Method 3 8/3/2017

While we have taken steps to ensure the accuracy of this Internet version of the document, it is not the
official version. To see a complete version including any recent edits, visit:
https://www.ecfr.gov/cgi-bin/ECFR?page=browse and search under Title 40, Protection of
Environment.

METHOD 3 - GAS ANALYSIS FOR THE DETERMINATION OF DRY MOLECULAR

WEIGHT

Note: This method does not include all of the specifications (e.g., equipment and supplies) and
procedures (e.g., sampling) essential to its performance. Some material is incorporated by
reference from other methods in this part. Therefore, to obtain reliable results, persons using this
method should also have a thorough knowledge of Method 1.

1.0 Scope and Application

1.1 Analytes.

Analytes CAS No. Sensitivity

Oxygen (O2) 7782–44–7 2,000 ppmv.
Nitrogen (N2) 7727–37–9 N/A.
Carbon dioxide (CO2) 124–38–9 2,000 ppmv.
Carbon monoxide (CO) 630–08–0 N/A.

1.2 Applicability. This method is applicable for the determination of CO2 and O2 concentrations
and dry molecular weight of a sample from an effluent gas stream of a fossil-fuel combustion
process or other process.

1.3 Other methods, as well as modifications to the procedure described herein, are also
applicable for all of the above determinations. Examples of specific methods and modifications
include: (1) A multi-point grab sampling method using an Orsat analyzer to analyze the
individual grab sample obtained at each point; (2) a method for measuring either CO2 or O2 and
using stoichiometric calculations to determine dry molecular weight; and (3) assigning a value of
30.0 for dry molecular weight, in lieu of actual measurements, for processes burning natural gas,
coal, or oil. These methods and modifications may be used, but are subject to the approval of the
Administrator. The method may also be applicable to other processes where it has been
determined that compounds other than CO2, O2, carbon monoxide (CO), and nitrogen (N2) are
not present in concentrations sufficient to affect the results.

1.4 Data Quality Objectives. Adherence to the requirements of this method will enhance the
quality of the data obtained from air pollutant sampling methods.

2.0 Summary of Method

1
Method 3 8/3/2017

2.1 A gas sample is extracted from a stack by one of the following methods: (1) single-point,
grab sampling; (2) single-point, integrated sampling; or (3) multi-point, integrated sampling. The
gas sample is analyzed for percent CO2 and percent O2. For dry molecular weight determination,
either an Orsat or a Fyrite analyzer may be used for the analysis.

3.0 Definitions[Reserved]

4.0 Interferences

4.1 Several compounds can interfere, to varying degrees, with the results of Orsat or Fyrite
analyses. Compounds that interfere with CO2 concentration measurement include acid gases
(e.g., sulfur dioxide, hydrogen chloride); compounds that interfere with O2 concentration
measurement include unsaturated hydrocarbons (e.g., acetone, acetylene), nitrous oxide, and
ammonia. Ammonia reacts chemically with the O2 absorbing solution, and when present in the
effluent gas stream must be removed before analysis.

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials, operations, and equipment. This
test method may not address all of the safety problems associated with its use. It is the
responsibility of the user of this test method to establish appropriate safety and health practices
and determine the applicability of regulatory limitations prior to performing this test method.

5.2 Corrosive Reagents.

5.2.1 A typical Orsat analyzer requires four reagents: a gas-confining solution, CO2 absorbent,
O2 absorbent, and CO absorbent. These reagents may contain potassium hydroxide, sodium
hydroxide, cuprous chloride, cuprous sulfate, alkaline pyrogallic acid, and/or chromous chloride.
Follow manufacturer's operating instructions and observe all warning labels for reagent use.

5.2.2 A typical Fyrite analyzer contains zinc chloride, hydrochloric acid, and either potassium
hydroxide or chromous chloride. Follow manufacturer's operating instructions and observe all
warning labels for reagent use.

6.0 Equipment and Supplies

Note: As an alternative to the sampling apparatus and systems described herein, other sampling
systems (e.g., liquid displacement) may be used, provided such systems are capable of obtaining
a representative sample and maintaining a constant sampling rate, and are, otherwise, capable of
yielding acceptable results. Use of such systems is subject to the approval of the Administrator.

6.1 Grab Sampling (See Figure 3–1).

6.1.1 Probe. Stainless steel or borosilicate glass tubing equipped with an in-stack or out-of-stack
filter to remove particulate matter (a plug of glass wool is satisfactory for this purpose). Any
other materials, resistant to temperature at sampling conditions and inert to all components of the

2
Method 3 8/3/2017

gas stream, may be used for the probe. Examples of such materials may include aluminum,
copper, quartz glass, and Teflon.

