CLEAN AIR ACT (CAA) SECTION 114 EMISSIONS DATA 

COLLECTION REQUEST FOR THE PRIMARY ALUMINUM 

REDUCTION PLANT SOURCE CATEGORY

TEST REPORT

POTLINE 3 163S A-398 SCRUBBER AND POTLINE 3, ROOM 6 ROOF MONITOR 

SAMPLING MANIFOLD (AKA DOWNCOMER)

Polycyclic Organic Matter (POM), Metallic Hazardous Air Pollutants (Metallic HAPS)

and Total Filterable Particulate Matter (PM)

A-446 ANODE BAKE FURNACE SCRUBBER AND

ANODE PASTE PLANT DRY COKE SCRUBBER (AKA PROCEDAIR)

Metallic HAPS and PM

Performed for:

RIO TINTO ALCAN

SEBREE WORKS

9404 State Route 2096

Robards, KY 42452

April 15 – 19, 2013

April 24, 2013

Submitted by:

Air Quality Services, LLC

425 Main Street

Evansville, Indiana 47708

Phone: (812) 452-4785

Fax: (812) 452-4786

AQS Project #’s 13661-21-001 & 13661-21-002
ii

SOURCE TESTING REPORT CERTIFICATION

Air Quality Services, LLC

425 Main Street

Evansville, Indiana 47708

Phone: (812) 452-4785

Fax: (812) 452-4786

Reproducing portions of this test report may omit critical substantiating documentation or 

be taken out of context and due care should be exercised in this regard.

I have prepared and reviewed this report and found the information accurate and complete

to the best of my ability. 

Report Writer

_________________________________ Date____________________

Stephen R. Endress

Air Quality Services, LLC

I have reviewed this report and found the information accurate and complete to the best of 

my ability.

Reviewer

_________________________________ Date____________________

Daniel L. Todd, QEP, CHMM

Air Quality Services, LLC

May 24, 2013

May 29, 2013
iii

TABLE OF CONTENTS

Page

SECTION 1 EXECUTIVE SUMMARY..............................................................1

SECTION 2 INTRODUCTION............................................................................3

SECTION 3 SUMMARY OF TEST RESULTS..................................................4

SECTION 4 PROCESS DESCRIPTIONS ...........................................................7

SECTION 5 SAMPLING AND ANALYTICAL PROCEDURES ....................13

 Location of Measurement Sites....................................................13

 Stack Gas Volumetric Flow Rate.................................................13

 Stack Gas Dry Molecular Weight ................................................14

 Stack Gas Moisture Content ........................................................14

 Filterable Particulate Matter.........................................................14

 Metallic HAPS.............................................................................16

 Methylene Chloride Extractable Matter.......................................17

 Performance Audits .....................................................................18

SECTION 6 QUALITY ASSURANCE / QUALITY CONTROL ....................19

APPENDIX A - EXAMPLE CALCULATIONS

APPENDIX B - DATA SUMMARIES

APPENDIX C - FIELD DATA 

APPENDIX D - POTROOM FLOW CALCULATIONS AND DATA

APPENDIX E - PRODUCTION DATA

APPENDIX F - LABORATORY DATA

APPENDIX G - QUALITY ASSURANCE / QUALITY CONTROL

APPENDIX H - ICR TABLE RESPONSES
iv

LIST OF TABLES

Table Page

 1.1 Average Non-metallic Emissions Test Results............................................1

 1.2 Metallic HAPS Emissions Test Results.......................................................2

 2.1 Test Program Contacts.................................................................................3

 5.1 Sampling Times.........................................................................................13

 5.2 Sample Volumes........................................................................................14

 6.1 Field Equipment Calibration Summary .....................................................19

LIST OF FIGURES

Figure Page

 4.1 Potline Operations Process Flow Diagram ..................................................8

 4.2 Combination Dry Alumina Scrubber/Baghouse ..........................................9

 4.3 A-398 Fume Control System .......................................................................9

 4.4 Anode Production Process Flow Diagram.................................................10

 4.5 A-446 Anode Bake Furnace Control Device .............................................11

 4.6 Procedair Anode Paste Plant Control Device ............................................12

 5.1 Method 5 Stack Sampling Train Diagram .................................................16

 5.2 Method 29 Stack Sampling Train Diagram ...............................................17

LIST OF ABBREVIATIONS

ascfm actual standard cubic feet per minute

dscfm dry standard cubic feet per minute

gr/dscf grains per dry standard cubic foot

lb/dscf pound(s) per dry standard cubic foot

lb/hr pound(s) per hour

fps feet per second

RX scrubber reactor
Page 1 of 19

AQS Project# 13661-21-001

SECTION 1

EXECUTIVE SUMMARY

Various stack tests were conducted to comply with the Clean Air Act (CAA) Section 114 

