### REVISIONS TO TEST METHODS AND TESTING REGULATIONS

**Redline/Strikeout of Proposed Revisions to Current Rules September 2011** 
For the reasons stated in the preamble, the Environmental Protection Agency proposes to amend title 40, chapter I of the Code of Federal Regulations as follows: **P ART**  **51 –**  **REQUIREMENTS FOR PREPARATION, ADOPTION, AND SUBMITTAL OF**  **IMPLEMENTATION PLANS** 1. The authority citation for part 51 continues to read as follows: Authority: 42 U.S.C. 7401 , et. seq. 2. In Appendix M by revising Section 4(a) of the introduction to read as follows: **Appendix M to Part 51 —**  **Recommended Test Methods for State Implementation Plans**  4 . * * * a. The source owner, operator, or representative of the tested facility shall obta in an audit sample, if commercially available, from an AASP for each test method used for regulatory compliance purposes. No audit samples are required for the following test methods: Methods 3A and 3C of Appendix A
- 3 of Part 60, Methods 6C, 7E, 9, and 10 of Appendix A
- 4 of Part 60, Methods 18 and 19 of Appendix A
- 6 of Part 60, Methods 20, 22, and 25A of Appendix A
- 7 ofPage **2** of **161**

Part 60, and Methods 303, 318, 320, and 321 of Appendix A of Part 63. If multiple sources at a single facility are tested during a compliance test event, only one audit sample is required for each method used during a compliance test. The compliance a uthority responsible for the compliance test may waive the requirement to include an audit sample if they believe that an audit sample is not necessary. “Commercially available” means that two or more independent AASPs have blind audit samples available fo r purchase. If the source owner, operator, or representative cannot find an audit sample for a specific method, the owner, operator, or representative shall consult the EPA Web site at the following URL, http://www.epa.gov/ttn/emc, to confirm whether there is a source that can supply an audit sample for that method. If the EPA Web site does not list an available audit sample at least 60 days prior to the beginning of the compliance test, the source owner, operator, or representative shall not be required to include an audit sample as part of the quality assurance program for the compliance test. When ordering an audit sample, the source owner, operator, or representative shall give the sample provider an estimate for the concentration of each pollutant that is emitted by the source or the estimated concentration of each pollutant based on the permitted level and the name, address, and phone number of the compliance authority. The source owner, operator, or representative shall report the results for the audit sample along with a summary of the emission test results for the audited pollutant to the compliance authorityPage **3** of **161**

and shall report the results of the audit sample to the AASP. The source owner, operator, or representative shall make both reports at the same time and in the same manner or shall report to the compliance authority first and report to the AASP. If the method being audited is a method that allows the samples to be analyzed in the field and the tester plans to analyze the samples in the field, the tester may analyze the audit samples prior to collecting the emission samples provided a representative of the compliance authority is present at the testing site. The tester may request and the compliance authority may grant a waiver to the requirement th at a representative of the compliance authority must be present at the testing site during the field analysis of an audit sample. The source owner, operator, or representative may report the results of the audit sample to the compliance authority and then report the results of the audit sample to the AASP prior to collecting any emission samples. The test protocol and final test report shall document whether an audit sample was ordered and utilized and the pass/fail results as applicable.
* * * * * 3. In Method 201A of Appendix M by revising Sections 8.3.4(b), 8.3.4.1, 8.7.2.2, 8.7.5.5(a), the introductory paragraph of Section 10.1, Section 11.2.1, Equation 9 in Section 12.5, and by deleting Section 10.5 and the term “V b ” and its definition from Section 12 .1 to read as follows:Page **4** of **161**

**Method 201A —**  **Determination of PM 10**  **and PM 2.5**  **Emissions f**  **rom Stationary Sources (Constant Sampling Rate Procedure)**  * * * * * 8.3.4 * * * (b) The appropriate nozzle to maintain the required gas sampling rate for the velocity pressure range and isokinetic range. If the isokinetic range cannot be met (e.g., batch processes, extreme process flow or temperature variation), void the sample or use methods subject to the approval of the Administrator to correct the data. The acceptable variation from isokinetic sampling is 80 to 120 percent and no more than 100 ± 21 percent ( 2 out of 12 or 5 out of 24) sampling points outside of this cri teria.
* * * * *
8.3.4.1 Preliminary traverse. You must use an S - type pitot tube with a conventional thermocouple to conduct the traverse. Conduct the preliminary traverse as close as possible to the anticipated testing time on sources that are subject to hour
- by
- hour gas flow rate variations of approximately ± 20 percent and/or gas temperature variations of approximately ± 10 °C (± 18 °F). (Note: You should be aware that these variations can cause errors in the cyclone cut diameters and the isokinetic sampling velocities.)
* * * * *Page **5** of **161**

8.7.2.2 Probe blockage factor. You must us e Equation 26 to calculate an average probe blockage correction factor (b f ) if the diameter of your stack or duct is between 25.7 and 36.4 inches for the combined PM 2.5 / PM 10 sampling head and pitot and between 18.8 and 26.5 inches for the PM 2. 5 cyclone and pitot. A probe blockage factor is calculated because of the flow blockage caused by the relatively large cross
- sectional area of the cyclone sampling head, as discussed in Section 8.3.2.2 and illustrated in Figures 8 and 9 of Section 17. You must dete rmine the cross
- sectional area of the cyclone head you use and determine its stack blockage factor. (Note: Commercially
available sampling heads (including the PM 10 cyclone , PM 2. 5 cyclone , pitot and filter holder) have a projected area of approximately 31. 2 square inches when oriented into the gas stream. As the probe is moved from the outer most to the inner most point, the amount of blockage that actually occurs ranges from approximately 13 square inches to the full 31.2 inches plus the blockage caused by the probe extension. The average cross
- sectional area blocked is 22 square inches .
* * * * * 8.7.5.5 * * * ( a) Container #1, Less than or equal to PM 2.5 micrometer filterable particulate. Use tweezers and/or clean disposable surgical gloves to remove the filter from the filter holder. Place the filter in the Petri dish that you labeled with the test identification andPage **6** of **161**

Container #1. Using a dry brush and/or a sharp
- edged blade, carefully transfer any PM and/or filter fibers that adhere to the filter holder gasket or filter support screen to the Petri dish. Seal the container. This container holds particles less than or equal to 2.5 micrometers that are caugh t on the in
- stack filter. (Note: If the test is conducted for PM 10 only , then Container #1 would be for less than or equal to PM 10 micrometer filterable particulate.) * * * * *
10.1 Gas Flow Velocities. You must use an S
- type pitot tube that meets the re quired EPA specifications (EPA Publication 600/4

– 77

– 0217b) during these velocity measurements. (Note:If, as specified in Section 8.7.2.3, testing is performed in stacks less than 26.5 inches in diameter, testers may use a standard pitot tube according to t he requirements in Method 1 or 2 of appendix A

– 3 to part 60.) You must also complete the following:
* * * * * * * * * *
11.2.1 Container #1, Less than or Equal to PM 2. 5 Micrometer Filterable Particulate. Transfer the filter and any loose particulate from the sample container to a tared weighing dish or pan that is inert to solvent or mineral acids. Desiccate for 24 hours i n a desiccators containing anhydrous calcium sulfate. Weigh to a constant weight and report the results to the nearest 0.1 mg. (SeePage **7** of **161**

Section 3.0 for a definition of c onstant weight.) If constant weight requirements cannot be met, data should be r eported and flagged as a minimum value. (Note: Regardless of the stack temperature , you are not required to speciate the Method 201A nozzle, front half or in
stack filter sample into organic and inorganic fractions. Neither Method 17 nor 201A require separ ate analysis of the filter for inorganic and organic PM. Since the in
- stack filter samples collected at ≤ 30  C (85  F) may include both filterable insoluble particulate and condensable particulate, the filter should be weighed after desiccation but not extracted since insoluble particulate will not be recovered from the extraction.)
* * * * * 12.5 * * *

For N re greater than or equal to 3,162: 

###                    

### D 1 T M P C μ 0.07657 = Q 50 1.241

s W S 0.3795 0.6205 IV (Eq. 9)
* * * * * 4. In Method 202 of Appendix M by revising the introductory paragraph in Section 8.5.3.1, Section 11.2.2, and Figures 2, 3, 4, 5, and 6 in Section 18.0 to read as follows: **Method 20 2**  **— Determination of PM**  **10 and PM**  **2.5 Emissions**  **f rom Stationary**  **Sources (Constant Sampling Rate Procedure)** * * * * *Page **8** of **161**

8.5.3.1 If you choose to conduct a pressurized nitrogen purge on the complete CPM sampling train, you may quantitatively transfer the water collected in the condenser and the water dropout impinger to the backup impinger as an alternative to replacin g the short stem impinger insert with a long stem insert prior to purging the sampling train. You must measure the water combined in the backup impinger and record the volume or weight as part of the moisture collected during sampling as specified in Sect ion 8.5.3.4.
* * * * *
11.2.2 CPM Container #1, Aqueous Liquid Impinger Contents. Analyze the water soluble CPM in Container # 1 as described in this section. Place the contents of Container #1 into a separatory funnel. Add approximately 30 ml of hexane to the funnel, mix well, and pour off the upper organic phase. Repeat this procedure twice with 30 ml of hexane each time combining the organic phase from each extraction. Each time, leave a small amount of the organic/hexane phase in the separatory funnel, ensuring that no water is collected in the organic phase. This extraction should yield about 90 ml of organic extra ct. Combine the organic extract from Container #1 with the organic train rinse in Container # 2.Page **9** of **161**

**Figure 2. Nitrogen Purge Train Configuration (Vacuum Purge) No**  **c heck**  **v alve**  **a fter**  **i mpingers**  **; Extended stem in first impinger; Condensed moisture and sample**  **impingers identified**WaterBath(<20to30C/68to85F)CondenserThermocoupleCondensedMoistureandSampleSilicaGel(~300grams)RecirculationPumpTemperatureSensorIceBathUHPnitrogenorequivalentFilter **O**

**O**RegulatorUseinlinerotameterwhenpullingpurgenitrogenthroughthesystem(excessflowrate)OrificeManometerDryGasMeterBy-PassValvePumpMainValveVacuumGaugeVacuumLinePage **10** of **161**

**Figure 3. Nitrogen Purge Train Configuration (Pressure Purge)**

**Extended stem in first impinger** * * * * *WaterBath(20to30C/68to85F)CondenserThermocoupleRecirculationPumpUHPnitrogenorequivalentFilter **O**

**O**Usewhenpushingpurgenitrogenthroughthesystem(flowrate14lpmorH@)RegulatorCondensedMoistureandSamplePage **11** of **161**

**Figure 4 —**  **Field Train Recovery Blank Condensable Particulate Calculations**  **Field Train Recovery Blank Condensable Particulate Calculations**  Plant Date Blank No. CPM Filter No. Water volume added to purge train (Vp) **Field Reagent Blank Mass a**  ml Water (Section 11.2.7) Acetone (Section 11.2.6) mg Hexane (Section 11.2.8) mg **Field Train Recovery Blank Mass** mg Mass of Organic CPM (m ob) (Section 11.2.3) Mass of Inorganic CPM (mib) (Equation 3) mg Mass of the Field Train Recovery Blank (not to exceed 2.0 mg) (Equation 2) mg mg

a Field reagent blanks are optional and intended to provide the testing contractor with information they can use to implement corrective actions, if necessary, to reduce the residual mass contribution from reagents used in the field. Field reagent blanks are not used to correct the CPM measurement results. **Table reprinted for improved clarity**Page **12** of **161**

**Figure 5 —** 

**Other Field Train Sample Condensable Particulate Data Other Field Train Sample Condensable Particulate Data**  Plant Date Run No. CPM Filter No. Water volume added to purge train (max 50 ml) (Vp) ml Date Run No. CPM Filter No. Water volume added to purge train (max 50 ml) (Vp) ml Date Run No. CPM Filter No. Water volume added to purge train (max 50 ml) (Vp) ml **Table reprinted for improved clarity** Page **13** of **161**
**Figure 6 —**  **CPM Work Table Calculations for Recovery of Condensable PM (CPM)**  Plant Date Run No. **Sample Preparation —**  **CPM Containers No. 1 and 2 (Section 11.1):** Was significant volume of water lost during transport? Yes or No If Yes, measure the volume received Estimate the volume lost during transport ml Plant Date Run No. Was significant volume of organic rinse lost during transport? Yes or No

If Yes, measure the volume received Estimate the volume lost during transport. ml **For Titration:**

Normality of NH4OH (N) (Section 10.2) N Volume of titrant (Vt) (Section 11.2.2.2) ml Mass of NH4 added (mc) (Equation 1) mg **For CPM Blank Weights:**

Inorganic Field Train Recovery Blank Mass(mib) (Section 9.9) mg Organic Field Train Recovery Blank Mass (mob) (Section 9.9) mg Mass of Field Train Recovery Blank (Mfb) (max. 2 mg) (Equation 2) mg **For CPM Train Weights:**

Mass of Organic CPM (mo) (Section 11.2.3) mg Mass of Inorganic CPM (mi) (Equation 3) mg Total CPM Mass (mcpm) (Equation 4) mg

**Table reprinted for improved clarity** Page **14** of **161**

**Part 60 –**  **STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES** 1. The authority citation for part 60 continues to read as follows: **Authority** : 42 U.S.C. 7401, et. seq. **§60.8 [Amended]** 2. By revising §60.8(g)(1) and adding new paragraphs ( h) and (i) to read as follows: **§60.8 Performance tests.**  * * * * * (g) * * * (1) The source owner, operator, or representative of the tested facility shall obtain an audit sample, if commercially availa ble, from an AASP for each test method used for regulatory compliance purposes. No audit samples are required for the following test methods: Methods 3A and 3C of Appendix A
- 3 of Part 60, Methods 6C, 7E, 9, and 10 of Appendix A
- 4 of Part 60, Methods 18 and 19 of Appendix A
- 6 of Part 60, Methods 20, 22, and 25A of Appendix A
- 7 of Part 60, and Methods 303, 318, 320, and 321 of Appendix A of Part 63. If multiple sources at a single facility are tested during a compliance test event, only one audit sampl e is required for each method used during a compliance test. The compliance authorityPage **15** of **161**

responsible for the compliance test may waive the requirement to include an audit sample if they believe that an audit sample is not necessary. “Commercially available” m eans that two or more independent AASPs have blind audit samples available for purchase. If the source owner, operator, or representative cannot find an audit sample for a specific method, the owner, operator, or representative shall consult the EPA w eb site at the following URL, www.epa.gov/ttn/emc, to confirm whether there is a source that can supply an audit sample for that method. If the EPA w eb site does not list an available audit sample at least 60 days prior to the beginning of the co mpliance test, the source owner, operator, or representative shall not be required to include an audit sample as part of the quality assurance program for the compliance test. When ordering an audit sample, the source owner , operator, or representative sha ll give the sample provider an estimate for the concentration of each pollutant that is emitted by the source or the estimated concentration of each pollutant based on the permitted level and the name, address, and phone number of the compliance authority. The source owner, operator, or representative shall report the results for the audit sample along with a summary of the emission test results for the audited pollutant to the compliance authority and shall report the results of the audit sample to the AAS P. The source owner, operator, or representative shall make both reports at the same time and in the same manner or shall report to the compliance authority first and then report to the AASP. If the methodPage **16** of **161**

being audited is a method that allows the samples to be analyzed in the field and the tester plans to analyze the samples in the field, the tester may analyze the audit samples prior to collecting the emission samples provided a representative of the compliance authority is present at the testing site. Th e tester may request , and the compliance authority may grant , a waiver to the requirement that a representative of the compliance authority must be present at the testing site during the field analysis of an audit sample. The source owner, operator, or rep resentative may report the results of the audit sample to the compliance authority and report the results of the audit sample to the AASP prior to collecting any emission samples. The test protocol and final test report shall document whether an audit samp le was ordered and utilized and the pass/fail results as applicable.
* * * * * (h) Unless otherwise specified in the applicable subpart, each test location must be verified to be free of cyclonic flow and evaluated for the existence of emission gas stratification and the required number of sampling traverse points. If other procedur es are not specified in the applicable subpart to the regulations, use the appropriate procedures in Method 1 to check for cyclonic flow and Method 7E to evaluate emission gas stratification and selection of sampling points.Page **17** of **161**

( i ) Whenever the use of mult iple cal ibration gases is required by a test method, performance specification , or quality assurance procedure in a part 60 standard or appendix , Method 205 of 40 CFR Part 51, Appendix M, “Verification of Gas Dilution Systems for Field Instrument Calibrati ons,” may be used. * * * * * **§60. 13**  **[Amended]** 3. By revising §60.13 (d)(1) as follows: **§ 60.13 Monitoring requirements.**  * * * * * (d)(1) Owners and operators of a CEMS installed in accordance with the provisions of this part, must check the zero (or low level value between 0 and 20 percent of span value) and span (50 to 100 percent of span value) calibration drifts at least once dail y in accordance with a written procedure. The zero and span must, a t a minimum, be adjusted whenever either the 24
- hour zero drift or the 24
- hour span drift exceeds two times the limit of the applicable performance specification in A ppendix B o f this part. The system must allow the amount of the excess zero and span drift to be recorded and quantified whenever specified. Owners and operators of a COMS installed in accordance with the provisions of this part must check the zero and upscale (span) calibration drifts at least once daily. For a particular COMS, the acceptable range of zero andPage **18** of **161**

upscale calibration materials is defined in the applicable version of PS

– 1 in A ppendix B of this part. For a COMS, the optical surfaces, exposed to the effluent gases, must be cleaned before performing the zero and upscale drift adjustments, except for systems using automatic zero adjustments. The optical surfaces must be cleaned when the cumulat ive automatic zero compensation exceeds 4 percent opacity.
* * * * * **§60. 17**  **[Amended]** 4. By revising § 60.17(e) and (e)(1) as follows: **§ 60.17**  **Incorporations by reference.** * * * * * ( e) The following material is available for purchase from the Water Environment Federation , 2626 Pennsylvania Avenue N .W ., Washington, DC 20037. (1) Method 209A, Total Residue Dried at 103

– 105 °C, in Standard Methods for the Examination of Water and Wastewater, 20 th Edition, 1999 , IBR approved February 25, 1985 , for §60.683(b).
* * * * * **§60. 46b**  **[Amended]** 5. By revising §60.46b ( f)(1)(ii) and (h)(1) and (2) as follows: **§60.46b Compliance and performance test methods and procedures for particulate matter**  **and nitrogen oxides.**Page **19** of **161**

* * * * * (f) * * * (1) * * * (ii) Method 7E of A ppendix A of this part or Method 320 of Appendix A of Part 63 shall be used to determine the NO X concentrations. Method 3A or 3B of A ppendix A of this part shall be used to determine O 2 concentration .
* * * * * (h) * * * (1) Conduct an initial performance test as required under §60.8 over a minimum of 24 consecutive steam generating unit operating hours at maximum heat input capacity to demonstrate compliance with the NO X emission standards under §60.44b using Method 7, 7A, or 7E of A ppendix A of this part , Method 320 of Appendix A of Part 63 , or other approved reference methods; and (2) Conduct subsequent performance tests once per calendar year or every 400 hours of oper ation (whichever comes first) to demonstrate compliance with the NO X emission standards under §60.44b over a minimum of 3 consecutive steam generating unit operating hours at maximum heat input capacity using Method 7, 7A, or 7E of A ppendix A of t his part , Method 320 of Appendix A of Part 63 , or other approved reference methods.Page **20** of **161**

