Appendix H to Part 75 - Revised Traceability Protocol No. 1  


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  • This appendix consists of section 3.0.4 of the Quality Assurance Handbook for Air Pollution Measurement Systems, Vol. 3, U.S. Environmental Protection Agency (revised 6/9/87). The Quality Assurance Handbook may be obtained from the Methods Research and Development Division, MD 78-A, Atmospheric Research Exposure and Assessment Laboratory, U.S. Environmental Protection Agency, Research Triangle Park, North Carolina 27711.

    3.0.4.Procedure for NBS-Traceable Certification of Compressed Gas Working Standards Used for Calibration and Audit of Continuous Source Emission Monitors (Revised Traceability Protocol No. 1) Contents SubsectionTitle3.0.4.0General Information3.0.4.1Procedure G1: Assay and Certification of a Compressed Gas Standard Without Dilution3.0.4.2References 4.0General Information 4.0.1Purpose and Scope of the Procedure

    Section 3.0.4 describes a procedure for assaying the concentration of gaseous pollutant concentration standards and certifying that the assay concentrations are traceable to an authoritative reference concentration standard. This procedure is recommended for certifying the local working concentration standards required by the pollutant monitoring regulations of 40 CFR part 601,2 for the calibration and audit of continuous source emission monitors. The procedure covers certification of compressed gas (cylinder) standards for CO, CO2, NO, NO2, and SO2 (Procedure G1).

    4.0.2Reference Standards

    Part 60 of the monitoring regulations 1,2 requires that working standards used for calibration and audit of continuous source emission monitors be traceable to either a National Bureau of Standards (NBS) gaseous Standard Reference Material (SRM or a NBS/EPA-approved Certified reference material (CRM) 3. Accordingly, the reference standard used for assaying and certifying a working standard for these purposes must be an SRM, a CRM, or a suitable intermediate standard (see the next paragraph). SRM cylinder gas standards available from NBS are listed in table 7.2 at the end of subsection 4.0. A current list of CRM cylinder gases and CRM vendors is available from the Quality Assurance Division (MD-77), Environmental Monitoring Systems Laboratory, U.S. EPA, Research Triangle Park, NC 27711.

    The EPA regulations define a “traceable” standard as one which“. . . has been compared and certified, either directly or via not more than one intermediate standard, to a primary standard such as a . . . NBS [gaseous] SRM or . . . CRM”4,5. Certification of a working standard directly to an SRM or CRM primary standard is, of course, preferred and recommended because of the lower error. However, an intermediate reference standard is permitted, if necessary. In particular, a Gas Manufacturer's Intermediate Standard (see subsection 4.0.2.1) that has been referenced directly to an SRM or a CRM according to Procedure G1 is an acceptable intermediate standard and could be used as the reference standard on that basis. However, purchasers of commercial gas standards referenced to an intermediate standard such as a GMIS should be aware that, according to the above definition, such a standard would have to be used directly for calibration or audit. Since a second intermediate standard is not permitted, such a standard could not be used as a reference standard to certify other standards.

    4.0.2.1Gas Manufacturer's Intermediate Standard (GMIS). A GMIS is a compressed (cylinder) gas standard that has been assayed with direct reference to an SRM or CRM and certified according to Procedure G1, and also meets the following requirements:

    1. A candidate GMIS must be assayed a minimum of three (3) times, uniformly spaced over a three (3) month period.

    2. Each of the three (or more) assays must be within 1.0 percent of the mean of the three (or more) assays.

    3. The difference between the last assay and the first assay must not exceed 1.5 percent of the mean of the three (or more) assays.

    4. The GMIS must be recertified every three months, and the reassay must be within 1.5 percent of the previous certified assay. The recertified concentration of the GMIS is the mean of the previous certified concentration and the reassay concentration.

    4.0.2.2Recertification of Reference Standards. Recertification requirements for SRMs and CRMs are specified by NBS and NBS/EPA, respectively. See 4.0.2.1 for GMIS recertification requirements.

