of Volumetric Flow Rate of Uncaptured Emissions
    8.1.1 Locate all points where uncaptured emissions are exhausted 
from the TTE. Using Method 1, determine the sampling points. Be sure to 
check each site for cyclonic or swirling flow.
    8.1.2  Measure the velocity at each sampling site at least once 
every hour during each sampling run using Method 2 or 2A.
    8.2  Determination of VOC Content of Uncaptured Emissions.
    8.2.1  Analysis Duration. Measure the VOC responses at each 
uncaptured emission point during the entire test run or, if applicable, 
while the process is operating. If there are multiple emission 
locations, design a sampling system to allow a single FIA to be used to 
determine the VOC responses at all sampling locations.
    8.2.2  Gas VOC Concentration.
    8.2.2.1  Assemble the sample train as shown in Figure 204D-1. 
Calibrate the FIA and conduct a system check according to the 
procedures in sections 7.1 and 7.3, respectively.
    8.2.2.2  Install the sample probe so that the probe is centrally 
located in the stack, pipe, or duct, and is sealed tightly at the stack 
port connection.
    8.2.2.3  Inject zero gas at the calibration valve assembly. Allow 
the measurement system response to reach zero. Measure the system 
response time as the time required for the system to reach the effluent 
concentration after the calibration valve has been returned to the 
effluent sampling position.
    8.2.2.4  Conduct a system check before, and a system drift check 
after, each sampling run according to the procedures in sections 7.2 
and 7.3. If the drift check following a run indicates unacceptable 
performance (see section 7.3), the run is not valid. Alternatively, 
recalibrate the FIA as in section 7.1 and report the results using both 
sets of calibration data (i.e., data determined prior to the test 
period and data determined following the test period). The data that 
results in the lowest CE value shall be reported as the results for the 
test run. The tester may elect to perform system drift checks during 
the run not to exceed one drift check per hour.
    8.2.2.5  Verify that the sample lines, filter, and pump 
temperatures are 1205  deg.C.
    8.2.2.6  Begin sampling at the start of the test period and 
continue to sample during the entire run. Record the starting and 
ending times and any required process information, as appropriate. If 
multiple emission locations are sampled using a single FIA, sample at 
each location for the same amount of time (e.g., 2 min.) and continue 
to switch from one location to another for the entire test run. Be sure 
that total sampling time at each location is the same at the end of the 
test run. Collect at least four separate measurements from each sample 
point during each hour of testing. Disregard the response measurements 
at each sampling location until 2 times the response time of the 
measurement system has elapsed. Continue sampling for at least 1 minute 
and record the concentration measurements.
    8.2.3  Background Concentration.

[[Page 32524]]

    8.2.3.1  Locate all natural draft openings (NDO's) of the TTE. A 
sampling point shall be at the center of each NDO, unless otherwise 
approved by the Administrator. If there are more than six NDO's, choose 
six sampling points evenly spaced among the NDO's.
    8.2.3.2  Assemble the sample train as shown in Figure 204D-2. 
Calibrate the FIA and conduct a system check according to the 
procedures in sections 7.1 and 7.3.
    8.2.3.3  Position the probe at the sampling location.
    8.2.3.4  Determine the response time, conduct the system check, and 
sample according to the procedures described in sections 8.2.2.3 
through 8.2.2.6.
    8.2.4  Alternative Procedure. The direct interface sampling and 
analysis procedure described in section 7.2 of Method 18 may be used to 
determine the gas VOC concentration. The system must be designed to 
collect and analyze at least one sample every 10 minutes. If the 
alternative procedure is used to determine the VOC concentration of the 
uncaptured emissions in a gas/gas protocol, it must also be used to 
determine the VOC concentration of the captured emissions. If a tester 
wishes to conduct a liquid/gas protocol using a gas chromatograph, the 
tester must use Method 204F for the liquid steam. A gas chromatograph 
is not an acceptable alternative to the FIA in Method 204A.

9. Data Analysis and Calculations

    9.1  Nomenclature.
Ai=area of NDO i, ft\2\.
AN=total area of all NDO's in the enclosure, ft\2\.
CBi=corrected average VOC concentration of background 
emissions at point i, ppm propane.
CB=average background concentration, ppm propane.
CDH=average measured concentration for the drift check 
calibration gas, ppm propane.
CD0=average system drift check concentration for zero 
concentration gas, ppm propane.
CFj=corrected average VOC concentration of uncaptured 
emissions at point j, ppm propane.
CH=actual concentration of the drift check calibration gas, 
ppm propane.
Ci=uncorrected average background VOC concentration at point 
i, ppm propane.
Cj=uncorrected average VOC concentration measured at point 
j, ppm propane.
F=total VOC content of uncaptured emissions, kg.
K1=1.830 x 10-6 kg/(m\3\-ppm).
n=number of measurement points.
QFj=average effluent volumetric flow rate corrected to 
standard conditions at uncaptured emissions point j, m\3\/min.
F=total duration of uncaptured emissions sampling 
run, min.
    9.2  Calculations.
    9.2.1  Total Uncaptured VOC Emissions.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.015
    
    9.2.2  VOC Concentration of the Uncaptured Emissions at Point j.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.016
    
    9.2.3  Background VOC Concentration at Point i.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.017
    
    9.2.4  Average Background Concentration.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.018
    
    Note: If the concentration at each point is within 20 percent of 
the average concentration of all points, use the arithmetic average.

