&EPA
United Stales
Eiviraimwilfll Protection
Agency
Characterization of Dioxin Emissions
From Sources That Use Ball Clays
Emission Test Report: Unimin Corporation,
Gleason, TN
Final Report
(Non-Confidential Version)
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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
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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 (BCSs)
Appendix F—BCSs Performance Criteria
Appendix G—Process Data and Material Sampling Log Sheets
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VI
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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 CC>2 and C>2 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
vn
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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 Results51 3-8
Table 3-6. Dioxin/Furan Mill Clay Product Homolog Results51 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 Results51 3-14
Table 3-12. Dioxin/Furan Dryer Clay Product Homolog Results51 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. BCSs Surrogate Recoveries 5-7
Table 5-6. Method 8290 Internal Standard Recoveries 5-8
Vlll
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Section 1.
Introduction
1.1 Test Summary
1.1.1 Background
The EPA has determined that certain ball clay mineral deposits contain naturally-
occurring 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 (€62), 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
CC>2 and 62 concentrations were measured during each run using EPA Method 3 at the
dryer and Method 3 A 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:
1-1
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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
Research Triangle Institute
800 Park Office
Highway 54
Research Triangle Park, NC 27709
Telephone: (919) 316-3743
Mr. John Hosenfeld
Midwest Research Institute
425 Volker Blvd.
Kansas City, MO 64110-2299
Telephone: (816) 753-7600, ext. 1336
Figure 1-1 presents the test program organization, major lines of communication, and
names and phone numbers of responsible individuals.
1-2
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US EPA
Office of Air Quality Planning & Standards
Emissions Standards Division
Brian Shrager
Work Assignment Manager
919-541-7689
Research Triangle Institute
Work Assignment Leader
Mark Turner
919-316-3743
US EPA
Office of Air Quality
Planning & Standards
Emissions Measurement Center
Clyde E. Riley
On-Site Work Assignment Manager
EMC Contact
J. Kaye Whitfield
919-541-2509
Midwest Research Institute
Director, Corporate QA Unit
Paul Constant
816-753-7600, ext. 1114
Midwest Research Institute
Task Assignment Leader
John Hosenfeld
816-753-7600, ext. 1336
Midwest Research Institute
Senior QA Officer
Tom Dux
816-753-7600, ext. 1242
Midwest Research Institute
Field Team & CEMS Leader
Dan Neal
816-753-7600, ext. 1409
Midwest Research Institute
Emissions Sampling
Method 23 Testing
April Sanders
816-753-7600, ext. 1859
Research Triangle Institute
Process Sampling
Mark Turner
919-316-3743
Alta Analytical
Perspectives
D/F Analysis
Yves Tondeur
910-794-1613
Direct reporting relationship
Communication
Figure 1-1. Test Program Organization
1-3
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1-4
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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.
2-1
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Table 2-1. Summary of Process Operating Parameters Monitored During Testing
for the Mill
Test
Run
No.
1Rea
2
3
Date
Tested
8/13/03
8/14/03
8/15/03
Ball Clay
Product
Processed
SB Blend
SB Blend
Rex
Average =
Mill Operating
Temperature,
°C (°F)
b
b
b
b
Baghouse Inlet
Temperature,
°C (°F)
b
b
b
b
Baghouse
Pressure Drop,
Inches of Water
2.5
2.5
2.5
2.5
Mill
Production Rate,
Mg/Hour
(Tons/Hour)
b
b
b
b
a1Re 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.
2-2
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Table 2-2. Summary of Process Operating Parameters Monitored During Testing
for the Dryer
Test
Run
No.
4
5
6
Date
Tested
8/18/03
8/19/03
8/20/03
Ball Clay
Product
Processed
SB Blend
SB Blend
SB Blend
Average =
Dryer Operating
Temperature,
°C(°F)
a
a
a
a
Baghouse Inlet
Temperature,
°C(°F)
a
a
a
a
Baghouse
Pressure Drop,
Inches of Water
5.5
5.6
5.7
5.6
Dryer
Production Rate,
Mg/Hour
(Tons/Hour)
a
a
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 62 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 CC>2 and C>2. The placement of the CEM probe
end in the stack was at a point of average velocity.
2-3
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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 CC>2 and 62 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 foil-
lined 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
2-4
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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)
4211
5211
6211
4221
5221
6221
2-5
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(CBI data removed. See confidential version of document.)
Figure 2-1. Process Flow Diagram for the Mill Process at Unimin Corporation,
Gleason, TN
2-6
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(CBI data removed. See confidential version of document.)
Figure 2-2. Process Flow Diagram for the Dryer Process at Unimin
Corporation, Gleason, TN
2-7
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Traverse r
A M
Points on a
diameter
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Probe mark
(inches)
1.0
1.4
2.4
3.5
4.6
5.9
7.3
9.0
11.0
14.0
22.0
25.0
27.0
28.7
30.1
31.4
32.5
33.6
33.6
33.6
Figure 2-3. Mill Sampling Location
2-8
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,
45'
1
X*X.
/^\
1
L
16.6'
1
o
4" ports
-*- 2' -*•
j
5.
1
1 J
24"
25' .---20 s^^^
Traverser f J2
A 41 10 10 /
\ /
x-^~iJr^X'^
Traverse
B
Points on a Probe mark
diameter (inches)
'
X
1 0.5
2 0.9
3 1,6
4 2.3
5 3.1
6 4.0
7 4.9
8 6.0
9 7.3
' 10 9.3
/ \ 11 14.7
/ \ 12 16.7
/ \ 13 18.0
| 14 19.1
15 20.0
16 20.9
17 21.7
s /-^/ 18 22'4
s ^^ 19 23.1
20 23.5
Figure 2-4. Dryer Sampling Location
2-9
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2-10
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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
3-1
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Table 3-1. Test Matrix: Summary of Emission and Process Sampling and Analytical Parameters and Methods
Sampling location
Mill baghouse
emission stack
Dryer baghouse
emission stack
Mill Feed sample
Dryer Feed sample
Mill product sample
Dryer product
sample
Sampling or
measurement time
4 hours
4 hours
Composite of grab
samples collected
every 30 min
thereafter for 4 hr
starting 30 min prior
to start of run
Composite of grab
samples collected
every 30 min
thereafter for 4 hr
starting 30 min prior
to start of run
Composite of grab
samples collected
every 30 min
thereafter for 4 hr
starting 30 min prior
to start of run
Composite of grab
samples collected
every 30 min
thereafter for 4 hr
starting 30 min prior
to start of run
Sampling method and
sample size
40 CFR 60, Appendix A, Method 23,
> 6.0 m3
40 CFR 60, Appendix A, Method 2
40 CFR 60, Appendix A, Method 4, >
6.0m3
40 CFR 60, Appendix A, Method 3A,
> 2L/min sampling rate
40 CFR 60, Appendix A, Method 23,
> 6.0 m3
40 CFR 60, Appendix A, Method 2
40 CFR 60, Appendix A, Method 4, >
6.0m3
40 CFR 60, Appendix A, Methods 3
and 3B
ASTM D6051-01, 50-g (approx) grab
samples
collected/composited/mixed/
quartered until two 8-oz samples
obtained
ASTM D6051-01 , 50-g (approx) grab
samples
collected/composited/mixed/
quartered until two 8-oz samples
obtained
ASTM D6051-01, 50-g (approx) grab
samples collected/composited then
mixed/quartered until two 8-oz
samples are obtained
ASTM D6051-01, 50-g (approx) grab
samples
collected/composited/mixed/
quartered until two 8-oz samples
obtained
Emission parameters
PCDDs/PCDFs
Velocity, pressure, temp.,
volumetric flow rate
Moisture
CO2 and O2
PCDDs/PCDFs
Velocity, pressure, temp.,
volumetric flow rate
Moisture
CO2 and O2
PCDDs/PCDFs
PCDDs/PCDFs
PCDDs/PCDFs
PCDDs/PCDFs
Number of runs/samples
3
3
3
Continuous during each run for
a total of 3 runs
3
3
3
One integrated bag during each
run for a total of 3 runs
2 composite samples collected
and split: one sample for
analysis and one sample to be
retained by the facility
2 composite samples collected
and split: one sample for
analysis and one sample to be
retained by the facility
2 composite samples collected
and split: one sample for
analysis and one sample to be
retained by the facility
2 composite samples collected
and split: one sample for
analysis and one sample to be
retained by the facility
Preparation method
Soxhlet extraction
NA
NA
Particulate matter and
moisture removal
Soxhlet extraction
NA
NA
NA
Soxhlet extraction
Soxhlet extraction
Soxhlet extraction
Soxhlet extraction
Analytical method
EPA Method 23
HRGC/HRMS
(SW-846, Method 8290A)
Pilot tube,
Thermocouple
Gravimetric
NDIRforCO2
Micro-fuel cell for O2
EPA Method 23
HRGC/HRMS
(SW-846, Method 8290A)
Pilot tube,
Thermocouple
Gravimelric
Orsal
HRGC/HRMS
(SW-846, Melhod 8290A)
HRGC/HRMS
(SW-846, Melhod 8290A)
HRGC/HRMS
(SW-846, Melhod 8290A)
HRGC/HRMS
(SW-846, Melhod 8290A)
3-2
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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, C>2 and CC>2 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 2V2 times the signal, but that it was observed at less than
one-tenth the lowest point on the calibration curve.
3-3
-------
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 62 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.
3-4
-------
Table 3-2. Summary of Total Dioxin/Furan Results for Mill Samples
Air Emissions
Total PCDDs and PCDFs
Total PCDDs (pg/dscm)
Total PCDFs (pg/dscm)
Total PCDDs and PCDFs (pg/dscm)
Run 1
Retest
117
16.3
134
Run 2
Run 3
Average
167
77.6
245
119
70.1
189
135
54.7
189
Emission Rates/Factors
Dry Clay Process Rate (Mg/hr)
Material Analyses
Clay Feed3
Total PCDDs and PCDFs (pg/g)
Clay Product3
Total PCDDs and PCDFs (pg/g)
Clay feed and product concentrations are calculated on a dry basis.
CBI data removed: See confidential version of document.
3-5
-------
Table 3-3. Dioxin/Furan Homolog Results for Mill Stack Samples
Analyte
Dioxins (pq/dscrrO
TCDD
PeCDD
HxCDD
HpCDD
OCDD
Total PCDDs (pg/dscm)a
Furans (pq/dscrrO
TCDF
PeCDF
HxCDF
HpCDF
OCDF
Total PCDFs (pg/dscm)a
Total PCDDs and PCDFs (pg/dscm)
Run 1 Retestb
27.1
16.6
10.7
12.1
50.8
117
4.86
2.98
3.55
27.4
2.15
16.3
134
Run 2
43.9
30.7
26.6
17.8
48.3
167
24.7
20.5
17.7
11.5
3.30
77.6
245
Run 3
30.0
15.7
8.4
15.4
49.6
119
17.6
17.5
17.2
12.4
5.39
70.1
189
Average
135
54.7
189
3 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.
3-6
-------
Table 3-4. Dioxin/Furan Homolog Emission Factors for Mill Stack Samples
Homolog
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total OCDD
Total CDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Total OCDF
Total CDF
Total CDD/CDF
2,3,7,8 TCDD
1,2,3,7,8 PeCDD
1,2,3,4,7,8 HxCDD
1,2,3,6,7,8 HxCDD
1,2,3,7,8,9 HxCDD
1,2,3,4,6,7,8 HpCDD
Total OCDD
2,3,7,8 TCDF
1,2,3,7,8 PeCDF
2,3,4,7,8 PeCDF
1,2,3,4,7,8 HxCDF
1,2,3,6,7,8 HxCDF
2,3,4,6,7,8 HxCDF
1,2,3,7,8,9 HxCDF
1,2,3,4,6,7,8 HpCDF
1,2,3,6,7,8,9 HpCDF
Total OCDF
Emission Rate, pg/hr
Run 1 Re
8.09E+05
4.96E+05
3.19E+05
3.61 E+05
1.52E+06
3.50E+06
1.45E+05
8.89E+04
1.06E+05
8.19E+04
6.43E+04
4.86E+05
3.99E+06
5.83E+04
2.89E+04
(1 .67E+04)
(<2.51 E+04)
2.73E+04
1.62E+05
1.52E+06
1.35E+04
(4.71 E+04)
(<2.51 E+04)
(<2.51 E+04)
(<2.51 E+04)
(<2.51 E+04)
(5.98E+03)
5.33E+04
(7.94E+03)
6.43E+04
Run 2
1.32E+06
9.18E+05
7.97E+05
5.32E+05
1.45E+06
5.01 E+06
7.40E+05
6.13E+05
5.29E+05
3.43E+05
9.89E+04
2.32E+06
7.33E+06
7.21 E+04
4.62E+04
(2.67E+04)
(<4.41 E+04)
5.38E+04
2.47E+05
1.45E+06
3.72E+04
(5.31 E+04}
7.22E+04
8.75E+04
7.85E+04
{7.90E+04}
(5.53E+03)
2.35E+05
(1.12E+04)
9.88E+04
Run3
9.89E+05
5.18E+05
2.79E+05
5.09E+05
1.64E+06
3.93E+06
5.82E+05
5.78E+05
5.67E+05
4.08E+05
1.78E+05
2.31 E+06
6.24E+06
6.08E+04
(<4.75E+04)
(3.65E+04)
(<4.75E+04)
(<4.75E+04)
2.27E+05
1.64E+06
8.66E+04
(<4.75E+04)
9.79E+04
9. 11 E+04
7.62E+04
7.78E+04
(6.97E+03)
2.37E+05
4.87E+04
1.78E+05
Process Rate, Mg/hrb
Run 1 RE
Run 2
Run3
Emission Factor, pg/Mgb
Run 1 Re
Run 2
Run3
Average
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.
3-7
-------
Table 3-5. Dioxin/Furan Mill Clay Feed Homolog Results"
Run 1
Analyte 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.)
3 CBI data removed: See confidential version of document.
3-8
-------
Table 3-6. Dioxin/Furan Mill Clay Product Homolog Results"
Run 1
Analyte 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.)
3 CBI data removed: See confidential version of document.
3-9
-------
Table 3-7. Mill Sampling and Stack Parameters
Mill
Run 1 Retest
Run 2
Run 3
Average =
Sampling
Time
(min)
240
240
240
Sample Gas
Volume
(acm)
6.271
3.556
3.666
(dscm)
5.942
3.392
3.471
Moisture
GEMS Analysis a Content
% CO2
0.69
0.69
0.60
0.66
%02
19.8
19.7
19.8
19.8
(%)
b
b
b
b
Average
Stack
Temp.
(°C)
62
63
61
62
Stack
Static
Pressure
(mm Hg)
-0.39
-0.39
-0.39
% Isokinetic
104
105
97.5
NA
Stack
Velocity
(m/min)
990
987
1,077
1,020
Stack
Flow
Rate
(dscm/hr)
29,860
29,940
33,000
30,930
a Percent CO2 and O2 for Runs 1 Retest through 3 were
analyzed by GEMS.
b CBI data removed: See confidential version of document.
3-10
-------
Table 3-8. Summary of Total Dioxin/Furan Results for Dryer Samples
Air Emissions
Total PCDDs/PCDFs
Total PCDDs (pg/dscm)
Total PCDFs (pg/dscm)
Total PCDDs and PCDFs (pg/dscm)
Emission Rates/Factors
Dry Clay Process Rate (Mg/hr)
Material Analyses
Clay Feed3
Total PCDDs and PCDFs (pg/g)
Total 2,3,7,8-TCDD TEQ (pg/g)
Clav Product3
Total PCDDs and PCDFs (pg/g)
Total 2,3,7,8-TCDD TEQ (pg/g)
Run 4 Run 5 Run 6 Averaqe
255 353 370 326
48.4 25.0 5.97 26.5
304 378 376 353
b b b b
b b b b
b b b b
b b b b
b b b b
Clay feed and product concentrations are calculated on a dry basis.
b CBI data removed: See confidential version of document.
3-11
-------
Table 3-9. Dioxin/Furan Homolog Results for Dryer Stack Samples
Analyte
Dioxins (pq/dscrrO
TCDD
PeCDD
HxCDD
HpCDD
OCDD
Total PCDDs (pg/dscm)a
Furans (pq/dscrrO
TCDF
PeCDF
HxCDF
HpCDF
OCDF
Total PCDFs (pg/dscm)a
Total PCDDs and PCDFs (pg/dscm)
Run 4
21.0
17.1
23.7
28.0
165.7
255
11.36
11.83
12.38
9.11
3.78
48.4
304
Run 5
13.0
20.6
28.3
37.2
253.5
353
9.27
7.23
3.99
2.68
1.88
25.0
378
Run 6
18.0
19.4
24.0
32.8
276.4
370
(0.479)
(0.997)
4.42
1.55
1.58
7.55
378
Average
326
27.0
353
3 Non-detect values, designated by parentheses 0, 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.
3-12
-------
Table 3-10. Dioxin/Furan Homolog Emission Factors for Dryer Stack Samples
Homolog
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total OCDD
Total CDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Total OCDF
Total CDF
Total CDD/CDF
2,3,7,8 TCDD
1,2,3,7,8 PeCDD
1,2,3,4,7,8 HxCDD
1,2,3,6,7,8 HxCDD
1,2,3,7,8,9 HxCDD
1,2,3,4,6,7,8 HpCDD
Total OCDD
2,3,7,8 TCDF
1,2,3,7,8 PeCDF
2,3,4,7,8 PeCDF
1,2,3,4,7,8 HxCDF
1,2,3,6,7,8 HxCDF
2,3,4,6,7,8 HxCDF
1,2,3,7,8,9 HxCDF
1,2,3,4,6,7,8 HpCDF
1,2,3,6,7,8,9 HpCDF
Total OCDF
Emission Rate, pg/hr
Run 4
4.40E+05
3.57E+05
4.95E+05
5.85E+05
3.46E+06
5.34E+06
2.37E+05
2.47E+05
2.59E+05
1.90E+05
7.90E+04
1.01E+06
6.35E+06
2.47E+04
2.60E+04
(1 .49E+04)
(<2.13E+04)
5.64E+04
2.51 E+05
3.46E+06
{1 .66E+04}
2.39E+04
3.78E+04
4.04E+04
3.59E+04
3.58E+04
(<2.13E+04)
1.04E+05
2.52E+04
7.90E+04
Run 5
2.68E+05
4.26E+05
5.83E+05
7.68E+05
5.23E+06
7.28E+06
1.91 E+05
1.49E+05
8.24E+04
5.53E+04
3.88E+04
5.17E+05
7.80E+06
{1.87E+04}
2.91 E+04
(1 .64E+04)
3.81 E+04
{6.61 E+04}
3.31 E+05
5.23E+06
2.27E+04
(1.91 E+04)
3.00E+04
{2.71 E+04}
(<2.15E+04)
{2.32E+04}
(4.98E+04)
5.54E+04
(1.19E+04)
(<4.29E+04)
Run 6
3.64E+05
3.91 E+05
4.84E+05
6.62E+05
5.59E+06
7.49E+06
(9.68E+03)
(2.01 E+04)
8.94E+04
3.13E+04
(<4.14E+04)
1.21 E+05
7.61 E+06
2.28E+04
3.07E+04
(1.16E+04)
2.42E+04
5.09E+04
2.67E+05
5.59E+06
(9.68E+04)
(2.10E+04)
(1 .94E+04)
(<2.07E+04)
(<2.07E+04)
(<2.07E+04)
(6.17E+04)
3.13E+04
(5.63E+04)
(4.14E+04)
Process Rate, Mg/hr1"
Run 4
Run 5
Run 6
Emission Factor, pg/Mgb
Run 4
Run 5
Run 6
Average
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.
3-13
-------
Table 3-11. Dioxin/Furan Dryer Clay Feed Homolog Results"
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.)
3 CBI data removed: See confidential version of document.
3-14
-------
Table 3-12. Dioxin/Furan Dryer Clay Product Homolog Results"
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.)
3 CBI data removed: See confidential version of document.
3-15
-------
Table 3-13. Dryer Sampling and Stack Parameters
Sampling Sample Gas Moisture
Time Volume Orsat Analysis a Content
Dryer
Run 4
Run 5
Run 6
Average =
(min) (acm) (dscm) % CO2
240 5.229 4.896 0.3
240 5.073 4.813 0.2
240 5.139 4.885 0.2
0.2
%02
19.7
19.7
19.8
19.7
(%)
b
b
b
b
Average Stack
Stack Static
Temp. Pressure
(°C) (mm Hg)
54.4 -0.11
55.3 -0.11
52.1 -0.11
54
% Iso-
kinetic
96.5
96.0
99.5
NA
Stack
Velocity
(m/min)
1,499
1,476
1,427
1,470
Stack
Flow
Rate
(dscm/hr)
20,900
20,650
20,210
20,590
3 Percent CO2 and O2 for Runs 4 through 6 were
analyzed by Orsat.
b CBI data removed: See confidential version of
document.
3-16
-------
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:
(l)Mill Baghouse
• EPA Method 23 isokinetic sampling train for PCDDs and PCDFs.
• EPA Method 3 A 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
4-1
-------
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 SiC>2.
6. 500 mL Modified Greenburg-Smith containing 200 g silica SiC>2.
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.
4-2
-------
Condantarand
XNJSoibantTrap
Quartz Liner
Tharmocoupto
Quartz NcazJa-
TVp.8
PtotTub*
Tharmocouptes Bypaw
^^^ VaKw
IndMd
Mutomater
M03M4
Figure 4-1 Method 23 Sampling Train for PCDDs and PCDFs
4-3
-------
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.
4-4
-------
Sorbent cartridge
(XAD-2)
Filter
Weigh sorbent cartidge
and subtract weights
from initial weights.
Replace blank-offs,
remove aluminum foil
covering, weigh, cover
with aluminum foil
Remove filter from filter
holder and transfer to
a Container No, 1.
Quantitatively remove
all filter fragments and
particulate matter
remaining in filter holder
and transfer to bottle.
Nozzle, probe liner,
sample transfer line
(if used), bypass or
cyclonefflask
assembly, and
filter holder front
Rinse components
with acetone three
times or more, with
brushing, until
clean. Follow with
additional acetone
rinses in the same
manner.
Filter, support, filter
holder back, 90°
connector, condenser
Rinse components with
acetone three times
or more until clean.
Follow with additional
acetone, but include
three 5-minute soaks
of the 90° connector
and the condenser.
Transfer all rinses
to a tared bottle
(Container No. 2),
then weigh the bottle.
Rinse components
with toluene in the
same manner used
previously with the
additional acetone
rinses in the same
manner, and include
three 5-minute soaks
of the 90° connector
and the condenser.
Transfer all rinses
to a tared bottle
(Container No. 3),
then weigh the bottle.
1st impinger (empty),
2nd & 3rd impingers
(H20), 4th impinger
(empty)-at start of run
5th & 6th
impingers (silica gel)
Measure impinger
contents-weigh
impingers and
subtract weights
from initial weights.
Measure impinger
contents—weigh
impingers and
subtract weights
from initial weights.
Discard contents.
Save contents for
regeneration and reuse.
Figure 4-2. Sample Recovery Scheme
4-5
-------
4.1.1.5 Sampling and Analysis for C02 and 62
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 C>2 at that location. Multi-point, integrated gas bag samples were
collected simultaneously with the traversing/isokinetic sampling for analysis of 62 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 3 A in Appendix A of 40 CFR 60 to sample and analyze for
CC>2 and C>2. 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
CO2
02
Zero-level gas
Zero in nitrogen
Zero gas
Mid-level gas
10% v/v
12% v/v
High-level gas
18% 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
4-6
-------
Urtheated Teflon
Bias Line
Servomex 1440C
CO2 Analyzer
Calibration Gases
Figure 4-3. Instrumental Measurement System for COi and
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.
4-7
-------
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.
Oi analyzer—Located in the sample trailer. Servomex, Model 01440CISTD uses
the principle of Magneto-pneumatic technique to measure the concentration of C>2(%) in
the gas stream. It has measurement ranges of 0% to 25% and 0% to 100%.
COi analyzer—Located in the sample trailer. Servomex, Model 01440CISTD uses
a single beam, dual wavelength IR technique to measure the concentration of CC>2(%) 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
4-8
-------
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 13Ci2 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 uL.
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 high-
resolution 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 (BCSs) has been incorporated into the
method in place of the Laboratory Control Spike. Information on BCSs matrix spiking is
provided in Appendix E. Specifically, Batch Control Spikes
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 CSs was initiated at the same
point as when the XAD cartridges were prepared for sampling.
4-9
-------
SAMPLE PATH
ANALYTICAL PERSPECTIVES
AAP PROJECT No.: P3O73
PROTOCOL: 23
SAMPLE PROCESSING
0 SDS
H Extraction Standards ("
H Alternate Standards "AS"
El Multi-Column Cleanup (ASECS)
0 Final Extract
El Injeaion Standards " JS "
0 HRGC/HBMS
0 12-H Performance Checks
ID Criteria
Interpretation \ 0 Detection Limits
0 Recoveries
SPIKE PROFIL
Ax: ZOO PC (2O HL; O.O1
ES: 4 NG (2O |-IL; O.2 NG/j.1
AS & SS: 4 NG (2O |1L; O.2 NG/|J
JS: 2 NG (1O HL; O.2 NG/p
EXTRACTION:
FRACTIONATION :
ANALYSIS:
CONCENTRATION:
FORTIFICATION:
DATA VALIDATION
SOPS
AP-SP-E
AP-SP-CU
AP-SP-A
AP-SP-N
AP-SP-F
: AP-SP-R
E
L)
L)
L)
QC PROFILE
LMB: ALWAYS REQUIRED
BCS3: ALWAYS REQUIRED
^^
REPORTING PLATFORM
LEVEL: 1 11 III PLATINUJ£-^_
SAMPLE EXTRACTION
SAMPLE ANALYSIS
8A.M.
8P.M.
SPECIAL
REQUIREMENTS
SUPPLIES IDS
SAND _
TOLUENE _
ACID SILICA _
BASE SILICA _
SILICA _
FLORISIL _
HEXANE _
TETRADECANE
Figure 4-4. Schematic of EPA Method 23 and SW846 8290 Emission Samples Analysis Path
4-10
-------
,H
ALTA ANALYTICAL PERSPECTIVES
SAMPLE PATH
AAP PROJECT No: P3O73
PROTOCOL: 23 PCDD/F
Probe Rinse
Ac/MC/Tol
Concentration!
(1/2)
XAD Pre-Spiked
(4 ng PCDD/F SS)
Sampling Modules Prep. Project No.:_
Add PCDD/F ES
Vote''2ft*nL; Cone.: 0.2 ng/nL „
Concentrate & Solvent Exchange
• Add PCDD/F'-AS'•
\oli 20 u L ; Cone.? 0.2
;Vol.: JO {iL ; Q»nc^0»2tig/ \i L
HRGC-" HRMS
M23; FV 2ftuL
(1/2)
Archive
Figure 4-4. Schematic of EPA Method 23 and SW846 8290 Emission Samples Analysis Path (Continued)
4-11
-------
• Consisted of one Batch CSs 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 CSss 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 CSss 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, BCSs Performance Criteria. Details on performance criteria
associated with the BCSs 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.
4-12
-------
SAMPLE PATH
ANALYTICAL PERSPECTIVES
AAP PROJECT No.: P3O14
PROTOCOL: 8290B 71613B SOLIDS
SAMPLE PROCESSING
Extraction \ H EttndiM Stmubrds I "C,, • KDD / F >
3 SlIS
I B Cleanup Stattdoftb " r.v "
Fractionation S3 Multi-column Cleanup (ASECS)
Analysis
i
»^| Interpret
El Injection Standard* "JS
m HRGCiHRMS
12-H Ptrjommnce Checks
0 ID Criteria
Interpretation I g} Detection Limits
SPIKE PROFILE
Ax(829OB): O.2 NG (2O uL; O.01 NO/f-tU
ES (829OB): 2 NG (2O f(L; 0.1 NG/nU
CS (829OB): O.8 NG (2O uL; 0.04 NG/iiL)
JS (8290B): 2 NG (10 ML; O.2 NG/^L)
SOPS
EXTRACTION: AP-CM-S
FRACTIONATION: AP-SP-CU
ANALYSIS: AP-SP-A
CONCENTRATION: AP-SP-N
FORTIFICATION: AP-SP-F
DATA VALIDATION: AP-SP-R
QC PROFILE
LMB:
OPR:
BATCH CS3:
ALWAYS REQUIRED
1613 ONLY; NO BCS3
ALWAYS REQUIRED
SAMPLE EXTRACTION
SAMPLE ANALYSIS
SPECIAL
REQUIREMENTS
SUPPLIES IDs
SAND
TOLUENE
ACID SILICA
BASE SIUCA
SILICA
FLORISIL
HEXANE
CH2CL2
TETRADECANE
HYDROMATRIX
K SILICATE
Figure 4-5. Schematic of Process Samples Analysis Path
4-13
-------
4-14
-------
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 BCSs, 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).
5-1
-------
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 BCSs
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 BCSs 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.
5-2
-------
Table 5-1. Calibration QC Criteria for Sampling Equipment
Parameter
Sampling
nozzle
Dry gas
metering
system —
volume
Dry gas meter
thermocouples
Stack Gas
stream
thermocouple
Final impinger
outlet
temperature
sensor
(thermocouple)
Filter
temperature
sensor
(thermocouple)
Aneroid
barometer
Type S pitot
tube
Calibration technique
Measure 3 diameters
to nearest 0.001 in and
average
measurements
Compare with
calibrated critical
orifices, 40 CFR 60,
Appendix A, Method 5,
Section 16.2
Use field test data to
compute a calibration
check value, EPA
Method ALT-009
Compare to mercury-
in-glass thermometer
Compare to value
generated by dry well
monitored with
potentiometer
thermocouple system
Compare to mercury-
in-glass thermometer
Compare to mercury-
in-glass thermometer
Compare to calibrated
mercury barometer
Measure dimensions
according to 40 CFR
60, Appendix A,
Method 2 for baseline
coefficient of 0.84
Reference
standard
Micrometer
Calibrated
critical orifice
NA
ASTM
thermometer
Hart Model
9100Adry
well
calibration
system
ASTM
thermometer
ASTM
thermometer
Mercury
column
barometer
Micrometer
and angle
finder
Acceptance limit
Difference between high
and low measurements,
< 0.004 in
Difference between
individual calibration factor
values and average value,
< ±0.02
Difference between
calibration check value
must be < ±5% of initial
calibration factor
< ±5.4°F difference from
reference
Difference of < ±1 .5% of
minimum absolute stack
temperature from absolute
reference temperature
(unsaturated gas streams)
< ±2°F difference from
reference
< ±5.4°F difference from
reference
< ±0.1 in Hg difference
from reference
Meets dimensional criteria
specified in Method 2,
Section 6.1 and
Figures 2-2 and 2-3
Frequency
Prior to
sampling
Prior to test
series, and in
the field after
test series
After test series
Before and after
test series
Before and after
test series
Before and after
test series
Before and after
test series
Before and after
test series
Before and after
test series
Criteria
met? (Y/N)
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
5-3
-------
Table 5-2. Criteria for Emission Measurement and Data Quality
Test parameters Matrix
Dioxin/ Furan Method 23 train
samples
Moisture (water Impinger contents
vapor)
Moisture, Gas stream being
Pressure, temp., measured
and velocity
CO2 and O2, by Stack Gas
Orsat
CO2 and O2, by Stack gas
instrument
analyzer on site
Method of determination
Surrogate standards
(spiked in lab during
preparation of XAD for
sampling trains)
Internal standards
BCS3 standards
Laboratory reagent blank
Balance calibration check
with calibration weight
Secondary technical
review of field test data
and equipment
calibration records
relative to EPA
Methods 1-5
Single analysis of
ambient air
Triplicate analysis of test
samples
Analyzer calibration error
check with zero, mid-
range, and high-range
calibration gases
Sampling system bias
check with zero and
either of the upscale
calibration gases
Response time
determination
Zero and calibration drift
tests
Frequency
Each field sample and
blank
Each field sample and
blank
Each analytical batch
One XAD/filter
Prior to initial and final
gravimetric
determinations
Ongoing during testing
Prior to sample analysis
Each sample
After system setup
each day and more
often when needed
After the calibration
error check, during
calibration drift tests
During the initial bias
check each day
Repeat the bias check
after each run or more
often if needed
Accuracy objective
70% to 130% recovery
40 - 130% recovery (tetra-hexa)
25 - 130% rec. (hepta-octa)
80- 120% recovery
Levels less than lowest calibration standard
±0.1g
Validated by meeting posttest equipment
calibration tolerances
98% to 102% (assuming air at 20.9% O2)
NA
< ±2% of span for the difference between
system response and calibration gas value
for any of the calibration gases
< ±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
< ±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
Precision objective
NA
NA
NA
NA
NA
NA
2% RPD
2% RPD
NA
NA
NA
< ±3% of span for
the difference
between final and
initial system.
Objective met? (Y/N)
Yes
see Note
Yes
Yes
RPD<0
weight.
Yes
Yes
Yes
Yes
Yes
Yes
Yes
1
1 % of check
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.
5-4
-------
Table 5-3. Criteria for Assessing Data Quality of Process Sample Analyses
Test
parameters Matrix
Dioxin/ Furan
Raw Feed, and Final Product
Method of
determination
Clean-up standards
Duplicate extraction
and analysis
Laboratory reagent
blank
Frequency
Each sample
One sample
per matrix for
the test
One sample
per matrix for
the test
Accuracy objective
40% to 135%
recovery for all
2,3,7,8-substituted
internal standards
NA
Levels less than
lowest calibration
standard
Precision
objective
NA
25% RPD
for analytes
present
above the
reporting
limit
NA
Objective
met? (Y/N)
Yes
NA
See Note 2.
Yes
Note 2: Duplicate extraction and analysis was not intended to be included in the test plan.