6.1.2 Pump. A one-way squeeze bulb, or equivalent, to transport the gas sample to the analyzer.

6.2 Integrated Sampling (Figure 3–2).

6.2.1 Probe. Same as in Section 6.1.1.

6.2.2 Condenser. An air-cooled or water-cooled condenser, or other condenser no greater than

250 ml that will not remove O2, CO2, CO, and N2, to remove excess moisture which would
interfere with the operation of the pump and flowmeter.

6.2.3 Valve. A needle valve, to adjust sample gas flow rate.

6.2.4 Pump. A leak-free, diaphragm-type pump, or equivalent, to transport sample gas to the
flexible bag. Install a small surge tank between the pump and rate meter to eliminate the
pulsation effect of the diaphragm pump on the rate meter.

6.2.5 Rate Meter. A rotameter, or equivalent, capable of measuring flow rate to ±2 percent of the
selected flow rate. A flow rate range of 500 to 1000 ml/min is suggested.

6.2.6 Flexible Bag. Any leak-free plastic (e.g., Tedlar, Mylar, Teflon) or plastic-coated
aluminum (e.g., aluminized Mylar) bag, or equivalent, having a capacity consistent with the
selected flow rate and duration of the test run. A capacity in the range of 55 to 90 liters (1.9 to
3.2 ft3) is suggested. To leak-check the bag, connect it to a water manometer, and pressurize the
bag to 5 to 10 cm H2O (2 to 4 in. H2O). Allow to stand for 10 minutes. Any displacement in the
water manometer indicates a leak. An alternative leak-check method is to pressurize the bag to 5
to 10 cm (2 to 4 in.) H2O and allow to stand overnight. A deflated bag indicates a leak.

6.2.7 Pressure Gauge. A water-filled U-tube manometer, or equivalent, of about 30 cm (12 in.),
for the flexible bag leak-check.

6.2.8 Vacuum Gauge. A mercury manometer, or equivalent, of at least 760 mm (30 in.) Hg, for
the sampling train leak-check.

6.3 Analysis. An Orsat or Fyrite type combustion gas analyzer.

7.0 Reagents and Standards

7.1 Reagents. As specified by the Orsat or Fyrite-type combustion analyzer manufacturer.

7.2 Standards. Two standard gas mixtures, traceable to National Institute of Standards and
Technology (NIST) standards, to be used in auditing the accuracy of the analyzer and the
analyzer operator technique:

3
Method 3 8/3/2017

7.2.1. Gas cylinder containing 2 to 4 percent O2 and 14 to 18 percent CO2.

7.2.2. Gas cylinder containing 2 to 4 percent CO2 and about 15 percent O2.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Single Point, Grab Sampling Procedure.

8.1.1 The sampling point in the duct shall either be at the centroid of the cross section or at a
point no closer to the walls than 1.0 m (3.3 ft), unless otherwise specified by the Administrator.

8.1.2 Set up the equipment as shown in Figure 3–1, making sure all connections ahead of the
analyzer are tight. If an Orsat analyzer is used, it is recommended that the analyzer be leak-
checked by following the procedure in Section 11.5; however, the leak-check is optional.

8.1.3 Place the probe in the stack, with the tip of the probe positioned at the sampling point.
Purge the sampling line long enough to allow at least five exchanges. Draw a sample into the
analyzer, and immediately analyze it for percent CO2 and percent O2 according to Section 11.2.

8.2 Single-Point, Integrated Sampling Procedure.

8.2.1 The sampling point in the duct shall be located as specified in Section 8.1.1.

8.2.2 Leak-check (optional) the flexible bag as in Section 6.2.6. Set up the equipment as shown
in Figure 3–2. Just before sampling, leak-check (optional) the train by placing a vacuum gauge at
the condenser inlet, pulling a vacuum of at least 250 mm Hg (10 in. Hg), plugging the outlet at
the quick disconnect, and then turning off the pump. The vacuum should remain stable for at
least 0.5 minute. Evacuate the flexible bag. Connect the probe, and place it in the stack, with the
tip of the probe positioned at the sampling point. Purge the sampling line. Next, connect the bag,
and make sure that all connections are tight.

8.2.3 Sample Collection. Sample at a constant rate (±10 percent). The sampling run should be
simultaneous with, and for the same total length of time as, the pollutant emission rate
determination. Collection of at least 28 liters (1.0 ft3) of sample gas is recommended; however,
smaller volumes may be collected, if desired.

8.2.4 Obtain one integrated flue gas sample during each pollutant emission rate determination.
Within 8 hours after the sample is taken, analyze it for percent CO2 and percent O2 using either
an Orsat analyzer or a Fyrite type combustion gas analyzer according to Section 11.3.

Note: When using an Orsat analyzer, periodic Fyrite readings may be taken to verify/confirm the
results obtained from the Orsat.