* * * * * **§60. 47b**  **[Amended]** 6. By revising §60.47b( b)(2)as follows: **§ 60.47b**  **Emission monitoring for sulfur dioxide** . * * * * * (b) * * * (2) Measuring SO 2 according to Method 6B of A ppendix A of this part at the inlet or outlet to the SO 2 control system. An initial stratification test is required to verify the adequacy of the sampling location for Method 6B of A ppendix A of this part . The stratification test shall consist of three paired runs of a suitable SO 2 and CO 2 measurement train operated at the candidate location and a second similar train operated according to the procedures in S ection 3.2 and the app licable procedures in S ection 7 of Performance Specification 2. Method 6B of A ppendix A of this part, Method 6A of A ppendix A of this part, or a combination of Methods 6 and 3 or 3B of A ppendix A of this part or Methods 6C or Method 320 of A ppendix A of Part 63 and 3A of A ppendix A of this part are suitable measurement techniques. If Method 6B of A ppendix A of this part is used for the second train, sampling time and timer oper ation may be adjusted for the stratification test as long as an adequate sample volume is collected; however, both sampling trains are to be operated similarly. For the location to be adequate for Method 6B of A ppendixPage **21** of **161**

A of this part , 24
- hour test s, the mean of the absolute difference between the three paired runs must be less than 10 percent.
* * * * * **§60. 51c**  **[Amended]** 7. By revising the definition of medical/infectious waste in §60.51c as follows: **§ 60.51c Definitions.** * * * Medical/infectious waste means any waste generated in the diagnosis, treatment, or immunization of human beings or animals, in research pertaining thereto, or in the production or testing of biologicals that are listed in paragraphs (1) through (7) of t his definition. The definition of medical/infectious waste does not include hazardous waste identified or listed under the regulations in part 261 of this chapter; household waste, as defined in §261.4(b)(1) of this chapter; ash from incineration of medica l/infectious waste, once the incineration process has been completed; human corpses, remains, and anatomical parts that are intended for interment or cremation ; and domestic sewage materials identified in §261.4(a)(1) of this chapter.
* * * * * **§60. 84**  **[Amended]** 8. By revising the equation in §60.84(d) as follows:Page **22** of **161**

**§60.84 Emission monitoring.** * * * * * (d) * * *

E s = (C s S )/[0.265

– ( 0. 0126 %O 2 )

– ( A %CO 2 )] * * * * * **§60.154 [Amended]** 9. By revising §60.154 (b)(5) as follows: **§60.154 Test**  **methods and procedures.** * * * * * (b) * * * (5) Samples of the sludge charged to the incinerator shall be collected in nonporous jars at the beginning of each run and at approximately 1
- hour intervals thereafter until the test ends ; and

“ 2540 G. Total, Fixed, and Volatile Solids in Solid and Semisolid Samples , in Standard Methods for the Examination of Water and Wastewater, 20th Edition, 1998 ” (incorporated by reference

— see §60.17) shall be used to determine dry sludge co ntent of each sample (total solids residue), except that:
* * * * * **§60. 284**  **[Amended]** 10. By revising the equation in §60.284(c)(3) as follows: **§ 60.284 Monitoring of emissions and operations.** * * * * *Page **23** of **161**

(c) * * * (3) * * *
C corr = C meas ×(21 − X ) /( 21 − Y ) * * * * * **§60. 335**  **[Amended]** 11. By revising two terms for the equation in paragraph §60.335(b)(1) as follows: **§60.335 Test methods and procedures.** * * * * * (b) * * * (1) * * *

P r = reference combustor inlet absolute pressure at 101.3 kilopascals ambient pressure . Alternatively, you may use 760 mm Hg (29.92 in Hg),

P o = observed combustor inlet absolute pressure at test, mm Hg . Alternatively, you may use the barometric pressure for the date of the test ,
* * * * * **§60. 374**  **[Amended]** 12. By revising §60.374(b)(1), (b)(2), and (c)(2) as follows: **§ 60.374 Test methods and procedures.** * * * * * (b) * * *Page **24** of **161**

(1) Method 12 or Method 29 shall be used to determine the lead concentration (C Pb ) and, if applicable, the volumetric flow rate (Q sda ) of the effluent gas. The sampling time and sample volume for each run shall be at least 60 minutes and 0.85 dscm (30 dscf). (2) When different operations in a three
- process operation facility are ducted to separate control devices, the lead emission concentration (C) from the facility shall be determined as follows: 

#   

#  

  

## 

    
 n

a sda n

a sda a 

## Q Q C C 1

1 

## /

W here:
C = concentration of lead emissions for the entire facility,mg/dscm (gr/dscf). C a = concentration of lead emissions from facility “a”, mg/dscm (gr/dscf). Q sda = volumetric flow rate of effluent gas from facility “a”, dscm/hr (dscf/hr). N = total number of control devices to which separate operations in the facility are ducted. * * * * * (c) * * * (2) Method 12 or Method 29 shall be used to determine the lead concentration (C Pb ) and the volumetric flow rate (Q sd ) of the effluent gas. The sampling time and sample volume for each run shall be at least 60 minutes and 0.85 dscm (30 dscf).Page **25** of **161**

* * * * * **§60. 382**  **[Amended]** 13. By revising paragraph 60.382(a)(1) as follows: **§ 60.382 Standard for particulate matter.**  * * * * * (a) * * * (1) Contain particulate matter in excess of 0.05 grams per dry standard cubic meter (0. 05 g/dscm).
* * * * * **§60.386 [Amended]** 14. By revising paragraph 60.386(b)(2) as follows: **§60.386 Test methods and procedures.** * * * * * (b) * * * (2) Method 9 and the procedures in §60.11 shall be used to determine opacity from stack emissions and process fugitive emissions. The observer shall read opacit y only when emissions are clearly identified as emanating solely from the affected facility being observed. A single visible emission observer may conduct visible emission observations for up to three fugitive, stack, or vent emission points within a 15
- se cond interval. This option is subject to the following limitations: (i) No more than three emission points are read concurrently;Page **26** of **161**

(ii) All three emission points must be within a 70o viewing sector or angle in front of the observer such that the proper sun position can be maintained for all three points; and (iii) If an opacity reading for any one of the three emission points is within 5 percent opacity of the application standard, then the observer must stop taking readings for the other two points an d continue reading just that single point. * * * * * **§60. 472**  **[Amended]**
15. By revising §60.472(a)(1)(ii) as follows: **§ 60.472 Standards for particulate matter.** * * * * * (a) * * * (1) * * * (ii) 0. 4 kg/Mg (0. 8 lb/ton) of saturated felt or smooth

- surfaced roll roofing produced;
* * * * * **§60. 660**  **[Amended]** 16. By revising §60.660 ( c )( 4) as follows: **§ 60 .660 Applicability and designation of affected facility.**  * * * * * (c) * * *Page **27** of **161**

(4) Each affected facility that has a total resource effectiveness (TRE) index value greater than 8.0 is exempt from all provisions of this subpart except for §§60.662; 60.664 ( e), (f), and ( g ); and 60.665 (h) and (l).
* * * * * **§60. 665**  **[Amended]** 17. By revising §60.665(h)(2) and (3) as f ollows: **§ 60.665 Reporting and recordkeeping requirements.** * * * * * (h) * * * (2) Any recalculation of the TRE index value performed pursuant to §60.664( g ); and (3) The results of any performance test performed pursuant to the methods and procedures required by §60.664( e ).
* * * * * 18. By revising Table 7 in the appendix to Subpart IIII as follows: **Subpart IIII**  **— Standards of Performance for Stationary Compression**  **Ignition Internal Combustion Engines** *** * * * ***Page **28** of **161**

**Table 7 to Subpart IIII of Part 60**  **— Requirements for Performance Tests for**  **Stationary CI ICE With a Displacement of ≥30 Liters per Cylinder**  [As stated in §60.4213, you must comply with the following requirements for performance tests

for stationary CI ICE with a displacement of ≥30 liters per cylinder:]

**E ach**  **Complying**

**with the requirement**  **to You must**  **Using According to the**  **following requirements** 

1. Stationary CI internal combustion engine with a displacement of ≥30 liters per cylinder a. Reduce

NO X emissions by 90 percent or more i. Measure NO X at

the centroid of the exhaust at the inlet and outlet of the control device ; (1) Method 7E

of 40 CFR part 60, A ppendix A, Method 320 of 40 CFR part 63, appendix A , or ASTM D 6348

– 03 (incorporated b y reference, see §60.17) (a) NO X concentration

must be at 15 percent O 2 , dry basis. Results of this test consist of the average of the three 1
- hour or longer runs.

ii. Measure O 2 at the inlet and outlet of the control device; and, (2) Method 3,

3A, or 3B of 40 CFR P art 60, A ppendix A (b) Measurements

to determine O 2 concentration must be made at the same time as the measurements for NO X concentration.

iii. If necessary, measure moisture content at the inlet and outlet of the control device . (3) Method 4

of 40 CFR P art 60, A ppendix A, Method 320 of 40 CFR Part 63, A ppendix A, or ASTM D 6348

– 03 (incorporated by reference, see §60.17) (c) Measurements

to determine moisture content must be made at the same time as the measurements for NO X concentration.

b. L imit the concentration of i . Measure NO X

at the centroid of ( 1 ) Method 7E

of 40 CFR P art (a) If using a control

device, the sampling sitePage **29** of **161** NO X in the stationary CI internal combustion engine exhaust. the exhaust of the

stationary internal combustion engine ; 60, A ppendix

A, Method 320 of 40 CFR P art 63, A ppendix A, or ASTM D 6348

– 03 (incorporated by reference, see §60.17) must be located at the

outlet of the control device. NO X concentration must be at 15 percent O 2 , dry basis. Results of this test consist of the average of the three 1
- hour or longer runs. ii. Determine the O 2 concentration of the stationary internal combustion engine exhaust at the sampling port location; and, (2) Method 3,

3 A, or 3B of 40 CFR P art 60, A ppendix A (b) Measurements

to determine O 2 concentration must be made at the same time as the measurement for NO X concentration.

iii. If necessary, measure moisture content of the stationary internal combustion engine exhaust at the sampling port location . (3) Method 4

of 40 CFR P art 60, A ppendix A, Method 320 of 40 CFR P art 63, A ppendix A, or ASTM D 6348

– 03 (incorporated by reference, see §60.17) (c) Measurements

to determine moisture content must be made at the same time as the measurement for NO X concentration.

c. Reduce PM emissions by 60 percent or more i. Select the

sampling port location and the number of traverse points; (1) Method 1

or 1A of 40 CFR Part 60, A ppendix A (a) Sampling sites

must be located at the inlet and outlet of the control device.
ii. Measure O 2 at the inlet and (2) Method 3,

3A, or 3B of (b) Measurements

to determine O 2Page **30** of **161** outlet of the control device; 40 CFR P art

60, A ppendix A concentration must be

made at the same time as the measurements for PM concentration. iii. If necessar y, measure moisture content at the inlet and outlet of the control device; and (3) Method 4

of 40 CFR P art 60, A ppendix A (c) Measurements

to determine and moisture content must be made at the same time as the measurements for PM concentration.

iv. Measure PM at the inlet and outlet of the control device (4) Method 5

of 40 CFR P art 60, appendix A (d) PM

concentration must be at 15 percent O 2 , dry basis. Results of this test consist of the average of the three 1
- hour or longer runs. d. Limit the concentration of PM in the stationary CI internal combustion engine exhaust i. Select the

sampling port location and the number of traverse points; (1) Method 1

or 1A of 40 CFR P art 60, A ppendix A (a) If using a

c ontrol device, the sampling site must be located at the outlet of the control device.
ii. Determine the O 2 concentration of the stationary internal combustion engine exhaust at the sampling port location; and (2) Method 3,

3A, or 3B of 40 CFR Part 60, A ppendix A (b) Measurements

to determine O 2 concentration must be made at the same time as the measurements for PM concentration.Page **31** of **161** iii. If necessary, measure moisture content of the stationary internal combustion engine exhaust at the sampling port location; (3) Method 4

of 40 CFR P art 60, A ppendix A (c) Measurements

to determine moisture content must be made at the same time as the measurements for PM concentration.

iv. Measure PM at the exhaust of the stationary internal combustion engine . (4) Method 5

of 40 CFR P art 60, A ppendix A (d) PM

concentration must be at 15 percent O 2 , dry basis. Results of this test consist of the average of the three 1
- hour or longer runs.
19. By revising Table 2 in the appendix to Subpart JJJJ as follows: **Subpart JJJJ** 

**— Standards of Performance for Stationary Spark Ignition**  **Internal Combustion Engines** *** * * * ***Page **32** of **161**

**Table 2 to Subpart JJJJ of Part 60 —**  **Requirements for Performance Tests** [As stated in §60.4244, you must comply with the following requirements for performance tests

within 10 percent of 100 percent peak (or the highest achievable) load]

**For each Complying with**  **the requirement to**  **You must Using**  **According to the**  **following requirements**  1. Stationary SI internal combustion engine demonstrating compliance according to §60.4244. a. limit the

concentration of NO X in the stationary SI internal combustion engine exhaust. i. Measure NO X at

the centroid of the exhaust of the stationary internal combustion engine; (1) Method 7E of

40 CFR P art 60, A ppendix A , Method D6522

– 00(2005) a , Method 320 of 40 CFR P art 63, A ppendix A, or ASTM D6348

– 03 (incorporated b y reference, see §60.17). (a) If using a control device, the sampling site must be located at the outlet of the control device. Results of this test consist of the average of the three 1
- hour or longer runs. ii. Determine the O 2 concentration of the stationary internal combustion engine exhaust ; (2) Method 3, 3A, or

3B b of 40 CFR P art 60, A ppendix A or ASTM Method D6522

– 00(2005) a (b)

M easurements to d etermine O 2 concentration must be made at the same time as the measurements for NO X concentration. iii. Determine the exhaust flow rate of the stationary internal combustion engine exhaust; and (3) Method 2 or 19 of

40 CFR P art 60.Page **33** of **161** iv. I f necessary , measure moisture content of the stationary internal combustion engine exhaust at the sampling port location
. (4) Method 4 of 40 CFR

P art 60, A ppendix A, Method 320 of 40 CFR P art 63, A ppendix A, or ASTM D6348

– 03 (incorporated b y reference, see §60.17). (c)

Measurements to determine moisture must be made at the same time as the measurement for NO X concentration. b. limit the concentration of CO in the stationary SI internal combustion engine exhaust
. i. Sample for CO

at the centroid of the stack of the stationary internal combustion engine; . ( 1 ) Method 10 of 40

CFR P art 60, A ppendix A, ASTM Method D6522

– 00(2005) a , Method 320 of 40 CFR Part 63, A ppendix A, or ASTM D 6348

– 03 (incorporated b y reference, see §60.17). (a) If using a

control device, the sampling site must be located at the outlet of the control device. Results of this test consist of the average of the three 1
- hour or longer runs
. ii. Determine the O 2 concentration of the stationary internal combustion engine exhaust at the sampling port location; . (2) Method 3, 3A, or

3Bb of 40 CF R Part 60, A ppendix A or ASTM Method D6522

– 00(2005) a

. (b)

Measurements to determine O 2 concentration must be made at the same time as the measurements for CO concentration
. iii. Determine the exhaust flow rate of the stationary internal combustion engine exhaust; and, (3) Method 2 or 19 of

40 CFR P art 60.Page **34** of **161** iv. I f necessary , measure moisture content of the stationary internal combustion engine exhaust at the sampling port location
. . (4) Method 4 of 40

CFR Part 60, A ppendix A, Method 320 of 40 CFR Part 63, A ppendix A, or ASTM D6348

– 03 (incorporated b y reference, see §60.17). (c)

Measurements to determine moisture must be made at the same time as the measurement for CO concentration
. c. limit the concentration of VOC in the stationary SI internal combustion engine exhaust
. i. Measure VOC at

the centroid of the exhaust of the stationary internal combustion engine ; . ( 1 ) Methods 25A and

18 of 40 CFR Part 60, A ppendix A, Method 25A with the use of a methane cutter as described in 40 CFR 1065.265, Method 18 or 40 CFR Part 60, A ppendix A, cd Method 320 of 40 CFR part 63, A ppendix A, or ASTM D6348

– 03 (incorporated b y reference, see §60.17). (a) If using a

control device, the sampling site must be located at the outlet of the control device. Results of this test consist o f the average of the three 1
- hour or longer runs
.

ii. Determine the O 2 concentration of the stationary internal combustion engine exhaust at the sampling port location; . (2) Method 3, 3A, or

3B b of 40 CFR Part 60, A ppendix A or ASTM Method D6 522

– 00(2005) a

. (b)

Measurements to determine O 2 concentration must be made at the same time as the measurements for VOC concentration
. iii. Determine the exhaust flow rate of the stationary internal combustion engine (3) Method 2 or 19 of

40 CFR part 60.Page **35** of **161** exhaust; and iv. I f necessary , measure moisture content of the stationary internal combustion engine exhaus t at the sampling por t location. . (4) Method 4 of 40

CFR Part 60, A p pendix A, Method 320 of 40 CFR Part 63, A ppendix A, or ASTM D6348

– 03 (incorporated b y reference, see §60.17). (c)

Measurements to determine moisture must be made at the same time as the measurement for VOC conce ntration

a ASTM D6522

– 00 is incorporated by reference; see 40 CFR 60.17. Also, you may petition the Administrator for approval to use alternative methods for portable analyzer.
b You may use ASME PTC 19.10

– 1981, Flue and Exhaust Gas Analyses, for measuring the O 2 content of the exhaust gas as an alternative to EPA Method 3 B.

c You may use EPA Method 18 of 40 CFR part 60, appendix A, provided that you conduct an adequate presurvey test prior to the emissions test, such as the one described in OTM 11 on EPA's Web site ( http://www.epa.gov/ttn/emc/prelim/otm11.pdf ).
d You may u se ASTM D6420

– 99 (2004), Test Method for Determination of Gaseous Organic Compounds by Direct Interface Gas Chromatography/Mass Spectrometry as an alternative to EPA Method 18 for measuring total nonmethane organic.
* * * * * 20. In Method 1 of Appendix A - 1 by revising Sections 11.2.2, 11.4.1, and Figures 1
- 1 and 1
- 2 as follows: **Method 1 –**  **Sample and Velocity Traverses f**  **rom Stationary Sources**
* * * * * 11.2.2 Velocity and Gaseous (Non
- Particulate) Traverses.
Perform a stratification test to determine the appropriate number of sample traverse points. If testing for multiple pollutants or diluents at the same site, a stratification test using only one pollutant or diluen t satisfies this requirement. A stratificationPage **36** of **161**

test is not required for small stacks that are less than 4 inches in diameter. When the 8
- and 2
- diameter criterion can be met, the minimum number of tra verse points for the stratification test will be 12. T est for stratification us ing a probe of appropriate length to measure the gas concentration at the required traverse points located according to Table 1

– 2. Alternatively (if the 8
- and 2
- diameter criter ion is met) , you may measure the gas concentration at three points on a line passing through the centroidal area. Space the three points at 16.7, 50.0, and 83.3 percent of the measurement line. Sample for a minimum of twi ce the system response time at each traverse point. Calculate the individual point and mean concentrations. If the concentration at each traverse point differs from the mean concentration for all traverse points by no more than: (a) ± 5.0 percent of the me an concentration; or (b) ± 0.5 ppm (whichever is less restrictive), the gas stream is considered unstratified and you may collect samples from a single point that most closely matches the mean. If the 5.0 percent or 0.5 ppm criterion is not met, but the co ncentration at each traverse point differs from the mean concentration for all traverse points by no more than: (a) ± 10.0 percent of the mean; or (b) ± 1.0 ppm (whichever is less restrictive), the gas stream is considered to be minimally stratified, and y ou may take samples from three points. Space the three points at 16.7, 50.0, and 83.3 percent of the measurement line. Alternatively, if a 12
- point stratification test was performed and the emissions were shown to be minimally stratifiedPage **37** of **161**

(all points within ± 10.0 percent of their mean or within ± 1 .0 ppm), and if the stack diameter (or equivalent diameter, for a rectangular stack or duct) is greater than 2.4 meters (7.8 ft), then you may use 3
- point sampling and locate the three poi nts along the measurement line exhibiting the highest average concentration during the stratification test at 0.4, 1. 0 and 2.0 meters from the stack or duct wall. If the gas stream is found to be stratified because the 10.0 percent or 1.0 ppm criterion fo r a 3
- point test is not met, locate 12 traverse points for the test in accordance with Table 1

– 2 .
* * * * *
11.4.1 In most stationary sources, the direction of stack gas flow is essentially parallel to the stack walls. However, cyclonic flow may exist (1) after such devices as cyclones and inertial demisters following venturi scrubbers, or (2) in stacks having tangential inlets or other duct configurations which tend to induce swirling . Determine the presence or absence of cyclonic flow at each sampling location . The following techniques are acceptable for this determination.
* * * * *Page **38** of **161**Page **39** of **161**

* * * * * 21. In Method 2 of Appendix A
- 1 by revising S ection s 8.1, 10.4, 12.6, and 12.7, by revising the note at the end of 10.1.1 , and by adding a term to Section 12.1 as follows: **Method 2 —**  **Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S Pitot Tube)**  * * * * *
8.1 Set up the apparatus as shown in Figure 2
- 1. Capillary tubing or surge tanks installed between the manometer and pitot tube may be used to dampen ΔP fluctuations. It is recommended, but not required, that a pretest leak
- check be conducted as follows: (1) blow through the pitot impact opening un til at least 7.6 cm (3.0 in.) H 2 O velocity head registers on the manometer; then, close off the impact opening. The pressure shall remain stable (±2.5 mm H 2 O, ±0.10 in. H 2 O) for at least 15 seconds; (2) do the same for the static pressure side, except usin g suction to obtain the minimum of 7.6 cm (3.0 in.) H 2 O. Other leak
- check procedures, subject to the approval of the Administrator, may be used.
* * * * * 10.1.1 * * * Note: Do not use a Type S pitot tube assembly that is constructed such that the impact pressure opening plane of the pitot tube is below the entry plane of the nozzle (see Figure 2

– 7B ).Page **40** of **161**

* * * * *
10.4 Barometer. Calibrate the barometer used against a mercury barometer or NIST - traceable barometer prior to each field test .
* * * * * 12.1 Nomenclature * * * T s(abavg) – Average absolute stack temperature, °K (°R). * * * * *
12.6 Average Stack Gas Velocity.