5-5
-------
Table 5-4. Method 23 Internal Standard and Surrogate Standard Recoveries
Analyte
Method Method
blank blank
Run 1 Retest Runs 2-6
Field
blank
train
Mill
Run 1 Retest Run 2
Run 3
Run 4
Dryer
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
13C-1,2,3,7,8-PeCDD
13C-1,2,3,6,7,8-HxCDD
13C-1, 2, 3,4,6,7, 8-HpCDD
13C-1,2-OCDD
13C-2,3,7,8-TCDF
13C-1,2,3,7,8-PeCDF
13C-1,2,3,6,7,8-HxCDF
13C-1,2,3,4,6,7,8-HpCDF
13C-OCDF
106
109
95.6
106
89.2
116
111
90.9
105
79.3
Surrogate Standard % Recoveries: QA objective
3/CI-2,3,7,8-TCDD
13C-1,2,3,4,7,8-HxCDD
13C-2,3,4,7,8-PeCDF
13C-1,2,3,4,7,8-HxCDF
l3C-1,2,3,4,7,8,9-HpCDF
Independent Laboratory
13C-1,2,3,7,8,9-HxCDF
Note 1
Note 1
Note 1
Note 1
Note 1
74.1
75.4
79.2
82.3
79.6
87.2
76.2
76.7
81.7
80.8
70-130%
98.8
101
98.2
102
98.0
82.2
85.8
88.7
88.3
87.7
82.1
86.1
88.4
87.2
88.6
99.1
100
96.7
98.9
97.7
139
143
138
147
133
152
146
132
147
127
75.7
73.4
75.0
75.8
70.3
84.7
87.5
88.6
90.9
90.6
86.2
86.3
88.2
89.6
89.3
97.9
99.7
97.0
98.7
98.1
82.4
82.9
86.9
91.9
90.9
83.9
83.6
84.7
90.3
90.1
102
106
100
104
103
87.0
90.0
92.2
96.3
99.9
87.6
89.1
92.2
95.5
98.9
97.9
99.4
98.9
99.4
97.7
60.8
63.5
64.5
67.6
68.0
62.2
63.7
62.9
66.9
67.4
100
102
102
104
99
51.9
53.8
54.4
57.8
57.4
49.9
52.0
52.3
56.6
56.2
103
102
103
106
104
Check Spike, %: QA objective 40-130%
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.
5-6
-------
Table 5-5. BCSs Surrogate Recoveries
Run 1 Retest
Analyte
Extraction Standard, ES
13C-2,3,7,8-TCDD
13C-1,2,3,7,8-PeCDD
13C-1,2,3,6,7,8-HxCDD
13C-1, 2, 3,4,6,7, 8-HpCDD
13C-OCDD
13C-2,3,7,8-TCDF
13C-1,2,3,7,8-PeCDF
13C-1,2,3,6,7,8-HxCDF
13C-1,2,3,4,6,7,8-HpCDF
13C-OCDF
Surrogate Spike, SS, %:
3'CI-2,3,7,8-TCDD
13C-1,2,3,4,7,8-HxCDD
13C-2,3,4,7,8-PeCDF
13C-1,2,3,4,7,8-HxCDF
13C-1,2,3,4,7,8,9-HpCDF
Alternate Standard, AS,
13C-1,2,3,7,8,9-HxCDF
BCS3A
, %: QA objective 80-120%
100
108
96.8
101
93.4
102
105
110
109
106
QA objective 80-120%
96.6
90.3
101
90.1
94.7
%: QA objective 80-120%
90.4
BCS3B
96.5
109
96
104
101
103
108
107
111
112
97.2
92
100
92.8
93.1
91
Runs
BCS3A
108
108
102
108
109
109
106
102
107
103
86.6
92.6
92.3
89.8
84.9
94.7
2-6
BCS3B
109
107
107
106
107
110
106
100
102
106
88
87.2
92.8
87.2
87.6
92.6
5-7
-------
Table 5-6. Method 8290 Internal Standard Recoveries
Analyte
Clay Feed
Dioxins
13C-TCDD
13C-PeCDD
13C-HxCDD
13C-HxCDD
13C-HxCDD
13C-HpCDD
13C-OCDD
Furans
13C-TCDF
13C-PeCDF
13C-PeCDF
13C-HxCDF
13C-HxCDF
13C-HxCDF
13C-HxCDF
13C-HpCDF
13C-HpCDF
13C-OCDF
Clay Product
Dioxins
13C-TCDD
13C-PeCDD
13C-HxCDD
13C-HxCDD
13C-HxCDD
13C-HpCDD
13C-OCDD
Furans
13C-TCDF
13C-PeCDF
13C-PeCDF
13C-HxCDF
13C-HxCDF
13C-HxCDF
13C-HxCDF
13C-HpCDF
13C-HpCDF
13C-OCDF
Method
blank
90.6
86.2
90.5
89.1
91.4
90.4
85
98.1
86.8
87.1
90.5
89
91.7
90.2
89.6
90.6
84.4
90.6
86.2
90.5
89.1
91.4
90.4
85
98.1
86.8
87.1
90.5
89
91.7
90.2
89.6
90.6
84.4
Run 1
92.3
91.5
84.6
85.8
83.3
82.8
74.2
92.9
90
92.4
95.8
94.7
91.1
92
80.2
85.8
86.2
87.5
86.6
82.5
80.5
81.6
76.5
72.7
91.2
85.4
86.8
90
90.1
87.7
89.7
78.2
80.9
81.5
Mill
Run 2
90.8
87.5
90.6
86.9
89.9
94.5
105
88.1
85.3
87.6
98
98.5
97.2
91.2
86.4
87.2
90.7
89.8
84.8
87.7
89.6
87.2
90.4
97.6
91
86.9
86.3
97.7
103
91.8
89.3
82.5
85.5
87.1
Run 3
92.2
88.4
86.5
84.4
83.9
86.6
98.4
92.7
90
89.3
89.6
91.9
89.3
83.3
82.1
79.5
83.9
92.6
87.9
85.2
83.5
83.3
87.1
100
91
87.4
87.6
86.7
86.9
86.4
85.3
81.6
77.3
81.9
Run 4
97.2
93.5
88.9
87.3
90.4
93.7
136
96.5
97.5
96.5
90.4
94.8
92.9
91.4
84.4
87
91.4
93.3
95.8
94.9
95.2
97.3
105
157
97.4
95.2
97.3
101
102
99.3
97.9
92.4
96.6
101
Dryer
Run 5
101
97.1
92.3
91.5
97
97.1
145
98.6
97.7
101
93.3
94.1
97.2
92.8
85.8
85.6
95.8
102
97.1
98.1
98.1
94.3
80.7
82.2
99.7
96.8
98.9
107
108
109
106
91.7
95.7
94
Run 6
77.4
76.8
73.6
72.9
73
79.2
107
77.4
76.5
77.8
76.5
75.9
76.4
73.2
70
68
75.5
89.7
89.2
81.3
80.2
79.7
76
84.3
97.2
90.1
88.6
92.1
92.7
91.4
89.1
82.9
82.6
87
Recoveries outside of the QA objectives (40% to 135%) are highlighted; see Section 5.2 for further explanation.
5-8
-------
Appendix A
Sample Custody Records
-------
ALTA ANALYTICAL PERSPECT.VES
Sample Log-In Checklist
1 Date Samples Arrived: _-£' -/#-
Client Project:
Time /Date logged in:
AAP Project No.:
(COC). Check as appropriate.
Sampler:
Relinquished by:
Date: Time:
Sample ID:
<\U-
SampleDate.S
Sample Description:
Analysis(es) Requested;
Turnaround Time Requested
Containers Qty:
Type:
Matrix Type
Preservative:
Drinking Water Requiremen
Other Comments
™t and Intact? «f not intact, describe condition below.
diervt Return orRetair
and/or Bottles Requested?
It yes, apply appropriate labe
A-l
-------
0 CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABILITY RECORD
Container (Cooler) No.
I nf
Page _J _ ot
Transfer No
—
Checked by (Initials)/Date
Lock or Seal
_ __ — —
Field Sample Custodian:
A r . Jij-j
i *
Storage Requirements:
3-ice water, < 4°C
D Dry ice
CS Room Temp., < 26 C
Q Other; —
_ _
'll0249. 2. 001. 04
H23 XAD CARTRIDGE
Emission Sample -
^0243. 2. COX. 04
M23 FILTER
Sarnple
I
:/m<
RemarKs:
p X- /.O#?
Remarks:
I Remarks:
RemarKs:
Relinquished By:
[Remarks:
i»* rs=a=^r»f^rPi1lf. r° """
Sample Transfers:
Received By:
"NoTI Reason for Transfer^
its 'i
J
93-4 SEV SUfmwteM 020293
A-2
-------
Storage Requirements:^
water •< 4s® jt% ^
Field Sample Custodian
® CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABILITY RECORD
Dry ice
Room Temp., <26°C
Other: '=?•—>^~ • - <=•
Container (Cooler) No
Page
Transfer No,
Checked by (Initials)/Date
.04
RINSES
Emission Sample - Hall
110249.2.001.04
H23 TOLUEHE QA RINSE
Emission Sample - Mill
Par disposal call -.Hosenf eld
«DWES7PRESEARCH INSTITUTE
Sample Transfers:
Relinquished B
93-» SEV surmwksM 020293
A-3
-------
Alta Analytical Perspectives - Sample Receiving Picture
: .
Project ID: P3265
File: V:\Pictures_Samples\P3265-2JPG
Created: 14 August 2003 10:42 am
A-4
-------
Sample Log-in Checklist
1 Oatft Rumples Arrived: S'ZL3,*ff} ^n'^^\f^fuu^'^\^tt^oMf~f 2
Yes
K3~
No
t Time / Date lagged in- /O:**i" f(~{L3L-O~\ Refrigerator: ^Ho Initials: "Vr—
3. Samples Arrived By: (circle one) Airborne Express ^ Federd Express^ UPS
Freezer Track Company Courier DHL Other
Emery
4, Shipping Preservation- (cirrfa) lea /"Sue k»7 Dry lea / None Temp «C # 3 J ^ /9
^- ' /o' H f
5. Shipping DocumantaUon Present? (circle one) Shipping Label JU/V Jfc 00 £fo<,
Airbill Oracling Number 5 J/* .//££Z*/^. Z,-OO/.O¥
Client Project: '
AAP Prefect No.: T>3pfn
CHAIN OF CUSTODY ANOMALY
Upon receipt of your samples, we found the
following items omitted from the chain-of-custody
(COC}. Check as appropriate.
Sampler: " ~ ~ " ^*Q=J
Relinquished by: ^ j J
Date: Time; 11— J
Sample ID; " ^ILoJ
Sample Description: ^ |j |
^ j=*
•pAnatysis(es) Requesle* ^ tl 1
^Turnaround tims Revested: ^ \\>^L
^ H'"' ''Tii
Corttaineis Qty: "^ 1 \
Type: U
Matrix Type: ^ ^^J
.„ ^, | "" i
Preserw^ive: ^^ 1 1
k. H " •
Drinking Water Requirement ^ 1 |
Other Comments:
-^^^>^jg!^75
"" *-'Z ^9 U"C«/3
Please note these omissions for Mure reference.
A-5
-------
Sample Log-In Checklist
1 Hafo .Qamnloc Arm/Ctrl" /f*^4L "ft"? IftlliftiS- i"*\« ^V-t_V^ ft
*> Time / Date togged in; A>.yf ^-.3i-f)^ Refrigerator: V"4> Inil
3. Samples Arrived By: (circle one) Airborne Express ^Federal Express^ UPS
Freezer Truck Company Courier DHL Other ,
4 Shipping Preservation: (circle) /teej(^aueT^f Dry Ice / None Temo "C & ' f
5. Shipping Documentation Present? (circle one) Shipping Label f J/^ 3 4 Od 5?fl<*
fraj'iJfefio «^9/ ff£/y J&oo S£n
tfAirbilr^ Tracking Number Suy_lLGn.
CHAIN OF CUSTODY AMOMALY
Upon receipt of your samples, we found the
following items omitted from ttte ctiain-ot-cusKxty
(COC). Check as appropriate.
Relinquished by: *" leJ
Dale: Tune: *" B — -1
Sampte Datej - ^|£^i
,...*, \ 1
Sample Description: ^ 1=1
Analysls{es) Requested: ^ LJ
Turnaround Time Requested: 1 i
fc. f— i
Containers Uty- ^^ |^Jlt|
Matrix Typa: ~ ^ H__l
... ^. |=|
h. If™!
Drfciking Water Requirement " ^ | |
Other Commwits:
Ptease note these omissions for ft/ft/re reference.
A-6
-------
SAMPLE CONDITION AT RECEIVING LABORATORY
MRI Project No. 110249.2.001,04
Sample Type; Filters, XAD cartridges, train rinse samples, and field reagent blank samples from emissions
testing
using Method 23 sampling trains.
Target Analytes: PCDD/PCDF by 40 CFRBQ, Appendix A. Method 23 according to project test protocol.
M^-fr^* f) Jt jL „ #/-3kf/A'
Field Sample Condition Infomiatton Documented By _£/ j^CJL^JAMAf^ "ale Q' -^ ( / U
Sample Field Weight (g), Lab Weight (g), Received and
No. or Condition or Condition Comments Checked By
1011
1014
1015
A.S
1017
1018
1019
The purpose of this form is to document the condition and to verify the integrity of samples received by the analytical
laboratory. The Field Laboratory Leader completes the first two columns with sample numbers and final gross field
sample weights of liquid samples or tte condition of other samples as applicable. The analytical laboratory sample
custodian the anaiytica! coordinator, the analyst, or a designee observes all samples received, reweighs liquid
samples that do not have contents level marks or that are suspsct, notes the condition of other samples, and
documents all observations on this form.
A-7
-------
SAMPLE CONDITION AT RECEIVING LABORATORY
MRl Project No, 110249.2.001.04
Sample Type: Filters, XAD cartridges, train rinse samples, and field reagent blank samples from emissions
testing
using Method 23 sampling trains.
Target Anatytes: PCDD/PCDF by 40 CFR 60, Appendix A, Method 23 according to project test protocol.
Field Sample Condition Information Documented By _^_
Sample
No.
~&
Field Weight (g),
or Condition
Lab Weight (g),
or Condition
Comments
Date:
Received and
Checked Bv
Trie purpose of this form is to document (he condition and to verify the integrity of samples received by the analytical
laboratory. The Field Laboratory Leader completes the first two columns with sample numbers and final gross fieid
sample weights of liquid samples or the condition of other samples as applicable. The analytical laboratory sample
custodian, the analytical coordinator, the analyst, or a deslgnee observes all samples received, reweighs liquid
samples that do not have contents level marts or that are suspect, notes the condition of other samples, and
documents all observations on this form.
A-8
-------
SAMPLE CONDITION AT RECEIVING LABORATORY
MRI Project No, 110249,2,001.04
Sample Type: Filters, XAD cartridges, train rinse samples, and field reagent blank samples from emissions
testing "
using Method 23 sampling trains.
Target Analytes: PCDD/PCDF by 40 CFR 60, Appendix A, Method 23 according to project test protocol .
: ?/ ?-( /
Re
*
if
Field Sample Condition Information Documented 8y jxy~*&*s~- pgte:
Sample Field Weight (g), Lab Weight (g), Received and
No. or Condition or Condition * Comments _ Checked By
4001 (o/V. 6
4002
4003
4004
4005
4007
4008
4009
4010
5001
5002
5003
5004
5005
5007
S008
5009*
5010
6001
6002
6003
6004
.SBQ6
6007
6008
6009
6010
The purpose of this form is to document the condition and to verify the integrity of samples received by the analytical
laboratory. The Field Laboratory Leader completes the first Iwo columns with sample numbers and final gross field
sample weights of liquid samples or the condition of other samples as applicable. The analytical laboratory sample
custodian, the analytical coordinator, the analyst, or a designee observes all samples received, reweighs liquid
samples that do not have contents level marks or that are suspect, notes the condition of other samples, and
documents all observations on this form.
A-9
-------
SAMPLE ID
TRAP ID
DATE SAMPLED
FILTER
XAD
<&MC
TOLUENE
ACE/MC
BACK HALF
RINSE
TOLUENE
BACK HALF
RINSE
IMPINGER
CATCH
NOTES &
OBSERVATIONS
»o.s-e^M*
**«*, -003
•zovv^a*
7
S
y
/
/X^^e^f*
*
•Z-Ooq
^^>\Lt(t -OO 1
I«f*0&o3
/
/
/
/
30C,.,
"^S>\(j>if —ocA
IS fto&d>3
'
'
/
•
^o^4
?3(u.(, - o/?
fT/»L>
-------
SAMPLE ID
TRAP 10
DATE SAMPLED
ACE/MC
BACK HALF
RINSE
TOLUENE
BACK HALF
RINSE
IMPINGER
CATCH
NOTES &
OBSERVATIONS
A-ll
-------
3 CHAIN OF CUS
D SAMPLE TRAC
Container (Cooler
Page / of 1
C
Lock or Seal
\ 110249,2.001.
j M23 XAD CARTi
i HNS ft'Q€?fs "t HX&nl
TODY RECORD
EAB1LITY RECORD
)No, &LI
Transfer No.
locked by (Initials)/Date
Intact (Yes or No)/Time
04 i O J_ 5
(Ifipfi #^/^T<»5
f 110249,2.OO1.O4 J.OJ.1
: M23 ACETONE -f ' ^ffljL
. Roa-oe-nt Blank -'Samples
110249,2.001.
M23 TOLUENE -j
fteagei^t Blank
11O249, 2.OO1.
M23 FILTER
' Reagent Blank
For disposal
•MIDWEST RESEA
\
O4 JL O J. 3
Samples
04 j. O J. 4
Samples
call : Hosenf eld
RCH INSTITUTE
\.
\
\
I
Relinquished By:
jLJ&^Ajv*.
sQ.jU
<;
^
^^_
^
\
\
\
Received By:
^P.^^vt
F^P&X
^J^X2_j^^
Field Sample Custodian:
n- S«iA^ut/T
/
j04 $/gj
Cd
*/
Storage Requirements:
S Ice water, < 4°C
D Dry ice
CI Room Temp,, 5 26°C
C& Other: £i.i/a~ ,c.s~
Ramams:
IS
Ftemants: ^ 0^^ *,
S\^ J ftf\ CM A_ . *
SUV IV- /^ Jf^^^r*.** t^maS /S^ru= ^y»» *»«
""^•^M^* /^^rZ^'*<^rJ'"<2J* ,!£,"££
f>^
RemarKs.
Remarks:
HemarKs:
Rsmartts:
RerrwVs:
Remartis
Remsrtcs:
Sample Transfers: ^ /'°^9/^J^ ^f'5"5
^ Date Time No,
o9/zi f°3 oBo~j (Vj
oefa/rf ~>n*t <£>
VtiA.n to'v^ 3
4
Reason for Transfer;
•^t^rSx.^^rr^
///, ^i^.-
«
93-4 SEV Blim wXshl 020ZS3
A-12
-------
0 CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABILITY RECORD
Container (Cooler) No. XAft - \
Of L_ Transfer No.
Checked by (!nitials)/Dale
Lock or Sea! Intact (Yes or Noyifme
',
*
I. 2.001. O-
M23 XAD CARTRIDGE #£_
Emission Sample - Mill
110249.2.001.04 C3OOS
H23 XAD CARTRIDGE
Emission Sample -
110249.2.001.04
M23 XAD CARTRIDGE
Emission Sample - Dryer
110249. 2.O01.04' "
M23 XAD CARTRIDGE
Emission Sample -
'11O249.2.001.04
M23 XAD CARTRIDGE #£2/64-
Emiesion Sample - Dryer
For dispoeal calliHossnfeld
MIDWEST RESEARCH INSTITUTE
Field Sample Custodian:
A
Storage Requirements:
£3 Ice water, s 48C
CD Dry Ice
D Room Temp,. < 26°C
CS Other: '
Memories:
SOO4S
Dryer
GOO4
Rtmarks
Renwrts:
Ramarte:
Hamarks:
Re.Tiarto:
Ftontartts:
Remark*:
Sample Transfers:
Relinquished By:
Received By:
Date
Time
No.
Reason for Transfer:
ffffO-f
93-4 SEV sutmwksM 02O293
A-13
-------
0 CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABiLITY RECORD
Container (Cooler) No. J^. If&rJ
Page ' of ] Transfer No.
Checked by (Inltla!s)/Date
Lock or Seal Irrtacl (Yes or No)/Time
110249.2.001^04 2OO"7
M23 FILTER
Emission Sample - Kill
11O249. 2.O01. O4 3OO"7^
M23 FILTER
Emission Sample - Mill
110249.2.001.04 tt.OO2'
M23 FILTER
Emission Sample - Dryer
110249.2.001.04 SOO2"
M23 FILTER
Emission Sample - Dryer
ilQ249.2.OOi.04 SOO2
M23 FILTER
Emission Sample - Dryer
' For diaposal call sHoaenfeld
X
^
^
^e^
^
^
^^
Relinquished By; Received By:
/£ sCkl ^/4&%/V2*' '& -/,&6-»^>i
fy sSfiL(t*£c' f^ti 9&x
Field Sample Custodian:
/f. Sisu/cduLO"
/••
f8K9jzi
(?J
i/
Remarks:
IS
Remarks,
if
Storage Requirements:
0* Ice waler, < 4°C
O Dry ice
D Room Temp., s 26°C
O Other: f^^if lfr* —
nomartts:
\s
RemarKs
} ^ |
Remarks:
•R«marKs:
RamarXs:
Remi'te:
J
1
RemaiXs;
Remarks:
fwrnarks:
Sample Transfers:
Date Time No.
^,/^5 ^^ <^
&{^,(|6^ ~n6« (^
1-JJ-O? ^5j
\£fa+* 3
4
Reason for Transfer:
^^^ ^ ^e
JH>S<>£^
93-4 SEV tumwksni 020293
A-14
-------
>S CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABILITY RECORD
Container (Cooler) isiQ.flw.5a^"**~
Page / of Transfer No.
Checked by (Initials)/Date
Lock or Seal Irrtact (Yes or NoVTime
04 S20OS
RINSES
Emission Sample - Mill
110249. 2.O01. 04 SOJ.O
K23 TOLUENE OA RINSE
_ Emission Sample - Mill
1102*49,2, ooi .04 3 o o ex
M 'tO^afiHMifiBsLCGL.f t>TUtCC"C
ttjC+j v ivuiu t fntoF ft j. n szc.z>
Emission Sample - Mill
110249. 2. OO1.O4 3OJLO
M23 TOLUENE QA RINSE
Emission Sample - Mill
11O249.2.OO1.O4
M23 FRONT-HAW*
Field Sample Custodian:
Storage Requirements
SI ice water, < 4°C
CD Dry ice
O Room Temp., s26eC
@ Other:
ff
Ramarks:
Remarks:
Emission Sample - Dryer
110249.2.001.04 /J.OOS\
M23 TOLUENE QA RINSE
__Emission Sample - Dryer
116249.2.001.04 soo
u^3 ^Trimn^ntiMT RINSES
, Emission Sample - Dryer
11O249.2. OO1.04
M23 TOLUENE QA RINSE
Emission Sample - Dryer
"1102.49.
M23
Renurks:
1,00
ct
iN ^ I
(RsmarKs:
SOOS
Ramarts:
1.O4
+UF RINSES
•yer __ |_
"eooiT
Emission Sample - Dryer
11O249.2.O01.O4
M23 TOLUENE QA RINSE
Emission Sample - Dryer
For disposal call:Hosenfeld
MIDWEST RESEARCH INSTITUTE
"•-"
/Remarks:
f*
Remarttj:
SamplaTrans«arS:
Relinquished By:
Received By:
Date
Time
No.
Reason for Transfer:
ft
rvv,
93-4 SEV sumtwteM 020293
A-15
-------
0 CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABIUTY RECORD
, ., ,-f/i.R/ 1
C t ' r (Cooler) Nn A^ft*-'
Paae / of_J_ Transfer No.
Checked by (lnitials)/Date
Lock or Sea! intact (Yes or No)/Time
11O249.2.O01.04 ^ O 1 J.
M23 ACETONE
Reagent Blank Samples
110249.2.001.04 2OJ.C3
M23 TOLUENE
Reagent Blank Samples _^
110249.2. OO1. O4 Z2O 1 -Q
M23 FILTER
Reagent Blank Samples
110249.2. 001. 04 "=2Q:L~?
M23 XAD CARTRIDGE #£3L*-'°e'5
Reagent Blank Samples
110249.2.001.04 2 O JL S
M23 MILLI-Q WATER
Reagent Blank Samples
For disposal call :Hoeen£ eld
NMIDWEST RESEARCH INSTITUTE
\-
V
\
\
\£)
X
^v^
^
\v
Relinquished By: Received By:
ff &3*Jb^. ^ A^/
^- /JM^/ U J^o^li^
Field Sample Custodian:
'i • O CL^*»^L ' ""
/
\;
^L
i/
Storage Requirements:
CD Ice water, < 4°C
ED Dry ice
C§ Ffbom Temp., < 26°C
D Other:
"*
RomarKs:
\J
iS
Remarks:
V
7
Remarks;
V
V
/
Remarks:
~\
V*
Rsmarks:
Remarks:
Remarks:
Remarks:
Remarks:
Remarks:
Remarks:
Sample Transfers:
Date Time
£/2i/o% 07Sd
QfoS/ffr lO'oO
No.
1
2
3
4
Reason for Transfer:
^v^x^TJ-/^/^
93-» SEV sumiwksM 020293
A-16
-------
JZJ CHAIN OF CUSTODY RECORD
D SAMPLE TRACEABILITY RECORD
Container (Cooler No. Aftv**- I
Page / Of >*• 6fe^,/ Transfer No.
Checked by (InitialsyDate
Lock or Seal Intact (Yes or NoXTime
(Sample Container Label)
/?//
//z/
,£///
Xiu
Sit/
3/2./
<^Z~li
^£V
S'Zn
^C*& *7 f
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Relinquished By: Received By:
/K . | w-N** <£)f&£k*~^
J^J, d$r*6\ /?£D£X,
8/*i/L-Ot /-2,
Storage Requirements:
§lce water, < 4°C
Dry ice
D Room Temp., < 26°C
B) Other: &L-*t&~ i e iT
Reason for Transfer:
SrV^^V^,^*
£u*rmi_
93-4 SEV surmwKsri! 020203
A-17
-------
El CHAIN OF CUSTODY RECORD
Q SAMPLE TRACEABIUTY RECORD
^
Page ^- Of ^- Transfer No.
Checked by (Initials)/Date
Lock or Seal Intact (Yes or No)/rime
(Sample Container UtMlt
63LH
(# 2.71-^
Relinquished By: Received By:
nA> it>***~^ &< <&ttH~*^~
'$:v.s" 3
4
Storage Requirements:
ClJ Ice water, s 4°C
d Dry ice
D Room Temp., < 26°C
S) Other: &L,vr~ tc-
-------
Alta Analytical Perspectives - Sample Receiving Picture
Project ID: P3290
File: V:\Pictures_Samples\P3290-1 JPG
Created: 22 August 2003 3:18 pm
A-19
-------
Alta Analytical Perspectives - Sample Receiving Picture
Project ID: P3289
File: V:\Pictures_Samples\P3289-1 .JPG
Created: 22 August 2003 2:19 pm
A-20
-------
Appendix B
Sampling Data and Field Analytical Records
-------
Appendix B-1
Emissions Sample Collection
-------
3roject Nc
Run No.
Plant
Sampling
Operator^
Barometric
Site to Ba
Corrected
Pilot No.
VELOCITY TRAVERSE DATA ^
f^ t Date ^'l\-fr^
_oca^on
;) H^tf^
^4i|_//M, / 1?M'?/ **"
4.wX7X3l*t1 .
; Pressure, in. tfg" r 'W 4T
8
•ometer Elevation "^f1 ft. |~^
Barometric Pressure
T/C No.
Stack Area, sq.ft.
Pilot Cp
Temp. M(
sterNo. ^ ^9/7
/
n f
H
i
r J
Static Pressure, in. H,O
Assumed Moisture,
Assumed %C02
%
Assumed %O^
nitial Pilot Leak Check j~44*>
Final Pilot Leak Check £>t2Ard
Comments:
TRAVERSE
POINT
NUMBER
£• i
fT i
J
J
y
^f
\\
ft
h
rf
f
ft
ifr
i
7
f
J
^
VELOCITY
HEAD, ip
in. H20
'?br
/ ^fc>
/.^^
/ * r
• * f\7
/ £r>
/•?**
/ ?-&
/ 9k,
/fa
fyo
K
/.9^
/ ^
' °&
Z-O
L.ti
1.,&
J7->G
1^0
/
STACK
TEMP.
f !*{"*' <^
/& f*} ^
r
/^/,ir
I?1' f
*3LL
/3/.tS
£?2 /
/, /-
i ••* f ^ ^
f5i 1s
_/'5/,y
£l>/^
rtj./.
/1//7
foi'i
ty\,i~
n>i, i
rtj, j
ROTATION
ANGLE
a
r 5C>*
-f^
+ r
~4-f-/
O
-*?
—¥
—&
-is
-i
~£
-7
-5
•~7
. ^
-r/.
/, ^
Start Time
TRAVERSE
POINT
NUMBER
&-/
P A
^
H
y
6
7
/
9
{&
/I
n.
/"5
/f
y^
/Is
/7
/^
tf
U-
Traverse Point Layout
'" End Time l't*o
VELOCITY
HEAD.AP
in. HjO
fi.76
°-7?
/<^?
I'L
_Z±2
r
/
7
?
A 5^
/*&
f
1
f-ti-tj
f-^5
5
AY 6
/. ?^r
2
,0
2.cJ
•^'^
"2^
STACK
TEMP.
ffl-i
( J^-i
nt.o
(3i-i
[3(,G
/?d,9
/ 3/'C2>
0 ,(
c^l,^
\ 3 1,9
1 3Z.7
UZ i
l"Jt.o
t3i-~7
/3/'£
nz,i
132,5
/T?-7
ni> /
/"?3,.2-
Vj
ROTATION
ANGLE
a
- ^
4 5
f T
~^7
-4 d,
^c-
O
O
o
-f-/
-2_
rjjt,. F
-y
-2-
-"^
-Z-
t_y
f j/
r-2»
1 93^ SEV surtrm 020JS3
Bl-1
-------
VELOCITY TRAVERSE DATA
Project No.
Run No.
Plant
Sampling Location
Operator(s) _
Barometric Pressure, lh. Hg
Site to Barometer Elevation "W
Corrected Barometric Pressure
Pitot No. Pitot Cp
T/C No. Temp. Meter No.
Stack Area, sq.ft.
Static Pressure, in. H2O
Assumed Moisture, %
Assumed %CO,
ft.
Initial Pitot Leak Check
Final Pitot Leak Check
Comments:
Assumed %O2
t
6 Tf
37
Traverse Point Layout
Start Time
End Time
TRAVERSE
POINT
NUMBER
A
H
VELOCITY
HEAD, ip
in. HaO
-tld-
li
STACK
TEMP.
M-
4*41
4HL
ROTATION
ANGLE
a
*
ii
TRAVERSE
POINT
NUMBER
VELOCITY
HEAD.^p
in. HjO
STACK
TEMP,
t
tit
^X
&L
ROTATION
ANGLE
a.
r
2-
$
93-3 SP/ sutlrm C2039J
Bl-2
-------
Emission Measurements Data Summary
Measurement Equipment Information and Leak Check Data
PCDD/PCDF
Project no. 110249,2,001.05
Client EPA/ESD/RTI
Facility CBI
Source tested Mill|lk
Emission measurement location Stack Outlet
Test run no. 1 -Retest Test run date(s) August 13, 2003
Sampling train no. M23-1 Run start time 05:30 AM
Operators) Dave Griffin Run stop time 10:48 AM
Measurement Equipment Identification and Specifications
Metering console no. N7
Dry gas meter (DGM) calibration factor (Y) 1.002
Orifice meter factor (AH@) 1.794 in. H2O
DGM calibration factor (Y,,) from sampling data 1,029
Comparison of Y,, to Y (must be within ±6% of Y) within ±5%
Temperature controller* no. N/A
Temperature meter* no. N/A
Additional thermocouple no. N/A
Sample transfer line no. N/A
Umbilical cable no(s). N-16-2
Sample box no. 10288
Impinger outlet connector no. U H-1
Filter no(s). 23-1 RE
Probe no. 3-2
Effective probe length 3.0 feet
Probe liner Heated glass tubing
Gas stream temperature thermocouple no, 36-2
Pilot tube no. M-126
Pitot tube coefficient 0.840
Sampling nozzle no. N7
Sampling nozzle type Nichol button-hook
Sampling nozzle inside diameter at Inlet tip 0 249 inches
Barometer no, X-4029
Altitude difference from emission measurement location
to barometer or reference point at the test site -29 feet
Altitude difference from metering console location
to barometer or reference point at the test site -20 feet
" Not part of console; or used with peripheral equipment.
Sampling Train Leak Check Data
Gas stream pressure
measurement system -
Leak check from pilot tube tip
0.91 m
6.32 mm
-8.8 m
-6,1 m
Time
Initial 05:20 AM
Final 10:55 AM
Result
Pass
PASS
Sampling system -
Leak check from nozzle
Time
Initial 05:30 AM
Final 07:35 AM
Initial 08:00 AM
Final 09:40 AM
Initial 09:50 AM
Final 10:00 AM
Initial 10:05 AM
Final 10:55 AM
Pump
Vacuum,
in. Ha
15.0
20.0
15,0
21.0
15.0
21,0
15.0
21.0
Leak
Rate,
dcftn
0.003
0.001
0.002
0.001
0,003
0,001
0.002
0.001
Nomoreptxls 10/31/2001 (rev.M5FinaiDataReport.xls [ReportA] 8/26/2003 2:12 PM)
-------
Emission Measurements Data Summary
Source and Sampling Data
PCDD/PCDF
Project no. 110249,2.001.05
Client EPA/ESD/RTI
Facility CBI
Source tested'
Emission measurement location Stack Outlet
Test run no. 1-Retest
Sampling train no. M23-1
Total sampling time 240.00 minutes
Test run date(s) August 13, 2003
Run start time 05:30 AM
Run stop time 10:48 AM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric flow rate at dry standard conditions
Volumetric flow rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
17,574 dscfm
1,054,451 dscf/hf
19,856 scfm
68 °F and
22,957 acfm
1,377 ,390 acf/hr
54.13 ft./sec.
3,248 ft./min.
0.9104 (in. H?0f J
0.829 in. H20
603.1 °R
143.4 *F
29.58 in. Hg
0.00 in. HsO
29.58 in. Bg
N/A in. Hg
11.49 % by volume
29.74 Ib/lb-mole
31 .27 Ib/ib-mole
19.5 % by volume
0.5 % by volume
% by volume
497.65 dscm/min.
29,858.7 dscm/hr
552.26 scm/min.
760 mm Hg
650.06 acm/min.
39,003.4 acm/hr
16.498 m/sec.
989.9 m/min.