    4.0.3Using the Procedure

    The assay/certification procedure described here is carefully designed to minimize both systematic and random errors in the assay process. Therefore, the procedure should be carried out as closely as possible to the way it is described. Similarly, the assay apparatus has been specifically designed to minimize errors and should be configured as closely as possible to the design specified. Good laboratory practice should be observed in the selection of inert materials (e.g. Teflon, stainless steel, or glass, if possible) and clean, non-contaminating components for use in portions of the apparatus in contact with the candidate or reference gas concentrations.

    4.0.4Certification Documentation

    Each assay/certification must be documented in a written certification report signed by the analyst and containing at least the following information:

    1. Identification number (cylinder number).

    2. Certified concentration of the standard, in ppm or mole percent.

    3. Balance gas in the standard mixture.

    4. Cylinder pressure at certification.

    5. Date of the assay/certification.

    6. Certification expiration date (see 4.0.6.3).

    7. Identification of the reference standard used: SRM number, cylinder number, and concentration for an SRM; cylinder number and concentration for a CRM or GMIS.

    8. Statement that the assay/certification was performed according to this section 3.0.4.

    9. Identification of the laboratory where the standard was certified and the analyst who performed the certification.

    10. Identification of the gas analyzer used for the certification, including the make, model, serial number, the measurement principle, and the date of the last multipoint calibration.

    11. All analyzer readings used during the assay/certification and the calculations used to obtain the reported certified value.

    12. Chronological record of all certifications for the standard.

    Certification concentrations should be reported to 3 significant digits. Certification documentation should be maintained for at least 3 years.

    4.0.5Certification Label

    A label or tag bearing the information described in items 1 through 9 of subsection 4.0.4 must be attached to each certified gas cylinder.

    4.0.6Assay/Certification of Compressed Gas (Cylinder) Standards

    4.0.6.1Aging of newly-prepared gas standards. Freshly prepared gas standard concentrations and newly filled gas cylinders must be aged before being assayed and certified. SO2 concentrations contained in steel cylinders must be aged at least 15 days; other standards must be aged at least 4 days.

    4.0.6.2Stability test for reactive gas standards. Reactive gas standards, including nitric oxide (NO), nitrogen dioxide (NO2), sulfur dioxide (SO2), and carbon monoxide (CO), that have not been previously certified must be tested for stability as follows: Reassay the concentration at least 7 days after the first assay and compare the two assays. If the second assay differs from the first assay by 1.5% or less, the cylinder may be considered stable, and the mean of the two assays should be reported as the certified concentration. Otherwise, age the cylinder for a week or more and repeat the test, using the second and third assays as if they were the first and second assays. Cylinders that are not stable may not be sold and/or used for calibration or audit purposes.

    4.0.6.3Recertification of compressed gas standards. Compressed gas standards must be recertified according to this section 3.0.4 within the time limits specified in table 7.13,6,7. The reassay concentration must be within 5% of the previous certified concentration. If not, the cylinder must be retested for stability (subsection 4.0.6.2). The certified concentration of a recertified standard should be reported as the mean of all assays, unless a clear trend or substantial change suggests that previous assays are no longer valid.