10. Method Performance

    The measurement uncertainties are estimated for each uncaptured 
emission point as follows: QFj=5.5 percent and 
CFj=5.0 percent. Based on these numbers, the 
probable uncertainty for F is estimated at about 7.4 
percent.

11. Diagrams

BILLING CODE 6560-50-P

[[Page 32525]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.031



[[Page 32526]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.032



BILLING CODE 6560-50-C

[[Page 32527]]

Method 204E--Volatile Organic Compounds Emissions in Uncaptured Stream 
From Building Enclosure

1. Scope and Application

    1.1  Applicability. This procedure is applicable for determining 
the uncaptured volatile organic compounds (VOC) emissions from a 
building enclosure (BE). It is intended to be used in the development 
of liquid/gas or gas/gas protocols for determining VOC capture 
efficiency (CE) for surface coating and printing operations.
    1.2  Principle. The total amount of uncaptured VOC emissions 
(FB) from the BE is calculated as the sum of the products of 
the VOC content (CFj) of each uncaptured emissions point, 
the flow rate (QFj) at each uncaptured emissions point, and 
time (F).
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    A gas sample is extracted from the uncaptured exhaust duct of a BE 
through a heated sample line and, if necessary, a glass fiber filter to 
a flame ionization analyzer (FIA).

3. Safety

    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.

4. Equipment and Supplies

    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Gas VOC Concentration. A schematic of the measurement system 
is shown in Figure 204E-1. The main components are as follows:
    4.1.1  Sample Probe. Stainless steel or equivalent. The probe shall 
be heated to prevent VOC condensation.
    4.1.2  Calibration Valve Assembly. Three-way valve assembly at the 
outlet of the sample probe to direct the zero and calibration gases to 
the analyzer. Other methods, such as quick-connect lines, to route 
calibration gases to the outlet of the sample probe are acceptable.
    4.1.3  Sample Line. Stainless steel or Teflon tubing to transport 
the sample gas to the analyzer. The sample line must be heated to 
prevent condensation.
    4.1.4  Sample Pump. A leak-free pump, to pull the sample gas 
through the system at a flow rate sufficient to minimize the response 
time of the measurement system. The components of the pump that contact 
the gas stream shall be constructed of stainless steel or Teflon. The 
sample pump must be heated to prevent condensation.
    4.1.5  Sample Flow Rate Control. A sample flow rate control valve 
and rotameter, or equivalent, to maintain a constant sampling rate 
within 10 percent. The flow rate control valve and rotameter must be 
heated to prevent condensation. A control valve may also be located on 
the sample pump bypass loop to assist in controlling the sample 
pressure and flow rate.
    4.1.6  Sample Gas Manifold. Capable of diverting a portion of the 
sample gas stream to the FIA, and the remainder to the bypass discharge 
vent. The manifold components shall be constructed of stainless steel 
or Teflon. If emissions are to be measured at multiple locations, the 
measurement system shall be designed to use separate sampling probes, 
lines, and pumps for each measurement location, and a common sample gas 
manifold and FIA. The sample gas manifold must be heated to prevent 
condensation.
    4.1.7  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated to the Administrator's 
satisfaction that they would provide equally accurate measurements. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.1.7.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.1.7.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.1.7.3  Calibration Error. Less than 5.0 percent of 
the calibration gas value.
    4.1.7.4  Response Time. Less than 30 seconds.
    4.1.8  Integrator/Data Acquisition System. An analog or digital 
device or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated values is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2  Uncaptured Emissions Volumetric Flow Rate.
    4.2.1  Flow Direction Indicators. Any means of indicating inward or 
outward flow, such as light plastic film or paper streamers, smoke 
tubes, filaments, and sensory perception.
    4.2.2  Method 2 or 2A Apparatus. For determining volumetric flow 
rate. Anemometers or similar devices calibrated according to the 
manufacturer's instructions may be used when low velocities are 
present. Vane anemometers (Young-maximum response propeller), 
specialized pitots with electronic manometers (e.g., Shortridge 
Instruments Inc., Airdata Multimeter 860) are commercially available 
with measurement thresholds of 15 and 8 mpm (50 and 25 fpm), 
respectively.
    4.2.3   Method 3 Apparatus and Reagents. For determining molecular 
weight of the gas stream. An estimate of the molecular weight of the 
gas stream may be used if approved by the Administrator.
    4.2.4  Method 4 Apparatus and Reagents. For determining moisture 
content, if necessary.
    4.3  Building Enclosure. The criteria for an acceptable BE are 
specified in Method 204.