4.588 (mm H2or
21,05 mm hfc,0
335,1 K
61 .9 °C
751 3mm Hg
0.0 mm HjO
751.3 mm Hg
N/A mm Hg
11.49 % by voiume
29.74 g/g-mole
31.27 g/g-mole
19.5 % by volume
0.5 % by volume
% by volume
at Emission Measurement Location
Stack or duct type Circular
First diameter 36.000 inches 0.9144m
Second diameter 36.000 inches 0.9144m
Gas stream cross-sectional area 7 0686 ft.2 0.656S9 mz
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 209.840 dscf
Gas sample volume as read on dry gas meter 221 453 ft.3
Volume correction for failed leak checks 0 000 ft."
Gas sample volume corrected for leakage 221 453 ft.3
Absolute dry gas meter temperature 555.7 "R
Dry gas meter temperature 96.0 *F
Absolute dry gas meter pressure 29,80 in. Hg
Orifice meter differential pressure (AH) 2.977 in H2O
Barometric pressure at start of run 29,59 in. Hg
Barometric pressure at end of run N/A in. Hg
Condensate collected in sampling train 577.8 grams
Isokinetic sampling variation 103.99 %
5.9420 dscm
6.2709 m5
0.0000 m*
6.2709 m»
308.7 K
35.6 °C
756.9 mm Hg
75.63 mm B,O
751.6 mm Hg
N/A mm Hg
577.8 grams
Other Supporting Data
Barometric pressure at test site at start of run 29.61 in. Hg 752.1 mm Hg
Barometric pressure at test site at end of run N/A in. Hg N/A mm Hg
Cross-sectional area of sampling nozzle inlet 3.382E-04 ft.' 3.142E-05 m2
Pltot tube coefficient 0.840
Dry gas meter calibration factor (Y)
Dry gas meter calibration factor (Yqa) from sampling data
Comparison of Y,,, to Y (difference must be within ±5% of Y)
Orifice meter factor (AH@)
Potential moisture (as water vapor) content based on condensate collected
Potential moisture {as water vapor) content based on gas stream parameters
1.002
1.029
within ±5%
1.794 in. H2O
11.49 % by volume
N/A % by volume
Nomorept.xls 10/31/2001 (rev. M5 Final Data Report.xls [Reports] 8/26/2003 2:12 PM)
Bl-4
-------
Test Run Field Data Sheet - PCDD/PCDF
Projectno. 110249.2.001.05 Emission measurement location: StackOutlel
Test run no. 1-Retest Date(s): August 13, 2003 Train no. M23-1 Page 1 of 2
Traverse
Pol-Point
Number
A1
A2
A3
A4
A5
A6
A7
A8
A9
A10
A11
A12
A13
A14
A1S
A16
A17
A18
A18
A18
B1
82
B3
B4
B5
B6
B7
B8
B9
BIO
B11
B12
Clock
Tirre
24-hr
5:36:00
5:42:00
5:48:00
5:54:00
6:00:00
6:06:00
6:12:00
6:18:00
6:24:00
6:30:00
6:36:00
6:42:00
6:48:00
6:54:00
7:00:00
7:06:00
7:12:00
7:18:00
7:24:00
7:30:00
8:00:00
8:06:00
8:12:00
8:18:00
8:24:00
8:30:00
8:36:00
8:42:00
8:48:00
8:54:00
9:00:00
9:06:00
9:12:00
Cumuiative
Sampiing
Time.
minutes
C\ f¥l
6.00
12.00
18.00
24.00
30.00
36,00
42.00
48.00
54.00
60,00
66.00
72,00
78,00
84,00
90.00
96,00
102.00
108.00
11400
120.00
120.00
126.00
132.00
138.00
144.00
150.00
156.00
162.00
168.00
174.00
180.00
186.00
192.00
Dry Gas Meter Reading.
(VJ.
ft'
Desired
843.689
848.099
852.641
857.401
862.367
867.351
872.570
877.543
882.487
887.212
892.641
898.310
904,598
911,322
918,046
924.770
931 .499
938.228
944.963
951 .693
955.299
959.539
964.354
969.501
974.271
978.968
983.833
988.887
993.559
998.702
1,004.135
1,010.003
Actual
843.480
848.000
852.820
857.600
862.470
867.450
872.700
877.850
882.990
888.050
893.370
898.950
904.900
91 1 .260
917.710
924.200
930.700
937.200
943.700
950.200
950.564
953.900
957.970
962.950
968.210
973.330
978.460
983.630
988.800
993 970
999.220
1 ,004.730
1 ,01 0.700
Orifice Pressure
Differential
;\H) mcleiHjO
Oared
1.734
1.676
1.774
1.938
2.101
2.108
2.303
2.087
2056
1.875
2.469
2.686
3.300
3763
3.760
3,758
3.764
3.761
3.767
3.761
0.884
1.510
1.945
2205
1.895
1 835
1,964
2121
1.810
2,188
2,442
2.851
Acft.al
1.800
1.800
1.900
2.100
2.100
2,200
2,400
2.300
2.300
2.100
2.500
2,700
3,300
3,600
3.600
3,700
3.700
3700
3700
3700
1.000
1.700
2200
2500
2.200
2.200
2.200
2.300
2.200
2300
2.700
3.100
Velocity
Head,
-
135
136
136
136
136
136
136
137
139
138
139
141
143
144
145
146
145
146
145
146
145
145
146
146
146
146
146
146
146
147
146
146
Dry Gas Meter
Temcerature
C.J, "F
Inlet
77
80
82
86
89
91
93
95
97
98
98
100
100
101
101
101
101
101
101
101
94
94
96
100
101
102
103
103
104
105
105
105
Outlet
77
78
79
81
82
84
86
87
89
90
91
92
93
94
95
96
96
97
97
97
94
94
93
95
95
96
97
97
98
99
99
100
Pump
Vacuum,
n Hg
8.0
11.0
12.0
12.0
12.0
12.0
13,0
13,0
13,0
120
13,0
14.0
1B.O
19.0
20.0
200
20.0
20.0
20.0
20.0
7.0
10.0
13.0
15.0
14.0
14.0
14.0
14.0
14.0
14.0
16.0
18.0
Irrpinger
Outlet
letp
F
58
53
53
55
57
54
53
53
53
52
52
52
54
57
58
56
54
54
54
54
65
43
44
50
53
55
56
55
55
55
55
52
Probe
Outlet
Tenp
F
248
252
253
248
249
251
250
248
252
248
249
248
252
251
249
252
251
251
248
250
252
251
249
253
249
252
249
252
252
248
253
252
Fitter
Holder
T-rp
F
260
259
258
257
257
257
257
256
255
257
258
257
257
257
257
256
257
257
257
257
259
261
260
258
258
257
257
257
257
257
257
257
XAC
Inlet
'F
44
42
42
42
43
43
44
44
44
43
44
I 44
45
46
47
48
50
52
50
49
59
50
47
46
46
46
46
47
47
47
48
48
STL
Cutlet
Tpfip
F
Isokmetic
Sampling
Variation,
percent
1000
107.6
111.4
105.4
102.9
104.8
105.6
108.7
109.1
112.3
102.8
103,3
99.3
99.3
100,6
101,3
101 4
101.4
101.3
101.4
107.9
100.7
108.5
107.4
112.7
114.6
111.5
107.3
116.1
107.1
106.4
106.7
Remarks: Note: Any DGM reading above that is flagged with an asterisk was not taken at the precise time. Operator(s): Dave Griffin
Sigr-atu re/Date
Nornorept.xls 10/31/2001 (rev.M5FinalDataReport.xls (Datasheet] 8/26/2003 2:12 PM)
Bl-5
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 1 10249.2.001
Test run no. 1-Retest
Traverse
Port-Point
Number
B13
B14
B15
B16
B17
B18
B18
818
Clock
Time
21-hr
9:18:00
9:24:00
9:30:00
9:36:00
9:54:00
9:55:00
10:25:00
10:30:00
10:36:00
10:42:00
10:48:00
05 Emission measurement location: Stack Outlet
Date(s): August 13, 2003 Train no. M23-1 Page 2 of 2
Cumulative
Sampling
Time.
mffiules
198.00
204.00
210.00
216.00
216.00
217.00
217.00
222.00
228.00
234.00
240.00
Dry Gas Meter Seating,
(VJ,
ft"
Desired
1,015.885
1 ,022.384
1,029.161
1 ,035.943
1 ,037,406
1 ,043.787
1 ,050.747
1,057.163
1 ,063.872
Actoal
1,016.670
1 ,022.900
1,029.120
1,035.293
1 ,035 592
1 ,036.700
1 ,037.247
1 ,042.530
1 ,048.950
1 ,055.420
1 ,061 874
Orifice Pressure
Differential
(AH), inches H3O
Desired
2.854
3.480
3.781
3.787
4.068
4.068
4.047
3.438
3.745
Actual
3.200
3.400
3.400
3.400
3.400
3.800
3.700
3.700
3.700
Valocty
Head.
(ap)
inches H,O
0.900
1 100
1.200
1.200
1 300
1.300
1 300
1 100
1 200
Gas
Stream
Temp
-------
Emission Measurements Data Summary
Measurement Equipment information and Leak Check Data
PCDD/PCDF
Project no. 1102492.00105
Client EPA/ESD/RTI
Facility CBI
Source tested Mill 0V
Emission measurement location Stack Outlet
Test run no. 2
Sampling train no. M23-2
Operatods| Dave Griffin
•Sk.
SjU*
Test run date(s) August 14, 2003
Run start time 05:50 AM
Run stop time 10:05 AM
Signature/Date
Measurement Equipment Identification and Specifications
Metering console no. N7
Dry gas meter (DGM) calibration factor (Y) 1.002
Orifice meter factor (AH@) 1.794 in. H30
DGM calibration factor (¥qa) from sampling data 1.002
Comparison of ¥<,, to Y (must be within 15% of Y) within ±5%
Temperature controller* no. N/A
Temperature meter* no. N/A
Additional thermocouple no. N/A
Sample transfer line no. N/A
Umbilical cable no(s). N-16-2
Sample box no. 012003
Impinger outlet connector no. UH-12
Filter no(s). 23-2
Probe no. 3-2
Effective probe length 3.0 feet
Probe liner Heated glass tubing
Gas stream temperature thermocouple no. 36-2
Pilot tube no. M-126
Pilot tube coefficient 0 340
Sampling nozzle no. N12
Sampling nozzle type Nichol button-hook
Sampling nozzle inside diameter at inlet tip 0.187 inches
Barometer no. X-4029
Altitude difference from emission measurement location
to barometer or reference point at the test site -29 feet
Altitude difference from metering console location
to barometer or reference point at the test site -20 feet
* Not part of console; or used with peripheral equipment.
Sampling Train Leak Check Data
0.91 m
4.75 mm
-8.8m
-6.1 m
Gas stream pressure
measurement system -
Leak check from oitot tube tip
Time Result
Initial 05:25 AM Pass
Final 10:07 AM PASS
Sampling system -
Leak check from nozzle
Pump
Vacuum,
Time in. Hq
Initial 05:30 AM 15.0
Initial 07:53 AM
9.0
Leak
Rate,
dcfm
0.001
0.001
Initial 07:57 AM 15.0 0.001
Initial 10:08 AM 9.0 0.006
Nomoreptxls 10/31/2001 (rev. MS Final Data Report.xls [ReportA] 8/26/2003 2:09 PM)
Bl-7
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Emission Measurements Data Summary
Source and Sampling Data
Project no.
Client
Facility
Facility location
Source tested
Emission measurement location
Test run no.
PCDD/PCDF
110249.2.001.05
EPA/ESD/RTI
CBI
Mill!
Stack Outlet
2
Sampling train no. M23-2
Total sampling time 240.00 minutes
Test run date(s) August 14, 2003
Run start time 05:50 AM
Run stop time 10:05 AM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric flow rate at dry standard conditions
Volumetric flow rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
17,620 dscfm
1,057,1 89 dscf/hr
19,900 scfm
68 °F and
22,899 acfm
1,373,919 acf/hr
53.99 fl./sec.
3,239 ft./min.
0.9103 (in. HjO)0"
0.829 in. H20
605.7 °R
146.1 °F
29.85 in. Hg
0.00 in. HaO
29.85 in. Hg
N/A in. Hg
1 1 .46 % by volume
29.75 Ib/lb-mole
31 .27 Ib/lb-mole
19,5 % by volume
0,5 % by volume
% by volume
498 94 dscm/min
29,936.3 dscm/hr
563.52 scm/min.
760 mm Hg
648.42 acm/min.
38,905.0 acm/hr
16.457 m/sec.
987.4 m/min.
4.588 (mm H20]T
21.05 mm HjO
336.5 K
63.4 "C
758.2 mm Hg
0.0 mm Hf>
758.2 mm Hg
N/A mm Hg
1 1 .46 % by volume
29.75 g/g-mole
31 .27 g/g-mole
19.5 % by volume
0.5 % by volume
% by volume
at Emission Measurement Location
Stack or duct type Circular
First diameter 36.000 inches 0.9144m
Second diameter 36.000 inches 09144m
Gas stream cross-sectional area 7.0686 ft.' 0.65669 m3
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 1 19.788 dscf
Gas sample volume as read on dry gas meter 125.574 ft.3
Volume correction for failed leak checks 0.000 ft 3
Gas sample volume corrected for leakage 125.574 ft3
Absolute dry gas meter temperature 554 .5 °R
Dry gas meter temperature 94 8 °F
Absolute dry gas meter pressure 29.93 in Hg
Orifice meter differential pressure (AH) 1.101 in. H20
Barometric pressure at start of run 29.86 in. Hg
Barometric pressure at end of run N/A in. Hg
Condensate collected in sampling train 328 8 grams
Isokinetic sampling variation 104 98 %
3.3920 dscm
3.5559 m3
0.0000 rn3
3.5559 rn3
308.0 K
34.9 "C
760.3 mm Hg
27.96 mm HjO
758.4 mm Hg
N/A mm Hg
328.8 grams
759.0 mm Hg
N/A mm Hg
1.772E-05 m'
Other Supporting Data
Barometric pressure at test site at start of run 29,83 in. Hg
Barometric pressure at test site at end of run N/A in. Hg
Cross-sectional area of sampling nozzle Inlet 1 .907E-04 ft *
Pilot tube coefficient 0.840
Dry gas meter calibration factor (Y)
Dry gas meter calibration factor |Y,|i() from sampling data
Comparison of Yq. to Y (difference must be within ±5% of Y)
Orifice meter factor (AH@)
Potential moisture (as water vapor) content based on condensate collected
Potential moisture (as water vapor) content based on gas stream parameters
1.002
1.002
within ±5%
1.794 in. H20
11.46 % by volume
N/A % by volume
Nomorept.xls 10/31/2001 (rev.M5FinalDataReport.xls [ReportB] 8/26/2003 2:09 PM)
Bl-8
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Test Run Field Data Sheet - PCDD/PCDF
Project no. 1 10249.2.001 .05 Emission measurement location: Stack Outlet
Test run no. 2 Date(s): August 14, 2003 Tram no. M23-2
Traverse
Port -Point
Number
STRT
A18
A18
A18
A17
A16
A15
A14
A13
A12
A11
A10
A9
A8
A7
A6
A5
A4
A3
A2
A1
B18
B18
B18
B17
B16
B15
B14
B13
B12
B11
B10
69
Clock
Tirre
24-hr
5:50:00
5:56:00
6:02:00
6:08:00
6:14:00
6:20:00
6:26:00
6:32:00
6:38:00
6.44:00
6:50:00
6:56:00
7:02:00
7:08:00
7:14:00
7:20:00
7:26:00
7:32:00
7:38:00
7:44:00
7:50:00
8:05:00
8:11:00
8:17:00
8:23:00
8:29:00
8:35:00
8:41 :00
8:47:00
8:53:00
8:59:00
90500
9:11:00
9:17:00
Cumulative
Sanripl'ng
Time
minutes
0.00
6,00
12.00
18.00
24.00
30.00
3600
4200
48.00
54.00
60.00
66.00
7200
7800
84.00
90,00
96,00
10200
108.00
114,00
120.00
120,00
12600
132.00
138.00
144.00
150.00
156.00
162.00
168.00
174.00
180.00
186.00
192.00
Dry Gas Meter Reading,
(Vn»
ft'
Desired
•^SsJUs
66.418
70.403
74.257
78.267
82.285
86.169
90.062
93.567
96.850
99.839
102.585
105.226
107.993
110.765
113.543
116 171
118.801
121.545
124.040
1 26.464
1 30.652
134.585
138.681
1 42.623
146.571
150.377
154.021
157.465
160.769
163.807
166.622
169.203
Actual
62.445
66.450
70.450
74.400
78.450
82.430
86.500
90.460
94.150
97.440
100.320
102.870
105.440
1 08.040
110.820
113.590
116290
118.950
121.750
124.270
126.700
126.956
130.850
134.730
139.110
143.030
146.950
150.780
154.580
157.940
161.040
163.900
166.700
169.230
Orifice ^ressyre
Differencial
(AH), incnes HP
De le
^S^ss
1.372
1.375
1.282
1.383
1.385
1.290
1.293
1.047
0.918
0.759
0.640
0.592
0.650
0.651
0653
0.584
0.584
0.635
0.525
0.495
1.304
1.304
1.409
1.304
1.308
1.213
1.111
0.991
0.911
0.770
0.661
0.556
A t a!
»^^ :
1.500
1.500
1.400
1,500
1.500
1.400
1.400
1.100
0.920
0.690
0.550
0.520
0.570
0.650
0650
0.580
0.580
0.630
0.522
0.470
1.400
1.400
1.500
1.400
1.400
1.300
1.200
0.910
0.790
0.680
0.560
0.510
Ve od:y
Head,
(AP),
rte H O
VNS,,^... .'
1.400
1.400
1.300
1.400
1.400
1.300
1.300
1.050
0.920
0.760
0.640
0.590
0.650
0.650
0650
0.580
0.580
0.630
0.520
0.490
1.300
1.300
1.400
1 300
1 300
1.200
1.100
0.980
0.900
0.760
0.650
0.550
Gas
Stream
Temp ,
t)
XV. '
142
143
143
144
144
145
145
144
145
146
145
145
146
146
145
145
145
145
145
145
146
147
147
149
148
147
148
148
148
148
147
149
Dry Gas Meter
^ernperature
(U "F
(ret
\^'V
80
83
86
88
90
92
94
94
94
95
94
95
94
95
96
97
97
98
98
98
96
98
101
101
102
104
104
104
104
104
104
103
Cu p
< V ,s^
79
80
81
83
83
85
86
86
87
89
89
90
90
91
92
92
93
93
94
95
95
95
96
96
96
97
97
98
99
99
100
99
Pump
Vacuum,
in Hg
"vJyv^N
8.0
8.0
9.0
9.0
9.0
9.0
9.0
8.0
7.0
6.0
6.0
5.0
6.0
6.0
6.0
6.0
6.0
6.0
6.0
5.0
9.0
9.0
9.0
9.0
9.0
8.0
8.0
7.0
7.0
7.0
6.0
6.0
Impinger
Outlet
Temp.
F
^\^_:
60
54
53
52
52
53
54
54
55
56
60
57
54
53
53
53
54
54
55
56
65
58
61
57
55
55
55
56
55
54
54
54
Pfobe
Outlet
Temp..
F
\V
248
248
254
249
249
251
250
251
254
250
252
252
252
248
249
248
253
253
251
250
251
249
250
249
249
248
249
253
249
249
249
250
Page 1 of 1
!- i«er
Holder
Temp ,
r
*XsV;
257
258
257
257
257
257
257
257
256
256
257
257
257
257
257
257
257
257
257
258
257
258
257
257
257
257
257
257
257
257
257
257
XAD
Intel
Temp,,
(r
vj:>s
66
61
60
43
43
44
45
45
46
47
49
50
50
50
50
50
50
50
51
51
59
50
50
49
49
50
50
50
50
50
50
50
STL
Outlet
Temp .
F
X
Isokmehc
Sampling
Variation,
percent
» \
105.7
105.3
107.5
105.9
103.9
109.9
106.7
110.4
105.1
101.0
97.4
102.1
98.6
105,2
104.6
107.8
106.1
107 1
105.9
105.1
103.9
103.5
112.2
1043
104.1
105.5
109.4
102.3
98,4
98,8
1043
102.8
Remarks: Note: Any DGM reading above that is flagged with an asterisk was not taken at the precise time. Operator(s): Dave Griffin
Nomorept.xls 10/31/2001 (rev. M5 Final Data Report xls [Datasheet] 8/26/2003 2:17 PM)
Bl-9
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Test Run Field Data Sheet - PCDD/PCDF
Project no 110249.2.001.05 Emission measurement location: Stack Outlet
Test run no. 2 Date(s): August 14, 2003 Train no. M23-2 Page 2 of 2
Traverse
Port-Point
Number
B8
87
B6
B5
B4
B3
B2
B1
Clock
Time
24-hr
9:23:00
9:29:00
9:35:00
9:41:00
9:47:00
9:53:00
9:59:00
10:05:00
Cumulative
Sampling
Time,
minutes
198.00
204.00
210.00
216.00
222.00
228.00
234.00
240.00
Dry Gas Meter Reading,
(VJ,
ft'
Desired
171.947
174.652
177286
179920
182.263
184.503
186.354
188.175
Actual
171.970
174.730
177.360
179.990
182.480
184.690
186.540
188.275
O'ifiee Pressure
Dtffsrental
(AH), inches H2O
Dssired
0.628
0.610
0.579
0.579
0.457
0.418
0.285
0.276
Actual
0.620
0.610
0.550
0.550
0.450
0.370
0.250
0.230
Velocity
Head.
0p),
inches HjC
0.620
0.600
0.570
0.570
0.450
0.410
0.280
0,270
Gas
Strean
Temp,,
(t,). f
149
147
148
148
148
148
148
147
Dry Gas Meter
Temperature
(U 'F
Inlet
104
104
104
104
104
105
105
105
Outlet
100
100
100
100
101
102
101
102
Pump
Vacuum,
in Hg
6.0
6,0
6.0
6.0
6.0
5.0
5.0
50
Impinger
Outlet
Temp.,
*F
54
55
54
55
56
56
55
56
Probe
Outlet
Temp.,
•F
248
249
248
252
254
250
250
252
Ffcr
Holder
Temp ,
T
257
257
257
257
258
258
258
257
XAD
Inlet
Temp.,
T
51
51
51
51
51
53
53
52
ST.
OuileS
Temp.,
•F
lso'
-------
Emission Measurements Data Summary
Measurement Equipment Information and Leak Check Data
PCDD/PCDF
Project no. 110249.2.001.05
Client EPA/ESD/RTI
Facility CBI
Source tested Millfp
Emission measyrement location Stack Outlet
Test run no. 3 Test run date(s) August 15, 2003
Sampling train no. M23-1 Run start tone 06:10AM
Operator^) Dave Griffin , Run stop time 10:20 AM
Signature/Date
Measurement Eguipment Identification and Specifications,
Metering console no. N7
Dry gas meter
-------
Emission Measurements Data Summary
Source and Sampling Data
Project no.
Client
Facility
Facility location
Source tested
Emission measurement location
PCDD/PCDF
110249.2.001.05
EPA/ESD/RTi
CBI
Mill*
Stack Outlet
Test ran no. 3
Sampling train no. M23-1
Total sampling time 24Q.OQ minutes
Test run date(sj Augus! 15, 2003
Run start time 06:10 AM
Run stop time 10:20 AM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric flow rate at dry standard conditions
Volumetric flow rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
19,421 dsefm
1 ,165,279 dscf/hr
21 ,828 scfm
68 °F and
24,976 acfm
1 ,498,578 acf/hr
58,89 fUsec.
3,533 ft./min.
0.9621 (in, H2G)UU
0.926 in, H2O
602.1 °R
142.5 °F
29.84 in. Hg
0.00 in. H2O
29.84 in. Hg
N/A in. Hg
1 1 .03 % by volume
27.77 Ibflb-mote
28.98 Ib/lb-mole
0.5 % by volume
19.5 % by volume
% by volume
549.95 dsem/min.
32,997.0 dscm/hr
618.10 scm/min.
760 mm Hg
707,25 acm/mtn.
42,435.0 acm/hr
17.950 m/sec.
1,077.0 m/min.
4.849 (mm H20f''
23.51 mm H;0
334.5 K
61.4 °C
757.9 mm Hg
0.0 mm H.,0
757.9 mm Hg
N/A mm Hg
1 1 ,03 % by volum
27,77 gig-mole
28.98 g/g-mole
0.5 % by volum
19.5 % by volum
% by volum
at Emission Measurement Location
Stack or duct type Circular
First diameter 36.000 inches 0.9144m
Second diameter 36.000 inches 0.9144m
Gas stream cross-sectional area 7.0686 ft.2 0.65669 m3
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 122.564 dscf
Gas sample volume as read on dry gas meter 129.465 ft.3
Volume correction for failed leak checks 0.000 ft.'
Gas sample volume corrected for leakage 129,465 ft.3
Absolute dry gas meter temperature 558.5 °R
Dry gas meter temperature 98.8 " F
Absolute dry gas meter pressure 29.92 in. Hg
Orifice meter differential pressure (AH) 1.080 in. H2O
Barometric pressure at start of run 29.85 in. Hg
Barometric pressure at end of run N/A in. Hg
Condensate collected In sampling train 322.1 grams
Isokinetic sampling variation 97.45 %
3.4706 dscm
3.6660 m*
0.0000 m*
3.6660 m1
310.3 K
37.1 X
760.0 mm Hg
27.44 mm HjO
758.2 mm Hg
N/A mm Hg
322.1 grams
Other Supporting Data
Barometric pressure at test site at start of run 29.87 in. Hg 758.7 mm Hg
Barometric pressure at test site at end of run N/A in. Hg N/A mm Hg
Cross-sectional area of sampling nozzle inlet 1 907E-04 ft.z 1.772E-05 m2
Pttot tube coefficient 0840
Dry gas meter calibration factor (Y) 1.002
Dry gas meter calibration factor (Yql) from sampling data 1.002
Comparison of Yqa to Y (difference must be within ±5% of Y) within
Orifice meter factor (AH@) 1.794
Potential moisture (as water vapor) content based on condensate collected 11.03
Potential moisture (as water vapor) content based on gas stream parameters N/A
±5%
in. H20
% by volume
% by volume
Nomorept.xls 10/31/2001 (rev. MS Final Data Report.xls [ReportBJ 8/26/2003 2:25 PM)
Bl-12
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Test Run Field Data Sheet - PCDD/PCDF __,
Project no. 110249. 2. 001. 05 Emission measurement location: Stack Outlet
T««jt run n" ^ DatefsV Auaust 15, 2003 Train no. M23-1
Traverse
Port-Port
Number
INITIAL
A1
A2
A3
A4
AS
A6
A7
A8
A9
A10
A11
A12
A13
A14
A15
A16
A17
A18
A18
A18
INITIAL
B1
B2
B3
B4
B5
86
B7
B8
B9
B10
B11
B12
Clock
Time
24-hr
6:10:00
6'16-00
6 '22 -00
6:28:00
6:34:00
6:40-00
6:46:00
6:52:00
6:58:00
7:04:00
| 7:10:00
7:16:00
7-22-00
7'2800
73400
7-40:00
7-46-00
7'52-dO
7:58:00
8:04:00
8:10:00
8:20:00
8:26:00
8:32:00
8:38:00
8:44:00
8:5000
S'SS'OO
9-02'OQ
9:08:00
9:14:00
9:20-00
9-26-00
9:32:00
Cumulative
Sampling
Time,
minutes
600
12.00
18,00
24,00
3000
3600
42.00
48.00
54.00
60.00
66.00
72.00
7800
84.00
90.00
96.00
10200
10800
114.00
12000
12000
126.00
132.00
138.00
144.00
15000
15600
16200
168.00
174.00
18000
18600
19200
Dry Gas Meter Readmg,
(VJ.
ft'
Desired
192.442
195.175
1 97 933
200 698
203582
206.548
209442
212.341
215 168
217919
220957
224 262
227.684
231 .350
235 170
238.987
242.966
246.944
250933
254.921
257409
260 168
262 804
265564
268.287
271.175
273.942
276 672
279 423
282 1 74
285 367
288 674
Actual
192,440
195 190
1 97.970
200.790
203.690
206.710
209.650
212580
215250
218200
221.210
224.51 0
227920
231 .450
235.100
238.960
242.960
246940
251 050
255.097
255 301
257500
260 200
262940
265.770
268 520
271 .300
274 050
276,800
279 590
282 270
285.470
288 890
Orifice Pressure
Differential
(AH), inches H2O
Desired
0.623
0641
0.651
0.653
0.708
0.749
0,712
0.713
0,677
0,639
0.780
0922
0987
1.130
1.224
1.224
1.327
1 326
1.330
1.330
0,438
0639
0,582
0.638
0.620
0.697
0639
0622
0.631
O.S31
0850
0.910
Actual
0.630
0650
0660
0660
0700
0.740
0.710
0.710
0650
0.590
0.750
0890
0.950
1.050
1,150
1.300
1.400
1 400
1.400
1.400
0440
0.640
0.580
0.640
0.600
0620
0.620
0620
0620
0.620
O.B50
0910
Velocity
Head,
(AP),
indies HjO
0.670
0.690
0.700
0.700
0.760
0.800
0.760
0.760
0.720
0680
0830
0.980
1.050
1.200
1.300
1.300
1 400
1.400
1.400
1.400
0.460
0.670
0.610
0.670
0,650
0,730
0670
0.650
0.660
0.660
0,890
0.950
Gsss
Stream
Temp .
(U *F
140
142
143
143
144
142
143
143
143
144
144
144
144
144
145
145
142
143
142
142
141
140
141
142
142
141
142
140
141
142
142
141
Pags 1 of 2
Dry Gas Metei
Temneratuie
Inlet
85
87
89
91
92
93
94
95
96
97
97
98
98
100
101
101
102
103
104
104
99
100
101
101
102
102
103
103
103
104
104
105
Outset
84
85
86
87
88
88
89
90
91
92
92
93
93
94
95
95
96
96
97
97
97
97
98
98
99
99
99
99
100
100
100
101
Pump
Vacuum.
in. Hg
4.0
5.0
5.0
5.0
5.0
6.0
6.0
6.0
6.0
6.0
6.0
6.0
7.0
70
7,0
8.0
8.0
8.0
8.0
8.0
4.0
5.0
5.0
60
6.0
6.0
6.0
6.0
6.0
6.0
7.0
7.0
jnpmger
Outlet
Temp, ,
'F
66
56
52
51
50
49
49
48
47
47
48
48
48
47
47
47
47
47
45
47
59
48
47
48
49
50
51
52
52
52
49
47
Probe
Outlet
Temp,,
"F
251
248
254
251
251
254
253
251
249
254
251
249
249
254
I 248
249
253
249
248
250
250
253
254
251
248
251
254
250
252
251
254
252
Filter
Holder
"emp ,
'F
258
261
260
257
256
257
257
257
257
256
258
258
257
257 '
257
257
257
257
257
257
258
257
257
257
257
257
257
257
257
257
257
257
XAD
inlet
"emp..
66
58
57
57
46
45
45
46
45
46
46
46
46
46
45
46
46
46
46
45
55
47
48
46
48
48
49
49
49
50
49
49
STL
Outlet
'F
Sampling
Variation,
percent
97.4
98.0
98,2
99.4
98.0
99.2
99.0
98.5
92.0
104.5
96.5
97.2
97.1
93.8
93.1
98.5
98.0
97.5
100.4
988
93.8
95.3
101.3
99.9
98.4
93.8
96.8
98.1
98,8
94.9
97.6
100.8
Remarks: Note: Any DGM reading above that is flagged with an asterisk was not taken at the precise time. Operator(s). Dave Griffin
NomoreDt.xls 10/31/2001 (rev.M5FinalDalaReport.xls [Datasheet] 8/26/2003 2:25 PM)
Bl-13
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 110249.2,001.05 Emission measurement location:
Test run no, 3 Date(s): August 15, 2O03 Train no.
Traverse
Port-Point
Number
B13
B14
B15
B16
B17
B18
B18
B18
Clock
Time
24-hr
9:38:00
9:44:00
9:50:00
9:56:00
1 0:02:00
10:08:00
10:14:00
10:20:00
Cumulative
Sampling
Tjrre
minutes
198.00
204.00
210.00
216.00
222.00
228.00
234.00
240.00
Dfy Gas Meter Reading
ivy.
a*
Desired
292.019
295.501
299.229
303.108
307 136
311.168
315.203
319.386
Actjal
292.200
295.690
299,41 0
303.240
307.240
311.270
315.310
319.421
Orifice Pressure
Differential
(AH), inches H2O
Desired
0.929
1 006
1.151
1.247
1.342
1.343
1.345
1.444
Actual
0.930
1.000
1.100
1.300
1.400
1.400
1.400
1.500
Stack Outlet
MZ3-1 page 2 of 2
Velocity
Head,
-------
Emission Measurements Data Summary
Measurement Equipment Information and Leak Check Data
PCDD/PCDF
Project no. 110249.2.001.05
Client EPA/ESD/RTI
Facility C8I
Facility location 4HHHH|k^^^
Source tested Dryer Stack ^^9
Emission measurement location Stack Outlet
Test run no. 4 Test run date(s) August 18, 2003
Sampling train no. M23-1 Run start time 07:50 AM
Operator^) Dave Griffin Run stop time 12:20 PM
Measurement Equipment Identification and Specifications
Metering console no. N7
Dry gas meter (DGM) calibration factor (Y) 1.002
Orifice meter factor (AH@) 1.794 in. H2O
DGM calibration factor (Y,,) from sampling data 1 021
Comparison of Y,, to Y (must be within ±5% of Y) within tS%
Temperature controller* no. N/A
Temperature meter* no. N/A
Additional thermocouple no. N/A
Sample transfer line no. N/A
Umbilical cable no(s). N-16-2
Sample box no. 10288
Impinger outlet connector no. UH-1
Filter no(s). 23-6
Probe no. 3-5
Effective probe length 30 feet
Probe liner Heated glass tubing
Gas stream temperature thermocouple no. 36-12
Pitottubeno. M-104
Pilot tube coefficient 0.840
Sampling nozzle no. N12
Sampling nozzle type Nichol button-hook
Sampling nozzle inside diameter at inlet tip 0 187 inches
Barometer no. X-4029
Altitude difference from emission measurement location
to barometer or reference point at the test site -29 feet
Altitude difference from metering console location
to barometer or reference point at the test site -20 feet
* Not part of console; or used with peripheral equipment.
