## CLEAN AIR ACT (CAA) SECTION 114 EMISSION S DATA

COLLECTION REQUEST F OR THE PRIMARY ALUMI NUM

REDUCTION PLANT SOUR CE CATEGORY

TEST REPORT

P OTLINE 

### 3 163S A

- 398 S CRUBBER AND 

### P OTLINE 

### 3, R OOM 

### 6 R OOF 

### M ONITOR



### S AMPLING 

### M ANIFOLD 

### ( AKA 

### D OWNCOMER 

### ) Polycyclic Organic Ma tter (POM), Metallic Hazardous Air Pollutants (Metallic HAPS)

and Total Filterable Particulate Matter (PM)



### A

- 446 A NODE 

### B AKE 

### F URNACE 

### S CRUBBER AND


### A NODE 

### P ASTE 

### P LANT 

### D RY 

### C OKE 

### S CRUBBER 

### ( AKA 

### P ROCEDAIR 

### )

Metallic HAPS and PM

Performed for:


### RIO TINTO ALCAN

SEBR EE WORKS

9404 State Route 2096

Robards , KY 424 52

April 15

– 19, 201 3 April 24 , 20 1 3

Submitted by :

Air Quality Services, LLC

425 Main Street Evansville, Indiana 47708 Phone: (812) 452

- 4785 Fax: (812) 452

- 4786

AQS Project # ’s 1 3 66 1

- 21

- 001 & 13661

- 2 1

- 002ii



## 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 2 9 , 2013iii TABLE OF CONTENTS

Page

SECTION 1 EXECUTIVE SUMMARY

................................ .............................. 1

SECTION 2 INTRODUCTION

................................ ................................ ............ 3

SECT ION 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 Ga s Moisture Content

................................ ........................ 14

Filterable Particulate Matter

................................ ......................... 14

Metallic HAPS

................................ ................................ ............. 16 Methylen e Chloride Extractable Matter

................................ ....... 17

Performance Audits

................................ ................................ ..... 18

SECTION 6 QUALITY ASSURANCE / QUALITY CONTROL

.................... 19

APPENDIX A

- EXAMPLE CALCULATIONS

APPENDIX B

- DATA SUMMAR IES

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 RESPONSESiv 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

................................ ..................... 1 9

LIST OF FIGUR ES

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

................................ ................. 1 6

5.2 Method 29 Stack Sampling Train Diagram

................................ ............... 17

LIST OF AB B REVIATIONS

ascfm actual standard cubic feet per minute

dscfm dry standard cubic feet per minute gr/ds cf 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 reactorPage 1 of 1 9 AQS Project# 1366 1

- 2 1

- 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 Works facility in Robards, Kentucky (Source ID # 21

- 101

- 00029 ). The testing program addresse d 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 wi th Potline 3: (1) the 163S A

- 398 S crubber 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 D ry C oke Scrubber (aka P rocedair )

During the test program, Potline #3, the A

- 446 Anode Bake Furnace

, and the Anode Paste Plant

w ere operat ed 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, Appe ndix A

.

T he test program was conducted from April 15

– 19 and April 24, 2013

. T he results of the

e missions t ests are summarized below:

TABLE 1.1

AVERAGE NON

- METALLIC EMISSIONS TEST RESULTSPage 2 of 1 9 AQS Project# 1366 1

- 2 1

- 001 TABLE 1. 2

METALLIC HAPS EMISSIONS T EST RESULTS

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 2012Page 3 of 1 9 AQS Project# 1366 1

- 2 1

- 001 SECT ION 2

INTRODUCTION

A lcan retain ed 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 S crubber and the Potline 3, Room 6 Roof Monitor Sampling Manifold (aka Downcomer) ; along with m etallic

HAPS and filterable PM from the three

- section A

- 446 Anode Bake Furnace Scrubber and the

An ode Paste Plant D ry C oke Scrubber (aka Procedair )

. The testing was conducted over two separate mobil i zations: April 15

– 19 and April 24, 2013

.

The sampling was conducted usin g EPA Methods 2, 3, 4, 5, 29

, and 315 to determine velocity

and volumetr ic flow rates, molecular weight , moisture content, selected metal lic HAPs

, and

POM (as methylene chloride extractable material) concentration s, respectively. Jeff Wollrab (Project Manager), Marshall Peters, Jacob Luker, Ryan Neumann

, and Austin Moore

, of AQS

, performed the samp ling procedures

. No regulatory observers were present during this testing.

