Characterization of Dioxin Emissions

From Sources That Use Ball Clays

Emission Test Report: Unimin Corporation, 

Gleason, TN

Final Report

(Non-Confidential Version)
EPA-453/R-10-001

 

CHARACTERIZATION OF DIOXIN EMISSIONS FROM SOURCES THAT USE BALL 

CLAYS

EMISSION TEST REPORT: UNIMIN CORPORATION, GLEASON, TN

FINAL REPORT (Non-Confidential Version)

U.S. ENVIRONMENTAL PROTECTION AGENCY

Office of Air Quality Planning and Standards

Sector Policies and Programs Division

Research Triangle Park, North Carolina 27711

v

Contents

Figures vii

Tables viii

Section 1. Introduction..................................................................................................... 1-1

1.1 Test Summary............................................................................................ 1-1

1.2 Test Program Organization........................................................................ 1-1

Section 2. Process Description and Test Locations......................................................... 2-1

2.1 Description of Processes Tested................................................................ 2-1

2.2 Process Operations During Testing ........................................................... 2-1

2.3 Sampling and Emission Measurement Locations...................................... 2-3

2.4 Process Feed and Product Sampling.......................................................... 2-4

2.5 Correlation of Sample Identification Numbers With Test Runs............... 2-5

Section 3. Test Results..................................................................................................... 3-1

3.1 Objectives.................................................................................................. 3-1

3.2 Test Matrix ................................................................................................ 3-1

3.3 Field Test Changes and Problems ............................................................. 3-1

3.4 Summary of Test Results........................................................................... 3-3

Section 4. Procedures for Sampling, Analysis, and Process Data Collection.................. 4-1

4.1 Sampling Methods..................................................................................... 4-1

4.2 Analytical Procedures................................................................................ 4-9

4.3 Process Data ............................................................................................ 4-12

Section 5. QA/QC Activities............................................................................................ 5-1

5.1 QA/QC Objectives Summary.................................................................... 5-1

5.2 Surrogate Recoveries................................................................................. 5-2

5.3 Discussion.................................................................................................. 5-2

Appendices

Appendix A—Sample Custody Records

Appendix B—Sampling Data and Field Analytical Records

Appendix C—Equipment Calibration Records

Appendix D—Analytical Reports and Data

Appendix E—Batch Control Spikes (BCS3)

Appendix F—BCS3 Performance Criteria

Appendix G—Process Data and Material Sampling Log Sheets
vi
vii

Figures

Figure 1-1. Test Program Organization ....................................................................... 1-3

Figure 2-1. Process Flow Diagram for the Mill Process at Unimin Corporation, 

Gleason, TN............................................................................................... 2-6

Figure 2-2. Process Flow Diagram for the Dryer Process at Unimin Corporation, 

Gleason, TN............................................................................................... 2-7

Figure 2-3. Mill Sampling Location............................................................................. 2-8

Figure 2-4. Dryer Sampling Location .......................................................................... 2-9

Figure 4-1. Method 23 Sampling Train for PCDDs and PCDFs ................................. 4-3

Figure 4-2. Sample Recovery Scheme ......................................................................... 4-5

Figure 4-3. Instrumental Measurement System for CO2 and O2.................................. 4-7

Figure 4-4. Schematic of EPA Method 23 and SW846 8290 Emission 

Samples Analysis Path ............................................................................ 4-10

Figure 4-5. Schematic of Process Samples Analysis Path ......................................... 4-13
viii

Tables

Table 2-1. Summary of Process Operating Parameters Monitored During Testing 

for the Mill .................................................................................................. 2-2

Table 2-2. Summary of Process Operating Parameters Monitored During Testing 

for the Dryer................................................................................................ 2-3

Table 2-3. Correlation of Sample Identification Numbers With Test Runs................. 2-5

Table 3-1. Test Matrix: Summary of Emission and Process Sampling and 

Analytical Parameters and Methods ........................................................... 3-2

Table 3-2. Summary of Total Dioxin/Furan Results for Mill Samples........................ 3-5

Table 3-3. Dioxin/Furan Homolog Results for Mill Stack Samples............................ 3-6

Table 3-4. Dioxin/Furan Homolog Emission Factors for Mill Stack Samples............ 3-7

Table 3-5. Dioxin/Furan Mill Clay Feed Homolog Resultsa........................................ 3-8

Table 3-6. Dioxin/Furan Mill Clay Product Homolog Resultsa................................... 3-9

Table 3-7. Mill Sampling and Stack Parameters........................................................ 3-10

Table 3-8. Summary of Total Dioxin/Furan Results for Dryer Samples ................... 3-11

Table 3-9. Dioxin/Furan Homolog Results for Dryer Stack Samples........................ 3-12

Table 3-10. Dioxin/Furan Homolog Emission Factors for Dryer Stack Samples....... 3-13

Table 3-11. Dioxin/Furan Dryer Clay Feed Homolog Resultsa .................................. 3-14

Table 3-12. Dioxin/Furan Dryer Clay Product Homolog Resultsa.............................. 3-15

Table 3-13. Dryer Sampling and Stack Parameters .................................................... 3-16

Table 5-1. Calibration QC Criteria for Sampling Equipment ...................................... 5-3

Table 5-2. Criteria for Emission Measurement and Data Quality................................ 5-4

Table 5-3. Criteria for Assessing Data Quality of Process Sample Analyses.............. 5-5

Table 5-4. Method 23 Internal Standard and Surrogate Standard Recoveries............. 5-6

Table 5-5. BCS3 Surrogate Recoveries ........................................................................ 5-7

Table 5-6. Method 8290 Internal Standard Recoveries................................................ 5-8
1-1

Section 1.

Introduction

1.1 Test Summary

1.1.1 Background

The EPA has determined that certain ball clay mineral deposits contain naturallyoccurring dioxins. Ball clay processing facilities use low temperature dryers and heated 

milling systems to process ball clay prior to shipment to customers. The purpose of this 

emission test was to characterize dioxin (and furan) emissions from these dryers and 

milling systems. The test results will be used by EPA to determine the need for gathering 

any additional data related to thermal processing of ball clay.

1.1.2 Scope

RTI presented MRI with Work Assignment No. 1-08 to conduct the emissions test 

from two process lines at the selected ball clay test site. Under the work assignment MRI 

conducted emissions testing for polychlorinated dibenzodioxins (PCDDs) and 

polychlorinated dibenzofurans (PCDFs), carbon dioxide (CO2), and oxygen (O2).

Three 4-hour test runs, using EPA Method 23 to measure dioxin and furan emissions, 

were conducted at each of the two test stack locations within the facility. In addition, the 

CO2 and O2 concentrations were measured during each run using EPA Method 3 at the 

dryer and Method 3A at the mill.

During testing, process and pollution control equipment operating data were obtained 

by RTI. In addition, RTI collected process samples at two points (feed and product) 

within each process line during the test runs. These samples also were analyzed for 

PCDDs/PCDFs.

1.2 Test Program Organization

The following individuals were the key personnel in the management and execution 

of this project:
1-2

The EPA Work Assignment Managers (WAMs):

Ms. Mary Johnson [during the test program]

U.S. Environmental Protection Agency 

Office of Air Quality Planning and Standards

Sector Policies and Programs Division

Research Triangle Park, NC 27711

Telephone: (919) 541-5025

Mr. Brian Shrager

U.S. Environmental Protection Agency 

Office of Air Quality Planning and Standards

Sector Policies and Programs Division

Research Triangle Park, NC 27711

Telephone: (919) 541-7689

The EPA on-site testing WAM:

Clyde E. Riley [during the test program]

U.S. Environmental Protection Agency

Office of Air Quality Planning and Standards

Emissions, Monitoring and Analysis Division

Emission Measurement Center

Research Triangle Park, NC 27711

J. Kaye Whitfield [current testing WAM]

U.S. Environmental Protection Agency

Office of Air Quality Planning and Standards

Emissions, Monitoring and Analysis Division

Source Measurement and Analysis Group

Research Triangle Park, NC 27711

Telephone: (919) 541-2509

The RTI Work Assignment Leader (WAL): The MRI Task Leader for this project:

Mr. Mark Turner Mr. John Hosenfeld

Research Triangle Institute Midwest Research Institute

800 Park Office 425 Volker Blvd.

Highway 54 Kansas City, MO 64110-2299

Research Triangle Park, NC 27709 Telephone: (816) 753-7600, ext. 1336

Telephone: (919) 316-3743

Figure 1-1 presents the test program organization, major lines of communication, and 

names and phone numbers of responsible individuals.
1-3

Figure 1-1. Test Program Organization
1-4
2-1

Section 2.

Process Description and Test Locations

2.1 Description of Processes Tested

Emissions testing for PCDDs and PCDFs was conducted at the Unimin Corporation 

ball clay processing facility located in Gleason, Tennessee during a two week period in 

August 2003. Two processes were tested during the emission testing program; Mill 

No. 3 (mill) was tested on August 13, 14, and 15, 2003, and the Semi-Dry Dryer (dryer) 

was tested on August 18, 19, and 20, 2003. This section provides a brief description of 

the processes tested. 

CBI Data Removed

This information is provided in the confidential version of this document.

2.2 Process Operations During Testing

This section describes process operations during testing. Summary data are 

presented that represent the average of the parameters monitored during each emission 

test run. CBI Data Removed: Additional information is provided in the confidential 

version of this document. The following sections describe process operations during 

testing for the mill and the dryer, respectively.

2.2.1 Mill No. 3

The mill was tested on August 13, 14, and 15, 2003. Several process operating 

parameters were monitored to ensure that the mill was operating normally during 

emissions testing. These parameters included baghouse inlet temperature, baghouse 

pressure drop, mill operating temperature, and mill production rate. CBI Data 

Removed: Additional information is provided in the confidential version of this 

document. During testing, values for each of these parameters were manually recorded 

on data log sheets at least every 30 minutes beginning before testing began and 

continuing for one reading after the test was concluded. The mill operating temperature 

is measured at the mill outlet. CBI Data Removed: Additional information is provided 

in the confidential version of this document. The average hourly rate (for each shift 

during which testing occurred) was obtained from plant personnel at the conclusion of 

testing the mill. 

CBI Data Removed

Additional information is provided in the confidential version of this document.

Table 2-1 presents a summary of the process operating parameters recorded for 

the mill during the testing program. CBI Data Removed: Additional information is 

provided in the confidential version of this document. Raw data sheets for these 

parameters are found in Appendix G. 
2-2

Table 2-1. Summary of Process Operating Parameters Monitored During Testing 

for the Mill

Test

Run 

No.

Date

Tested

Ball Clay 

Product 

Processed

Mill Operating 

Temperature,

°C (°F)

Baghouse Inlet

Temperature,

°C (°F)

Baghouse 

Pressure Drop,

Inches of Water

Mill

Production Rate, 

Mg/Hour

(Tons/Hour)

1Rea 8/13/03 SB Blend b b 2.5 b

2 8/14/03 SB Blend b b 2.5 b

3 8/15/03 Rex b b 2.5 b

Average = b b 2.5 b

a

1Re refers to Run 1 retest; Run 1 was aborted due to failed leak check.

b CBI data removed: See confidential version of document.

2.2.2 Semi-Dry Dryer

The dryer was tested on August 18, 19, and 20, 2003. Several process operating 

parameters were monitored to ensure that the dryer was operating normally during 

emissions testing. These parameters included baghouse inlet temperature, baghouse 

pressure drop, dryer operating temperature, and dryer production rate. CBI Data 

Removed: Additional information is provided in the confidential version of this 

document. During testing, values for each of these parameters were recorded on data log 

sheets at least every 30 minutes beginning before testing began and continuing for one 

reading after the test was concluded. The dryer operating temperature is the temperature 

of the supply air to the dryer. CBI Data Removed: Additional information is provided 

in the confidential version of this document. The average hourly rate (for each shift 

during which testing occurred) was obtained from plant personnel at the conclusion of 

testing the dryer.

CBI data removed

Additional information is provided in the confidential version of this document.

Table 2-2 presents a summary of the process operating parameters recorded for the 

dryer during the testing program. CBI Data Removed: Additional information is 

provided in the confidential version of this document. Raw data sheets for these 

parameters are found in Appendix G. 
2-3

Table 2-2. Summary of Process Operating Parameters Monitored During Testing 

for the Dryer

Test

Run 

No.

Date

Tested

Ball Clay 

Product 

Processed

Dryer Operating 

Temperature,

°C (°F)

Baghouse Inlet

Temperature,

°C (°F)

Baghouse 

Pressure Drop, 

Inches of Water

Dryer

Production Rate, 

Mg/Hour

(Tons/Hour)

4 8/18/03 SB Blend a a 5.5 a

5 8/19/03 SB Blend a a 5.6 a

6 8/20/03 SB Blend a a 5.7 a

Average = a a 5.6 a

a CBI data removed: See confidential version of document.