    Table 7.1—Recertification Limits for Compressed Gas StandardsPollutantBalance gas 1Concentration rangeMaximum months until recertification for cylinder materialPassivated AluminumOtherCarbon monoxideN2 or air" 8 ppm366Nitric oxideN2" 5 ppm246Sulfur dioxideN2 or air 50-499 ppm246Sulfur dioxideN2 or air" 500 ppm366Oxides of nitrogenAir" 100 ppm246Nitrogen dioxideAir" 1000 ppm246Carbon dioxideN2 or air" 300 ppm3618Carbon dioxide and oxygen, (i.e. blood gas)N2" 5% CO2, "0% O2366OxygenN2" 2 percent3618Carbon dioxide and nitrous oxideAir" 300 ppm CO2, "300 ppb N2 O366Others not specifically listed66Multicomponent mixtures____See 26Mixtures with lower concentrations____See 361 When used as a balance gas, “air” is defined as a mixture of O2 and N2 where the minimum concentration of O2 is 10% and the concentration of N2 is greater than 60%.2 This protocol may be used to assay and certify individual components of multicomponent standards, provided that none of the components interferes with the analysis of other components and provided that individual components must not react with each other or with the balance gas. A multicomponent standard can be certified for a period of time equal to that of its most briefly certifiable component. For example, a standard containing 250 ppm sulfur dioxide and 100 ppm carbon monoxide in nitrogen can be certified for 24 months because the shortest certification period is 24 months.3 This protocol may be used for the certification of standards with concentrations that may be lower than those listed in table 7.1. The initial certification period for such a lower concentration standard is 6 months. After this period, the standards may be recertified. If the recertification demonstrates that the standard is not unstable, the second certification period for this lower concentration standard is the same time period as indicated for the corresponding concentration standard listed in table 7.1.

    4.0.6.4Minimum cylinder pressure. No compressed gas cylinder standard should be used when its gas pressure is below 700 kPa (100 psi), as indicated by the cylinder pressure gauge.

    4.0.6.5Assay/certification of multi-component compressed gas standards. Procedure G1 may be used to assay and certify individual components of multi-component gas standards, provided that none of the components other than the component being assayed cause a detectable response on the analyzer.

    4.0.7Analyzer Calibration

    4.0.7.1Basic analyzer calibration requirements. The assay procedure described in this section 3.0.4 employs a direct ratio referencing technique that inherently corrects for minor analyzer calibration variations (drift) and DOES NOT depend on the absolute accuracy of the analyzer calibration. What is required of the analyzer is as follows: 1) it must have a linear response to the pollutant of interest (see subsection 4.0.7.5), 2) it must have good resolution and low noise, 3) its response calibration must be reasonably stable during the assay/certification process, and 4) all assay concentration measurements must fall within the calibrated response range of the analyzer.

    4.0.7.2Analyzer multipoint calibration. The gas analyzer used for the assay/certification must have had a multipoint calibration within 3 months of its use when used with this procedure. This calibration is not used to quantitatively interpret analyzer readings during the assay/certification of the candidate gas because a more accurate, direct ratio comparison of the candidate concentration to the reference standard concentration is used. However, this multipoint calibration is necessary to establish the calibrated range of the analyzer and its response linearity.

    The multipoint calibration should consist of analyzer responses to at least 5 concentrations, including zero, approximately evenly spaced over the concentration range. Analyzer response units may be volts, millivolts, percent of scale, or other measurable analyzer response units. The upper range limit of the calibrated range is determined by the highest calibration point used. If the analyzer has a choice of concentration ranges, the optimum range for the procedure should be selected and calibrated. Plot the calibration points and compute the linear regression slope and intercept. See subsection 4.0.7.5 for linearity requirements and the use of a mathematical transformation, if needed. The intercept should be less than 1 percent of the upper concentration range limit, and the correlation coefficient (r) should be at least 0.999.

    4.0.7.3Zero and span check and adjustment. On each day that the analyzer will be used for assay/certification, its response calibration must be checked with a zero and at least one span concentration near the upper concentration range limit. If necessary, the zero and span controls of the analyzer should be adjusted so that the analyzer's response (i.e. calibration slope) is within about ±5 percent of the response indicated by the most recent multipoint calibration. If a zero or span adjustment is made, allow the analyzer to stabilize for at least an hour or more before beginning the assay procedure, since some analyzers drift for a period of time following zero or span adjustment. If the analyzer is not in continuous operation, turn it on and allow it to stabilize for at least 12 hours before the zero and span check.