Sampling Train Leak Check Data
0.91 m
4.75 rnm
-8.8 m
-6.1 m
Gas stream pressure
measurement system -
Leak check from pitot tube tip
Sampling system -
Leah check from nozzle
Pump Leak
Vacuum, Rate,
Time
Initial 07:25 AM
Final 09:55 AM
Initial 10:15 AM
Final 12:25PM
Result
Pass
PASS
PASS
PASS
Time
Initial 07:30 AM
Final 10:00 AM
Initial 10:16 AM
Final 12:26PM
in. Hq
15.0
12.0
15.0
12.0
dcfm
0.001
0.002
0.001
0.002
Nomorept.xls 10/31/2001 (rev. MS Final Data Report.xls [ReportA] 8/26/2003 2:28 PM)
Bl-15
-------
Emission Measurements Data Summary
Source and Sampling Data
PCDD/PCDF
Project no. 110249.2.001.05
Client EPA/ESD/RTI
Facility CBI
Facility location'
Source tested
Emission measurement location
Test run no. 4
Sampling train no. M23-1
Total sampling time
Dryer Stack '
Stack Outlet
240.00 minutes
Test run date(s) August 18, 2003
Run start time 07:50 AM
Run stop time 12:20 PM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric flow rate at dry standard conditions
Volumetric flow rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
12,303 dscfm
738,195 dscf/hr
13,664 scfm
68 °F and
15,448 acfm
926,881 acf/hr
81.95ft./sec.
4,917 ft./mm.
1.3493 (in. H20)uu
1.821 in, H2O
589 6 °R
129.9 °F
29.57 in. Hg
0.00 in, H2O
29.57 in, Hg
N/A in, Hg
9.96 % by volume
27.87 Ib/lb-mole
28.96 Ib/lb-mole
0.3 % by volume
19.7 % by volume
% by volume
348.39 dscm/min.
20,903.4 dscm/hr
386.93 scm/min.
760 mm Hg
437.44 acm/min.
26,246.4 acm/hr
24.980 m/sec.
1 ,498.8 m/min.
6.800 {mm H20:f-
46.24 mm HjO
327.5 K
54.4 "C
751.1 mm Hg
0.0 mm HjO
751.1 mmHg
N/A mm Hg
9.96 % by volume
27.87 g/g-mole
28.96 g/g-mole
0.3 % by volume
19.7 % by volume
% by volume
at Emission Measurement Location
Stack or duct type Circular
First diameter 24.000 inches 0 6096 m
Second diameter 24.000 inches 0.6096 m
Gas stream cross-sectional area 3.1416ft.2 0.29186m2
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 172 892 dscf 48958dscm
Gas sample volume as read on dry gas meter 184.670ft* 52293m3
Volume correction for failed leak checks 0.000 ft * Q.QQOO m'
Gas sample volume corrected for leakage 184.670 ft1 5.2293 m3
Absolute dry gas meter temperature 560 9 *R 311 6 K
Dry gas meter temperature 101 2 °F 38.5 °C
Absolute dry gas meter pressure 29.72 in. Hg 754.8 mm Hg
Orifice meter differential pressure JiH) 2.009 in. H20 51.04mmHzO
Barometric pressure at start of run 29.58 in. Hg 751.3 mm Hg
Barometric pressure at end of run N/A in. Hg N/A mm Hg
Condensate collected in sampling train 405,6 grams 405.6 grams
Isokinetic sampling variation 96.45 %
Other Supporting Data
Barometric pressure at test site at start of run 29.60 in. Hg 751.8 mm Hg
Barometric pressure at test site at end of run N/A in. Hg N/A mm Hg
Cross-sectional area of sampling nozzle inlet 1.907E-04 ft.1 1.772E-05m1
Pilot tube coefficient 0840
Dry gas meter calibration factor (Y) 1 002
Dry gas meter calibration factor (Y,,) from sampling data 1 021
Comparison of Yqa to Y (difference must be within i5% of Y) within
Orifice meter factor (4H@) 1.794
Potential moisture (as water vapor) content based on condensate collected 9.95
Potential moisture (as water vapor) content based on gas stream parameters N/A
±5%
in. HjO
% by volume
% by volume
Nomoreptxls 10/31/2001 (rev. MS Final Data Report.xls [ReportB] 9/10/2003 11:17 AM)
Bl-16
-------
Test Run Field Data Sheet - PCDD/PCDF
Proiectno. 110249.2.001.05 Emission measurement location: Stack Outlet
Test run no. A Date{s): August 18. 2003 Train no. M23-1 Page 1 of 2
"raverse
Port-Point
Number
INITIAL
B1
B2
B3
B4
INITIAL
B5
B6
B7
B8
B9
BIO
B11
B12
B13
B14
B15
B16
B17
B18
B18
B18
INITIAL
A1
A2
A3
A4
AS
A6
A7
A8
A9
A10
A11
Clock
Time
24-hr
7:50:00
7:56:00
8:02:00
8:08:00
8:14:00
8:17:00
8:23:00
8:29:00
8:35:00
8:41:00
8:47:00
8:53:00
8:59:00
9:05:00
9:11:00
9:17:00
9:23:00
9:29:00
9:35:00
9:41 :00
9:47:00
9:53:00
10:20:00
10:26:00
10:32:00
10:38:00
10.44:00
10:50:00
10:56:00
11:02:00
11:08:00
11:14:00
11:20:00
11:26:00
Cumulative
Sampl.ng
Time,
rmmfes
0,00
6.00
12.00
18,00
24.00
24.00
30.00
36.00
42.00
4800
54.00
60.00
66.00
72.00
78.00
84.00
90.00
96.00
102.00
108.00
114.00
120.00
120.00
126.00
132.00
138.00
144.00
150.00
156.00
162.00
168.00
174.00
180.00
186.00
Dry Gas Mete? Reading.
(V*>.
P.°
DM Hi
\^\^\
322.933
326.266
330.368
334.736
339.184
343.707
348.295
352.888
357555
362.242
366.990
371 .746
376.574
381 .399
386.359
391 .324
396298
401 326
406.349
411.252
414.969
418.998
423.443
427.965
432.553
437213
441 938
446.675
451 .474
456.286
461.161
Actual
320.295
322.970
326.400
330.150
334.500
334.500
338.950
343.410
348.070
352.780
357.510
362.280
367.090
371.950
376.790
381 .650
386.520
391 .420
396.320
401 .280
406.220
411.082
411.396
414.950
418.840
423.200
427.610
432.200
436.910
441 .630
446.410
451.210
456.1 40
461 .000
Orifice Pressure
Differential
(AH), inches HjO
Desired
iSl^
0.591
0.941
1.422
1.613
1,667
1.719
1,767
1.765
1.820
1.830
1,878
1.881
1.936
1.931
2.038
2.040
2.045
2.090_^
2.085
1.984
0.960
1,345
1 .637
1.689
1.738
1.789
1.840
1.847
1.895
1.901
1.951
Actual
0.590
0.940
1.500
1.700
1.700
1,800
1,900
1.900
1.900
1.900
1.950
1.950
2.000
2.000
2.050
2.050
2.050
2.100
2.100
2.000
1.000
1.400
1.700
1.700
1.800
1.850
1.950
2.000
2.000
2.000
2.100
Velocity
Head,
SAP)
inches H.O
0,620
0.990
1.500
1,700
1 750
1.800
1,850
1 850
1.900
1.900
1.950
1,950
2.000
2,000
2.100
2.100
2.100
2150
2150
2050
1.000
.400
.700
.750
.800
.850
.900
1.900
1.950
1.950
2.000
Gas
Stream
Temp.
(U -F
127
129
131
130
129
129
130
132
130
129
129
129
128
130
127
127
126
127
129
131
136
135
133
133
133
133
132
131
131
130
130
Dry Gas Meter
Temperature
ft.). "F
Inlet
^^^i
86
88
90
91
92
94
95
97
98
100
100
101
102
102
103
103
103
103
104
104
100
101
101
103
104
105
105
106
106
107
108
Outlet
87
88
89
88
90
91
92
93
93
95
95
96
97
98
98
99
100
100
100
101
100
100
100
101
101
102
102
103
103
104
104
Puma
Vacuum,
in. Hg
s.o
8.0
9.0
10.0
11.0
11.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12,0
12,0
12.0
12.0
12.0
120
12.0
8.0
9.0
10,0
10.0
11.0
11.0
11.0
12.0
12.0
12.0
12.0
Impinger
Cutlet
Temp .
•F
53
51
50
51
52
54
56
56
59
54
54
55
56
57
54
54
55
56
57
58
67
46
48
51
54
52
50
50
50
51
53
Probe
Outlet
Temp .
•F
250
249
250
250
250
250
249
250
250
250
251
250
249
249
249
251
248
250
248
249
250
250
251
248
248
250
250
251
249
251
252
Filtei
Holder
Temp
T
257
256
257
257
247
254
256
257
257
257
257
257
257
257
256
257
256
257
257
256
261
259
257
257
257
257
257
257
257
257
257
XAD
Inlet
Temp .
'F
49
43
44
44
45
45
46
46
47
45
45
46
46
47
47
47
47
46
47
48
57
46
45
45
46
46
47
46
46
47
47
STL
Outlet
Temp .
T
250
250
250
250
248
250
250
248
250
250
250
250
250
250
250
250
250
250
250
250
fc
Isoksnetic
Sampling
Vacation.
percent
97.8
99.2
88.1
96,0
96.5
95.1
97.9
98.9
977
98.1
97.7
98.5
96.6
971
94.7
- 95.2
95.0
95.1
948
95.6
100,7
93.1
94.6
94.0
96.5
97.5
96.3
97.3
96.4
98.8
96.1
Remarks: Note Any DGM reading above that is flagged with an asterisk was not taken at the precise time.
Nomorept.xls 10/31/2001 (rev.M5FinalDataReport.xls [DataSheetJ 8,76/2003 2:27 PM)
Bl-17
Operator(s): Dave Griffin
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no, 11Q249.2.QQ1,&5 Emission measurement location: Stack Outlet
Test run no. 4 Date(s): August 18, 2003 Train no, M23-1 Page 2 of 2
Traverse
Port-Point
Number
A12
A13
A14
A15
A16
At?
A18
A19
A20
Clo
Desred
1.956
1,960
1.960
1.960
1.961
1.963
1.968
1.972
1.923
Actual
2.100
2.100
2100
2.100
2.100
2.050
2.000
2.000
1.900
Velocity
Head.
-------
Emission Measurements Data Summary
Measurement Equipment Information and Leak Check Data
PCDD/PCDF
Project no. 110249.2.001.05
Client EPA/ESD/RT1
Facility CB1
Facility location
Source tested Dryer Stack
Emission measurement location Stack Outlet
Test run no. 5 Test run date(s) August 19, 2003
Sampling train no. M23-1 Run start time 06:05 AM
Run stop time 10:30 AM
S^isture/Qate
Measurement Equipment Identification and Specification^
Metering console no. N7
Dry gas meter |DGM| calibration factor (Y) 1.002
Orifice meter factor (AH@) 1 794 in. H;O
DGM calibration factor (Yqa) from sampling data 1.022
Comparison of Yqa to Y (must be within ±5% of Y) within ±5%
Temperature controller* no. N/A
Temperature rneter* no. N/A
Additional thermocouple no. N/A
Sample transfer line no. N/A
Umbilical cable no(s). N-16-2
Sample box no. 10288
Impinger outlet connector no. UH-1
Filter no(s). 23-9
Probe no. 3-5
Effective probe length 3.0 feet
Probe liner Heated glass tubing
Gas stream temperature thermocouple no. 36-12
Pilot tube no. M-104
Pttot tube coefficient 0.840
S amp I i ng nozzle no. N12
Sampling nozzle type Nichol button-hook
Sampling nozzle inside diameter at inlet tip 0.187 inches
Barometer no. X-4029
Altitude difference from emission measurement location
to barometer or reference point at the test site -29 feet
Altitude difference from metering console location
to barometer or reference point at the test site -20 feet
1 Hot part of console; or used with peripheral equipment.
Sampling Train Leah Check Data
0.91 m
4.75 mm
-8.8 m
-6.1 m
Gas stream pressure
measurement system -
Leak cheeh from pltot tube tin
Time
Initial 05:55 AM
Final 08:08 AM
Initial 08:25 AM
Final 10:35 AM
Result
Pass
PASS
PASS
PASS
Sampling system -
Leak check from nozzle
Pump
Vacuum,
Time in. Hg
Initial 08:00 AM 15.0
Final 08:10AM 11.0
Initial 08:26 AM 15.0
Final 10:33 AM 11.0
Leak
Rate,
dcfm
0.003
0.002
0.003
0.001
Nomorept.xls 10/31/2001 (rev.M5FinaiDataReport.xls [ReportA] 8/26/2003 2.30 PM>
Bl-19
-------
Emission Measurements Data Summary
Source and Sampling Data
Project no.
Client
Facility
Facility location
Source tested
Emission measurement location
PCDD/PCDF
110249.2.001.05
EPA/ESD/RTI
CBI
Dryer Stack ,
Stack Outlet
Test run no. 5
Sampling train no. M23-1
Total sampling time 240 00 minutes
Test run date(s) August 19, 2003
Run start time 06:05 AM
Run stop time 10:30 AM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric flow rate at dry standard conditions
Volumetric flow rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
12,155 dscfm
729,325 dscf/hr
13,434 scfm
68 "F and
15,212 acfm
912,690 acf/hr
80.70 ft/sec.
4,842 ft/min.
1.3284 (in. H20)aj
1 .765 in. H2O
591.3 °R
131.6 °F
29.61 in. Hg
0.00 in H2O
29.61 in. Hg
N/A in. Hg
9.52 % by volume
27.90 Ib/lb-mole
28.94 Ib/lb-mole
0.2 % by volume
19.7 % by volume
% by volume
344.20 dscm/min.
20,652.2 dscm/hr
380.42 scrn/min.
760 mm Hg
430.74 acm/tnin.
25,844.5 acm/hr
24.597 m/sec.
1,475.8 m/min.
6.695 (mm H2O)U
44.82 mm HjO
328.5 K
55.3 °C
752.1 mm Hg
0.0 mm HjO
752.1 mm Hg
N/A mm Hg
9.52 % by volur
27.90 g/g-mole
28.94 g/g-mole
0,2 % by volur
19.7 % by volur
% by volur
at Emission Measurement Location
Stack or duct type Circular
First diameter 24.000 inches 0,6096 m
Second diameter 24.000 inches 0.6096 m
Gas stream crass-sectional area 3.1416 ft* 0.29186 m3
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 169.974 dscf
Gas sample volume as read on dry gas meter 179.155 ft.1
Volume correction for failed leak checks 0.000 ft,1
Gas sample volume corrected for leakage 179.155 ft,3
Absolute dry gas meter temperature 5542 °R
Dry gas meter temperature 945 "f
Absolute dry gas meter pressure 29.75 in Hg
Orifice meter differential pressure (^H) 1,933 in R..O
Barometric pressure at start of run 29.62 in Hg
Barometric pressure at end of run N/A in Hg
Condensate collected In sampling train 379 3 grams
Isokinetic sampling variation 95.97 %
4,8131
5.0731
0.0000
5.0731
307.9
34.7
755.7
49.23
752.3
N/A
379.3
dscm
m*
m3
m'
K
•c
mm Hg
mm HjO
mm Hg
mm Hg
grams
752.9 mm Hg
N/A mm Hg
1.772E-05 mj
Other Supporting Data
Barometric pressure at test site at start of run 29.64 in Hg
Barometric pressure at test site at end of run N/A in Hg
Cross-sectional area of sampling nozzle Inlet 1.907E-04 ft *
Pilot tube coefficient 0.840
Dry gas meter calibration factor (Y)
Dry gas meter calibration factor (Y,J from sampling data
Comparison of Y,, to Y (difference must be within +5% of Y)
Orifice meter factor (AH@)
Potential moisture (as water vapor) content based on condensate collected
Potential moisture (as water vapor) content based on gas stream parameters
1.002
1.022
within ±5%
1.794 in. H2O
9.52 % by volume
N/A % by volume
Nomorept.xls 10/31/2001 (rev.M5FinalDataReport.xls [Reports] 8/26/2003 2:30 PM)
Bl-20
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 110249 -2.001. 05 Emission measurement location: Stack Outlet
Test run no 5 Date(s): August 19, 2003 Train no. M23-1
T raverse
Port-Point
Nunber
INITIAL
B1
B2
B3
B4
B5
B6
B7
68
B9
B10
B11
B12
B13
B14
B15
B16
817
B18
819
820
INITIAL
A1
A2
A3
A4
AS
A6
A7
A8
A9
A10
A11
A12
Remarks:
Clock
Time
24-hr
6-05-00
6:11:00
6-17:00
623:00
629:00
635:00
641:00
647:00
653:00
6-59:00
705:00
7:11:00
7:17:00
7:23:00
7:29:0»«
7 35'OQ
7:41:00
7:47:00
7:53:00
7-5900
805:00
8:30.00
8-36-00
8:42:00
8:48:00
8:54:00
9-00:00
9-06-00
9-12-00
9:18:00
9:24:00
9:3000
9:3600
9:42:00
Cumulative
Sampling
Time.
mhutes
0.00
6.00
12.00
18.00
24.00
30.00
36.00
42.00
48.00
54.00
6000
6500
7200
78.00
8400
90,00
96,00
102,00
108.00
114.00
120.00
120.00
126.00
132.00
138.00
144.00
150.00
156.00
162.00
168.00
174.00
180.00
186.00
192.00
Diy Gas Mster Reading,
(Vm>
ft'
Desired
^UPSPHI^
507.345
510.727
514.710
518.904
523.242
527.555
531 .949
536.417
540.966
545.51 1
550.121
554.806
559.492
564.241
568.998
573.755
578.637
583.461
588.274
593,103
596,857
600.518
604.690
609.076
613611
618217
622 897
627,581
632,269
637026
641 792
646557
Actual
505489
507.430
510.890
514.850
519.070
523.380
527.700
532.060
536.520
541 .060
545.580
550.190
554.830
559.510
564.220
568,980
573.750
578.580
583.440
588.220
593.031
593.246
596.830
600.570
604.710
609.130
613670
618.270
622.950
627.630
632.330
637.070
641 .820
646.570
Orifice Pressure
Differential
(AH), inches H,O
Desired
^nniy^
0,295
0.979
1.358
1.501
1.601
1.580
1.639
1.691
1.751
1,748
1.797
1.853
1.852
1.902
1.907
1.907
2.006
1.957
1.948
1 958
1.055
1.130
1.464
1.616
1.723
1.775
1.828
1.832
1.832
1 883
1.886
1.886
AcUai
nmn^i
0.310
1.000
1 400
1 600
1.700
1.700
1.700
1.750
1.800
1.800
1.850
1.900
1.900
1.950
2.000
2.000
2.100
2.050
2.000
2.000
1.100
1.200
1.500
1.700
1.800
1.850
1.900
1.900
1.900
1.950
1 950
1.950
Velocity
Head,
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 1 10249.2.001 .05 Emission measurement location; Stack Outlet
Tost run no 5 DafefsJ: Auaust 19. 2003 Train no. M23-1 Page 2 of 2
Traverse
Po't-Poin!
Number
A13
A14
A15
A16
A17
A18
A19
A20
CkKX
Time
24-hr
9-48:00
9:54:00
10:00:00
10:06:00
10:12:00
10:18:00
1 0-24:00
10:30:00
Cumulative
Sampling
Time.
minutes
198.00
204.00
210.00
216.00
222.00
228.00
234,00
240,00
Dry Gas Meter Reading,
w
ft3
Desired
651 .392
656.235
661.010
665.853
670.628
675.408
680.200
684.932
Actual
651 .350
656.160
660.940
665.750
670.580
675.370
680.140
684.859
Orifice Pressure
Differential
(iH), incnes HjO
Desired
1.937
1.941
1.886
1,938
1.882
1,882
1.890
1.839
Actual
2.000
2.000
1.950
2.000
2.000
1.950
1.950
1.900
Veiocity
Head,
(AP).
inches H;O
2.000
2.000
1.950
2,000
1.950
1,950
1.950
1.900
Gas
Stream
Tcmo..
(U. 'F
129
129
131
131
134
135
133
135
Dry Gas Meter
Temperature
«, T
Into!
103
104
104
105
106
107
107
108
Outlet
99
100
100
101
101
102
103
104
Pump
vacujm.
in. Kg
11.0
11.0
11.0
11.0
11.0
11.0
11.0
11.0
Jmpinger
Outle-
Temp.,
49
51
52
53
52
53
53
53
Probe
Outle!
Temp
250
250
250
251
249
250
251
251
Filter
Holder
Temp..
257
257
257
257
257
257
257
257
XAD
Inlet
Temp ,
46
46
46
46
46
46
47
48
STL
Outlet
Temp..
Isokmete
Sampling
Variation,
percent
94.9
95.4
96.1
95.3
97.1
96.2
95.6
95.8
Remarks: Note: Any DGM reading above that is (lagged with an asterisk was not taken at the precise time. Operator(s): Dave Griffin
Nomoreptxls 10/31/2001 (rev. M5 Final Data Report xls {Datasheet] 8/26/2003 2.29PM)
El-22
-------
Emission Measurements Data Summary
Measurement Equipment Information and Leak Check Data
PCDD/PCDF
Project no. 110249.2.00105
Client EPA/ESD/RTI
Facility CBI
Source tested Dryer Stack
Emission measurement location Stack Outlet
Test run no. 6
Sampling train no. M23-2
Test run date(s) August 20, 2003
Run start time 06:10 AM
Run stop time 10:35 AM
Signature/Date
Measurement Equipment Identification and Specifications
Metering console no. N7
Dry gas meter (DGM) calibration factor (Y) 1 002
Orifice meter factor (AH@) 1 .794 in. HjO
DGM calibration factor (Y,,) from sampling data 1 ,023
Comparison of Y,, to Y (must be within ±5% of Y) within ±5%
Temperature controller* no. N/A
Temperature meter* no. N/A
Additional thermocouple no. N/A
Sample transfer line no. N/A
Umbilical cable no(s). N-1 6-2
Sample box no. 012003
Impinger outlet connector no. UH-1 2
Filter no(s), 23-8
Probe no, 3-5
Effective probe length 3.0 feet
Probe liner Heated glass tubing
Gas stream temperature thermocouple no, 36-1 2
Pilot tube no. M-1 04
Pitot tube coefficient 0.840
Sampling nozzle no. N 1 2
Sampling nozzle type Nichol button-hook
Sampling nozzle inside diameter at inlet tip 0.1 87 inches
Barometer no. X-4029
Altitude difference from emission measurement location
to barometer or reference point at the test site -29 feet
Altitude difference from metering console location
to barometer or reference point at the test site -20 feet
* Not part of console; or used with peripheral equipment.
Sampling Train Leak Check Data
0.91 rn
4.75 mm
-8.8 m
-6.1 m
Gas stream pressure
measurement system -
Leak check from pilot tube tip
Time Result
Initial 05:25 AM Pass
Final 08: 13 AM PASS
Initial 08-30 AM PASS
Final 10:39 AM PASS
Sampling system -
Leak check from nozzle
Pump
Vacuum,
in. Hq
Time
Initial 05:27 AM
Final 08:12 AM
Initial 06:05 AM
Final 10:37 AM
Initial 08:29 AM
15.0
12.0
15.0
12.0
15.0
Leak
Rate,
dcfm
0.003
0.007
0.001
0.005
0.006
Nomorept.xls 10/31/2001 (rev. MS Final Data Report.xis [ReportA] 8/26/2003 2:32 PM)
Bl-23
-------
Emission Measurements Data Summary
Source and Sampling Data
Project no.
Client
Facility
Facility location
Source tested
Emission measurement location
PCDD/PCDF
110249.2.001.05
EPA/ESD/RTI
CBI
Dryer Staclf J
Stack Outlet
Test run no. 6
Sampling train no. M23-2
Total sampling time 240.00 minutes
Test run date(s) August 20, 2003
Run start time 06; 10 AM
Run stop time 10:35 AM
Gas Stream Measurement Results
Volumetric flow rate at dry standard conditions
Volumetric (low rate at dry standard conditions
Volumetric flaw rate at standard conditions
Standard Conditions are
Volumetric flow rate at actual conditions
Volumetric flow rate at actual conditions
Average velocity
Average velocity
Square root of velocity head
Velocity head
Absolute temperature
Temperature
Absolute pressure
Static pressure
Barometric pressure at start of run
Barometric pressure at end of run
Moisture (as water vapor) content
Wet gas molecular weight
Dry gas molecular weight
Carbon dioxide concentration, dry-basis
Oxygen concentration, dry-basis
Carbon monoxide concentration, dry-basis
Gas Stream Cross-Sectional Area
1 1 ,898 dscfm
713,855 dscf/hr
13,125scfm
68 °F and
14,709 acfm
882,526 acf/hr
78.03 ftVsec.
4,682 ft/min.
13401 (in. H2GT
1.796 in. H20
585.4 °R
125.7 T
29.62 in. Hg
0.00 in. H2O
29.62 in. Hg
N/A in, Hg
9.35 % by volume
30.06 IWlb-mole
31.3Qlb/lb-mole
19.8 % by volume
0.2 % by volume
% by volume
336.90 dscm/min.
20,214.1 dscm/hr
371 .67 scm/min.
760 mm Hg
416.51 acm/min.
24,990.4 acm/hr
23.784 m/sec.
1,427.1 m/min.
6.754 {mm H20f ;l
45.62 mm HjO
325.2 K
52.1 "C
752.4 mm Hg
0.0 mm HjO
752.4 mm Hg
N/A mm Hg
9.35 % by volume
30.06 g/g-mole
31.30 g/g-mole
19.8 % by volume
0.2 % by volume
% by volume
at Emission Measurement Location
Stack or duct type Circular
First diameter 24.000 inches 0.6096m
Second diameter 24.000 inches 0.6096 m
Gas stream cross-sectional area 3.1416ft.2 0.29186m*
Gas Sampling Results
Gas sample volume, corrected, at standard conditions 172.515 dscf
Gas sample volume as read on dry gas meter 181.473 ft.1
Volume correction for failed leak checks 0.000 ft.1
Gas sample volume corrected for leakage 181.473 ft.3
Absolute dry gas meter temperature 553,3 °R
Dry gas meter temperature 93.6 °F
Absolute dry gas meter pressure 29.77 in Hg
Orifice meter differential pressure (AH) 1.973 in. H;O
Barometric pressure at start of run 29.63 in. Hg
Barometric pressure at end of run N/A in, Hg
Condensate collected In sampling train 377.5 grams
Isokinetic sampling variation 99 52 %
4.8851 dscm
5.1387 m3
0.0000 m"
5.1387 m'
307.4 K
34.2 °C
756.0 mm Hg
50.12 mm KfeO
752.6 mm Hg
N/A mm Hg
377.5 grams
Other Supporting Data
Barometric pressure at test site at start of run 29.65 in. Hg 753.1 mm Hg
Barometric pressure at test site at end of run N/A in. Hg N/A mm Hg
Cross-sectional area of sampling nozzle inlet 1 907E-04 ft.' 1.772E-D5 m2
Pitot tube coefficient 0 840
Dry gas meter calibration factor (Y)
Dry gas meter calibration factor (Y,|a) from sampling data
Comparison of Y,, to Y (difference must be within ±5% of Y)
Orifice meter factor (AH@)
Potential moisture (as water vapor) content based on condensate collected
Potential moisture (as water vapor) content based on gas stream parameters
Nomorept.xls 10/31/2001 (rev. M5 Final Data Report.xls [Reports] 8/26/2003 2:32 PM)
1.002
1.023
within ±5%
1794 in. H5O
9,35 % by volume
N/A % by volume
El-24
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 110249.2, 001,05 Emission measurement location: Stack Outlet
Test run no. 6 Date(s): August 20, 2003 Train no. M23-2 Page 1 of 2
Traverse
Port-Point
Number
STRT
B1
B2
B3
B4
B5
B6
B7
B8
B9
810
B11
B12
B13
B14
B15
B16
B17
B1S
B19
B20
INITIAL
A1
A2
A3
A4
AS
A6
A7
A3
A9
AID
A11
AI2
Uock
Time
24-hr
6:10:00
6:16:00
6:22:00
6:28:00
6:34:00
6:40:00
6:46:00
6:52:00
6:58:00
7:04:00
7:10:00
7:16:00
7:22:00
7:28:00
7:34:00
7:40:00
7:46:00
7:52:00
7:58:00
8:04:00
8:tO:00
8:35:00
8:41 :00
8:47:00
8:53:00
8:59:00
9:05:00
9:11:00
9:17:00
9:23:00
9:29:00
9:35:00
9:41 :00
9:47:00
Cumulative
Sampling
Time.
minutes
0.00
6.00
12.00
18,00
24,00
30.00
36.00
42.00
48.00
54.00
60.00
66,00
72.00
78.00
84.00
90,00
96.00
102.00
108.00
114.00
120.00
120.00
12600
132,00
138.00
144.00
1 50.00
156,00
162.00
168.00
174.00
180.00
186.00
192.00
Dry Gas Meter Readino.,
(VJ.
ft."
Cesred
iwSfil
687954
691.253
695.242
699.442
703.782
708.122
712.536
717.086
721.701
726.323
730.942
735629
740.375
745.125
749.880
754.701
759.581
764.407
769.225
774.048
777900
781 .962
786.297
790.776
795.330
799.955
804.646
809.341
814.043
818.754
823.535
S28.255
Actual
685.232
688.030
691.290
695.190
699.400
703.720
708.100
712.530
717.090
721 .700
726.320
730.960
735.700
740.450
745.220
749.980
754.820
759.630
764.460
769.290
774.053
774.286
778.030
781 .990
786.310
790.770
795.300
799,880
804.500
809.180
813.920
818.670
823.480
828.320
Onlice Pressure
Differential
(AH), inches HjO
Desired
0.637
0.935
.364
.510
.609
.608
.661
1.761
1.811
1.814
1.813
1.863
1.912
1.914
1.916
1.968
2.016
1.968
1.962
1.960
1.108
1.394
1.584
1.686
1.739
1,790
1.839
1.839
1.843
1.846
1.897
1.848
Actual
0.640
0.940
,400
.600
.700
.700
.750
.850
.900
1.900
1.900
1.950
2.000
2.000
2.000
2.050
2.050
2.050
2.050
2.050
1.150
1.450
1.650
1 .750
1.800
1.850
1.900
1.900
2.000
2.000
2.000
2.000
Velocity
Head,
(API.
inches H2O
0.690
.000
.450
,600
.700
.700
750
.850
,900
1,900
1.900
1.950
2.000
2.000
2.000
2.050
2 100
2.050
2.050
2.050
.150
.450
.650
.750
.800
.850
1.900
1.900
1.900
1.900
1,950
1.900
Gas
Stream
Temp .
(U. T
139
132
128
127
126
127
126
»25
124
124
124
124
123
123
123
122
122
123
125
127
123
124
126
125
125
125
125
126
126
126
126
127
Dry Gas Meter
I emperature
(U °F
Inlet
iHH
80
81
83
85
86
87
88
89
89
90
89
90
90
90
91
91
91
92
92
94
90
91
93
95
97
98
99
100
101
102
103
103
Outlet
81
82
82
82
83
83
84
85
85
86
86
87
86
87
87
88
88
89
89
90
90
90
91
92
93
94
94
95
96
97
98
99
Pump
Vacuum,
m. HD
6.0
8.0
9.0
10.0
10.0
10.0
11.0
11,0
11.0
11.0
11.0
11.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
9.0
9.0
10.0
11.0
11.0
11.0
11.0
11.0
11.0
11.0
12,0
12.0
tmpsnaer
Outlet
Terap.,
"F
59
51
50
51
52
53
54
54
55
56
44
44
44
47
48
51
55
56
57
58
57
55
56
56
57
57
57
57
58
58
57
59
Prose
Outlet
Temp.,
•f
251
249
250
250
251
251
250
249
251
247
248
247
251
250
248
249
251
248
250
250
250
249
250
250
251
252
250
251
250
250
250
248
niter
Holder
Temp.
°F
257
256
256
257
257
257
257
256
257
257
257
257
257
257
257
257
258
257
257
257
261
259
257
257
257
258
257
257
258
257
257
257
XAD
Inlet
Temp ,
T
48
41
49
40
41
41
41
41
41
42
42
43
43
44
44
44
45
46
47
48
48
45
44
44
44
45
46
47
49
51
49
47
STL
Outlet
Temp..
>F
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
2504
250
250
250
250
¥•
Isokittetic
Sampling
Vacation,
percent
102.3
983
97.2
99.7
99.0
100.4
99.8
99.7
99.4
99,4
99.9
100.6
99.6
99.9
99.6
99.8
98.0
99.5
99.7
98.2
1029
970
99.1
99.0
98.9
98.5
98.0
99.1
100.3
100.3
100.1
102.0
Remarks: Note: Any DGM reading above that is Bagged with an asterisk was not taken at the precise time. Operators): Dave Griffin
Nomorept.xls 10/31/2001 (rev.M5FinalDataReport.xls [Datasheet] 8/26/2003 2:3t PM)
Bl-25
-------
Test Run Field Data Sheet - PCDD/PCDF
Project no. 1 10249.2. OO1.05 Emission measurement location: Stack Outlet
Test ran no 6 Date(s): August 20, 2003 Train no. M23-2 Page 2 of 2
Traverse
Port-Point
Number
A13
A14
A15
A16
A17
A18
A19
A20
Clock
Time
24-hr
9:53:00
9:59:00
1 0:05:00
10:11:00
10:17:00
10:23:00
10:29:00
10:35:00
Cumulative
Sampling
Time
m outes
198.00
204.00
210.00
216.00
222.00
228.00
234.00
240.00
Dry Gas Meter Reading,
(V,).
ft'
Desired
833.044
837838
842.706
847.521
852.406
857.234
862.070
866.841
Actual
833.170
837.990
842.860
847.690
852.490
857.330
862.170
866.938
Orifice Pressure
Differential
(AH), inches N;O
Desired
1.899
1.899
1.954
1.909
1.961
1.914
1.918
1.866
Actual
2.000
2.000
2.000
1.950
2.000
2.000
2.000
1.900
Velocity
Head,
!Ap).
inches H3O
1 950
1 950
2.000
1.950
2000
1 950
1 950
1 900
Gas
Stream
Temp,
(!,), 'F
127
128
127
127
127
127
127
128
Dry Gas Meter
Temperature
(U. *F
Inlet
104
105
106
107
108
109
110
110
Outlet
100
101
102
103
104
104
105
105
Pump
Vacuum.
in Itg
12.0
12.0
12.0
12.0
12.0
12.0
12.0
11.0
Impsnfier
Outlet
Temp,.