2.3 Sampling and Emission Measurement Locations

2.3.1 Location 1—Mill Baghouse

Sampling was conducted for PCDD/PCDF emissions at the mill baghouse outlet 

stack. The existing test platform plus an added platform section was used for the 

sampling trains and test personnel. The modified platform was L-shaped to allow access 

to both ports. The metering box (console) was located and operated approximately 5 feet 

away, on one section of the new platform. Gas sampling and analytical instrumentation 

for CO2 and O2 was located and operated approximately 100 feet away in the 

environmentally-controlled MRI mobile lab.

The sampling location was within the 28-foot-long straight vertical section of the 

mill baghouse outlet stack. Sampling was conducted approximately 16 feet downstream 

and 12 feet upstream of the nearest flow disturbances. Because a downstream flow 

disturbance existed at about 5 duct diameters (rather than 8) from the sample location, 

40 traverse points were used during sampling. The sampling location is presented in 

Figure 2-3. Two 4-inch ports were installed in the stack at approximately 40 inches 

above the platform. The top rail of the existing platform railing was removed 9 inches on 

either side of the additional ports to accommodate train movement on the platform. A 

small 2-inch port was installed to accommodate CEMS sampling 12 inches below and 

offset 180 degrees from the existing ports. 

The internal diameter of the cross-sectional sampling area inside the stack is 

approximately 36 inches. A total of 40 traverse (sampling) points were used for the 

Method 23 traversing sampling train, 20 on each traverse (through each port) across the 

internal diameter of the duct. Each traverse consisted of one pass with 6-minute readings 

per point at isokinetic conditions. Total sampling time for each run was 240 minutes or 4 

hours for the Method 23 sampling train. 

One 2-inch port with threaded plug (2-inch pipe coupling) was installed for gas 

sampling and instrumental analysis for CO2 and O2. The placement of the CEM probe 

end in the stack was at a point of average velocity.
2-4

2.3.2 Location 2—Dryer Baghouse

Sampling was also conducted for PCDD/PCDF emissions at the dryer baghouse 

outlet stack. A modified test platform and the existing walkway adjacent to the product 

screw feeder were used for the sampling trains and test personnel. The metering box 

(console) was located on the modified test platform. Fugitive emissions were observed in 

the dryer baghouse vicinity. Thus, with the concurrence of the on-site WAM, the MRI 

mobile lab was left at the mill to avoid potential contamination from ambient conditions. 

The distance from the mobile lab with the CEMS to the dryer precluded installing the 

CEMS sampling line. Therefore, gas sampling for CO2 and O2 was performed by 

collecting an integrated bag sample from the console during the test run.

The sampling location was in the 16.6-foot long straight vertical run of the dryer 

baghouse outlet stack (45 feet total height). Sampling was conducted approximately 

5 feet upstream and 11 feet downstream of the nearest flow disturbances. Because a 

downstream flow disturbance existed at about 5 duct diameters (rather than 8) from the 

sample location, 40 traverse points were used during sampling. This location is presented 

in Figure 2-4. Two 4-inch ports were installed at approximately 40 inches above the 

platform. The ideal port location would have been to have one port with a traverse that is 

congruent to the direction of the bend prior to the ports. However, due to process 

obstructions interfering with the operation of the sampling equipment at the test location, 

the ports were positioned 45 degrees off this ideal direction. This requirement becomes 

less critical as the distance from the disturbance increases and is not expected to have a 

significant effect on data. The top rail of the existing platform railing was removed 

9 inches on either side of the additional ports to accommodate train movement on the 

platform. 

The internal diameter of the cross sectional sampling area inside the stack is 

approximately 24 inches. A total of 40 traverse (sampling) points were used by the 

Method 23 traversing sampling train, 20 on each traverse (through each port) across the 

internal diameter of the duct. Each traverse consisted of one pass with 6-minute readings 

per point at isokinetic conditions. Total sampling time for each run was 240 minutes or 

4 hours for the Method 23 sampling train.

2.4 Process Feed and Product Sampling

An integral part of the test program was the sampling and subsequent analysis of 

both the ball clay feed and product from the mill and the dryer. During each test run, 

samples of the feed material and samples of the product were taken using aluminum foillined scoops at least every 30 minutes beginning before testing began and continuing for 

one sample after the test was concluded. The feed material and product samples were 

placed in separate aluminum-foil-lined trays; each tray was covered with aluminum foil 

after each sample was placed in the tray to protect the sample from contamination. At the 

end of each test run, the trays were removed to a secure location, the samples were mixed 

and composited, and the composited samples were placed in labeled sample bottles for 
2-5

PCDD/PCDF analysis. A duplicate of each sample was provided to the Unimin 

representative.

Samples of the ball clay feed material to the mill were collected at the inlet to the 

mill using an aluminum-foil-lined scoop. Samples of the ball clay product from the mill 

were collected from one of the primary cyclone product collection pipes using a separate 

aluminum-foil-lined scoop. Material sampling logs for the ball clay feed material to the 

mill and the mill product are located in Appendix G.

Samples of the ball clay feed material to the dryer were collected at the inlet to the 

dryer using an aluminum-foil-lined scoop. Samples of the ball clay product from the 

dryer were collected from the sampling port for the second stage bucket elevator for the 

dryer using a separate aluminum-foil-lined scoop. Material sampling logs for the ball 

clay feed material to the dryer and the dryer product are located in Appendix G.

2.5 Correlation of Sample Identification Numbers With Test 

Runs

Table 2-3 provides a correlation of the sample identification numbers with the test 

runs. The data in Table 2-3 are provided to allow the reader to readily identify the 

relevant raw data for the test runs in the Appendices.

Table 2-3. Correlation of Sample Identification Numbers With Test Runs

Test

Run

No.

Sample

Collection 

Date

Method 23 

Sample ID

Numbers

Mill Feed 

Sample ID 

Numbers

(Method 8290)

Mill Product 

Sample ID 

Numbers

(Method 8290)

Dryer Feed 

Sample ID 

Numbers

(Method 8290)

Dryer Product 

Sample ID 

Numbers

(Method 8290)

1Re 8/13/03 1009 1111 1121

2 8/14/03 2009 2111 2121

3 8/15/03 3009 3111 3121

4 8/18/03 4004 4211 4221

5 8/19/03 5004 5211 5221

6 8/20/03 6004 6211 6221
2-6

(CBI data removed. See confidential version of document.)

Figure 2-1. Process Flow Diagram for the Mill Process at Unimin Corporation, 

Gleason, TN
2-7

(CBI data removed. See confidential version of document.)

Figure 2-2. Process Flow Diagram for the Dryer Process at Unimin 

Corporation, Gleason, TN
2-8

Figure 2-3. Mill Sampling Location
2-9

Figure 2-4. Dryer Sampling Location
2-10
3-1

Section 3.

Test Results

3.1 Objectives

The purpose of this test was to assist EPA in determining the emission levels of 

PCDDs and PCDFs from a ball clay facility. PCDDs and PCDFs include the 2,3,7,8-

congeners and their totals.

The primary objectives of this EPA-sponsored demonstration were:

• To determine if PCDDs and PCDFs are emitted from dryers at ball clay 

processing facilities

• To determine if PCDDs and PCDFs are emitted from heated mills at ball clay 

processing facilities

• To estimate potential PCDDs and PCDFs emissions from these sources.

3.2 Test Matrix

Testing was conducted during periods of production that were expected to be 

representative of the facility’s normal operations. Testing was conducted over three test 

runs at two sampling locations. Each test run was performed over a 4-hour period. 

The test matrix, which includes the number of samples or sample component sets 

collected during each run is presented in Table 3-1. The emission stack and process 

samples (feed and product) to be analyzed for PCDDs/PCDFs were transferred to Alta 

Analytical Perspectives in Wilmington, North Carolina, for subsequent analysis. 

3.3 Field Test Changes and Problems

The leak check at port change during Run 1 (mill baghouse test location) did not pass 

the < 0.02 cubic feet per minute criteria, and, consequently, the run was aborted; thus, the 

corresponding next run of the test sequence was identified as Run 1 Retest. A high 

pressure drop across the sampling train was observed during Runs 1 and 1 Retest, most 

likely due to restrictions in the XAD-2 trap. The high pressure drop was compensated for 

by using a smaller nozzle during subsequent test runs. The smaller nozzles were large 

enough to ensure an adequate sample volume collection.

The sampling time was reduced from 5.3 hours to 4 hours due to the limited work 

schedule at the facility. This decision was jointly made by the on-site EPA WAM, RTI, 

and MRI. Plant operations stopped promptly at 1:00 pm daily, leaving limited time to 

complete setup, make port changes, and complete a 4-hour run. A quick turnaround 
3-2

Table 3-1. Test Matrix: Summary of Emission and Process Sampling and Analytical Parameters and Methods 

Sampling location

Sampling or 

measurement time

Sampling method and

sample size Emission parameters Number of runs/samples Preparation method Analytical method

Mill baghouse 

emission stack

4 hours 40 CFR 60, Appendix A, Method 23, 

≥ 6.0 m3

PCDDs/PCDFs 3 Soxhlet extraction EPA Method 23

HRGC/HRMS

(SW-846, Method 8290A)

40 CFR 60, Appendix A, Method 2 Velocity, pressure, temp.,

volumetric flow rate

3 NA Pitot tube,

Thermocouple

40 CFR 60, Appendix A, Method 4, ≥

6.0 m3

Moisture 3 NA Gravimetric

40 CFR 60, Appendix A, Method 3A, 

≥ 2L/min sampling rate

CO2 and O2 Continuous during each run for 

a total of 3 runs

Particulate matter and 

moisture removal

NDIR for CO2

Micro-fuel cell for O2

Dryer baghouse 

emission stack

4 hours 40 CFR 60, Appendix A, Method 23, 

≥ 6.0 m3

PCDDs/PCDFs 3 Soxhlet extraction EPA Method 23

HRGC/HRMS

(SW-846, Method 8290A)

40 CFR 60, Appendix A, Method 2 Velocity, pressure, temp., 

volumetric flow rate

3 NA Pitot tube,

Thermocouple

40 CFR 60, Appendix A, Method 4, ≥

6.0 m3

Moisture 3 NA Gravimetric

40 CFR 60, Appendix A, Methods 3 

and 3B

CO2 and O2 One integrated bag during each 

run for a total of 3 runs

NA Orsat

Mill Feed sample Composite of grab 

samples collected 

every 30 min 

thereafter for 4 hr 

starting 30 min prior 

to start of run

ASTM D6051-01, 50-g (approx) grab 

samples 

collected/composited/mixed/

quartered until two 8-oz samples 

obtained

PCDDs/PCDFs 2 composite samples collected 

and split: one sample for 

analysis and one sample to be 

retained by the facility

Soxhlet extraction HRGC/HRMS 

(SW-846, Method 8290A)

Dryer Feed sample Composite of grab 

samples collected 

every 30 min 

thereafter for 4 hr 

starting 30 min prior 

to start of run

ASTM D6051-01, 50-g (approx) grab 

samples 

collected/composited/mixed/

quartered until two 8-oz samples 

obtained

PCDDs/PCDFs 2 composite samples collected 

and split: one sample for 

analysis and one sample to be 

retained by the facility

Soxhlet extraction HRGC/HRMS 

(SW-846, Method 8290A)

Mill product sample Composite of grab 

samples collected 

every 30 min 

thereafter for 4 hr 

starting 30 min prior 

to start of run

ASTM D6051-01, 50-g (approx) grab 

samples collected/composited then 

mixed/quartered until two 8-oz 

samples are obtained

PCDDs/PCDFs 2 composite samples collected 

and split: one sample for 

analysis and one sample to be 

retained by the facility

Soxhlet extraction HRGC/HRMS

(SW-846, Method 8290A)

Dryer product 

sample 

Composite of grab 

samples collected 

every 30 min 

thereafter for 4 hr 

starting 30 min prior 

to start of run

ASTM D6051-01, 50-g (approx) grab 

samples 

collected/composited/mixed/

quartered until two 8-oz samples 

obtained 

PCDDs/PCDFs 2 composite samples collected 

and split: one sample for 

analysis and one sample to be 

retained by the facility

Soxhlet extraction HRGC/HRMS

(SW-846, Method 8290A)
3-3

analysis of the first test run emission sample provided results that were above detection 

limits for dioxins, supporting the adequacy of using 4-hour test runs. With the shortened 

run time, only one traverse through a port was needed during all test runs.

