97-15374. Preparation, Adoption, and Submittal of State Implementation Plans; Appendix M, Test Methods 204, 204A-204F  

  • [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]
    
    
    =======================================================================
    -----------------------------------------------------------------------
    
    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.
    
    -----------------------------------------------------------------------
    
    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.
    
    [[Page 32534]]
    
    [GRAPHIC] [TIFF OMITTED] TR16JN97.022
    
    
        9.2.3  Bag sample VOC concentration as propane.
        [GRAPHIC] [TIFF OMITTED] TR16JN97.023
        
        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
    
    [[Page 32535]]
    
    [GRAPHIC] [TIFF OMITTED] TR16JN97.034
    
    
    
    [[Page 32536]]
    
    [GRAPHIC] [TIFF OMITTED] TR16JN97.035
    
    
    
    [FR Doc. 97-15374 Filed 6-13-97; 8:45 am]
    BILLING CODE 6560-50-C
    
    
    

Document Information

Effective Date:
6/16/1997
Published:
06/16/1997
Department:
Environmental Protection Agency
Entry Type:
Rule
Action:
Final rule.
Document Number:
97-15374
Dates:
These methods are effective June 16, 1997.
Pages:
32500-32536 (37 pages)
Docket Numbers:
FRL-5836-1
RINs:
2060-AF02: Addition of Methods 204, 204A - 204F for Measurement of VOC Emissions From Stationary Sources
RIN Links:
https://www.federalregister.gov/regulations/2060-AF02/addition-of-methods-204-204a-204f-for-measurement-of-voc-emissions-from-stationary-sources
PDF File:
97-15374.pdf
Supporting Documents:
» Legacy Index for Docket A-91-70
» Preparation, Adoption, and Submittal of State Implementation Plans; Appendix M, Test Methods 204, 204A - 204F
» Preparation, Adoption, and Submittal of State Implementation Plans; Appendix M, Test Methods 204, 204A - 204F
CFR: (1)
40 CFR 51