= ∑ ∆ ( )

. 2
− 7 Where:
K p = Metric O H mm K Hg mm mole g g m o 2 / 1

2 ) )( ( ) )( / ( sec 97
. 34      


English

O H in R Hg in mole lb lb ft
o 2 / 1

2 )
. )( ( )

. )( / ( sec 49
. 85      

 

12.7 Average Stack Gas Dry Volumetric Flow Rate.

Q = 3600 ( 1
− B ) ( ) . 2
− 8
* * * * * 22. In Method 2A of Appendix A
- 1 by revising Section s 10.3 and 12.2 as follows: **Method 2A —**  **Direct Measurement of Gas Volume Through Pipes and Small**  **Ducts**Page **41** of **161**

* * * * *
10.3 Barometer. Calibrate the barometer used against a mercury barometer or NIST - traceable barometer prior to the field test.
* * * * *
12.2 Test Meter Calibration Coefficient. 1 2
. / ) )( ( /

) ( ) ( ) (

     A Eq T P P V V T

P V V Y abs m g b mi mf abs r b ri rf m * * * * * 23. In Method 2B of Appendix A
- 1 by revising Section 12.1 as follows: **Method 2B –**  **Determination of Exhaust Gas Volume Flow Rate from Gasoline Vapor Incinerators**  * * * * *
12.1 Nomenclature. C O e = Mean carbon monoxide concentration in system exhaust, ppm. (CO 2 ) a = Ambient carbon dioxide concentration, ppm (if not measured during the test period, may be assumed to equal 3 80 ppm). (CO 2 ) e = Mean carbon dioxide concentration in system exhaust, ppm.Page **42** of **161**

HC e = Mean organic concentration in system exhaust as defined by the calibration gas, ppm.

Hc i = Mean organic concentration in system inlet as defined by the calibration gas, ppm.

K e = Hydrocarbon calibration gas factor for the exhaust hydrocarbon analy zer, unitless [equal to the number of carbon atoms per molecule of the gas used to calibrate the analyzer (2 for ethane, 3 for propane, etc.)].

K i = Hydrocarbon calibration gas factor for the inlet hydrocarbon analyzer, unitless.

V es = Exhaust gas volume, m 3
. V is = Inlet gas volume, m 3
. Q es = Exhaust gas volume flow rate, m 3 /min. Q is = Inlet gas volume flow rate, m 3 /min. Θ = Sample run time, min. S = Standard conditions: 20 °C, 760 mm Hg. * * * * * 24. In Method 2D of Appendix A
- 1 by revising Section 10.4 as follows: **Method 2D —**  **Measurement of Gas Volume Flow Rates in Small Pipes and Ducts**  * * * * *Page **43** of **161**

10.4 Barometer. Calibrate the barometer used against a mercury barometer o r NIST - traceable barometer prior to the field test.
* * * * * 2 5 . In Method 3A of Appendix A
- 2 by revising Section 7.1 as follows: **Method 3A –**  **Determination of Oxygen and Carbon Dioxide Concentrations in Emissions From Stationary Sources (Instrumental**  **Analyzer Procedure)**  * * * * *
7.1 Calibration Gas. What calibration gases do I need? Refer to Section 7.1 of Method 7E for the calibration gas requirements. Example calibration gas mixtures are listed below. Pre - cleaned or scrubbed air may be used for the O 2 high
- calibration gas provided it does not contain other gases that interfere with the O 2 measurement . (a) CO 2 in Nitrogen (N 2 ). (b) CO 2 in air. (c) CO 2 / SO 2 gas mixture in N 2 . (d) O 2 / SO 2 gas mixture in N 2 . (e) O 2 /CO 2 / SO 2 gas mixture in N 2 . (f) CO 2 /NO x gas mixture in N 2 . (g) CO 2 /SO 2 /NO x gas mixture in N 2 .Page **44** of **161**

The tests for analyzer calibration error and system bias require high
- , mid
- , and low
- level gases.
* * * * * 26. In Method 4 of Appendix A
- 3 by revising Section s 9.1 and 16 as follows: **Method 4 —**  **Determination of M**  **oisture C**  **ontent in S**  **tack G**  **ases** * * * * *
9.1 Miscellaneous Quality Control Measures.

**Section Quality control measure**  **Effect** Section 8.1.1.4 Leak rate of the sampling system

cannot exceed four percent of the average sampling rate or 0.00057 m 3 /min (0. 0 20 cfm) Ensures the accuracy of the volume of gas sampled. (Reference Method) Section 8.2.1 Leak rate of the sampling system

cannot exceed two percent of the average sampling rate Ensures the accuracy of the volume of gas sampled. (Approximation Method)
* * * * * 16.0 Alternative Procedures 16.1 The procedure described in Method 5 for determining moisture content is an acceptable alternative to Method 4 . 16.2 The procedures in Method 6A for determining moisture is an acceptable alternative to Method 4 . 16.3 Method 320 is an acceptable alternative to Method 4 for determining moisture .Page **45** of **161**

16.4 Using F
- factors to determine moisture is an acceptable alternative to Method 4 . For a combustion stack not using a scrubber, the moisture content may be calculated as follows:

= + +
Where:

B A = Mole fraction of moisture in the ambient air.

= % 100 [ 10 [
. (

. ) ]

B F = Mole fraction of moisture from free water in the fuel.

= 0
. 0036 + 0
. 075

100 [ 20
. 9
−

20
. 9 ]

B H = Mole fraction of moisture from the hydrogen in the fuel.



##   9
. 20 9
. 20 1 2

O F F B
w

d H 

       

 

B ws = Mole fraction of moisture in the stack gas. F d = Volume of dry combustion components per unit of heat content at 0 percent oxygen, dscf/10 6 Btu (scm/J). See Table 19

- 2 in Method 19.Page **46** of **161**

F W = Volume of wet combustion components per unit of heat content at 0 percent oxygen, wet scf/10 6 Btu (scm/J). See Ta ble 19
- 2 in Method 19. %RH = Percent relative humidity (calibrated hydrometer acceptable), percent. P Bar = Barometric pressure, in. Hg (mm Hg). T = Ambient temperature, oF (oC). W = Percent free water by weight, percent. O 2 = Percent oxygen in stack gas, dry basis, percent . * * * * * 27. In Method 5 of Appendix A
- 3 by deleting Section 7.1.5 and by revising S ection s 6.1.1.5, 6.1.1.7, 6.1.1.9, 7.1.3, 8.1, 8.3.4, 8.7.3, 8.7.5, 10.3.3, 10.4, 10. 5, 10.6 , Equation 5
- 13 in Section 16.2.3.3, Section 16.3, and by adding Section 16.3 and reference 13 to Section 17.0 as follows: **Method 5 —**  **Determination of Particulate Matter Emissions From Stationary Sources**  * * * * *
6.1.1.5 Filter Holder. Borosilicate glass, with a glas s frit filter support and a silicone rubber gasket. Alternatively, Teflon filter holders may be used. Other materials of construction ( e.g., stainless steel or Viton) may be used, subject to the approval of the Administrator. The holder design shall provide a positive seal against leakage from the outside or around the filter. The holderPage **47** of **161**

shall be attached immediately at the outlet of the probe (or cyclone, if used).
* * * * *
6.1.1.7 Temperature Sensor. A calibrated temperature sensor (rechecked at at least one point after each test ) shall be installed so that the sensing tip of the temperature sensor i s in direct contact with the sample gas, and the temperature around the filter holder can be regulated and monitored during sampling.
* * * * *
6.1.1.9 Metering System. Vacuum gauge, leak
- free pump, calibrated temperature sensors (rechecked at at least on e point after each test ), dry gas meter (DGM) capable of measuring volume to within 2 percent, and related equipment, as shown in Figure 5

– 1. Alternatively, an Isostack metering system may be used if all Method 5 calibrations are performed, with the exception of those related to ∆H@ in Section 9.2.1, wherein the sample flow rate system shall be calibrated in lieu of ∆H@ and shall not deviate by more than 5 percent. Other metering systems capable of mai ntaining sampling rates within 10 percent of isokinetic and of determining sample volumes to within 2 percent may be used, subject to the approval of the Administrator. When the metering system is used in conjunction with a pitot tube, the system shall all ow periodic checks of isokinetic rates.Page **48** of **161**

* * * * *
7.1.3 Water. When analysis of the material caught in the impingers is required, deionized distilled water (to conform to ASTM D 1193

– 77 or 91 Type 3 (incorporated by reference

— see §60.17)) with ≤0.001 perc ent residue shall be used. Run blanks prior to field use to eliminate a high blank on test samples , and use only water with low blank values ( ≤0.001 percent).
* * * * *
8.1 Pretest Preparation. It is suggested that sampling equipmen t be maintained according to the procedures described in APTD - 0576. Alternative mercury
- free thermometers may be used if the thermometers are at a minimum equivalent in terms of performance or suitably effective for the specific temperature measurement app lication .
* * * * *
8.3.4 Set up the train as shown in Figure 5

– 1 ensuring that the connections are leak
- tight. Subject to the approval of the Administrator, a glass cyclone may be used between the probe and filter holder when the total particulate catch is expected to exceed 100 mg or when water droplets are pres ent in the stack gas.
* * * * *Page **49** of **161**

8.7.3 Before moving the sample train to the cleanup site, remove the probe from the sample train and cap the open outlet of the probe. Be careful not to lose any condensate that might be prese nt. Cap the filter inlet where the probe was fastened . Remove the umbilical cord from the last impinger, and cap the impinger. If a flexible line is used between the first impinger or condenser and the filter h older, disconnect the line at the filter holder, and let any condensed water or liquid drain into the impingers or condenser. C ap off the filter holder outlet and impinger inlet. Either ground
- glass stoppers, plast ic caps, or serum caps may be used to close these openings.
* * * * *
8.7.5 Save a portion of the acetone used for cleanup as a blank. For each container of acetone used for cleanup, save 200 ml and place it i n a glass sample container labeled “acetone blank.” To minimize any particulate contamination, rinse the wash bottle prior to filling from the tested container. Take 200 ml of this acetone directly from the wash bottle being used, and place it in a glass
sa mple container labeled “acetone blank.”
* * * * *
10.3.3 Acceptable Variation in Calibration Check . If the DGM coefficient values obtained before and after a test series differ by more than 5 percent, the test series shall either be voided, orPage **50** of **161**

calculation s for the test series shall be performed using whichever meter coefficient value ( i.e., before or after) gives the lower value of total sample volume.
* * * * *
10.4 Probe Heater Calibration. Use a heat source to generate air heated to selected temperatu res that approximate those expected to occur in the sources to be sampled. Pass this air through the probe at a typical sample flow rate while measuring the probe inlet and outlet temperatures at various probe heater settings. For each air temperature gene rated, construct a graph of probe heating system setting versus probe outlet temperature. The procedure outlined in APTD

– 0576 can also be used. Probes constructed according to APTD

– 0581 need not be calibrated if the calibration curves in APTD

– 0576 are used . Also, probes with outlet temperature monitoring capabilities do not require calibration. As an a lternative, the following single
point calibration procedure may be used. After each test run series, check the accuracy (and, hence, the calibration) of each thermocouple system at ambient temperature, or any other temperature, within the range specified by the manufacture r , using a reference thermometer (either ASTM reference thermometer or a thermometer that has been calibrated against an ASTM reference ther mometer). The temperatures of the thermocouple and reference thermometers shall agree to within ±2 o F. NOTE : The probe heating system shall be calibrated before its initial use in the field.Page **51** of **161**

10.5 Temperature Sensors. Use the procedure in Section 10.3 of Method 2 to calibrate in
- stack temperature sensors. Dial thermometers, such as are used for the DGM and condenser outlet, shall be calibrated against mercury
- in
- glass thermometers. An alternative mercury
- free NIST
- traceable thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
10.6 Barometer. Calibrat e against a mercury barometer or NIST traceable barometer prior to the field test. Alternatively, barometric pressure may be obtained from a weather report that has been adjusted for the test point (on the stack) elevation .
* * * * * 16.2.3.3 * * *

( ) = ′ Eq. 5
- 13 * * * * * 16.3 Alternative Post
- Test Metering System Calibration. The following procedure may be used as an alternative to the post
- test calibration described in Section 10.3.2. This alternative procedure does not detect leakages between the inlet of the metering system and the dry gas meter. Therefore, two steps must be included to make it an equivalent alternative : 1) The metering system must pass the post
test leak
- check from either the inlet of the samp ling train or thePage **52** of **161**

inlet of the metering system. Therefore, if the train fails the former leak
- check, another leak
- check from the inlet of the metering system must be conducted ; 2) The metering system must pass the leak
check of that portion of the train fr om the pump to the orifice meter as described in Section 10.3.1.1. 16.3.1 After each test run, do the following: 16.3.1.1 Ensure that the metering system has passed the post
test leak
- check. If not, conduct a leak
- check of the metering system from its in let. 16.3.1.2 Conduct the leak
- check of that portion of the train from the pump to the orifice meter as described in Section 10.3.1.1. 16.3.1.3 Calculate Y qa for each test run using the following equation:

= .

∆ @ ∆

. √ ∆ Eq. 5
- 15

Where: Y qa = Dry gas meter calibration check value, dimensionless. 0.0319 = (29.92/528)(0.75) 2 (in. Hg/  R) cfm 2

. ∆ H@ = Orifice meter calibration coefficient, in. H 2 O . M d = Dry molecular weight of stack gas, lb/lb

- mole . 29 = Dry molecular weight of air, lb/lb

- mole . 16.3.2 After each test run series, do the following:Page **53** of **161**

1 6 .3.2.1 Average the three or more Y qa ’s obtained from the test run series and compare this average Y qa with the dry gas meter calibration factor Y. The average Y qa must be within 5 percent of Y. 16.3.2.2 If the average Y qa does not meet the 5 percent criterion, recalibrate the meter over the full range of orifice settings as detailed in Section 10.3.1. Th en follow the procedure in Section 10.3.3. * * * * * 17.0 References. * * * 13. Shigehara, Roger T., P.G. Royals, and E.W. Steward. “Alternative Method 5 Post
- Test Calibration.” Entropy Incorporated, Research Triangle Park, NC 27709. * * * * * 28. In Method 5A of Appendix A
- 3 by revising S ection 8.1 as follows: **Method 5 A**  **— Determination of Particulate Matter Emissions From the**  **Asphalt Processing and Asphalt Roofing Industry**  * * * * *
8.1 Pretest Preparation. Unless otherwise specified, maintain and calibrate all components according to the procedure described in APTD - 0576, “Maintenance, Calibration, and Operation of Isokinetic Source - Sampling Equipment” (Reference 3 in Method 5, Section 17.0). Alternative mercury
- free thermometers may be used if the thermometersPage **54** of **161**

are, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * * 29. In Method 5E of Appendix A
- 3 by r edesignat ing S ection 16 as 17 , S ection 17 a s 18 , and by adding a new Section 16 as follows: **Method 5E —**  **Determination of Particulate Matter Emissions From the Wool Fiberglass Insulation Manufacturing Industry**  * * * * *
16.0 Alternative Procedures
16.1 Total Organic Carbon Analyzer. Tekmar
- Dohrmann analyzers using the single injection technique may be used as an alternative to Rosemount Model 2100A analyzers. * * * * * 30. In Method 5H of Appendix A
- 3 by revising Section 12.1, adding Section 12.15, r edesignat ing S ection 16 as 17 and Section 17 as 18, and adding a new S ection 16 as follows: **Method 5H –**  **Determination of P**  **articulate Matter E**  **missions F**  **rom W**  **ood H**  **eaters F**  **rom a S**  **tack L**  **ocation** * * * * *
12.1 Nomenclature.

A = Sample flow rate adjustment factor.Page **55** of **161**

BR = Dry wood burn rate, kg/hr (lb/hr), from Method 28, Section 8.3.

B ws = Water vapor in the gas stream, proportion by volume.
C i = Tracer gas concentration at inlet, ppmv. C o = Tracer gas concentration at outlet, ppmv.
C s = Concentration of particulate matter in stack gas, dry basis, corrected to standard conditions, g/dscm (g/dscf).

E = Particulate emission rate, g/hr (lb/hr).

ΔH = Average pressure differential across the orifice meter (see Figure 5H

– 1), mm H 2 O (in. H 2 O).

L a = Maximum acceptable leakage rate for either a post
- test leak
check or for a leak
- check following a component change; equal to 0.00057 cmm (0.020 cfm) or 4 percent of the average sampling rate, whichever is less.

L 1 = Individual leakage rate observed during the leak
- check conducted before a component change, cmm (cfm).

L p = Leakage rate observed during the post
- test leak
- check, cmm (cfm).

m n = Total amount of particulate matter collected, mg.

M a = Mass of residue of solvent after evaporation, mg.Page **56** of **161**

N C = Grams of carbon/gram of dry fuel (lb/lb), equal to 0.0425.

N T = Total dry moles of exhaust gas/kg of dry wood burned, g

moles/kg (lb

- moles/lb).

PR = Percent of proportional sampling rate.

P bar = Barometric pressure at the sampling site, mm Hg (in.H g).

P std = Standard absolute pressure, 760 mm Hg (29.92 in.Hg).
Q i = Gas volumetric flow rate at inlet, cfm ( l / m in ).
Q o = Gas volumetric flow rate at outlet, cfm ( l / m in). * * * * * 12.15 Alternative Tracer Gas Flow Rate Determination .