Due to process obstructions at the mill, the appropriate length probe could not be 

used to reach the farthest two points on each traverse. Thus, with the concurrence of the 

on-site EPA WAM, the third to the last point on each traverse point was sampled three 

times for a total of 18 minutes.

Additionally, the process obstructions at the dryer created a need to use a heated 

sample transfer line on the first traverse (Port B), and then the second traverse (Port A) 

was sampled with the probe directly attached to the train hot box.

Due to concerns that ball clay dust generated during loading operations at the dryer 

location could cause high background contamination of samples, the mobile laboratory 

with CEMS was not moved to this area. Therefore, O2 and CO2 samples were collected 

using a gas bag for an integrated sample during the run. Analysis was performed by 

Orsat instead of CEMS.

3.4 Summary of Test Results

A summary of dioxin and furan testing performed is provided in Table 3-1. Since 

process data were collected by RTI, emissions as related to feed rates or other process 

parameters were calculated by RTI. Results are reported for the mill in Tables 3-2 

through 3-7 and for the dryer in Tables 3-8 through 3-13. Sample custody records are 

given in Appendix A. Field sampling and analytical data are included in Appendix B, 

and field equipment calibration records are given in Appendix C. Summary analytical 

reports are included in Appendix D.

For each location, dioxin and furan emission results are presented first by total 

amount found within a given homologue with the resultant emission factor, and next by 

the 2,3,7,8-substituted compounds, followed by the resultant emission factor. The feed 

and product sample results are reported on a dry basis. 

Any value below the detection limit is treated as a null value when presenting totals 

for dioxins and furans. The detection limit is determined as any peak with less than a 

21⁄2 signal-to-noise ratio and is represented in the report tables by parentheses (#). Values 

reported in parentheses with a less-than sign in front of them (< #) indicate that a peak 

was observed at greater than 21⁄2 times the signal, but that it was observed at less than 

one-tenth the lowest point on the calibration curve.
3-4

3.4.1 Mill Test Results

A summary of total PCDD/PCDF results at the mill baghouse outlet is provided in 

Table 3-2. PCDD/PCDF results for the mill baghouse outlet are provided in Tables 3-3

and 3-4. As noted in Table 3-3, the internal quantitation standard (IQS) recoveries (used 

for sample quantification) corresponding to the Run 1 Retest sample were greater than 

130 percent but less than 152 percent. The internal standard recovery values are 

presented and discussed in Section 5. 

Clay feed and product sample results for the mill process are provided in Tables 3-5

and 3-6. As noted in these tables, results for the 1,2,3,4,6,7,8-heptachloro-dioxins 

(HpCDD) and octochloro-dioxins (OCDDs) exceeded the upper limit of the calibration 

curve. Alta Analytical Perspectives has examined the data and found that these results 

are within the linear range of the calibration curve. Note that these results already reflect 

a ten-fold dilution for the OCDD samples.

Data obtained from the emission sampling trains at the mill are summarized in 

Table 3-7. Each sampling train provided data on gas velocity, stack temperature, stack 

pressure, and volumetric flow rates. The O2 and CO2 results reported were obtained by 

CEMS for the first three runs. Stack flow rates appear slightly elevated at the mill for 

Run 3. 

3.4.2 Dryer Test Results

A summary of PCDD/PCDF results at the dryer is provided in Table 3-8. 

PCDD/PCDF results for dryer stack emissions are provided in Tables 3-9and 3-10.

Clay feed and product sample results for the dryer process are provided in 

Tables 3-11 and 3-12. As noted in these tables, results for HpCDD and OCDD exceeded 

the upper limit of the calibration curve. Alta Analytical Perspectives has examined the 

data and found that these results are within the linear range of the curve with the 

exception of Run 4 feed and product, as well as Run 5 feed. For these three samples, the 

reported concentrations for OCDD may be underestimated by as much as 50 percent. 

Note that these results already reflect a ten-fold dilution for the OCDD sample results. 

Data obtained from the emission sampling trains at the dryer are summarized in 

Table 3-13.
3-5

Table 3-2. Summary of Total Dioxin/Furan Results for Mill Samples

Run 1

Retest Run 2 Run 3 Average

Air Emissions

Total PCDDs and PCDFs

Total PCDDs (pg/dscm) 117 167 119 135

Total PCDFs (pg/dscm) 16.3 77.6 70.1 54.7

Total PCDDs and PCDFs (pg/dscm) 134 245 189 189

Emission Rates/Factors

Dry Clay Process Rate (Mg/hr) b b b b

Material Analyses

Clay Feeda

Total PCDDs and PCDFs (pg/g) b b b b

Clay Producta

Total PCDDs and PCDFs (pg/g) b b b b

a Clay feed and product concentrations are calculated on a dry basis. b CBI data removed: See confidential version of document.
3-6

Table 3-3. Dioxin/Furan Homolog Results for Mill Stack Samples

Analyte Run 1 Retestb Run 2 Run 3 Average

Dioxins (pg/dscm)

TCDD 27.1 43.9 30.0

PeCDD 16.6 30.7 15.7

HxCDD 10.7 26.6 8.4

HpCDD 12.1 17.8 15.4

OCDD 50.8 48.3 49.6

Total PCDDs (pg/dscm)a 117 167 119 135

Furans (pg/dscm)

TCDF 4.86 24.7 17.6

PeCDF 2.98 20.5 17.5

HxCDF 3.55 17.7 17.2

HpCDF 27.4 11.5 12.4

OCDF 2.15 3.30 5.39

Total PCDFs (pg/dscm)a 16.3 77.6 70.1 54.7

Total PCDDs and PCDFs (pg/dscm) 134 245 189 189

a Totals do not include values below detection limit; they are treated as zeros.

b Recoveries for corresponding Internal Quantitation Standards were all above 130 percent, but less 

than 152 percent. See Section 5.2 for further explanation.
3-7

Table 3-4. Dioxin/Furan Homolog Emission Factors for Mill Stack Samples

Homolog

Emission Rate, pg/hr Process Rate, Mg/hrb Emission Factor, pg/Mgb

Run 1 Re Run 2 Run 3 Run 1 RE Run 2 Run 3 Run 1 Re Run 2 Run 3 Average

Total TCDD 8.09E+05 1.32E+06 9.89E+05

Total PeCDD 4.96E+05 9.18E+05 5.18E+05

Total HxCDD 3.19E+05 7.97E+05 2.79E+05

Total HpCDD 3.61E+05 5.32E+05 5.09E+05

Total OCDD 1.52E+06 1.45E+06 1.64E+06

Total CDD 3.50E+06 5.01E+06 3.93E+06

Total TCDF 1.45E+05 7.40E+05 5.82E+05

Total PeCDF 8.89E+04 6.13E+05 5.78E+05

Total HxCDF 1.06E+05 5.29E+05 5.67E+05

Total HpCDF 8.19E+04 3.43E+05 4.08E+05

Total OCDF 6.43E+04 9.89E+04 1.78E+05

Total CDF 4.86E+05 2.32E+06 2.31E+06

Total CDD/CDF 3.99E+06 7.33E+06 6.24E+06

2,3,7,8 TCDD 5.83E+04 7.21E+04 6.08E+04

1,2,3,7,8 PeCDD 2.89E+04 4.62E+04 (<4.75E+04)

1,2,3,4,7,8 HxCDD (1.67E+04) (2.67E+04) (3.65E+04)

1,2,3,6,7,8 HxCDD (<2.51E+04) (<4.41E+04) (<4.75E+04)

1,2,3,7,8,9 HxCDD 2.73E+04 5.38E+04 (<4.75E+04)

1,2,3,4,6,7,8 HpCDD 1.62E+05 2.47E+05 2.27E+05

Total OCDD 1.52E+06 1.45E+06 1.64E+06

2,3,7,8 TCDF 1.35E+04 3.72E+04 8.66E+04

1,2,3,7,8 PeCDF (4.71E+04) {5.31E+04} (<4.75E+04)

2,3,4,7,8 PeCDF (<2.51E+04) 7.22E+04 9.79E+04

1,2,3,4,7,8 HxCDF (<2.51E+04) 8.75E+04 9.11E+04

1,2,3,6,7,8 HxCDF (<2.51E+04) 7.85E+04 7.62E+04

2,3,4,6,7,8 HxCDF (<2.51E+04) {7.90E+04} 7.78E+04

1,2,3,7,8,9 HxCDF (5.98E+03) (5.53E+03) (6.97E+03)

1,2,3,4,6,7,8 HpCDF 5.33E+04 2.35E+05 2.37E+05

1,2,3,6,7,8,9 HpCDF (7.94E+03) (1.12E+04) 4.87E+04

Total OCDF 6.43E+04 9.88E+04 1.78E+05 a

 Non-detect values, designated by parentheses ( ), listed are sample- and analyte-specific and are calculated as "0" in the table "subtotals and totals" results. Estimated 

Maximum Possible Concentration (EMPC) peak values, designated by brackets { }, listed are sample- and analyte-specific, and using the Table isomer value shown, are 

included in the "subtotals" results.

b CBI data removed: See confidential version of document.
3-8

Table 3-5. Dioxin/Furan Mill Clay Feed Homolog Resultsa

Analyte

Run 1 

Retest Run 2 Run 3 Average

Clay Feed SB Blend SB Blend REX

Dioxins (pg/g dry wt.)

TCDD

PeCDD

HxCDD

HpCDD

OCDD

Total PCDDsb

Furans (pg/g dry wt.)

TCDF

PeCDF

HxCDF

HpCDF

OCDF

Total PCDFsb

Total PCDDs and PCDFs (pg/g, ng/kg, dry wt.)

a CBI data removed: See confidential version of document.

.
3-9

Table 3-6. Dioxin/Furan Mill Clay Product Homolog Resultsa

Analyte

Run 1 

Retest Run 2 Run 3 Average

Clay Product SB Blend SB Blend REX

Dioxins (pg/g dry wt.)

TCDD

PeCDD

HxCDD

HpCDD

OCDD

Total PCDDsb

Furans (pg/g dry wt.)

TCDF

PeCDF

HxCDF

HpCDF

OCDF

Total PCDFsb

Total PCDDs and PCDFs (pg/g, ng/kg, dry wt.)

a CBI data removed: See confidential version of document.
3-10

Table 3-7. Mill Sampling and Stack Parameters

Average Stack Stack

Sampling Sample Gas Moisture Stack Static Stack Flow 

Time Volume CEMS Analysis a Content Temp. Pressure Velocity Rate

(min) (acm) (dscm) % CO2 % O2 (%) ( °C) (mm Hg) % Isokinetic (m/min) (dscm/hr)

Mill 

Run 1Retest 240 6.271 5.942 0.69 19.8 b 62 -0.39 104 990 29,860

Run 2 240 3.556 3.392 0.69 19.7 b 63 -0.39 105 987 29,940

Run 3 240 3.666 3.471 0.60 19.8 b 61 -0.39 97.5 1,077 33,000

Average = 0.66 19.8 b 62 NA 1,020 30,930

a

 Percent CO2 and O2 for Runs 1 Retest through 3 were

analyzed by CEMS.

b CBI data removed: See confidential version of document.
3-11

Table 3-8. Summary of Total Dioxin/Furan Results for Dryer Samples

Run 4 Run 5 Run 6 Average

Air Emissions

Total PCDDs/PCDFs

Total PCDDs (pg/dscm) 255 353 370 326

Total PCDFs (pg/dscm) 48.4 25.0 5.97 26.5 

Total PCDDs and PCDFs (pg/dscm) 304 378 376 353 

Emission Rates/Factors

Dry Clay Process Rate (Mg/hr) b b b b

Material Analyses

Clay Feeda

Total PCDDs and PCDFs (pg/g) b b b b

Total 2,3,7,8-TCDD TEQ (pg/g) b b b b

Clay Producta

Total PCDDs and PCDFs (pg/g) b b b b

Total 2,3,7,8-TCDD TEQ (pg/g) b b b b a

 Clay feed and product concentrations are calculated on a dry basis. b

 CBI data removed: See confidential version of document.
3-12

Table 3-9. Dioxin/Furan Homolog Results for Dryer Stack Samples

Analyte Run 4 Run 5 Run 6 Average

Dioxins (pg/dscm)

TCDD 21.0 13.0 18.0

PeCDD 17.1 20.6 19.4

HxCDD 23.7 28.3 24.0

HpCDD 28.0 37.2 32.8

OCDD 165.7 253.5 276.4

Total PCDDs (pg/dscm)a 255 353 370 326

Furans (pg/dscm)

TCDF 11.36 9.27 (0.479)

PeCDF 11.83 7.23 (0.997)