'F
57
57
58
58
57
56
56
59
Probe
Outlet
Temp.,
249
251
251
29
251
250
249
251
Fifter
Holder
Teirp.,
T
257
257
257
257
257
257
257
257
XAD
Inlet
Temp.,
48
47
46
46
45
45
45
45
STL
Cutlet
Temp-,
"F
Iso kinetic
Sampling
Variation,
percent
100.7
100.0
99.5
99.8
97.7
99.7
99.5
99.4
Remarks: Note: Any DGM reading above that is flagged with an asterisk was not taken at the precise time. Operator(s): Dave Griffin
Signature/Dat
Nomoreptxls 10/31/2001 (rev MS Final Data Report xls [Datasheet] 8/26/2003 2:31 PM)
Bl-26
-------
Appendix B-2
Emissions Sample Recovery
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLAT1LE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.; 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location: fvA I |\ 9tt
Run No.
Set-up person(s):
Sampling Train No.
Sample Box No.
Date:
Transfer to Sampler* «
Relinquished By n • Set i^JcLl
Received Byf/l.1otn(f/:£fitSr*
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.: 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location: ^V] < // flpB
Run No. o<^ Sampling Train No. /vt3L?-~ ^
Set-up person(s): A • J£<.*r@ji/^
Transfer to Sampler: «
Relinquished By "^, Hoi^A^~ej. (•
TRAIN COMPONENT*
Sample Box No. fl/csLQ o3>
Date: %/li/G2)
jfi^Mft/U'M^i I Date/Time <3//y/O,3 t'5'£'i
/
LOADING DATA
Sampling Nozzle (Quartzckej
Heated Coupling and Teflon STL" )J / A.
Filter Type/W,.Whatman QM-A/^; J - 5-
Condenser Thermocouple No. K r\ T) - 3~^
XAD-2 Resin Cartridge spike date g / % /'# 3
XAD-2 Resin Cartridge Lab ID"*P3/C&? - QQJ
Impinger OuBet Connector () K - / 3~
Initial Weights (grams)**
' Empty .__,_ Loaded
1st Impinger (500-mL oK-rt KO), Empty
1st Impinger Replacement™ (KO), Empty
COMMENTS:
2nd Impinger (MGBS), 100 mLs ASTM Type II Water Y"^ Y> o^ £ S'7>~7
3rd Impinger (GBS), 100 mLs ASTM Type II Water */S?3. Sf J^?3. V
4th Impinger (MGBS), Empty
5th Impinger (MGBS), Si Gel
6th Impinger** (MGBS), Si Gel Vff^ •i/
S
I 00 I, Q IOUL\O @ ,00 O. '
" Before and after sampling: Nozzle openings covered with Teflon or pre-rinsed aluminum foil, and nozzle placed in Ziploc bag.
Probe liner outlet sealed with glass female blank-off, and union sealed with Teflon plug. Cyclone/Bypass inlet covered (not
sealed) with Teflon or pfe-rinsed aluminum foil. Vertical traverse adapter (VTA) openings, filter holder outlet, and condenser
inlet sealed with Teflon or glass blank-offs. Sample transfer line (STLI openings joined with giass/Teflon coupling used at filter
holder outlet during sampling.
Optional for moisture gas streams andfor special situations as applicable.
* Cartridge weighed with blank-offs in place; then, cartridge covered with aluminum foil to seal out light during storage and
sampling. Documentation of standards injection is separate. Cartridges are maintained at near 4° until use. /
Initial weights of additional components exchanged during the run also entered here. All exchange component openings a l
covered with Teflon or pre-rinsed aluminum foil or as described above.
B2-2
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGAIMICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.: 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location:
Run No. ^_jj:g^ Campling Train No. 4j »Z-?—'/ Sample Box No.
Set-up person(s): "S .j&fHCfoaSfcCg.) Date:
Transfer to Sampler:
Relinquished By *$\3-<£r&*l&I<& Received By V^rf&LSAJj&eUtL Date/Time
y- £/
TRAIN COMPONENT* „ , LOADING DATA
Sampling Nozzle (Quartz/NickeJ) __AJ_
Heated Coupling and Teflon STL" /O/
Filter Type Whatman QM-A
Condenser Thermocouple No. X/^D
XAD-2 Resin Cartridge spike date
XAD-2 Resin Cartridge Lab ID***
Impinger Outlet Connector
Initial Weights (grams)****
Empty Loaded
1st Impinger (500-mL orp-L;* KO), Empty
1st Impinger Replacement** (KO), Empty
2nd Impinger (MGBS), 100 mLs ASTM Type II Water
3rd Impinger (GBS), 100 mLs ASTM Type II Water
4th Impinger (MGBS), Empty jf(?. ^p" <\) /A
5th Impinger (MGBS), Si Gel
6th Impinger** (MGBS), Si Gel ¥j£><£> 7/Q-3. 7
COMMENTS:
•-JOO- 3
iooo-1
' Safore and after sampling: Nozzle openings covered with Teflon or pre-rinsed aluminum foil, and nozzle placed in Ziploc bag.
Probe liner outlet sealed with glass female blank-off, and union sealed with Teflon plug. Cyclone/Bypass inlet covered (not
sealed) with Teflon or pre-rinsed aluminum foil. Vertical traverse adapter (VTA) openings, filter holder outlet, and condenser
inlet sealed with Teflon or glass blank-offs. Sample transfer line (STL) openings joined with glass/Teflon coupling used at filter
holder outlet during sampling.
Optional for moisture gas streams and/or special situations as applicable.
' Cartridge weighed with blank-offs in place; then, cartridge covered with aluminum foil to seal out light during storage and
sampling. Documentation of standards injection is separate. Cartridges are maintained at near 4° until use.
' Initial weights of additional components exchanged during the run also entered here. AH exchange component openings
covered with Teflon or pre-rinsed aluminum foil or as described above.
B2-2
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MR! Project No.; 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBt
Sampling Location:
Run No. -Jp / Sampling Train No. 3->~ I Sample Box No. JQ3-
Set-up persoo(s): A . S. 6r i "{ft A _ Date/Time
TRAIN COMPONENT* __ LOADING DATA
Sampling Nozzle (QuartzMctel) A)
Heated Coupling anci Teflon STL
, //
O ,
Filter Type Whatman QM-A &?3 ~~l 0
Condenser Thermocouple No. X/r.P-7 _
XAD-2 Resin Cartridge spike date rf/efs A?3 _
XAD-2 Resin Cartridge Lab ID***P3/ (,(*- Q\ 3^
Impinger Outlet Connector OH- f _
Initial Weights (grams)"**
v^fN « + • i Empty Loaded
Mu Z&MM0Qp
1st Impinger (500-mL orC-L KO), Empty /.3 V4>. 5
1 st Impinger Replacement** (KO), Empty M/A
2nd Impinger (MGBS), 100 mLs ASTM Type II Water i&*1i (f>
3rd Impinger (GBS), 100 mLs ASTM Type II Water V73.3
4th Impinger (MGBS), Empty VY^.g -J/A
5th Impinger (MGBS), Si Gel
6th Impinger' (MGBS), Si Gel 116 O
COMMENTS:
3
3
(9 /ff
' Before and after sampling: Nozzle openings covered with Teflon or pre-rinsed aluminum foil, and nozzle placed in Ziploc bag.
Probe liner outlet sealed with glass female blank-off, and union sealed with Teflon plug. Cyclone/Bypass inlet covered {not
sealed) with Teflon or pre-rinsed aiuminum foil. Vertical traverse adapter (VTA) openings, filter holder outlet, and condenser
inlet sealed with Teflon or glass blank-offs. Sample transfer line (STL) openings joined with glass/Teflon coupling used at filter
holder outlet during sampling.
Optional for moisture gas streams and/or special situations as applicable.
Cartridge weighed with blank-offs in place; then, cartridge covered with aluminum foil to seal out light during storage and
sampling. Documentation of standards injection is separate. Cartridges are maintained at near 4" until use. V,j ////fti
' Initial weights of additional components exchanged during the run also entered here. All exchange component openings //'
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANiCS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.: 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location:
Run No, ^T Sampling Train No. J- $ " Sample Box No. /
Set-up person(s): A. Sgu^LT.5 Date: %//?/r>*^
Transfer to Sampler: If* -v
Relinquished By .4. OgM^aT-^ Received By D. fcrr? t4i^ Date/Time
TRAIN COMPONENT LOADING DATA
Sampling Nozzle (Qyartz/feke^ f J 1 3 ==Q:jA ff Z
Heated Coupling and Teflon STL**
Filter Type Whatman QM-A/^. 3 -
Condenser Thermocouple No. *)C A D -• / _
XAD-2 Resin Cartridge spike date
XAD-2 Resin Cartridge Lab ID***JP '.?/££•— C?\ Q
Impinger Outlet Connector OK" I _
Initial Weights (grams)**"'
\ek^ a j- • i Empty Loaded
XA£k C^GuJy -
1 st Impinger (500-mL orfc-LT KO), Empty ) ,1 (o
1 st Impinger Replacement" (KO), Empty
2nd Impinger (MGBS), 100 mLs ASTM Type II Water V F V, (j? __S ^
3rd Impinger (GBS), 1 00 mLs ASTM Type 1 1 Water __t/73^% _.___5~.%/> f
4th Impinger (MGBS), Empty
COMMENTS:
5th Impinger (MGBS), Si Gel i.{ g $'. J-^ 7 ( I ,
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.: 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location: ~Dr Sampling Train No. 23 " £• Sample Box No. Qj
Set-up person(s): A. Sft/tntfc/y Date:
Transfer to Sampler: ^ ... .
Relinquished By fj - :>&*J0f$' _ Received By O. 6r/f*T/>a Date/Time
TRAIN COMPONENT* LOADING DATA
Sampling Nozzle (Quartz/Nickejl A5 IX O..7S7"
Heated Coupling and Teflon STL**
Filter Type Whatman QM-A
Condenser Thermocouple No. *^C/i D ~
XAD-2 Resin Cartridge spike date <%/&/(, 3
XAD-2 Resin Cartridge Lab ID
Impinger Outlet Connector (_ ) M - / ^L _
Initial Weights (grams)*"*
Loaded
1 st Impinger (500-mL oi-LF KO), Empty 3 7 7,
1st Impinger Replacement** (KO), Empty /J/
2nd Impinger (MGBS), 100 mLs ASTM Type II Water
3rd Impinger (GBS), 1 00 mLs ASTM Type II Water ^ $ 3, 9
4th Impinger (MOBS), Empty */fr 3. g
COMMENTS:
5th Impinger (MGBS), Si Gel f£t>. (j &,r( '/. 5"
6th Impinger" (MGBS), Si Gel VtiC.I 7/«2 . ^
yco 0 WO* I Vc>° 3
. J
f 000.7
Before and after sampling: Noz2le openings covered with Teflon or pre-rinsed aluminum foil, and nozzle placed in Ziploc bag.
Probe liner outlet sealed with glass female blank-off, and union sealed with Teflon plug. Cyclone/Bypass inlet covered (not
sealed) with Teflon or pre-rinsed aluminum foil. Vertical traverse adapter (VTA) openings, filter holder outlet, and condenser
inlet sealed with Teflon or glass blank-offs. Sample transfer line !STU openings joined with glass/Teflon coupling used at filter
holder outlet during sampling.
-------
40 CFR 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY TRAIN SET-UP DATA
MRI Project No.: 110249.2.001
Client/Source: EPA / Ball Clay
Source Location: CBI
Sampling Location:
Run No. v •ys. pWyvK Sampling Train No. /yf »&? ~"*£ Sample Box No.
Set-up person(s): "^ ^j{^?gO*(&Q& Date:
Transfer to Sampler: .
Relinquished By fl. Sa^t/r/S Received By p. (rrffi'•',* Date/Time $//b/f,3 0 $: /0
TRAIN COMPONENT* LOADING DATA
Sampling Nozzle (Quartz/fck^l) M ""/
Heated Coupling and Teflon STL** p ) ft
Filter Type/gp Whatman QM-A/12-3 "7
Condenser Thermocouple No. XA D ' 2. _
XAD-2 Resin Cartridge spike date *% / *&
XAD-2 Resin Cartridge Lab \0*" P3I(*(,-
Impinger Outlet Connector Off- — >
Initial Weights (grams)****
Empty Loaded
1st Impinger (500-mL orE-L^r KO), Empty p* Q 9. f^
1st Impinger Replacement** (KO), Empty
2nd Impinger (MGBS), 100 mLs ASTM Type II Water "T 7Aff -4 7/t
3rd Impinger (GBS), 100 mLs ASTM Type II Water
4th Impinger (MGBS), Empty
5th Impinger (MGBS), Si Gel
6th Impinger** (MGBS), Si Gel
COMMENTS:
" &>t 9^
'•3
i ^ "i
' Before and after sampling: Nozzle openings covered with Teflon or pre-rinsed aluminum foil, and nozzle placed in Ziploc bag.
Probe 'iner outlet sealed with glass female blank-off, and union sealed with Teflon plug. Cyclone/Bypass inlet covered (not
sealed) with Teflon or pre-rinsed aluminum foil. Vertical traverse adapter (VTA) openings, filter holder outlet, and condenser
inlet sealed with Teflon or glass blank-offs. Sample transfer line (STL) openings joined with glass/Teflon coupling used at filter
holder outlet during sampling.
Optional for moisture gas streams and/or special situations as applicable. *S
' Cartridge weighed with blank-offs in place; then, cartridge covered with aluminum foil to seal out light during storage and
sampling. Documentation of standards injection is separate. Cartridges are maintained at near 4" until use.
' Initial weights of additional components exchanged during the run also entered here. All exchange component openings
covered with Teflon or pre-rinsed aluminum foil or as described above.
B2-7
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
MR! Project No. 11 0249. 2.001
Client/Source: EPA EMC OAQPS/EMAD/ Bail Clay Emissions
Source Location: CBI
Sampling Location:
Run No. f_*t>*f Sampling Train No.
Transfer for Recovery:
Relinquished By5>/>(UL>.'
Sample Box No.
Sample box recovery persorisi:
>.' f-Y
ersoriisi:
Received B
Probe/STL recovery persontsl: ^
Weights below are in grams.
Date/Time
^f
Date:
Date: Sr//3/
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMiVOLATiLE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
MRI Project No. 1 10249.2.001
Client/Source: EPA EMC OAQPS/EMAD/ Bali Clay Emissions
Source Location: CBI '
Source Location: CBI ' . /
Sampling Location: f*\ i [ I
Run No, o*>^ Sampling Train No.
Transfer for Recovery:
Relinquished By /Jp-^tD / ,—.
Sample box recovery pefson(s)r
Probe/STL recovery person(s):
Weights below are in grams.
Sample Box No.
_ Date/Time
..V^^afig
Date:
Date:
l/r /
impinger: XAD-2
Cartridge*
Final Wt. ^
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
MRI Project No.
Client/Source:
Source Location:
Sampling Location:
Run No. j Sampling Train No.
Transfer for Receive
Relinquished By
Sample box recovei"V person
Probe/STL recovery person(s): &r
Weights below are in grams.
If'LQ
Impinger:
Final Wt. $5
Initial Wt.
Net Wt.
XAD-2
Cartridge*
7
Replacement
1st
RESIN CARTRIDGE AND IMPINGERS RECOVERY
4th 5th
6th
Description
and/or color:
U
grams!
Sample Recovery: Cartridge*
Sample Number:
Dispose of properly
% Blue
CYCLONE/FLASK ASSEMBLY:
Sample Number: ^/f^C Description/Color:
FILTER RECOVERY AND TRAIN RINSES,
A///4
Gross Wt.
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
MRI Project No,
Client/Source:
Source Location:
Sampling Location:
Run No. > Sampling Train No. -23 '~'
Transfer for Recovery:
Relinquished By £> . fa cj_£j_m _ Received By _^_L
Sample box recovery person(s): ^.,
Probe/STL recovery person(s): D.
Weights below are in grams.
Sample Box No. / C>3-
Date/Time I// %ft%
_
6r.. -T(,/v
Date:
Date:
RESIN CARTRIDGE AND IMPINGERS RECOVERY
Impinger: XAD-2
Cartridge*
Final Wt, Jf f?. 3
Initial Wt. '$%¥.•%, __
wet wt. y.T
1st
Replacement
1st
2nd
3rd
4th
5th
SM.V
flM
-0.. 5
^.g
3.
Sample Number: M C Q J-, Description/Color:
_ FILTER RECQVERYAND 1RAI_N RINSES,
Gross Wt.
TRAIN RINSES:
FRONT/BACK
QA RINSES
¥
Sample Number: tyOQ i „
Sample Bottle Tare Wt. 3 6. t. 3
Components Rinsed***: Front -- nozzle, union, probe liner, cyclone/flask assembly or bypass, filter holder front;
Back - filter support, filter holder back, 45/90° connector or short 90° connector, condenser
Sample Bottle Final Wt. fo/ 3> o
Net Sample Wt.
. D
* Replace blank-offs and remove aluminum foil, then weigh the cartridge; replace aluminum foil to cover the entire cartridge.
* * If the paniculate matter catch in the cyclone/flask assembly is large, the sample may be left intact for transfer to the
analytical laboratory for recovery. If the sample is not recovered in the field, weight the assembly before shipment,
* * * For TRAIN FRONT/BACK RINSES; Acetone rinses with brushing of front components 3 times or more until
clean, and acetone rinses of back components 3 times, and inoluda 5 minute lenlrn of undarlinod oomponont
For QA RINSES: Follow with toluene rinses and soaks in the same manner as above for the acetone rinses.
COMMENTS: _- -j. : /-' ,?,',, ,- . }
-
'& Zoo. 3.
M23RCV.WD, DecemtierS, 1S99 (rev. Ausuat 7, 20031
B2-11
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMIVOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
MRI Project No.
Client/Source:
Source Location:
Sampling Location:
Run No. _s-2__ Sampling Train No.
Transfer for Recovery:,, J •
Relinquished By O JL3~r (\\ {y\
Sample Box No. /O<
Sample box recovery person(sj:
Probe/STL recovery person(s):
Weights below are in grams.
Received By"
Date/Time
"p. &-f\ -f-4 \ n
Date:
Date:
Irnpinger: XAD-2
Cartridge*
Final Wt.
Initial Wt.
Net Wt.
Description
and/or color:
Sample Recovery: Cartridge*
Sample Number: 5 0 G ~"j
RESIN CARTRIDGE AND IMPINGERS RECOVERY
Replacement £,1 r~
1st 2nd, 3rd® 4th
/U/.4 SSI.H r-Aft-H IT I.
5th
6th
[ Total Condensate Collected: ~3 -J^. 3
7£7
grams)
Dispose of properly
% Blue
FILTER RECOVERY AND TRAIN RINSES
CYCLONE/FLASK ASSEMBLY:
Sample Number: f^/A Description/Color:
Gross Wt. AJ /A
FILTER:
Sample Number: 5 o i
Description/Color:
TRAIN RINSES:
FRONT/BACK
QA RINSES
Sample Number: SCO [
Sample Bottle Tare Wt. 2 Srf, 3 SoQ»S
Components Rinsed***: Front - nozzle, union, probe liner, cyclone/flask assembly or bypass, filter holder front;
Back -- filter support, filter holder back, 45/90° connector or short 90° connector, condenser
Sample Bottle Final Wt.
Net Sample Wt.
(020, |
Replace blank-offs and remove aluminum foil, then weigh the cartridge; replace aluminum foil to cover the entire cartridge.
If the participate matter catch in the cyclone/flask assembly is large, the sample may be left intact for transfer to the
analytical laboratory for recovery. If the sample is not recovered in the field, weight the assembly before shipment.
For TRAIN FRONT/BACK RINSES: Acetone rinses with brushing of front components 3 times or more until perceivably
clean, and acetone rinses of back components 3 times, unfl inrluria fi minutn coal'.t of undcrlinod componnnft 3 timfiff^
For QA RINSES: Follow with toluene rinses and soaks in the san
COMMENTS: -, ^ /»
ie manner as above for the acetone rinses.
5 oo. 3
I OOO, "7
ber 8, !999 a rev, August 7, 20O3]
B2-12
-------
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMIVOLAT1LE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
cftl
MRI Project No.
Client/Source:
Source Location:
Sampling Location:
r
Run No. C/7 Sampling Train No. r- 3 " cr^
Transfer for Recovery: :•. .
Relinquished By D. CTfi.T'» \v\ Received By A-t
Sample Box No. Q j liL.
Sample box recovery person(s):_
Probe/STL recovery person(s):
Weights below are in grams.
6,rA<\*7c.
>\.l
'
Date/Time (6 $5>
Date:. "
Date:
RESIN CARTRIDGE AND IMPINGERS RECOVERY
Impinger: XAD-2
Cartridge*
Final Wt.
Initial Wt.
Net Wt.
1st
Replacement
1st
2nd
3-??,'
57/.
3rd
4th
5th
6th
11.7,0
•6?
Description
and/or color:
Total Condensate Collected: 3 ~7~J*£
C&£L*->
7W
grams]
Sample Recovery: Cartridge*
Sample Number:
Dispose of properly •
% Blue
FILTER RECOVERY AND TRAIN RINSES
CYCLONE/FLASK ASSEMBLY:
Sample Number: £>Z.£t_
Description/Color:
Gross Wt.
FILTER:
Sample Number:
TRAIN RINSES:
4 OO^A Description/Color:
FRONT/BACK
Sample Number:
Sample Bottle Tare Wt.
Components Rinsed***:
Sample Bottle Final Wt.
Net Sample Wt.
A 5_f7,'3.
QA RINSES
feoo-5
SOQ.Q
Front - nozzle, union, probe liner, cyclone/flask assembly or bypass, filter holder front;
Back -- filter support, filter holder back, 45/90° connector or short 90° connector, condenser
go;
Replace blank-offs and remove aluminum foil, then weigh the cartridge; replace aluminum foil to cover the entire cartridge.
If the particulate matter catch in the cyclone/flask assembly is large, the sample may be left intact for transfer to the
analytical laboratory for recovery. If the sample is not recovered in the field, weight the assembly before shipment.
For TRAIN FRONT/BACK RINSES: Acetone rinses with brushing of front components 3 times or more until perceivably
clean, and acetone rinses of back components 3 times, and include D UllflUlU i»uaka ef underlined oomiauiieutj 3 tin*
For QA RINSES: Follow with toluene rinses and soaks in the same manner as above for the acetone rinses.
%>• 3
M23ftCV.WO, DacemberB. 1999 \na. August 7. 2O03)
B2-13
-------
MRI Project No.
Client/Source:
Source Location:
Sampling Location:
40 CFR 60, APPENDIX A, METHOD 23 -
MODIFIED SEMI VOLATILE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD LABORATORY SAMPLE RECOVERY DATA
ito+H1.
Epft-
TL / £xJ! C.^f
Run No. LftM \ Sampling Train No.
Transfer for Recovery:
Relinquished By I!).
FRONT/BACK
/Of f
QA RINSES
Sample Number:
Sample Bottle Tare Wt.
Components Rinsed***: Front -- nozzle, union, probe liner, cyclone/flask assembly or bypass, filter holder front;
Back -- filter support, filter holder back, 45/90° connector or short 90° connector, condenser
Sample Bottle Final Wt.
Net Sample Wt. £1 ~$£>. 3
* Replace blank-offs and remove aluminum foil, then weigh the cartridge; replace aluminum foil to cover the entire cartridge.
** If the participate matter catch in the cyclone/flask assembly is large, the sample may be left intact for transfer to the
analytical laboratory for recovery. If the sample is not recovered in the field, weight the assembly before shipment.
* ** For TRAIN FRONT/BACK RINSES: Acetone rinses with brushing of front components 3 times or more until perceivable.,
clean, and acetone rinses of back components 3 times, and include 5 minute joolto of undarlined oumpuiiuillS 3 UlllHb.
For QA RINSES: Follow with toluene rinses and soaks in the same manner as above for the acetone rinses.
COMMENTS:
M23RCV.WO, December 3. 1999 ^»v. August 7, 2O03)
B2-14
-------
40 Cm 60, APPENDIX A-7, METHOD 23 -
MODIFIED SEMIVOLAT1LE ORGANICS TRAIN (M23) FOR PCDDs/PCDFs
FIELD REAGENT BLANK PREPARATION DATA
MRI Project No. / ( Q3 & 11 C
Source Location: ^CjjyT,
Sampling Location:
Blank(s) Prepared By: /f. ^>ce^<^/> _ Date:
Weights below are in grams.
Sample Bottle Tare Bottle Gross Net Sample
Reagent Blank Description Number __Weight Weight Weight
Acetone to be archived .^
Volume needed: Y/,A mLs ,
Lot Number: fo/A fl/4 A)/,4 A/'/Xj
Toluene to be archived
Volume needed: ..L0O mLs _ — _^
Lot Number: &/\f ^- 5'3? / 3 t£(iQ _i ^^ S~ O •*• Jii I
Filter to be archived (i $(^) ,. ^ A
Type: Whatman QM-A i O/ V •
Lot Number: — ~~~
XAD Cartridge to be archived ' ' *
-------
SAMPLE CONDITION AT FIELD LABORATORY
MRI Project No. :110249.2.001
fo/ f6 Xft-d 5^3
B2-16
-------
SAMPLE CONDITION AT FIELD LABORATORY
MRI Project No. :110249.2.001
B2-17
-------
B2-18
-------
Appendix B-3
Ball Clay Sample Collection
-------
11/24/03 15:08 FAX 919 541 1155
RTI-CEA
BIQPJL_
Source;
Process: 1 =
2 =
Ball Clay Sample Collection Data Sheet
Process Sampling During Emission Test
MRI Project 110249.1.003
Sampling Locatiqn(s):
2 =
3 =
Sample collection person(s):
SAMPLE NUMBER
un
ZUI
^\^\
Si
Collection
Date Time
(0:5-5
5-t>3
COMMENTS
&uf£to£
NOU-24-2003 14:18
919 541 7155
97%
P. 03
B3-1
-------
11/24/03 15:08 FAX 919 541 7155
RTI-CEA
Sg}002
Source:
Process: 1 =
2 =
(^^
Sample collection person(s):
SAMPLE NUMBER
qn
05
03 If
Ball Clay Sample Collection Data Sheet
Process Sampling During Emission Test
MRI Project 110249.1,003
Sampling Location(s)
1 =
2=
3 =
Collection
Date Time
COMMENTS
J2-JU.
u*~
M^rf^ | *\ I
-------
Type & No. of Apparatus
No. XAD Module: 12
Resin Batch No.: (?t"C'
No. PUF: N/A
PUF Batch No.: N/A
Filter Size: 4.9 in.
No. Filters: sending box
Filter Batch No.: fr£T
Spike
Vol. PCDD/F:
Solution ID:^
Vol. HR_PAH
Solution ID:
Vol. HR_PCB
Solution ID:
Vol. LR_PAH
Solution ID:
Vol. SVOST:
Solution ID:
Profile
20jiL
^-^->J;
: 200 p
/
: N/A
N/A
: N/A
N/A
: N/A
N/A
N/A
N/A
(4ng)
g/uL
/«£~
l&j>
7
Air Apparatus Shipping Request
AAP Protect ID: P3166
Following sample recovery,
please return this form with the
field samples to:
ALTA ANALYTICAL PERSPECTIVES
2714 Exchange Drive
Wilmington, NC 28405
Ph.: 910-794-1613
Fax: 910-794-3919
Spiked t
?£yf\V-^ ^
Date: f;?>
Witnessed
by: l^tf
Client Information
Name; MRI
Contact Name: John Hosenfeld
Date Requested: 16JUL2003
Project No.: 110249.2.001.04
Date Required: 11 AUG 201
Ship to:
Attn: John Hosenfeld
Briarwood Inn.
16180 Highland Drive
McKenzie, TN 38201
Ph.: 731-352-1083
Fax: 816-531-0315
Carrier: (Fed Ex> / UPS
Special Requirements
HR_D/Fs
* ALSO SEND 30-8 OUNCE JARS*
*for Saturday delivery*
*add blue ice*
Air Bill No.:
Date Shipped:
Note: 40 g of the same resin is spiked and stored at 4C at
Alta. This sample will serve as the method blank upon
return of the field samples.
B3-3
-------
Appendix B-4
O2 and CO2 Analysis
-------
O2 Measurement System Calibration Data By Method 3A
Job No
Client:
Plant: CBI
Location: Mill
110249.2.001.04
EPA / Ball clay
Operator Daniel Neal
Date: August 13, 2003
Analyzer Type:
Analyzer Span:
Zero Gas:
Cal. Gas Mixture:
Magneto pneumatic
25 %O2 by volume
Signature/Date
Analyzer Mfgr.: Servomex
Model No. 01440CISTD
Prepurlfled nitrogen
Serial No. 1391
Oxygen In nitrogen
Analyzer Calibration Error Determination
Run No. 1 -RE Test Condition:
Calibration
Ending
Time
4:36
4:39
4:42
Calibration Gas
Concentration
Level
Zero Gas
High-range
Mid-range
Value,
%O2
000
21.13
12.02
Cylinder
ID Number
3AA2400
1L2234
ALM036712
Analyzer Response
Value Following
Calibration, %Oj
-003
21.24
12.04
Run Time: Start
5:30
Gas Value - Analyzer
Response Difference
As % of Span
-0.12%
0.44%
0.08%
End
10:48
Cal. Error
Check
Result*
Pass
Pass
Pass
a. Calibration error check must not exceed ±2% of the span value.
Measurement System Calibration Bias, Response Time, and Drift
Initial Bias and Response Time Determinations
Calibration
Ending
Time
4:46
4:49
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
Analyzer
Response,
%02
-003
12.04
System
Response,
%O5
-0.02
12.07
Response
Time",
seconds
24
24
System
Cal. Bias,
% of Span
0.04%
0.12%
Bias
Check
Result"
Pass
Pass
Final Bias and Drift Determinations
Calibration
Ending
Time
11:14
11:17
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
System
Response,
%O2
-0.02
11.86
System
Cal. Bias,
% of Span
0.04%
-0.72%
Bias
Check
Result"
Pass
Pass
Drift,
% of Span
0.00%
-0.84%
Drift
Check
Result4
Pass
Pass
b. Response time check according to Method 3A. The longer time is used.
e. System bias check must not exceed ±5% of the span value.
d. Drift check must not exceed ±3% of the span value.
System Calibration Bias =-
System Cal. Response - Analyzer Cal. Response
Span
Drift = •
Final System Cal. Response - Initial System Cal. Response
Span
• x100
• x100
lnstrmds.xls [3A O2] 03/26/2001 (rev.BallClayRun1DataWorkbook.xls [3A O2] 9/9/2003 3:15 PM)
B4-1
-------
CO2 Measurement System Calibration Data By Method 3A
Job No
Client:
Plant:
Location: Mill
110249.2.001.04
EPA / Ball clay
Operator: Daniel Neal
Date:
CB1
August 13, 2003
Analyzer Type:
Analyzer Span:
Zero Gas:
Cal. Gas Mixture:
single beam, dual wavelength IR
20 %CO2 by volume
P re purified nitrogen
Carbon dioxide in nitrogen
*-' Signature/Date
Analyzer Mfgr: Servomex
Model No. 01440CISTD
Serial No. 1382
Analyzer Calibration Error Determination
Run No. 1-RE Test Condition:
Calibration
Ending
Time
4:36
4:39
4:42
Calibration Gas
Concentration
Level
Zero Gas
High-range
Mid-range
Value,
%COj
O.DO
18.04
10.05
Cylinder
ID Number
3AA2400
1L2234
ALM036712
Analyzer Response
Value Following
Calibration, %CO2
-0.10
17.81
10.29
Run Time: Start End
5:30 10:48
Gas Value - Analyzer
Response Difference
As % of Span
-0.50%
-1.15%
1.20%
Cal. Error
Check
Result*
Pass
Pass
Pass
a. Calibration error check must not exceed ±2% of the span value.
Measurement System Calibration Bias, Response Time, and Drift
Initial Bias and Response Time Determinations
Calibration
Ending
Time
4:46
4:49
Calibration Gas
Concentration
Level
Zero Gas
Mid- range
Analyzer
Response,
%C02
-0.10
10.29
System
Response,
%COj
0.13
10.05
Response
Time',
seconds
21
20
System
Cal. Bias,
% of Span
1.15%
-1.20%
Bias
Check
Result'
Pass
Pass
Final Bias and Drift Determinations
Calibration
Ending
Time
11:14
11:17
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
System
Response,
%C02
0.15
10.20
System
Cal. Bias,
% of Span
1.25%
-0.45%
Bias
Check
Result'
Pass
Pass
Drift,
% of Span
0.10%
0.75%
Drift
Check
Result'1
Pass
Pass
b. Response time check according to Method 3A, The longer time is used,
c. System bias check must not exceed ±5% of the span value.
d. Drift check must not exceed £3% of the span value.
System Calibration Bias =-
System Cal. Response - Analyzer Cal. Response
Span
Drift
Final System Cal, Response - Initial System Cal. Response
Span
x100
x100
T/i
Instrmds.xls [3A C02J 03/26/2001 (rev. Ball Clay Run 1 Data Workbook.xls [3A C02) 9/9/2003 3:27 PM)
B4-2
-------
GEMS Data - Dry Basis
Job No. 110249.1.001.04
Client: JEPAI Ball Clay
Plant: CBi ~ _
Location: Mill 41
Operator: JDaimejjNeal
Date: AugusM3,J!p03
Run No. 1-RE
Time
O2
C02
Time
02
CQ2
5:31
5:32
5:33
5:34
5:35
5:36
5:37
5:38
5:39
5:40
5:41
5:42
5:43
5:44
5:45
5:46
5:47
5:48
5:49
5:50
5:51
5:52
5:53
5:54
5:55
5:56
5:57
5:58
5:59
6:00
6:01
6:02
6:03
6:04
6:05
6:06
6:07
6:08
6:09
6:10
6:11
6:12
6:13
6:14
19.98
19.90
1984
19.85
19.83
19.78
19.81
19.88
19.89
19.89
19.89
19.90
19.88
19.87
19.90
19.88
19.82
19.79
19.81
19.91
19.98
19.96
19.91
19.96
19.96
19.97
19.89
19.88
19.87
19.87
19.86
19.85
19.85
19.91
19.89
19.90
19.89
19.90
19.89
19.83
19.85
19.90
19.87
19.88
0.54
0.75
0.76
0.73
0.73
0.82
0.79
0.58
0.55
0.55
0.52
0.53
0.54
0.66
0.72
0.71
0.74
0.81
0.79
0.70
0.51
0.55
0.52
0.52
0.55
0.55
0.68
0.72
0.74
0.77
0.76
0.76
0.68
0.54
0.53
0.54
0.57
0.52
0.53
0.75
0.78
0.75
0.74
0.74
6:15
6:16
6:17
6:18
6:19
6:20
6:21
6:22
6:23
6:24
6:25
6:26
6:27
6:28
6:29
6:30
6:31
6:32
6:33
6:34
6:35
6:36
6:37
6:38
6:39
6:40
6:41
6:42
6:43
6:44
6:45
6:46
6:47
6:48
6:49
6:50
6:51
6:52
6:53
6:54
6:55
6:56
6:57
6:58
19.86
19.87
19.84
19.33
19.26
19.61
19.96
20.04
20.06
19.94
19.55
19.47
19.77
19.94
20.07
19.86
19.72
19.82
20.08
20.02
19.67
19.57
19.54
19.44
19.60
19.91
19.95
19.92
19.78
19.62
19.64
19.71
19.94
19.92
19.70
19.65
19.69
19.73
19.77
19.87
19.84
19.74
19.75
19.76
0.76
0.61
0.57
0.83
0.85
0.65
0.50
0.55
0.66
0.72
0.90
0.97
0.81
0.71
0.48
0.60
0.63
0.58
0.46
0.51
0.77
0.86
0.90
0.97
0.89
0.74
0.64
0.53
0.62
0.68
0.68
0.61
0.51
0.74
0.87
0.85
0.83
0.84
0.83
0.63
0.58
0.65
0.61
0.59
B4-2
-------
GEMS Data - Dry Basis
Job No.