Emissions Data Collection Request for the Primary Aluminum Reduction Plant Source Category 

(hereafter referred to as the PMACT ICR) at Rio Tinto Alcan’s (Alcan) Sebree Worksfacility in 

Robards, Kentucky (Source ID # 21-101-00029). The testing program addressed the following 

pollutants and sampling locations:

 Polycyclic organic matter (POM), metallic hazardous air pollutants (metallic HAPS), and 

total filterable particulate matter (PM) at the following two locations associated with 

Potline 3: (1) the 163S A-398 Scrubber and (2) the Potline 3, Room 6 Roof Monitor 

Sampling Manifold (aka Downcomer)

 Metallic HAPS and PM from the A-446 Anode Bake Furnace Scrubber

 Metallic HAPS and PM from the Anode Paste Plant Dry Coke Scrubber (aka Procedair)

During the test program, Potline #3, the A-446 Anode Bake Furnace, and the Anode Paste Plant

were operated under normal conditions. 

These tests followed the procedures for EPA Methods 1, 2, 3, 4, 5, 29, and 315 as specified in 40 

CFR 60, Appendix A.

The test program was conducted from April 15 – 19 and April 24, 2013. The results of the 

emissions tests are summarized below:

TABLE 1.1

AVERAGE NON-METALLIC EMISSIONS TEST RESULTS

Volumetric 

Flow Rate

dscfm lb/hr lbs/ton 

Aluminum

lbs/ton 

green 

anode

lb/hr lbs/ton 

Aluminum

lbs/ton 

green 

anode

163S A-398 

Scrubber 36,526 0.434 0.097 - - - 0.149 0.033 - - -

Potline 3 Roof 

Monitors 1,043,761 9.77 4.26 - - - 1.190 0.519 - - -

A-446 Anode Bake 

Furnace Scrubber 19,263 0.592 N/A 0.0375 - - - - - - - - -

Anode Paste Plant 

Dry Coke Scrubber 42,302 0.841 N/A 0.0362 - - - - - - - - -

Location

Particulate Matter (PM) Polycyclic Organic 

Matter (POM)
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AQS Project# 13661-21-001

TABLE 1.2

METALLIC HAPS EMISSIONS TEST RESULTS

lb/hr lb/ton 

aluminum Flag lb/hr lb/ton aluminum Flag lb/hr lb/ton green anode Flag lb/hr lb/ton green anode Flag

Antimony (Sb) 7.23E-05 1.61E-05 ADL 9.04E-04 3.95E-04 ADL 4.26E-05 2.64E-06 ADL 4.88E-05 2.12E-06 ADL

Arsenic (As) 1.49E-04 3.32E-05 DLL 2.73E-03 1.19E-03 DLL 6.05E-05 3.64E-06 DLL 9.06E-05 3.93E-06 DLL

Beryllium (Be) 4.61E-06 1.03E-06 DLL 7.12E-04 3.11E-04 DLL 2.08E-06 1.31E-07 DLL 1.34E-06 5.83E-08 DLL

Cadmium (Cd) 6.92E-06 1.54E-06 DLL 3.89E-04 1.70E-04 ADL 1.82E-05 1.07E-06 ADL 1.41E-06 6.13E-08 DLL

Chromium (Cr) 5.57E-04 1.24E-04 ADL 2.58E-03 1.13E-03 ADL 1.56E-04 1.00E-05 ADL 4.17E-04 1.81E-05 ADL

Cobalt (Co) 8.71E-06 1.94E-06 DLL 9.09E-05 3.96E-05 DLL 7.93E-06 4.76E-07 DLL 7.98E-06 3.48E-07 DLL

Lead (Pb) 3.42E-05 7.63E-06 DLL 8.23E-04 3.61E-04 DLL 1.03E-04 6.19E-06 ADL 2.10E-05 9.10E-07 DLL

Manganese (Mn) 2.13E-04 4.75E-05 ADL 8.86E-04 3.86E-04 ADL 1.08E-03 7.09E-05 CNT 1.63E-02 7.13E-04 CNT