HxCDF 12.38 3.99 4.42

HpCDF 9.11 2.68 1.55

OCDF 3.78 1.88 1.58

Total PCDFs (pg/dscm)a 48.4 25.0 7.55 27.0

Total PCDDs and PCDFs (pg/dscm) 304 378 378 353

a

 Non-detect values, designated by parentheses (), listed are sample- and analyte-specific and are calculated as "0" in the table "subtotals 

and totals" results. Estimated Maximum Possible Concentration peak values, designated by brackets {}, listed are sample- and analytespecific, and using the Table isomer value shown, are included in the "subtotals" results.
3-13

Table 3-10. Dioxin/Furan Homolog Emission Factors for Dryer Stack Samples

Homolog

Emission Rate, pg/hr Process Rate, Mg/hrb Emission Factor, pg/Mgb

Run 4 Run 5 Run 6 Run 4 Run 5 Run 6 Run 4 Run 5 Run 6 Average

Total TCDD 4.40E+05 2.68E+05 3.64E+05

Total PeCDD 3.57E+05 4.26E+05 3.91E+05

Total HxCDD 4.95E+05 5.83E+05 4.84E+05

Total HpCDD 5.85E+05 7.68E+05 6.62E+05

Total OCDD 3.46E+06 5.23E+06 5.59E+06

Total CDD 5.34E+06 7.28E+06 7.49E+06

Total TCDF 2.37E+05 1.91E+05 (9.68E+03)

Total PeCDF 2.47E+05 1.49E+05 (2.01E+04)

Total HxCDF 2.59E+05 8.24E+04 8.94E+04

Total HpCDF 1.90E+05 5.53E+04 3.13E+04

Total OCDF 7.90E+04 3.88E+04 (<4.14E+04)

Total CDF 1.01E+06 5.17E+05 1.21E+05

Total CDD/CDF 6.35E+06 7.80E+06 7.61E+06

2,3,7,8 TCDD 2.47E+04 {1.87E+04} 2.28E+04

1,2,3,7,8 PeCDD 2.60E+04 2.91E+04 3.07E+04

1,2,3,4,7,8 HxCDD (1.49E+04) (1.64E+04) (1.16E+04)

1,2,3,6,7,8 HxCDD (<2.13E+04) 3.81E+04 2.42E+04

1,2,3,7,8,9 HxCDD 5.64E+04 {6.61E+04} 5.09E+04

1,2,3,4,6,7,8 HpCDD 2.51E+05 3.31E+05 2.67E+05

Total OCDD 3.46E+06 5.23E+06 5.59E+06

2,3,7,8 TCDF {1.66E+04} 2.27E+04 (9.68E+04)

1,2,3,7,8 PeCDF 2.39E+04 (1.91E+04) (2.10E+04)

2,3,4,7,8 PeCDF 3.78E+04 3.00E+04 (1.94E+04)

1,2,3,4,7,8 HxCDF 4.04E+04 {2.71E+04} (<2.07E+04)

1,2,3,6,7,8 HxCDF 3.59E+04 (<2.15E+04) (<2.07E+04)

2,3,4,6,7,8 HxCDF 3.58E+04 {2.32E+04} (<2.07E+04)

1,2,3,7,8,9 HxCDF (<2.13E+04) (4.98E+04) (6.17E+04)

1,2,3,4,6,7,8 HpCDF 1.04E+05 5.54E+04 3.13E+04

1,2,3,6,7,8,9 HpCDF 2.52E+04 (1.19E+04) (5.63E+04)

Total OCDF 7.90E+04 (<4.29E+04) (4.14E+04) a

 Non-detect values, designated by parentheses ( ), listed are sample- and analyte-specific and are calculated as "0" in the table "subtotals and totals" results. Estimated Maximum Possible Concentration peak values, 

designated by brackets { }, listed are sample- and analyte-specific, and using the Table isomer value shown, are included in the "subtotals" results. b

 CBI data removed: See confidential version of document.
3-14

Table 3-11. Dioxin/Furan Dryer Clay Feed Homolog Resultsa

Analyte Run 4 Run 5 Run 6 Average

Product Type SB Blend SB Blend SB Blend

Dioxins (pg/g dry wt.)

TCDD

PeCDD

HxCDD

HpCDD

OCDD

Total PCDDsc

Furans (pg/g dry wt.)

TCDF

PeCDF

HxCDF

HpCDF

OCDF

Total PCDFsc

Total PCDDs and PCDFs (pg/g dry wt.)

a CBI data removed: See confidential version of document.

.
3-15

Table 3-12. Dioxin/Furan Dryer Clay Product Homolog Resultsa

Analyte Run 4 Run 5 Run 6 Average

Product Type SB Blend SB Blend SB Blend

Dioxins (pg/g dry wt.)

TCDD

PeCDD

HxCDD

HpCDD

OCDD

Total PCDDsc

Furans (pg/g dry wt.)

TCDF

PeCDF

HxCDF

HpCDF

OCDF

Total PCDFsc

Total PCDDs and PCDFs (pg/g dry wt.)

a CBI data removed: See confidential version of document.
3-16

Table 3-13. Dryer Sampling and Stack Parameters

Average Stack Stack

Sampling Sample Gas Moisture Stack Static Stack Flow 

Time Volume Orsat Analysis a Content Temp. Pressure % Iso- Velocity Rate

(min) (acm) (dscm) % CO2 % O2 (%) (°C) (mm Hg) kinetic (m/min) (dscm/hr)

Dryer

Run 4 240 5.229 4.896 0.3 19.7 b 54.4 -0.11 96.5 1,499 20,900

Run 5 240 5.073 4.813 0.2 19.7 b 55.3 -0.11 96.0 1,476 20,650

Run 6 240 5.139 4.885 0.2 19.8 b 52.1 -0.11 99.5 1,427 20,210

Average = 0.2 19.7 b 54 NA 1,470 20,590

a

 Percent CO2 and O2 for Runs 4 through 6 were 

analyzed by Orsat.

b CBI data removed: See confidential version of 

document.
4-1

Section 4.

Procedures for Sampling, Analysis, and Process 

Data Collection

This section describes the sampling, analysis, and process data collection procedures 

that were used for this test project. The published methods and Standard Operating 

Procedures (SOPs) that were used are cited. Details providing clarification and any 

modifications to or deviations from the published methods are presented in this section. 

Otherwise, the cited methods were followed.

4.1 Sampling Methods

4.1.1 Emissions Sampling Procedures

The emission samples collected required the use of the sampling system(s) as shown 

at each test location:

(1) Mill Baghouse

• EPA Method 23 isokinetic sampling train for PCDDs and PCDFs.

• EPA Method 3A for CO2 and O2.

(2) Dryer Baghouse

• EPA Method 23 isokinetic sampling train for PCDDs and PCDFs.

• EPA Method 3 for CO2 and O2.

The following methods were employed in the use and operation of these sampling 

trains and systems.

4.1.1.1 Sample and Velocity Traverses

Method 1 in Appendix A of 40 CFR 60 (basis for MRI SOP MRI-8401) was used to

establish traverse (sampling) points at the two test locations for the traversing sampling 

trains. A check for absence of cyclonic flow was conducted at each location prior to the 

start of sampling. No cyclonic or nonparallel flow conditions were found at either 

location.

4.1.1.2 Determination of Gas Velocity and Volumetric Flow Rates

Method 2 in Appendix A of 40 CFR 60 (basis for MRI SOP MRI-8402) was used to 

measure gas velocities and volumetric flow rates with Type S pitot tubes that are 
4-2

components of the traversing sampling trains. Pitot tubes meeting the dimensional 

specifications in the method were used. The pitot tube coefficient was adjusted for 

blockage in the gas stream caused by the probe assembly used during sampling in the 

duct having internal an diameter of 24 inches. An average adjusted coefficient for each 

such pitot tube was calculated in a spreadsheet using procedures cited in Method 2. The 

static pressure was determined within the gas stream as indicated in Method 2. 

An aneroid barometer calibrated against a mercury barometer was used to measure 

atmospheric pressure at the sampling locations.

4.1.1.3 Determination of Moisture Content

Method 4 in Appendix A of 40 CFR 60 incorporated as part of Method 23 was used 

to determine the moisture (water vapor) content of the gas stream. Moisture collected 

during sampling was determined gravimetrically from the difference between the initial 

and final weights of all of the impingers in a train, including the resin cartridge.

4.1.1.4 Sampling of PCDDs and PCDFs

Method 23 in Appendix A of 40 CFR 60 (basis for MRI SOP MRI-8404) was used 

to collect samples to be analyzed for dioxins and furans. A schematic of a sampling train 

is presented in Figure 4-1. The Method 23 sampling train is based upon the apparatus 

design normally employed for sampling conducted under USEPA Method 5 modified to 

include a special coiled condenser and sorbent module assembly for collection for 

PCDDs/PCDFs. The types and content of each impinger was as follows:

1. 2-L Modified Greenburg-Smith with a shortened stem (knockout), empty.

2. 500 mL Modified Greenburg-Smith containing 100 mL of Milli-Q grade water.

3. 500 mL Greenburg-Smith containing 100 mL of Milli-Q grade water.

4. 500 mL Modified Greenburg-Smith, empty.

5. 500 mL Modified Greenburg-Smith containing 200 g silica SiO2.

6. 500 mL Modified Greenburg-Smith containing 200 g silica SiO2.

Clarifications of and modifications to the method are included in the following 

discussion.

Nickel-plated stainless steel nozzles and quartz glass probe liners were used in the 

probes. The internal surface of the compression fittings used for connecting nozzles to 

probe liners are permanently coated with abrasion-resistant Teflon to prevent sample 

gas contact with the stainless steel, and the connections were positioned within each 

probe. Due to the very limited space at the mill baghouse, a heated sample transfer line 

was used between the probe and sampling train.
4-3

Figure 4-1. Method 23 Sampling Train for PCDDs and PCDFs
4-4

Since no significant quantities of particulate matter were observed during the first sampling 

run, no cyclone/flask assembly was used in front of the filter holder thereafter. During the first 

sampling run a significant pressure drop across the sampling train was observed and sampling 

was stopped so that the filter could be recovered and replaced. Leak checks were conducted 

prior to replacing filters and before continuing the sampling. The large pressure drop across the 

sampling train was compensated for in subsequent runs by using a smaller nozzle diameter. All 

filters were submitted to the analytical laboratory for analysis as described below in 

Section 4.2.1. 

Filter supports in the filter holders were Teflon frits. Quartz fiber filters having the same 

specifications described in the method were used. Each cartridge (sorbent trap) was loaded with 

approximately 40 grams of XAD-2 resin.

Two silica gel impingers were used in each train. In addition, the first 500-mL impinger in 

the sampling train was replaced with a 2-L impinger to minimize any need to swap impinger 

components during test runs.

Sample recovery procedures used were those specified in the method with one exception: 

excluding methylene chloride rinses for train components as preapproved by EPA prior to the 

field test. Acetone and toluene were used for rinsing train components. The acetone and toluene 

solvents used during the test were each from one lot. The acetone and toluene rinses were 

collected separately in the field, but in the lab were combined for extraction and analysis of 

dioxins and furans. The sample recovery scheme used for the trains is presented in Figure 4-2. 

The condensate collected in the impingers was weighed and discarded. 

Blanks were collected in the field during the test. A Method 23 sampling train (using 

previously recovered glassware) was charged and leak checked at one sampling location and 

then returned for sample recovery. This sample (blank train) was submitted for PCDDs/PCDFs 

analysis along with the field samples. In addition, a set of reagent blanks consisting of one filter, 

one XAD, 400 mL acetone, 200 mL toluene, and 200 mL Milli-Q water was collected and 

archived for possible future evaluation. The reagent blank samples will remain in MRI storage 

until approval of the final test report and will not be sent to the laboratory for analysis unless 

requested by the WAM.

A summary of isokinetic results from each run was provided to the on-site WAM for review 

before the next run was initiated. 

All post-test calibrations were performed at the MRI facility.
4-5

Figure 4-2. Sample Recovery Scheme
4-6

4.1.1.5 Sampling and Analysis for CO2 and O2

Because of concerns with background contamination at the mill test location, 

Method 3 in Appendix A of 40 CFR 60 (basis for MRI SOP MRI-8406) was used to 

determine CO2 and O2 at that location. Multi-point, integrated gas bag samples were 

collected simultaneously with the traversing/isokinetic sampling for analysis of O2 and 

CO2 with subsequent determination of dry gas molecular weight. The integrated gas 

sampling apparatus used to collect the samples was a component of each traversing 

sampling train. Integrated gas samples were extracted at a constant rate from the exhaust 

of a traversing sampling train just upstream from the outlet of the dry gas meter outlet 

orifice.