8.3 Multi-Point, Integrated Sampling Procedure.

4
Method 3 8/3/2017

8.3.1 Unless otherwise specified in an applicable regulation, or by the Administrator, a

minimum of eight traverse points shall be used for circular stacks having diameters less than 0.61
m (24 in.), a minimum of nine shall be used for rectangular stacks having equivalent diameters
less than 0.61 m (24 in.), and a minimum of 12 traverse points shall be used for all other cases.
The traverse points shall be located according to Method 1.

8.3.2 Follow the procedures outlined in Sections 8.2.2 through 8.2.4, except for the following:
Traverse all sampling points, and sample at each point for an equal length of time. Record
sampling data as shown in Figure 3–3.

9.0 Quality Control

Section Quality control measure Effect

8.2 Use of Fyrite to confirm Ensures the accurate measurement of CO2 and O2.
Orsat results
10.1 Periodic audit of analyzer and Ensures that the analyzer is operating properly and that
operator technique the operator performs the sampling procedure correctly
and accurately.
11.3 Replicable analyses of Minimizes experimental error.
integrated samples

10.0 Calibration and Standardization

10.1 Analyzer. The analyzer and analyzer operator's technique should be audited periodically as
follows: take a sample from a manifold containing a known mixture of CO2 and O2, and analyze
according to the procedure in Section 11.3. Repeat this procedure until the measured
concentration of three consecutive samples agrees with the stated value ±0.5 percent. If
necessary, take corrective action, as specified in the analyzer users manual.

10.2 Rotameter. The rotameter need not be calibrated, but should be cleaned and maintained
according to the manufacturer's instruction.

11.0 Analytical Procedure

11.1 Maintenance. The Orsat or Fyrite-type analyzer should be maintained and operated
according to the manufacturers specifications.

11.2 Grab Sample Analysis. Use either an Orsat analyzer or a Fyrite-type combustion gas
analyzer to measure O2 and CO2 concentration for dry molecular weight determination, using
procedures as specified in the analyzer user's manual. If an Orsat analyzer is used, it is
recommended that the Orsat leak-check, described in Section 11.5, be performed before this
determination; however, the check is optional. Calculate the dry molecular weight as indicated in
Section 12.0. Repeat the sampling, analysis, and calculation procedures until the dry molecular
weights of any three grab samples differ from their mean by no more than 0.3 g/g-mole (0.3

5
Method 3 8/3/2017

lb/lb-mole). Average these three molecular weights, and report the results to the nearest 0.1 g/g-
mole (0.1 lb/lb-mole).

11.3 Integrated Sample Analysis. Use either an Orsat analyzer or a Fyrite-type combustion gas
analyzer to measure O2 and CO2 concentration for dry molecular weight determination, using
procedures as specified in the analyzer user's manual. If an Orsat analyzer is used, it is
recommended that the Orsat leak-check, described in Section 11.5, be performed before this
determination; however, the check is optional. Calculate the dry molecular weight as indicated in
Section 12.0. Repeat the analysis and calculation procedures until the individual dry molecular
weights for any three analyses differ from their mean by no more than 0.3 g/g-mole (0.3 lb/lb-
mole). Average these three molecular weights, and report the results to the nearest 0.1 g/g-mole
(0.1 lb/lb-mole).

11.4 Standardization. A periodic check of the reagents and of operator technique should be
conducted at least once every three series of test runs as outlined in Section 10.1.

11.5 Leak-Check Procedure for Orsat Analyzer. Moving an Orsat analyzer frequently causes it
to leak. Therefore, an Orsat analyzer should be thoroughly leak-checked on site before the flue
gas sample is introduced into it. The procedure for leak-checking an Orsat analyzer is as follows:

11.5.1 Bring the liquid level in each pipette up to the reference mark on the capillary tubing, and
then close the pipette stopcock.

11.5.2 Raise the leveling bulb sufficiently to bring the confining liquid meniscus onto the
graduated portion of the burette, and then close the manifold stopcock.

11.5.3 Record the meniscus position.

11.5.4 Observe the meniscus in the burette and the liquid level in the pipette for movement over
the next 4 minutes.

11.5.5 For the Orsat analyzer to pass the leak-check, two conditions must be met:

11.5.5.1 The liquid level in each pipette must not fall below the bottom of the capillary tubing
during this 4-minute interval.

11.5.5.2 The meniscus in the burette must not change by more than 0.2 ml during this 4-minute
interval.

11.5.6 If the analyzer fails the leak-check procedure, check all rubber connections and stopcocks
to determine whether they might be the cause of the leak. Disassemble, clean, and regrease any
leaking stopcocks. Replace leaking rubber connections. After the analyzer is reassembled, repeat
the leak-check procedure.