    4.0.7.4Pollutant standard for multipoint calibration and zero and span adjustment. The pollutant standard or standards used for multipoint calibration or zero and span checks or adjustments must be obtained from a compressed gas standard certified traceable to an NBS SRM or a NBS/EPA CRM according to Procedure G1 of this section 3.0.4. This standard need not be the same as the reference standard used in the assay/certification. The zero gas must meet the requirements in subsection 4.0.8.

    4.0.7.5Linearity of analyzer response. The direct ratio assay technique used in Procedure G1 requires that the analyzer have a linear response to concentration. Linearity is determined by comparing the quantitative difference between a smoothly-drawn calibration curve based on all calibration points and a straight line drawn between zero and an upper reference point (see Figure 1). This difference is measured in concentration units, parallel to the concentration axis, from a point on the calibration curve to the corresponding point for the same response on the straight line.

    For the general linearity requirement, the straight line is drawn between zero and the highest calibration point (Figure 1a). Linearity is then acceptable when no point on the smooth calibration curve deviates from the straight line by more than 1.5 percent of the value of the highest calibration concentration. An alternative linearity requirement is defined on the basis of the actual reference and candidate concentrations to be used for the assay. In this case, the reference and candidate concentrations are plotted on the calibration curve, and the straight line is drawn from zero to the reference concentration and extrapolated, if necessary, beyond the candidate concentration (Figure 1b). The deviation of the smooth calibration curve from the straight line at the candidate concentration point then must not exceed 0.8 percent of the value of the reference concentration. This latter specification may allow the use of an analyzer having greater nonlinearity when the reference and candidate concentrations are nearly the same.

    For analyzers having an inherently non-linear response, the response can usually be linearized with a simple mathematical transformation of the response values, such as R′=square root(R) or R′=log(R), where R′ is the transformed response value and R is the actual analyzer response value. Using the transformed response values, the multipoint calibration should meet one of the above linearity requirements as well as the requirements for intercept and correlation coefficient given in subsection 4.0.7.2.

    4.0.8Zero Gas

    Zero gas used for dilution of any candidate or reference standard should be clean, dry, zero-grade air or nitrogen containing a concentration of the pollutant of interest equivalent to less than 0.5 percent of the analyzer's upper range limit concentration. The zero gas also should contain no contaminant that causes a detectable response on the analyzer or that suppresses or enhances the analyzer's response to the pollutant. The oxygen content of zero air should be the same as that of ambient air.

    4.0.9Accuracy Assessment of Commercially Available Standards

    Periodically, the USEPA will assess the accuracy of commercially available compressed gas standards that have been assayed and certified according to this section 3.0.4. Accuracy will be assessed by EPA audit analysis of representative actual commercial standards obtained via an anonymous agent. The accuracy audit results, identifying the actual gas manufacturers or vendors, will be published as public information.

