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Test Procedures, Methods and Reporting Requirements for 

the Information Collection Request for Petroleum Refineries 

This document provides an overview of approved methods, target pollutants and units of 

measure, and reporting requirements for petroleum refineries. All recipients must complete and 

submit test results within 6 months of receipt of your Section 114 letter. This document will be 

referred to as the ‘petroleum refinery test program.’ The document is organized as follows: 

1.0 Testing Procedures and Methods 

2.0 How to Report Data 

3.0 How to Submit Data 

4.0 Contact Information for Questions on Test Plan and Reporting 

1.0 Testing Procedures and Methods 

The EPA petroleum refinery test program requires emissions and other test data for several 

pollutants, including specific hazardous air pollutants (HAP), criteria pollutants, and potential 

surrogate groups. If EPA is requesting that you complete emissions testing, the cover letter of 

this packet (CAA section 114 letter) will include a list of emissions sources selected for testing. 

For each petroleum refinery emissions source listed in your Section 114 letter, you must perform 

an emissions test for some combination of pollutants (i.e., simultaneous or overlapping 

measurements per group) and diluents according to the test protocols presented in Sections 1.1 

through 1.4 of this section. 

Please refer to your Section 114 letter for additional testing information. As noted previously, 

the Section 114 letter includes the specific sources for which we are requesting that you perform 

emissions testing. Please note that you do not have to submit a test plan to EPA for approval 

prior to testing; however, we recommend that you prepare a test plan for your own use to assist 

in the planning and to ensure that you address all of the testing and reporting requirements. 

Please note that you also must report your process and emissions testing data using the EPA 

Electronic Reporting Tool (ERT), where applicable. The ERT requires you to report most 

elements of a test plan. Enclosure 7 of this ICR provides an example of the EPA ERT test plan. 

You are directed to the ERT (http://www.epa.gov/ttn/chief/ert/ert_tool.html) for a more complete 

and interactive description of these test plan elements. 

You must follow all of the procedures as specified in the test methods, including the quality 

assurance and quality control measures, and document the results in the ERT and in any test 

report provided to EPA. For this program, you need not obtain audit materials from your state or 

local agency or from EPA. You may apply any third party audit materials you have on hand and 

document the results, but you are not required to do so. 

You may have submitted test data for some of these pollutants already. If you have conducted 

any of the requested groups of tests (i.e., any complete set of tests required to be conducted 

simultaneously) in the past 5 years and reported the data in Part IV of Enclosure 1 of this ICR, 

you are not required to do additional testing for those pollutants. 
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1.1 Stack Test Methods 

The following emissions sources must follow the stack test method procedures described in this 

section: 

• Fluid catalytic cracking unit 

• Thermal catalytic cracking unit 

• Fluid coking unit (including flexicoking units) 

• Delayed coking unit 

• Catalytic hydrocracking unit 

• Hydrogen production unit 

• Asphalt blowing still 

• Sulfur recovery unit 

During a 30-day period that includes emissions testing and fuel analysis, you should also collect 

relevant process data, such as: total heat input; material description, composition, and feed rate; 

coke burn-off rate; emissions control devices in use during the test; control device operating or 

monitoring parameters (including, as appropriate to the control device, flue gas flow rate, 

pressure drop, scrubber liquor pH, scrubber liquor flow rate, sorbent type and sorbent injection 

rate, primary and secondary voltage and current, temperature); process parameters (such as type 

of crude, oxygen concentration, temperature); and any pollution prevention or other hazardous 

air pollutant emission reduction approaches being implemented during the test program. You 

should report the above process data as daily averages in the Process Data spreadsheet; you can 

download this spreadsheet from the ICR website (http://icr2010.rti.org, click on “Petroleum 

Refineries”). For process data that you record during testing, make clear, using the Notes section 

of the ERT or spreadsheet, the correlation between emissions measurements and process data 

(e.g., identify Method 23, run 1 for the associated process data on the process data details tab of 

the ERT). 

The owner/operator of the petroleum refinery must certify that the unit tested was operating in a 

normal and representative manner during the performance test. The owner/operator must also 

certify that it operated the pollution control equipment, if any, on the unit tested in accordance 

with manufacturers’ specifications and requirements for proper operation during the emissions 

testing. 

1.1.1 Sample Location and Gas Composition Analysis Methods 

You must use U.S. EPA Method 1 of Appendix A-1 to 40 CFR Part 60 to select the locations and 

number of traverse points for sampling for the tests in this section. See 

http://www.epa.gov/ttn/emc/methods/method1.html for a copy of the method and guidance 

information for sampling situations not meeting Method 1 criteria. 

For analysis of flue gas composition, including oxygen concentration, you must use U.S. EPA 

Method 3A or 3B of Appendix A-2 to 40 CFR Part 60. See 

http://www.epa.gov/ttn/emc/methods/method3a.html for Method 3A or 

http://www.epa.gov/ttn/emc/methods/method3b.html for Method 3B information. 
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1.1.2 Emissions Measurement Methods 

Table 1.1 summarizes the testing required to be performed for each type of process unit. Where 

indicated in the tables, you must conduct the tests for the indicated pollutants simultaneously for 

your process unit. If the table does not indicate simultaneous sampling is required for multiple 

pollutants, you may still choose to do so. For example, if you are asked to test your fluid 

catalytic cracking unit, you may conduct four separate sets of tests, one set that includes all 

pollutants indicated with an “a”, another set that includes all pollutants marked with a “b,” etc., 

or you may choose to conduct all the testing at the same time (if possible). 

Table 1.2 presents a list of the test methods to use for completing the tests required in Table 1.1. 

Tables 1.3 through 1.5 provide listings of target analytes for volatile and semi-volatile organic 

HAP and aldehyde test methods. Table 1.6 provides a listing of target analytes for C1 through 

C5 hydrocarbons. For copies of the U.S. EPA test methods, continuous emissions monitoring 

systems (CEMS) performance specifications, and additional information, please refer to EPA’s 

Emission Measurement Center website, http://www.epa.gov/ttn/emc/, and EPA’s Hazardous 

Waste website, http://www.epa.gov/waste/hazard/testmethods/sw846/online/index.htm, as 

appropriate. If you would like to use a method not on this list, please contact EPA for approval 

of an alternative method. Please see Section 4.0 of this document for a list of persons to contact 

with questions regarding test methods and reporting. 