Client:
Plant:
Location:
110249.1.001.04
EPA / Bail Clay
CBI
Mm a
Operator:
Date:
Run No.
Daniel Neal -
August 13, 2003
1-RE
Time
02
C02
Time
O2
CO2
6:59
7:00
7:01
7:02
7:03
7:04
7:05
7:06
7:07
7:08
7:09
7:10
7:11
7:12
7:13
7:14
7:15
7:16
7:17
7:18
7:19
7:20
7:21
7:22
7:23
7:24
7:25
7:26
7:27
7:28
7:29
7:30
8:01
8:02
8:03
8:04
8:05
8:06
8:07
8:08
8:09
8:10
8:11
8:12
19.79
19.74
19.77
19.73
19.71
19.68
19.69
19.70
19.65
19.72
19.74
19.76
19.78
19.81
19.78
19,75
19.74
19.72
19.69
19.67
19.68
19.75
19,75
19.71
19.73
19.71
19.77
19,74
19.76
19.68
19.70
19.64
19.80
19.82
19.75
19.74
19.85
19.77
19.77
19.74
19.74
19.74
19,77
19.86
0.58
0.76
0.80
0.80
0.83
0.86
0.83
0.81
0.65
0.63
0.61
0.61
0.62
0.58
0.75
0.81
0.85
0.84
0.83
0.82
0.75
0.60
0.57
0.64
0.61
0.60
0.59
0.83
0.80
0.82
0.81
0.86
0.55
0.55
0.68
0.83
0.70
0.78
0.81
0.84
0.81
0.59
0.59
0.53
8:13
8:14
8:15
8:16
8:17
8:18
8:19
8:20
8:21
8:22
8:23
8:24
8:25
8:26
8:27
8:28
8:29
8:30
8:31
8:32
8:33
8:34
8:35
8:36
8:37
8:38
8:39
8:40
8:41
8:42
8:43
8:44
8:45
8:46
8:47
8:48
8:49
8:50
8:51
8:52
8:53
8:54
8:55
8:56
19.85
19.79
19.73
19.62
19.68
19.70
19.70
19.70
19.63
19.68
19.84
19.90
19.87
19.69
19.59
19.59
19.51
19.66
19.78
19.71
19.61
19.53
19.50
19.56
19.65
19.70
19.75
19.69
19.61
19.54
19.51
19.42
19.42
19.47
19.76
19.85
19.74
19.70
19.61
19.65
19.60
19.63
1965
1984
0.53
0.56
0.61
0.74
0.80
0.82
0.87
0.83
0.82
0.74
0.55
0.48
0.52
0.60
0.63
0.62
0.84
0.82
0.72
0.74
0.78
0.86
0.71
0,62
0.57
0.56
0.51
0.55
0.66
0.83
0.82
0.86
0.89
0.86
0.68
0.46
0.55
0.55
0.61
0.63
0.64
0.73
0.79
0.70
B4-4
-------
CEMS Data - Dry Basis
Job No. 110249.1.001.M
Client: EJM7 Ball Clay
ant:
ication:
Time
8:57
8:58
8:59
9:00
9:01
9:02
9:03
9:04
9:05
9:06
9:07
9:08
9:09
9:10
9:11
9:12
9:13
9:14
9:15
9:16
9:17
9:18
9:19
9:20
9:21
9:22
9:23
9:24
9:25
9:26
9:27
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:55
10:26
10:27
10:28
CBI
O2
19.80
1967
19.54
19.52
19.49
19.53
19.53
19.61
19.75
19.77
19.70
19.72
19.73
19.68
19.69
19.68
19.83
19.88
19.87
19.92
19.92
19.88
19.86
19.89
19.86
19.77
19.78
19.91
20.01
20.01
19.98
19.79
19.81
19.83
19.89
19.94
19.89
19.87
19.84
19.80
19.77
19.81
19.80
19.65
CO2
0.75
0.77
0.82
0.76
0.66
0.64
0.63
0.62
0.55
0.55
0.81
0.87
0.83
0.82
0.82
0.86
0.67
0.56
0.57
0.55
0.52
0.54
0.66
0.77
0.75
0.81
0.83
0.77
0.71
0.51
0.53
0.59
0.58
0.58
0.60
0.66
0.72
0.76
0.82
0.82
0.57
0.80
0.77
0.87
Operator:
Date:
Run No.
Time
Daniel Neal o
August 13, 2003
O2
CO2
10:29
10:30
10:31
10:32
10:33
10:34
10:35
10:36
10:37
10:38
10:39
10:40
10:41
10:42
10:43
10:44
10:45
10:46
10:47
10:48
Average:
Minimum:
Maximum:
19.76
19.94
19.91
19.88
19.69
19.59
19.65
19.65
19.71
19.72
19.74
19.72
19.70
19.69
19.80
20.03
20.02
19.90
19.86
19.78
19.77
19.26
20.08
0.66
0.51
0.54
0.56
0.60
0,63
0.70
0.86
0.82
0.81
0.81
0.83
0.83
0.64
0.60
0.43
0.43
0.53
0.59
0.74
0.69
0.43
0.97
3 7///AJ
B4-5
-------
O2 Measurement System Calibration Data By Method 3A
Job No. 110249.2.001.04
Client: ' EPA/
Ball clay
Plant: CBI
Location: Mlttljt
Analyzer Type:
Analyzer Span:
Zero Gas:
Cai. Gas Mixture:
M agnetopneu mafic
25 %O2 by volume
Prepu rifled nitrogen
Oxygen in nitrogen
Operator: Daniel Meal
Date: . August 14. 2003
-an value.
d. Drift check must not exceed ±3% of the span value.
System Calibration Bias =-
System Cai. Response - Analyzer Cal. Response
Span
Drift = •
Final System Cal. Response - Initial System Cal. Response
Span
• xlOO
• X1QQ
T
instrmds.xls [3A O2] 03/26/2001 (rev Ball Clay Run 2 Data Workbook.xls |3A O2] 9/9/2003 3:26 PM)
B4-6
-------
CO2 Measurement System Calibration Data By Method 3A
Job No
Client:
Plant: CBI
Location: Mill
110249.2.001.04
EPA / Ball clay
Operator: Daniel Neal
Date: A August 14,2003
Analyzer Type:
Analyzer Span:
Zero Gas:
CaL Gas Mixture:
single beam, dual wavelength IR
20 %CO2 by volume
Prepurified nitrogen
Carbon dioxide In nitrogen
Signature/Date
Analyzer Mfgr.: Servomex
Model No, 01440CISTD
Serial No. 1382
Analyzer Calibration Error Determination
Run No.
Calibration
Ending
Time
4:23
4:28
4:31
2 Test Condition:
Calibration Gas
Concentration
Level
Zero Gas
High-range
Mid-range
Value,
%CO2
0.00
18,04
10.05
Cylinder
ID Number
3AA2400
1L2234
ALM036712
Analyzer Response
Value Following
Calibration, %CO2
-0.02
17.93
10.00
Run Time: Start End
5:50 10:05
Gas Value - Analyzer
Response Difference
As % of Span
-0.10%
-0.55%
-0.25%
Cal. Error
Check
Result"
Pass
Pass
Pass
a. Calibration error check must not exceed ±2% of the span value.
Measurement System Calibration Bias, Response Time, and Drift
Initial Bias and Response Time Determinations
Calibration
Ending
Time
4:34
4:37
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
Analyzer
Response,
%CQ2
-0.02
1000
System
Response,
%C02
-0.15
9,82
Response
Time'1,
seconds
21
20
System
Cal. Bias,
% of Span
-0.65%
-0.90%
Bias
Check
Result1
Pass
Pass
Final Bias and Drift Determinations
Calibration
Ending
Time
10:36
10:39
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
System
Response,
%C02
0.14
9.89
System
Cat. Bias,
% of Span
0.80%
-0.55%
Bias
Check
Result"
Pass
Pass
Drift,
% of Span
1.45%
0.35%
Drift
Check
Result'
Pass
Pass
b. Response time check according to Method 3A. The longer time is used.
c. System bias check must not exceed ±5% of the span value.
d. Drift check must not exceed ±3% of the span value.
System Calibration Bias =-
System Cal. Response - Analyzer Cal. Response
Span
Drift =
Final System Cal. Response - Initial System Cal. Response
Span
• x 100
x 100
lnstrmds.xls [3A CO2] 03/26/2001 (rev. Bail Clay Run 2 Data Workbook.xls [3A CO2] 9/W2003 3:26 PM)
B4-7
-------
OEMS Data - Dry Basis
Job No. 110249,1.001,04
Client: EPA/Ball Clay
Plant: CBI
Location: Mill .1
Operator Daniel Meal ^. A/ 7?
Date: AugusM4,2003
Run No, 2
Time
O2
C02
Time
O2
CO2
5:51
5:52
5:53
5:54
5:55
5:56
5:57
5:58
5:59
6:00
6:01
6:02
6:03
6:04
6:05
6:06
6:07
6:08
6:09
6:10
6:11
6:12
6:13
6:14
6:15
6:16
6:17
6:18
6:19
6:20
6:21
6:22
6:23
6:24
6:25
6:26
6:27
6:28
6:29
6:30
6:31
6:32
6:33
6:34
19,64
19.61
19.56
19.51
19.55
19.67
19.74
19.78
19.72
19.73
19.65
19.58
19.65
19.70
19.84
19.83
19.75
19.70
19.56
19.54
19.57
19.66
19.83
19.81
19.79
19.77
19.74
19.67
19.63
19.62
19.74
19.80
19.82
19.73
19.69
19,63
19.65
19,77
19.81
19.85
19.90
19.72
19.62
19.49
0.63
0.63
0.69
0.87
0.88
0.81
0.78
0.75
0.84
0.63
0.61
0.63
0.61
0.59
0.54
0.64
0.75
0.78
0.82
0.87
0,85
0.80
0.54
0.54
0.52
0.55
0.56
0.64
0,74
0.81
0.79
0.79
0.74
0.78
0.73
0.64
0.62
0.56
057
0.54
0.50
0.76
0.83
0.93
6:35
6:36
6:37
6:38
6:39
6:40
6:41
6:42
6:43
6:44
6:45
6:46
6:47
6:48
6:49
6:50
6:51
6:52
6:53
6:54
6:55
6:56
6:57
6:58
6:59
7:00
7:01
7:02
7:03
7:04
7:05
7:06
7:07
7:08
7:09
7:10
7:11
7:12
7:13
7:14
7:15
7:16
7:17
7:18
19.59
19.60
19.74
19,78
19.84
19.79
19.75
19.59
19.61
19.62
19.69
19.78
19,81
19.81
19.65
19.40
19.59
19.71
19.77
19.79
19.73
19.69
19.58
19.54
19.50
19.60
19.63
19.68
19.73
19,76
19,74
19.70
19.63
19.62
19.67
19.69
19.64
19.66
19.69
19.70
19.64
19.67
19,69
19.70
0.83
083
0.80
0.65
054
0.55
0.61
0.62
0.61
0.66
0.83
0.77
0.74
0.72
0.84
0.93
0.69
0.62
0.59
0.54
0.57
0.60
0.77
0.86
0.88
0,84
0.83
0.82
0.77
0,59
0.57
0.58
0.61
0.65
0.64
0.77
0.82
0.83
0.82
0.81
0.84
0.76
0.60
0.59
*3
B4-8
-------
OEMS Data - Dry Basis
Job No.
Client:
Plant: CBJ
Location: Mill
Operator: Daniel Neal
Date: August 14,2003
Run No, 2
Time
02
CO2
Time
O2
C02
7:19
7:20
7:21
7:22
7:23
7:24
7:25
7:26
7:27
7:28
7:29
7:30
7:31
7:32
7:33
7:34
7:35
7:36
7:37
7:38
7:39
7:40
7:41
7:42
7:43
7:44
7:45
7:46
7:47
7:48
7:49
7:50
8:06
8:07
8:08
8:09
8:10
8:11
8:12
8:13
8:14
8:15
8:16
8:17
19.74
19.69
19.72
19.73
19.66
19.64
19.71
19.71
19.68
19.66
19.71
19.74
19.67
19.72
19.77
19.80
19.80
19.70
19.74
19.65
19.48
19.61
19.65
19.78
19.60
19.66
19.75
19.76
19.74
19.71
19.63
19.59
19.71
19.51
19.24
19.57
19.78
19.92
19.92
19.81
19.30
19.52
19.70
19.86
0.56
0.64
0.59
0.60
0.80
0.83
0.79
0.80
0.84
0.84
0.62
0.57
0.61
0.60
0.54
0.52
0.61
0.76
0.77
0,82
0.89
0.83
0.80
0.53
0.65
0.59
0.52
0.53
0.54
0.66
0.82
0.84
0.76
0.75
0.76
0.60
0.50
0.43
0.45
0.59
0.99
0.87
0.79
0.71
8:18
8:19
8:20
8:21
8:22
8:23
8:24
8:25
8:26
8:27
8:28
8:29
8:30
8:31
8:32
8:33
8:34
8:35
8:36
8:37
8:38
8:39
8:40
8:41
8:42
8:43
8:44
8:45
8:46
8:47
8:48
8:49
8:50
8:51
8:52
8:53
8:54
8:55
8:56
8:57
8:58
8:59
9:00
9:01
19.95
19.90
19.81
19.39
19.55
19.83
1994
2003
19,93
19,79
19.33
19.53
19.68
19.85
19.88
19.91
19.79
19.70
19.64
19.60
19,68
19,78
19,79
19.79
19.76
19.76
19.72
19.66
19.65
1969
19.69
19.77
19,82
19.74
1965
19.66
19.60
19.68
19.78
19.77
19.75
19.71
19.71
19.67
0.73
0.73
0.57
0.74
0.66
0.52
0.47
0.45
0.61
0.75
0.96
0.90
0.87
0.74
0.69
0.50
0.56
0.59
0.63
0.65
0.59
0.68
0.72
0.76
0.78
0.75
0.77
0.74
0.60
0.58
0.57
0.57
0.51
0.53
0.76
0.82
0.85
0.82
0.73
0.77
0.61
0.58
0.58
0.63
B4-9
-------
GEMS Data - Dry Basis
Job No. 110249.1.001,04
Client: EPA / BaJ Clay
Plant: CBI
Location: MillNV
Operator: Daniel Neal
Time
02
CO2
9:02
9:03
9:04
9:05
9:06
9:07
9:08
9:09
9:10
9:11
9:12
9:13
9:14
9:15
9:16
9:17
9:18
9:19
9:20
9:21
9:22
9:23
9:24
9:25
9:26
9:27
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
9:39
9:40
9:41
9:42
9:43
9:44
9:45
19.73
19.66
19.81
19.84
19.81
19.58
1922
19,57
1962
19.75
19.85
19.77
19.55
19.52
19.51
19.54
19.57
19.72
19.61
19.59
19.70
19.60
19.38
19.64
19.69
19.77
19.69
19.64
19.53
19.55
19.59
19.56
19.59
19.56
19.54
19.55
19.55
19.59
19.57
19.61
19.59
19.55
19.49
19.45
0.54
0.56
055
0.71
073
0,82
0.97
0,84
0.79
0.55
0.48
0.55
0.60
0.61
0.62
0.75
0.82
0.74
0.82
0.83
0.75
0.80
0.74
0.61
0.55
0.52
0.52
0.58
0.79
0.83
0.83
0.83
0.81
0.82
0.76
0.65
0.61
0.57
0.57
0.56
0.57
0.81
0.85
0.84
Date:
Run No,
Time
9:46
9:47
9:48
9:49
9:50
9:51
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10:03
10:04
10:05
Average:
Minimum:
Maximum:
August 14,
2
O2
19.48
19.40
19.49
19.49
19.56
19.55
19.51
19.42
19.52
19.53
19.62
19.67
19.68
19.61
19.54
19.58
19.64
19.66
19.70
19.64
19.67
19.22
20.03
2003
CO2
0.82
0.85
0.83
0.73
0.57
0.59
0.61
0.63
0.59
0.63
0.82
0.82
0.78
0.81
0,84
0.85
0.65
0.57
0.56
0.57
0.69
0.43
0.99
B4-10
-------
O2 Measurement System Calibration Data By Method 3A
Job No
Client:
Plant: CBI
Location: Mill
110249.2.001.04
EPA / Ball clay
Operator: Daniel Neal
Date:
August 15, 2003
Analyzer Type:
Analyzer Span:
Zero Gas:
Cal. Gas Mixture:
Magnetopneumatic
25 %O2 by volume
Signature/Date
Analyzer Mfgr,: Servomex
Model No. 01440CISTD
Prepu rifled nitrogen
Serial No 1391
Oxygen In nitrogen
Analyzer Calibration Error Determination
Run No. 3 Test Condition:
Calibration
Ending
Time
5:03
5:07
5:10
Calibration Gas
Concentration
Level
Zero Gas
High-range
Mid-range
Value,
%02
0.00
21.13
12.02
Cylinder
ID Number
3AA2400
1L2234
ALM036712
Analyzer Response
Value Following
Calibration, %C^
-0,13
21.18
12.04
Run Time: Start End
6:10 10:20
Gas Value - Analyzer
Response Difference
As % of Span
-0.52%
0.20%
0.08%
Cal. Error
Check
Result9
Pass
Pass
Pass
a. Calibration error check must not exceed ±2% of the span value.
Measurement System Calibration Bias, Response Time, and Drift
Initial Bias and Response Time Determinations
Calibration
Ending
Time
5:14
5:20
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
Analyzer
Response,
%02
-0.13
12.04
System
Response,
%O2
-0.04
12.06
Response
Tlmeb,
seconds
24
24
System
Cai. Bias,
% of Span
0.36%
0.08%
Bias
Check
Result2
Pass
Pass
Final Bias and Drift Determinations
Calibration
Ending
Time
10:44
10:47
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
System
Response,
%O2
-0.11
11.88
System
Cal. Bias,
% of Span
0.08%
-0.64%
Bias
Check
Result"
Pass
Pass
Drift,
% of Span
-0.28%
-0.72%
Drift
Check
Result"
Pass
Pass
b. Response time check according to Method 3A. The longer time is used.
c. System bias check must not exceed 15% of the span value.
d. Drift check must not exceed £3% of the span value.
System Calibration Bias =-
System Cal. Response - Analyzer Cal. Response
Span
Drit = •
Final System Cal. Response - Initial System Cal. Response
Span
x100
X100
instrrnds.xls [3A 02] 03/26/2001 (rev, BallClayRuns1-3DataWorkbook.xls [3A 02] 9/9/2003 3:32 PM)
B4-11
-------
CO2 Measurement System Calibration Data By Method 3A
Job No.
Client:
Plant: CBI
Location: Mill
110249.2.001.04
EPA / Ball clay
Operator Daniel Neal
Date: August 1S, 2003
W
Analyzer Type:
Analyzer Span:
Zero Gas:
Cat Gas Mixture:
single beam, dual wavelength IR
20 %CO2 by volume
Signature/Date
Analyzer Mfgr.: Servomex
Model No. 01440CISTD
Prepu rifled nitrogen
Serial No. 1382
Carbon dioxide In nitrogen
Analyzer Calibration Error Determination
Run No. 3 Test Condition:
Calibration
Ending
Time
5:03
5:07
5:10
Calibration Gas
Concentration
Level
Zero Gas
High-range
Mid-range
Value,
%C02
0.00
18.04
10.05
Cylinder
ID Number
3AA2400
1L2234
ALM036712
Analyzer Response
Value Following
Calibration, %CO2
0.15
17.80
10.03
Run Time: Start End
6:10 10:20
Gas Value - Analyzer
Response Difference
As % of Span
0.75%
-1.20%
-0.10%
Cal. Error
Check
Result'
Pass
Pass
Pass
a. Calibration error check must not exceed 12% of the span value,
Measurement System Calibration Bias, Response Time, and Drift
Initial Bias and Response Time Determinations
Calibration
Ending
Time
5:14
5:20
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
Analyzer
Response,
%C02
0.15
10.03
System
Response,
%C02
0.13
9.90
Response
Time',
seconds
21
20
System
Cal. Bias,
% of Span
-0.10%
-0.65%
Bias
Check
Result1
Pass
Pass
Final Bias and Drift Determinations
Calibration
Ending
Time
10:44
10:47
Calibration Gas
Concentration
Level
Zero Gas
Mid-range
System
Response,
%C02
0.16
10.09
System
Cal. Bias,
% of Span
0.05%
0.30%
Bias
Check
Result"
Pass
Pass
Drift,
% of Span
0.15%
0.95%
Drift
Check
Result"1
Pass
Pass
b. Response time check according to Method 3A. The longer time is used,
c. System bias check must not exceed iS% of the span value.
d. Drift check must not exceed ±3% of the span value.
System Calibration Bias
Drift
System Cal. Response - Analyzer Cal. Response
Span
Final System Cal. Response - Initial System Cal. Response
Span
•xlOO
x100
lnstrmds.xls [3ACO2) Q3/26/20G1 (rev.BallClayRuns1-3DataWorkbook.xls [3ACO2] 9/9/2003 3:35 PM)
B4-12
-------
GEMS Data - Dry Basis
Job No. 110249.1.001.04
Client EPA / Ball Clay
Plant: CBI ^~
Location: _Mii|g_J
I , i /> Q f
Operator: ^nten^e^^j^/• s\/. / —/-'
Date: AugusMS, 2003 ^11
Run No. 3
Time
02
CO2
Time
O2
C02
6:11
6:12
6:13
6:14
6:15
6:16
6:17
6:18
6:19
6:20
6:21
6:22
6:23
6:24
6:25
6:26
6:27
6:28
6:29
6:30
6:31
6:32
6:33
6:34
6:35
6:36
6:37
6:38
6:39
6:40
6:41
6:42
6:43
6:44
6:45
6:46
6:47
6:48
6:49
6:50
6:51
6:52
6:53
6:54
19.82
19.56
19.72
20.01
19.73
19.50
19.54
20.00
19.66
19.50
19.58
19.90
19.86
19.63
19.62
19.83
19.96
19.65
19.62
19.82
20.05
19.76
19.57
19.78
20.09
19.75
19.66
19.71
20.04
19.95
19.66
19.63
19.60
19.79
20.00
19.69
19.66
19.66
19.61
19.76
20.08
19.80
19.63
19.59
0.54
0.63
0.58
0.44
0.69
0.85
0.84
0.63
0.83
0.88
0.78
0.52
0.51
0.62
0.62
0.53
0.45
0.76
0.82
0.77
0.61
0.75
0.83
0.67
0.39
0.57
0.60
0.58
0.40
0.50
0.82
0.83
0.82
0.73
0.67
0.80
0.63
0.62
0.63
0.55
0.40
0.55
0.74
0.81
6:55
6:56
6:57
6:58
6:59
7:00
7:01
7:02
7:03
7:04
7:05
7:06
7:07
7:08
7:09
7:10
7:11
7:12
7:13
7:14
7:15
7:16
7:17
7:18
7:19
7:20
7:21
7:22
7:23
7:24
7:25
7:26
7:27
7:28
7:29
7:30
7:31
7:32
7:33
7:34
7:35
7:36
7:37
7:38
19.75
19.91
19.66
19.64
19.68
19.72
19.78
19.98
19.90
19.72
19.79
20.01
19.68
19.59
19.60
20.03
19.95
19.67
19.69
19.66
20.02
20.08
19.74
19.64
19.69
20.04
19.98
19.69
19.75
20.00
20.00
19.58
19.91
19.98
19.76
19.77
19.84
19.93
19,73
19.61
19.59
19.79
20.00
19.72
0.76
0.69
0.85
0.83
0.74
0.59
0.54
0.44
0.49
0.58
0.52
0.58
0.80
0.86
0.81
0,59
0.67
0.72
0.60
0.60
0.42
0.37
0.53
0.66
0.80
0.59
0.61
0.79
0.79
0.63
0.43
0.62
0.47
0.43
0.54
0.55
0.60
0.61
0.73
0.84
0.81
0.70
0.56
0.59
B4-13
-------
Job No. 110249J.p01.04
Client: §PA7B^jhClay_
Plant: CB\ ~
Location: Mill A
CEMS Data - Dry Basis
Operator:
Date:
Run No.
Daniel Neal
-------
GEMS Data - Dry Basis
Job No.
Client:
Plant
Location:
110Z49.JI.p01.04
EPA/ Ball Clay
"
Operator: Daniel Neal_ $. A/-_f' ?~
Date: AugusM5^j2003
Run No. 3
Time
02
CO2
Time
O2
CO2
9:17
9:18
9:19
9:20
9:21
9:22
9:23
9:24
9:25
9:26
9:27
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
9:39
9:40
9:41
9:42
9:43
9:44
9:45
9:46
9:47
9:48
9:49
9:50
9:51
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
20.05
19.95
19.70
19.94
20.08
20.04
19.82
19.75
19.96
20.00
19.81
19.53
19.69
19.85
20.00
19.96
19.80
19.67
19.93
20.00
19.94
19.76
19.83
19.91
19.90
19.83
19.79
19.93
20.03
20.02
19.80
19.80
19.93
19.97
19.90
19.60
19.70
19.80
19.85
19.84
19.81
19.80
19.96
19.98
0.57
0.59
0.60
0.47
0.36
0.40
0.50
0.52
0.61
0.61
0.71
0.81
0.74
0.68
0.51
0.43
0.50
0.57
0.45
0.41
0.49
0.73
0.69
0.63
0.66
0.74
0.72
0.45
0.41
0.43
0.51
0.53
0.44
0.54
0.64
0.82
0.79
0.71
0.66
0.62
0.55
0.53
0.44
0.42
10:01
10:02
10:03
10:04
10:05
10:06
10:07
10:08
10:09
10:10
10:11
10:12
10:13
10:14
10:15
10:16
10:17
10:18
10:19
10:20
Average:
Minimum:
Maximum:
19.93
19.76
19.66
19.79
19.94
20.00
19.76
19.78
19.78
19.92
19.98
19.98
20.06
20.03
19.82
19.74
19.88
19.96
20.00
19.95
19.84
19.37
2021
0.47
0.52
0.76
0.72
0.65
0.61
071
073
0.63
0.47
0.43
044
0.35
0.39
0.55
0.76
0.65
0.62
0.61
0.64
0.60
0.33
0.96
B4-15
-------
ORSAT ANALYSIS DATA SHEET
(Dry Molecular Weight Determination)
Plant
Dale
Operator
Sampling Time
C0Z
&-/&-03
2)jffrJ''$i. A&Oi-
/S'Ji
Sampling Location
Run Number
Analyjjoal Method
((yrite^orsatjnjomlof)
Samole^IxP6
(bag,(ml£2ra(ej?, continuous)
/)^yt> ^
— — • •
Run 3
Net
i
n.i
— - — *.
Average
Net
Volume
. 3
/?/?
Multiplier
0.44
0.32
1L2&— —
0.28
Molecular Weight
Fraction of Stack Gas
(Dry Basis)
Ib/lb-mole
0 13^
& 1^1
Comments:
TOTAL=
B4-16
-------
ORSAT ANALYSIS DATA SHEET
(Dry Molecular Weight Determination)
Plant
Date
Operator
Sampling Time
6-
Sampling Location
Run Number
Analytical Method
(bag, ^nte
; continuous)
r
Sorbing Reauents: (CO.) . (O2) (CO)
RUN
GAS
CO2
O2 (Net is actual O2 reading
minus actual CO2 reading)
CO (Nel a actual CO reading
minus actual O2 reading)
NI (Nel is 100 minus actual
CO reading)
Run 1
Actual
Reading
„ 2-
Jl.J
^_
Run 1
Net
. 2-
/f7
Run 2
Actual
Reading
,• >^
/9,9
Run 2
Net
, *-
/9-1
Run 3
Actual
Reading
. 2^
/?,<}
Run 3
Net
, ^
/f.7
Average
Net
Volume
. 2^
n.i
Multiplier
0.44
0.32
0.28
0.28
Molecular Weight
Fraction of Slack Gas
(Dry Basis)
Ib/lb-mole
0 *%$
6 .'M
Comments:
TOTAL =
B4-17
-------
ORSAT ANALYSIS DATA SHEET
(Dry Molecular Weight Determination)
Plant
Date
Operator
Sampling Time
£1#I
8-70-*$
$4«jii*t /W*«-
/^xr
Sampling Location
Run Number
Analytical Method
(fyrile, usatf monitor)
Sampl&Jwe
{tag,(|nleg£5»l.e
/f.e
Run 2
Actual
Reading
.>
0* .*
Run 2
Net
<>
/?.*
Run 3
Actual
Reading
.j-
"%$£-
j*o . ^
Run 3
Net
->-
/f,g
Average
Net
Volume
- 'Is
,
-------
OXYGEN AND CARBON DIOXIDE BY ORSAT
' rj., Ji?/,£>j*
**
te
RAMP1FND VA DATE 8-10-03 DHDrrrrr /£t/
PLANT SAMPLING LOCATK
ANALYSIS TIME (24hr-CLCK
SAMPLE TYPE (BAG, GRA
/"vpCpAT^P \S ' f\s{*
\>. RUN
GAS ^\^
C02
02 (NET IS SECOND
READING MINUS ACTUAL
COg READING)
IN ^Wc'/L ,5r<'C/v mnrTrro /?.«
>IA 0$">°
ORSAT LEAK CHECK AFTEI
RliDPTTC /WJ-f r
* *~^ PIPFTTF^ /^^^ r
i
ACTUAL
READING
1 /
2 /y/>c —
3
tS
NET
-~— -
**
2
ACTUAL
READING
1
3
1 >o.S
2H .*
3 x>. a
NET
~
>*>. P
3
ACTUAL
READING
1
2
^y .—mi
o
3 >« - 8
NET
—
"'
Ht ANALYSIS:
HANGEJN4MIN
HANGEIN4MIN
^ANALYSIS:
HANGEIN4yiN
HANGEIN4ytN
NET
VOLUME
— >
^
91 16 SEY SUHMWlHM 052191
Acceptance Criteria
CO 2 >4% .3% by Volume 02 215% .2% by Volume
£4% .2% by Volume <15% ,3% by Volume
Comments:
B4-19
-------
Appendix C
Field Sampling Equipment Calibration Records
-------
Appendix C-1
Pre-Test Calibration Records
-------
MS Console Pre-Calibration Checklist
Job No,
Console No.
110249,2.001.04
N7
Date
Performed By
Augusts, 2003
Parrel Sprague
(Place an "X" in the space provided after the required checks are performed.)
Perform positive leak check of Delta H manometer.
Procedure for positive leak cheek Delta H manometer:
Pump must not be run prior to this test. Pump needs to be cool in order to get an accurate reading.
Pump pressure and vacuum lines must be connected to console.
Null switch on console must be in the down position so solenoid valve is open to the sampling
stream as it is during testing.
Plug meter exhaust and clamp off bottom tube from exhaust which goes to the Great pump.
Plug sample orifice.
Close main flow control valve.
Open fine control valve.
Disconnect right side Delta H manometer tube on front of console.
Blow into tubing until manometer reads 5 to 7 inches of water, and ciamp off.
There should be no change in manometer reading.
10.
test to avoid damage to the meter cumo when oumo is started UD!
2.
3,
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
X
N/A
X
X
X
(Note:
within
X
'._*_
X
X
X
X
X
X
Leak check Delta P manometer.
Clean pump
Clean muffler jar(s).
Inspect/refill oiler jar.
Calibrate DGM thermocouples: Reference
0
Reading must be
+/-2.5°F
DGM Inlet: 75
DGM Outlet: 7S
Pyrometer Console Pyrometer
F °F
.4 80.0
.4 80.0
Digital clock/timer in place and functional.
Vacuum check. (Leak check at 25 in. Hg. Vacuum. Leak rate should be zero)
Check indicator lights
Check thermocouple switches.
Check fan.
Check pump heater.
check heat controllers.
Check Orsat pump and rotameter.
If any of the above items were replaced or repaired, please document that information below:
Signature:
Date:
Cl-1
-------
ANEROID BAROMETER CALIBRATION CHECK
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude: 39° 05,8' north
Meteorological Gravity: 32.1525 feet/seconcP
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lot 791802000
MRI Project No. 110249.2.001.04
Date; 37840
Time: 10:21
Readings Obtained By: Daniel Neal ''
Observed Barometer Reading: 29.33 in. Hg
Mercury Column Temperature: 81 °F
Correction For Temperature: -0.14 in. Hg
Correction For Gravity: -0.02 in. Hg
Corrected Barometric Pressure: 29.17 in. Hg
Aneroid Barometer i.D. No.: X-4029
Reading Before Adjustment: 29.18 in. Hg
Calibration Check Result: within 0.1 in. Hg
Reading After Adjustment: ^~?« I** in. Hg
Remarks:
BAROMETR.xls 10/27/99 (rev. Equipment Calibration Workbook.xls 8/7/2003 10:25 AM)
Cl-2
-------
MERCURY BAROMETER PRESSURE READING CORRB
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude: 39° 05,8' north
Meteorological Gravity: 32.1525 feet/second2
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lc
MRI Project No. 110249.2.001.04
Date: Augusts, 2003
Time: 0.647916667
Readings Obtained By: Darrel Sprague
Observed Barometer Reading: 29,24 in. Hg
Mercury Column Temperature: 81 °F
Correction For Temperature: -0.14 in. Hg
Correction For Gravity: -0.02 in, Hg
Corrected Barometric Pressure: 29,08 in. Hg
Remarks:
Signature:
Date:
BAROMETR.xls 10/27/99 (rev. N7 Pretest Calibration Workbook,xis 8/7/2003 3:14 PM)
Cl-3
-------
MS Console Calibration Worksheet
Job No, 110249.2.001.04 Metering Console No N7
Date August 6, 2003 Previous Dry Gas Meter Factor (Y): -| QQ2
Operator Parrel Sprague Calibrated Critical Orifice No. Q24
Barometer 29.08 in. Hg. Critical Orifice Coefficient in English Units (K'): 06417
Ambient Temperature Meter No, 810
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18,0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18.0 in, Hg. +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: JL4_ + 8.6 = 18.00 in, Hg.