12.0 Calculations and Data Analysis

6
Method 3 8/3/2017

12.1 Nomenclature.

Md = Dry molecular weight, g/g-mole (lb/lb-mole).

%CO2 = Percent CO2 by volume, dry basis.

%O2 = Percent O2 by volume, dry basis.

%CO = Percent CO by volume, dry basis.

%N2 = Percent N2 by volume, dry basis.

0.280 = Molecular weight of N2 or CO, divided by 100.

0.320 = Molecular weight of O2 divided by 100.

0.440 = Molecular weight of CO2 divided by 100.

12.2 Nitrogen, Carbon Monoxide Concentration. Determine the percentage of the gas that is N2
and CO by subtracting the sum of the percent CO2 and percent O2 from 100 percent.

12.3 Dry Molecular Weight. Use Equation 3–1 to calculate the dry molecular weight of the stack
gas.

Note: The above Equation 3–1 does not consider the effect on calculated dry molecular weight of
argon in the effluent gas. The concentration of argon, with a molecular weight of 39.9, in
ambient air is about 0.9 percent. A negative error of approximately 0.4 percent is introduced. The
tester may choose to include argon in the analysis using procedures subject to approval of the
Administrator.

13.0 Method Performance[Reserved]

14.0 Pollution Prevention[Reserved]

15.0 Waste Management[Reserved]

16.0 References

1. Altshuller, A.P. Storage of Gases and Vapors in Plastic Bags. International Journal of Air and
Water Pollution. 6 :75–81. 1963.

2. Conner, William D. and J.S. Nader. Air Sampling with Plastic Bags. Journal of the American
Industrial Hygiene Association. 25 :291–297. 1964.
7
Method 3 8/3/2017

3. Burrell Manual for Gas Analysts, Seventh edition. Burrell Corporation, 2223 Fifth Avenue,
Pittsburgh, PA. 15219. 1951.

4. Mitchell, W.J. and M.R. Midgett. Field Reliability of the Orsat Analyzer. Journal of Air
Pollution Control Association. 26 :491–495. May 1976.

5. Shigehara, R.T., R.M. Neulicht, and W.S. Smith. Validating Orsat Analysis Data from Fossil
Fuel-Fired Units. Stack Sampling News. 4 (2):21–26. August 1976.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

8
Method 3 8/3/2017

Time Traverse point Q (liter/min) % Deviationa

Average

a
% Dev.=[(Q−Qavg)/Qavg]×100 (Must be ≤±10%)

Figure 3–3. Sampling Rate Data

9
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Observer/Report Review Checklists for Source Tests

The following checklists are to assist the on-site observer during a performance or compliance test. These checklists
were developed with the expectation that the observer has a general working knowledge of the applicable test
method(s). For each question on the checklists, the corresponding test method section citation is included to the left of
the question. Use of these checklists does not in and of itself create a regulatory requirement for each item in the
checklist. Rather, these checklists are intended to serve as an informative aid to the observer of source tests and to the
reviewer of source test reports.

The checklists contained in this package cover the following:

• Pre-Test Questionnaire;
• Methods 1-4;
• Method 5;
• Instrumental Methods 3A-O2/CO2, 6C-SO2, 7E-NOx, and 10-CO;
• Method 29; and
• Contents of a source test report.

Before observing the source test, the following activities should be considered:
• Review the Pre-Test Questionnaire;
• Review the applicable standards for the source (permit, NSPS, NESHAP, etc.);
• Read the approved test protocol;
• Review any previous test reports;
• Read the performance standard(s)/test method(s) listed in the test protocol;
• Review the checklists. If you have questions, refer to the citation to the left of the question or additional
information on the EMC website (https://www.epa.gov/emc); and
• Contact the site test coordinator to get a list of security and health and safety requirements necessary to get on
site.

Strongly encourage the testing company to completely fill out the Pre-Test Questionnaire. Using the information
provided on the Pre-Test Questionnaire, determine the traverse points, calculate nozzle size(s), and review the
calibration data. When on-site, check the information provided and compare traverse points and nozzle size
determinations with the tester. Check that the calibration records provided are for the equipment being used for the
source test. Inspect pitot tips for damage.

INTRO Page i
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

On the day of the test, be sure to have your ID and safety cards, appropriate and required personal protective
equipment (PPE), and checklists together before entering the facility. When arriving at the test site, let the lead for the
testing company/facility representative (test coordinator) know the information you will collecting, which should include
but not be limited to:
• Equipment calibration sheets;
• Daily calibration sheets;
• Certificate of Analysis of cylinder gases;
• Field data sheets;
• Recovery data sheets; and
• Chains of custody.