The contacts for this test program were a s follows:

TABLE 2.1

TEST PROGRAM CONTACTS

Rio Tinto A lcan

– 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

42 5 Main Street Evansville, IN 47708 Phone: (812) 452

- 4785 Fax: (812) 452

- 4786

E

- mail: dtodd@aqsllc.net jwollrab @aqsllc.netPage 4 of 1 9 AQS Project# 1366 1

- 2 1

- 001 SECTION 3

SUMMARY OF TEST RESULTS

Potline 3 163S A

- 398 Scrubber

The pro duction rate of the pro cess 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 Appendi x B.

Using the procedures described in EPA Methods 5, 29

, and 315

, total fi lterable 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) fou r

- 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 (CO 2 )

, 19.5 % oxygen (O 2 )

, and

80

. 0 % nitrogen (N 2 ); the ga s temperature averaged 21 5

. 9 oF; the moisture content averaged 1.9 %; and the velocity averaged 39

. 9 feet per second (fps). The measured volumetric flow rate averaged 4 7

, 9 31 actual cubic feet per minute (acfm). Converting the measured volumetric flow rate to standard conditions, the exhaust averaged 3 6

, 526 dry standard cubic feet per minute (dscfm).

The average si x

- 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 Table s 1.1 and

1.2 of this report. Individual test run s tack 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 ar e 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 ox ygen 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 averag ed approximately 0

. 3 % CO 2, 20.0 % O 2, and 79

. 7 % N 2 ; the ga sPage 5 of 1 9 AQS Project# 1366 1

- 2 1

- 001 temperature averaged 99. 4 oF; the moisture content averaged 1. 4 %; and the velocity averaged

49. 2 fps. The measured volumetric flow rate averaged 3,1 60 acfm. Converting the measured

volumetric flow rate to standard conditions, the exhaust averaged 2

, 9 10 dscfm. In order to extrapolate the Downcomer test results to reflect Pot room 6 South , the flow measurements from

the roof

- mounted anemometers were used. Based upon the anemometer data, the roof mon itor exhaust averaged 1,137,777 acfm. Converting the measured volumetric flow rate to standard

condi tions, the exhaust averaged 1,0 4 3

, 76 1 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 Table s 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 pro duction 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 Appendi x B.

Using the procedures described in EPA Met hods 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 f

rom representative reactor sections of the A

- 446 Anode Bake Furnace Scrubber

on April 1 5 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 (moi sture).

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

- 446

Anode Bake Furnace Scrubber averaged approximately 0

. 3 % CO 2, 19

. 5 % O 2, and 80

. 2 % N 2 ; the

ga s temperature averaged 177 .9 oF; the moisture content averaged 9

. 4 %; and the velocity averaged 4 6

. 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 Table s 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 pro duction rate of the proces s 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 Appendi x B.

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

were measured at the Procedair exhaust. GPS coordinates for this sampling location are latitudePage 6 of 1 9 AQS Project# 1366 1

- 2 1

- 001 37.658877 and longitude 87.499145. Three (3) four

- hour test runs were conducted at the exhaust

of the Procedair control devi ce on April 1 9 and 2 2 , 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 ga s composition at the Procedair averaged approximately 0

. 5 % CO 2, 19.5 % O 2, and 80

. 0 % N 2 ; the ga s temperature averaged

98

. 3 oF; the moisture content averaged 1

. 0 %; and the velocity averaged 4 7

. 9 fps . The measured volumetric flow rate averaged 45

, 697 acfm . C onverting 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 Table s 1.1 and 1.2 of this report. Individual test run stack gas p arameter measurements and test results are presented in Appendix B.4.