= ×

. 5
− 10

Note: This gives Q for a single instan ce only. Repeated multiple determinations are needed to track temporal variations. Very small variations in Q i, C i , or C o may give very large variations in Q o . * * * * * **16.0 Alternative Procedures** 16.1 Alternative Stack Gas Volumetric Flow Rate Determination (Tracer Gas) . 16.1.1 Apparatus.Page **57** of **161**

16.1.1.1 Tracer Gas Injector System. This is t o inject a known concentration of tracer gas into the stack. This system consists of a cylinder of tracer gas, a gas cylinder regulator, a stainless steel needle valve or a flow controller, a nonreactive (stainless steel or glass) rotameter, and an injection loop to disperse the tracer gas evenly in the stack. 16.1.1.2 Tracer Gas Probe. A glass or stainless steel sampling probe. 16.1.1.3 Gas Conditioning System. A gas conditioning is a
s ystem suitable for delivering a cleaned sample to the analyzer consisting of a filter to remove partic ulate and a condenser capable of lowering the dew point of the sample gas to less than 5  C (40  F). A desiccant such as anhydrous calcium sulfate may be used to dry the sample gas. Desiccants which react or absorb tracer gas or stack gas may not be used, e. g. silica gel absorbs CO 2 . 16.1.1.4. Pump. An inert (i.e., stainless steel or Teflon head) pump to deliver more than the total sample required by the manufacturer’s specifications for the analyzer used to measure the downstream tracer gas concentration. 16.1.1.5 Gas Analyzer. A gas analyzer is a ny analyzer capable of measuring the tracer gas concentration in the range necessary at least every 10 minutes. A means of controlling the analyzer flow rate and a device for determining proper sample flow rate s hall be provided unless data is provided to show that the analyzer is insensitive to flow variations over the range encountered during thePage **58** of **161**

test. The gas analyzer needs to meet or exceed the flowing performance specifications: Linearity ± 1 percent of full scale Calibration Error ≤ 2 percent of span Response Time ≤ 10 seconds Zero Drift (24 hour) ≤ 2 percent of full scale Span Drift (24 hour) ≤ 2 percent of full scale Resolution ≤ 0.5 percent of span
16.1.1.6 Recorder (optional). To provide a permanent record of the analyzer output. 16.1.2 Reagents. 16.1.2.1 Tracer Gas. The tracer gas is s ulfur hexafluoride in an appropriate concentration for accurate analyzer measurement or pure sulfur dioxide. The gas used must be nonreactive with the stack effluent and give minimal (<3 percent) interference to measurement by the gas analyzer. 16.1.3 Procedure. Select upstream and downstream locations in the stack or duct for introducing the tracer gas and delivering the sampled gas to the analyzer. The inlet location should be 8 or more duct diameters beyond any upstream flow disturbance. The outlet should be 8 or more undisturbed duct diameters from the inlet and 2 or more duct diameters from the duct exit. After installing the apparatus, meter a known conce ntration of the tracer gas into the stack at the inlet location. Use the gas sample probe and analyzer toPage **59** of **161**

show that no stratification of the tracer gas is found in the stack at the measurement locations. Monitor the tracer gas concentration from the outlet location and record the concentration at 10
- minute intervals or more often at the option of the tester. A minimum of three measured intervals is recommended to determine the stack gas volumetric flow rate. Other statistical procedures may be applied for
c omplete flow characterization and additional QA/QC. * * * * * 31. In Method 6 of Appendix A
- 4 by revising Section s 10.2 and 10.4 as follows: **Method 6 —**  **Determination of Sulfur Dioxide Emissions From Stationary Sources**  * * * * *
10.2 Temperature Sensors. Calibrate against mercury
- in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * *
10.4 Barometer. Calibrate against a mercury barometer or NIST traceable barometer prior to the field test .
* * * * *Page **60** of **161**

32. In Method 6C of Appendix A
- 4 by revising S ection s 4.0 and 8.3 as follows: **Method 6C —**  **Determination of Sulfur Dioxide Emissions From Stationary Sources (Instrumental Analyzer Procedure)**  * * * * * 4.0 Interferences Refer to Section 4. 0 of Method 7E . * * * * *
8.3 Interference Check. You must follow the procedures of Section 8.2.7 of Method 7E to conduct an interference check, substituting SO 2 for NO X as the method pollutant. For dilution
- type measurement systems, you must use the alternative interferenc e check procedure in Section 16 and a co
- located, unmodified Method 6 sampling train. Quenching in f luorescence analyzers must be evaluated and remedied unless a dilution system and ambient
- level analyzer is used. This may be done by prepar ing the calibration gas to contain within 1 percent of the absolute oxygen and carbon dioxide content of the measured gas , preparing the calibration gas in air and using vendor nomographs , or by other acceptable means.
* * * * * 33. In Method 7 of Appendix A
- 4 by revising S ection s 4.0, 10.2, and 10.3 as follows: **Method 7 —**  **Determination of Nitrogen Oxide Emissions From Stationary Sources** Page **61** of **161**

* * * * *
4.0 Interferences Biased results have been observed when sampling under conditions of high sulfur dioxide concentrations . At or above 2100 ppm SO 2 , use five times the H 2 O 2 concentration of the Method 7 absorbing solution. Laboratory tests have shown that high concentrations of SO 2 (about 2100 ppm) cause low results in Method 7 and 7A. Increasing the H 2 O 2 conce ntration to five times the original concentration eliminates this bias. However, when no SO 2 is present, increasing the concentration by five times results in a low bias.
* * * * *
10.2 Barometer. Calibrate against a mercury barometer or NIST traceable barometer prior to the field test . 10.3 Temperature Gauge. Calibrate dial thermometers against mercury - in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * * 34. In Method 7A of Appendix A
- 4 by revising S ect ions 4.0 and 10.4 as follows:Page **62** of **161**

**Method 7A –**  **Determination of N**  **itrogen O**  **xide E**  **missions F**  **rom S**  **tationary S**  **ources (Ion Chromatographic Method)** * * * * *
4.0 Interferences Biased results have been observed when sampling under conditions of high sulfur dioxide concentrations . At or above 2100 ppm SO 2 , use five times the H 2 O 2 concentration of the Method 7 absorbing solution. Laboratory tests have shown that high concentrations of SO 2 (about 2100 ppm) cause low results in Method 7 and 7A. Increasing the H 2 O 2 concentration to five times the original concentration eliminates this bias. However, when no SO 2 is present, increasing the concentration by five times results in a low bias.
* * * * *
10.4 Temperature Gauge. Calibrate dial thermometers against
merc ury - in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * * 35. In Method 7E of App endix A
- 4 by revising Sections 6.1, 7.1.1, 8.1.2, 8.2.5, and 16.2.2 as follows:Page **63** of **161**

**Method 7E —**  **Determination of Nitrogen Oxides Emissions From Stationary Sources (Instrumental Analyzer Procedure)**  * * * * *
6.1 What do I need for the measurement system? You may use any equipment and supplies meeting the following specifications : 1) Sampling system components that are not evaluated in the system bias or system calibration error test must be glass, Teflon, or stainless steel. Other materials are potentially a cceptable, subject to approval by the Administrator. 2) The interference, calibration error, and system bias criteria must be met. 3) Sample flow rate must be maintained within 10 percent of the flow rate at which the system response time was measured. 4) All system components (excluding sample conditioning components, if used) must maintain the sample temperature above the moisture dew point. Ensure minimal contact between any condensate and the sample gas. Section 6.2 provides example equipment specif ications for a NO x measurement system. Figure 7E
- 1 is a diagram of an example dry
- basis measurement system that is likely to meet the method requirements and is provided as guidance. For wet
- basis systems, you may use alternative equipment and supplies as needed (some of which arePage **64** of **161**

described in Section 6.2), provided that the measurement system meets the applicable performance specifications of this method.
* * * * *
7.1.1 High
- Level Gas. This concentration is chosen to set the calibration span as defined in Section 3.4. Choose this high
- level concentration so that emission measurements will be within 20 to 100 percent of this concentration .
* * * * *
8.1.2 Determination of Stratification. Perform a stratifica tion test at each test site to determine the appropriate number of sample traverse points. If testing for multiple pollutants or diluents at the same site, a stratification test using only one pollutant or diluent satisfies this requirement. A stratificati on test is not required for small stacks that are less than 4 inches in diameter. To test for stratification, use a probe of appropriate length to measure the NO x (or pollutant of interest) concentration at 12 traverse points located according to Ta ble 1
- 1 or Table 1
- 2 of Method 1. Alternatively, you may measure at three points on a line passing through the centroidal area. Space the three points at 16.7, 50.0, and 83.3 percent of the measurement line. Sample for a minimum of twice the system respons e time (see Section 8.2.6) at each traverse point. Calculate the individual point and mean NO x concentrations. If the concentration at each traverse point differs from the meanPage **65** of **161**

concentration for all traverse points by no more than: (a) ± 5.0 percent of the mean concentration; or (b) ± 0.5 ppm (whichever is less restrictive), the gas stream is considered unstratified and you may collect samples from a single point that most closely matches the mean. If the 5.0 percent or 0.5 ppm criterion is not met, but the concentration at each traverse point differs from the mean concentration for all traverse points by no more than: (a) ± 10.0 percent of the mean; or (b) ± 1.0 ppm (whichever is less restrictive), the gas stream is considered to be minimally stratified, an d you may take samples from three points. Space the three points at 16.7, 50.0, and 83.3 percent of the measurement line. Alternatively, if a 12 point stratification test was performed and the emissions shown to be minimally stratified (all poi nts within ± 10.0 percent of their mean or within ± 1.0 ppm), and if the stack diameter (or equivalent diameter for a rectangular stack or duct) is greater than 2.4 meters (7.8 ft), then you may use 3
- point sampling and locate the three points along the m easurement line exhibiting the highest average concentration during the stratification test at 0.4, 1. 2, and 2.0 meters from the stack or duct wall. If the gas stream is found to be stratified because the 10.0 percent or 1.0 ppm criterion for a 3
- point test is not met, locate 12 traverse points for the test in accordance with Table 1
- 1 or Table 1
- 2 of Method 1. This stratification test may not be meaningful at sources with temporally varying emissions or where emission concentrations are low. In these cases, the stratification test is not required.Page **66** of **161**

* * * * *
8.2.5 Initial System Bias and System Calib ration Error Checks. Before sampling begins, determine whether the high
- level or mid
- level calibration gas best approximates the emissions and use it as the upscale gas. Introduce the upscale gas at the probe upstream of all sample conditioning components in system calibration mode. Record the time it takes for the measured concentration to increase to a value that is within 95 percent or 0.5 ppm (whichever is less restrictive) of a stable response for both the low
- level and upscale gases. Continue to observe the gas concentration reading until it has reached a final, stable value. Record this value on a form similar to Table 7E

– 2.
* * * * *
16.2.2 Bag Procedure. Perform the analyzer calibration error test to document the calibration (both NO and NO X modes , as applicable). Fill a Tedlar or equivalent bag approximately half full with either ambient air, pure oxygen, or an oxygen standard gas with at least 19.5 percent by volume oxygen content. Fill the remainder of the bag with mid
- to high
- level NO in N 2 (or other appropriate concentration) calibration gas. (Note that the concentration of the NO standard should be sufficiently high enough for the diluted concentration to be easily and accurately measured on the scale used. The size of the bag should be large enough to accommodate thePage **67** of **161**

procedure and time required . Contact the bag manufacturer for guidance on the applicability of Tedlar equivalent materials for NO .)
* * * * * 36. In Method 8 of Appendix A
- 4 by revising Sections 11.2.1 and 11.2.2, by revising two definition s in Section 12.1 , and by revising Figure 8
- 1 as follows: **Method 8 –**  **Determination of S**  **ulfuric A**  **cid M**  **ist and S**  **ulfur D**  **ioxide E**  **missions F**  **rom S**  **tationary S**  **ources** * * * * *
11.2.1 Container No. 1. Shake the container holding the isopropanol solution and the filter. If the filter breaks up, allow the fragments to settle for a few minutes before removing a sample aliquot. For determination of SO 3 /H 2 SO 4 concentration, pipette a 10
- ml aliquot of this solution into a 250
- ml Erlenmeyer flask, add 2 to 4 drops of thorin indicator, and titrate to a pink endpoint using 0.0100 N barium standard solution. Repeat the titration with a second aliquot of sample, and average th e titration values. Replicate titrations must agree within 1 percent or 0.2 ml, whichever is greater.
11.2.2 Container No. 2. Thoroughly mix the solution in the container holding the contents of the second and third impingers. For determination of SO 2 con centration, pipette a 100
- ml aliquot of sample into a 250
- ml Erlenmeyer flask. Add 40 ml of isopropanol, 2 to 4Page **68** of **161**

drops of thorin indicator, and titrate to a pink endpoint using 0.0100 N barium standard solution. Repeat the titration with a seco nd aliquot of sample, and average the titration values. Replicate titrations must agree within 1 percent or 0.2 ml, whichever is greater.
* * * * * 12.1 * * *

V a = Volume of sample aliquot titrated, 10 ml for H 2 SO 4 and 100 ml for SO 2 .
V soln = Total volume of solution in which the sample is contained, 1000 ml for the SO 2 sample and 250 ml for the H 2 SO 4 sample. * * * * *Page **69** of **161**

Te mperature Ice Bath Vacuum Line

Dry Gas Meter Main Valve Vacuum

Gauge By-pass Valve
Pump Orifice Sensors

Manometer Impingers Silica Gel Te mperature Sensor Type S Pitot Tube Probe Te mperature Sensor

Te mperature Sesnor Stack

Wa ll Heat T raced Glass-Lined Probe

Manometer Type S Pitot Tube Filter Holder SO

Components

2 H SO /SO Components 4 2 3

**Figure 8 -**  **1. Sulfuric Acid Sampling Train. H**  **2 SO4/SO**  **3 and**  **SO 2**  **collection components**  **identified** * * * * * 37. In Method 10 of Appendix A
- 4 by revising S ections 6.2.5 and 8.4.2 as follows: **Method 10 –**  **Determination of C**  **arbon M**  **onoxide E**  **missions F**  **rom S**  **tationary S**  **ources** * * * * *
6.2.5 Flexible Bag. Tedlar, or equivalent, with a capacity of 60 to 90 liters (2 to 3 ft 3 ). (Contact the bag manufacturer forPage **70** of **161**

guidance on the applicability of Tedlar equivalent materials for the compound of interest.) Leak
- test the bag in the laboratory before using by evacuating with a pump followed by a dry gas meter. When the evacuation is complete, there should be no flow through the meter. Gas tanks may be used in place of bags if the samples are analyze d within one week.
* * * * *
8.4.2 Integrated Sampling. Evacuate the flexible bag. Set up the equipment as shown in Figure 10

– 1 with the bag disconnected. Place the probe in the stack and purge the sampling line. Connect the bag, making sure that all conn ections are leak
- free. Sample at a rate proportional to the stack velocity. If needed, the CO 2 content of the gas may be determined by using the Method 3 integrated sample procedures, or by weighing an ascarite CO 2 removal tube used and computing CO 2 concentration from the gas volume sampled and the weight gain of the tube. Data may be recorded on a form similar to Table 10

– 1 . If a tank is used for sample collection, follow procedures similar to those in Sections 8.1.2, 8.2.3, 8.3, and 12.4 of Method 2 5 as appropriate to prepare the tank, conduct the sampling, and correct the measured sample concentration .
* * * * *Page **71** of **161**

38. In Method 10A of Appendix A
- 4 by revising S ections 2.0, 8.2.1, 8.2.3, 11.1, 11.2, and 13.5 and by revising the narrative in Section 12.3 as follows: **Method 10A —**  **Determination of Carbon Monoxide Emissions in Certifying Continuous Emission Monitoring Systems at Petroleum Refineries**  * * * * *
2.0 Summary of Method An integrated gas sample is extracted from the stack, passed through an alkaline permanganate solution to remove sulfur oxides and nitrogen oxides, and collected in a Tedlar or equivalent bag. (Contact the bag manufacturer for guidance on the applicability of Tedlar equivalent materials for the compound of interest.) The CO concentration in the sample is measured spectrophotometrically using the reaction of CO with p - sulfaminobenzoic acid.
* * * * *
8.2.1 Evacuate the bag completely using a vac uum pump. Assemble the apparatus as shown in Figure 10A

– 1. Loosely pack glass wool in the tip of the probe. Place 400 ml of alkaline permanganate solution in the first two impingers and 250 ml in the third. Connect the pump to the third impinger, and follo w this with the surge tank, rate meter, and 3
- way valve. Do not connect the bag to the system at this time.Page **72** of **161**

* * * * *
8.2.3 Purge the system with sample gas by inserting the probe into the stack and drawing the sample gas through the system at 300 ml/min ±10 percent for 5 minutes. Connect the evacuated bag to the system, record the starting time, and sample at a r ate of 300 ml/min for 30 minutes, or until the bag is nearly full. Record the sampling time, the barometric pressure, and the ambient temperature. Purge the system as described above immediately before each sample.
* * * * *
11.1 Assemble the syste m shown in Figure 10A

– 3, and record the information required in Table 10A

– 1 as it is obtained. Pipet 10.0 ml of the colorimetric reagent into each gas reaction bulb, and attach the bulbs to the system. Open the stopcocks to the reaction bulbs, but leave th e valve to the bag closed. Turn on the pump, fully open the coarse
- adjust flow valve, and slowly open the fine
- adjust valve until the pressure is reduced to at least 40 mm Hg. Now close the coarse adjust valve, and observe the manometer to be certai n that the system is leak
- free. Wait a minimum of 2 minutes. If the pressure has increased less than 1 mm Hg, proceed as described below. If a leak is present, find and correct it before proceeding further.
11.2 Record the vacuum pressure (P v ) to the near est 1 mm Hg, and close the reaction bulb stopcocks. Open the bag valve, and allow the system to come to atmospheric pressure. Close the bag valve, open thePage **73** of **161**

pump coarse adjust valve, and evacuate the system again. Repeat this fill/evacuation procedur e at least twice to flush the manifold completely. Close the pump coarse adjust valve, open the bag valve, and let the system fill to atmospheric pressure. Open the stopcocks to the reaction bulbs, and let the entire system come to atmospheric press ure. Close the bulb stopcocks, remove the bulbs, record the room temperature and barometric pressure (P bar , to nearest mm Hg), and place the bulbs on the shaker table with their main axis either parallel to or perpendicular to the plane of the table top. P urge the bulb
- filling system with ambient air for several minutes between samples. Shake the samples for exactly 2 hours.
* * * * *
12.3 CO Concentration in the Bag. Calculate C b using Equations 10A

– 2 and 10A

– 3. If condensate is visible in the bag, calculate B w using Table 10A

– 2 and the temperature and barometric pressure in the analysis room. If condensate is not visible, calculate B w using the temperature and barometric pressure at the sampling site. * * *
* * * * *
13.5 Stability. The indi vidual components of the colorimetric reagent are stable for at least one month. The colorimetric reagent must be used within two days after preparation to avoid excessive blank correction. The samples in the bag should be stable for at least on e week if the bags are leak
- free.Page **74** of **161**

* * * * * 39. In Method 10B of Appendix A
- 4 by revising S ections 2.1 and 6.2.3 and by revising the narrative in Section 12.2 as follows: **Method 10B —**  **Determination of Carbon Monoxide Emissions From Stationary Sources**  * * * * *
2.1 An integrated gas sample is extracted from the sampling point, passed through a conditioning system to remove interferences, and collected in a Tedlar or equivalent bag. (Contact the bag manufacturer for guidance on the applicability of Tedlar equ ivalent materials for the compound of interest.) The CO is separated from the sample by gas chromatography (GC) and catalytically reduced to methane (CH 4 ) which is determined by flame ionization detection (FID). The analytical portion of this method is identical to applicable sections in Method 25 detailing CO measurement.
* * * * *
6.2.3 Sample Injection System. Same as in Method 25, Section 6.3.1.4, equipped to accept a sample line from the bag.
* * * * *
12.2 CO Concentration in the Bag. Cal culate C b using Equations 10B