The train was purged for one minute with stack gas then integrated gas sampling was 

started. Sampling was conducted at a constant rate throughout the run while the 

traversing/isokinetic sampling was in progress. Each integrated gas sampling apparatus 

was leak checked before and after each test run. The tubing at the connection to the dry 

gas meter outlet orifice was closed off, the integrated sampling apparatus pump was 

turned on, and the integrated sampling apparatus flow control valve was fully opened. 

No flow at the tubing outlet (i.e., where the gas sample bag would be connected during 

sampling), was used to indicate the apparatus was leak-free. Gas samples were analyzed 

with an Orsat analyzer.

At the dryer, a Continuous Emission Monitoring System (CEMS) was set up and 

operated according to Method 3A in Appendix A of 40 CFR 60 to sample and analyze for 

CO2 and O2. Clarifications of and modifications to the methods are included in the 

following discussion.

All calibration gases were certified according to EPA Protocol 1. Gas concentrations 

that were used are shown in Table 4-1.

Table 4-1. Calibration Gases

Emission 

parameter Zero-level gas Mid-level gas High-level gas

CO2 Zero in nitrogen 10% v/v 18% v/v

O2 Zero gas 12% v/v 21% v/v

A schematic of the sampling and analytical system used is presented in Figure 4-3. 

A brief description of each component follows:

Probe—3/8-inch outside diameter (OD) stainless steel (SS) sample line housed in a 

1-inch SS heated sheath of sufficient length to reach the center of the stack. The stack 

end of the probe was fitted with a sintered SS 10-micron prefilter which was back-flushed 

after each run.

Sample gas conditioner (for moisture removal)—Chiller. The sample gas 

conditioner attaches to the back of the probe. It has a probe bracket, which is attached to 
4-7

Figure 4-3. Instrumental Measurement System for CO2 and O2

an ice bath. At this point the probe liner is connected to a 3/8-inch Teflon tube. The 

Teflon tube is coiled within the ice bath. As the hot stack gas is pulled through the 

chilled section of tubing in the ice bath the moisture in the gas is turned to condensate, 

which is collected in a moisture trap at the bottom of the coil. The conditioned gas 

sample is pulled out the top of the moisture trap into the sample line. The condensate is 

drained out the bottom of the moisture trap by a peristaltic pump. 

Sample line—Consists of a 3/8-inch OD Teflon tube, which is attached to the exit of 

the sample gas conditioner and to the inlet of the sample gas distribution system at the 

other end. In the same nylon sheath is a 1/4-inch OD Teflon tube, or Bias line, which is 

used to deliver calibration gases to a tee located at the back of the probe and in front of 

the sample gas conditioner. Various length sections from 25 to 100 feet are available and 

can be jointed together to reach sampling locations.
4-8

Sample gas and calibration gas distribution manifold—Located in the sample 

trailer. It is capable of pulling 1 to 10 L/minute (dry gas), although normal gas delivery 

to the CEMS is typically 2 L/minute, and can distribute the sample gas flow to five 

separate analyzers simultaneously. It can also deliver EPA Protocol 1 gases directly to 

the analyzers or to the back of the probe for a system bias check. The gas distribution 

manifold is located in the sampling trailer downstream of the sample gas conditioner and 

upstream of the selected analyzer(s). 

Data acquisition system—Located in the sample trailer. MRI uses LABTECH 

Notebook Pro for Windows 95, Version 10.12, which is an integrated system that 

provides data acquisition, monitoring, and control. The system is designed such that each 

data channel can be configured separately with different characteristics. The normal 

mode of operation is continuous data collection written to disk in the background, while 

performing foreground tasks and displaying data in real time (1-minute averages). This 

system is run on a Pentium laptop computer with a 1-G hard drive. MRI also uses an 

identical computer (which can serve as a backup) for data transfer and processing. With 

the use of a spreadsheet designed and developed by MRI, calibration results are 

instantaneous and preliminary test results are available while on-site.

O2 analyzer—Located in the sample trailer. Servomex, Model 01440CISTD uses 

the principle of Magneto-pneumatic technique to measure the concentration of O2 (%) in 

the gas stream. It has measurement ranges of 0% to 25% and 0% to 100%.

CO2 analyzer—Located in the sample trailer. Servomex, Model 01440CISTD uses 

a single beam, dual wavelength IR technique to measure the concentration of CO2 (%) in 

the gas stream. It has measurement ranges of 0% to 20% and 0% to 25%.

4.1.2 Process Sampling Procedures

During each of the test runs, raw feed and product samples were collected for 

PCDDs/PCDFs analysis. Sampling was conducted as during the pretest site survey. 

Individual, representative “grab” samples, were collected using EPA-accepted methods 

(ASTM D6051-96) whereby several equal, grab samples of approximately 50 g each 

were collected over a period of time (if possible, every 30 minutes, beginning at least 

30 minutes prior to the start of each test run and ending 30 minutes after the completion 

of each test run) and composited/mixed/quartered until the ideal sample size became 

available. An aluminum scoop wrapped in disposable aluminum foil and a large mixing 

container was used for sample collection and mixing. 

Sufficient material was taken from the composited process sample to fill an 8-ounce 

glass container. A second sample was collected from this composite with one each of 

these samples sent to the lab for analysis, and the second sample retained by the plant. 

Any remaining material was returned to the plant. Special precleaned glass containers 

provided by the laboratory were used to collect, store and ship the field samples. The 

sealed field samples were wrapped with aluminum foil and placed in plastic bags along 

with a sample traceability form. The samples were then placed in their own insulated 
4-9

shipping containers (separate from the emission samples) with ice and shipped by Federal 

Express overnight at the conclusion of the entire sample collection period.

4.2 Analytical Procedures

The analytical methodology and procedures used by Alta Analytical Perspectives for 

this project are standardized methods and EPA-approved procedures. Any modifications 

to the analytical methods used on this project are described below. 

4.2.1 EPA Method 23 Samples

Before the sampling event, the sampling modules were prepared by the laboratory 

using precleaned XAD-2 resin and spiked with a known amount of five labeled PCDD/F

surrogate standards. Upon return to the laboratory, the sample components recovered 

from the Method 23 trains (i.e., XAD-2 resin, rinses, and filter) were combined and 

extracted in the laboratory using toluene Soxhlet Dean-Stark extraction. The procedure 

for extraction involved placing the XAD-2 resin, concentrated rinses, and filter samples 

in the Soxhlet apparatus, spiking with 13C12 PCDD/PCDF internal standards, and 

extracting for a minimum of 16 hours.

The extract was split, with one-half being subjected to the sample fractionation 

procedures and analyzed for dioxins and furans, and one-half being archived. The final 

extract was prepared with the addition of recovery standards and provided for analysis by 

HRGC/HRMS using a final volume of 20 μL.

Extracts were analyzed for dioxins and furans based on the procedures specified in 

Method 8290A, “Polychlorinated Dibenzodioxins (PCDDs) and Polychlorinated 

Dibenzofurans (PCDFs) by High-Resolution Gas Chromatography/High-Resolution Mass 

Spectrometry (HRGC/HRMS),” found in “Test Methods for Evaluating Solid Waste, 

Physical/Chemical (SW-846).” This analytical procedure included the separation of 

isomers of dioxin and furan using high-resolution gas chromatography followed by highresolution mass spectrometry. Initial and continuing calibration criteria adhered to 

Method 23 criteria. The target analyte amounts and surrogate and internal standard 

recoveries were quantitated according to Method 23. A schematic of the analytical 

process is presented in Figure 4-4. 

Note that a more robust Batch Control Spike (BCS3) has been incorporated into the 

method in place of the Laboratory Control Spike. Information on BCS3 matrix spiking is 

provided in Appendix E. Specifically, Batch Control Spikes (BCS3): 

• Were prepared in stages at the same time as the batch of field samples; i.e., at 

each phase involving the addition to the samples of the extraction, cleanup, and 

injection standards. For air matrices, the Batch CS3 was initiated at the same 

point as when the XAD cartridges were prepared for sampling.
4-10

Figure 4-4. Schematic of EPA Method 23 and SW846 8290 Emission Samples Analysis Path
4-11

Figure 4-4. Schematic of EPA Method 23 and SW846 8290 Emission Samples Analysis Path (Continued)
4-12

• Consisted of one Batch CS3 per batch of 20 samples or less—regardless of the 

matrix type—processed through the same spiking scheme with the same spiking 

solutions, same analyst, same delivery system, and at the same time as the field 

samples. The laboratory ensured that sufficient Batch CS3s was prepared to 

provide front- and back-end calibration verifications for all the samples as well 

as re-injections, when necessary. 

• Were then analyzed at the beginning and at the end of each 12-hour analytical 

sequence during which samples are analyzed. 

In order to use the front- and back-end Batch CS3s averaged RRFs to process the 

samples, the individual front- and back-end RRFs needed to meet a number of 

requirements (independent verification, RPD, and PD or bias). This information is 

provided in Appendix F, BCS3 Performance Criteria. Details on performance criteria 

associated with the BCS3 are also available from the laboratory SOPs.

4.2.2 Process Samples

EPA Method 8290A was used to analyze the process samples. Method 8290A is a 

high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) 

analytical procedure capable of measuring low parts per trillion levels (picograms per g). 

Each process sample was thoroughly mixed and a 10-gram sample was removed, 

weighed, extracted, and analyzed for 17 PCDD/F congeners. The extracts were 

reanalyzed following a ten-fold dilution due to OCDD detector saturation. Reported 

concentrations have been adjusted. Even though HpCDD and OCDD results were above 

the highest point on the calibration curve, only OCDD was reanalyzed because review of 

HpCDD data suggested results were within the linear range of the curve. A separate 

aliquot is mixed, oven-dried at 125°C for 16 hours, and percent moisture is determined to 

calculate an equivalent 10-gram sample. A schematic of the analytical process is 

presented in Figure 4-5.

4.3 Process Data

In order to ensure that the processes were operating in a manner that was 

representative of normal operating conditions during testing, close contact was 

maintained with the facility operators and specific process data were collected. As the 

data were collected, process and control device operating parameters were monitored to 

ensure that they were within the normal ranges, as specified by the facility. In addition, 

at the beginning of each test day, a schedule was obtained of any planned process 

changes, product changeovers, or other process-related information that could impact the 

test program. Any abnormal process conditions were discussed with the facility 

operators to determine if testing should be suspended.
4-13

Figure 4-5. Schematic of Process Samples Analysis Path
4-14
5-1

Section 5.

QA/QC Activities

This section summarizes the QA/QC activities associated with this project. The 

QA/QC requirements and emission measurement and data quality objectives for this 

project were presented in the Quality Assurance Project Plan (QAPP). Major 

components of QC procedures included: (1) sampling equipment calibrations, 

(2) procedural elements of the methods such as leak checks, proper traversing, placement 

of sampling probes, verification of the integrity of metering systems prior to the start of 

sampling, etc., and (3) the use of QC samples in the analytical approach such as reagent 

blanks, run-used train blank, method blanks, batch control spikes, duplicate injections of 

the BCS3, and internal standard and surrogate standard spiking. Data quality objectives, 

as specified in the project QA plan, are evaluated in Section 5.1. Internal standard and 

surrogate standard recoveries are presented in Section 5.2. Based on the QA activities, a 

discussion of data quality is presented in Section 5.3.

5.1 QA/QC Objectives Summary

Data quality criteria along with an evaluation results based on the QC criteria are 

provided in Tables 5-4 through 5-6. 

Results for blank samples associated with this test are summarized in Table 5-4. All 

blank sample results were well below the lowest point on the calibration curve.

Clay feed and product sample results for the 1,2,3,4,6,7,8-Hepta-Dioxins and 

OCDDs exceeded the upper limit of the calibration curve. Alta Analytical Perspectives 

has examined the data and found that these results are within the range of the curve for 

the clay samples except for the Run 5 product, and Run 6 feed and product samples, 

which may be underestimated by as much as 50 percent. Note that these results already 

reflect a ten-fold dilution for the OCDD samples.

For one emission sampling train sample, the recoveries for the internal standards 

exceeded the Method 23 specification of 130 percent. This is addressed in more detail in 

Section 5.2 below.

All sample transfers were documented on Chain-of-Custody sheets. Samples were 

maintained in the field at temperatures between 1.0 and 7.5°C; after shipping they arrived 

at the lab at temperatures between 8 and 23°C. All samples were analyzed within the 

specified holding times (sampled < 28 days after XAD preparation, extracted < 30 days 

after sample collection, and analyzed < 45 days after extraction).
5-2

5.2 Internal Standard and Surrogate Standard Recoveries

Internal standard and surrogate standard recovery results are summarized in 

Tables 5-4 and 5-5. Additional standard recovery data are included in Appendix D of this 

report. 