5. Reagents and Standards

    5.1  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be certified 
by the manufacturer to 1 percent of the tag value. 
Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing calibration gas mixtures may be used with the 
approval of the Administrator.
    5.1.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He or 40 percent 
H2/60 percent N2 gas mixture is recommended to 
avoid an oxygen synergism effect that reportedly occurs when oxygen 
concentration varies significantly from a mean value. Other mixtures 
may be used provided the tester can demonstrate to the Administrator 
that there is no oxygen synergism effect.
    5.1.2  Carrier Gas. High purity air with less than 1 ppm of organic 
material (propane or carbon equivalent) or less than 0.1 percent of the 
span value, whichever is greater.

[[Page 32528]]

    5.1.3  FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentrations of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
to the Administrator's satisfaction that equally accurate measurements 
would be achieved.
    5.2  Particulate Filter. An in-stack or an out-of-stack glass fiber 
filter is recommended if exhaust gas particulate loading is 
significant. An out-of-stack filter must be heated to prevent any 
condensation unless it can be demonstrated that no condensation occurs.

6. Quality Control

    6.1  Required instrument quality control parameters are found in 
the following sections:
    6.1.1  The FIA system must be calibrated as specified in section 
7.1.
    6.1.2  The system drift check must be performed as specified in 
section 7.2.
    6.1.3  The system check must be conducted as specified in section 
7.3.
    6.2  Audits.
    6.2.1  Analysis Audit Procedure. Immediately before each test, 
analyze an audit cylinder as described in section 7.2. The analysis 
audit must agree with the audit cylinder concentration within 10 
percent.
    6.2.2  Audit Samples and Audit Sample Availability. Audit samples 
will be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B), Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Laboratory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    6.2.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

7. Calibration and Standardization

    7.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system and 
adjust the back-pressure regulator to the value required to achieve the 
flow rates specified by the manufacturer. Inject the zero-and the high-
range calibration gases, and adjust the analyzer calibration to provide 
the proper responses. Inject the low-and mid-range gases and record the 
responses of the measurement system. The calibration and linearity of 
the system are acceptable if the responses for all four gases are 
within 5 percent of the respective gas values. If the performance of 
the system is not acceptable, repair or adjust the system and repeat 
the linearity check. Conduct a calibration and linearity check after 
assembling the analysis system and after a major change is made to the 
system.
    7.2  Systems Drift Checks. Select the calibration gas that most 
closely approximates the concentration of the captured emissions for 
conducting the drift checks. Introduce the zero and calibration gases 
at the calibration valve assembly and verify that the appropriate gas 
flow rate and pressure are present at the FIA. Record the measurement 
system responses to the zero and calibration gases. The performance of 
the system is acceptable if the difference between the drift check 
measurement and the value obtained in section 7.1 is less than 3 
percent of the span value. Alternatively, recalibrate the FIA as in 
section 7.1 and report the results using both sets of calibration data 
(i.e., data determined prior to the test period and data determined 
following the test period). The data that results in the lowest CE 
value shall be reported as the results for the test run. Conduct a 
system drift check at the end of each run.
    7.3  System Check. Inject the high-range calibration gas at the 
inlet of the sampling probe and record the response. The performance of 
the system is acceptable if the measurement system response is within 5 
percent of the value obtained in section 7.1 for the high-range 
calibration gas. Conduct a system check before each test run.

8. Procedure

    8.1  Preliminary Determinations. The following points are 
considered exhaust points and should be measured for volumetric flow 
rates and VOC concentrations:
    8.1.1  Forced Draft Openings. Any opening in the facility with an 
exhaust fan. Determine the volumetric flow rate according to Method 2.
    8.1.2  Roof Openings. Any openings in the roof of a facility which 
does not contain fans are considered to be exhaust points. Determine 
volumetric flow rate from these openings. Use the appropriate velocity 
measurement devices (e.g., propeller anemometers).
    8.2  Determination of Flow Rates.
    8.2.1  Measure the volumetric flow rate at all locations identified 
as exhaust points in section 8.1. Divide each exhaust opening into nine 
equal areas for rectangular openings and into eight equal areas for 
circular openings.
    8.2.2  Measure the velocity at each site at least once every hour 
during each sampling run using Method 2 or 2A, if applicable, or using 
the low velocity instruments in section 4.2.2.
    8.3   Determination of VOC Content of Uncaptured Emissions.
    8.3.1  Analysis Duration. Measure the VOC responses at each 
uncaptured emissions point during the entire test run or, if 
applicable, while the process is operating. If there are multiple 
emissions locations, design a sampling system to allow a single FIA to 
be used to determine the VOC responses at all sampling locations.
    8.3.2  Gas VOC Concentration.
    8.3.2.1  Assemble the sample train as shown in Figure 204E-1. 
Calibrate the FIA and conduct a system check according to the 
procedures in sections 7.1 and 7.3, respectively.
    8.3.2.2  Install the sample probe so that the probe is centrally 
located in the stack, pipe, or duct, and is sealed tightly at the stack 
port connection.
    8.3.2.3  Inject zero gas at the calibration valve assembly. Allow 
the measurement system response to reach zero. Measure the system 
response time as the time required for the system to reach the effluent 
concentration after the calibration valve has been returned to the 
effluent sampling position.
    8.3.2.4  Conduct a system check before, and a system drift check 
after, each sampling run according to the procedures in sections 7.2 
and 7.3. If the drift check following a run indicates unacceptable 
performance (see section 7.3), the run is not valid. Alternatively, 
recalibrate the FIA as in section 7.1 and report the results using both 
sets of calibration data (i.e., data determined prior to the test 
period and data determined following the test period). The data that 
results in the lowest CE value shall be reported as the results for