During your observation of the test, if you notice anything wrong or done well, let the source testing lead and facility
test coordinator know. If something is being or was performed incorrectly, it may be possible to correct the problem and
save the test run. If something was performed well, letting the test team know may ease tension and open up
communication. Either way, speak up.

INTRO Page ii
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Pre-Test Questionnaire
PLEASE COMPLETE AND SUBMIT THIS QUESTIONNAIRE 7 DAYS PRIOR TO THE TEST
Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :

Process Data / Production Rate :

Is there an approved test protocol? If yes, please submit it with this questionnaire. YES NO
Are there any anticipated or expected deviations or alternatives from the approved test methods? YES NO
If yes, note in the comments section below
Have you or your company tested this source before? YES NO
Are there any diagrams/schematics/pictures of testing location(s)? If yes, please submit it with this YES NO
questionnaire.
Are the testing location adequate to perform testing safely and accurately? YES NO
Do sampling location(s) meet the criteria of Method 1? If not, please provide testing approach in YES NO
comments below.
Are the planned total sampling times and volumes greater than or equal to the specified test YES NO
procedures?

Comments:

Pre-test Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Please provide a proposed schedule for testing in Table 1.

Please provide a schematic of the testing location(s) in Figures 1 & 2.

Please provide calibration records for all testing equipment to be used during this source test program. If the
most current calibration is not available for this submission, please provide the most recent calibration or
standard operating procedures (SOPs) for equipment calibrations and have the current calibration available on
the first day of testing.

Pre-test Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Table 1. Source Testing Daily Schedule

Test Total Daily

Date Activity
Day Hrs
AM
PM
AM
PM
AM
PM
AM
PM
AM
PM
AM
PM
AM
PM

Example of Source Testing Daily Schedule

Test Total Daily

Date Activity
Day Hrs
AM Safety training and set-up
1 10
PM RATA
AM Runs 1 & 2 (M5/26A and CEMS)
2 10
PM Run 3 (M5/26A and CEMS) and breakdown
AM
PM
AM
PM
AM
PM
AM
PM
AM
PM

Pre-test Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Schematic of Source(s)
Figure 1. Top View

Stack Diameter ____________

Port “A” Length ____________

Port “B” Length ____________

Figure 2. Side View

Pre-test Page 4
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
January 12, 2021

Date:_______________
Observer:_______________

Observer Checklist – Methods 1-4

Facility Name / Location :
Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :

Process Data / Production Rate :

If the answer is NO to any questions below, provide comments.

Method 1 – Sample and Velocity Traverses for Stationary Sources YES NO
§ 11.2 Were traverse points determined correctly? (see Figures PRELIM-1 and 2)
§ 11.4 Was a cyclonic flow check completed? (Avg of absolute value of all angles <20°)
§ 11.5 Alternative Measurement Site Selection (answer questions below only if needed)
Were a minimum of 40 traverse points (42 pts for rectangular ducts) used for gas flow
§ 11.5.2
angle determination?
§ 11.5.3.1 Did the pre-test leak check pass? (optional) Leak rate:
§ 11.5.3.2 Is the manometer leveled and zeroed?
§ 11.5.3.3 Were the yaw angles and pressure readings for pitch angle recorded?
§ 11.5.3.3 Was a back purge completed between traverse points?
§ 11.5.3.4 Did the post-test lek check pass? (mandatory) Leak rate:
Method 2 – Determination of Stack Gas Velocity and Volumetric Flow Rate YES NO
§ 8.1 Is the measurement system set up properly? (see Figure PRELIM-3)
§ 8.2 Is the manometer level and zeroed correctly?
§ 8.3 Are the velocity and stack temperature recorded at each sampling point?
§ 8.3 Are the pitot tube leak checks completed after each run?
§ 8.4 Was the static pressure measured during the test day?
§ 8.5 Is the barometric pressure recorded and adjusted for elevation (if needed)?
§ 10.1 Visual check of pitot tube heads – good condition?

M 1-4 Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:_______________
Observer:_______________

Observer Checklist – Methods 1-4 (continued)

Method 3 – Gas Analysis for O2, CO2, and Dry Molecular Weight YES NO
If Method 3A is being used to determine O2 and CO2 concentrations, skip this section.
§8.0 Single- or multi-point sampling used? Circle answer.
§8.0 Grab or integrated sampling used? Circle answer.
§8.0 Orsat or Fyrites being used? Circle answer.
§11.0 Is Orsat performed in triplicate? Is analysis consistent?
Method 4 – Determination of Moisture Content in Stack Gases YES NO
Method 5, 6A, 320, and using F-factors are acceptable alternatives to Method 4.
§8.1.1.2 Minimum sample volume of 0.60 scm (21 scf) at ≤ 0.021 m3/min (0.75cfm) achieved?
§8.1.2.1 Was the sampling train set up correctly? (see Figure PRELIM-4)
§8.1.3.1 Did the pre-test leak check pass? (optional) Leak rate:
§8.1.4.1 Temperature at the exit of impingers/condenser <68 °F?
8.1.4.2 Did the post-test leak check pass? (mandatory) Leak rate:
§12.1.6 From point to point, was the ΔVm >10% from the average sampling rate?
§12.1.7 For saturated or moisture-laden gas steam, was the lower Bws used?