Report all pollutant emission data as indicated in Table 1.2. Report the results of your emissions 

tests according to the directions provided in Section 2.0 of this enclosure. 

Unless otherwise specified, each pollutant emissions test should consist of at least three test runs 

for the sampling duration and/or volume indicated for each specified unit or operation. You 

should collect emissions samples for the identified pollutants downstream of the last relevant 

emissions control device (i.e., stack or other point representing the composition of the flue gases 

at the exit to the atmosphere), unless otherwise indicated. 

You must keep the following records for 3 years: 

• Documentation that each emissions test was conducted in accordance with the enclosed 

sampling protocol; and 

• The results of each emissions test. 
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Table 1.1: Required Test Matrix for Process Units by Process Type 

Process Unit 

Catalytic 

Reforming 

Pollutant1

Delayed Coking2

Fluid Catalytic 

Cracking, 

Thermal 

Catalytic 

Cracking, Fluid 

Coking, 

Catalytic 

Hydrocracking2

Purge 

Vent2

Coke Burn 

Vent2

Hydrogen 

Production2

Asphalt Blowing2

Sulfur Recovery2

Speciated Volatile Organic HAP a a a a a a a 

Speciated Semi-volatile Organic 

HAP a a a a a a 

Aldehydes a a a a a a 

Total hydrocarbons (THC) a a a a a a 

Methane and ethane a a a a a 

C1 through C5 hydrocarbons a 

Carbon Monoxide (CO) a a a a a a 

Dioxins and Furans (D/F), 

Polychlorinated biphenyls (PCB) b b b 

Hydrogen chloride (HCl), chlorine 

gas (Cl2), hydrogen fluoride (HF), 

and hydrogen cyanide (HCN) 

c e e 

Hydrogen sulfide (H2S), carbonyl 

sulfide ( COS), and carbon disulfide 

(CS2) 

c f f 

Total reduced sulfur compounds 

(TRS) c f f 

Mercury (Hg) d d d 

Hexavalent chromium (Cr+6) d3 

Other Metals d d d 

PM/PM2.5 (filterable) d d d 

PM2.5 (condensable) d d d 

Ammonia (NH3) d3 

Oxides of nitrogen (NOX) d d d g g 

Sulfur dioxide (SO2) d d d g g 

Gas flow rate a, b, c, d a, b, d, e a, b, d, e a, g a, f, g a, f 

Oxygen (O2) and Carbon dioxide 

(CO2) a, b, c, d a, b, d, e a, b, d, e a, g a, f, g a, f 

Moisture a, b, c, d a, b, d, e a, b, d, e a, g a, f, g a, f 

1

 Three runs per test, unless otherwise noted 

2

 For each process unit, simultaneous sampling for pollutants marked with same letter 

3

 For fluid catalytic cracking units and fluid coking units only 
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Table 1.2: Summary of Test Methods and Alternative Methods 

Pollutant Recommended Method Alternative Method Target Reported 

Units of Measure1

Speciated 

Volatile Organic 

HAP2

SW-846 Method 0031 with SW-846 

Method 8260B. Collect a minimum 

of four sets of adsorbent traps over 

each 1-hour period test run (total of 

three test runs).

 U.S. EPA Method 18. Use a 

minimum sample time of 1 hour 

per run. 

lb/hr and μg/dscm 

Speciated Semivolatile Organic 

HAP3

SW-846 Method 0010. Collect at 

least 4 cubic meters per each of three 

test runs. Use SW-846 Method 

8270C or D for the analytical finish. 

 lb/hr and μg/dscm 

Aldehydes4 SW-846 Method 0011 with SW-846 

Method 8315A. Collect a minimum 

volume of 1.3 cubic meters 

U.S. EPA Method 320 only if 

concentrations are known to be 

1 ppmvd or greater. Use a 

minimum test run time of 2 hours. 

lb/hr and μg/dscm 

THC U.S. EPA Method 25A. Use a 

minimum sampling time of 1 hour 

per run. Calibrate the measuring 

instrument with propane. 

You may calibrate the measuring 

instrument with a mixture 

representing the organic 

compounds being emitted. Provide 

the chemical make-up and 

response factors for the alternative 

standards; report the results as the 

alternative organic mixture and as 

propane equivalent concentrations. 

lb/hr and ppmvd as 

propane 

Methane and 

ethane 

U.S. EPA Method 18. Use a 

minimum sample time of 1 hour per 

run. 

U.S. EPA Method 320 lb/hr and ppmvd 

C1 through C5 

hydrocarbons5

U.S. EPA Method 18. Use a 

minimum sample time of 1 hour per 

run. 

U.S. EPA Method 320 lb/hr and ppmvd 

CO6 U.S. EPA Method 10 or 10B. Collect 

a minimum volume of 60 liters over a 

minimum sample time of 1 hour per 

run. 

None lb/hr and ppmvd 

D/F, PCB7 U.S. EPA Method 23. Collect a 

minimum volume of 3 cubic meters. 

Use high resolution GC/MS for the 

analytical finish. 

None lb/hr and pg/dscm 

HCl, Cl2, and 

HF 

U.S. EPA Method 26A. Collect a 

minimum volume of 2 cubic meters.. 

U.S. EPA Method 26 or U.S. EPA 

Method 320 if there are no 

entrained water droplets in the 

emissions stream. 

lb/hr and mg/dscm 

HCN U.S. EPA Conditional Test Method 

033 (CTM-033). Collect a minimum 

volume of 1 cubic meter with 

particular attention to maintaining the 

collection solution pH as per section 

4.1 of the method. 

U.S. EPA Method 320 if there are 

no entrained water droplets in the 

emissions stream. 

lb/hr and μg/dscm 

Hg ASTM D6784-02 (Ontario-hydro 

method). Collect a minimum volume 

of 3 cubic meters. 