Nickel (Ni) 4.40E-04 9.81E-05 ADL 2.35E-02 1.03E-02 DLL 5.82E-05 3.65E-06 ADL 8.97E-05 3.89E-06 ADL

Selenium (Se) 7.07E-05 1.58E-05 ADL 3.87E-04 4.22E-06 DLL 6.92E-05 2.25E-08 DLL 4.92E-05 2.14E-06 ADL

Mercury (Hg) [<1.64E-08] [<3.65E-09] BDL [<3.05E-05] [<1.33E-05] BDL [<4.18E-06] [<2.58E-07] BDL [<4.92E-06] [<2.14E-07] BDL

Production

Pollutant

A-446 Anode Bake Furnace 

Scrubber

Anode Paste Plant Dry Coke 

Scrubber

4.483 Tons of Aluminum per 

Hour

2.283 Tons of Aluminum per 

Hour

16.40 Tons of Green Anode 

per Hour

23.03 Tons of Green Anode 

per Hour

163S A-398 Scrubber Potline 3 Downcomer

Flag Legend*

BDL Below Detection Level

DLL Detection Level Limited

ADL Above Detection Level

CTN Contaminated

* as defined in EPA’s Electronic Reporting Tool (ERT)

User’s Guide, Version 4, September 2012
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AQS Project# 13661-21-001

SECTION 2

INTRODUCTION

Alcan retained Air Quality Services, LLC (AQS) to plan and conduct a testing program to 

determine POM, metallic HAPS, and filterable PM at the Potline 3 163S A-398 Scrubber and the 

Potline 3, Room 6 Roof Monitor Sampling Manifold (aka Downcomer); along with metallic 

HAPS and filterable PM from the three-section A-446 Anode Bake Furnace Scrubber and the 

Anode Paste Plant Dry Coke Scrubber (aka Procedair). The testing was conducted over two

separate mobilizations: April 15 – 19 and April 24, 2013.

The sampling was conducted using EPA Methods 2, 3, 4, 5, 29, and 315 to determine velocity 

and volumetric flow rates, molecular weight, moisture content, selected metallic HAPs, and 

POM (as methylene chloride extractable material) concentrations, respectively. Jeff Wollrab

(Project Manager), Marshall Peters, Jacob Luker, Ryan Neumann, and Austin Moore, of AQS,

performed the sampling procedures. No regulatory observers were present during this testing.

The contacts for this test program were as follows:

TABLE 2.1

TEST PROGRAM CONTACTS

Rio Tinto Alcan – Sebree Works:

Mr. Brandon Coomes

9404 State Route 2096

Robards, KY 42452

Phone: (270) 521-7454

Fax: (270) 521-7455

E-mail: brandon.coomes@riotinto.com

Air Quality Services, LLC:

Mr. Dan Todd / Jeff Wollrab

425 Main Street

Evansville, IN 47708

Phone: (812) 452-4785

Fax: (812) 452-4786

E-mail: dtodd@aqsllc.net

 jwollrab@aqsllc.net
Page 4 of 19

AQS Project# 13661-21-001

SECTION 3

SUMMARY OF TEST RESULTS

Potline 3 163S A-398 Scrubber

The production rate of the process vented through this scrubber during this testing program was 

4.48 tons of aluminum produced per hour. Complete tabulations of measured parameters and 

calculated results are included in Appendix B.

Using the procedures described in EPA Methods 5, 29, and 315, total filterable PM, metallic 

HAPS, and POM (as methylene extractable material) were measured at the Potline 3 163S A-398 

Scrubber exhaust. GPS coordinates for this sampling location are latitude 37.657951 and 

longitude 87.502835. Three (3) four-hour test runs were conducted at the A-398 Scrubber on 

April 17 and 18, 2013. Gas characteristics were determined by the use of EPA Method 2 

(velocity and flow rate), Method 3 (carbon dioxide and oxygen content), and Method 4 

(moisture). 