– 1 and 10B

– 2. If condensate is visible in the bag, calculate B w using Table 10A

– 2 of Method 10A and the temperature and barometricPage **75** of **161**

pressure in the analysis room. If condensate is not visible, calculate B w using the tempe rature and barometric pressure at the sampling site. * * *
* * * * * 40. In Method 11 of Appendix A
- 5 by revising S ections 8.5 and 10.1.2 as follows: **Method 11 —**  **Determination of Hydrogen Sulfide Content of Fuel Gas Streams in Petroleum Refineries**  * * * * *
8.5 Sample for at least 10 minutes. At the end of the sampling time, close the sampling valve, and record the final volume and temperature readings. Conduct a leak
- check as described in Section 8.2 . A yellow color in the final cadmium sulfate impinger ind icates depletion of the absorbing solution. An additional cadmium sulfate impinger should be added for subsequent samples and the sample with yellow color in the final impinger should be voided .
* * * * *
10.1.2 Temperature Sensors. Calibrate agains t mercury - in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is at a minimum equivalent in terms of performance or suitably effective for the specific temperature measurement application.Page **76** of **161**

* * * * * 41. In Method 12 of Appendix A
- 5 by revising Section 16.1 and adding S ection s 16.4, 16.4.1, and 16.4.2 as follows: **Method 12 –**  **Determination of Inorganic Lead Emissions From Stationary Sources**  * * * * *
16.1 Simultaneous Determination of Particulate Matter and Lead Emissions. Method 12 may be used to simultaneously determine Pb provided: (1) acetone is used to remove particulate from the probe and inside of the filter holder as specified by Method 5, (2) 0.1 N HNO 3 is used in the impingers, (3) a glass fib er filter with a low Pb background is used, and (4) the entire train contents, including the impingers, are treated and analyzed for Pb as described in Sections 8.0 and 11.0 of this method.
* * * * * 16.4 Alternative Analyzer. Inductively coupled plasma
- atomic emission spectrometry (ICP
- AES) may be used as an alternative to atomic absorption analysis provided the following conditions are met: 16.4.1 Sample collection, sample preparation, and analytical preparation procedures are as defined in the method except as necessary for the ICP
- AES application. 16.4.2 The limit of quantitation for the ICP
- AES must be demonstrated , and the sample concentrations reported should be no less than two times the limit of quantitation. The limit ofPage **77** of **161**

quantitation is defined as ten times the standard deviation of the blank value. The standard deviation of the blank value is determined from the analysis of seven blanks. It has been reported that for mercury and those elements that form hydrides, a continuous
- flow generator cou pled to an ICP
- AES offers detection limits comparable to cold vapor atomic absorption. * * * * * 42. In Method 14A of Appendix A
- 5 by adding a sentence to S ection 10.1.1 as follows: **Method 14A —**  **Determination of Total Fluoride Emissions from Selected Sources**  **at Primary Aluminum Production Facilities** * * * * * 10.1.1 Metering system. * * * Allowable tolerances for Y and ΔH@ are given in Figure 5

– 5 6 of Method 5 of this appendix. * * * * * 43. In Method 16A of Appendix A
- 6 by revising S ection 1.2 as follows: **Method 16A —**  **Determination of Total Reduced Sulfur Emissions From Stationary Sources (Impinger Technique)**  * * * * *
1.2 Applicability. This method is applicable for the determination of TRS emissions from recovery boilers, lime kilns, and smelt dissolving tanks at kraft pulp mills, reduced sulfur compoundsPage **78** of **161**

(H 2 S, carbonyl sulfide, and carbon disulfide ) from sulfur recovery units at onshore natural gas processing facilities, and from other sources when specified in an applicable subpart of the regulations. The flue gas must contain at least 1 percent oxygen for complete oxidation of all TRS to SO 2 . **Note** : If sources other than kraft pulp mills experience low oxygen levels in the emissions, the method results may be biased low.
* * * * * 44. In Method 18 of Appendix A
- 6 by revising S ections 8.2.1.1.2, 8.2.1.4, 8.2.1.4.2, 8.2.1.5.2.2, 16.1.1.12, 16.1.3.2, and th e titles to Figures 18
- 3 and 18
- 10 as follows: **Method 18 —**  **Measurement of Gaseous Organic Compound Emissions By Gas Chromatography**  * * * * *
8.2.1.1.2 Sampling Procedure. To obtain a sample, assemble the sample train as shown in Figure 18

– 9. Leak
- check both the bag and the container. Connect the vacuum line from the needle valve to the Teflon sample line from the probe. Place the end of the probe at the centroid of the stack or at a point no closer to the walls than 1 m, and start the pump. Set the flow rate so that the final volume of the sample is approximately 80 percent of the bag capacity. After allowing sufficient time to purge the line several times, connect the vacuum line to the bag, and evacuate until the rotameter indicates no flow. Then positi on the sample and vacuum lines for sampling, andPage **79** of **161**

begin the actual sampling, keeping the rate proportional to the stack velocity. As a precaution, direct the gas exiting the rotameter away from sampling personnel. At the end of the sample period, shut off t he pump, disconnect the sample line from the bag, and disconnect the vacuum line from the bag container. Record the source temperature, barometric pressure, ambient temperature, sampling flow rate, and initial and final sampling time on the data sheet show n in Figure 18

– 10. Protect the bag and its container from sunlight. Record the time lapsed between sample collection and analysis, and then conduct the recovery procedure in Section 8.4.2.
* * * * *
8.2.1.4 Other Modified Bag Sampling Procedures. I n the event that condensation is observed in the bag while collecting the sample and a direct interface system cannot be used, heat the bag during collection and maintain it at a suitably elevated temperature during all subsequent operations. (Note:Take c are to leak
- check the system prior to the dilutions so as not to create a potentially explosive atmosphere.) As an alternative, collect the sample gas, and simultaneously dilute it in the bag.
* * * * *
8.2.1.4.2 Second Alternative Procedure. Prefi ll the bag with a known quantity of inert gas. Meter the inert gas into the bag according to the procedure for the preparation of gas concentrationPage **80** of **161**

standards of volatile liquid materials (Section 10.1.2.2), but eliminate the midget impinger section. Take the partly filled bag to the source, and meter the source gas into the bag through heated sampling lines and a heated flowmeter, or Teflon positive displacement pump. Verify the dilution factors before sampling each bag through dilution and analysis of gases of known concentration.
* * * * * 8.2.1.5.2.2 Analyze the two field audit samples as described in Section 9.2 by connecting each bag containing an audit gas mixture to the sampling valve. Calculate the results; record and report the data to the audit supervisor. * * * * *
16.1.1.12 Flexible Bags. Tedlar or equivalent, 10
- and 50
- liter capacity, for preparation of standards. (Contact the bag manufacturer for guidance on the applicability of Tedlar equivalent materials for the compound of interest.)
* * * * *
16.1.3.2 Flexible Bag Procedure. Any leak
- free plastic ( e.g., Tedlar , Mylar, Teflon) or plastic
- coated aluminum (e.g., aluminized Mylar ) bag, or equivalent, can be used to obtain the pre - survey sample. Use new bags, and leak
- check them before field use. In addition, check the bag before use for contamination by filling it with nitrogen or air and analyzing the gas by GC at high sensitivity.Page **81** of **161**

Experience indicates that it is desirable to allow the inert gas to remain in the bag about 24 hours or longer to check for desorption of organics from the bag. Follow the leak
- check and sample collection procedures given in Section 8.2.1.
* * * * * Figure 18

– 3. Preparation of Standards in Tedlar or Tedlar
Eq ulivalent Bags and Calibration Curve * * * * * Figure 18

– 10. Field Sample Data Sheet

— Tedlar or Tedlar
Equivalent Bag Collection Method * * * * * 45. In Method 23 of Appendix A
- 7 by revising S ection s 2.2.7, 4.1.1.3, and 4.2.7 as follows: **Method 23 —**  **Determination of Polychlorinated Dibenzo -**  **p -**  **Dioxins and Polychlorinated Dibenzofurans From Stationary Sources**  * * * * *
2.2.7 Storage Container. Air
- tight container to store silica gel.
* * * * *
4.1.1.3 Sample Train. It is suggested that all components be maintained according to the procedure described in APTD
- 0576. Alternative mercury
- free thermometers may be used if the thermometersPage **82** of **161**

are, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measu rement application .
* * * * *
4.2.7 Silica Gel. Note the color of the indicating silica gel to determine if it has been completely spent and make a mention of its condition. Transfer the silica gel from the fifth impinger to its original container and sea l. If a moisture determination is made, follow the applicable procedures in sections 8.7.6.3 and 11.2.3 of Method 5 to handle and weigh the silica gel. If moisture is not measured, the silica gel may be disposed.
* * * * * 46. In Method 24 of Appendix A
- 7 by r evising S ection 11.2.2 as follows: **Method 24 —**  **Determination of Volatile Matter Content, Water Content, Density, Volume Solids, and Weight Solids of Surface Coatings**  * * * * *
11.2.2 Volatile Content. To determine total volatile content,
use the apparatus and reagents described in ASTM D2369 (incorporated by reference

— see §60.17 for the approved versions of the standard), respectively, and use the following pro cedures:
* * * * *Page **83** of **161**

47. In Method 25 of Appendix A
- 7 by revising S ection 7.1.3 as follows: **Method 25 –**  **Determination of T**  **otal G**  **aseous N**  **onmethane O**  **rganic E**  **missions as C**  **arbon** * * * * *
7.1.3 Filters. Glass fiber filters, without organic binder, exhibiting at least 99.95 percent efficiency (<0.05 percent penetration) on 0.3 micron dioctyl phthalate smoke particles. The filter efficiency test shall be conducted in accordance with ASTM Method D2986
- 71, 78, or 95a (incorporated by reference

– see §60.17). Test dat a from the supplier’s quality control program are sufficient for this purpose .
* * * * * 48. In Method 25C of Appendix A
- 7 by revising Sections 6.1 and 12.1, redesignating Equation 25C
- 2 in Section 12.3 as Equation 25 C - 3, redesignating Section 12.3 as 12.4, and adding new Sections 8.2.3 and 12.3 as follows: **Method 25C –**  **Determination of N**  **onmethane O**  **rganic C**  **ompounds (NMOC) in MSW**  **L andfill**  **G ases**  * * * * *
6.1 Sample Probe. Stainless steel, with the bottom third perforated. Teflon probe liners and sampling lines are also allowed. Non - perforated probes are allowed as long as they are withdrawn toPage **84** of **161**

create a gap equivalent to having the bottom third perforated. The sample probe must be capped at the bottom and must h ave a threaded cap with a sampling attachment at the top. The sample probe must be long enough to go through and extend no less than 0.9 m (3 ft) below the landfill cover. If the sample probe is to be driven into the landfill, the bottom cap should be desi gned to facilitate driving the probe into the landfill.
* * * * * 8.2.3 Driven Probes. Closed
- point probes may be driven directly into the landfill in a single step. This method may not require backfilling if the probe is adequately sealed by its insertio n. Unperforated probes that are inserted in this manner and withdrawn a distance from a detachable tip to create an open space are also acceptable. * * * * *
12.1 Nomenclature.
B w = Moisture content in the sample, fraction.
C N2 = Measured N 2 concentration (by Method 3C), fraction.
C N2Corr = Measured N 2 concentration corrected for dilution , fraction.
C t = Calculated NMOC concentration, ppmv C equivalent.
C tm = Measured NMOC concentration, ppmv C equivalent.Page **85** of **161**

P b = Barometric pressure, mm Hg.
P t = Gas sample tank pressure after sampling, but before pressurizing, mm Hg absolute.
P tf = Final gas sample tank pressure after pressurizing, mm Hg absolute.
P ti = Gas sample tank pressure after evacuation, mm Hg absolute.
P w = Vapor pressure of H 2 O (from Table 25C

– 1), mm Hg.

r = Total number of analyzer injections of sample tank during analysis (where j=injection number, 1 * * * r).
T t = Sample tank temperature at completion of sampling, °K.
T ti = Sample tank temperature before sampling, °K.
T tf = Sample tank tempera ture after pressurizing, °K.
* * * * * 12.3 Measured N 2 Concentration Correction. Use the following equation to correct the measured concentration of N 2 as determined by Method 3C for dilution.

=

− . 25
− 2

* * * * * 49. In Method 25D of Appendix A
- 7 by revising the first sentence in S ection 9.1 a s follows:Page **86** of **161**

**Method 25D —**  **Determination of the Volatile Organic Concentration of Waste Samples**  * * * * * 9.1 Quality Control Samples. If audit samples are not available, prepare and analyze the two types of quality control samples (QCS) listed in Sections 9. 1 .1 and 9. 1 .2. * * * * * * * * 50. In Method 26 of Appendix A
- 8 by revising S ection s 6.1.1 and 8.1.2, by r edesignat ing S ection 16 as 17 and Section 17 as 18, and by adding a new S ection 16 as follows: **Method 26 —**  **Determination of Hydrogen Halide and Halogen Emissions From Stationary Sources Non**  **- Isokinetic Method**  * * * * *
6.1.1 Probe. Borosilicate glass, approximately 3 /8

- in. (9
- mm) I.D. with a heating system capable of maintaining a probe gas temperature during sampling of 120 ±14 °C (248 ±25 °F) to prevent moisture condensation ; or Teflon where stack probes are below 210  C. If HF is a target analyte, then preconditioning of new teflon components by heating should be considered to prevent potential HF outgassing . A Teflon
- glass filter in a mat configuration should be installed in the gas stream, not the filter box, to remove particulate matter from the gas stream (see Section 6.1.6).
* * * * *Page **87** of **161**

8.1.2 Adjust the probe temperature and the temperature of the filter and the stopcock ( i.e., the heated area in Figure 26

– 1 ) to a temperature sufficient to prevent water condensation. This temperature should be greater than 120 °C (248 °F). The temperature should be monitored throughout a sampling run to ensure that the desired temperature is maintained. It is important to maintain a temperature around the probe and filter of greater than 120 °C (248 °F) since it is extremely difficult to purge acid gases off these components. (These components are not quantitatively recovered and , hence , any collection of acid gases on these components would result in poten tial undereporting of these emission s . The applicable subparts may specify alternative higher temperatures.)
* * * * * **16.0 Alternative Procedures** Method 26A. Method 26A, which uses isokinetic sampling equipment, is an acceptable alternative to Method 26. * * * * * 51. In Method 29 of Appendix A
- 8 by redesignating Section 16 as Section 17 and redesignating Section 17 as Section 18 and by adding a new S ection 16 as follows: **Method 29**  **– Determination**  **of Metals Emissions F rom**  **Stationary Sources** * * * * * **16.0 Alternative Procedures**Page **88** of **161**

16.1 Alternative Analyzer. Samples may also be analyzed by cold vapor atomic fluorescence spectrometry. * * * * * 52. In Method 30B of Appendix A
- 8 by revising Table 9
- 1 in S ection 9 and revising Section 10.3 as follows: **Method 30B —**  **Determination of Total Vapor Phase Mercury Emissions From Coal**  **- Fired Combustion Sources Using Carbon Sorbent Traps**  * * * * * 9.0 Quality Assurance and Quality Control * * *
**Table 9 –**  **1 —**  **Quality Assurance/Quality Control Criteria for Method 30B**  **QA/QC test or specification**  **Acceptance criteria**  **Frequency Consequences if not**  **met** Gas flow meter calibration (At 3 settings or points) Calibration

factor (Y i ) at each flow rate must be within ±2% of the average value (Y) Prior to initial use and when post - test check is not within ±5% of Y Recalibrate at 3 points until the acceptance criteria are met.

Gas flow meter post - test calibration check (Single
point) Calibration

factor (Y i ) must be within ±5% of the Y value from the most recent 3
- point calibration After each field test. For mass flow meters, must be done on
site, using stack gas Recalibrate gas flow meter at 3 points to determine a new value of Y. For mass flow meters, must be done on
- site, using stack gas. Apply the new Y value to the f ield test data. Temperature sensor calibration Absolute

temperature measures by sensor within ±1.5% of a Prior to initial use and before each test thereafter Recalibrate; sensor may not be used until specification is met.Page **89** of **161** reference sensor Barometer calib ration Absolute pressure

measured by instrument within ±10 mm Hg of reading with a mercury barometer or NIST traceable barometer Prior to initial use and before each test thereafter Recalibrate; instrument may not be used until specification is met.

Pre - test leak check ≤4% of target

sampling rate Prior to sampling Sampling shall not commence until the leak check is passed. Post - test leak check ≤4% of average

sampling rate After sampling Sample invalidated.* Analytical matrix interference test (wet chemical analysis, only) Establish minimum

dilution (if any) needed to eliminate sorbent matrix interferences Prior to analyzing any field samples; repeat for each type of sorbent used Field sample results not validated.

Analytical bias test Average recov ery

between 90% and 110% for Hg 0 and HgCl 2 at each of the 2 spike concentration levels Prior to analyzing field samples and prior to use of new sorbent media Field samples shall not be analyzed until the percent recovery criteria has been met.
Multipoint analyzer calibration Each analyzer

reading within ±10% of true value and r 2 ≥0.99 On the day of analysis, before analyzing any samples Recalibrate until successful.
Analysis of independent calibration standard Within ±10% of

true value Following daily calibration, prior to analyzing field samples Recalibrate and repeat independent standard analysis until successful. Analysis of continuing calibration verification standard (CCVS) Within ±10% of

true value Following daily calibration, after analyzing ≤10 field samples, and at end of each set of analyses Recalibrate and repeat independent standard analysis, reanalyze samples until successful, if possible; for destructivePage **90** of **161** techniques, samples invalidated. Test run total sample volume Within ±20 % of

total volume sampled during field recovery test Each individual sample Sample invalidated.