    EC01SE92.136 Table 7.2—NBS SRM Reference GasesSRM No.TypeNominal concentration2627NO/N25 ppm.2628NO/N210 ppm.2629NO/N220 ppm.1683bNO/N250 ppm.1684bNO/N2100 ppm.1685bNO/N2250 ppm.1686bNO/N2500 ppm.1687bNO/N21000 ppm.2630NO/N21500 ppm.2631NO/N23000 ppm.2653NO/2 Air250 ppm.2654NO/2 Air500 ppm.2655NO/2 Air1000 ppm.2656NO/2 Air2500 ppm.2612aCO/Air10 ppm.2613aCO/Air20 ppm.2614aCO/Air45 ppm.1677cCO/N210 ppm.2635CO/N225 ppm.1678cCO/N250 ppm.1679cCO/N2100 ppm.2636CO/N2250 ppm.1680cCO/N2500 ppm.1681cCO/N21000 ppm.2637CO/N22500 ppm.2638CO/N25000 ppm.2639CO/N21 percent.2640CO/N22 percent.2641CO/N24 percent.2642CO/N28 percent.2657O2/N22 percent.2658O2/N210 percent.2659O2/N221 percent.1693SO2/N250 ppm.1694SO2/N2100 ppm.1661aSO2/N2500 ppm.1662aSO2/N21000 ppm.1663aSO2/N21500 ppm.1664aSO2/N22500 ppm.1696SO2/N23500 ppm.1670CO2/Air330 ppm.1671CO2/Air340 ppm.1672CO2/Air350 ppm.2632CO2/N2300 ppm.2633CO2/N2400 ppm.2634CO2/N2800 ppm.2619aCO2/N20.5 percent.2720aCO2/N21.0 percent.2621aCO2/N21.5 percent.2622aCO2/N22.0 percent.2623aCO2/N22.5 percent.2624aCO2/N23.0 percent.2625aCO2/N23.5 percent.2626aCO2/N24.0 percent.1674bCO2/N27.0 percent.1675bCO2/N214.0 percent.1665bC3 H8/Air3 ppm.1666bC3 H8/Air10 ppm.1667bC3 H8/Air50 ppm.1668bC3 H8/Air100 ppm.1669bC3 H8/Air500 ppm.2643C3 H8/N2100 ppm.2644C3 H8/N2250 ppm.2645C3 H8/N2500 ppm.2646C3 H8/N21000 ppm.2647C3 H8/N22500 ppm.2648C3 H8/N25000 ppm.2649C3 H8/N21 percent.2650C3 H8/N22 percent.NBS-SRM cylinders contain approximately 870 liters of gas at STP.For availability, contact: Office of Standard Reference Materials, Chemistry Building, Room B311, NBS, Gaithersburg, Maryland 20899, (301) 975-6776. (FTS 879-6776). 4.1Procedure G1: Assay and Certification of a Compressed Gas Standard Without Dilution 4.1.1Applicability

    This procedure may be used to assay the concentration of a candidate compressed gas (cylinder) pollutant standard, based on the concentration of a compressed gas (cylinder) reference standard of the same pollutant compound, and certify that the assayed concentration thus established for the candidate standard is traceable to the reference standard. The procedure employs a pollutant gas analyzer to compare the candidate and reference gas concentrations by direct measurement—without dilution of either gas—to minimize assay error.

    4.1.2Limitations

    1. The concentration of the candidate gas standard must be between 0.3. and 1.3 times the concentration of the reference gas standard.

    2. The analyzer must have a calibrated range capable of directly measuring both the candidate and the reference gas concentrations.

    3. The analyzer's response (or transformed response) must be linear with respect to concentration.

    4. The balance gas in both the candidate and reference standards must be identical, unless it can be shown that the analyzer is insensitive to any difference in the balance gases.

    5. A source of clean, dry zero gas is required.

    4.1.3Assay Apparatus

    Figure G1 illustrates the relatively simple assay apparatus. The configuration is designed to allow convenient routing of the zero gas and undiluted samples of the reference gas and candidate gases, in turn, to the analyzer for measurement, as selected by three-way valves V1 and V2. Pressure regulators and needle valves (V3 and V4) control the individual gas flows. The pollutant concentrations are delivered to the analyzer via a vented tee, which discharges excess flow and insures that the assay concentrations sampled by the analyzer are always at a fixed (atmospheric) pressure. A small, uncalibrated rotameter monitors the vent flow to verify that the total gas flow rate exceeds the sample flow rate demand of the analyzer so that no room air is admitted through the vent. Valves V1 and V2 could be replaced by a single four-way valve (with 3 inputs and 1 output) or by manually moving the output connection to each of the gases as needed. See also subsection 4.0.3.