Console vacuum gauge reading: 17.00 in. Hg.
console vacuum gauge correction factor 1,00 in. Hg.
DGM Initial Volume:
DGM Inlet Temperature: Initial:
Final:
DGM Outlet Temperature: Initial:
Time of run (In seconds):
Orifice Delta H (in. H2O):
Room Temperature:
Pump Vacuum (in. Hg.):
Initial:
Final.
Initial:
Final:
Initial:
Final:
Initial:
Final:
RUN#1
678.798
687.172 _
83
83
81
81
600
2.15
80.8
81.4
18.0
RUN #2
687,172
695.573
84
86
81
82
600
2.15
81,2
81.4
18,0
RUN #3
695.573
703.965
87
_^_8Z___.
83
82
600
2.15
81,8
82.4
18.0
Signature: W rtMMAt^ Date:
Cl-4
-------
METHOD 5 METERING CONSOLE CALIBRATION WITH CRITICAL ORIFICE
MR! Project No.
Date:
Operator:
1102492001.04
August 6, 2003
Darrel Sprague
Critica
Metering Console No.
Previous Dry Gas Meter Factor (Y):
Calibrated Critical Orifice No.
Orifice Coefficient in English Unite (K1):
I Ambient Temperature Meter No.
N7
1.002
D24
0.64170
81.0
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Meter Gas Volume, ft.3
Final Dry Gas Meter Gas Volume , ft.'
Net Dry Gas Mater Gas Volume (\Q, ft.3
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, °F:
Initial Inlet Temperature, °F
Final Inlet Temperature, °F
Initial Outlet Temperature, °F
Final Outlet Temperature, °F
Average Dry Gas Meter Temperature (t,J, °F
Time, seconds
Orifice Meter AH, inches h^O
Barometric Pressure, in. Hg
Critical Orifice Inlet (Ambient) Temperature, °F:
Initial Ambient Temperature, °f
Final Ambient Temperature, °F
Avg. Critical Orifice Inlet Temperature (^i, °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume (\4r«u))> standard ft.3
Dry Gas Meter Gas Volume (Vn (SM1), standard ft?
Dry Gas Meter Calibration Factor (Y)
Orifice Meter AH @
AVERAGE CALIBRATION RESULTS
Average Dry Gas Meter Calibration Factor (Y
Average Orifice Meter /H@
CALIBRATION RESULTS COMPARISON
Criterion: Y Must Be Within 2% Of Average Y
Percent Difference Of Y From Average Y
Tolerance Result
COMPARISON WITH PRETEST RESULTS
Criterion: Y Must Be Within 5% Of Previous Y
% Difference Of Average Y From Previous Y
Tolerance Result
Y = 1 K)6970&«S564950
Run 1
678.798
687.172
8.374
83.0
83.0
81.0
81.0
82.0
600
215
29.08
' ,
80.8
81.4
81.1
18.0
8.025
7.971
1.007
1.798
1,007
1.794
0.03%
PASS
0.50%
PASS
Run 2
687.172
695.573
8.401
84.0
86.0
81.0
82.0
B3,3
600
2.15
29.08
81.2
81.4
81.3
18.0
8023
7.979
1.006
1.794
0.14%
PASS
Run 3
695.573
703.965
8.392
87.0
87.0
83.0
82.0
84.8
600
2.15
29.08
81.8
82.4
82.1
18.0
8,017
7.948
1,009
1,792
0.17%
PASS
Remarks;
Signature:
Date:
CRORCALB.xls 10/29/99 (rev. N7 Console Calibration V\forkbook.xls 8/7/2003 3:11 PM)
Cl-5
-------
MS Console Critical Orifice Bracketing Worksheet
MRI Project No.
Date:
Operator:
Metering Console No.
Dry Gas Meter Factor (Y):
Orifice Used for the Calibration:
Ambient Temperature Meter No.
110249.2.001.04
August 6, 2003
Parrel Sprague
N7
1,006970646
D24
81.0
Critical Orifice Being Evaluated D24
First Critical Orifice No, D30
Coefficient (Kr): 0.8202
Second Critical Orifice No. D21
Coefficient (K1): _ 0.5693
Note: Critical orifice coefficients are in English units.
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18.0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18.0 in. Hg, +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: 8.4 + 8.6 =
Console vacuum gauge reading:
console vacuum gauge correction factor:
DGM Initial Volume:
DGM Inlet Temperature: Initial:
Final:
DGM Outlet Temperature: Initial:
Time of run (In seconds):
Orifice Delta H (in, H2O):
Room Temperature:
Pump Vacuum (in. Hg.):
Signature:
.6 =
jading:
factor:
Initial:
Final:
Initial:
Final:
Initial:
Final:
Initial:
Final:
18.00 in. Hg.
17.00 in. Hg.
1.00 in. Hg.
RUN#1
709.302
720.057
88
90
84
84
600
3.50
82.0
82.8
18.0
RUN #2
720.400
727.855
88
89
85
86
600
1.70
83.0
82.6
18,0
Date:
Cl-6
-------
METHOD 5 METERING CONSOLE CALIBRATION
CRITICAL ORIFICE BRACKETING DATA
MRI Project No.
Date:
Operator:
Metering Console No.
Dry Gas Meter Factor (Y);
Orifice Used for the Calibration:
Ambient Temperature Meter No,
110249.2.001,04
August 6, 2003
Darrel Sprague
N7
1.007
D24
81,0
Note: Critical orifice coefficients are in English units.
Critical Orifice Being Evaluated
Critical Orifice No.
D24
Critical Orifices Used For Bracketing
First Orifice
Critical Orifice No.
Coefficient («'):
Second Orifice
Critical Orifice No.
Coefficient (K1):
D30
0,82020
D21
0.56930
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Meter Gas Volume, ft3
Final Dry Gas Meter Gas Volume, ft.3
Net Dry Gas Meter Gas Volume (VJ, ft.3
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, °F:
Initial Inlet Temperature, "F
Final Inlet Temperature, °F
Initial Outlet Temperature, °F
Final Outlet Temperature, *F
Average Dry Gas Meter Temperature (y, °F
Time, seconds
Orifice Meter AH, inches H20
Barometric Pressure, in. Hg
Critical Orifice Inlet (Ambient) Temperature, °F:
Initial Ambient Temperature, °F
Final Ambient Temperature, "F
Average Critical Orifice Inlet Temperature (tani °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume {Vcr(std)), standard ft,3
Dry Gas Meter Gas Volume (V,,, jstd)), standard ft.3
Factor (Y) Obtained With Bracketing Orifice
CRITICAL ORIFICE ACCEPTABILITY
Criterion: A/I Ys Must Be Within 2% Of Ail Other Ys
Larger % Difference Between Dry Gas Meter Factor (Y)
And Factor (Y) Obtained With The Bracketing Orifice
Larger % Difference Between Factors (Ys)
Obtained With Bracketing Orifices
Acceptability Resull
First Orifice
709.302
720.057
10.755
88000
90.000
84000
84.000
8S.5
600.000
3.500
29.08
82.000
82.800
82.4
18.000
10.244
10.188
1,006
0.14%
0.64%
Second Orifice
720,400
727.855
7,455
88.000
89,000
85.000
86.000
87.0
600.000
1.700
29.08
83.000
82600
82.8
18000
7.108
7.024
1.012
0.50%
All Orifices Are Acceptable
Remarks:
Signature:
Date:
CRORBRKT.xb 10/29/98 (rav. N7 Console Calibration Workbook.xls B/7C003 3:11 PM)
Cl-7
-------
WI5 Console Pre-Calibration Checklist
Job No.
Console No.
1 X
110249.2.001.04
N12
Date
Performed By
August 7, 2003
Darrel Sprague
(Place an "X" In the space provided after the required checks are performed.)
Perform positive leak check of Delta H manometer.
Procedure for positiva leak check Delta H manometer:
1. Pump must not be run prior to this test. Pump needs to be cool in order to get an accurate reading.
2. Pump pressure and vacuum lines must be connected to console.
3. Null switch on console musl be in the down position so solenoid valve is open to the sampling
stream as it is during testing.
4. Plug meter exhaust and clamp off bottom tube from exhaust which goes to the Orsat pump.
5. Plug sample orifice.
6. Close main flow control valve.
7. Open fine control valve,
8. Disconnect right side Delta H manometer tube on front of console.
9. Blow into tubing until manometer reads 5 to 7 inches of water, and clamp off.
There should bs no change in manometer reading.
10. Be certain to remove plug and clamp from meter exhaust Immediately after this
test to avoid damage to the meter pump when pump is started uoi
2,
3.
4.
5.
6.
X
N/A
X
X
X
Leak check Delta P manometer.
Clean pump
Clean muffler jar(s).
Inspect/refill oiler jar.
Calibrate DGM thermocouples:
(Note
within
Reading must be
+/-2.5°F
DGM Inlet:
DGM Outlet
Reference Pyrometer
Op
78
78
.4
.8
Console Pyrometer
°F
78.0
78.0
7. X ___ Digital clock/timer in place and functional,
8. X Vacuum check. (Leak check at 25 in. Hg. Vacuum. Leak rate should be zero)
9. x Check indicator lights
10. X Check thermocouple switches.
11- ^^^ Check fan,
12. X Check pump heater.
13. ___X__ _ check heat controllers.
14. X Check Orsat pump and rotameter.
If any of the above items were replaced or repaired, please document that information below:
Signature:
Date:
Cl-8
-------
MERCURY BAROMETER PRESSURE READING CORRB
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude: 39° 05,8' north
Meteorological Gravity: 32.1525 feet/second2
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lc
MRI Project No. 110249.2.001.04
Date: August 7, 2003
Time: 13:14
Readings Obtained By: Darrei Sprague
Observed Barometer Reading: 29.30 in. Hg
Mercury Column Temperature: 81 °F
Correction For Temperature: -0.14 in. Hg
Correction For Gravity: -0.02 in. Hg
Corrected Barometric Pressure: 29.14 in. Hg
Remarks:
Signature:
Date: £>~
BAROMETR.xls 10/27/99 (rev. N12_Console Calibration Workbook.xls 8/7/2003 3:09 PM)
Cl-9
-------
MS Console Calibration Worksheet
Job No.
Date
Operator
Barometer
110249.2,001.04
August 7, 2003
Parrel Sprague
29.14
in. Hg.
Metering Console No. N12
Previous Dry Gas Meter Factor (Y): 0.987
Calibrated Critical Orifice No. D24
Critical Orifice Coefficient in English Units (K1): 0.6417
Ambient Temperature Meter No. 81 _Q
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18.0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18,0 in. Hg. +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: 9.0 + 9.2 = 18.00 in. Hg.
Console vacuum gauge reading: 18.20 in. Hg,
console vacuum gauge correction factor: -0.20 in. Hg.
DGM Initial Volume:
DGM Inlet Temperature:
DGM Outlet Temperature:
Time of run (In seconds):
Orifice Delta H (in. H2O):
Room Temperature:
Pump Vacuum (in. Hg.):
Initial:
Final:
Initial:
Final:
Initial:
Final:
Initial:
Final:
RUN#1
692.500
701.076
79
80
78
78
600
2.15
80.8
81.6
18.0
RUN #2
701.076
709.459
81
82
82
79
600
2.15
82.1
81.8
18.0
RUN #3
709.459
718.028
93
84
79
80
600
2.15
82.0
81.6
18.0
Signature:
Date:
Cl-10
-------
METHOD 5 METERING CONSOLE CALIBRATION WITH CRITICAL ORIFICE
MRi Project No.
Date:
Operator:
110249.2.001.04
August?, 2003
Darrel Sprague
Metering Console No.
Previous Dry Gas Meter Factor (Y):
Calibrated Critical Orifice No.
Critical Orifice Coefficient in English Units (K'):
| Ambient Temperature Meter No.
N12
0.987
D24
0.64170
B1.0
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Meter Gas Volume, ft3
Final Dry Gas Meter Gas Volume, ft.3
Net Dry Gas Meter Gas Volume (\y , ft.3
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, "F:
Initial Inlet Temperature, °F
Final Inlet Temperature, "F
Initial Outlet Temperature, °F
Final Outlet Temperature, °F
Average Dry Gas Meter Temperature (tj. °F
Time, seconds
Orifice Meter AH, inches H20
Barometric Pressure, in. Hg
Critical Orifice Inlet (Ambient) Temperature, °F:
Initial Ambient Temperature, °F
Final Ambient Temperature, °F
Avg. Critical Orifice Inlet Temperature (t,^, °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume (Vr(5W)), standard ft.3
Dry Gas Meter Gas Volume (Vm (sta)), standard ft3
Dry Gas Meter Calibration Factor (Y)
Orifice Meter fH@
AVERAGE CALIBRATION RESULTS
Average Dry Gas Meter Calibration Factor (Y)
Average Orifice Meter /H@
CALIBRATION RESULTS COMPARISON
Criterion: Y Must Be Within 2% Of Average Y
Percent Difference Of Y From Average Y
Tolerance Result
COMPARISON WITH PRETEST RESULTS
Criterion: Y Must Be Within 5% Of Previous Y
% Difference Of Average Y From Previous Y
Tolerance Result
Y = C .MMO 1 1 67-563774
Run 1
692.500
701 .076
8.576
79.0
80.0
78.0
78.0
78.8
600
2.15
29.14
80.8
81.6
81.2
18.0
8.040
8.230
0.977
1.805
0.989
1.798
1,21%
PASS
0,19%
PASS
Run 2
701.076
709.459
8.383
81.0
82.0
82.0
79.0
81.0
600
2.15
29.14
82.1
81.8
82.0
18.0
8.035
8.011
1.003
1.800
1 .42%
PASS
Run 3
709.459
718.028
8.569
93.0
84.0
79,0
800
84.0
600
2.15
29.14
- '
82.0
81.6
81.8
18.0
8.036
8,144
0.987
1.790
0,22%
PASS
Remarks:
Sig nature:
Dale;
CRORCALB.xls 10/29/95 (reu.N12_CansnteCaIibratinnWorkbook.xls 8/7/2003 3:10 PM)
Cl-11
-------
M5 Console Pre-Calibration Checklist
Job No. 110249,2,001,04 Date August 7,2003
Console No. N13 Performed By Parrel Sprague
{Place an "X" in the space provided after the required checks are performed.)
1. X Perform positive leak check of Delta H manometer.
Procedure for positive leak check Delta H manometer:
1. Pump must not be run prior to ttlis test. Pump needs to be cool in order to get an accurate reading.
2, Pump pressure and vacuum lines must be connected to console,
3, Null switch on console must be in the down position so solenoid valve is open to the sampling
stream as it is during testing.
4, Plug meter exhaust and clamp off bottom tube from exhaust which goes to the Orsat pump.
5. Plug sample orifice.
6. Close main flow control valve.
7. Open fi ne control va Ive.
8. Disconnect right side Delta H manometer tube on front of console.
9. Blow into tubing until manometer reads 5 to 7 inches of water, and clamp off.
There should be no change in manometer reading.
10. Be certain to remove plug and clamp from meter exhaust Immediately after this
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
X
N/A
X
X
X
(Note:
within
NO
X
X
X
X
X
X
X
test to avoic
damage to the meter pump when pump is started up!
Leak check Delta P manometer.
Clean pump
Clean muffler jar(s).
Inspect/refill oiler jar.
Calibrate DGM thermocouples: Reference
Reading must be
+/-2.5°F
o
DGM Inlet: 7?
DGM Outlet: 7£
Pyrometer Console Pyrometer
F °F
.8 80.0
i.8 80.0
Digital clock/timer in place and functional.
Vacuum check. (Leak check at 25 in. Hg. Vacuum. Leak rate should be zero)
Check indicator lights
Check thermocouple switches.
Check fan.
Check pump heater.
check heat controllers.
Check Orsat purnp and rotameter.
If any of the above items were replaced or repaired, please document that information below:
Signature: t-A/HW/ WJ^KCf^^ Date: #^ 7-0-3
7 ^^
Cl-12
-------
MERCURY BAROMETER PRESSURE READING CORRE'
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude: 39° 05.8' north
Meteorological Gravity: 32,1525 feet/second2
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lc
MRIProjectNo. 110249.2.001.04
Date: August 7, 2003
Time: 14:53
Readings Obtained By: Darrel Sprague
Observed Barometer Reading: 29.30 in. Hg
Mercury Column Temperature: 81 °F
Correction For Temperature: -0.14 in. Hg
Correction For Gravity: -0.02 in. Hg
Corrected Barometric Pressure: 29.14 in. Hg
Remarks:
Signature:
7/^
Date:
BAROMETR.xls 10/27/99 (rev.N13PretestCallbratlonWorkbook.xls 8/7/2003 3:07 PM)
Cl-13
-------
MS Console Calibration Worksheet
Job No. 110249.2.001.04 Metering Console No. _ N13
Date August 7, 2003 Previous Dry Gas Meter Factor (Y): Q.987
Operator Parrel Sprague Calibrated Critical Orifice No.
Barometer 29.14 in. Hg. Critical Orifice Coefficient in English Units (K'): 0.64J7^
Ambient Temperature Meter No. 81.0
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18.0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18.0 in. Hg. +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: 8.8 + 8.9 = 18.00 in. Hg.
Console vacuum gauge reading: 17.70 in. Hg.
console vacuum gauge correction factor: 0.30 in. Hg.
DGM Initial Volume:
DGM Inlet Temperature:
DGM Outlet Temperature: Initial:
Time of run (In seconds):
Orifice Delta H (in. H2O):
Room Temperature:
Pump Vacuum (in. Hg.):
Initial:
Final:
Initial:
Final:
Initial:
Final:
Initial:
Final:
RUN#1
337.000
345,523
80
82
79
80
600
2.15
80.6
81.4
18.0
RUN #2
345.523
353.207
83
84
80
80
540
2.15
82.2
82.4
18.0
RUN #3
353.207
361.765_
85
87
81
81
600
2.15
82.8
83.8
18.0
Signature LA//^^^ S%L^&e/£~£"''~ Date:
Cl-14
-------
METHOD 5 METERING CONSOLE CALIBRATION WITH CRITICAL ORIFICE
MRI Project No.
Date:
Operator:
110249.2.001,04
August!, 2003
Darrel Sprague
Metering Console No.
Previous Dry Gas Meter Factor (Y):
Calibrated Critical Orifice No.
Critical Orifice Coefficient in English Units (K1)
Ambient Temperature Meter No.
N13
0.987
D24
0.64170
81.0
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Metier Gas Volume, ft.3
Final Dry Gas Meter Gas Volume, ft3
Net Dry Gas Meter Gas Volume (VJ, ft 1
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, °F:
Initial Inlet Temperature, °F
Final Inlet Temperature, "F
Initial Outlet Temperature, "F
Final Outlet Temperature, "F
Average Dry Gas Meter Temperature (tj, °F
Time, seconds
Orifice Meter M, inches H2O
Barometric Pressure, in. Hg
Critical Orifice Inlet (Ambient) Temperature, °F:
Initial Ambient Temperature, *F
Final Ambient Temperature. °F
Avg. Critical Orifice Inlet Temperature (t,mj, °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume (V,r(SK)), standard ft,3
Dry Gas Meter Gas Volume (\4 (5M)), standard ft 1
Dry Gas Meter Calibration Factor (Y)
Orifice Meter AH@
AVERAGE CALIBRATION RESULTS
Average Dry Gas Meter Calibration Factor (Y)
Average Orifice Meter *(@
CALIBRATION RESULTS COMPARISON
Criterion: Y Must Be Within 2% Of Average Y
Percent Difference Of Y From Average Y
Tolerance Result
COMPARISON WITH PRETEST RESULTS
Criterion: Y Must Be Within 5% Of Previous Y
% Difference Of Average Y From Previous Y
Tolerance Result
Y = 0.9SS853517146527 |
Run 1
337.000
345,523
8.523
80.0
82.0
79.0
80.0
80.3
600
215
29.14
80.6
814
81.0
18,0
8.042
8.156
0.986
1.799
0.986
1.798
0.01%
PASS
0.12%
PASS
Run 2
345.523
353.207
7.684
83.0
84.0
800
80.0
81.8
540
2.15
29.14
822
824
82.3
18.0
7229
7.333
0.986
1.799
0.00%
PASS
Run 3
353.207
361 .765
8.558
85.0
87.0
81.0
81.0
83.5
600
2.15
29.14
82.8
83.8
83.3
18.0
8.025
8,141
0.986
1.796
0.01%
PASS
Remarks:
Signature:
Oats:
CRORCALB.xls 10/29/99 (rev, N13 Pretest Calibration Workbook.xls 8/7/2003 3:07 PM)
Cl-15
-------
Stack Thermocouple Calibration Data
Job.No:
Date:
Ambient Temp. (°F)
Performed By:
Stack Thermocouple No:
Reference Pyrometer No:
Probe Number: *^
Avg. Stack Temp. (UF)
Barometer:
in. Hg.
Reference Instrument: Hart Scientific Model Number 9100A, Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
is calibrated in accordance with ITS-90 and ANSi/NCSL Z540-1.
Reference Instrument
Temp. (°F)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Temperature Difference
(Reference Instrument Temp. °F + 460) - (Reference Pyrometer Temp. °F + 460) x 10Q
-------
Stack Thermocouple Calibration Data
Job.No:
Date:
Ambient Temp. (°F)
Performed By:
D. Neal
i.
Stack Thermocouple No:
Reference Pyrometer No:
Probe Number:
Avg. Stack Temp. (°F)
Barometer:
in. Hg.
Reference Instrument: Hart Scientific Model Number 9100A, Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
is calibrated in accordance with ITS-90 and ANSI/NCSL Z540-1.
Reference Instrument
Temp. (°F)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Temperature Difference
12M/L
0,8
frtt-
^Reference^lnstrument Temp, °F + 460) - (Reference Pyrometer Temp. °F + 460)
(Reference Instrument Temp. °F + 460)
x 100
-------
Job.No:
Date:
Ambient Temp. ( F)
Performed By:
Stack Thermocouple Calibration Data
Stack Thermocouple No: _
Reference Pyrometer No:
Probe Number:
Avg. Stack Temp. (°F)
Barometer:
in. Hg.
Reference Instrument: Hart Scientific Model Number 9100A. Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
Is calibrated in accordance with ITS-90 and ANSI/NCSL Z540-1.
Reference Instrument
Temp. ( f)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Temperature Difference
r-J
(Reference jnstrument Temp. °F + 460) - (Reference Pyrometer Temp. °FjM60)
(Reference Instrument Temp. °F + 460)
x 100
-------
Stack Thermocouple Calibration Data
J0b.No:
Ambient Temp. (°F)
Performed By:
D.
Stack Thermocouple No:
Reference Pyrometer No: ,7^-
Probe Number: __£v5_
Avg. Stack Temp, (°F) / ~f £
Barometer: 0
in, Hg.
Reference Instrument: Hart Scientific Model Number 9100A, Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
Is calibrated in accordance with ITS-90 and ANSI/NCSL ZS40-1,
Reference Instrument
Temp. (°F)
Reference Pyrometer
Temp. <°F)
Temperature Difference
Temperature Difference
(MM
(Reference Instrument Temp. °F + 460)jL(Reference Pyrometerjemp. _
(Reference Instrument Temp. °F + 460)
_+_ 460)
x 100
-------
Job.No:
Date:
Ambient Temp. ( F)
Performed By:
XAD Thermocouple Calibration Data
110249.2.001.04
JAugust_7,_2003_
81
Dave Griffin
Pyrometer No:
Reference Thermometer:
Serial Number:
Barometer:
ASTM 63F
1979299
29.17 in Hg.
Calibration Method: Water bath with ASTM thermometer at ambient temperature.
XAD Thermocouple
Number
Reference Thermometer
Temp. (°F)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Tolerance: +/• 2°F
Comments:
Signature:
Date:
Cl-20
-------
Gooseneck Thermocouple Calibration Data
Job.N0;
Ambient Temp. <°F)
Performed By:
D. Neal
Pyrometer No:
Reference Thermometer:
Serial Number:
Barometer:
ASTM 63F
1979299
0
in. Hg.
Calibration Method: Water bath with ASTM thermometer at ambient temperature.
Gooseneck
T.C. No.
tt#l
UJft
tiltll'
Mtf
utfr)
Leak Check &
Check Valve
Pass/No Pass
A**
L$^&^^
fa
/V
A0
Reference Thermometer
Temp. (DF)
n*>
7U
?7X
n,*
T/<0
Reference Pyrometer
Temp. (°F)
7*'fc
11 <1
ILL
~76-i-
*7&<£
Temperature Difference
Tolerance: +/- 2°F
*,y
0
-------
MS Console
Number
Request For Post Test Calibrations
Date:
Requested By:
Average
Delta H
Pyrometer
Number
XAD Thermocouple
Number
D. Neal
Sample Box
Number
Probe
Number
VOST Console
Number
Stack Thermocouple
Number
VOST Train
Number
List other equipment to be calibrated:
Average Stack
Temperature
VOST Thermocouple
Number
Pilot
Number
M
Gooseneck
Number
..(Aft^Z
u # 2z_
£L.
titt-f
Barometer
Number
Cl-22
-------
Type S Pitot Tube Inspection Data Form
Pitot Tube #: /n-'/Z*9
Probe #:
Pitot tube
Pitot tube
J^.'
l~
assembly level?
openings damagei
Dale: j
Job#:
d?
^l>~ ffy P erformed
lloft*
s
<*>,*
Yes
Yes
^"Tt $">•
(explain
By: U-6r
^
below)
Ank
No
K"" No
a. - 0
Pi = ^^
y
/ = A sin y
w = A sin 0
PA= f
- C
A =
, 7*0
(in)
(in); (< 0.125 in)
(in); (< 0.03 1 25 in)
(in), PR =
Dt =
Calibration required?
Comments:
Yes
No
T
(in)
A - Side Plane
J. Note:
B - Side Plane
0.48 CM
-------
Type S Pitot Tube Inspection Data Form
Pilot Tube #: /*f
Probe*: f~1
Date:
Job #:
Performed By:
Pitot tube assembly level?
Pitot tube openings damaged?
a, - f " (<10°),
Pi ~
Yes
Yes (explain below)
No
No
fe =
°» e = j. •, A =
(in)
z = Asiny
vv = A sin 9
(in); (< 0.1 25 in)
(in); (< 0,03 125 in)
(in),
(in), D,=
(in)
Calibration required?
Comments:
Yes
No
»l !*--,
^ 7
-"_;{
n - side Plane
0.48 CM < Dt «= 0.95 CM
(3/16 in) (3/8 in.)
Transverse
Transverse f ~~~~ ~~ /^~ ^^
TubsAxis " 0 ^^U V V
ir
Transverse
Tube Axis
/ i
~%/—
A"7v~
Calibration Rccards\CaIihraliun I nrms\nfwpitnt.doc
01/18/99
Cl-24
-------
Tvoe S Pitot Tube Inspection Data Form
Pilot Tube #:
Probe//.
Date:
Jobfr.
Performed By;
Pitot tube assembly level?
Pitot tube openings damaged?
Yes
Yes (explain below)
r
No
No
, - # °
z = A sin y
w = A sin 6
I = __(_ °, A - tltf* (in)
(in); (< 0.125 in)
(in); (< 0.03125 in)
(in), PB = **flf (in), D, =
(in)
Calibration required?
Comments:
Yes
No
A-Side Plane |
longitudinal
A TgBeAxis —
Longitudinal f
Tube Axis —«• — i
Note:
l.oslht < 0.95 CM
(3/16 in.) (3/B m.)
Transverse
TubeAxi
se _^ f /^ ^N
™ n A m- B V ^/
.-i_
>P
r—^~
Face
^Opening
Planes
Transverse
Tubs Axis
Calibration KecordsXCulibration F<>rins\newpitot.tloc
(lit \^ ;3^.
01/IS/99
Cl-25
-------
Tvne S Pitot Tube Inspection Data Form
Pitot Tube #: fll
Probe #:
Date:
Job #:
Performed By:
/*rf
Pitot tube assembly level?
Pitot tube openings damaged?
' Yes
Yes (explain below)
No
No
0
y == _3. _ '- 0 = J_ ", A = n). Di = -
(in)
Calibration required?
Comments:
Yes
No
0.48 CM < nt < 0.95 CM
(3/19 in.) <3ffl in.)
Transverse Jf
TubeAxis " t> A'orB
Transverse
Tube Axis
Calibration Ri>cords\Calibra«tm Korms\ncwpitnt.duc
01/18/99
Cl-26
-------
Appendix C-2
Post-Test Calibration Records
MRI-AED\UNIMIN TEST REPORT NON-CBI VERSION REVISED BY LIBRARY 3-24-10.DOC
-------
Request For Post Test Calibrations
Job No:
Job Name:
110249.2.001,05
Characterization of Dioxin in Ball Clay
M5 Console Average Pyrometer
Number Delta H Number
N7
Probe
Number
3-2
3-5
1.35 Y-0815
Stack Thermocouple Average Stack
Number Temperature
36-2 144
36-12 129
Date: August 27, 2003
Requested By: D. Neal
XAD Thermocouple Sample Box
Number Number
XAD-1 10288
XAD-2 12003
Pitot Gooseneck
Number Number
M-126 UH-1
M-104 UH-1 2
VOST Console
Number
VOST Train
Number
VOST Thermocouple
Number
Barometer
Number
X-4029
List other equipment to be calibrated:
If*
C2-1
-------
MS Console Pre-Calibration Checklist
Job No.
Console No.
1.
110249.2.001.05
N7
Date
Performed By
August 27, ^003
Daniel Neal
1
2.
3.
4.
5,
6.
7.
8.
9.
10.
(Place an "X" in the space provided after the required checks are performed.)
Perform positive leak check of Delta H manometer.
Procedure for positive leak check Delta H manometer:
Pump must not be run prior to this test. Pump needs to be cool in order to get an accurate reading.
Pump pressure and vacuum lines must be connected to console.
Null switch on console must be in the down position so solenoid valve is open to the sampling
stream as it is during testing-
Plug meter exhaust and clamp off bottom tube from exhaust which goes to the Orsat pump.
Plug sample orifice.
Close main flow control valve.
Open fine control valve.
Disconnect right side Delta H manometer tube on front of console.
Blow into tubing until manometer reads 5 to 7 inches of water, and clamp off.
There should be no change in manometer reading.
Be certain to remove plug and clamp from mater exhaust immediately after this
test to avoid damage to the meter oumo when pump Is started UP!
2.
3.
4.
5.
6,
X
N/A
X
X
X
(Note
within
Leak check Delta P manometer.
Clean pump
Clean muffler jar(s).
Inspect/refill oiler jar.
Calibrate DGM thermocouples:
Reading must be DGM Inlet:
+/-2.5°F DGM Outlet:
Reference Pyrometer
°F
78.4
78.4
Console Pyrometer
°F
79.0
79.0
7.
8.
9.
10.
11.
12,
13,
14.
X
X
X
JL
X
X
X
Digital clock/timer in place and functional.
Vacuum check. (Leak check at 25 in, Hg. Vacuum. Leak rate should be zero)
Check indicator lights
Check thermocouple switches.
Check fan.
Check pump heater.
check heat controllers.
Check Orsat pump and rotameter.
If any of the above items were replaced or repaired, please document that information below:
Signature:
Date:
-
C2-2
-------
MS Console Calibration Worksheet
Job No. 110249.2.001.05 Metering Console No. N7
Date August 27, 2003 Previous Dry Gas Meter Factor (Y): 1002
Operator Daniel Neal Calibrated Critical Orifice No. £15
Barometer 29.13 in. Hg. Critical Orifice Coefficient in English Units (K1): 0,4146
Ambient Temperature Meter No. Y-0815
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18.0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18.0 in. Hg. +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: 8.9 + 9.1 = 18.00 in. Hg.
Console vacuum gauge reading: 19.00 in. Hg.
console vacuum gauge correction factor: -1.00 in. Hg.
DGM Initial Volume:
DGM Inlet Temperature. Initial:
Final:
DGM Outlet Temperature: Initial:
Time of run (In seconds):
Orifice Delta H (in. H2O):
Room Temperature:
Pump Vacuum (in. Hg.):
Initial:
Final:
Initial:
Final:
Initial:
Final:
Initial:
Final:
RUN#1
884.700
890.157
83
84
81
81
600
0.90
80.6
82.2
18.0
RUN #2
890.157
895.607
85
85
82
82
600
0.90
80.0
83.4
18.0
RUN #3
895.607
901.082
86
87
83
83
600
0.90
82.0
82.8
18.0
Signature: f ]£iU<-Lj6 /v^^f Date
•-————-• ^nfilf^"1
,_ 7M, .
03
C2-3
-------
METHOD 5 METERING CONSOLE CALIBRATION WITH CRITICAL ORIFICE
MRI Project No.
Date:
Operator:
110249.2.001.05
August 27, 2003
Daniel Neal
Metering Consols No.
Previous Dry Gas Meter Factor (Y):
Calibrated Critical Orifice No.
Critical Orifice Coefficient in English Units (K1):
| Ambient Temperature Meter No.