In order to perform these tests, there were two sample trains operated concurrently. Based upon 

the data recorded during the testing (average of the two trains), the exhaust gas composition at 

the A-398 Scrubber averaged approximately 0.5% carbon dioxide (CO2), 19.5% oxygen (O2), and 

80.0% nitrogen (N2); the gas temperature averaged 215.9oF; the moisture content averaged 1.9%; 

and the velocity averaged 39.9 feet per second (fps). The measured volumetric flow rate 

averaged 47,931 actual cubic feet per minute (acfm). Converting the measured volumetric flow 

rate to standard conditions, the exhaust averaged 36,526 dry standard cubic feet per minute 

(dscfm). 

The average six-run test results for the PM (three runs Method 315 plus three runs Method 5/29) 

and the three-run test results for the POM and the metallic HAPS are presented in Tables 1.1 and 

1.2 of this report. Individual test run stack gas parameter measurements and test results are 

presented in Appendix B.1.

Potline 3, Room 6 Roof Monitor Sampling Manifold (aka Downcomer)

Using the procedures described in EPA Methods 5, 29, and 315, total filterable PM, metallic 

HAPS, and POM (as methylene extractable material) were measured at the Potline 3, Room 6 

Roof Monitor Sampling Manifold (aka Downcomer) exhausts. GPS coordinates for this 

sampling location are latitude 37.658877 and longitude 87.499145. Three (3) 24-hour test runs 

were conducted at the downcomer from April 16 – 19, 2013. Gas characteristics were 

determined by the use of Method 3 (carbon dioxide and oxygen content) and Method 4 

(moisture). 

In order to perform these tests, there were two sample trains operated concurrently. Based upon 

the data recorded during the testing (average of the two trains), the exhaust gas composition at 

the Downcomer averaged approximately 0.3% CO2, 20.0% O2, and 79.7% N2; the gas 
Page 5 of 19

AQS Project# 13661-21-001

temperature averaged 99.4oF; the moisture content averaged 1.4%; and the velocity averaged 

49.2 fps. The measured volumetric flow rate averaged 3,160 acfm. Converting the measured 

volumetric flow rate to standard conditions, the exhaust averaged 2,910 dscfm. In order to 

extrapolate the Downcomer test results to reflect Potroom 6 South, the flow measurements from 

the roof-mounted anemometers were used. Based upon the anemometer data, the roof monitor 

exhaust averaged 1,137,777 acfm. Converting the measured volumetric flow rate to standard 

conditions, the exhaust averaged 1,043,761 dscfm.

The average six-run test results for the PM (three runs Method 315 plus three runs Method 5/29) 

and the three-run test results for the POM and the metallic HAPS are presented in Tables 1.1 and 

1.2 of this report. Individual test run stack gas parameter measurements and test results are 

presented in Appendix B.2.

A-446 Anode Bake Furnace Scrubber

The production rate of the process vented through this scrubber during this testing program was 

16.4 tons of green anodes per hour. Complete tabulations of measured parameters and calculated 

results are included in Appendix B.

Using the procedures described in EPA Methods 5 and 29, total filterable PM and metallic HAPS 

were measured at the A-446 Anode Bake Furnace Scrubber exhaust. GPS coordinates for this 

sampling location are latitude 37.658648 and longitude 87.497999. Three (3) four-hour test runs 

were conducted from representative reactor sections of the A-446 Anode Bake Furnace Scrubber 

on April 15 and 23, 2013. Gas characteristics were determined by the use of EPA Method 2 

(velocity and flow rate), Method 3 (carbon dioxide and oxygen content), and Method 4 

(moisture). 

Based upon the data recorded during the testing, the exhaust gas composition at the A-446 

Anode Bake Furnace Scrubber averaged approximately 0.3% CO2, 19.5% O2, and 80.2% N2; the 

gas temperature averaged 177.9oF; the moisture content averaged 9.4%; and the velocity 

averaged 46.8 fps. The measured volumetric flow rate averaged 29,965 acfm. Converting the 

measured volumetric flow rate to standard conditions, the exhaust averaged 19,263 dscfm. 

The average three-run test results of the PM and the metallic HAPS are presented in Tables 1.1 

and 1.2 of this report. Individual test run stack gas parameter measurements and test results are 

presented in Appendix B.3.

Anode Paste Plant Dry Coke Scrubber (aka Procedair)

The production rate of the process vented through this scrubber during this testing program was 

23.0 tons of green anodes per hour. Complete tabulations of measured parameters and calculated 

results are included in Appendix B.