    EC01SE92.137 4.1.4Analyzer

    See subsection 4.0.7.1. The pollutant gas analyzer must have a linear response function and a calibrated range capable of measuring the full concentration of both the candidate and the reference gas standards directly, without dilution. It must have good resolution (readability), good precision, a stable response, and low output signal noise. In addition, the analyzer must have good specificity for the pollutant of interest so that it has no detectable response to any contaminant that may be contained in either the candidate or reference gas. If the candidate and reference gases contain dissimilar balance gases (air versus nitrogen or different proportions of oxygen in the balance air, for example), the analyzer must be proven to be insensitive to the different balance gases. This may be accomplished by showing no difference in analyzer response when measuring pollutant concentrations diluted with identical flow rates of the two balance gases.

    The analyzer should be connected to a suitable, precision chart recorder or other data acquisition device to facilitate graphical observation and documentation of the analyzer responses obtained during the assay.

    4.1.5Analyzer Calibration

    4.1.5.1Multipoint calibration. See subsections 4.0.7.2 and 4.0.7.4.

    4.1.5.2Calibration range. The calibrated range of the analyzer must include both the candidate and reference gas concentrations, such that the higher concentration does not exceed 97 percent of the upper range limit, and the lower concentration is not below 25 percent of the upper range limit (assuming a lower range limit of zero). Within these limits, select a calibrated analyzer range that will produce the highest analyzer responses.

    4.1.5.3Linearity. The direct ratio assay technique used in this procedure requires that the analyzer have a linear response to concentration (see subsection 4.0.7.5). High-concentration-range analyzers of the type that are required for this procedure may not be inherently linear, but they usually have a predictable, non-linear response characteristic that can be mathematically transformed to produce a sufficiently linear response characteristic suitable for use in this procedure. Any such response transformation should be verified by using it for the multipoint calibration. Caution should be exercised in using a transformed response curve because physical zero or span adjustments to the analyzer may produce unexpected effects on the transformed characteristic.

    4.1.5.4Zero and span adjustment. See subsections 4.0.7.3 and 4.0.7.4. Prior to carrying out the assay/certification procedure, check the calibration of the analyzer and, if necessary, adjust the analyzer's zero and span controls to reestablish the response characteristic determined at the most recent multipoint calibration. Allow the analyzer to stabilize for an hour or more after any zero or span adjustment. If there is any doubt that a transformed response characteristic is still linear following a zero or span adjustment, verify linearity with a multipoint calibration (subsection 4.0.7.2) using at least 3 known pollutant concentrations, including zero.

    4.1.6Assay Gases

    4.1.6.1Candidate gas standard. See subsections 4.0.6 and 4.1.2.

    4.1.6.2Reference gas standard. See subsections 4.0.2, 4.1.2, and 4.0.6.4. Select a reference standard such that the concentration of the candidate gas is not more than 30 percent above nor less than 70 percent below the concentration of the standard.

    4.1.6.3Zero gas. See subsection 4.0.8. The zero gas should match the balance gas used in the cylinder concentrations.

    4.1.7Assay Procedure

    1. Verify that the assay apparatus is properly configured, as described in subsection 4.1.3 and shown in Figure G1.

    2. Verify that the linearity of the analyzer has been checked within the last 3 months (see subsections 4.0.7.2, 4.0.7.5, and 4.1.4), that the zero and span are adjusted correctly (subsection 4.0.7.3), that the candidate and reference gas concentrations are within 25 and 97 percent of the upper range limit of the calibrated measurement range of the analyzer, and that the analyzer is operating stably.

    3. Adjust the flow rates of the three gases (reference, candidate, and zero) to approximately the same value that will provide enough flow for the analyzer and sufficient excess to assure that no ambient air will be drawn into the vent.

    4. Conduct a triad of measurements with the analyzer. Each triad consists of a measurement of the zero gas concentration, a measurement of the reference gas concentration, and a measurement of the candidate gas concentration. Use valves V1 and V2 to select each of the three concentrations for measurement. For each measurement, allow ample time for the analyzer to achieve a stable response reading. Record the stable analyzer response for each measurement, using the same response units (volt, millivolts, percent of scale, etc.) used for the multipoint calibration and any transformation of the response readings necessary for linearity. Do not translate the response readings to concentration values via the calibration curve (see the footnote following equation G1). Do not make any zero, span, or other physical adjustments to the analyzer during the triad of measurements.