U.S. EPA Method 30B only if you 

have the knowledge and capability 

to speciate mercury using this 

method. 

lb/hr and μg/dscm 
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Table 1.2: Summary of Test Methods and Alternative Methods (cont.) 

Pollutant Recommended Method Alternative Method Target Reported 

Units of Measure1

Hexavalent 

Chromium 

(Cr+6) 

SW-846 Method 0061. Collect a 

minimum sample volume of 3 cubic 

meters per run (or the maximum 

sample volume possible while 

maintaining the pH of first impinger 

solution above 8.5 if less than 3 cubic 

meters can be collected) and use a 

sample preconcentrator according to 

§4.4 and 4.5. 

None lb/hr and μg/dscm 

Metals8 U.S. EPA Method 29. Collect a 

minimum volume of 3 cubic meters 

per run. Use ICAP/MS or GFAAS 

for the analytical finish. For stacks 

without entrained water droplets, 

determine filterable PM emissions 

according to §8.3.1.1 with a filter 

temperature of 320°F +/- 25°F. For 

stacks with entrained water droplets, 

do not determine filterable PM with 

Method 29 (see PM/PM2.5 below). 

For stacks without entrained water 

droplets, you may opt to conduct a 

separate EPA Method 5 or 5F test 

with a filter temperature of 320°F 

+/- 25°F in lieu of measuring PM 

with the Method 29 train (see 

PM/PM2.5 below). 

lb/hr and mg/dscm 

PM/PM2.5

(filterable plus 

condensable)9 

from stacks 

without 

entrained water 

droplets (e.g., 

not from units 

with wet 

scrubbers)9

U.S. EPA Other Test Methods 27 

(OTM 27) and 28 (OTM 28). Collect 

a minimum volume of 2 cubic meters 

per run. 

None lb/hr and gr/dscf 

lb/hr and gr/dscf 

(if use Method 5F, 

report both total 

filterable catch and 

non-sulfate PM) 

PM/PM2.5

(filterable plus 

condensable)9 

from stacks with 

entrained water 

droplets 

AND 

Total Dissolved 

Solids (TDS) 

and Total 

Suspended 

Solids (TSS) 

from wet 

scrubber 

recirculation 

liquid9 

U.S. EPA Method 5 or 5B with a 

filter temperature of 320°F +/- 25°F 

and Other Test Method 28 (OTM 

28). Collect a minimum volume of 2 

cubic meters per run. 

AND 

ASTM D5907 For TDS and TSS, Standard 

Methods of the Examination of 

Water and Wastewater Method 

2540B for solids in scrubber 

recirculation liquid (as fed to the 

wet scrubber) 

lb/hr and gr/dscf 

AND 

mg solids per liter of 

scrubber 

recirculation liquid10

NH3 South Coast AQMD Method 207.1 U.S. EPA Conditional Test Method 

027 (CTM-027) 

lb/hr and ppmvd 

NOX 11 U.S. EPA Method 7E; 2-hr sample 

time 

U.S. EPA Method 7 lb/hr and ppmvd 
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Table 1.2: Summary of Test Methods and Alternative Methods (cont.) 

Pollutant Recommended Method Alternative Method Target Reported 

Units of Measure1

SO2

11 U.S. EPA Method 6C; 2-hr sample 

time 

U.S. EPA Method 6 lb/hr and ppmvd 

H2S, COS, CS2 U.S. EPA Method 15. Per method, a 

minimum of 16 individual samples 

during a period of 3 to 6 hours, per 

run 

None lb/hr and ppmvd 

TRS U.S. EPA Method 15A or 16A; 3-hr 

sample time per run; (one 3-hr 

sample per run or three 1-hr samples 

per run) 

U.S. EPA Method 16B combined 

with the analysis procedures of 

U.S. EPA Method 15. 

ppmvd 

Gas flow rate U.S. EPA Method 2 U.S. EPA Method 2A, 2B, 2C, 2D, 

2F, or 2G, as appropriate 

acfm, scfm, and 

dscfm 

O2/CO2 U.S. EPA Method 3A U.S. EPA Method 3B percent volume, dry 

Moisture U.S. EPA Method 4 None percent volume 

1

 lb/hr = pounds per hour; μg/dscm = micrograms per dry standard cubic meter; ppmvd = parts per million by volume, dry basis; 

pg/dscm = picograms per dry standard cubic meter; mg/dscm = milligrams per dry standard cubic meter; gr/dscf = grains per 

dry standard cubic foot; acfm = actual cubic feet per minute; scfm = standard cubic feet per minute; dscfm = dry standard 

cubic feet per minute. 

2

 Target analytes are given in Table 1.3; test runs must occur during the test runs for speciated semi-volatile organic HAP (i.e., 

one volatile organic HAP run conducted per each semi-volatile organic HAP run). 

3

 Target analytes are given in Table 1.4; use either SW-846 Method 8270C or 8270D for the analysis of Method 0010 samples. 

Follow SW-846 Method 3542 for Method 0010 sample train components extraction and preparation for analyses. This 

procedure will result in three separate sample fractions for analyses – the front half (filter and front half rinse), the back half 

(XAD-2 and back half rinse), and condensate (first impinger and impinger rinse). You may combine the three analytical 

fractions collected in the Method 0010 sampling train and analyze as one sample. If you choose this option rather than 

analyzing the fractions separately, you must track the various fractional extraction and condensate volumes carefully in order 

to calculate the relative in-stack concentrations correctly. You may use acetone followed by MeCl for the solvent rinse in lieu 

of the 50/50 MeCl/MeOH rinse (i.e., no liquid/liquid extraction). In addition, the analytical finish for either method should 

also employ high resolution gas chromatography and either low resolution or high resolution mass spectrometry with selective 

ion monitoring (SIM) specifically for targeted polycyclic aromatic hydrocarbons (PAH). 

4

 Target analytes are given in Table 1.5; test runs must occur during the test runs for speciated volatile and speciated semi-volatile 

organic HAP. 