Using the procedures described in EPA Methods 5 and 29, total filterable PM and metallic HAPS

were measured at the Procedair exhaust. GPS coordinates for this sampling location are latitude 
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AQS Project# 13661-21-001

37.658877 and longitude 87.499145. Three (3) four-hour test runs were conducted at the exhaust 

of the Procedair control device on April 19 and 22, 2013. Gas characteristics were determined 

by the use of EPA Method 2 (velocity and flow rate), Method 3 (carbon dioxide and oxygen 

content), and Method 4 (moisture). 

Based upon the data recorded during the testing, the exhaust gas composition at the Procedair

averaged approximately 0.5% CO2, 19.5% O2, and 80.0% N2; the gas temperature averaged 

98.3oF; the moisture content averaged 1.0%; and the velocity averaged 47.9 fps. The measured 

volumetric flow rate averaged 45,697 acfm. Converting the measured volumetric flow rate to 

standard conditions, the exhaust averaged 42,302 dscfm. 

The average three-run test results of the PM and the metallic HAPS are presented in Tables 1.1 

and 1.2 of this report. Individual test run stack gas parameter measurements and test results are 

presented in Appendix B.4.

Example calculations, the formulae used in the AQS spreadsheets, are included as Appendix A. 

The field data sheets are included as Appendix C, potroom flow calculations are included as

Appendix D, laboratory data are contained in Appendix F and ICR Table Responses are included 

as Appendix H.
Page 7 of 19

AQS Project# 13661-21-001

SECTION 4

PROCESS DESCRIPTIONS

Rio Tinto Alcan owns and operates a primary aluminum production facility near Robards, 

Kentucky (Sebree Works). The facility is a major source under the Title V and Prevention of 

Significant Deterioration (PSD) permit programs due to its source-wide emissions. All processes 

were operating under normal conditions during the test program. 

Potlines

At Sebree Works, Alcan produces primary aluminum from raw alumina (Al2O3) by applying 

electric current to the alumina in vessels termed reduction cells or pots. Alcan operates three 

nearly identical potlines. Each potline is composed of two potrooms that each contains 64 

reduction cells for a total of 128 cells per potline. The pots are constructed to form an 

electrolytic cell with an anode, cathode, and electrolyte. As the electric current is applied, an 

electrolytic reaction occurs reducing the alumina into its constituent species aluminum (Al) and 

O2. The emission from the reduction cells in each potline are captured through hooding systems 

and are sent to two Alcoa A-398 alumina fluidized bed dry scrubbers, each of which has five 

reactors. Any fugitive emissions not caught by the hooding system are vented through the roof of

each potline. 

The exterior of the pots consists of rectangular steel lined with refractory thermal insulation. 

Within the pot is an inner lining of carbon (the cathode). Carbon anode blocks are placed just 

below the surface of a fluoride electrolyte (cryolite) to complete the reaction circuit. A current is 

applied to metal rods attached to the anode blocks, which passes through the molten bath (molten 

aluminum, cryolite, and alumina) and the carbon cathode lining and then to current collector 

bars. The molten aluminum formed in the reduction cells (as it is liberated from alumina with 

oxygen) settles between the anode and cathode where it accumulates. The oxygen liberated 

reacts with the carbon anode blocks forming carbon dioxide. The accumulated molten metal is 

siphoned from the pots into crucibles each day. The anode blocks, which are gradually 

consumed by the reaction in the pots, last a few weeks before they must be replaced with new 

anodes. Figure 4.1 presents a process flow diagram of the potline operations.
Page 8 of 19

AQS Project# 13661-21-001

FIGURE 4.1

POTLINE OPERATIONS PROCESS FLOW DIAGRAM
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AQS Project# 13661-21-001

FIGURE 4.2

COMBINATION DRY ALUMINA SCRUBBER/BAGHOUSE

FIGURE 4.3

A-398 FUME CONTROL SYSTEM

Anode Production

To provide baked carbon anodes to the reduction cells, Alcan operates an anode paste mixing 

and forming operation and an anode bake furnace, in which the “green anodes” are baked. The 

green anodes are formed from petroleum coke, recycled spent anode material, and coal tar pitch, 

which serves as a binder. The emissions from the paste mixing and anode forming units are 

vented to a common control device, a Procedair dry coke scrubber.