Comments:

M 1-4 Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure PRELIM-1. Minimum Number of Traverse Point for Particulate Traverse

M 1-4 Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Figure PRELIM-2. Minimum Number of Traverse Point for Velocity (non-particulate) Traverse

M 1-4 Page 4
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure PRELIM-3. Pitot Tube and Manometer Assembly

M 1-4 Page 5
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure PRELIM-4. Method 4 Sampling Train Assembly

M 1-4 Page 6
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Reference Method 5 - Particulate Matter Emissions

Facility Name / Location :
Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :

Process Data / Production Rate :

Method 5 – Determination of Particulate Matter Emissions from Stationary Sources YES NO

If the answer is NO to any questions, provide comments below.
Is the planned total sampling time and volume greater than or equal to the specified test
§8.2.4
procedure?
Was the sampling train set up correctly? (see Figure M5-1)
§8.3
Nozzle Diameter:___________ Probe Length:____________
§8.3.2 Was the filter properly centered in the filter holder and free from tears?
§8.3.3 Glass or metal probe liner? Circle answer.
§8.4.2 Did the sampling train pre-test leak check pass? (optional) Leak rate:
§8.4.4 Did the sampling train post-test leak check pass? (mandatory) Leak rate:

M5 Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Reference Method 5 - Particulate Matter Emissions (continued)

If the answer is NO to any questions, provide comments below. YES NO

Was the temperature gas flow through the filter during the run at 120 ± 14 °C (248 ± 25
§8.5
°F)?
Is the data being recorded on a datasheet at least once at each sample point during each
§8.5.1
time increment?
§8.5.2 Were the portholes cleaned prior to the test run?
For stack with significant negative pressure, sampling pumps can be started prior to
§8.5.3
going into the stack.
§8.5.4 Is the port properly sealed around the sample probe?
§8.5.5 Is the sampling train being traversed per Method 1?
§8.5.6 Is the temperature of the gas exiting the sampling train <20 °C (68° F)?
§8.5.7 Was the test run completed without changing the filter?
§8.5.8 Was the test run completed without changing the sampling train?
§8.6 Was the sampling train operated isokinetically (100 ± 10%)?

Comments:

M5 Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Reference Method 5 - Particulate Matter Emissions (continued)

If the answer is NO to any questions, provide comments below. YES NO

After the probe has cooled and safe to handle, was any external PM wiped off the nozzle
§8.7.1
and then the nozzle capped to prevent losing or gaining PM?
§8.7.5 Was an acetone blank collected?
Any abnormal conditions noted during inspection of sample train prior to and during
§8.7.6
disassembly?
§8.7.6.1 Container 1. Was the filter carefully transferred into a petri dish?
Container 2. Was the front half of the sampling train (nozzle to front half of the filter
§8.7.6.2
holder) properly rinsed?
Container 3. Is the silica gel in good condition? Note the color of the silica gel to
§8.7.6.3
determine if it is spent.
§8.7.6.4 Was the moisture content for the test run determined using the impingers’ weight gain?
§10.1 Is the nozzle free of nicks, dents, or corrosion?
§10.2 Are the pitot tubes free of nicks, dents, or corrosion?

Comments:

M5 Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure M5-1. Particulate Sampling Train

M5 Page 4
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Methods 3A, 6C, 7E, or 10

Facility Name / Location :

Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :

Process Data / Production Rate :

Instrumental Methods: 3A-O2/CO2, 6C SO2, 7E-NOx, and 10-CO (circle method(s)) YES NO
Citations are for Method 7E
If the answer is NO to any questions, provide comment below and see Figure CEMS-2
§8.1 Were the sample point(s) determined correctly?
§8.2.1 Are the calibration gas certificates current?
§8.2.1 Are the calibration gases within acceptable ranges?
§8.2.2 Is the sampling system properly configured? (See CEMS-1)
Is the 3-pt direct calibration error (CE) (or 3-pt system CE for dilution systems) within
§8.2.3
±2.0% of the calibration span or ≤0.5 ppmv absolute difference?
§8.2.4 Method 7E only. Was the NO2 to NO conversion efficiency test preformed? Was it >90%?
Is the initial system bias check (or pre and post 2-pt CE for dilution systems) within ±5.0%
§8.2.5
of calibration span or ≤0.5 ppmv absolute difference?
§8.2.6 What is the system response time? Response time:
§8.2.7 Was interference test paperwork available and representative?