5

 Target analytes for C1 through C5 hydrocarbons are given in Table 1.6; test runs must occur during the test runs for speciated

volatile and speciated semi-volatile organic HAP. 

6 If a unit has a certified CEMS installed for CO, you may report hourly averages from 30 days of CEMS data for the unit in lieu 

of conducting a CO stack test. In order to correlate these emissions with other stack test emissions, a portion of the CEMS 

data submitted should contain the emissions data collected during performance of the other requested stack tests and hourly O2

concentrations should also be provided, if continuously monitored. The CEMS must meet the requirements of Performance 

Specification 4 and 40 CFR 60.13 or the CEMS accuracy and ongoing QA/QC requirements of 40 CFR part 60, subpart J or 

Ja. Also provide the data of the most recent CEMS accuracy certification. 

7

 Just the 12 “dioxin-like” PCB congeners (IUPAC Numbers PCB-77, -81, -105, -114, -118, -123, -126, -156, -157, -167, -169, 

and -189) 

8 Metals to be tested include antimony (Sb), arsenic (As), beryllium (Be), cadmium (Cd), chromium (Cr), cobalt (Co), lead (Pb), 

manganese (Mn), nickel (Ni), and selenium (Se). 

9

 Conduct either the test for PM/PM2.5 (filterable) from stacks without entrained water droplets or the PM/PM2.5 (filterable) from 

stacks with entrained water droplets (with the TDS and TSS analysis), whichever is appropriate for your stack. 

10 Also report scrubber recirculation liquid flow rate in liters/min. 

11 If a unit has a certified CEMS installed for NOX and/or SO2, you may report hourly averages from 30 days of CEMS data for 

the unit in lieu of conducting a NOX and/or SO2 stack test. Also provide hourly O2 concentrations for the 30 days of CEMS 

data. In order to correlate these emissions with other stack test emissions, a portion of the CEMS data submitted should 

contain the emissions data collected during performance of the other requested stack tests. The CEMS must meet the 

requirements of Performance Specification 2 and 40 CFR 60.13 or the CEMS accuracy and ongoing QA/QC requirements of 

40 CFR part 60, subpart J or Ja. Also provide the data of the most recent CEMS accuracy certification. 
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NOTE: Special criteria apply for simultaneous sampling, sampling run time, and sample volumes 

for the semi-continuous and batch processes related to the delayed coking unit and cyclic and 

semi-regenerative catalytic reforming units. Sampling should be conducted over the duration of 

the venting cycle. For vent cycles lasting less than 6 hours, testing over a vent cycle constitutes a 

single test run. For venting cycles shorter than the specified sampling time (or insufficient to 

allow collection of the required sample volume), sampling over the duration of the vent cycle 

shall constitute an acceptable test run. For semi-regenerative catalytic reforming units (only one 

cycle), the anticipated venting cycle should be divided into three roughly equivalent periods, and 

testing over each period would constitute a single run so that the three test runs would cover the 

duration of the entire venting event. Generally, you will need to apply U.S. EPA Method 1A in 

sampling these locations. A sample testing plan for a delayed coking unit is provided on the ICR 

website (http://icr2010.rti.org, click on “Petroleum Refineries”); this testing plan may be used as 

guidance in developing testing plan for the particular batch emissions source required to be 

tested. 

Table 1.3: Target Volatile Analytes 

Compound CAS Number Compound CAS Number 

Acetone1 67-64-1 Methyl t-butyl ether2 91-20-3 

Acetonitrile 75-05-8 Methylene chloride 75-09-2 

Acrolein1 107-05-8 Naphthalene 91-20-3 

Acrylonitrile 107-13-1 Nitrobenzene 98-95-3 

Benzene 71-43-2 2-Nitropropane 79-46-9 

1,3-Butadiene2 106-99-0 Pentane2 109-66-0 

Carbon disulfide 75-15-0 Styrene 100-42-5 

Chlorobenzene 108-90-7 Tetrachloroethene 127-18-4 

Cumene (isopropylbenzene) 98-82-8 Toluene 108-88-3 

1,2-Dibromoethane 106-93-4 Trichloroethene 79-01-6 

Ethylbenzene 100-41-4 Triethylamine 121-44-8 

Hexane2 110-54-3 2,2,4 Trimethylpentane2 540-84-1 

Methanol1 67-56-1 Xylenes (mixed isomers) 1330-20-7 

Methyl isobutyl ketone 108-10-1 

1

 Analyte is not applicable to SW-846 Method 0031 sampling procedure. Collection of samples for these compounds is required 

only for hydrogen plant vent and requires collection in tedlar bags or evacuated canisters. 

2

 Not specifically listed as an analyte for SW-846 Method 8260B. 
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Table 1.4: Target Semi-volatile Analytes 

Compound CAS Number Compound CAS Number 

Acenaphthene 83-32-9 Dimethylaminobenzene 60-11-7 

Acenaphthylene 208-96-8 7,12-Dimethylbenz(a)anthracene 57-97-6 

Aniline 62-53-3 3,3’-Dimethylbenzidine 119-93-7 

Anthracene 120-12-7 α,α-Dimethylphenethylamine 122-09-8 

Benzidine1 92-87-5 2,4-Dimethylphenol 105-67-9 

Benz[a]anthracene 56-55-3 Fluoranthene 206-44-0 

Benzo[b]fluoranthene 205-99-2 Fluorene 86-73-7 

Benzo[k]fluoranthene 207-08-9 Indeno(1,2,3-cd)pyrene 193-39-5 

Benzo[g,h,i]perylene 191-24-2 Isophorone 78-59-1 

Benzo[a]pyrene 50-32-8 3-Methylcholanthrene 56-49-5 

Benzo[e]pyrene2 192-97-2 2-Methylnaphthalene 91-57-6 

Biphenyl2, 92-52-4 Naphthalene 91-20-3 

Cresol (mixed isomers) 1319-77-3 Perylene2 198-55-0 

Chrysene 218-01-9 Phenanthrene 85-01-8 

Dibenz[a,h]anthracene 53-70-3 Phenol 108-95-2 

Dibenzofuran 132-64-9 1,4-Phenylenediamine 106-50-3 

Dibenzo(a,e)pyrene 192-65-4 Pyrene 129-00-0 

3,3’-Dimethoxybenzidine 119-90-4 o-Toluidine 95-53-4 

1

 Notes non-reproducible chromatographic performance in SW-846 Method 8270D 

2

 Not specifically listed as an analyte for SW-846 Method 8270D 

Table 1.5: Aldehydes 

Compound CAS Number 

Formaldehyde 100-41-4 

Acetaldehyde 106-99-0 

Propanal 123-38-6 
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Table 1.6: C1 through C5 Hydrocarbons 

Description Compound CAS No. 