[[Page 32529]]

the test run. The tester may elect to perform drift checks during the 
run, not to exceed one drift check per hour.
    8.3.2.5  Verify that the sample lines, filter, and pump 
temperatures are 120 5  deg.C.
    8.3.2.6  Begin sampling at the start of the test period and 
continue to sample during the entire run. Record the starting and 
ending times, and any required process information, as appropriate. If 
multiple emission locations are sampled using a single FIA, sample at 
each location for the same amount of time (e.g., 2 minutes) and 
continue to switch from one location to another for the entire test 
run. Be sure that total sampling time at each location is the same at 
the end of the test run. Collect at least four separate measurements 
from each sample point during each hour of testing. Disregard the 
response measurements at each sampling location until 2 times the 
response time of the measurement system has elapsed. Continue sampling 
for at least 1 minute, and record the concentration measurements.
    8.4  Alternative Procedure. The direct interface sampling and 
analysis procedure described in section 7.2 of Method 18 may be used to 
determine the gas VOC concentration. The system must be designed to 
collect and analyze at least one sample every 10 minutes. If the 
alternative procedure is used to determine the VOC concentration of the 
uncaptured emissions in a gas/gas protocol, it must also be used to 
determine the VOC concentration of the captured emissions. If a tester 
wishes to conduct a liquid/gas protocol using a gas chromatograph, the 
tester must use Method 204F for the liquid steam. A gas chromatograph 
is not an acceptable alternative to the FIA in Method 204A.

9. Data Analysis and Calculations

    9.1  Nomenclature.
CDH=average measured concentration for the drift check 
calibration gas, ppm propane.
CD0=average system drift check concentration for zero 
concentration gas, ppm propane.
CFj=corrected average VOC concentration of uncaptured 
emissions at point j, ppm propane.
CH=actual concentration of the drift check calibration gas, 
ppm propane.
Cj=uncorrected average VOC concentration measured at point 
j, ppm propane.
FB=total VOC content of uncaptured emissions from the 
building, kg.
K1=1.830  x  10-6 kg/(m \3\-ppm).
n=number of measurement points.
QFj=average effluent volumetric flow rate corrected to 
standard conditions at uncaptured emissions point j, m \3\/min.
F=total duration of CE sampling run, min.

    9.2  Calculations
    9.2.1  Total VOC Uncaptured Emissions from the Building.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.019
    
    9.2.2  VOC Concentration of the Uncaptured Emissions at Point j.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.020
    
10. Method Performance

    The measurement uncertainties are estimated for each uncaptured 
emissions point as follows: QFj=10.0 percent and 
CFj= 5.0 percent. Based on these numbers, the 
probable uncertainty for FB is estimated at about 
11.2 percent.

11. Diagrams

BILLING CODE 6560-50-P

[[Page 32530]]

[GRAPHIC] [TIFF OMITTED] TR16JN97.033



BILLING CODE 6560-50-C

[[Page 32531]]

Method 204F--Volatile Organic Compounds Content in Liquid Input Stream 
(Distillation Approach)

1. Introduction

    1.1  Applicability. This procedure is applicable for determining 
the input of volatile organic compounds (VOC). It is intended to be 
used as a segment in the development of liquid/gas protocols for 
determining VOC capture efficiency (CE) for surface coating and 
printing operations.
    1.2  Principle. The amount of VOC introduced to the process (L) is 
the sum of the products of the weight (W) of each VOC containing liquid 
(ink, paint, solvent, etc.) used, and its VOC content (V), corrected 
for a response factor (RF).
    1.3  Sampling Requirements. A CE test shall consist of at least 
three sampling runs. Each run shall cover at least one complete 
production cycle, but shall be at least 3 hours long. The sampling time 
for each run need not exceed 8 hours, even if the production cycle has 
not been completed. Alternative sampling times may be used with the 
approval of the Administrator.