Duct work Cells – 64 on each side:

One Bank vents 128 cells One Bank (group of 5 Reactors)
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AQS Project# 13661-21-001

The formed anodes are compressed and placed within the bake furnace, where they are baked to 

remove volatiles, leaving a solid carbon block. The emissions from the anode baking furnace are 

vented to a common control device; the A-446 scrubber. Figure 4.4 presents a process flow 

diagram of Anode Production. Figures 4.5 and 4.6 illustrate the A-446 and Procedair control 

devices.

FIGURE 4.4

ANODE PRODUCTION PROCESS FLOW DIAGRAM
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AQS Project# 13661-21-001

FIGURE 4.5

A-446 ANODE BAKE FURNACE CONTROL DEVICE
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AQS Project# 13661-21-001

FIGURE 4.6

PROCEDAIR ANODE PASTE PLANT CONTROL DEVICE
Page 13 of 19

AQS Project# 13661-21-001

SECTION 5

SAMPLING AND ANALYTICAL PROCEDURES

The sampling and analytical procedures used in this test program conformed to EPA Reference 

Methods 2, 3, 4, 5, and 29, as published in the Code of Federal Regulations, Title 40, Part 60, (40 

CFR 60) Appendix A. Additionally, Method 315, as published at 40 CFR 63 Appendix A.

LOCATION OF MEASUREMENT SITES

AQS utilized the pre-determined sampling points outlined in the Test Plan, as approved by the 

Kentucky Division for Air Quality. Sampling times were determined in consideration of the 

sample volumes specified in the ICR. Specific sampling locations, traverse points, and sampling 

times are listed in Table 5.1.

TABLE 5.1

SAMPLING TIMES

down 

stream

up stream POM PM - Metals

163S A-398 

Scrubber

1.3 3.0 10 240 240

Potline 3 

Downcomer

3.4 12.2 24 1,440 1,440

A-446 Anode Bake 

Furnace Scrubber

2.3 4.4 24 N/A 240

Anode Paste Plant 

Dry Coke Scrubber >2.0 >8.0 24 N/A 240

Sampling 

Location

Method 1 

Equivalent Diameters 

(from flow disturbance)

No. of 

Traverse 

Points

Test Run Duration, 

minutes

STACK GAS VOLUMETRIC FLOW RATE

EPA Method 2, “Stack Gas Velocity and Volumetric Flow Rate”, was used to determine 

volumetric flow rate. A Type “S” Pitot tube, with a standard coefficient of 0.84, and an inclined 

manometer were used to measure velocity pressure. A calibrated Type “K” thermocouple 

attached directly to the Pitot tube was used to measure stack gas temperature, which was 

displayed on a digital temperature indicator. The average stack gas velocity was calculated from: 

the average velocity pressure; the average stack gas temperature; stack gas molecular weight; and 
Page 14 of 19

AQS Project# 13661-21-001

absolute static pressure. The volumetric flow rate is the product of velocity and the stack crosssectional area. The specific actual sample volumes are listed in Table 5.2.

TABLE 5.2

SAMPLE VOLUMES

POM PM/Metals POM PM/Metals

163S A-398 Scrubber 3.0 4.0 4.5 4.5

Potline 3 Downcomer 3.0 4.0 22.5 27.9

A-446 Anode Bake 

Furnace Scrubber - - - 4.0 - - - 4.4

Anode Paste Plant Dry 

Coke Scrubber - - - 4.0 - - - 6.4

Sampling Location

Min. Sample Volume 

Required, dscm

Avg. Sample Volume 

Obtained, dscm

STACK GAS DRY MOLECULAR WEIGHT

EPA Method 3, “Gas Analysis for the Determination of Dry Molecular Weight”, was used to 

measure the CO2 and O2 concentrations of the stack gas at both the inlet and outlet sampling 

locations. The stack gas was collected from the center of the stack and extracted through a 

stainless steel tube, filter, and pump. The collected sample was analyzed using a Fyrite®

analyzer. Each sample was measured in duplicate or until a reading was repeated within 0.5%.

STACK GAS MOISTURE CONTENT

Concurrent with the Method 5/29 testing, EPA Method 4, “Determination of Moisture Content in 

Stack Gases”, was employed for these tests. AQS used a stainless steel probe assembly that 

connected to a series of Greenburg-Smith impingers by use of a Teflon®line. Once the sampling 

train was completely assembled, a leak check was performed before the start of the test run. 