C1 Alkanes Methane 74-82-8 

C2 Alkanes Ethane 74-84-0 

C3 Alkanes Propane 74-98-6 

C4 Alkanes n-Butane 106-97-8 

 Isobutane 75-28-5 

C5 Alkanes n-Pentane 109-66-0 

 2-Methylbutane 78-78-4 

 Cyclopentane 287-92-3 

C2 Olefins Ethylene 74-85-1 

C2 Alkynes Acetylene 74-86-2 

C3 Olefins Propylene 115-07-1 

C4 Olefins 1-Butene 106-98-9 

 2-Butene 107-01-7 

 Isobutene 115-11-7 

C5 Olefins 1-Pentene 109-67-1 

 Cis-2-pentene 627-20-3 

 Trans-2-pentene 646-04-8 

 2-Methyl-1-butene 563-46-2 

 3-Methyl-1-butene 563-45-1 

 2-Methyl-2-butene 513-35-9 

 Cylcopentene 142-29-0 

C3 Alkadienes Propadiene 463-49-0 

C4 Alkadienes 1,2-Butadiene 590-19-2 

 1,3-Butadiene 106-99-0 

C5 Alkadienes 1,2-Pentadiene 591-95-7 

 1-cis-3-Pentadiene 1574-41-0 

 1-trans-3-Pentadiene 2004-70-8 

 1,4-Pentadiene 591-93-5 

 2,3-Pentadiene 591-96-8 

 3-Methyl-1,2-butadiene 598-25-4 

 2-Methyl-1,3-butadiene 78-79-5 

 Cyclopentadiene 542-92-7 

1.2 Fuel Gas Analysis Methods 

Table 1.7 describes the tests and procedures required for the analysis of your fuel gas. In 

addition to providing the results of the tests indicated in this section, you should also indicate 

whether the fuel gas system you tested includes gas from a coking unit. 

You will find copies of EPA methods at http://www.epa.gov/ttn/emc/tmethods.html. You can 

find instructions on how to obtain ASTM methods at http://www.astm.org/. 
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Table 1.7: Summary of Test Methods and Alternative Methods for Organic Compounds, Reduced 

Sulfur, and Other Parameters for Refinery Fuel Gas 

Pollutant Recommended Method Alternative Method Target Reported 

Units of Measure1

C1 through C5 

hydrocarbons 

plus benzene2 

ASTM D1945-03. Use a minimum 

sample time of 2 hours per run. 

U.S. EPA Method 18; U.S. EPA 

Method 320; ASTM D1946-90; 

GPA 2261-00; ASTM/UOP539-

97 

lb/hr and ppmvd 

H2S, COS, CS2

3

 U.S. EPA Method 15. Per method, 

a minimum of 16 individual 

samples during a period of 3 to 6 

hours, per run. 

 lb/hr and ppmvd 

TRS U.S. EPA Method 15A or 16A; 

3-hr sample time per run; (one 2-hr 

sample per run or three 40-minute 

samples per run) 

U.S. EPA Method 16B combined 

with the analysis procedures U.S. 

EPA Method 15. 

ppmvd 

Inorganics/other4 ASTM D1945-03 ASTM D1946-90; GPA 2261-00; 

ASTM/UOP 539-97 

Higher Heating 

Value 

Any of the following methods, as appropriate: 

ASTM D240-02 (Reapproved 2007), Standard Test Method for Heat of 

Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter; 

ASTM D1826-94 (Reapproved 2003), Standard Test Method for 

Calorific (Heating) Value of Gases in Natural Gas Range by Continuous 

Recording Calorimeter; 

ASTM D3588-98 (Reapproved 2003), Standard Practice for Calculating 

Heat Value, Compressibility Factor, and Relative Density of Gaseous 

Fuels 

 ASTM D4809-06, Standard Test Method for Heat of Combustion of 

Liquid Hydrocarbon Fuels by Bomb Calorimeter (Precision Method) 

 ASTM D4891-89 (Reapproved 2006), Standard Test Method for 

Heating Value of Gases in Natural Gas Range by Stoichiometric 

Combustion 

Gas Processors Association Standard 2172-09, Calculation of Gross 

Heating Value, Relative Density, Compressibility and Theoretical 

Hydrocarbon Liquid Content for Natural Gas Mixtures for Custody 

Transfer 

Calculated based on detailed gas compositional analysis using: ASTM 

D1945-03, Standard Method for Analysis of Natural Gas by Gas 

Chromatography; ASTM D1946-90 (Reapproved 2006), Standard 

Method for Analysis of Reformed Gas by Gas Chromatography; GPA 

2261-00, Analysis for Natural Gas and Similar Gaseous Mixtures by Gas 

Chromatography; or ASTM/UOP 539-97, Refinery Gas Analysis by Gas 

Chromatography 

 Any of the methods specified in section 2.2.7 of Appendix D to part 75 

MMBtu/scf 

Gas flow rate ASME MFC-3M, - 4M, -6M, -7M, 

-11M, -14M, or -18M; or AGA 

Report No. 11 (Measurement of 

Natural Gas by Coriolis Meter) 

U.S. EPA Method 2, 2A, 2B, 2C, 

2D, 2F, or 2G, as appropriate 

acfm, scfm, and 

dscfm 

Moisture U.S. EPA Method 4 None percent volume 

1

 lb/hr = pounds per hour; ppmvd = parts per million by volume, dry basis; MMBtu/scf = million British thermal units per 

standard cubic foot; acfm = actual cubic feet per minute; scfm = standard cubic feet per minute; dscfm = dry standard cubic 

feet per minute. 
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2

 Target analytes are given in Table 1.6, but include benzene (CAS No. 71-43-02) as a specific analyte.