    5. Conduct at least 2 additional measurement triads, similar to step 4 above. However, for these subsequent triads, change the order of the three measurements (e.g. measure reference gas, zero gas, candidate gas for the second triad and zero gas, candidate gas, reference gas for the third triad, etc.).

    6. If any one or more of the measurements of a triad is invalid or abnormal for any reason, discard all three measurements of the triad and repeat the triad.

    7. For each triad of measurements, calculate the assay concentration of the candidate gas as follows:

    EC01SE92.138 Equation G1 where: Cc = Assay concentration of the candidate gas standard, ppm or percent; Cr = Concentration of the reference gas standard, ppm or percent; Rc = Stable response reading of the analyzer for the candidate gas, analyzer response units;* Rz = Stable response reading of the analyzer for the zero gas, analyzer response units;* Rr = Stable response reading of the analyzer for the reference gas, analyzer response units.* *Analyzer response units are the units used to express the direct response readings of the analyzer, such as volts, millivolts, percent of scale, etc. DO NOT convert these direct response readings to concentration units with the multipoint calibration curve or otherwise adjust these readings except for transformation necessary to achieve response linearity.

    8. Calculate the mean of the 3 (or more) valid assays. Calculate the percent difference of each assay from the mean. If any one of the assay values differs from the mean by more than 1.5%, discard that assay value and conduct another triad of measurements to obtain another assay value. When at least 3 assay values all agree within 1.5% of their mean, report the mean value as the certified concentration of the candidate gas standard. For newly-prepared reactive standards, a reassay at least 7 days later is required to check the stability of the standard; see subsection 4.0.6.2.

    4.1.8Stability Test for Newly-Prepared Standards

    See subsections 4.0.6.1 and 4.0.6.2.

    4.1.9Certification Documentation

    See subsections 4.0.4 and 4.0.5.

    4.1.10Recertification Requirements

    See subsections 4.0.6.3 and 4.0.6.4.

    4.2References

    1. Code of Federal Regulations, title 40, part 60, “Standards of Performance for New Stationary Sources,” Appendix A, Method 20 (1982).

    2. Standards of Performance for New Stationary Sources; Quality Assurance Requirements for Gaseous Continuous Emission Monitoring Systems Used for Compliance Determination, promulgated in the Federal Register, June 4, 1987, pp. 21003-21010.

    3. “A Procedure for Establishing Traceability of Gas Mixtures to Certain National Bureau of Standards Standard Reference Materials. EPA-600/7-81-010. Joint publication by NBS and EPA, May 1981. Available from the U.S. Environmental Protection Agency, Environmental Monitoring Systems Laboratory (MD-77), Research Triangle Park, NC 27711.

    4. Code of Federal Regulation, title 40, part 50, “National Ambient Air Quality Measurement Methodology”.

    5. Code of Federal Regulations, title 40, part 58, “Ambient Air Quality Surveillance,” appendixes A and B.

    6. Shores, R.C. and F. Smith, “Stability Evaluation of Sulfur Dioxide, Nitric Oxide, and Carbon Monoxide Gases in Cylinders”. NTIS No. PB 85-122646. Available from the National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161.

    7. Method 6A and 6B, “Determination of Sulfur Dioxide, Moisture, and Carbon Dioxide Emissions from Fossil Fuel Combustion Sources,” Quality Assurance Handbook for Air Pollution Measurement Systems, Volume III, Section 3.13.8, July 1986. Available from the U.S. Environmental Protection Agency, Center for Environmental Research Information, Cincinnati, OH 45268.

    8. “List of Designated Reference and Equivalent Methods.” Current edition available from the U.S. Environmental Protection Agency, Environmental Monitoring Systems Laboratory, Quality Assurance Division (MD-77), Research Triangle Park, NC 27711.