2. Summary of Method

    A sample of each coating used is distilled to separate the VOC 
fraction. The distillate is used to prepare a known standard for 
analysis by an flame ionization analyzer (FIA), calibrated against 
propane, to determine its RF.
    3. Safety
    Because this procedure is often applied in highly explosive areas, 
caution and care should be exercised in choosing, installing, and using 
the appropriate equipment.
    4. Equipment and Supplies
    Mention of trade names or company products does not constitute 
endorsement. All gas concentrations (percent, ppm) are by volume, 
unless otherwise noted.
    4.1  Liquid Weight.
    4.1.1  Balances/Digital Scales. To weigh drums of VOC containing 
liquids to within 0.2 lb or 1.0 percent of the total weight of VOC 
liquid used.
    4.1.2 Volume Measurement Apparatus (Alternative). Volume meters, 
flow meters, density measurement equipment, etc., as needed to achieve 
the same accuracy as direct weight measurements.
    4.2 Response Factor Determination (FIA Technique). The VOC 
distillation system and Tedlar gas bag generation system apparatuses 
are shown in Figures 204F-1 and 204F-2, respectively. The following 
equipment is required:
    4.2.1  Sample Collection Can. An appropriately-sized metal can to 
be used to collect VOC containing materials. The can must be 
constructed in such a way that it can be grounded to the coating 
container.
    4.2.2  Needle Valves. To control gas flow.
    4.2.3  Regulators. For calibration, dilution, and sweep gas 
cylinders.
    4.2.4  Tubing and Fittings. Teflon and stainless steel tubing and 
fittings with diameters, lengths, and sizes determined by the 
connection requirements of the equipment.
    4.2.5  Thermometer. Capable of measuring the temperature of the hot 
water and oil baths to within 1  deg.C.
    4.2.6  Analytical Balance. To measure 0.01 mg.
    4.2.7  Microliter Syringe. 10-l size.
    4.2.8  Vacuum Gauge or Manometer. 0- to 760-mm (0- to 30-in.) Hg U-
Tube manometer or vacuum gauge.
    4.2.9  Hot Oil Bath, With Stirring Hot Plate. Capable of heating 
and maintaining a distillation vessel at 110  3  deg.C.
    4.2.10  Ice Water Bath. To cool the distillation flask.
    4.2.11  Vacuum/Water Aspirator. A device capable of drawing a 
vacuum to within 20 mm Hg from absolute.
    4.2.12  Rotary Evaporator System. Complete with folded inner coil, 
vertical style condenser, rotary speed control, and Teflon sweep gas 
delivery tube with valved inlet. Buchi Rotavapor or equivalent.
    4.2.13  Ethylene Glycol Cooling/Circulating Bath. Capable of 
maintaining the condenser coil fluid at -10  deg.C.
    4.2.14  Dry Gas Meter (DGM). Capable of measuring the dilution gas 
volume within 2 percent, calibrated with a spirometer or bubble meter, 
and equipped with a temperature gauge capable of measuring temperature 
within 3  deg.C.
    4.2.15  Activated Charcoal/Mole Sieve Trap. To remove any trace 
level of organics picked up from the DGM.
    4.2.16  Gas Coil Heater. Sufficient length of 0.125-inch stainless 
steel tubing to allow heating of the dilution gas to near the water 
bath temperature before entering the volatilization vessel.
    4.2.17  Water Bath, With Stirring Hot Plate. Capable of heating and 
maintaining a volatilization vessel and coil heater at a temperature of 
100  5  deg.C.
    4.2.18  Volatilization Vessel. 50-ml midget impinger fitted with a 
septum top and loosely filled with glass wool to increase the 
volatilization surface.
    4.2.19  Tedlar Gas Bag. Capable of holding 30 liters of gas, 
flushed clean with zero air, leak tested, and evacuated.
    4.2.20  Organic Concentration Analyzer. An FIA with a span value of 
1.5 times the expected concentration as propane; however, other span 
values may be used if it can be demonstrated that they would provide 
equally accurate measurements. The FIA instrument should be the same 
instrument used in the gaseous analyses adjusted with the same fuel, 
combustion air, and sample back-pressure (flow rate) settings. The 
system shall be capable of meeting or exceeding the following 
specifications:
    4.2.20.1  Zero Drift. Less than 3.0 percent of the span 
value.
    4.2.20.2  Calibration Drift. Less than 3.0 percent of 
the span value.
    4.2.20.3  Calibration Error. Less than 3.0 percent of 
the calibration gas value.
    4.2.21  Integrator/Data Acquisition System. An analog or digital 
device or computerized data acquisition system used to integrate the 
FIA response or compute the average response and record measurement 
data. The minimum data sampling frequency for computing average or 
integrated value is one measurement value every 5 seconds. The device 
shall be capable of recording average values at least once per minute.
    4.2.22  Chart Recorder (Optional). A chart recorder or similar 
device is recommended to provide a continuous analog display of the 
measurement results during the liquid sample analysis.