Each of the impingers was weighed prior to use then reweighed after the test run to quantify the 

moisture gained. Following the leak check, the impingers were separated, the moisture on the 

exterior was removed, and they were reweighed to the nearest one-tenth gram. The totaled 

differences between the initial and final weights represented the moisture content of the stack gas 

during each test run.

FILTERABLE PARTICULATE MATTER

Method 17 (§8.1.2, also referencing Figure 17.2) specifies that the cross-section blockage caused 

by the sampling probe and filter holder assembly may not exceed 5% of the stack cross-sectional 

area. At the Downcomer testing location, the stack diameter is 14”, which calculates to 153.9 
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AQS Project# 13661-21-001

square inches stack area. The probe and in-stack filter assembly total 12 square inches in crosssectional area: 7.8% blockage. Thus, Method 5 was utilized at that location. The field work 

sheet is included in Appendix C. Concurrent with Method 29, EPA Method 5, “Determination 

of Filterable Particulate Emissions from Stationary Sources”, was used to determine filterable 

particulates at all sampling locations. AQS used a borosilicate glass nozzle and probe liner 

assembly connected to a glass filter bell containing a three-inch quartz-fiber filter with a Teflon®

frit to collect and separate the filterable particulate emissions. The filter holder was attached to 

the Method 29 sampling train. The impingers were placed in an ice bath during the sampling 

process. USEPA Method 5 is published at 40 CFR 60, Appendix A.

When the sampling train was completely assembled, a leak check was performed before the start 

of the test run. Stack gas volumes and sampling rates were controlled using a dry gas meter with 

calibrated orifice and a rotary vane vacuum pump. Meter temperature, stack temperature, and 

differential pressure were recorded at the appropriate intervals during each particulate test run. 

Upon completion of each test run, the system was post-leak checked at a vacuum greater than 

that achieved during the sample test run. Following the leak check, the impingers were 

separated, the moisture on the exterior was removed, and each impinger was reweighed to the 

nearest one-tenth gram. The totaled differences between the initial and final weights represented 

the moisture content of the stack gas during each test run.

The particulate matter was recovered from the test equipment by disassembling the filter bell and 

probe and rinsing and brushing the probe and front half of the filter bell with acetone, in 

triplicate. The acetone rinses from each test run were collected in amber glass bottles. The glass 

fiber filters were removed with forceps, placed in Petri dishes, and sealed for transport to the inhouse laboratory. 

At the laboratory, the filters were placed in a desiccator for a minimum of 24 hours prior to 

weighing. The acetone rinses were transferred to beakers and evaporated at room temperature 

until dry. The beakers were also placed in a desiccator for 24 hours prior to weighing. Filter and 

acetone blanks were processed in a similar manner. 
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AQS Project# 13661-21-001

FIGURE 5.1

METHOD 5 STACK SAMPLING TRAIN DIAGRAM

METALLIC HAPS

Concurrent with Method 5, EPA Method 29, “Determination of Metals Emissions from 

Stationary Sources”, was employed for these tests. AQS used a borosilicate glass nozzle and 

probe liner assembly connected to a glass filter bell containing a three-inch quartz-fiber filter 

with a Teflon®frit. The stack gases passed through the filter before entering the sampling train. 

The first and second impingers contained 5% HNO3/10% H2O2, the third impinger was empty, 

the fourth and fifth impingers contained 4% KMnO/10% H2SO4 and the final impinger contained 

approximately 300 grams of indicating silica gel. This impinger assembly allows for the 

collection of gaseous metallic HAPS, including mercury. The impingers were placed in an ice 

bath during the sampling process. 

When the sampling train was completely assembled, a leak check was performed before the start 

of the test run. Stack gas volumes and sampling rates were controlled using a dry gas meter with 

calibrated orifice and a rotary vane vacuum pump. Meter temperature, stack temperature, and 

differential pressure were recorded at five-minute intervals during each 120-minute test run. 

Upon completion of each test run, the system was post-leak checked at a vacuum greater than 

that achieved during the sample test run. Following the leak check, the impingers were 

separated, the moisture on the exterior was removed, and each impinger was reweighed to the 

nearest one-tenth gram. 
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AQS Project# 13661-21-001

The particulate matter was recovered from the test equipment by removing the nozzle, probe, and 

front half of the filter holder then rinsing and brushing each component with 0.1 N HNO3, in 

triplicate. The acetone rinses from each test run were collected in amber glass bottles. The glass 

fiber filters were placed in glass bottles, and sealed prior to delivery to the laboratory. 