As noted in Table 5-4, the internal standard recoveries corresponding to the Run 1 

Retest sample were above the 130 percent requirement of Method 23, but beneath 

152 percent. Because the internal standard recoveries were all consistently high for Run 

1 Retest, and the surrogate standard recoveries for the same run were all consistently 

lower (70 to 76 percent) than those for the other two runs at the mill (97 to 106 percent), 

it is reasonable to conclude that the amount of the internal standard solution added to the 

Run 1 Retest sample slightly exceeded that specified. This, in turn, could have resulted 

in a low bias in the sample results. Since the surrogate standard recoveries for Run 1 are 

within the method objectives of 70 to 130 percent, the sample data are reasonable to use. 

Results could be corrected for the apparent low bias, but MRI has selected not to do this 

since the collection efficiency results indicated by the surrogate standard recoveries are 

within the QA limits, and the accompanying method blank, sampling standard, and BCS3

results are all within the QA objectives.

Internal standard recoveries corresponding to Run 4 Product and Run 5 Feed were 

also greater than 130 percent for 13C-OCDD. No attributable cause is discernable

considering the recoveries for the remaining labeled congeners were within limits. The 

fact that the accompanying method blank, sampling standard, and BCS3 results are all 

within the QA objectives suggests that the results are acceptable.

5.3 Discussion

As part of the QA review process to ensure accurate reporting the report and 

supporting records were audited. One run was traced from the field measurement records

to original analytical data through the derived test results. Based on the data review, the 

test results were found to be correctly reported, traceable, and met the quality assurance 

objectives of the test program. Any exceptions from data quality criteria are discussed in 

the report and associated results have been flagged in the data tables.
5-3

Table 5-1. Calibration QC Criteria for Sampling Equipment

Parameter Calibration technique

Reference 

standard Acceptance limit Frequency

Criteria 

met? (Y/N)

Sampling 

nozzle

Measure 3 diameters 

to nearest 0.001 in and 

average 

measurements

Micrometer Difference between high 

and low measurements, 

≤ 0.004 in

Prior to 

sampling

Yes

Dry gas 

metering 

system

volume

Compare with 

calibrated critical 

orifices, 40 CFR 60, 

Appendix A, Method 5, 

Section 16.2

Calibrated 

critical orifice

Difference between 

individual calibration factor 

values and average value, 

≤ ±0.02

Prior to test 

series, and in 

the field after 

test series

Yes

Use field test data to 

compute a calibration 

check value, EPA 

Method ALT-009

NA Difference between 

calibration check value 

must be ≤ ±5% of initial 

calibration factor

After test series Yes

Dry gas meter 

thermocouples

Compare to mercuryin-glass thermometerASTM 

thermometer

≤ ±5.4°F difference from 

reference

Before and after 

test series

Yes

Stack Gas 

stream 

thermocouple

Compare to value 

generated by dry well 

monitored with 

potentiometer 

thermocouple system

Hart Model 

9100A dry 

well 

calibration 

system

Difference of ≤ ±1.5% of 

minimum absolute stack 

temperature from absolute 

reference temperature 

(unsaturated gas streams)

Before and after 

test series

Yes

Final impinger 

outlet 

temperature 

sensor 

(thermocouple)

Compare to mercuryin-glass thermometerASTM 

thermometer

≤ ±2°F difference from 

reference

Before and after 

test series

Yes

Filter 

temperature 

sensor 

(thermocouple)

Compare to mercuryin-glass thermometerASTM 

thermometer

≤ ±5.4°F difference from 

reference

Before and after 

test series

Yes

Aneroid 

barometer

Compare to calibrated 

mercury barometer

Mercury 

column 

barometer

≤ ±0.1 in Hg difference 

from reference

Before and after 

test series

Yes

Type S pitot 

tube

Measure dimensions 

according to 40 CFR

60, Appendix A, 

Method 2 for baseline 

coefficient of 0.84

Micrometer 

and angle 

finder

Meets dimensional criteria 

specified in Method 2, 

Section 6.1 and 

Figures 2-2 and 2-3

Before and after 

test series

Yes
5-4

Table 5-2. Criteria for Emission Measurement and Data Quality

Test parameters Matrix Method of determination Frequency Accuracy objective Precision objective Objective met? (Y/N)

Dioxin/ Furan Method 23 train 

samples

Surrogate standards 

(spiked in lab during 

preparation of XAD for 

sampling trains)

Each field sample and 

blank

70% to 130% recovery NA Yes

Internal standards Each field sample and 

blank

40 - 130% recovery (tetra-hexa)

25 - 130% rec. (hepta-octa)

NA see Note 1

BCS3 standards Each analytical batch 80 - 120% recovery NA Yes

Laboratory reagent blank One XAD/filter Levels less than lowest calibration standard NA Yes

Moisture (water 

vapor)

Impinger contents Balance calibration check 

with calibration weight

Prior to initial and final 

gravimetric 

determinations

± 0.1g NA RPD < 0.1% of check 

weight.

Moisture, 

Pressure, temp., 

and velocity

Gas stream being 

measured

Secondary technical 

review of field test data 

and equipment 

calibration records 

relative to EPA 

Methods 1-5

Ongoing during testing Validated by meeting posttest equipment 

calibration tolerances

NA Yes

CO2 and O2, by 

Orsat

Stack Gas Single analysis of 

ambient air

Prior to sample analysis 98% to 102% (assuming air at 20.9% O2) 2% RPD Yes

Triplicate analysis of test 

samples

Each sample NA 2% RPD Yes

CO2 and O2, by 

instrument 

analyzer on site

Stack gas Analyzer calibration error 

check with zero, midrange, and high-range 

calibration gases

After system setup 

each day and more 

often when needed

≤ ±2% of span for the difference between 

system response and calibration gas value 

for any of the calibration gases

NA Yes

Sampling system bias 

check with zero and 

either of the upscale 

calibration gases

After the calibration 

error check, during 

calibration drift tests

≤ ±5% of span for the difference between 

analyzer response for the initial calibration 

error check and system response for the 

initial bias check for either of the calibration 

gases

NA Yes

Response time 

determination

During the initial bias 

check each day

NA NA Yes

Zero and calibration drift 

tests

Repeat the bias check 

after each run or more 

often if needed

≤ ±5% of span for the difference between 

analyzer response for the initial calibration 

error check and system response for the 

final bias check for either of the calibration 

gases

≤ ±3% of span for 

the difference 

between final and 

initial system.

Yes

NA = Not Applicable.

Note 1: Method 23 internal standard recoveries corresponding to Run 1 Retest were >130%. A likely cause is discussed in the text and may have resulted in a low bias for this sample. The 

accompanying method blank, sampling standard, and BCS3 results are all within the QA objectives.

 
5-5

Table 5-3. Criteria for Assessing Data Quality of Process Sample Analyses

Test 

parameters Matrix

Method of

determination Frequency Accuracy objective

Precision 

objective

Objective 

met? (Y/N)

Dioxin/ Furan

Raw Feed, and Final Product

Clean-up standards Each sample 40% to 135% 

recovery for all 

2,3,7,8-substituted 

internal standards

NA Yes

Duplicate extraction 

and analysis

One sample 

per matrix for 

the test

NA 25% RPD 

for analytes 

present 

above the 

reporting 

limit

NA

See Note 2.

Laboratory reagent 

blank

One sample 

per matrix for 

the test

Levels less than 

lowest calibration 

standard

NA Yes

Note 2: Duplicate extraction and analysis was not intended to be included in the test plan.
5-6

Table 5-4. Method 23 Internal Standard and Surrogate Standard Recoveries

Analyte

Method

blank

Run 1 Retest

Method

blank

Runs 2-6

Field

blank

train

Mill Dryer

Run 1 Retest Run 2 Run 3 Run 4 Run 5 Run 6

Internal Standard (IQS) % Recoveries: QA objective 40-130% for tetra-hexa; 25-130% for hepta-octa

13C-2,3,7,8-TCDD 106 74.1 82.2 139 84.7 82.4 87.0 60.8 51.9

13C-1,2,3,7,8-PeCDD 109 75.4 85.8 143 87.5 82.9 90.0 63.5 53.8

13C-1,2,3,6,7,8-HxCDD 95.6 79.2 88.7 138 88.6 86.9 92.2 64.5 54.4

13C-1,2,3,4,6,7,8-HpCDD 106 82.3 88.3 147 90.9 91.9 96.3 67.6 57.8

13C-1,2-OCDD 89.2 79.6 87.7 133 90.6 90.9 99.9 68.0 57.4

13C-2,3,7,8-TCDF 116 87.2 82.1 152 86.2 83.9 87.6 62.2 49.9

13C-1,2,3,7,8-PeCDF 111 76.2 86.1 146 86.3 83.6 89.1 63.7 52.0

13C-1,2,3,6,7,8-HxCDF 90.9 76.7 88.4 132 88.2 84.7 92.2 62.9 52.3

13C-1,2,3,4,6,7,8-HpCDF 105 81.7 87.2 147 89.6 90.3 95.5 66.9 56.6

13C-OCDF 79.3 80.8 88.6 127 89.3 90.1 98.9 67.4 56.2

Surrogate Standard % Recoveries: QA objective 70-130%

37Cl-2,3,7,8-TCDD Note 1 98.8 99.1 75.7 97.9 102 97.9 100 103

13C-1,2,3,4,7,8-HxCDD Note 1 101 100 73.4 99.7 106 99.4 102 102

13C-2,3,4,7,8-PeCDF Note 1 98.2 96.7 75.0 97.0 100 98.9 102 103

13C-1,2,3,4,7,8-HxCDF Note 1 102 98.9 75.8 98.7 104 99.4 104 106

13C-1,2,3,4,7,8,9-HpCDF Note 1 98.0 97.7 70.3 98.1 103 97.7 99 104

Independent Laboratory Check Spike, %: QA objective 40-130%

13C-1,2,3,7,8,9-HxCDF 107 79.9 87.8 112 90.3 87.3 91.8 65.8 51.7

Recoveries outside of the QA objectives are highlighted; see Section 5.2 for further explanation.

Note 1: This lab method blank was prepared with sand in lieu of XAD-2 resin in order to save the resin for Runs 2-6.
5-7