5. Reagents and Standards

    5.1  Zero Air. High purity air with less than 1 ppm of organic 
material (as propane) or less than 0.1 percent of the span value, 
whichever is greater. Used to supply dilution air for making the Tedlar 
bag gas samples.
    5.2  THC Free N2. High purity N2 with less 
than 1 ppm THC. Used as sweep gas in the rotary evaporator system.
    5.3  Calibration and Other Gases. Gases used for calibration, fuel, 
and combustion air (if required) are contained in compressed gas 
cylinders. All calibration gases shall be traceable to National 
Institute of Standards and Technology standards and shall be certified 
by the manufacturer to 1 percent of the tag value. 
Additionally, the manufacturer of the cylinder should provide a 
recommended shelf life for each calibration gas cylinder over which the 
concentration does not change more than 2 percent from the 
certified value. For calibration gas values not generally available, 
dilution systems calibrated using Method 205 may be used. Alternative 
methods for preparing

[[Page 32532]]

calibration gas mixtures may be used with the approval of the 
Administrator.
    5.3.1  Fuel. The FIA manufacturer's recommended fuel should be 
used. A 40 percent H2/60 percent He, or 40 percent 
H2/60 percent N2 mixture is recommended to avoid 
fuels with oxygen to avoid an oxygen synergism effect that reportedly 
occurs when oxygen concentration varies significantly from a mean 
value. Other mixtures may be used provided the tester can demonstrate 
to the Administrator that there is no oxygen synergism effect.
    5.3.2  Combustion Air. High purity air with less than 1 ppm of 
organic material (as propane) or less than 0.1 percent of the span 
value, whichever is greater.
    5.3.3  FIA Linearity Calibration Gases. Low-, mid-, and high-range 
gas mixture standards with nominal propane concentration of 20-30, 45-
55, and 70-80 percent of the span value in air, respectively. Other 
calibration values and other span values may be used if it can be shown 
that equally accurate measurements would be achieved.
    5.3.4  System Calibration Gas. Gas mixture standard containing 
propane in air, approximating the VOC concentration expected for the 
Tedlar gas bag samples.

6. Quality Control

    6.1  Required instrument quality control parameters are found in 
the following sections:
    6.1.1  The FIA system must be calibrated as specified in section 
7.1.
    6.1.2  The system drift check must be performed as specified in 
section 7.2.
    6.2  Precision Control. A minimum of one sample in each batch must 
be distilled and analyzed in duplicate as a precision control. If the 
results of the two analyses differ by more than 10 percent 
of the mean, then the system must be reevaluated and the entire batch 
must be redistilled and analyzed.
    6.3  Audits.
    6.3.1  Audit Procedure. Concurrently, analyze the audit sample and 
a set of compliance samples in the same manner to evaluate the 
technique of the analyst and the standards preparation. The same 
analyst, analytical reagents, and analytical system shall be used both 
for compliance samples and the EPA audit sample. If this condition is 
met, auditing of subsequent compliance analyses for the same 
enforcement agency within 30 days is not required. An audit sample set 
may not be used to validate different sets of compliance samples under 
the jurisdiction of different enforcement agencies, unless prior 
arrangements are made with both enforcement agencies.
    6.3.2  Audit Samples. Audit Sample Availability. Audit samples will 
be supplied only to enforcement agencies for compliance tests. The 
availability of audit samples may be obtained by writing: Source Test 
Audit Coordinator (STAC) (MD-77B), Quality Assurance Division, 
Atmospheric Research and Exposure Assessment Laboratory, U.S. 
Environmental Protection Agency, Research Triangle Park, NC 27711 or by 
calling the STAC at (919) 541-7834. The request for the audit sample 
must be made at least 30 days prior to the scheduled compliance sample 
analysis.
    6.3.3  Audit Results. Calculate the audit sample concentration 
according to the calculation procedure described in the audit 
instructions included with the audit sample. Fill in the audit sample 
concentration and the analyst's name on the audit response form 
included with the audit instructions. Send one copy to the EPA Regional 
Office or the appropriate enforcement agency, and a second copy to the 
STAC. The EPA Regional Office or the appropriate enforcement agency 
will report the results of the audit to the laboratory being audited. 
Include this response with the results of the compliance samples in 
relevant reports to the EPA Regional Office or the appropriate 
enforcement agency.

7. Calibration and Standardization

    7.1  FIA Calibration and Linearity Check. Make necessary 
adjustments to the air and fuel supplies for the FIA and ignite the 
burner. Allow the FIA to warm up for the period recommended by the 
manufacturer. Inject a calibration gas into the measurement system and 
adjust the back-pressure regulator to the value required to achieve the 
flow rates specified by the manufacturer. Inject the zero-and the high-
range calibration gases and adjust the analyzer calibration to provide 
the proper responses. Inject the low-and mid-range gases and record the 
responses of the measurement system. The calibration and linearity of 
the system are acceptable if the responses for all four gases are 
within 5 percent of the respective gas values. If the performance of 
the system is not acceptable, repair or adjust the system and repeat 
the linearity check. Conduct a calibration and linearity check after 
assembling the analysis system and after a major change is made to the 
system. A calibration curve consisting of zero gas and two calibration 
levels must be performed at the beginning and end of each batch of 
samples.
    7.2  Systems Drift Checks. After each sample, repeat the system 
calibration checks in section 7.1 before any adjustments to the FIA or 
measurement system are made. If the zero or calibration drift exceeds 
3 percent of the span value, discard the result and repeat 
the analysis. Alternatively, recalibrate the FIA as in section 7.1 and 
report the results using both sets of calibration data (i.e., data 
determined prior to the test period and data determined following the 
test period). The data that results in the lowest CE value shall be 
reported as the results for the test run.