CEMS Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Methods 3A, 6C, 7E, or 10 (continued)

If the answer is NO to any questions, provide comment below and see Figure Instrumental YES NO
Methods-2
Dilution system only. Is the diluted sample dew point below the sample line and
§8.3
analyzer temperatures?
§8.3 Dilution system only. Is the dilution ratio consistent through the test runs?
Dilution system only. Are the molecular weights (MW) of the calibration and stack gases
§8.3
addressed in dilution ratio and measurement calculations?
Was the post-run system bias check (or 2-pt system CE for dilution systems) within ±5.0%
§8.5
of calibration span or ≤0.5 ppmv absolute difference?
Was the post-run system drift check within ±3.0% of calibration span or ≤0.5 ppmv
§8.5
absolute difference?
§8.6 Was dynamic spiking procedure used?

Comments:

CEMS Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure CEMS-1. Example of equipment configuration.

Figure CEMS-2. Test Run Calibration Flow Chart

CEMS Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Method 29 – Metals Emissions

Facility Name / Location :
Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :
Process Data / Production Rate :

Method 29 – Metal Emissions from Stationary Sources YES NO

If the answer is NO to any questions, provide comment below.
§8.1.3 Was the sampling train set up correctly? (see Figure M29-1)
§8.1.4 Did the sampling train pre-test leak check pass? (optional) Leak rate:
§8.1.4 Did the sampling train post-test leak check pass? (mandatory) Leak rate:
Was the temperature of the gas flow through the filter during the run at 120 ± 14 °C
§8.1.5
(248 ± 25 °F)?
For a stack with significant negative pressure, sampling pumps can be started prior to
§8.1.5
going into the stack.
§8.1.5 Is the port properly sealed around the sample probe?
§8.1.5 Is the sampling train being traversed per Method 1?
§8.1.5 Is the temperature of the gas exiting the sampling train <20 °C (68° F)?
§8.1.5 Was the test run completed without changing out the filter?
§8.1.5 Was the test run completed without changing out the sampling train?
§8.1.6 Was the sampling train operated isokinetically (100 ± 10%)?

M29 Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Method 29 – Metals Emissions (continued)

If the answer is NO to any questions, provide comment below. YES NO
§8.2.5 Container 1. Was the filter carefully transferred into a petri dish?
Container 2. If PM is being measured, was the front half of the sampling train (nozzle to
§8.2.6
front half of the filter holder) properly rinsed with 100mls of acetone?
Container 3. Was the front half of the sampling train (nozzle to front half of the filter
§8.2.7
holder) properly rinsed with 100mls 0.1N HNO3?
§8.2.8 Container 4. Were impingers 1 through 3 weighed and then emptied into container 4?
§8.2.8 Was the moisture content for the test run determined using the impingers’ weight gain?
Container 4. Was the back half of the filter holder and all glassware through impinger 3
§8.2.8
rinsed with 100mls 0.1N HNO3?
Container 5A. If mercury (Hg) is being measured, was impinger 4 weighed and emptied
§8.2.9.1
into container 5A?
§8.2.9.1 Container 5A. If Hg is being measured, was impinger 4 rinsed with 100mls of 0.1N HNO3?
Container 5B. If Hg is being measured, were impingers 5 and 6 weighed and emptied
§8.2.9.2
into container 5B?
Container 5B. If Hg is being measured, were impingers 5 and 6, and the connecting
§8.2.9.2 glassware triple rinsed with 100mls of fresh acidified KMnO4 solution followed with
100mls of reagent grade H2O?
§8.2.9.3 Container 5C. If Hg is being measured, were impingers 5 and 6 rinsed the 8N HCl?
§8.2.10 Container 6. Was the silica gel impinger weighed and in good condition?
§8.2.11 Container 7. If PM is being measured, was a 100ml acetone blank taken?
§8.2.12 Container 8A. Was a 300ml 0.1N HNO3 blank taken?
§8.2.13 Container 8B. Was a 100ml reagent water blank taken?
§8.2.14 Container 9. Was a 200ml 5% HNO3/10% H2O2 blank taken?
Container 10. If Hg is being measured, was a 100ml acidified KMnO4 solution blank
§8.2.15
taken?
Container 11. If Hg is being measured, was a 25ml 8N HCl blank in 200ml of reagent H2O
§8.2.16
taken?
§8.2.17 Container 12. Was a filter blank taken?
§10.1 Is the nozzle free of nicks, dents, or corrosion?
§10.1 Are the pitot tubes free of nicks, dents, or corrosion?

M29 Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Date:________________
Observer:________________

Observer Checklist – Method 29 – Metals Emissions (continued)

Comments:

M29 Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021
Figure M29-1. Metals Sampling Train.