Sorbent trap section 2 breakthrough ≤10% of section 1

Hg mass for Hg concentrations > 1 μg/dscm; Every sample Sample invalidated.*
≤20% of section 1 Hg mass for Hg concentrations ≤1 μg/dscm Paired sorbent trap agreement ≤10% Relative

Deviation (RD) mass for Hg concentrations >1 μg/dscm; Every run Run invalidated.*

≤20% RD or ≤0.2 μg/dscm absolute difference for Hg concentrations ≤1 μg/dscm Sample analysis Within valid

calibration range (within calibration curve) All Section 1 samples where stack Hg concentation is ≥0.5 μg/dscm Reanalyze at more concentrated level if possible, samples invalidated if not within calibrated range. Sample analysis Within bounds of

Hg 0 and HgCl 2 Analytical Bias Test All Section 1 samples where stack Hg concentration is ≥0.5 μg/dscm Expand bounds of Hg 0 and HgCl 2 Analytical Bias Test; if not successful, samples invalidated. Field recovery test Average recovery

between 85% and 115% for Hg 0 Once per field test Field sample runs not validated without successful field recovery test. *And data from the pair of sorbent traps are also invalidated.Page **91** of **161**

* * * * *
10.3 Thermocouples and Other Temperature Sensors. Use the procedures and criteria in Section 10.3 of Method 2 in Appendix A

– 1 to this part to calibrate in
- stack temperature sensors and thermocouples. Dial thermometers shall be calibrated against mercury
in
- glass thermometers or equivalent. * * *
* * * * * 53. In Performance Specification 1 of Appendix B by revising S ection 3.5 to read as follows: **Performance Specification 1 —**  **Specifications and Test Procedures for Continuous Opacity Monitoring Sys**  **tems in Stationary Sources** * * * * *
3.5 Full Scale. The maximum data display output of the COMS. For purposes of recordkeeping and reporting, full scale will be greater than 80 percent opacity. Note: “Full scale” means “span.” * * * * * 54. In Performance Specification 3 of Appendix B by revising Section 13.2 as follows: **Performance Specification 3**  **— Specifications and Test Procedures for**  **O 2**  **and CO 2**  **Continuous Emission Monitoring Systems in Stationary Sources**  * * * * *Page **92** of **161**

13.2 CEMS Relative Accuracy Performance Specification. The RA of the CEMS must be no greater than 20 percent of the mean value of the RM test data or 1.0 percent O 2 or CO 2 , whichever is greater .
* * * * * 55. In Performance Specification 4 of Appendix B by revising Section 8.2 as follows: **Performance Specification 4 —**  **Specifications and Test Procedures for Carbon Monoxide Continuous Emission Monitoring Systems in Stationary**  **Sources** * * * * *
8.2 Reference Methods. Unless otherwise specified in an applicable subpart of the regulation, Method 10, 10A, 10B or other approved alternative are the RM for this PS.
* * * * * 56 . In Performance Specification 4B of Appendix B by revising Section 7.1.1 as follows: **Performance Specification 4B —**  **Specifications and Test Procedures for Carbon**  **Monoxide and Oxygen Continuous Monitoring Systems in Stationary Sources**  * * * * *
7.1.1 Calculations. Summarize the results on a data sheet. Average the differences between the instrument response and thePage **93** of **161**

certified cylinder gas value for each gas. Calcu late the CE results for the CO monitor according to:

CE = |d/FS| x 100 (1)
Where d is the mean difference between the CEMS response and the known reference concentration , and FS is the span value. The CE for the O 2 monitor is the average percent O 2 difference between the O 2 monitor and the certified cylinder gas value for each gas.
* * * * * 57. In Performance Specification 7 of Appendix B by revising Section 8.4 and adding a reference to the end of Section 16.0. **Performance Specification 7 —**  **Specifications and Test Procedures for Hydrogen Sulfide Continuous Emission Monitoring Systems**  **in Stationary Sources**  * * * * *
8 .4 Relative Accuracy Test Procedure.
8.4.1 Sampling Strategy for RM Tests, Number of RM Tests, C orrelation of RM and CEMS Data, and Calculations . These are the same as that in PS
- 2, Sections 8.4.3 (except as specified below), 8.4.4 , 8.4.5, and 8.4. 6 , respectively.Page **94** of **161**

8.4.2 Reference Methods. Unless otherwise specified in an applicable subpart of the regulation, Methods 11, 15, and 16 may be used for the RM for this PS. 8.4.2.1 Sampling Time Per Run
- Method 11. A sampling run , when Method 11 (integrated sampling) is used , shall consist of a single measurement for at least 10 minutes and 0.010 dscm (0.35 dscf). Each sample shall be taken at approximately 30
- minute intervals. 8.4.2.2 Sampling Time Per Run
- Methods 15 and 16. The sampling run shall consist of two injections equally spaced over a 30
- minute period following the procedures described in the particular method. NOTE: Caution! Heater or non
- approved electrical probes should not be used around explosive or flammable sources. * * * * * 16.0 Refere nces. * * * 5. Letter to RAMCON Environmental Corp. from Robert Kellam, December 27, 1992 . * * * * * 58. In Performance Specification 11 of Appendix B by revising Sections 12.1 (1) and (2) as follows: **Performance Specification 11 —**  **Specifications and Test Procedures for**  **Particulate Matter Continuous Emission Monitoring Systems at Stationary Sources**  * * * * *Page **95** of **161**

12.1 * * * (1) Calculate the upscale drift (UD) using Equation 11

– 1:

UD = | | × 100 (Eq. 11
- 1)
Where: UD = The upscale (high
- level) drift of your PM CEMS in percent,
R CEM = The measured PM CEMS response to the upscale reference standard, and
R U = The pre - established numerical value of the upscale reference standard. FS= Full
- scale value. (2) Calculate the zero drift (ZD) using Equation 11

– 2:

ZD = | | × 100 (Eq. 11
- 2)
Where: ZD = The zero (low
- level) drift of your PM CEMS in percent,
R CEM = The measured PM CEMS response to the zero reference standard,
R L = The pre - established numerical value of the zero reference standard, and FS= Full
- scale value . * * * * *Page **96** of **16 1** 

59. In Performance Specification 15 of Appendix B by revising Sections 11.1.1.4.2 and 11.1.1.4.3 as follow s: **Performance Specification 1 5**  **— Performance**  **Specification for**  **Extractive FTIR Continuous Emission Monitoring Systems**  **in Stationary**  **Sources** * * * * *
11.1.1.4.2 RMs Using a Grab Sampling Technique. Synchronize the RM and FTIR CEM measurements as closely as possible. For a grab sampling RM , record the volume collected and the exact sampling period for each sample. Synchronize the FTIR CEM so that the FTIR measures a spectrum of a similar cell volume at the same time as the RM grab sample was collected. Me asure at least five independent samples with both the FTIR CEM and the RM for each of the minimum nine runs. Compare the run concentration averages by using the relative accuracy analysis procedure in Performance Specification 2 of Appendix B of 40 CFR Part 60 . 11.1.1.4.3 Continuous Emission Monitors as RMs. If the RM is a CEM, synchronize the sampling flow rates of the RM and the FTIR CEM. Each run is at least 1 hour long and consists of at least 10 FTIR CEM measurements and the corresponding 10 RM measurements (or averages). For the statistical comparison , use the relative accuracy analysis procedure in Performance Specification 2 of Appendix B of 40 CFR Part 60 . If the RM time constant is < 1⁄2 the FTIR CE M time constant, brief fluctuations in analyte concentrations that are not adequatelyPage **97** of **161**

measured with the slower FTIR CEM time constant can be excluded from the run average along with the corresponding RM measurements. However, the FTIR CEM run average must still include at least 10 measurements over a 1
- hour period.
* * * * * 60. In Performance Specification 1 6 of Appendix B by revising Section s 6.1.7, 8.2.1, 9.1, 9.3, 9.4, 12.4, and 13.5 as follows: **Performance Specification 1 6**  **— Specification**  **s and Test Procedures for**  **Predictive Emission Monitoring Systems in Stationary Sources**  * * * * *
6.1.7 Sensor Location and Repair. We recommend you install sensors in an accessible location in order to perform repairs and replacements. Permanently
- instal led platforms or ladders may not be needed. If you install sensors in an area that is not accessible, you may be required to shut down the emissions unit to repair or replace a sensor. Conduct a new RATA after replacing a sensor that supplies a critical PE MS parameter if the new sensor provides a different output or scaling or changes the historical training dataset of the PEMS. Replacement of a non
- critical sensor that does not cause an impact in the accuracy of the PEMS does not trigger a RATA. All senso rs must be calibrated as often as needed but at least as often as recommended by the manufacturers.Page **98** of **161**

* * * * *
8.2.1 Reference Methods. Unless otherwise specified in the applicable regulations, you must use the test methods in Appendix A of this part for t he RM test. Conduct the RM tests at three operating levels . The RM tests shall be performed at a low
- load (or production) level between the minimum safe, stable load and 50 percent of the maximum level load, at the mid
- load level (an intermediary level between the low and high levels), and at a high
- load level between 80 percent and the maximum load. Alternatively, if practicable , you may test at three levels of the key operating parameter (e.g. selected based on a covariance analysis between each parameter and the PEMS output) equally spaced within the normal range of the parameter .
* * * * *
9.1 QA/QC Summary. Conduct the applicable ongoing tests listed below. **Ongoing Quality Assurance Tests Test**  **PEMS**

Regulatory Purpose **Acceptability Frequency** 

Sensor Evaluation Check All Daily

RAA Compliance 3
- test avg ≤10% of simultaneous analyzer or RM average Each quarter except

quarter when RATA performed

RATA All Same as for RA in Sec. 13.1 Yearly in quarter when

RAA not performedPage **99** of **161**

Bias Correction All If d avg ≤  cc  Bias test passed (no correction factor needed) PEMS Training All If F critical  F r  0.8 Optional after initial

and subsequent RATAs Sensor Evaluation Alert Test (optional) All See Section 6.1.8 After each PEMS

training

* * * * *
9.3 Quarterly Relative Accuracy Audits. In the first year of operation after the initial certification, perform a RAA consisting of at least three 30
- minute portable analyzer or RM determinations each quarter a RATA is not performed. To conduct a RAA, fol low the procedures in Section 8.2 for the relative accuracy test, except that only three sets of measurement data are required, and the statistical tests are not required. The average of the three or more portable analyzer or RM determinations must not e xceed the limits given in Section 13.5. Report the data from all sets of measurement data. If a PEMS passes all quarterly RAAs in the first year and also passes the subsequent yearly RATA in the second year, you may elect to perform a single mid
- year RAA in the second year in place of the quarterly RAAs. This option may be repeated, but only until the PEMS fails either a mid
- year RAA or a year ly RATA. When such a failure occurs, you must resume quarterly RAAs in the quarter following the failure and continue conducting quarterly RAAs until the PEMS successfully passes both a year of quarterly RAAs and a subsequent RATA.Page **100** of **161**

9.4 Yearly Relative Acc uracy Test . Perform a minimum 9
- run RATA at the normal operating level on a yearly basis in the quarter that the RAA is not performed. The statistical tests in Section 8.3 are not required for the yearly RATA.
* * * * *
12.4 Relative Accuracy Audit. Calculate the quarterly RAA using Equation 16
- 9 .
100 x RM RM PEMS RAA   Eq. 16
- 9

* * * * *
13.5 Relative Accuracy Audits. The average of the three portable analyzer or RM determinations must not differ from the simultaneous PEMS average value by more than 10 percent of the analyzer or RM for concentrations greater than 100 ppm or 20 percent for concentrations between 100 and 20 ppm, or the test is f ailed. For measurements at 20 ppm or less, this difference must not exceed 2 ppm for a pollutant PEMS and 1 percent absolute for a diluents PEMS .
* * * * * 61. In Procedure 1 of Appendix F by revising Section 6.2 as follows: **Procedure 1**  **— Quality A**  **ssurance Requirements for Gas**  **Continuous Emission Monitoring Systems**  **Used for Compliance Determination**Page **101** of **161**

*** * * * ***
6.2 RAA Accuracy Calculation. Use the calculation procedure in the relevant performance specification to calculate the accuracy for the RAA. The RAA must be calculated in the units of the applicable emission standard .
* * * * * 62. In Procedure 2 of Appendix F by revis ing paragraphs (3) and (4) in S ection 12.0 as follows: **Procedure 2 —**  **Quality A ssurance Requirements for Particulate Matter**  **Continuous Emission Monitoring Systems at Stationary Sources** * * * * * 12.0 * * * (3) How do I calculate daily upscale and zero drift? You must calculate the upscale drift using Equation 2
- 2 and the zero drift using Equation 2
- 3:
UD = | | × 100 (Eq. 2
- 2)
Where: UD = The upscale drift of your PM CEMS, in percent,
R CEM = Your PM CEMS response to the upscale check value, and
R U = The upscale check value.
FS = Full
- scale value.Page **102** of **161** ZD = | | × 100 (Eq. 2
- 3)
Where: ZD = The zero (low
- level) drift of your PM CEMS, in percent,
R CEM = Your PM CEMS response of the zero check value,
R L = The zero check value, and * * * (4) How do I calculate SVA accuracy? You must use Equation 2
- 4 to calculate the accuracy, in percent, for each of the three SVA tests or the daily sample volume check: Accuracy = ( ) × 100 (Eq. 2
- 4)

Where:
V M = Sample gas volume determined/reported by your PM CEMS ( e.g., dscm),
V R = Sample gas volume measured by the independent calibrated reference device ( e.g., dscm) for the SVA or the reference value for the daily sample volume check . Note: Before calculating SVA accuracy, you must correct the sample ga s volumes measured by your PM CEMS and the independent calibrated reference device to the same basis of temperature, pressure, and moisture content. You must document all data and calculations.Page **103** of **161**

* * * * * 63. In Procedure 5 of Appendix F by re designating the second listing of Section 6.2.6 as Section 6.2.7. **PART 61 –**  **NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS** 1. The authority citation for part 61 continues to read as follows: 42 U.S.C. 7401, et seq. **§ 61.13 [Amended]** 2. By revis ing § 61.13(e)(1)(i) to read as follows: **6 1**  **.13 Emission tests and waiver of emission tests.** * * * * * (e) * * * (1) * * * (i) The source owner, operator, or representative of the tested facility shall obtain an audit sample, if commercially available, from an AASP for each test method used for regulatory compliance purposes. No audit samples are required for the following tes t methods: Methods 3A and 3C of Appendix A
- 3 of Part 60 ; Methods 6C, 7E, 9, and 10 of Appendix A
- 4 of Part 60 ; Method 18 and 19 of Appendix A
- 6 of Part 60 ; Methods 20, 22, and 25A of Appendix A
- 7 of Part 60 ; and Methods 303, 318, 320, and 321 of Ap pendix A of Part 63. If multiple sources at a single facility are tested during a compliance test event, only one audit sample is required for each method used during a compliance test. The compliance authority responsible for the compliance test may waive the requirement toPage **104** of **161**

include an audit sample if they believe that an audit sample is not necessary. “Commercially available” means that two or more independent AASPs have blind audit samples available for purchase. If the source owner, operator, or represen tative cannot find an audit sample for a specific method, the owner, operator, or representative shall consult the EPA w eb site at the following URL, www.epa.gov/ttn/emc, to confirm whether there is a source that can supply an audit sample for that met hod. If the EPA w eb site does not list an available audit sample at least 60 days prior to the beginning of the compliance test, the source owner, operator, or representative shall not be required to include an audit sample as part of the quality assur ance program for the compliance test. When ordering an audit sample, the source owner, operator, or representative shall give the sample provider an estimate for the concentration of each pollutant that is emitted by the source or the estimated concentrati on of each pollutant based on the permitted level and the name, address, and phone number of the compliance authority. The source owner, operator, or representative shall report the results for the audit sample along with a summary of the emission test res ults for the audited pollutant to the compliance authority and shall report the results of the audit sample to the AASP. The source owner, operator, or representative shall make both reports at the same time and in the same manner or shall report to the
co mpliance authority first and report to the AASP. If the method being audited is a method that allows the samples to be analyzed inPage **105** of **161**

the field and the tester plans to analyze the samples in the field, the tester may analyze the audit samples prior to collect ing the emission samples provided a representative of the compliance authority is present at the testing site. The tester may request , and the compliance authority may grant , a waiver to the requirement that a representative of the compliance authority mus t be present at the testing site during the field analysis of an audit sample. The source owner, operator, or representative may report the results of the audit sample to the compliance authority and then report the results of the audit sample to the AASP prior to collecting any emission samples. The test protocol and final test report shall document whether an audit sample was ordered and utilized and the pass/fail results as applicable.
* * * * * **§6 1**  **. 33**  **[Amended]** 3. By revising §61.33(a) as follows: **§ 61.33 Stack sampling.** (a) Unless a waiver of emission testing is obtained under §61.13, each owner or operator required to comply with §61.32(a) shall test emissions from the source according to Method 104 of A ppendix B to this part or accordi ng to Method 29 of A ppendix A to P art 60. Method 103 of A ppendix B to this part is approved by the Administrator as an alternative method for sources subject to §61.32(a). The emission test shall be performed

—Page **106** of **161**

(1) Within 90 days of the effective date in the case of an existing source or a new source which has an initial startup date preceding the effective date; or (2) Within 90 days of startup in the case of a new source which did not have an initial startup d ate preceding the effective date.
* * * * * 4. By revising §61.42(a) as follows: **§ 61.42 Emission standard.** (a) Emissions to the atmosphere from rocket
- motor test sites shall not cause time
- weighted atmospheric concentrations of beryllium to exceed 75 micr ogram minutes per cubic meter (μg
- min/m 3 ) (4.68 x 10 - 9 pound minutes per cubic foot (lb
- min/ft 3 )) of air within the limits of 10 to 60 minutes, accumulated during any 2 consecutive weeks, in any area in which an adverse effect to public health could
occur.
* * * * * 5. By revising §61.53(d)(2) as follows: **§ 61.53 Stack sampling.** * * * * * (d) * * * (2) Method 101A in A ppendix B or Method 29 in A ppendix A to part 60 shall be used to test emissions as follows:Page **107** of **161**

* * * * * 6. By revising §61.164(d)(2)(i), (e)(1)(i), and (e)(2) as follows: **§ 61.164 Test methods and procedures.** * * * * * (d) * * * (2) * * * (i) Use Method 108 in A ppendix B to this part or Method 29 in A ppendix A to part 60 for determining the arsenic emission rate, g/hr (lb/hr). The emission rate shall equal the arithmetic mean of the results of three 60
- minute test runs.
* * * * * (e) * * * (1) * * * (i) Use Method 108 in A ppendix B to this part or Method 29 in A ppendix A to part 60 to determine the concentration of arsenic in the gas streams entering and exiting the control device. Conduct three 60
- minute test runs, each consisting of simultaneous testing of the inlet and outlet gas streams. The gas streams shall contain all the gas exhausted from the glass melting furnace.
* * * * *Page **108** of **161**

(2) Calculate the percent emission reduction for each run as follows:

b a b C x C C D 100

) (

 

Where:

D = the percent emission reduction.
C b = the arsenic concentration of the stack gas entering the control device, as measured by Method 108 or Method 29 .
C a = the arsenic concentration of the stack gas exiting the control device, as measured by Method 108 or Method 29 .
* * * * * 7. In Method 101 of Appendix B by redesignating Section 16 as Section 17 and redesignating Section 17 as Section 18, and by adding a new S ection 16 as follows: **Method 101**  **– Determination**  **of Particulate and Gaseous Mercury Emissions F**  **rom Chlor**  **- Alkali Plants (Air Streams)**  * * * * * 16.0 Alternative Procedures 16.1 Alternative Analyzer. Samples may also be analyzed by cold vapor atomic fluorescence spectrometry. * * * * *Page **109** of **161**

8. In Method 101A of Appendix B by redesignating Section 16 as Section 17 and redesignating Section 17 as Section 18, and by adding a new S ect ion 16 as follows: **Method 101A –**  **Determination of P**  **articulate and G**  **aseous M**  **ercury E**  **missions F**  **rom S**  **ewage S**  **ludge I**  **ncinerators** * * * * * 16.0 Alternative Procedures 16.1 Alternative Analyzer s . 16.1.1 Inductively coupled plasma
- atomic emission spectrometry (ICP
- AES) may be used as an alternative to atomic absorption analysis provided the following conditions are met: 16.1.1 .1 Sample collection, sample preparation, and analytical preparation procedures are as defined in the method except as
nece ssary for the ICP
- AES application. 16.1. 1. 2 The quality control procedures are conducted as prescribed. 16.1. 1. 3 The limit of quantitation for the ICP
- AES must be demonstrated and the sample concentrations reported should be no less than two times the li mit of quantitation. The limit of quantitation is defined as ten times the standard deviation of the blank value. The standard deviation of the blank value is determined from the analysis of seven blanks. It has been reported that for mercury and those ele ments that form hydrides, a continuous
- flow generator coupled to an ICP
- AES offers detection limits comparable to cold vapor atomic absorption.Page **110** of **161**

6.1.2 Samples may also be analyzed by cold vapor atomic fluorescence spectrometry. * * * * * 9. In Met hod 102 in A ppendix B by revising Section 8.1.1.1 as follows: **Method 10 2**  **– Determination of**  **Particulate and Gaseous Mercury Emissions from Chlor**  **- Alkali Plants (Hydrogen Streams)**  * * * * *
8.1.1.1 Calibrate the meter box orifice. Use the techniques described in APTD
- 0576 (see Reference 9 in Section 17.0 of Method 5 of Appendix A to Part 60 ). Calibration of the orifice meter at flow conditions that simulate the conditions at the source is suggested. Calibration should either be done with hydrogen or with some other gas having a similar Reynolds Number so that there is similarity between the Reynolds Numbers during calibration and during sampling. Alternative mercury
- free thermometers may be used if the thermometers are, at a minimum, equivalent in ter ms of performance or suitably effective for the specific temperature measurement application.
* * * * *
10. In Method 104 in A ppendix B by revising Sections 4.1 and 11.5.3, by redesignating Sections 16 and 17 as Sections 17 and 18 respectively, and by adding a new Section 16 as follows:Page **111** of **161**