8. Procedures

    8.1  Determination of Liquid Input Weight
    8.1.1  Weight Difference. Determine the amount of material 
introduced to the process as the weight difference of the feed material 
before and after each sampling run. In determining the total VOC 
containing liquid usage, account for: (a) The initial (beginning) VOC 
containing liquid mixture; (b) any solvent added during the test run; 
(c) any coating added during the test run; and (d) any residual VOC 
containing liquid mixture remaining at the end of the sample run.
    8.1.1.1  Identify all points where VOC containing liquids are 
introduced to the process. To obtain an accurate measurement of VOC 
containing liquids, start with an empty fountain (if applicable). After 
completing the run, drain the liquid in the fountain back into the 
liquid drum (if possible), and weigh the drum again. Weigh the VOC 
containing liquids to 0.5 percent of the total weight 
(full) or 1.0 percent of the total weight of VOC containing 
liquid used during the sample run, whichever is less. If the residual 
liquid cannot be returned to the drum, drain the fountain into a 
preweighed empty drum to determine the final weight of the liquid.
    8.1.1.2  If it is not possible to measure a single representative 
mixture, then weigh the various components separately (e.g., if solvent 
is added during the sampling run, weigh the solvent before it is added 
to the mixture). If a fresh drum of VOC containing liquid is needed 
during the run, then weigh both the empty drum and fresh drum.
    8.1.2  Volume Measurement (Alternative). If direct weight 
measurements are not feasible, the tester may use volume meters and 
flow rate meters (and density measurements) to determine the weight of 
liquids used if it can be demonstrated that the technique produces 
results equivalent to the direct weight measurements. If a single 
representative mixture cannot be

[[Page 32533]]