Table 5-5. BCS3 Surrogate Recoveries

Analyte

Run 1 Retest Runs 2-6

BCS3A BCS3B BCS3A BCS3B

Extraction Standard, ES, %: QA objective 80-120%

13C-2,3,7,8-TCDD 100 96.5 108 109

13C-1,2,3,7,8-PeCDD 108 109 108 107

13C-1,2,3,6,7,8-HxCDD 96.8 96 102 107

13C-1,2,3,4,6,7,8-HpCDD 101 104 108 106

13C-OCDD 93.4 101 109 107

13C-2,3,7,8-TCDF 102 103 109 110

13C-1,2,3,7,8-PeCDF 105 108 106 106

13C-1,2,3,6,7,8-HxCDF 110 107 102 100

13C-1,2,3,4,6,7,8-HpCDF 109 111 107 102

13C-OCDF 106 112 103 106

Surrogate Spike, SS, %: QA objective 80-120%

37Cl-2,3,7,8-TCDD 96.6 97.2 86.6 88

13C-1,2,3,4,7,8-HxCDD 90.3 92 92.6 87.2

13C-2,3,4,7,8-PeCDF 101 100 92.3 92.8

13C-1,2,3,4,7,8-HxCDF 90.1 92.8 89.8 87.2

13C-1,2,3,4,7,8,9-HpCDF 94.7 93.1 84.9 87.6

Alternate Standard, AS, %: QA objective 80-120%

13C-1,2,3,7,8,9-HxCDF 90.4 91 94.7 92.6
5-8

Table 5-6. Method 8290 Internal Standard Recoveries

Analyte

Method

blank

Mill Dryer

Run 1 Run 2 Run 3 Run 4 Run 5 Run 6

Clay Feed

Dioxins

13C-TCDD 90.6 92.3 90.8 92.2 97.2 101 77.4

13C-PeCDD 86.2 91.5 87.5 88.4 93.5 97.1 76.8

13C-HxCDD 90.5 84.6 90.6 86.5 88.9 92.3 73.6

13C-HxCDD 89.1 85.8 86.9 84.4 87.3 91.5 72.9

13C-HxCDD 91.4 83.3 89.9 83.9 90.4 97 73

13C-HpCDD 90.4 82.8 94.5 86.6 93.7 97.1 79.2

13C-OCDD 85 74.2 105 98.4 136 145 107

Furans

13C-TCDF 98.1 92.9 88.1 92.7 96.5 98.6 77.4

13C-PeCDF 86.8 90 85.3 90 97.5 97.7 76.5

13C-PeCDF 87.1 92.4 87.6 89.3 96.5 101 77.8

13C-HxCDF 90.5 95.8 98 89.6 90.4 93.3 76.5

13C-HxCDF 89 94.7 98.5 91.9 94.8 94.1 75.9

13C-HxCDF 91.7 91.1 97.2 89.3 92.9 97.2 76.4

13C-HxCDF 90.2 92 91.2 83.3 91.4 92.8 73.2

13C-HpCDF 89.6 80.2 86.4 82.1 84.4 85.8 70

13C-HpCDF 90.6 85.8 87.2 79.5 87 85.6 68

13C-OCDF 84.4 86.2 90.7 83.9 91.4 95.8 75.5

Clay Product

Dioxins

13C-TCDD 90.6 87.5 89.8 92.6 93.3 102 89.7

13C-PeCDD 86.2 86.6 84.8 87.9 95.8 97.1 89.2

13C-HxCDD 90.5 82.5 87.7 85.2 94.9 98.1 81.3

13C-HxCDD 89.1 80.5 89.6 83.5 95.2 98.1 80.2

13C-HxCDD 91.4 81.6 87.2 83.3 97.3 94.3 79.7

13C-HpCDD 90.4 76.5 90.4 87.1 105 80.7 76

13C-OCDD 85 72.7 97.6 100 157 82.2 84.3

Furans

13C-TCDF 98.1 91.2 91 91 97.4 99.7 97.2

13C-PeCDF 86.8 85.4 86.9 87.4 95.2 96.8 90.1

13C-PeCDF 87.1 86.8 86.3 87.6 97.3 98.9 88.6

13C-HxCDF 90.5 90 97.7 86.7 101 107 92.1

13C-HxCDF 89 90.1 103 86.9 102 108 92.7

13C-HxCDF 91.7 87.7 91.8 86.4 99.3 109 91.4

13C-HxCDF 90.2 89.7 89.3 85.3 97.9 106 89.1

13C-HpCDF 89.6 78.2 82.5 81.6 92.4 91.7 82.9

13C-HpCDF 90.6 80.9 85.5 77.3 96.6 95.7 82.6

13C-OCDF 84.4 81.5 87.1 81.9 101 94 87

Recoveries outside of the QA objectives (40% to 135%) are highlighted; see Section 5.2 for further explanation.
Appendix A

Sample Custody Records
A-1
A-2
A-3
A-4
A-5
A-6
A-7
A-8
A-9
A-10
A-11
A-12
A-13
A-14
A-15
A-16
A-17
A-18
A-19
A-20
Appendix B

Sampling Data and Field Analytical Records
Appendix B-1

Emissions Sample Collection
B1-1
B1-2
B1-3
B1-4
B1-5
B1-6
B1-7
B1-8
B1-9
B1-10
B1-11
B1-12
B1-13
B1-14
B1-15
B1-16
B1-17
B1-18
B1-19
B1-20
B1-21
B1-22
B1-23
B1-24
B1-25
B1-26
Appendix B-2

Emissions Sample Recovery
B2-1
B2-2
B2-3
B2-4
B2-5
B2-6
B2-7
B2-8
B2-9
B2-10
B2-11
B2-12
B2-13
B2-14
B2-15
B2-16
B2-17
B2-18
Appendix B-3

Ball Clay Sample Collection
B3-1
B3-2
B3-3
Appendix B-4

O2 and CO2 Analysis
B4-1
B4-2
B4-3
B4-4
B4-5
B4-6
B4-7
B4-8
B4-9
B4-10
B4-11
B4-12
B4-13
B4-14
B4-15
B4-16
B4-17
B4-18
B4-19
Appendix C

Field Sampling Equipment Calibration Records
Appendix C-1

Pre-Test Calibration Records
C1-1
C1-2
C1-3
C1-4
C1-5
C1-6
C1-7
C1-8
C1-9
C1-10
C1-11
C1-12
C1-13
C1-14
C1-15
C1-16
C1-17
C1-18
C1-19
C1-20
C1-21
C1-22
C1-23
C1-24
C1-25
C1-26
MRI-AED\UNIMIN TEST REPORT NON-CBI VERSION REVISED BY LIBRARY 3-24-10.DOC

Appendix C-2

Post-Test Calibration Records
C2-1
C2-2
C2-3
C2-4
C2-5
C2-6
C2-7
C2-8
C2-9
C2-10
C2-11
C2-12
C2-13
C2-14
C2-15
C2-16
C2-17
Appendix D

Summary Analytical Reports and Data
Appendix D-1

Run 1 Retest Emission Samples
D1-1
D1-2
D1-3
D1-4
D1-5
D1-6
D1-7
D1-8
D1-9
D1-10
D1-11
Appendix D-2

Runs 2 Through 6 Emission Samples
D2-1
D2-2
D2-3
D2-4
D2-5
D2-6
D2-7
D2-8
D2-9
D2-10
D2-11
D2-12
D2-13
D2-14
D2-15
D2-16
D2-17
D2-18
Appendix D-3

Runs 1 Through 6 Clay Feed and Product Samples

(CBI data removed. See confidential version of document.)
Appendix E

Batch Control Spikes (BCS3)
E-1

9.3.1 Batch CS3

9.3.1.1 Definition: 

• A QC sample used for true-stable isotope-dilution GC/MS 

methodologies to ensure the reliability and accuracy (bias 

and precision) of the determinations.

• It is a new concept introduced to, not only, enhance the 

accuracy of the measurements, but to provide a basis for 

assigning an uncertainty to each measurements (NOTE:

this is limited to the measurement step because it does not 

directly address the sampling errors), and abridge the level 

of effort involved in the documentation of the system’s 

performance (i.e., what used to require three separate 

analyses are now combined into one). 

• It is prepared—inside the same type of vial used for the 

GC/MS analysis—in stages at the same time as the batch 

of field samples; i.e., at each phase involving the addition 

of the ES, CS, JS to the samples. For air matrices, the 

Batch CS3 is initiated at the same instant as the XAD/PUF 

cartridges are prepared for sampling.

One Batch CS3 per batch of 20 samples or less—regardless of the matrix type—is going 

through the same spiking scheme with the same spiking solutions, same analyst, same 

delivery system, and at the same time as the field samples. It is the laboratory’s 

responsibility to ensure sufficient Batch CS3’s are prepared to provide front- and backend calibration verifications for all the samples as well as reinjections when necessary. 

The Batch CS3 is then analyzed at the beginning and at the end of a 12-H analytical 

sequence during which samples are analyzed. For an example of BCS3 (M8290B), click 

here.

• In order to use the front- and back-end Batch CS3s 

averaged RRFs to process the samples, the individual 

front- and back-end RRFs need to meet a number of 

requirements (independent verification, RPD, and PD or 

bias):

9.3.1.1.1 The NS solution should be verified against an 

independent source. The maximum allowable 

difference for the “intra-source product area” ratios 

(vide infra) for the unlabeled compound’s RRFs is 

±20 percent (from the laboratory normal source) 

relative to the ES (from an independent source). This 

verification should be performed every time a new set 

of ICAL solutions and new sets of spiking solutions 
E-2

(ES, CS/SS, JS, NS) are prepared from new primary 

stock standards with a minimum of one verification 

per year.

9.3.1.1.2 The ES solution should be verified against an 

independent source. The maximum allowable 

difference for the “intra-source product area” ratios 

(vide infra) for the unlabeled compound’s RRFs is 

±20 percent (from an independent source) relative to 

the ES (from the laboratory normal source). This 

verification should be performed every time a new set 

of ICAL solutions and new sets of spiking solutions 

(ES, CS/SS, JS, NS) are prepared from new primary 

stock standards with a minimum of one verification 

per year.

9.3.1.1.3 More specifically, it is necessary for the “intra-source 

product area” ratio below to range from 0.8 to 1.20.

where:

Ax

ls = the area of the unlabeled analyte from the 

laboratory source

AES

ls = the area of the labeled extraction standard 

from the laboratory source

Ax

is = the area of the unlabeled analyte from the 

independent source

AES

is = the area of the labeled extraction standard 

from the independent source

α is equal to 1 when the concentrations of the 

respective analytes are the same between the 

independent and laboratory sources; the appropriate 

factor should be applied for situations whereby the 

concentrations of the respective analytes are 

different.

laboratory source

independent 

is

ES

is

x

ls

ES

ls

x

A A

A A

α

×

×

×
E-3

NOTE: It is highly recommended that the above 

mixtures be prepared in the same solvent 

and analyzed under the same GC/MS 

conditions.

NOTE: Intra-source product area ratios only apply 

to analytes for which matching standards 

are available between the laboratory and 

independent sources.

9.3.1.1.4 Similarly, for air samples, it is necessary for the 

“intra-source product area” ratio below to range 

from 0.7 to 1.30.

where:

ASS

ls = the area of the sampling standard from the 

laboratory source

AES

ls = the area of the labeled extraction standard 

from the laboratory source

ASS

is = the area of the sampling standard from the 

independent source

AES

is = the area of the labeled extraction standard 

from the independent source

α is equal to 1 when the concentrations of the 

respective analytes are the same between the 

independent and laboratory sources; the appropriate 

factor should be applied for situations whereby the 

concentrations of the respective analytes are 

different.

NOTE: When the SS are used as cleanup standards for 

non-air matrices, replace SS by CS and ES by 

JS in the expression above.

laboratory source

independent 

is

ES

is

SS

ls

ES

ls

SS

A A

A A

α

×

×

×
E-4

9.3.1.1.5 The RPDs between the front- and back-end Batch CS3s 

should remain within 

9.3.1.1.5.1 Ten percent for the unlabeled compounds

9.3.1.1.5.2 Twenty percent for the labeled compounds 

9.3.1.1.6 The RRFs Percent Differences (PD) relative to the ICAL 

should remain within 

9.3.1.1.6.1 Twenty percent for the unlabeled compounds 

9.3.1.1.6.2 Thirty-five percent for the non-air matrices labeled 

ES compounds

9.3.1.1.6.3 Fifty percent for air matrices labeled ES compounds

9.3.1.1.6.4 Twenty percent for air’s labeled SS, and 

9.3.1.1.6.5 Thirty percent for non air’s labeled CS compounds

9.3.1.1.6.6 Other requirements are shown in Table Insert 1 and 

Table Insert 2. 

9.3.1.1.7 The addition of both NS and ES should be performed using 

the same technique and the same volume. That way, any 

systematic error (within acceptable limits as defined 

herein) will “ratio out” when the two Batch CS3 

calibration analyses are used to compute the analyte 

concentrations in the samples. By using this approach, the 

accuracy of the measurements is superior to the traditional 

approaches. It is also a benefit that flows directly from 

true stable isotope-dilution GC/MS, which until now was 

regrettably ignored. 

9.3.1.1.8 For air samples where a split factor is involved, i.e., the 

sample extract is split and a portion is archived as backup, 

the Batch CS3 is not subjected to an actual physical 

division. The latter is simulated by the addition of an 

appropriate volume of the same solvent as for the ICAL 

and the samples (e.g., if the split factor is 2, then, the 

Batch CS3 needs to be diluted two fold before analysis to 

allow the analytes to be at the same concentration as for 

the ICAL CS3). 

9.3.1.1.9 For air samples, the Batch CS3 is initiated at the same time 

as the preparation of the air sampling modules before the 

sampling session. To that effect, the same amount of the 

Sampling Standards is added to a vial, which is kept in the 

laboratory at room temperature and away from light. The 

corresponding Lab Method Blank prepared with the same 

batch of sorbent and spiking solution (i.e., 40 g XAD-2 

resin, or PUF) is kept refrigerated.
E-5

9.3.1.2 At the beginning and end of each 12-hour period during which 

samples are analyzed, an aliquot of the Batch CS3 is analyzed to 

demonstrate adequate GC resolution and sensitivity, response 

factor reproducibility, to establish the PCDD/PCDF retention 

time windows and isomer-specificities, and to validate the ES 

standards and the spiking technique. 

9.3.1.3 As defined above, the criteria for an acceptable Batch CS3 are 

summarized in the table inserts below. When the Batch CS3 

fails, it is important to discern the following:

9.3.1.3.1 The fundamental objective of the Batch CS3 is to “validate” 

the ES and the RRFs used to quantitatively characterize 

the analytes in the samples at the time the standards are 

used to prepare and analyze the samples. They are four 

types of standards involved in the preparation of the Batch 

CS3 that provide various probes into assessing this 

“validation” procedure. They are the NS (symbolized as 

Ax in expressions or tables), ES, SS or CS, and JS. The 

question becomes how can one “extract” the information 

needed to complete the validation, or how does one “filter” 

out the irrelevant information to help with the distinction 

between a critical error and a minor one. A critical error 

means erroneous data resulting from a seriously flawed 

spiking technique (e.g., wrong amount of ES added) while 

other minor errors can provide useful information or 

feedback on the measurement step (e.g., instrumentation 

variation). The interpretation of the information obtained 

from the analysis of the Batch CS3 is best handled when 

done contextually. This analytical protocol does not claim 

that it offers a comprehensive analysis but merely puts 

forward guidelines to help the analyst in assessing the 

quality and reliability of the data.