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

The f ield d ata sh eets are included as Appendix C , potroom flow calculations are included as Appendix D, l aboratory data are contained in Appendix F and ICR Table Responses are included as Appendix H

.Page 7 of 1 9 AQS Project# 1366 1

- 2 1

- 001 SECTION 4

PROCESS DESCRIPTION S

Rio Tint o 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 (Al 2 O 3 ) 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 cons tituent sp ecies aluminum (Al) and

O 2 . 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 bloc ks 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 ne w anodes. Figure 4.1 presents a process flow diagram of the potline operations.Page 8 of 1 9 AQS Project# 1366 1

- 2 1

- 001 FIGURE 4.1

POTLINE OPERATIONS P ROCESS FLOW DIAGRAMPage 9 of 1 9 AQS Project# 1366 1

- 2 1

- 001 FIGURE 4.2

COMBINATION DRY ALUMINA SCRUBBER/BAGHOUSE

FIGURE 4.3

A

- 398 FUME CONTROL SY STEM

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, re cycled 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 C ells

– 64 on each side:
One Bank vents 128 cells One Bank (group of 5 R eactors)Page 10 of 1 9 AQS Project# 1366 1

- 2 1

- 001 The formed anodes are compressed and placed withi n 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 Product ion. Figures 4. 5 and 4. 6 illustrate the A

- 446 and P rocedair control

devices.

FIGURE 4. 4

ANODE PRODUCTION PROCESS FLOW DIAGRAMPage 11 of 1 9 AQS Project# 1366 1

- 2 1

- 001 FIGURE 4. 5

A

- 446 ANODE BAKE FURNA CE CONTROL DEVICEPage 12 of 1 9 AQS Project# 1366 1

- 2 1

- 001 FIGURE 4. 6

PROCEDAIR ANODE PASTE PLANT CO NTROL DEVICEPage 13 of 1 9 AQS Project# 1366 1

- 2 1

- 001 SECTION 5

S AMPLING 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. Addition ally, 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 con sideration 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

STACK GAS VOLUMETRIC FLOW RATE

EPA Method 2, “ Stack G as Vel ocity and Volumetric Flow Rate”, was used to determine

vol umetric flow rate. A Type “S” P itot tube, with a standard coefficient of 0.84, and an inclined manometer were used to measure velocity pressure. A calibrated Type “K” thermocouple

attached d irectly to the P itot 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 mo lecular weight; andPage 14 of 1 9 AQS Project# 1366 1

- 2 1

- 001 absolute static pressure. The volumetric flow rate is the product of velocity and the stack cross

sectional area. The specific actual sample volumes are listed in Table 5.2.

TABLE 5.2

SAMPLE VOLUMES

STAC K GAS DRY MOLECULAR WEIGHT

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

measure the CO 2 and O 2 concentration s of the stack gas at both the inlet and outlet sampling locations. The stack gas was collected from th e 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 CON TENT

Concurrent with the Method 5 /29 testing, EPA Method 4, “ Determination of M oisture 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 Te flon ® 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 le ak 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 153.9Page 15 of 1 9 AQS Project# 1366 1

- 2 1

- 001 square inches stack area. The probe and in

- stack filter assembly total 12 square inches in cross

sectional 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 b orosilicate 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 2 9 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 parti culate 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 e ach 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 b y 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 in

house 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 evapora ted 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.Page 16 of 1 9 AQS Project# 1366 1

- 2 1

- 001 FIGURE 5.1

METHOD 5 STACK SAMPLING TRAIN DIAGRAM

METALLIC HAPS

Concurren t 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% HNO 3 /10% H 2 O 2 , the third impinger was empty, the fourth and fifth impingers contained 4% KMnO/10% H 2 SO 4 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. F ollowing 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.Page 17 of 1 9 AQS Project# 1366 1

- 2 1

- 001 The particulate matter was recovered from the test equipment by removing the nozzle, probe, an d front half of the filter holder then rinsing and brushing each component with 0.1 N HNO 3 , 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 HNO 3 and collected with the impinger contents in 0.1 N HNO 3 rinsed amber glass bottle s

. Samples were analyzed by TestAmerica Laboratories of Kn oxville.

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 us e 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 i s 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, th en brushed and rinsed with methylene chloride.Page 18 of 1 9 AQS Project# 1366 1

- 2 1

- 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

W eb site was accessed at least 60 days prior t o the test date s. At that time, there were commercially available performance audit samples for particulate s 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 sam ples were utilized in this test program. D ocument ation can be found on
EPA’s Web site: http://www. epa.gov/ttn/emc/email.html

.Page 19 of 1 9 AQS Project# 1366 1

- 2 1

- 001 SECTION 6

QUALITY ASSURANCE / QUALITY CONTROL

All manual stack gas sampling equipment was calibrated before the test progra m 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 summ arized 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

Δ H @ + 0.15

Post T est 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 Thermomet er 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 imparti ng 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 satis fy 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 resu lts

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

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