measured, measure the components separately.
    8.2  Determination of VOC Content in Input Liquids
    8.2.1  Collection of Liquid Samples.
    8.2.1.1  Collect a 1-pint or larger sample of the VOC containing 
liquid mixture at each application location at the beginning and end of 
each test run. A separate sample should be taken of each VOC containing 
liquid added to the application mixture during the test run. If a fresh 
drum is needed during the sampling run, then obtain a sample from the 
fresh drum.
    8.2.1.2  When collecting the sample, ground the sample container to 
the coating drum. Fill the sample container as close to the rim as 
possible to minimize the amount of headspace.
    8.2.1.3  After the sample is collected, seal the container so the 
sample cannot leak out or evaporate.
    8.2.1.4  Label the container to identify clearly the contents.
    8.2.2  Distillation of VOC.
    8.2.2.1  Assemble the rotary evaporator as shown in Figure 204F-1.
    8.2.2.2  Leak check the rotary evaporation system by aspirating a 
vacuum of approximately 20 mm Hg from absolute. Close up the system and 
monitor the vacuum for approximately 1 minute. If the vacuum falls more 
than 25 mm Hg in 1 minute, repair leaks and repeat. Turn off the 
aspirator and vent vacuum.
    8.2.2.3  Deposit approximately 20 ml of sample (inks, paints, etc.) 
into the rotary evaporation distillation flask.
    8.2.2.4  Install the distillation flask on the rotary evaporator.
    8.2.2.5  Immerse the distillate collection flask into the ice water 
bath.
    8.2.2.6  Start rotating the distillation flask at a speed of 
approximately 30 rpm.
    8.2.2.7  Begin heating the vessel at a rate of 2 to 3 deg.C per 
minute.
    8.2.2.8  After the hot oil bath has reached a temperature of 
50 deg.C or pressure is evident on the mercury manometer, turn on the 
aspirator and gradually apply a vacuum to the evaporator to within 20 
mm Hg of absolute. Care should be taken to prevent material burping 
from the distillation flask.
    8.2.2.9  Continue heating until a temperature of 110 deg.C is 
achieved and maintain this temperature for at least 2 minutes, or until 
the sample has dried in the distillation flask.
    8.2.2.10  Slowly introduce the N2 sweep gas through the 
purge tube and into the distillation flask, taking care to maintain a 
vacuum of approximately 400-mm Hg from absolute.
    8.2.2.11  Continue sweeping the remaining solvent VOC from the 
distillation flask and condenser assembly for 2 minutes, or until all 
traces of condensed solvent are gone from the vessel. Some distillate 
may remain in the still head. This will not affect solvent recovery 
ratios.
    8.2.2.12  Release the vacuum, disassemble the apparatus and 
transfer the distillate to a labeled, sealed vial.
    8.2.3  Preparation of VOC standard bag sample.
    8.2.3.1  Assemble the bag sample generation system as shown in 
Figure 204F-2 and bring the water bath up to near boiling temperature.
    8.2.3.2  Inflate the Tedlar bag and perform a leak check on the 
bag.
    8.2.3.3  Evacuate the bag and close the bag inlet valve.
    8.2.3.4  Record the current barometric pressure.
    8.2.3.5  Record the starting reading on the dry gas meter, open the 
bag inlet valve, and start the dilution zero air flowing into the 
Tedlar bag at approximately 2 liters per minute.
    8.2.3.6  The bag sample VOC concentration should be similar to the 
gaseous VOC concentration measured in the gas streams. The amount of 
liquid VOC required can be approximated using equations in section 9.2. 
Using Equation 204F-4, calculate CVOC by assuming RF is 1.0 
and selecting the desired gas concentration in terms of propane, 
CC3. Assuming BV is 20 liters, ML, the 
approximate amount of liquid to be used to prepare the bag gas sample, 
can be calculated using Equation 204F-2.
    8.2.3.7  Quickly withdraw an aliquot of the approximate amount 
calculated in section 8.2.3.6 from the distillate vial with the 
microliter syringe and record its weight from the analytical balance to 
the nearest 0.01 mg.
    8.2.3.8  Inject the contents of the syringe through the septum of 
the volatilization vessel into the glass wool inside the vessel.
    8.2.3.9  Reweigh and record the tare weight of the now empty 
syringe.
    8.2.3.10  Record the pressure and temperature of the dilution gas 
as it is passed through the dry gas meter.
    8.2.3.11  After approximately 20 liters of dilution gas have passed 
into the Tedlar bag, close the valve to the dilution air source and 
record the exact final reading on the dry gas meter.
    8.2.3.12  The gas bag is then analyzed by FIA within 1 hour of bag 
preparation in accordance with the procedure in section 8.2.4.
    8.2.4  Determination of VOC response factor.
    8.2.4.1  Start up the FIA instrument using the same settings as 
used for the gaseous VOC measurements.
    8.2.4.2  Perform the FIA analyzer calibration and linearity checks 
according to the procedure in section 7.1. Record the responses to each 
of the calibration gases and the back-pressure setting of the FIA.
    8.2.4.3  Connect the Tedlar bag sample to the FIA sample inlet and 
record the bag concentration in terms of propane. Continue the analyses 
until a steady reading is obtained for at least 30 seconds. Record the 
final reading and calculate the RF.
    8.2.5  Determination of coating VOC content as VOC 
(VIJ).
    8.2.5.1  Determine the VOC content of the coatings used in the 
process using EPA Method 24 or 24A as applicable.

9.  Data Analysis and Calculations

    9.1.  Nomenclature.
BV=Volume of bag sample volume, liters.
CC3=Concentration of bag sample as propane, mg/liter.
CVOC=Concentration of bag sample as VOC, mg/liter.
K=0.00183 mg propane/(liter-ppm propane)
L=Total VOC content of liquid input, kg propane.
ML=Mass of VOC liquid injected into the bag, mg.
MV=Volume of gas measured by DGM, liters.
PM=Absolute DGM gas pressure, mm Hg.
PSTD=Standard absolute pressure, 760 mm Hg.
RC3=FIA reading for bag gas sample, ppm propane.
RF=Response factor for VOC in liquid, weight VOC/weight propane.
RFJ=Response factor for VOC in liquid J, weight VOC/weight 
propane.
TM=DGM temperature,  deg.K.
TSTD=Standard absolute temperature, 293 deg.K.
VIJ=Initial VOC weight fraction of VOC liquid J.
VFJ=Final VOC weight fraction of VOC liquid J.
VAJ=VOC weight fraction of VOC liquid J added during the 
run.
WIJ=Weight of VOC containing liquid J at beginning of run, 
kg.
WFJ=Weight of VOC containing liquid J at end of run, kg.
WAJ=Weight of VOC containing liquid J added during the run, 
kg.
    9.2  Calculations.
     9.2.1  Bag sample volume.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.021
    
    9.2.2  Bag sample VOC concentration.

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[GRAPHIC] [TIFF OMITTED] TR16JN97.022


    9.2.3  Bag sample VOC concentration as propane.
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    9.2.4  Response Factor.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.024
    
    9.2.5  Total VOC Content of the Input VOC Containing Liquid.
    [GRAPHIC] [TIFF OMITTED] TR16JN97.025
    
10. Diagrams

BILLING CODE 6560-50-P

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[GRAPHIC] [TIFF OMITTED] TR16JN97.034



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[FR Doc. 97-15374 Filed 6-13-97; 8:45 am]
BILLING CODE 6560-50-C