**Method 104 –**  **Determination of Beryllium Emissions From Stationary Sources**  * * * * *
4.1 Matrix Effects. Analysis for Be by flame atomic absorption spectrophotometry is sensitive to the chemical composition and to the physical properties ( e.g., viscosity, pH) of the sample. Aluminum and silicon , in particular , are known to interfere when present in appreciable quantities. The analytical procedure includes (optionally) the use of the Method of Standard Additions to check for these matrix effects, and sample analysis using the Method of Standard Additions if significant matrix effects are f ound to be present (see Reference 2 in Section 17 .0).
* * * * *
11.5.3 Check for Matrix Effects (optional). Use the Method of Standard Additions (see Reference 2 in Section 17 .0) to check at least one sample from each source for matrix effects on the Be results. If the results of the Method of Standard Additions procedure used on the single source sample do not agree to within 5 percent of the value obtained by the routine atomic absorption analysis, then reanalyze all samples from the source using the Method of Standard Additions procedure.
* * * * * 16.0 Alternative ProceduresPage **112** of **161**

16.1 Alternative Analyzer. Inductively coupled plasma
- atomic emission spectrometry (ICP
- AES) may be used as an alternative to atomic absorption analysis provided the follo wing conditions are met: 16.1.1 Sample collection, sample preparation, and analytical preparation procedures are as defined in the method except as necessary for the ICP
- AES application. 16.1.2 Quality Assurance/Quality Control procedures, including audi t material analysis, are conducted as prescribed in the method. The QA acceptance conditions must be met. 16.1.3 The limit of quantitation for the ICP
- AES must be demonstrated and the sample concentrations reported should be no less than two times the lim it of quantitation. The limit of quantitation is defined as ten times the standard deviation of the blank value. The standard deviation of the blank value is determined from the analysis of seven blanks. It has been reported that for mercury and those elem ents that form hydrides, a continuous
- flow generator coupled to an ICP
- AES offers detection limits comparable to cold vapor atomic absorption. * * * * * 11. In Method 108 of Appendix B by redesignating Sections 16 and 17 as Sections 17 and 18 respectively, and by adding a new Section 16 as follows: **Method 108 –**  **Determination of Particulate and Gaseous A**  **rsenic Emissions**  * * * * *Page **113** of **161**

16.0 Alternative Procedures 1 6.1 Alternative Analyzer. Inductively coupled plasma
- atomic emission spectrometry (ICP
- AES) may be used as an alternative to atomic absorption analysis provided the following conditions are met: 16.1.1 Sample collection, sample preparation, and analytica l preparation procedures are as defined in the method except as necessary for the ICP
- AES application. 16.1.2 Quality Assurance/Quality Control procedures, including audit material analysis, are conducted as prescribed in the method. The QA acceptance con ditions must be met. 16.1.3 The limit of quantitation for the ICP
- AES must be demonstrated and the sample concentrations reported should be no less than two times the limit of quantitation. The limit of quantitation is defined as ten times the standard deviation of the blank value. The standard deviation of the blank value is determined from the analysis of seven blanks. It has been reported that for mercury and those elements that form hydrides, a continuous
- flow generator coupled to an ICP - AES offers detection limits comparable to cold vapor atomic absorption. * * * * * 12. In Method 108A of Appendix B by redesignating Sections 16 and 17 as Sections 17 and 18 respectively, and by adding a new Section 16 as follows: **Method 108A –**  **Determin ation of**  **Arsenic C ontent in**  **O re**  **S amples from**  **Nonferrous S melters** Page **114** of **161**

* * * * * 16.0 Alternative Procedures 16.1 Alternative Analyzer. Inductively coupled plasma
- atomic emission spectrometry (ICP
- AES) may be used as an alternative to atomic absorption analysis provided the following conditions are met: 16.1.1 Sample collection, sample preparation, and analytical preparation procedures are as defined in the method except as necessary for the ICP
- AES application. 16.1.2 Quality Assurance/Quality Control procedures, including audit material analysis, are conducted as prescribed in the method. The QA acceptance conditions must be met. 16.1.3 The limit of quantitation for the ICP
- AES must be demonstrated and the sample concentrations reported should be no less than two times the limit of quantitation. The limit of quantitation is defined as ten times the standard deviation of the blank value. The standard deviation of the blank value is determined from the analysis of seven blanks. It has been reported that for mercury and those elements that form hydrides, a continuous
- flow generator coupled to an ICP
- AES offers detection limits compara ble to cold vapor atomic absorption. * * * * * **PART 63 –**  **NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES**  1. The authority citation for part 6 3 continues to read as follows: Authority: 42 U.S.C. 7401 et seq .Page **115** of **161**

**§6 3**  **. 7**  **[Amended]** 2. By revising Section 63.7(c)(iii)(A) as follows: **§63.7 Performance testing requirements.**
* * * * * (c) * * * (2) * * * (iii) * * * (A) The source owner, operator, or representative of the tested facility shall obtain an audit sample, if commercially available, from an AASP for each test method used for regulatory compliance purposes. No audit samples are required for the following tes t methods: Methods 3A and 3C of Appendix A
- 3 of Part 60 ; Methods 6C, 7E, 9, and 10 of Appendix A
- 4 of Part 60 ; Methods 18 and 19 of Appendix A
- 6 of Part 60 ; Methods 20, 22, and 25A of Appendix A
- 7 of Part 60 ; and Methods 303, 318, 320, and 321 of Appendix A of Part 63. If multiple sources at a single facility are tested during a compliance test event, only one audit sample is required for each method used during a compliance test. The compliance authority resp onsible for the compliance test may waive the requirement to include an audit sample if they believe that an audit sample is not necessary. “Commercially available” means that two or more independent AASPs have blind audit samples available for purchase. I f the source owner, operator, or representative cannot find an audit sample for a specific method, the owner, operator, or representativePage **116** of **161**

shall consult the EPA w eb site at the following URL, www.epa.gov/ttn/emc, to confirm whether there is a source that can supply an audit sample for that method. If the EPA w eb site does not list an available audit sample at least 60 days prior to the beginning of the compliance test, the source owner, operator, or representat ive shall not be required to include an audit sample as part of the quality assurance program for the compliance test. When ordering an audit sample, the source owner, operator, or representative shall give the sample provider an estimate for the concentra tion of each pollutant that is emitted by the source or the estimated concentration of each pollutant based on the permitted level and the name, address, and phone number of the compliance authority. The source owner, operator, or representative shall repo rt the results for the audit sample along with a summary of the emission test results for the audited pollutant to the compliance authority and shall report the results of the audit sample to the AASP. The source owner, operator, or representative shall ma ke both reports at the same time and in the same manner or shall report to the compliance authority first and report to the AASP. If the method being audited is a method that allows the samples to be analyzed in the field and the tester plans to analyze th e samples in the field, the tester may analyze the audit samples prior to collecting the emission samples provided a representative of the compliance authority is present at the testing site. The tester may request , and the compliance authority may grant , a waiver to the requirement thatPage **117** of **161**

a representative of the compliance authority must be present at the testing site during the field analysis of an audit sample. The source owner, operator, or representative may report the results of the audit sample to the compliance authority and then report the results of the audit sample to the AASP prior to collecting any emission samples. The test protocol and final test report shall document whether an audit sample was ordered and utilized and the pass/fail results as applicable.
* * * * * **§63. 8**  **[Amended]** 3. By adding a sentence to the end of §63.8(f)(6)(iii) as follows: **§63.8 Monitoring requirements.** * * * * * (f) * * * (6) * * * (iii) * * * The Administrator will review the notification and may rescind permission to use an alternative and require the owner or operator to conduct a relative accuracy test of the CEMS as specified in section 8.4 of Performance Specification 2. * * * * * **§ 63.144**  **[Amended]**

4. By revising §63.144(b)(5)(i) by adding paragraphs (G) and (H) as follows:Page **118** of **161**

**§63.144 Process wastewater provisions —**  **test methods and procedures for determining applicability and Group 1/Group 2 determinations**  **(determining which wastewater streams require control).**  * * * * * (b) * * * (5) * * * (i) * * * (G) Method 8260B . Use procedures specified in Method 8260 B in the SW
- 846 Compendium of Methods. (H) Method 316 . Use Method 316 to determine formaldehyde concentration. * * * * * **§ 63.344**  **[Amended]** 5. By adding §63.344(c)(5) as follows: **§63.344 Performance test requirements and test methods.** * * * * * (c) * * * (5) The South Coast Air Quality Management District (SCAQMD) Method 205.1 (which is available by contacting the South Coas t AQMD , 21865 Copley Dr , Diamond Bar, CA 91765 ) may be used to determine the total chromium concentration from hard and decorative chromium electroplating tanks and chromium anodizing tanks . * * * * * **§ 63.364**  **[Amended]** 6. By revising §63.36 4(e) as follows:Page **119** of **161**

**§63.36 4**  **Monitoring requirements .**  * * * * * (e) Measure and record once per hour the ethylene oxide concentration at the outlet to the atmosphere after any control device according to the procedures specified in §63.365(c)(1). The owner or operator shall compute and record a 24
- hour average daily. T he owner or operator will install, calibrate, operate, and maintain a monitor consistent with the requirements of performance specification (PS) 8 or 9 in 40 CFR P art 60, A ppendix B, to measure ethylene oxide. The daily calibration requiremen ts of section 7.2 of PS - 9 or S ection 13.1 of PS
- 8 are required only on days when ethylene oxide emissions are vented to the control device.
* * * * * **§ 63.365**  **[Amended]** 7. By revising the introductory paragraph to §63.365 (b) as follows: **§63.365 Test methods and procedures.** * * * * * (b) Efficiency at the sterilization chamber vent. California Air Resources Board (CARB) Method 431 or the following procedures shall be used to determine the efficiency of all types of control devices us ed to comply with §63.362(c), sterilization chamber vent standard.Page **120** of **161**

* * * * * **§ 63.565**  **[Amended]** 8. By revising §63.565(d)(5), (8), and (10) and §63.565(g) as follows: **§63.565 Test methods and procedures.** * * * * * (d) * * * (5) Recovery devices. The average VOC concentration in the vent upstream and downstream of the control device shall be determined using Method 25A or 25B of A ppendix A to part 60 of this chapter for recovery devices. The average VOC concentration shall correspond to the volume measurement by taking into account the sampling system response time.
* * * * * (8) Where Method 25 , 25A, or 25B is used to measure the percent
r eduction in VOC, the percent reduction across the combustion or recovery device shall be calculated as follows:

Where:

R = control efficiency of control device, percent.Page **121** of **161**

E i = mass flow rate of VOC at the inlet to the combustion or recovery device as calculated under paragraph (c)(7) of this section, kg/hr.

E o = mass flow rate of VOC at the outlet of the combustion or recovery device, as calculated under paragraph (c)(7) of this section, kg/hr.
* * * * * (10) Use of methods other than Method 25 , 25A, or 25B shall be validated pursuant to Method 301 of Appendix A to part 63 of this chapter.
* * * * * (g) Baseline outlet VOC concentration. The procedures in th is paragraph shall be used to determine the outlet VOC concentration required in §63.563(b)(4), (6), (7), and (8) for combustion devices except flare, carbon adsorbers, condenser/refrigeration units, and absorbers, respectively, and to monitor the VOC conc entration as required in §63.564(e), (g), (h), and (i). The owner or operator shall use the procedures outlined in Method 25A or 25B . For the baseline VOC concentration, the arithmetic average of the outlet VOC concentration from three test runs from parag raph (d) of this section shall be calculated for the control device. The VOC concentrationPage **122** of **161**

shall be measured at least every 15 minutes. Compliance testing of VOC CEMS shall be performed using PS 8.
* * * * * **§ 63.750**  **[Amended]** 9. By revising § 63. 750(o) as follows: **§63.750 Test methods and procedures.** * * * * * (o) Inorganic HAP emissions

— dry particulate filter certification requirements. Dry particulate filters used to comply with §63.745(g)(2) or §63.746(b)(4) must be certified by the filter manufact urer or distributor, paint/depainting booth supplier, and/or the facility owner or operator using method 319 in A ppendix A of this part, to meet or exceed the efficiency data points found in Tables 1 and 2, or 3 and 4 of §63.745 for existing or new sources respectively.
* * * * * **§ 63.1251**  **[Amended]** 10. By revising the definition of “process vent” in §63.1251 as follows : **§63.1 251 Definitions.**  * * *
Process vent means a vent from a unit operation or vents from multiple unit operations within a process that are manifolded together into a common header, through which a HAP
- containing gasPage **123** of **161**

stream is, or has the potential to be, released to the atmosphere. Examples of process vents include, but are not limited to, vents on condensers used for product recovery, bottom receivers, surge control vessels, reactors, filters, centrifuges, and process tanks. Emission streams that are undi luted and uncontrolled containing less than 50 ppmv HAP, as determined through process knowledge that no HAP are present in the emission stream or using an engineering assessment as discussed in §63.1257(d)(2)(ii ) ; test data using Method 18 of 40 CFR part 60, A ppendix A ; Method 320 of 40 CFR p art 63 ; or any other test method that has been validated according to the procedures in Method 301 of A ppendix A of this part, are not considered process vents. Process vents do no t include vents on storage tanks regulated under §63.1253, vents on wastewater emission sources regulated under §63.1256, or pieces of equipment regulated under §63.1255. * * * * * **§ 63.1511**  **[Amended]** 11. By revising § 63. 1511(c)(9) as follows: **§63.1511 Performance test/compliance demonstration general**  **requirements.** * * * * * (c) * * * (9) Method 26A for the concentration of HCl. Where a lime
injected fabric filter is used as the control device to comply with the 90 percent reduction standard, the owner o r operator must measure the fabric filter inlet concentration of HCl at a point before lime is introduced to the system. Method 26 may be used in place of Method 26A where it can be demonstrated that there are no water droplets inPage **124** of **161**

the emission stream. This can be demonstrated by showing that the vapor pressure of water in the emission stream that you are testing is less than the equilibrium vapor pressure of water at the emission stream temperature, and by certifying that the emission stream is not controll ed by a wet scrubber.
* * * * * 12. By revising Table 2 of Subpart CCCC as follows: **Subpart CCCC —** 

**National Emission Standards for Hazardous Air Pollutants: Manufacturing of Nutritional Yeast**  *** * * * ***Page **125** of **161**

**Table 2 to Subpart CCCC of Part 63 —**  **Requirements for Performance**  **Tests** As stated in §63.2161, if you demonstrate compliance by monitoring brew ethanol, you must comply with the requirements for performance tests in the following table: [Brew Ethanol Monitoring Only] **For each fed -**  **batch fermenter for which**  **compliance is determined by monitoring brew ethanol**  **concentration and calculating VOC concentration in the fermenter**  **exhaust according to the procedures in §63.2161, you must** 
**... Using**  **... According to the**  **following requirements**  **...**

1. Measur e VOC as propane Method 25A*, or an alternative validated by EPA Method 301* and approved by the Administrator You must measure the VOC concentration in the fermenter exhaust at any point prior to the dilution of the exhaust stream. *EPA Test Methods found in **Appendix** A of 40 CFR part 60 *** * * * *** 13. By revising Table 4 in the appendix to Subpart UUUU as follows: **Subpart UUUU** 

**— National Emission Standards for Hazardous Air Pollutants**  **for Cellulose Products Manufacturing**  *** * * * *** **Table 4 to Subpart UUUU of Part 63 —**  **Requirements for Performance Tests** Page **126** of **161**

As required in §§63.5530(b) and 63.5535(a), (b), (g)(1), and (h)(1), you must conduct performance tests, other initial compliance demonstrations, and CEMS perf ormance evaluations and establish operating limits according to the requirements in the following table:

**For . . . at . . .**  **you must .**

**. . using . . .**  **according to the following**  **requirements . .**

**.** 1. the sum of all process vents a. each

existing or new affected source i. select

sampling port's location and the number of traverse points; EPA Method 1 or

1A in Appendix A to 40 CFR §63.7(d)(1)(i); sampling sites must be located at the inlet and outlet to each control device;

ii. determine velocity and volumetric flow rate; EPA Method 2, 2A,

2C, 2D, 2F, or 2G in A ppendix A to part 60 of this chapter; you may use EPA Method 2A, 2C, 2D, 2F, or 2G as an alternative to using EPA Method 2, as appropriate; iii. conduct gas analysis; and , (1) EPA Method 3,

3A, or 3B in A ppendix A to part 60 of this chapter; or , you may use EPA Method 3A or 3B as an alternative to using EPA Method 3; or , (2) ASME PTC 19.10

– 1981

— Part 10; and , you may use ASME PTC 19.10

– 1981

— Part 10 (available for purchase from Three Park Avenue, New York, NY 10016

– 5990) asPage **127** of **161** an alternative to using EPA Method 3B. iv. measure moisture content of the stack gas . EPA Method 4 in

A ppendix A to part 60 of this chapter
.
2. the sum of all viscose process vents a. each

existing or new viscose process source i. measure

total sulfide emissions (1) EPA Method 15

in Appendix A to part 60 of this chapter; or (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you must conduct testing of emissions from continuous viscose process vents and combinations of batch and continuous viscose process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (c) you must conduct testing of emissi ons from batch viscose process vents as specified in §63.490(c), except that the emission reductionsPage **128** of **161** required for process vents under this subpart supersede the emission reductions required for process vents under subpart U of this part; and (d) you must c ollect CPMS data during the period of the initial compliance demonstration and determine the CPMS operating limit during the period of the initial compliance demonstration; or (2) carbon disulfide and/or hydrogen sulfide CEMS, as applicable ; (a) you must measure emissions at the inlet and outlet of each control device using CEMS; (b) you must install, operate, and maintain the CEMS according to the applicable performance specification (PS

– 7, PS

– 8, PS

– 9, or PS

– 15) of 40 CFR part 60, appendix B; and (c) you mustPage **129** of **161** collect CEMS emissions data at the inlet and outlet of each control device during the period of the initial compliance demonstration and determine the CEMS operating limit during the period of the initial compliance demonstration. 3. the sum of all solvent coating process vents a. each

existing or new cellophane operation i. measure

toluene emissions (1) EPA Method 18

in A ppendix A to part 60 of this chapter, or Method 320 in appendix A to part 63, or (a) you must conduct testi ng of emissions at the inlet and outlet of each control device; (b) you may use EPA Method 18 or 320 to determine the control efficiency of any control device for organic compounds; for a combustion device, you must use only HAP that are present in the inl et to the control device to characterize the percent reduction across the combustionPage **130** of **161** device; (c) you must conduct testing of emissions from continuous solvent coating process vents and combinations of batch and continuous solvent coating process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch solvent coating process vents as specified in §63.490(c), except that the emission reductions required for process v ents under this subpart supersede the emission reductions required for process vents under subpart U of this part; andPage **131** of **161** (e) you must collect CPMS data during the period of the initial compliance demonstration and determine the CPMS operating limit during the initial compliance demonstration; or (2) ASTM D6420

– 99 (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use ASTM D6420

– 99 (available for purchase from at least one of the following addresses: 100 Barr Harbor Drive, West Conshohocken, PA 19428

– 2959; or University Microfilms International, 300 North Zeeb Road, Ann Arbor, MI 48106) as an alternative to EPA Method 18 only where: the target compound(s) arePage **132** of **161** those listed in Sectio n 1.1 of ASTM D6420

– 99; and the target concentration is between 150 parts per billion by volume (ppbv) and 100 ppmv; for target compound(s) not listed in Section 1.1 of ASTM D6420

– 99, but potentially detected by mass spectrometry, the additional system con tinuing calibration check after each run, as detailed in Section 10.5.3 of the ASTM method, must be followed, met, documented, and submitted with the data report even if there is no moisture condenser used or the compound is not considered water soluble; a nd for target compound(s) not listed in Section 1.1 of ASTM D6420

– 99 and not amenable to detection by massPage **133** of **161** spectrometry, ASTM D6420