3

 If your fuel gas system has a certified continuous monitoring system (CMS) installed to measure H2S concentrations, you may 

report daily averages from 30 days of data from that CMS in lieu of conducting a H2S test. In order to correlate these 

emissions with other emissions tests, a portion of the monitoring data submitted should contain the data collected during 

performance of the other requested tests. The CMS must meet the requirements of Performance Specification 7 or the 

accuracy and ongoing QA/QC requirements of 40 CFR part 60, subpart J or Ja. 

4

 Target analytes are given in Table 1.8. 

Table 1.8: Analytes for “Inorganics/Other” in Fuel or Flare Gas 

Compound CAS No. 

Hydrogen 1333-74-0 

Carbon monoxide 630-08-0 

Carbon dioxide 124-38-9 

Nitrogen 7727-37-9 

Oxygen 7782-44-7 
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1.3 Sampling and Analysis Methods for Cooling Water Systems 

Collect a sample from each cooling water system return line prior to exposure to air using “Air 

Stripping Method (Modified El Paso Method) for Determination of Volatile Organic Compound 

Emissions from Water Sources.”a

Table 1.9 describes the tests and procedures required for the analysis of your cooling water 

system sample. You will find copies of EPA methods at 

http://www.epa.gov/ttn/emc/tmethods.html. You can find instructions on how to obtain Standard 

Methods for the Examination of Water and Wastewater at http://www.standardmethods.org/. 

Table 1.9: Summary of Test Methods for Analysis via Texas El Paso Stripping Column 

Pollutant Recommended Method Alternative Method Target Reported Units of 

Measure1

Speciated 

Volatile Organic 

HAP2

Standard Methods 6200 for water 

U.S. EPA Method TO-15 for 

stripping air 

U.S. EPA Method TO-14A for 

stripping air 

ppmvd in air (as measured) 

and ppmw in cooling water 

Speciated Semivolatile Organic 

HAP3

Standard Methods 6410 for water 

U.S. EPA Method TO-13A for 

stripping air 

None ppmvd in air (as measured) 

and ppmw in cooling water 

Formaldehyde U.S. EPA Method TO-5 for 

stripping air. 

U.S. EPA Method TO-11A for 

stripping air 

ppmvd in air (as measured) 

and ppmw in cooling water 

(back-calculated) 

THC U.S. EPA Method TO-12 for 

stripping air. 

None ppmvd in air (as measured) 

and ppmw in cooling water 

(back-calculated) 

CH4 U.S. EPA Method 18. U.S. EPA Method 320 ppmvd in air (as measured) 

and ppmw in cooling water 

(back-calculated) 

HCl, Cl2 U.S. EPA Method 26 U.S. EPA Method 26A ppmvd in air (as measured) 

and ppmw in cooling water 

(back-calculated) 

1

 ppmvd = parts per million by volume, dry basis; ppmw = parts per million by weight 

2

 Target analytes are given in Table 1.3. 

3

 Target analytes are given in Table 1.4. 

 

a

 “Air Stripping Method (Modified El Paso Method) for Determination of Volatile Organic Compound Emissions 

from Water Sources” Revision Number One, dated January 2003, Sampling Procedures Manual, Appendix P: 

Cooling Tower Monitoring, prepared by Texas Commission on Environmental Quality, January 31, 2003. 
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1.4 Sampling and Analysis Methods for Enhanced Biodegradation Units (EBU) 

Table 1.10 lists the procedures required for the analysis of your EBU(s). You will find copies of 

EPA methods at http://www.epa.gov/ttn/emc/tmethods.html and copies of EPA SW-846 methods 

at http://www.epa.gov/waste/hazard/testmethods/sw846/online/index.htm. You can find 

instructions on how to obtain Standard Methods for the Examination of Water and Wastewater at 

http://www.standardmethods.org/. 

1.4.1 Sampling Methods 

You should follow the sampling methods described in the EPA document “Handbook for 

Sampling and Sample Preservation of Water and Wastewater” (EPA-600/4-82-029). 

Additionally, you should conduct sample collection and preservation in accordance to 40 CFR 

Part 136, which can be accessed at: http://www.epa.gov/region9/qa/pdfs/40cfr136_03.pdf. 

The sample chain-of-custody should also include the volumetric flow (m3/s), pH, and 

temperature of each sample. You should include this information with the results of this study. 

1.4.2 Sampling Location 

Influent: One (1) grab sample of each influent stream to the EBU 

EBU: One (1) grab sample within ten (10) feet of each influent location 

Effluent: One (1) grab sample of each effluent stream of the EBU 

1.4.3 Sampling Times 

The sampling and testing events (e.g., well-mixed assessment and Fbio determination) should 

occur at the same time and during normal operating conditions. 
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Table 1.10: Summary of Analytical Methods and Alternative Methods for Wastewater Treatment 

Systems 

Pollutant Recommended Method Alternative Method 

Target 

Reported 

Units of 

Measure1

Speciated Volatile 

Organic HAP2

SW-846 Method 8260B Standard Methods 6200 μg/L 

Speciated Semivolatile Organic 

HAP3

SW-846 Method 8270C or D Standard Methods 6410 μg/L 

Aldehydes4 SW-846 Method 8315A Standard Methods 6252 μg/L 

Sulfide (as S) EPA Method 376.1 Standard Methods 4500-S2- μg/L 

BOD5 5 EPA Method 405.1 Standard Methods 5210 mg/L 

COD 5 EPA Method 410.1 Standard Methods 5220 mg/L 

Well-mixed 

assessment

Technical Support Document for 

Evaluation of Thoroughly Mixed 

Biological Treatment Units, 1998.6

None N/A 

Site-specific 

biodegradation rates 

Appendix C to 40 CFR Part 63 – Aerated 

reactor batch test with oxygen addition 

(BOX test). Do one test using benzene as 

the sole substrate and perform a second 

test using benzene, toluene, xylene, and 

naphthalene at equal concentrations. 