The impingers and the connecting glassware were rinsed in duplicate with 0.1 N HNO3 and 

collected with the impinger contents in 0.1 N HNO3 rinsed amber glass bottles. Samples were 

analyzed by TestAmerica Laboratories of Knoxville. 

FIGURE 5.2

METHOD 29 STACK SAMPLING TRAIN DIAGRAM

METHYLENE CHLORIDE EXTRACTABLE MATTER

EPA Method 315 (40 CFR 63, Appendix A), “Determination of Particulate and Methylene 

Chloride Extractable Matter from Stationary Sources”, was employed for to determine POM at 

the Potline 3 163S A-398 Scrubber and Potline 3, Room 6 Roof Monitor Sampling Manifold

(aka Downcomer). The collected samples and blanks were sent to a Resolution Analytics of 

Sanford, NC for analysis.

Method 315 specifies the use of the standard particulate sampling train described in Method 5 

(40 CFR 60, Appendix A). In Method 5, the gas sample is pulled though a sampling nozzle, 

probe, and a filter – all are heated to 250°F. At the point the gas leaves the filter holder, it is no 

longer heated. Downstream of the filter, the gas is cooled in a condenser consisting of a train of 

impingers. Following each test run, the front half of the sample train (nozzle, probe liner, front 

of filter holder) is brushed and acetone-rinsed, then brushed and rinsed with methylene chloride. 
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AQS Project# 13661-21-001

The water in the condenser is recovered, and then the back half of the sample train (back of filter 

holder, all impingers, and all connecting lines) is rinsed with water, then acetone, then methylene 

chloride. These preparation, sampling, and recovery procedures were followed without 

deviation. 

PERFORMANCE AUDITS

In accordance with the applicable requirements specified in 40 CFR 63.7(c)(2)(iii), the US EPA 

Web site was accessed at least 60 days prior to the test dates. At that time, there were 

commercially available performance audit samples for particulates on filter from one supplier. 

EPA rules do not require the use of performance audit samples unless there are at least two 

suppliers. No audit samples were utilized in this test program. Documentation can be found on

EPA’s Web site: http://www.epa.gov/ttn/emc/email.html.
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AQS Project# 13661-21-001

SECTION 6

QUALITY ASSURANCE / QUALITY CONTROL

All manual stack gas sampling equipment was calibrated before the test program in accordance 

with the procedures outlined in the Quality Assurance Handbook for Air Pollution Measurement 

Systems, Volume III, EPA-600/4-72-027B. The stack gas sampling equipment calibrations that 

were performed in preparation for this project are summarized in Table 5.1. Calibration data are 

included as Appendix G.

TABLE 6.1

FIELD EQUIPMENT CALIBRATION SUMMARY

Field Equipment Calibrated Against Allowable Error

Method 5 Dry Gas Meter Stainless Steel Critical

Orifice Set

Y + 0.02 Y

ΔH @ + 0.15

Post Test Y + 0.05 Y

Pitot Tube Geometric Specifications See EPA Method 2

Probe nozzles Calipers Max. Difference 0.004 in. 

between two measurements

Thermocouple ASTM – 3F thermometer + 1.5%

Condenser Thermometer ASTM – 3F thermometer + 2°F

Dry Gas Thermometer ASTM – 3F thermometer + 5°F

Barometer NBS Traceable Barometer + 0.01 in. Hg

AQS’ stack testing policies and practices conform to ASTM D7036-04 “Standard Practice for 

Competence of Air Emission Testing Bodies” for emission testing programs affected by the 

requirements of 40 CFR 75.21(f), as performed on Part 72 sources and Part 75 sources.

ASTM D7036-04 notwithstanding, it is our mission to be a trusted provider of air-related 

environmental services. We aspire to exceed client expectations by imparting exceptional 

quality and value in meeting corporate needs and fulfilling regulatory requirements.

The AQS Quality Objectives are:

 to continually monitor and improve our ability to deliver the scope of services

 to assign qualified test personnel to satisfy the needs of our clients

 to comply with quality control procedures established in test methods, in the AQS 

Quality Manual, and by regulatory agencies that have jurisdiction over test programs

 to prepare reports that clearly communicate test program results

 to utilize recordkeeping systems that allow for data retrieval and reconstruction

 to keep clients apprised of project progress and promptly respond to concerns