– 99 does not apply; (c) you must conduct testing of emissions from continuous solvent coating process vents and combin ations of batch and continuous solvent coating process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch solvent coating process vents as specified in §63.490(c), exc ept that the emission reductions required for process vents under this subpart supersede the emission reductions required for process vents under subpart U of this part;Page **134** of **161**
and , (e) you must collect CPMS data during the period of the initial compliance demonstration and determine the CPMS operating limit during the period of the initial compliance demonstration. 4. the sum of all cellulose ether process vents a. each

existing or new cellulose ether operation i. measure

total organic HAP emissions (1) EPA Method 18

in A ppendix A to part 60 of this chapter or Method 320 in appendix A to part 63, or (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use EPA Method 18 or 320 to determine the control efficiency of any control device for organic compounds; for a combustion device, you must use only HAP that are present in the inlet to the control device to characterize the percent reduction across the combustionPage **135** of **161** device; (c) you must conduct testing of emissions from continuous cellulose ether process vents and combinations of batch and continuous cellulose ether process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch cellulose ether process vents as specified in §63.490(c), except that the emission reductions required for process vents under this subpart supersede the emission reductions required for process vents under subpart U of this part; andPage **136** of **161** (e) you must collect CPMS data during the period of the initial performance test and determine the CPMS operating limit during the period of the initial performance test; (2) ASTM D6420

– 99 (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use ASTM D6420

– 99 (available for purchase from at least one of the following addresses: 100 Barr Harbor Drive, West Conshohocken, PA 19428

– 2959; or University Microfilms Internati onal, 300 North Zeeb Road, Ann Arbor, MI 48106) as an alternative to EPA Method 18 only where: the target compound(s) are those listed inPage **137** of **161** Section 1.1 of ASTM D6420

– 99; and the target concentration is between 150 ppbv and 100 ppmv; for target compound(s) no t listed in Section 1.1 of ASTM D6420

– 99, but potentially detected by mass spectrometry, the additional system continuing calibration check after each run, as detailed in Section 10.5.3 of the ASTM method, must be followed, met, documented, and submitted w ith the data report even if there is no moisture condenser used or the compound is not considered water soluble; and for target compound(s) not listed in Section 1.1 of ASTM D6420

– 99 and not amenable to detection by mass spectrometry, ASTM D6420

– 99 does no t apply;Page **138** of **161** target concentration is between 150 ppbv and 100 ppmv for target compound(s). (c) you must conduct testing of emissions from continuous cellulose ether process vents and combinations of batch and continuous cellulose ether process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch cellulose ether process vents as specified in §63.490(c), except that the emission reductions required for process vents und er this subpart supersede the emission reductions required forPage **139** of **161** process vents under subpart U of this part; and (e) you must collect CPMS data during the period of the initial performance test and determine the CPMS operating limit during the period of the initial performance test
. (3) EPA Method 25 in A ppendix A to part 60 of this chapter; or (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use EPA Method 25 to determine the control efficiency of combustion devices for organic compounds; you may not use EPA Method 25 to determine the control efficiency of noncombustion control devices; (c) you must conduct testingPage **140** of **161** of emissions from continuous cellulose ether process vents and combinations of batch and continuous cellulose ether process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch cellulose ether process vents as specified in §63.49 0(c), except that the emission reductions required for process vents under this subpart supersede the emission reductions required for process vents under subpart U of this part; and (e) you must collect CPMS data during the period of the initial pe rformance test and determine thePage **141** of **161** CPMS operating limit during the period of the initial performance test; or (4) EPA Method 25A in A ppendix A to part 60 of this chapter (a) you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use EPA Method 25A if: an exhaust gas volatile organic matter concentration of 50 ppmv or less is required in order to comply with the emission limit; the volatile organic matter concentration at the inlet to the control device and the required level of control are such as to result in exhaust volatile organic matter concentrations of 50 ppmv or less; or because of the high control efficiency of the control device,Page **142** of **161** the anticipated volatile organic matter concentration at the control device exhaust is 50 ppmv or less, regardless of the inlet concentration; (c) you must conduct testing of emissions from continuous cellulose ether process vents and combinations of batch and continuous cellulose ether process vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535; (d) you must conduct testing of emissions from batch cellulose ether process vents as specified in §63.490(c), except that the emission reductions required for process vents unde r thisPage **143** of **161** subpart supersede the emission reductions required for process vents under subpart U of this part; and , (e) you must collect CPMS data during the period of the initial performance test and determine the CPMS operating limit during the period of the initial performance test. 5. each toluene storage vessel a. each

existing or new cellophane operation i. measure

toluene emissions (1) EPA Method 18

in A ppendix A to part 60 of this chapter or Method 320 in appendix A to part 63 ; or (a) if venting to a control device to reduce emissions, you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use EPA Method 18 or 320 to determine the control efficiency of any control device for organic compounds; for a combustion device, you mustPage **144** of **161** use only HAP that are present in the inlet to the control device to characterize the percent reduction across the combustion device; (c) you must conduct testing of emissions from continuous storage vessel vents and combinations of batch and continuous storage vessel vents at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535 for continuous process vents; (d) you must conduct testing of emissions from batch storage vessel vents as specified in §63.490(c) for batch process vents, except that the emission reductions required for process ventsPage **145** of **161** under this subpart supersede the emission reductions required for proce ss vents under subpart U of this part; and , (e) you must collect CPMS data during the period of the initial compliance demonstration and determine the CPMS operating limit during the period of the initial compliance demonstration; or (2) ASTM D6420

– 99 (a) if venting to a control device to reduce emissions, you must conduct testing of emissions at the inlet and outlet of each control device; (b) you may use ASTM D6420

– 99 (available for purchase from at least one of the following addresses: 100Page **146** of **161** Barr Harbor Drive, West Conshohocken, PA 19428

– 2959; or University Microfilms International, 300 North Zeeb Road, Ann Arbor, MI 48106) as an alternative to EPA Method 18 only where: the target compound(s) are those listed in Section 1.1 of A STM D6420

– 99, and the target concentration is between 150 ppbv and 100 ppmv; for target compound(s) not listed in Section 1.1 of ASTM D6420
- 99, but potentially detected by mass spectrometry, the additional system continuing calibration check after each ru n, as detailed in Section 10.5.3 of the ASTM method, must be followed, met, documented, and submitted with the data report even ifPage **147** of **161** there is no moisture condenser used or the compound is not considered water soluble; and for target compound(s) not listed in Section 1.1 of ASTM D6420

– 99 and not amenable to detection by mass spectrometry, ASTM D6420

– 99 does not apply; (c) you must conduct testing of emissions from continuous storage vessel vents and combinations of batch and continuous storage vessel ve nts at normal operating conditions, as specified in §§63.7(e)(1) and 63.5535 for continuous process vents; (d) you must conduct testing of emissions from batch storage vessel vents as specified inPage **148** of **161** §63.490(c) for batch process vents, except that the emission reductions required for process vents under this subpart supersede the emission reductions required for process vents under subpart U of this part; and , (e) you must collect CPMS data during the period of the initial compliance demonstratio n and determine the CPMS operating limit during the period of the initial compliance demonstration. 6. the sum of all process vents controlled using a flare a. each

existing or new affected source i. measure

visible emissions (1) EPA Method 22

in A ppendix A to part 60 of this chapter (a) you must conduct the flare visible emissions test according to §63.11(b).

7. equipment a. each

existing or new i. measure

leak rate (1) applicable

equipment leak test methods in (a) you must follow all requirements forPage **149** of **161**

leaks cellulose

ether operation §63.180; or the applicable equipment leak test methods in §63.180; or (2) applicable equipment leak test methods in § 63.1023 (a) you must follow all requirements for the applicable equipment leak test methods in §63.1023. 8. all sources of wastewater emissions a. each

existing or new cellulose ether operation i. measure

wastewater HAP emissions (1) applicable

wastewater test methods and procedures in §§63.144 and 63.145; or (a) You must follow all requirements for the applicable wastewater test methods and procedures in §§63.144 and 63.145; or (2) applicable wastewater test methods and procedures in §§63.144 and 63.145, using ASTM D5790

– 95 as an alternative to EPA Method 624 in A ppendix A to part 163 of this chapter (a) you must follow all requirements for the applicable waste water test methods and procedures in §§63.144 and 63.145, except that you may use ASTM D5790

– 95 (available for purchase from at least one of the following addresses: 100 Bar r Harbor Drive, West Conshohocken, PAPage **150** of **161** 19428

– 2959; or University Microfilms International, 300 North Zeeb Road, Ann Arbor, MI 48106) as an alternative to EPA Method 624, under the condition that this ASTM method be used with the sampling procedures of EPA M ethod 25D or an equivalent method. 9. any emission point a. each

existing or new affected source using a CEMS to demonstrate compliance i. conduct

a CEMS performance evaluation (1) applicable

requirements in §63.8 and applicable performance specification (PS

– 7, PS

– 8, PS

– 9, or PS

– 15) in A ppendix B to part 60 of this chapter (a) you must conduct the CEMS performance evaluation during the period of the initial compliance demonstration according to the applicable requirements in §63.8 and the applicab le performance specification (PS

– 7, PS

– 8, PS

– 9, or PS

– 15) of 40 CFR part 60, A ppendix B; (b) you must install, operate, and maintain the CEMS according toPage **151** of **161** the applicable performance specification (PS

– 7, PS

– 8, PS

– 9, or PS

– 15) of 40 CFR part 60, A pp endix B; and (c) you must collect CEMS emissions data at the inlet and outlet of each control device during the period of the initial compliance demonstration and determine the CEMS operating limit during the period of the initial compliance demon stration.

* * * * * 14. By revising Table 4 in the appendix to Subpart ZZZZ as follows: **Subpart ZZZZ**  **—**

**National Emission Standards for Hazardous Air Pollutants**  **for Stationary Reciprocating Internal Combustion Engines** * * * * * **Table 4 to Subpart ZZZZ of Part 63**  **— Requirements for Performance Tests**  [ As stated in §§63.6610, 63.6611 , 63.6620, and 63.6640, you must comply with the following requirements for performance tests for stationary RICE ]Page **152** of **161**

**For each .**

**. . Complying** 

**with the requirement**  **to . . . You**  **must . .**

**. Using . . .**  **According to the following**  **requirements .**

**. .** 1. 2SLB, 4SLB, and CI stationary RICE a. Reduce CO

emissions i. Measure

the O 2 at the inlet and outlet of the control device; and (1) Portable CO

and O 2 analy

zer (a) Using ASTM D6522

– 00 (2005) a (heated probe not necessary ; single
- point sampling ) (incorporated by reference, see §63.14). Measurements to determine O 2 must be made at the same time as the measurements for CO concentration. ii. Measure the CO at the inlet and the outlet of the control device
. (1) Portable CO

and O 2 analy

zer (a) Using ASTM D6522

– 00 (2005) a (heated probe not necessary ; single
- point sampling ) (incorporated by reference, see §63.14) or Method 10 of 40 CFR part 60 , appendix A. The CO concentration must be at 15 percent O 2 , dry basis. 2. 4SRB stationary RICE a. Reduce

formaldehyde emissions i. Sample at the

centroid of the (a) Sampling sites must be located at thePage **153** of **161** exhaust; inlet and outlet of the control device. ii. Measure O 2 at the inlet and outlet of the control device; (1) Method 3 or

3A or 3B of 40 CFR part 60, A ppendix A, or ASTM Method D6522

– 00 (2005 ) (heated probe not necessary ; single
point sampling ). (a)

Measurements to determine O 2 concentration must be made at the same time as the measurements for formaldehyde concentration. iii. Measure moisture content at the inlet and outlet of the control device; and , (1) Method 4 of

40 CFR part 60, A ppendix A, or Test Method 320 of 40 CFR part 63, A ppendix A, or ASTM D 6348

– 03 (a)

Measurements to determine moisture content must be made at the same time and location as the measurements for formaldehyde concentration. iv. Measure formaldehyde at the inlet and the outlet of the control device
. (1) Method 320

or 323 of 40 CFR part 63, A ppendix A; or ASTM D6348

– 03 b , provided in ASTM D6348

– 03 Annex A5 (Analyte Spi king Technique), the percent R must be greater than or equal to 70 (a)

Formaldehyde concentration must be at 15 percent O 2 , dry basis. Results of this test consist of the average of the three 1
- hour or longer runs.Page **154** of **161** and less than or equal to 130 3. Station ary RICE a. Limit the

concentration of formaldehyde in the stationary RICE exhaust i. Sample at the

centroid of the exhaust; (a) If using a control device, the sampling site must be located at the outlet of the control device. ii. Determine the O 2 concentration of the stationary RICE exhaust at the sampling port location; (1) Method 3 or

3A or 3B of 40 CFR part 60, A ppendix A, or ASTM Method D6522

– 00 (2005) (heated probe not necessary ; single
point sampling ). (a)

Measurements to determine O 2 concentration must be made at the same time and location as the measurements for formaldehyde concentrati on. iii. Measure moisture content of the stationary RICE exhaust at the sampling port location; and , (1) Method 4 of

40 CFR part 60, A ppendix A, or Test Method 320 of 40 CFR part 63, A ppendix A, or ASTM D 6348

– 03 (a)

Measurements to determine moisture content must be made at the same time and location as the measurements for formaldehyde concentration. iv. Measure formaldehyde at the exhaust of the stationary (1) Method 320

or 323 of 40 CFR part 63, A ppendix A; or ASTM D6348

– 03 b , provided in ASTM (a)

Formaldehyde concentration must be at 15 percent O 2 , dry basis. Results of th is testPage **155** of **161** RICE . D6348

– 03 Annex

A5 (Analyte Spiking Technique), the percent R must be greater than or equal to 70 and less than or equal to 130 consist of the

average of the three 1
- hour or longer runs.

a You may also use Methods 3A and 10 as options to ASTM

– D6522

– 00 (2005). You may obtain a copy of ASTM

– D6522

– 00 (2005) from at least one of the following addresses: American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428

– 2959, or University Microfilms International, 300 North Zeeb Road, Ann Arbor, MI 48106.

b You may obtain a copy of ASTM

– D6348

– 03 from at least one of the following addresses: American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428

– 2959, or University Microfilms International, 300 North Zeeb Road, Ann Arbor, M I 48106.
* * * * * 15. In Method 306 of Appendix A by revising S ection s 2.2.1, 6.1.4, and 8.0 as follows: **Method 306 —** 

**Determination of Chromium Emissions From Decorative and Hard Chromium Electroplating and Chromium Anodizing Operations**  **— Isokinetic Method**  * * * * *
2.2.1 Total chromium samples with high chromium concentrations ( ≥35 μg/L) may be analyzed using inductively coupled plasma emission spectrometry (ICP) at 267.72 nm. Note: The ICP analysis is applicable for this method only when the solution analyzed has a Cr concentration greater than or equal toPage **156** of **161**

35 μg/L or five times the method detection limit as determined according to Appendix B in 40 CFR p art 136. Similarly, inductively coupled plasma
- mass spectroscopy (ICP
- MS) may be used for total chromium analysis provided the procedures for ICP
- MS analysis described in Method 6020 or 6020A (EPA Office of Solid Waste, publication SW
- 846) are followed .
* * * * *
6.1.4 Operating and maintenance procedures for the sampling train are described in APT D

– 0576 of Method 5. Users should read the APTD

– 0576 document and adopt the outlined procedures. Alternative mercury - free thermometers may be used if the thermometers are, at a minimum, equivalent in terms of performance or suitably effective for the specif ic temperature measurement application.
* * * * * 8.0 Sample Collection, Preservation, Holding Times, Storage, and Transport Note: Prior to sample collection, consideration should be given to the type of analysis (Cr +6 or total Cr) that will be performed. Which analysis option(s) will be performed will determine which sample recovery and storage procedures will be required to process the sample . * * * * *Page **157** of **161**

16. In Method 306A of Appendix A by revising S ection 8.2 as follows: **Method 306A —**  **Determination of Chromium Emissions From Decorative and Hard Chromium Electroplating and Chromium Anodizing Operations**  * * * * *
8.2 Sample Recovery. After the train has been transferred to the sample recovery area, disconnect the tubing tha t connects the jar/impingers. The tester shall select either the total Cr or Cr+ 6 sample recovery option. Samples to be analyzed for both total Cr and Cr+6 shall be recovered using the Cr+6 sample option (Section 8.2.2). Note: Collect a reagent blank sample for each of the total Cr or the Cr+6 analytical options. If both analyses (Cr and Cr+6) are to be conducted on the samples, collect separate reagent blanks for each analysis. Also, s ince particulate matter is not usually present at chromium electrop lating and/or chromium anodizing operations, it is not necessary to filter the Cr +6 samples unless there is observed sediment in the collected solutions. If it is necessary to filter the Cr +6 solutions, please refer to Method 0061, Determination of Hexaval ent Chromium Emissions from Stationary Sources, Section 7.4, Sample Preparation in SW
- 846 (see Reference 1).
* * * * * 17. In Method 308 of Appendix A by revising S ection 10.1.3 as follows:Page **158** of **161**

**Method 308 —**  **Procedure for Determination of Methanol Emission From Stationary Sources**  * * * * *
10.1.3 Temperature Sensors. Calibrate against mercury
- in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * * 18. In Method 315 of Appendix A by revising S ection s 6.1.1 and 10.5 and by redesignating Section 8.11 as 8.1 and revising as follows: **Method 315 —**  **Determination of Particulate and Methylene Chloride Extractable Matter (MCEM) From Selected Sources at Primary Aluminum**  **Production Facilities** * * * * *
6.1.1 Sampling train. A schematic of the sampling train used in this method is shown in Figure 5

– 1, Method 5, 40 CFR part 60, A ppendix A. Complete construction details are given in APTD

– 0581 (Reference 2 in section 17.0 of this method); commercial models of this train are also available. For changes from APTD

– 0581 and for allowable modifications of the train shown in Figure 5

– 1, Method 5 , 40 CFR part 60, A ppendix A, see the following subsections. Note: The operating andPage **159** of **161**

maintenance procedures for the sampling train are described in APTD

– 0576 (Reference 3 in section 17.0 of this method). Since correct usage is important in obtaini ng valid results, all users should read APTD

– 0576 and adopt the operating and maintenance procedures outlined in it, unless otherwise specified herein . Alternative mercury
- free thermometers may be used if the thermometers are, at a minimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application. The use of grease for sealing sampling train components is not recommended because many greases are soluble in methylene chloride. The sampling train consists of the following components:
* * * * *
8. 1 Pretest preparation. It is suggested that sampling equipment be maintained according to the procedures described in APTD

– 0576. Alternative mercury
- free thermometers may be used if the thermometers are at a mini mum equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * *
10.5 Temperature sensors. Use the procedure in S ection 10.3 of Method 2, 40 CFR part 60, A ppendix A to calibrate in
- stack temperature sensors. Dial thermometers, such as are used for the DGM and condenser outlet, shall be calibrated against mercury
- in
- glassPage **160** of **161**

thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a m inimum, equivalent in terms of performance or suitably effective for the specific temperature measurement application.
* * * * * 19. In Method 316 of Appendix A by revising S ection 10.5 as follows: **Method 316 —**  **Sampling and Analysis for Formaldehyde Emissions From**  **Stationary Sources in the Mineral Wool and Wool Fiberglass Industries** * * * * *
10.5 Temperature gauges: Use the procedure in S ection 4.3 of EPA Method 2 to calibrate in
- stack temperature gauges. Dial thermometers , such as are used for the dry gas meter and condenser outlet, shall be calibrated against mercury
- in
- glass thermometers. An alternative mercury
- free thermometer may be used if the thermometer is, at a minimum, equivalent in terms of performance or suitabl y effective for the specific temperature measurement application.
* * * * * 20. In Method 321 of Appendix A by revising the definition for the term “D f ” after equation (2) in Section 9.3.1 as follows:Page **161** of **161**

**Test Method 321 —** 

**Measurement of Gaseous Hydrogen Chloride Emissions at**  **Portland Cement Kilns by Fourier Transform Infrared (FTIR) Spectroscopy**  * * * * * 9.3 * * *

D F = D ilution Factor (Total flow/Spike flow). T otal flow = spike flow plus effluent flow.
* * * * *