9.3.1.3.2 A failure on the “PD” requirements may be indicative of 

an instrumentation difficulty or spiking error. The latter 

can be of Level PD-1 (i.e., at the standard solution level) 

or Level PD-2 (i.e., at the spiking operation level). A third 

Level PD-3 is associated with instrumentation. An error at 

the standard solution level (Level PD-1) constitutes the 

most serious failure and requires that a new set of standard 

solutions be prepared, independently validated (vide infra, 

intra-source ratio study) before repeating the sample 

extraction and analysis. A new initial calibration is 

required before analyzing the Batch CS3 and the samples. 

However, if the error is a Level PD-2 error, a re-extraction 

and analysis is the most suitable action after correcting the 

flawed spiking technique. As customarily done, a new 

Batch CS3 is prepared with a Level PD-2 error. 

Distinction between Levels PD-1 and PD-2 can be 

accomplished contextually by examination of the initial 
E-6

independent validation study and control charts (showing 

for instance a trend suggesting a degradation of the ES 

solution), and using the matrices shown in Table Inserts 3

or 4. The Level PD-3 error is associated with 

instrumentation when an out-of-calibration situation is 

present or a temporary or localized instrumentation 

variation is operative. Depending on the severity of the 

Level PD-3 error, a new calibration (either ICAL or 

rerunning the Batch CS3 and all the affected samples) 

following a new “tuning” of the instrumentation may be 

required. 

9.3.1.3.3 A failure on the “RPD” requirements may be indicative of 

instrumentation instability or inability to sustain the 

instrumentation’s performance over a 12-H period. Again, 

two levels are possible. Level RPD-1 is strictly associated 

with instrumentation difficulties that are unrelated to the 

samples under analysis. A re-analysis (i.e., re-injection) of 

the Batch CS3 and of the samples can be considered as a 

corrective action after correction of the source of the 

instrumentation’s shortfall. If however, the re-analysis of 

the Batch CS3 fails again, and there are indications that the 

spiking procedure is questionable (Level PD-1 or PD-2), 

the associated extraction batch must undergo re-extraction 

and analysis with the preparation of a new associated 

Batch CS3 as discussed above for the Batch CS3 PD 

deviations. A Level RPD-2 Batch CS3 failure may be 

found with the analysis of samples presenting special 

challenges (i.e., highly complex matrices that do not 

cleanup well under the various options offered by this 

protocol). Depending on the severity of the deviation, 

additional cleanup or other appropriate actions may be 

required before re-analysis of the samples and associated 

Batch CS3. If such action proves to be ineffective, the 

data should be qualified accordingly.

9.3.1.3.4 A “PD” failure for 2,3,7,8-TCDD and/or 2,3,7,8-TCDF 

results in the inability to reliably quantify 2,3,7,8-TCDD/F 

until proper corrective action is implemented (e.g., 

following GC column maintenance). When the corrective 

action involves a different liquid phase, the correct Batch 

CS3 is used to demonstrate adequate performance. Note 

that the laboratory is encouraged to adopt a similar stance 

for 1,2,3,7,8-PeCDD and 2,3,4,7,8-PeCDF (or any other 

2,3,7,8-substituted congeners, which significantly 

contributes to the TEQ). 

9.3.1.3.5 The Batch CS3 “PD Requirements” are summarized in the 

four table inserts below. In addition to the traditional 

RRFs, another set of “pseudo-RRFs” is computed from the 

Batch CS3 data to help with the validation of the ES and 
E-7

RRFs used to report the sample analytes. The pseudoRRFs are used to further differentiate the various “A” to 

“C” types PD Requirements. Use Table Insert 3 (non air) 

or Table Insert 4 (air) for departing-from-the-norm groups 

of analytes (e.g., all 17 Ax or the five SS show a deviation 

similar in “sign” and “amplitude”). It is also 

recommended to examine the data contextually (e.g., using 

QC charts). 
E-8

Table Insert 1: 

Batch CS3 PD Requirements 

Based on Traditional RRFs 

(“A” to “C” Types)

Type Analytes Requirement Failure Possible Causea,b Failure Level Suggested

Corrective Action

A Ax vs ES ±20% 1. Calibration out

2. Spiking error

1. PD-3

2. PD-1/PD -2

1. New Calibration

2. New Standards/New 

Extraction

B ES vs. JS ±35% non air

±50% for airc

1. Calibration out

2. Spiking error

1. PD-3

2. PD-1/PD-2

1. New Calibration

2. New Standards/New 

Extraction

C1 CS vs. JS

(non air)

±35% 1. Calibration out

2. Spiking error

1. PD-3

2. -

1. New Calibration

2. Affects other Types

C2 SS vs. ES

(air)

±20% 1. Calibration out

2. Spiking error

1. PD-3

2. PD-1/PD -2

1. New Calibration

2. New Standards/New 

Extraction/New 

Samplingd

a) Calibration out = usually when one (localized) or several/all analytes are affected; 

instrumental source.

b) Spiking error = when all analytes are affected with the same “sign” and “amplitude”; 

must be considered contextually; i.e., using historical data or other information on the 

set of standards such as the “pseudo-RRFs”. Situations when selected analytes 

degrade are rare but should not be excluded from consideration.

c) This wider tolerance recognizes the fact that, by design for air matrices, the amounts 

of ES and JS added during the preparation of the Batch CS3 are different. Thus, an

additional error is introduced, which can deceive the analyst’s interpretation. In this 

case, the QC emphasis is shifted towards the “C2” type PD requirement.

d) Because of the nature of an “air” sample, there is no additional sample volume 

available to repeat the extraction. The laboratory is required to qualify the data by 

estimating and documenting accordingly the “error” associated with the reported 

measurements. If such documentation is not possible, and/or the information points 

toward a seriously flawed ES addition (as opposed to a spiking error associated with 

the SS), the data can be rejected and re-sampling efforts may be necessary. See the 

“Air Spiking Related Error Matrix” tables for an alternative approach whereby the Ax

vs. SS RRFs are used to determine the analyte’s concentrations (Table Insert 4). 
E-9

Table Insert 2:

Batch CS3 PD Requirements

Based on Pseudo-RRFs 

(“D” to “G” Types)

a) Pseudo-RRFs are limited to analytes, for 

which an analogous/homologous standard is 

available:

• 2,3,7,8-TCDD (Ax) vs. 13C12-1,2,3,4-

TCDD (JS)

• 2,3,4,7,8-PeCDF (Ax) vs. 13C12-

1,2,3,4,6-PeCDF (CS)

• 13C12-1,2,3,7,8-PeCDD (ES) vs. 13C12-

1,2,3,4,7-PeCDD (CS)

• Do not consider pairs such as OCDD 

(Ax) vs. 13C12-1,2,3,4,6,8,9-HpCDF 

(SS) or 13C12-1,2,3,4,7-PeCDD (CS or 

SS) vs. 13C12-1,2,3,4,6,7-HxCDD (JS) 

Type Analytesa Requirement

D Ax vs. CS/SS ±25%

E1 Ax vs. JS

(non air)

±35%

E2 Ax vs. JS

(air)

±50%

F1 ES vs. CS

(non air)

±20%

G2 SS vs. JS

(air)

±50%
E-10

Table Insert 3:

“Non-Air” Spiking Related PD Errors 

(departing-from-the-norm group of analytes)

“PD Requirements Decision Matrix”—Normal Configuration

(use BCS3 RRFs)

Ax ES CS JS

Ax – Y Y Y

ES – – Y Y

CS – – – Y

“PD Requirements Decision Matrix”—Defective Ax Spiking

(use ICAL RRFs)

Ax ES CS JS

Ax – N N N

ES – – Y Y

CS – – – Y

“PD Requirements Decision Matrix” – Defective JS Spiking

(use BCS3 RRFs) 

percent recovery measurements for CS & ES affected, not the analytes

Ax ES CS JS

Ax – Y Y N

ES – – Y N

CS – – – N

“PD Requirements Decision Matrix”—Defective CS Spiking

(use BCS3 RRFs) 

percent recovery measurements for CS affected, not the analytes

Ax ES CS JS

Ax – Y N Y

ES – – N Y

CS – – – N

“PD Requirements Decision Matrix”—Defective ES Spiking

(Levels PD-1 or PD-2)

Ax ES CS JS

Ax – N Y Y

ES – – N N

CS – – – Y
E-11

Table Insert 4:

“Air” Spiking Related PD Errors 

(departing-from-the-norm group of analytes)

“PD Requirements Decision Matrix”—Normal Configuration

(use BCS3 RRFs)

Ax ES SS JS

Ax – Y Y Y

ES – – Y Y

SS – – – Y

“PD Requirements Decision Matrix”—Defective Ax Spiking

(use ICAL RRFs)

Ax ES SS JS

Ax – N N N

ES – – Y Y

SS – – – Y

“PD Requirements Decision Matrix”—Defective JS Spiking

(use BCS3 RRFs) 

percent recovery measurements for ES affected, not the analytes or the SS

Ax ES SS JS

Ax – Y Y N

ES – – Y N

SS – – – N

“PD Requirements Decision Matrix”—Defective SS Spiking

(use BCS3 RRFs) 

percent recovery measurements for SS affected, not the analytes

Ax ES SS JS

Ax – Y N Y

ES – – N Y

SS – – – N

“PD Requirements Decision Matrix”—Defective ES Spiking

(Levels PD-1 or PD-2; for air samples only, consider using the Ax vs. SS RRFs)

Ax ES SS JS

Ax – N Y Y

ES – – N N

SS – – – Y
Appendix F

BCS3 Performance Criteria
F-1
F-2
F-3
Appendix G

Process Data and Material Sampling Log Sheets

(CBI data removed. See confidential version of document.)
TECHNICAL REPORT DATA

(Please read Instructions on reverse before completing)

1. REPORT NO.

 EPA2. 3. RECIPIENT'S ACCESSION NO.

4. TITLE AND SUBTITLE

Characterization of Dioxin Emissions From Sources That Use Ball Clays

Emission Test Report: Unimin Corporation, Gleason, TN

5. REPORT DATE

March 2010 

6. PERFORMING ORGANIZATION CODE

7. AUTHOR(S)

Clyde E. Riley, USEPA Mark B. Turner, RTI International 

Mary Johnson, USEPA John Hosenfeld, Midwest Research Institute

Brian Shrager, USEPA 

Robin Segall, USEAP 

8. PERFORMING ORGANIZATION REPORT NO.

9. PERFORMING ORGANIZATION NAME AND ADDRESS

U.S. Environmental Protection Agency

Office of Air Quality Planning and Standards

Research Triangle Park, NC 27711

10. PROGRAM ELEMENT NO.

11. CONTRACT/GRANT NO. 68-D-01-079 

12. SPONSORING AGENCY NAME AND ADDRESS

Director

Office of Air Quality Planning and Standards

Office of Air and Radiation

U.S. Environmental Protection Agency

Research Triangle Park, North Carolina 27711

13. TYPE OF REPORT AND PERIOD COVERED

Final; March 2010

14. SPONSORING AGENCY CODE

EPA/200/04

15. SUPPLEMENTARY NOTES

16. ABSTRACT

This test report is part of a study designed to determine the magnitude of emissions of dibenzo-p-dioxins and dibenzofurans 

released from thermal processing of ball clay. In this test program, a heated ball clay mill and a dryer at a ball clay manufacturing 

facility were tested on consecutive weeks during the time period from August 21 through August 20, 2003.

17. KEY WORDS AND DOCUMENT ANALYSIS

a. DESCRIPTORS b. IDENTIFIERS/OPEN ENDED TERMS c. COSATI 

Field/Group

Dioxins/furans

Ball Clay

Air pollution control

Ball Clay

18. DISTRIBUTION STATEMENT 19. SECURITY CLASS (Report)

 

21. NO. OF 

PAGES

20. SECURITY CLASS (Page)

 

22. PRICE

EPA Form 2220-1 (Rev. 4-77)
MRI-AED\UNIMIN TEST REPORT NON-CBI VERSION REVISED BY LIBRARY 3-24-10.DOC

United States

Environmental Protection

Agency

Office of Air Quality Planning and 

Standards

Sector Policies and Programs 

Division

Research Triangle Park, NC

Publication No. 

EPA- 453/R-10-001

March, 2010