Technical Support Document for 

the Evaluation of Aerobic 

Biological Treatment Units with 

Multiple Mixing Zones.7

(Fbio) 

1 μg/L = micrograms per liter; mg/L = milligrams per liter; Fbio = site-specific fraction of organic compounds biodegraded 

2

 Target analytes are given in Table 1.3. 

3

 Target analytes are given in Table 1.4. 

4

 Target analytes are given in Table 1.5. 

5

BOD5 = 5-day biological oxygen demand; COD = chemical oxygen demand. 

6

 A copy of this document is located at http://www.epa.gov/ttncaaa1/t3/reports/guidfn.pdf. 

7

 A copy of this document is located at http://www.epa.gov/ttn/caaa/t3/reports/mulmix5.pdf. 

2.0 How to Report Data 

The method for reporting the results of any testing and monitoring requests depend on the type of 

tests and the type of methods used to complete the test requirements. This section discusses the 

requirements for reporting the data. 

2.1 Reporting stack test data 

If you conducted testing using one of the methods listed in Table 2.1 you must report your data 

using the EPA Electronic Reporting Tool (ERT) Version 3. ERT is a Microsoft® Access 

database application. Two versions of the ERT application are available. If you are not a 

registered owner of Microsoft® Access, you can install the runtime version of the ERT 

Application. Both versions of the ERT are available at 

http://www.epa.gov/ttn/chief/ert/ert_tool.html. The ERT supports a Microsoft® Excel 

spreadsheet application (which is included in the files downloaded with the ERT) to document 
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the collection of the field sampling data. After completing the ERT, you will also need to attach 

an electronic copy of the emission test report (PDF format preferred) to the Attachments module 

of the ERT. 

Table 2.1: List of Test Methods Supported by ERT 

EPA Test Methods (40 CFR parts 60 and 61; EMC website, 

http://www.epa.gov/ttn/emc/tmethods.html; and SW 846, 

http://www.epa.gov/waste/hazard/testmethods/sw846/online/index.htm) 

Methods 1 through 4 (testing locations, velocity, moisture, dilution gases) 

Method 3A (O2 and CO2) 

Method 5 (filterable PM) 

Other test method (OTM) 27 (formerly Conditional test method (CTM) 40) (filterable PM2.5) 

OTM 28 (revised Method 202, formerly CTM 39) (condensable PM) 

Method 6C (SO2) 

Method 7E (NOX) 

Method 10 (CO) 

Method 17 (in-stack filterable PM) 

Method 23 (PCDD and PCDF) 

Method 25A (THC) 

Method 26A (HCl and HF) 

Method 29 (multiple metals including Hg) 

Method 101 (Hg) 

Method 101A (Hg) 

Method 201A 

Method 202 

CT Method 39 

CT Method 40 

At present, only the methods shown in Table 2.1 are supported by the ERT. If you conducted 

testing using a method not currently supported by the ERT, you must report the results of this 

test in a Microsoft® Excel Emission Test Template. The Excel templates are specific to each 

pollutant and type of emissions source and they can be downloaded from the ICR website 

(http://icr2010.rti.org, click on “Petroleum Refineries”). You must report the results of each test 

on the appropriately labeled worksheet corresponding to the specific tests requested at your 

emissions source. If you conducted testing at more than one source at your refinery using 

methods not currently supported by the ERT, you must make a copy of the worksheet and revise 

the unit ID in order to distinguish between each separate test. After completing the worksheet, 

you must also submit an electronic copy of the emission test report (PDF format preferred). 

If you have a CO Continuous Emissions Monitoring System (CEMS) that meets Performance 

Specification 4 (or other specified procedures) or a SO2 and/or NOX CEMS that meets 

Performance Specification 2 (or other specified procedures) installed on the exhaust of your 

emissions unit, and you used CEMS data to meet CO, SO2 and/or NOX test requirements as 

noted in the footnotes of specific tables, you must report daily averages from the last 30 days 

(including those days where manual testing was conducted) of CEMS data in a Microsoft® Excel 

CEMS Template. Similarly, if you have an H2S continuous monitoring system (CMS) that meets 

Performance Specification 7, and you used CMS data to meet the H2S testing requirements as 
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noted in the footnotes of specific tables, you must report daily averages from the last 30 days 

(including those days where manual testing was conducted) of CMS data in a Microsoft® Excel 

CMS Template. The Excel spreadsheet templates are specific to each pollutant and type of 

emissions source, and they can be downloaded from the ICR website (http://icr2010.rti.org, click 

on “Petroleum Refineries”). 

2.2 Required Fields for ERT Reporting 

The list of fields within the ERT with notes explaining whether or not the field is required or 

optional can be found on the ICR website (http://icr2010.rti.org, click on “Petroleum 

Refineries”). 

2.3 Calculating and Reporting Values Measured Below Detection Levels 

See Appendix A to this enclosure for guidance on calculating and reporting measurements less 

than detection levels for emissions data collection (ICR) programs. 

3.0 How to Submit Data 

As explained in the previous section, where applicable, you must report your data using the ERT. 

If the ERT does not support a particular pollutant or method, you must report your data using the 

data reporting spreadsheet we provide. When you are ready to submit your data to EPA, use one 

of three transmittal ways listed below. In order to avoid duplicate data and keep all data for a 

particular facility together, we request that you submit all of the data requested from your facility 

in the same way.* To submit your data: 

• Use the ICR website to upload your files. Detailed directions for uploading your files are 

provided on the ICR website (http://icr2010.rti.org, click on “Petroleum Refineries”). 

• E-mail an electronic copy of all requested files to refineryicr@epa.gov. 

• Mail a CD or DVD containing an electronic copy of all requested files to the EPA 

address shown in your Section 114 letter. If no electronic copy is available, mail a hard 

copy of all requested files to the EPA address shown in your Section 114 letter. 