M29 Page 4
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Observer Checklist – Emission Test Report Checklist

Facility Name / Location :

Facility Contact / Phone :
Testing Firm / Contact :
Permit #:
Source Tested:
Applicable Regulation(s) / Pollutant(s) :

Emissions Test Report Checklist YES NO

If the answer is NO to any questions below, provide comment below.
Responsible groups (participating organizations)
Overall purpose of the emission test
Applicable regulations
Industry
Name of facility
1.0 Introduction

Facility location
1.1 Summary of Test Program
Processes of interest
Air pollution control equipment, if applicable
Emission points and sampling locations
Pollutants to be measured and testing methods
used
Dates of emission testing
Names, affiliations, and telephone numbers of
1.2 Key Personnel
key personnel

REPORT Page 1
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Observer Checklist – Emission Test Report Checklist (continued)

If the answer is NO to any questions below, provide comment below. YES NO
General description of the basic process
Flow diagram (indicate emission and process
2.0 Plant and Sampling Location Description

test points)
Discussion of typical process operations, such as:
• Production rates;
2.1 Process Description and
• Feed material and feed rates or batch
Operation
size;
• Equipment sizes and capacities (rates);
and
• Production schedules (hours/day,
days/week, peak periods).
Description of all air pollution control systems, if
applicable
Discussion of typical control equipment
operation and, if necessary, a schematic.
2.2 Control Equipment Description
Discussion on parameter(s) monitored and
monitoring results for parameters for which
operating limits will be set

REPORT Page 2
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Observer Checklist – Emission Test Report Checklist (continued)

If the answer is NO to any questions below, provide comment below. YES NO
Provide a schematic of each location. Include:
• Duct diameter;
• Direction of flow;
• Dimension (include number of duct
diameters);
• Location and configuration of
sampling ports
2.0 Plant and Sampling Location Description

• Nipple length and port

2.3 Flue Gas Sampling Location diameters
• Number and configuration of
traverse points
• Confirm that the sampling location met
the EPA Method 1 criteria – If not, give
reasons and discuss effect on results;
and
• Discuss any special traversing or
measurement schemes.
If process stream samples were taken, include
the following:
• Schematic of location, if helpful;
• Description of each sampling or
measurement location;
• Description of procedure used
2.4 Process Sampling Location
to obtain samples or
measurements
• Discussion on the
representativeness of each of
the process stream sampling
locations and samples.

REPORT Page 3
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Observer Checklist – Emission Test Report Checklist (continued)

If the answer is NO to any questions below, provide comment below. YES NO
Restate the overall purpose of the test program.
List the specific objectives.
Include a test matrix table showing the following
3.0 Summary and Discussion of Test Results

(including schematics, if helpful):

• Run number and date;
3.1 Objectives and Test Matrix
• Sample type/pollutant;
• Test method;
• Sampling locations;
• Clock time; and
• Sampling time.
List and discussion of any changes in sampling
3.2 Field Test Changes and
and analytical methods for emissions or process
Problems
information.
Address each of the specific objectives and
present a summary of the results in tabular
form.
• Compare field data sheets with report
3.3 Presentation of Results
tables,
• Compare lab data with report tables,
• Check report calculations
Discuss data.
Schematic of each sampling train
4.0 Sampling and Analytical

Flow diagram of the sample recovery

Flow diagram of the sample analysis
4.1 Test Methods
Description of any modifications
Procedures

Discussion of any problematic sampling or

analytical conditions
Description of procedures used to obtain
process stream samples, process data, and
4.2 Process Test Methods control equipment data
Calibration procedures for any test equipment, if
appropriate.

REPORT Page 4
 GD-54
Methods 1-5, 6C, 7E, 10, and 29
Revision 1
February 1, 2021

Observer Checklist – Emission Test Report Checklist (continued)

If the answer is NO to any questions below, provide comment below. YES NO

QA/QC problems that occurred during the test.
5.1 QA/QC Problems
5.0 Internal QA/QC Activities

Sample identification and custody problems

For each of the test methods for which an audit
was conducted, list (if applicable) the following:
• Type of audit;
• Limits of acceptability;
• Supplier of audit material;
5.2 QA Audits
• Audit procedure; and
• Summary of results
o Calibrations
o Analytical QC
o Sampling QC
Required information from the General
Provision, §60.8(f)(2)(v) but not limited to:
• Test run raw data sheets;
• Instrumental method data;
o Instrument calibration(s)
Appendices

o QC checks
o Certificate of analysis
• Equipment calibration
• Sample calculations;
• Process data; and
• Analytical data
o Record of standard preparation
o Raw data sheets
o Chain-of-custody documentation

Comments:

REPORT Page 5