*

 Please Note: If you are submitting Confidential Business Information (CBI), DO NOT use 

one of the methods listed above to submit your CBI. You must mail a separate CD, DVD, or 

hard copy package containing only the CBI portion of your data to the EPA address shown in 

your Section 114 letter. 
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4.0 Contact Information for Questions on Test Plan and Reporting 

For questions on how to report data using the ERT, contact: 

Ron Myers 

U.S. EPA 

(919) 541-5407 

myers.ron@epa.gov

 OR 

Barrett Parker 

U.S. EPA 

(919) 541-5635 

parker.barrett@epa.gov 

For questions on the test methods, including the use of alternative methods, contact: 

Peter Westlin 

U.S. EPA 

(919) 541-1058 

westlin.peter@epa.gov

 OR 

Robin Segall 

U.S. EPA 

(919) 541-0893 

segall.robin@epa.gov 

 OR 

Jason DeWees 

U.S. EPA 

(919) 541-9724 

dewees.jason@epa.gov 

For questions on the petroleum refinery test plan, including emissions sources selected for 

testing and reporting mechanisms other than the ERT, contact: 

Brenda Shine 

U.S. EPA 

(919) 541-3608 

shine.brenda@epa.gov 

For questions on uploading files to the HTTP site, please visit the ICR website 

(http://icr2010.rti.org, click on “Petroleum Refineries”) and use the toll free technical support 

hotline or technical support email address. 
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Appendix A 

Guidance For Calculating And Reporting Measurements Less Than 

In-Stack Method Detection Levels For Emissions Data 

Submitted in Response to Information Collection Request (ICR) Programs 

Identify the status of measured values relative to detection levels on the spreadsheet or in the 

ERT using the following descriptions: 

• BDL (below detection level) – all analytical values used to calculate and report an instack emissions value are less than the laboratory’s reported detection level(s); 

• DLL (detection level limited) – at least one but not all values used to calculate and report 

an in-stack emissions value are less than the laboratory’s reported detection level(s); or 

• ADL (above detection level) – all analytical values used to calculate and report an instack emissions value are greater than the laboratory’s reported detection level(s). 

For each reported emissions value, insert the appropriate flag (BDL, DLL, or ADL) in the Note 

line of the Microsoft® Excel emission test spreadsheet template or in the Comments line of the 

Electronic Reporting Tool (ERT). 

When reporting and calculating individual test run data: 

• For analytical data reported from the lab as “nondetect” or “below detection level”: 

− Include a brief description of the procedures used to determine the analytical 

detection and in-stack detection levels: 

o In the Note line of Excel emission test spreadsheet template; or 

o In the Comments line of Lab Data tab in the Run Data Details in the ERT. 

− Describe these procedures completely in a separate attachment including the 

measurements made, the standards used, and the statistical procedures applied. 

− Calculate in-stack emissions rate for any analytical measurement below detection 

level using the relevant detection level as the “reported” value. 

− Report the calculated emissions concentration or rate result: 

o As a bracketed “less than” detection level value (e.g., [<0.0105]) in the 

Excel emission test spreadsheet template and include the appropriate flag 

in the Note line; or 

o As a numerical value in the ERT with the appropriate general flag in the 

Flag column and as a bracketed “less than” detection level value (e.g., 

[<0.0105]) followed by a space and any specific flag identifier in the 

Comments column. The following specific flag identifiers are commonly 

used by laboratories: B, E, J, Int, R, DPE. 

− Report as numerical values (i.e., no brackets or < symbol) any analytical data 

measured above the detection level, including any data between the analytical 

detection level and a laboratory-specific reporting or quantification level (i.e., flag 

as ADL). 

− Apply these reporting and calculation procedures to measurements made with 

Method 23: 
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o Report data in the Excel emission test spreadsheet template for each of the 

D/F congeners measured with Method 23 below the detection level as 

[< detection level] 

o Do not report emissions as zero as described in the method 

• For pollutant measurements composed of multiple components or fractions (e.g., Hg and 

other metals sampling trains) when the result for the value for any component is 

measured below the analytical detection level; 

− Calculate in-stack emissions rate or concentrations as outlined above for each 

component or fraction; 

− Sum the measured and detection level values as outlined above using the in-stack 

emissions rate or concentrations for all of the components or fractions; and 

− Report the sum of all components or fractions: 

o As a bracketed “less than” detection level value (e.g., [<0.0105]) in the 

Excel emission test spreadsheet template and include the appropriate flag 

in the Note line; or 

o As a numerical value in the ERT with the appropriate flag in the 

Comments line. 

− Report also the individual component or fraction values for each run if the Excel 

emission test spreadsheet template or ERT format allows; if not (i.e., the format 

allows reporting only a single sum value): 

o For the Excel emission test spreadsheet template, next to the sum reported 

as above, report in the Notes line the appropriate flag along with the 

values for the measured or detection level value for each component or 

fraction as used in the calculations (e.g., 0.036, [<0.069], 1.239, [<0.945] 

for a four fraction sample) 

o For the ERT, next to the sum reported as above, report in the Flag column 

the appropriate general flag and in the Comments column the measured or 

detection level value for each component or fraction as used in the 

calculations followed by a space and any specific flag identifier provided 

by the laboratory (e.g., 0.036, [<0.069] J, 1.239, [<0.945] B for a four 

fraction sample). 

• For measurements conducted using instrumental test methods (e.g., Methods 3A, 6C, 7E, 

10, 25A) 

− Record gaseous concentration values as measured including negative values and 

flag as ADL; do not report as BDL 

− Calculate and report in-stack emissions rates using these measured values 

− Include relevant information relative to calibration gas values or other technical 

qualifiers for measured values in Comments line in the ERT

• When reporting and calculating average emissions rate or concentration for a test when 

some results are reported as BDL 

− Sum all of the test run values including those indicated as BDL or DLL as “real” 

values 

− Calculate the average emissions rate or concentration (e.g., divide the sum by 3 

for a three-run test) 
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− Report the average emissions rate or concentration average: 

o As a bracketed “less than” detection level value (e.g., [<20.06]) in the 

Excel emission test spreadsheet template and include the appropriate flag 

in the Note line 

o As a numerical value in the ERT and include the appropriate flag in the 

Comments line.