N7
1.002
E15
0.41460
Y-0815
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Meter Gas Volume, ft.3
Final Dry Gas Meter Gas Volume, ft.3
Net Dry Gas Meter Gas Volume (\4), ft.3
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, °F:
Initial Inlet Temperature, °F
Final Inlet Temperature, °F
Initial Outlet Temperature, *F
Final Outlet Temperature, "F
Average Dry Gas Meter Temperature (y, °F
Time, seconds
Orifice Meter AH, inches H2O
Barometric Pressure, in Hg
Critical Orifice Inlet (Ambient) Temperature. °F:
Initial Ambient Temperature, °F
Final Ambient Temperature, °F
Avg. Critical Orifice Inlet Temperature (tjm}, °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume (\& (SM)), standard ft.3
Dry Gas Meter Gas Volume (\4 (SM)), standard ft.3
Dry Gas Meter Calibration Factor (Y)
Orifice Meter AH@
AVERAGE CALIBRATION RESULTS
Average Dry Gas Meter Calibration Factor (Y]
Average Orifice Meter Ai@
CALIBRATION RESULTS COMPARISON
Criterion: Y Must Be Within 2% Of Average Y
Percent Difference Of Y From Average Y
Tolerance Result
COMPARISON WITH PRETEST RESULTS
Criterion: Y Must Be Within 5% Of Previous Y
% Difference Of Average Y From Previous Y
Tolerance Result
Y = 1.032651356453530 1
Run 1
884.700
890.157
5.457
83.0
84.0
81,0
81.0
82.3
600
0.90
29.13
80.6
822
81 4
1S.O
5.192
5.185
1.001
1.788
1.003
1.786
0.12%
PASS
0.07%
PASS
Run 2
890.157
895.607
5.450
85.0
85.0
82.0
82.0
83.5
600
0.90
29.13
80.0
83.4
81.7
18.0
5.191
5.166
1.005
1.785
0,21%
PASS
Run 3
895.607
901 ,082
5.475
86.0
87.0
83.0
83.0
84.8
600
090
29.13
82.0
828
82.4
18.0
5.187
5.178
1.002
1.783
0.08%
PASS
Remarks:
Signature;
CRORCALB.xls 10/29/99 (rev.N7ConsoleCaIibrationWbrkbook.xls 8/27/2003 9:S8AM)
C2-4
-------
MS Console Critical Orifice Bracketing Worksheet
MR! Project No. 110249.2.001.05 Critical Orifice Being Evaluated El5
Dafe; __ August 27, 2003 First Critical Orifice No. E12
Operator; __Daniel Neai Coefficient (K1): 0.3264
Metering Console No. N7 Second Critical Orifice No. E21
Dry Gas Meter Factor (Y): 1002651356^ Coefficient (K'}: _ 0.5693 _
Orifice Used for the Calibration: E15 Note: Critical orifice coefficients are in English unite.
Ambient Temperature Meter No. Y-0815
Note: Prior to running calibration, connect mercury manometer to sample orifice. Turn on pump and bring
mercury manometer up to 18.0 in. Hg. Record mercury manometer and console vacuum gauge readings
below. Insert critical orifice into console sample orifice. Set console vacuum gauge at 18.0 in. Hg. +/- the
console vacuum gauge correction factor calculated below.
Mercury manometer readings: 8.9 + 9.1 = 18,00 in. Hg.
Console vacuum gauge reading: 19.00 in. Hg.
console vacuum gauge correction factor: -1.00 in. Hg.
RUN#1 RUN #2
DGM Initial Volume: Initial: 903.100 908.002
Final: ^907,444 915.560
DGM In let Temperature: Initial: 86 88
Final: 86 89
DGM Outlet Temperature: Initial: 84 84
Final: 84 85
Time of run (In seconds): 600 600
Orifice Delta H (in. HZO): 0.55
Room Temperature: Initial: 82.6 82.6
Final; 82.2 82.4
Pump Vacuum (in. Hg.): 18.0 18.0
A
Signature: yX/&<^A?' A-yUx-f Date:
C2-5
-------
METHOD 5 METERING CONSOLE CALIBRATION
CRITICAL ORIFICE BRACKETING DATA
MRI Project No.
Date:
Operator:
Metering Console No,
Dry Gas Meter Factor (Y):
Orifice Used for the Calibration:
Ambient Temperature Meter No.
110249.2.001.05
August 27, 2003
Daniel Neal
N7
1.003
E15
Y-0815
Note; Critical orifice coefficients are in English units.
Critical Orifice Being Evaluated
Critical Orifice No.
E15
Critical Orifices Used For Bracketing
First Orifice
Critical Orifice No.
Coefficient (K1):
Second Orifice
Critical Orifice No.
Coefficient (K1);
E12
0.32640
E21
0.56930
CALIBRATION GAS VOLUME DATA
Initial Dry Gas Metier Gas Volume, ft3
Final Dry Gas Meter Qas Volume, ft.3
Net Dry Gas Meter Gas Volume (VJ, ft.3
CALIBRATION CONDITIONS DATA
Dry Gas Meter Temperature, "F:
Initial Inlet Temperature, "F
Final Inlet Temperature, °F
Initial Outlet Temperature, °F
Final Outlet Temperature, "F
Average Dry Gas Meter Temperature (t,), °F
Time, seconds
Orifice Meter AH, inches HjO
Barometric Pressure, in. Hg
Critical Orifice Inlet (Ambient) Temperature, °F:
Initial Ambient Temperature, "F
Final Ambient Temperature, "F
Average Critical Orifice Inlet Temperature (t^i °F
Pump Vacuum, in. Hg
COMPUTED CALIBRATION RESULTS
Critical Orifice Gas Volume (\4(St
-------
XAD Thermocouple Calibration Data
Job.No;
Date:
Ambient Temp. (°F)
Performed By:
110249.2.001.05
August 27, 2003
79
D. Neal
Pyrometer No:
Reference Thermometer:
Serial Number:
Barometer:
Y-081S
ASTM 63F
29.13
1979299
in. Hg.
Calibration Method: Water bath with ASTM thermometer at ambient temperature.
XAD Thermocouple
Number
Reference Thermometer
Temp. (°F)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Tolerance: +/- 2°F
XAD-1
XAD-2
79.7
79.7
81.2
81.4
-1.5
-1.7
Comments:
Signature:
C2-7
-------
Samole Box Filter Thermocouple Calibration Data
Job.No.
Date:
Ambient Temp, (°F)
Performed By:
110249.2.001.05
August 27, 2003
_ 79
D. Neal
Console Pyrometer No:
Reference Pyrometer No:
Reference Thermocouple Number:
Barometer:
N7
Y-0815
29.13
in. Hg.
Calibration Method: Heat sample box to 250°F with HIS console. After temperature has stabilized, check filter box temperature
by comparing MS console temperature meter against calibrated pyrometer and thermocouple.
Sample Box
Number
Console Pyrometer
Temp. (°F)
Reference Pyrometer
Temp. (°F)
Temperature Difference
Tolerance: +/-5.4°F
10288_
12003
245
250
245.2
251
-0.2
-1.0
Comments:
Signature:
Date: ff~>7'°J
C2-8
-------
Stack Thermocouple Calibration Data
Job.No:
Date:
Ambient Temp. (°F)
Performed By;
_110249.2.001.05
Augugt_27,_20Q3
79
D. Neai
Stack Thermocouple No:
Reference Pyrometer No:
Probe Number:
Avg. Stack Temp. (°F)
Barometer
36-2
Y-0815
3-2
144
29.13
in. Hg.
Reference Instrument: Hart Scientific Mods! Number 9100A, Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
is calibrated in accordance with ITS-90 and ANSI/NCSL ZS40-1.
Reference Instrument
Temp. (°FJ
Reference Pyrometer
Temp. <°F)
Temperature Difference
Temperature Difference
81.0
150.8
199.9
80.4
150.4
200.2
0,60
0.40^
-0.30
0.11%
0.07%_
-0.05%
(Reference Instrument Temp. °F + 460) - (Reference Pyrometer Temp. °F + 460)
(Reference Instrument Temp. °F +• 460)
1QQ
-------
Stack Thermocouple Calibration Data
Job.No:
Date:
Ambient Temp. (°F)
Performed By:
110249.2.001.05
August 27. 2003
79
D. Neal
Stack Thermocouple No:
Reference Pyrometer No;
Probe Number:
Avg. Stack Temp. (°F)
Barometer:
36-12
Y-0815
3-5
129
29.13
in. Hg.
Reference Instrument: Hart Scientific Model Number 9100A, Serial Number 84414 Dry-well, HDRC handheld Block A. This Instrument
is calibrated in accordance with ITS-90 and ANSI/NCSL Z540-1.
Reference Instrument
Temp. (°F)
81.0
150.8
199.9
Reference Pyrometer
Temp. <°F)
80.6
150.4
200.6
Temperature Difference
<°F)
0.40
0.40
-0.70
Temperature Difference
(%)
0.07%
0.07%
-0.11%
(Reference Instrument Temp. °F + 460) - (Reference Pyrometer Temp. °F + 46p|
(Reference Instrument Temp. °F + 460)
Signature:
Date:
x 100
-------
Gooseneck Thermocouple Calibration Data
JobNo:
Date:
Ambient Temp. (°F)
Performed By:
110249.2.001.05
August 27, 2003
79
D. Neal
Pyrometer No:
Reference Thermometer:
Serial Number:
Barometer:
Y-0815
ASTM 63F
1979299
29.13
in. Hg
Calibration Method: Water bath with ASTM thermometer at ambient temperature.
Gooseneck
T.C. No.
UH-1
UH-12
Leak Check &
Check Valve
Pass/No Pass
Pass
Pass
Reference Thermometer
Temp. (°F)
726
72.6
Reference Pyrometer
Temp. (°F)
73.4
73.2
Temperature Difference
Tolerance: +/- 2°F
-0.8
-0.6
Comments:
Signature:
Date:
\7
C2-11
-------
MERCURY BAROMETER PRESSURE READING CORRE
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude: 39° 05.8' north
Meteorological Gravity: 32.1525 feet/second2
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lot
MR1 Project No. 110249.2.001.05
Date: August 27, 2003
Time: 8:17
Readings Obtained By: Daniel Neal
Observed Barometer Reading: 29.28 in. Hg
Mercury Column Temperature: 79 °F
Correction For Temperature: -0.13 in. Hg
Correction For Gravity: -0.02 in. Hg
Corrected Barometric Pressure: 29.13 in. Hg
Remarks:
Signature:
Date:
BAROMETR.xls 10/27/99 (rev.N7ConsoleCalibrationWorkbook.xls 8/27/2003 9:58 AM)
C2-12
-------
ANEROID BAROMETER CALIBRATION CHECK
Location: Kansas City, Missouri
Altitude Above Sea Level: 850 feet
Latitude. 39° 05.8' north
Meteorological Gravity: 32.1525 feet/second2
Mercury Barometer Description: Sargent Welch, Cat. S-4519, Lot 791802000
MRI Project No. 110249.2.001.05
Date: August 27, 2003
Time: 8:17 A
Readings Obtained By: D. Neal
Observed Barometer Reading: 29.28 in. Hg
Mercury Column Temperature: 79 °F
Correction For Temperature: -0.13 in. Hg
Correction For Gravity: -0.02 in. Hg
Corrected Barometric Pressure: 29.13 in. Hg
Aneroid Barometer I.D. No.: X-4029
Reading Before Adjustment: 29.14 in. Hg
Calibration Check Result: within 0.1 in. Hg
Reading After Adjustment: P1?. ^Y in. Hg
Remarks:
BAROMETRjds 10/27/99 (rev.EquipmentCallbrattonWorkbook.xls 8/27/2003 10:12 AM)
C2-13
-------
SAMPLING NOZZLE CALIBRATION CHECK DATA
MR! Project No. 110249.2.001
Client/Source: EPA EMC OAQPS/EMAD / Ball Clay Emissions
Source Location: CBI
Sampling Location: W, fJ
Nozzle I.D. Number or
Dedicated Sampling
Train Number
Nozzle Type
(Shape and Material
of Construction)
Three Measured Diameters, inches
D1 D2 D3
Average
Diameter,
inches
Measured By
Date
JL,
/j, ^X^c&^
6-3-50 O.^Vfo
COMMENTS:
NOZZLCAX.WPD April 29, 1996 (feu. NOZZLCX.WPO Auoust 8, 2003)
C2-14
-------
Balance Caiabratioa. Data Sheet
MRIJF Q | \ I (p S Manufacturer
Model
S/N
1 Balance C
Coarse Range: ^OOOt
\ Fine Ranne:
liaracteristics
^ Readability: ^- f q
> -> "
Readabilitv:
L
Accuracy Test
: Tesl Wt. As Found As Left
^DOCc. SbO/.^t .5ooO'O«i
1 ~J — -- ^k *«njiuj — vj >
i Toleranix-
_.^_^
' Test Sequence
! Fine Range Fine
1
1 Tolerance
i , —
1 Coarse Range
h&ix 200&
\ ^ _J
Tolerance
0.2« 1
\
" a
j Pass ;X|
Corner Load Test
Test Wt. As Found As Lsf:
c^OOO^ i Q./ ^ • O-Qv
Tolerance 2, _
4
«_J O
J^P -a ^ ^ o-/^
C • / ^ 4. -• O -1. •.
4 2 23 Pass ^|
f] Fail LJ
Linearity Test
As Found As Left
Coarse Fine Coarse
JiQQl'/ ^ «^DC)Ci 'O &
Jtoo/.o
3
AO$/-L«v
3 "
IB Pass
D Fail
.J
Reoeatabilit'y Test i
Test Wt. 1 . ^CQO'O oj
i
Tolerance j. ^Q^jQ-^i*
J ; _J -a
^.OOCi-o ^ 5 _2.ncjfi-n_i
^
[
J Q9
J O
j
* ftd
7 -a°« ^4
i
Std. Dev. 9. JlOOQ-O-i
•CA 10 JteOtt-0*'
Pass ^ Fail [^
Weight ID ) QO Notes/Remarks
Wi. Gal Date C» " / O ~ O^-
Ni-S'!'" <2OA4'1^)S'(^i-"0^
Date;
C2-15
-------
Tvoe S Pitot Tube Inspection Data Form
Pilot Tube #: M-104 Date: 9-16-03 Performed By: A Daniel Neal
Job#: 110249.2.001.05
Probe*:
3-5
#
Pitot tube assembly level?
Pitot tube openings damaged?
ai = 0
p, = 0 ° (<5 °), P2 = _
•y = 2 °, 0 = 1 °, A -
0.026
X Yes
Yes (explain below)
~- 2 ° (
= 2 ° (<5 °)
.75 (in)
z = A sin y
w = Asin9
PA= ^L
(in); (< 0.125 in)
(in); (< 0.03125 in)
(in), Pn= __ .34 (in), D» =
0.013
Calibration required?
Comments:
Yes
No
.24
t'/l-oj
No
X No
(in)
0.48 CM < Dt < 0.95 CM
(3/19 in.) (3/8 in.)
Transverse
Tube Axi$
Transverse
Tube Axis
Talibralion Recurds\CaIibrntion Forms\newpitot.doc
01/18/W
C2-16
-------
Type S Pitot Tube Inspection Data Form
Pitot Tube #: M-126 Date: 9-16-0
Probe #: 3-2 Job#: 1
Pitot tube assembly level? X
Pilot tube openings damaged?
a\ 0 (<10°), 0,2 -
0, = ] w (<5«), P, =
y 2 °, 0 = 0 ", A
z=Asiny 0.026 (in); (<
3 Performed By: uaniei Neai
{'kUttdd /d*^ $~
10249.2.001.05 ^
Yes No
Yes (explain below) X No
0 ° (<10°)
0 ° (<5g)
.75 (in)
0.1 25 in)
w = A sin 0 0.000 (in); (< 0.03 1 25 in)
PA= -37 (in), PB =
Calibration required? Yes
Comments:
.38 (in), D,- .25 (in)
X No
I
1 1 1* o
"MM--, |-U|
^H- -T Ml
S~~ ~^ 7^
-\ 3 *
' i 1
i |~f
A - Side Plans j
1 I Note:
Longitudinal n-fe T ^/ I p* f i o^
T&Axis -. ^^ § < t^ \
U- Side Plane
0.48 CM < i>i < 0.9S CM
(3/16 In.) (3J8 in.)
Tube Axis * 0 A at B V_ ^) \
I
^-
_.i«V i .ja
1 i
!/ I
'' ' /
Transverse J/ _JTL ] . M
Tube Axis T-A^V B 1 p
1 i
Longitudinal O B Flowt ^X
-- ^"T7
k u Fiowt .y1
Dr < P < 1 50 Dl U -""^
-*r-*-
1 -v^- --
— Y — i ^° -^"V
-^-T PA "S^
Opening > ^ ~
Ranes
1 z
'fc. >\'"!«- C ^-^5i
11 o A vi :z*^
/ \ i H
AJ^_^Jj...-- {j-A -^-^^S^-^-f
j OT0114
Calibration R«ords\Calihralioii Fonna\newpitot>doc
01/18/99
C2-17
-------
Appendix D
Summary Analytical Reports and Data
-------
Appendix D-1
Run 1 Retest Emission Samples
-------
ALTA ANALYTICAL PERSPECTIVES
16 ALIG 20U3
John Hosenfeld
Midwest Research Institute
425 Volker Blvd.
Kansas City, MO 64110
Ph.: 816-753-7600x1336
1-ax: 816-531-0315
Subject: Certificate of Results
Dear John;
Attached to this narrative are the analytical results you requested on the rapid
turn-around time sample submitted for the determination of polychlorinated dibenzo-/>-
dioxins and dibenzofurans. The insert below summarizes the relevant information
pertaining to your project. In particular, the QC annotations bring to your attention
specific analytical observations and assessments made during the sample handling and
data interpretation phases.
Project Information Summary
Client Project No.
AAP Project No.
Analytical Protocol
No. Samples Submitted
No. Samples Analyzed
No. Laboratory Method Blanks
No. OPRs / Batch CS3
No. Outstanding Samples
Date Received
Condition Received
Temperature upon Receipt (C)
Extraction within Holding Time
Analysis within Holding Time
Data meet OA/OC Requirements
Exceptions
Analytical Difficulties
When applicable, see QC Annotations for details
110249.2.001.4
P32S5
23
1
1
1
1
0
14-Aug-2003
good
16, 17
yes
yes
yes
high extraction standards recoveries
none
2714 EXCHANGE DRIVE
WILMINGTON
NORTH CAROLINA ZBAOS
TEL: 91O-794-1613 FAX 91 O-7 94-391 9
Dl-1
-------
QC Annotations:
1 The new ratio - [Ra] - for 2,3,7,8-TCDD following the 37CLr2,3,7,8-TCDD
correction is shown between squared brackets in the DL column.
2. An "A" data qualifier is used for analytes with a concentration below the
reporting limit.
3 The recoveries of the extraction standards in the field sample exceed the normal
acceptance limits of 130 percent. A close examination of the data points to the
addition of the extraction standards as a possible source for the observation
(extremely rare). The accompanying lab method blank and BCS, are entirely
normal Using information from the BCS, and the recoveries ot the sampling
standards, we determined that the bias results in an underestimation ot the
analyte concentrations by 25 percent; i.e., within the experimental error allowed
by Method 23.
The lab method blank prepared with this rapid TAT sample was obtained using
purified sand in lieu of XAD-2 resin. Normally, our procedures caU for the use
of the resin prepared alongside the sampling modules before sampling I his
substitution was necessary in order to keep the actual 1* methodI blank for the
batch of samples returning from the field. Therefore, the lab method blank does
not contain the sampling standards.
4.
Alta Analytical Perspectives remains committed to serving you in the most
effective manner. Should you have any questions or need additional ^formation and
technical support, please, do not hesitate to contact us. We wanted to thank you for
choosing Alta Analytical Perspectives as part of your analytical support team.
Sincerely,
'Yves Tondeur, Ph.D.
President & CEO
Dl-2
-------
Ji±rjrL"'"ui"""'"'v'
Parti
Narrative
i Letter
, QC Annotations
Project Information
The electronic version of this report contain y?gr pages.
P3265
t|j^——'
Part 3
Results
AMAtTYiCAi- PERSPECTIVES
Fart 2
Path
6-3 Overview
1=1 Protocol
t~i Extraction
» Analysis
a Spike Profile
6=1 SOPS
EE)QC
i_ Reporting
Special Requirements
fa< Summary' Topsheets
is Raw Data
s SICPs
5^1 Areas
s Retention Times
,^,8/N
i™ Ion Abundance Ratios
Extraction
Tracking Sheets
Fractionation
Tracking Sheets
Injection
Tracking Sheets
Part 4
Performance
c=> System Checks
S Mass Spectrometry
» Gas Chromatography
so Initial Calibration
_, Continuing Calibration
=o OPR
Part 4
GC, MS,
BCS3
ConCal
Part 4D
ICal
Part 4E
Audit
Dl-3
-------
P3265 - TEQ
Project ID: MRI
Sample Summary
Analyte
2,3,7,8-TCDD
1,2,3,7.8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7.8-TCDF
1,2,3,7,8-PeCDF
2,3,4.7.8-PeCDF
1,2,3,4,7,8-HxCDF
1,2.3.6.7,8-HxCDF
2,3,4,6,7,8-HxCDF
1 ,2,3,7,8,9-HxCDF
1,2,3.4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
ITEF TEQ (ND=0; EMPOO)
ITEF TEQ (ND=0; EMPC=EMPC)
ITEF TEQ {MD-DU2; EMPOO)
ITEF TEQ (ND=DU2; EMPOEMPC)
ITEF TEQ (ND=DL; EMPC=EMPC)
-Parti ili^^r " " Method 23
0_1529_MB001
pg
(0.993)
(0.459)
(2.04)
(1.74)
(1.83)
(<5)
(3.2)
(0.965)
(1.98)
(1.83)
(0.581)
(0.521)
(0.599)
(0.693)
(<5)
(1.37)
(6.63)
0.00
0.00
1.63
1.63
3.26
1009
pg
11.6
5.75
(3.32)
(<5)
544
32.3
302
2,68
(0.938)
(<5)
(<5)
(<5)
(<5)
(1.19)
10.6
(1.58)
12.8
16.1
16.1
18.6
18.6
21.1
[I=EMPC
Reviewer
Date
Dl-4
-------
P3265 - Totals
Project ID: MRI
Sample Summary - Pa
Analyte
Totals
TCDDs
PeCDOs
HxCDDs
HpCDDs
OCDD
TCDFs
PeCDFs
HxCDFs
HpCDFs
OCDF
Total PCDD/Fs (ND=0; EMPC=0)
Total PCDD/Fs (NCMJ; £MPO=EMPC)
Total PCDD/Fs (2378-X ND=DL; EMPC=EMPC)
Total 237Ss (ND=0; EMPC=0)
Total 2378s {ND-0.5; EMPOO)
Total 2378S (ND=1; EMPC=0)
Total 2378s (ND=0; EMPC=1)
Total 2378s (ND=0.5; EMPC=1)
Total 2378s (ND=1; EMPC=1)
irt 2 tli^ ~s Method 23
0_1529_MB001
pg
0
0
0
4.71
0
0
0
0
391
0
8.62
14.S
40,2
0.00
17.7
35.4
0.00
17.7
35.4
1009
pg
161
98.7
63,5
71.9
302
289
17.7
21.1
16.3
12.8
794
823
830
383
399
415
383
399
415
fI = EMPC
Total 2378s = Sum of 17 2378-substituted PCDD/PCDF congeners (SARA 313)
Reviewer
Date
Dl-5
-------
P3265 - Others
Project ID: MRI
Sample Summary •
Analyte
Other PCDD/Fs (ND=0, EMPC=0)
Other TCDD
Other PeCDD
Other HxCDD
Other HpCDD
Other TCDF
Other PeCOF
Other HxCDF
Other HpCDF
other PCDD/FS (ND=O, EMPC=EMPC)
Other TCDD
Other PeCDD
Other HxCDD
Other HpCDD
Other TCDF
Other PeCDF
Other HxCDF
Other HpCDF
• Part 3 ••• ALTA ANAi-yTic
0_1529_MB001
pq
0
0
0
0
0
0
0
0
0
0
0
3.6
0
0
2,53
0
meinoa ^o
1009
PQ
150
92.9
55.1
39.6
26.2
14.5
10.8
5.71
177
92.9
55.1
39.6
26.2
14.5
13.1
5.71
()=DL
[] = EMPC
Reviewer
Date
Dl-6
-------
ITEF-TEQ
Project ID: MRI
P3265
0ND=0; EMPOQ
QNDK);EMPC=EMPC
OND=DL/2;EMPC=0
• ND-DU2; EMPC=EMPC
QND=DL; EMPC=EMPC
2500
20.00
15.00
10.00
5.00
0.00
Dl-7
-------
Totals
Project ID: MRI
P3265
El Total PCDD/Fs (ND=0; EMPC=0)
DTotal PCDD/Fs (ND=0; EMPC=EMPC)
QTotal PCDD/Fs (2378-X ND=DL; EMPC=EMPC)
Dl-8
-------
% Rec.
Mean Recoveries of Extraction Standards (N=2)
Project ID: MRI
P3265
QMean
DStd. Dev.
Dl-9
-------
Mean Recoveries of Sampling Standards (N=2)
Project ID: MRI
P3265
DMean
DStd. Dev.
Dl-10
-------
Sam pip ID: o 1529 MB001 Method 23
Client Data
ijame: MR!
Project ID: MRI
>ate Collected: n/a
Analyte
2,3,7,8-TCDD
1. 2,3,7 ,8~PeCDD
1 ,2,3,4.7,8-HxCDD
1,2,3,6,7,8-HxGDD
1,2,3,7,8,9-HxCDD
1, 2,3.4,6,7 ,8-HpCDD
OCDD
2,3,7,8-TCDF
1 ,2,3,7,8-PeCOF
2,3,4,7.8-PeCDF
1, 2,3,4 ,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2.3.7.6,9-HxCDF
1, 2,3,4,6,7 ,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDDs
HpCDDs
TCOFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (MD=0)
TEQ (NDgDL/2)
Cone.
pg
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
4.71
ND
ND
ND
3.91
8.62
0.00
1 .63
Sample Data
Matrix: Air
Weight/Volume: 1
DL
pg
0.993
0.459
2.04
1.74
1.83
<5
3.2
0.965
1.98
1.83
0.581
0.521
0,599
0.693
<5
1.37
6.63
0.993
0.459
1.86
0.965
1.9
EMPC
pg
8.31
2.53
14.8
0.00
1.63
.aboratorv Data
Project No.: P3265 Date Received; n/a
Sample ID: 0_1529_MB001 Date Extracted: 14Aug03
QC Batch No.: 1529 Date Analyzed: 15Aug03
Qualifier
ITEF
ITEF
Recoveries
ES
106
109
95.6
95.6
95.6
106
89.2
116
111
111
90.9
90.9
90.9
90.9
105
105
79.3
SS
AS
107
107
j /VT
107
107
j /\"T
107
107
4 f\~7
107
107
107
107
•t f\~t
107
4 f\~I
107
107
107
107
4 f\-j
107
1 1 ALTA ANALYTICAL PERSPECTIVES
•_ — — -
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 91 0794-1 61 3
Fax:910794-3919
e-mail: yt@ultratrace.com
web: www.ultratrace.com
Checkcode: 1489
Reviewer
Date
Dl-11
-------
Appendix D-2
Runs 2 Through 6 Emission Samples
-------
ALTA ANALYTICAL PERSPECTIVES
11 SEP 2003
John Hosenfeld
Midwest Research Institute
425 Volker Blvd.
Kansas City, MO 64110
Ph.: 816-753-7600x1336
Fax: 816-531-0315
Subject: Certificate of ResuHs
Dear John;
Attached to this narrative are the analytical results you requested on the samples
submitted for the determination of polychlorinated dibenzo-p-dioxins and dibenzofurans.
The insert below summarizes the relevant information pertaining to your project. In
particular, the QC annotations bring to your attention specific analytical observations and
assessments made during the sample handling and data interpretation phases.
Project Information Summary
Client Project No,
AAP Project No.
Analytical Protocol
No. Samples Submitted
No. Samples Analyzed
No. Laboratory Method Blanks
No. OPRs/Batch CSS
No. Outstanding Samples
Date Received
Condition Received
Temperature upon Receipt (C)
Extraction within Holding Time
Analysis within Holding Time
Data meet QA/QC Requirements
Exceptions
Analytical Difficulties
When applicable, see QC Annotations for details
110249.2.001,4
P3290
23
6
6
1
1
0
22-Aug-2003
good
8, 10, 11, 19,23
yes
yes
yes
none
none
2714 EXCHANGE DRIVE
WILMINGTON
NORTH CAROLINA 284O5
TEL: 91O-794-!6l3 FAX 910-794-391 9
D2-1
-------
QC Annotations:
1. The new ratio - [Ra] -- for 2,3,7,8-TCDD following the 37CU-2,3,7,8-TCDD
correction is shown between squared brackets in the DL column.
2. An "A" data qualifier is used for analytes with a concentration below the
reporting limit.
Alta Analytical Perspectives remains committed to serving you in the most
effective manner. Should you have any questions or need additional information and
technical support, please, do nol hesitate to contact us. We wanted to thank you for
choosing Alta Analytical Perspectives as part of your analytical support team.
Sincerely,
fves Tondeur, Ph.D.
President & CEO
D2-2
-------
I[ AlT. An.tVIICAL rtniPECTLVES
Parti
Narrative
1=1 Letter
QC Annotations
e=i Project Information
The electronic version of this report contains3^f pages.
P3290
art!
Path
EF-, Overview
3 Protocol
?=i Extraction
a Analysis
5=1 Spike Profile
Part 3
Results
w Summary Topsheets
em Raw Date
B SICPs
M Areas
EEI Retention Times
c^ Ion Abundance Ratios
Extraction
Tracking Sheets
s Reporting
6=1 Special Requirements
Fractionation
Tracking Sheets
Injection
Tracking Sheets
Part 4
Performance
= System Checks
sa Mass Speetrometry
=i Gas Chromatography
^ Initial Calibration
;::,, Continuing Calibration
« OPR
Part 4
GC, MS,
BCS3
ConCal
Part4D
ICal
Part 4E
Audit
D2-3
-------
P3290 - TEQ
Project ID: 110249.2.001.04
Sample Summary - Part 1
Analyte
2,3,7,8-TCDD
1.2,3,7.8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1, 2,3,7 .8,9-HxCDD
1, 2,3,4 ,6,7,8-HpCDO
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1, 2,3,4,7,8- HxCDF
1,2,3.6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
ITEF TEQ (ND=0; EMPC=0)
ITEF TEQ (ND=0; EMFC-EMPC)
ITEF TEQ (ND=DL/2; EMPC=0)
rTEF TEQ
(3.84)
(<5)
(<5)
23.9
172
9.11
(<5>
10.3
9.58
8.01
8.18
(0.733)
24.9
5.12
18.7
15.7
15.7
17.8
17.8
19.9
Method 23
4004
pg
5.78
6.1
(3.49)
(<5)
13.2
58.9
811
[3.89]
5.59
8.85
9.47
8.41
8.38
(<5)
24.4
5.91
18.5
19.2
19.6
19.9
20.3
20.9
5004
pg
[4.36]
6.78
(3.83)
8.89
[15.4]
77.1
1220
5.3
(4.45)
7
[6.32]
(<5)
[5.41]
(1.16)
12.9
(2.78)
(<10)
10.4
17.5
11.1
18.1
18.8
6004
pg ,
5.51
7.43
(2.81)
5.86
12.3
64.6
1350
(2.34)
(5.08)
(4.68)
(<5)
(<5)
(<5)
(1.49)
7.56
(1.36)
(<10)
13.1
13.1
15.5
15.5
17.9
)=DL
I = EMPC
Reviewer
Date
D2-4
-------
P3290 - Totals
Project ID: 110249.2.001.04
Sample Summary - Part 2
Analyte
Totals
TCDDs
PeCDDs
HxCDDs
HpCDDs
OCOD
TCOFs
PeCDFs
HxCDFs
HpCDFs
OCDF
Total PCDD/Fs (MO=0; EMPC=0)
Total PCDD/Fs (N0=0; EMPC=EMPC)
Total PCOD/Fs <2378-X ND=Ot; EMPC=EMPC)
Total 2378s (ND=0; EMPC=0)
Total 2378s (ND=0,5; EMPC=0)
Total 2378s (ND=1; EMPC=0)
Total 2378s (NO=0; EMPC=1)
Total 2378s (N0=0.5; EMPC=1)
Total 2378s (ND=1 : EMPC=1 )
0_1551_MB001
P9
0
0
0
0
12.1
0
0
0
0
0
12.1
12.1
47.9
12.1
30.0
47.9
12.1
30.0
47.9
1015 BLANK
pg
0
0
9.52
23-5
90.5
0
0
27.6
9.92
5.83
167
171
193
112
135
159
112
135
159
-
J| ALT* AN"-"1CAl- «-»««,«.
2009
pg
149
104
90.3
60.3
164
83.8
69.5
59.9
38.9
11.2
831
876
880
280
285
290
295
300
305
3009
P§
104
54.5
29.3
53.5
172
61.2
60.8
59.6
42.9
18.7
657
728
733
296
309
321
296
309
321
Method 23
4004
pg
103
83.6
116
137
811
55.6
57.9
60.6
44.6
18.5
1490
1540
1540
985
991
998
988
995
1000
5004
pg
62.5
99.3
136
179
1220
44.6
34.8
19.2
12.9
9.05
1820
1890
1900
1340
1350
1360
1370
1380
1400
6004
PS
88
94.6
117
160
1350
0
0
21.6
7.56
7.74
1840
1870
1880
1450
1470
1490
1450
1470
1490
Total 2378s = Sum of 17 2378-substrtuted PCDD/PCDF congeners (SARA 313)
[] = EMPC
Reviewer
Date
D2-5
-------
P3290 • Others
Project ID: 110249.2.001.04
Sample Summary - Part 3
Analyte
Other PCDD/Fs (MD=0, EMPC=0)
OlherTCDO
Other PeCDD
Other HxCDD
Other HpCDD
Other TCDF
Other PeCDF
Other HxCDF
Other HpCDF
Other PCDD/Fs (ND=0, EMPOEMPC)
Other TCDD
Other PeCDD
Other HxCDD
Other HpCDD
Other TCDF
Other PeCDF
Other HxCDF
Other HpCDF
0_1551_MB001
pg
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1015 BLANK
PS
0
0
9.52
12.1
0
0
14.8
0
0
0
13.1
12.1
0
0
14.8
0
jL^r**!"-"1"
2009
pg
141
98.8
79.5
32.4
79.6
61.3
41.1
12.4
148
103
79.5
32.4
84.8
71.3
44.1
12.4
3009
pg
97.6
50.6
22
29.6
52
50.5
33.8
12.9
106
62.2
41.9
29.6
71.3
56.4
35.9
12.9
4004
Pfl
97.2
77.5
98.4
78.4
55.6
43.4
31.2
14.3
114
81.8
98.4
78.4
62.6
55.5
35.2
14.3
Method 23
5004
pg
62.5
92.5
127
101
39.3
27.8
14.7
0
84.8
96.2
127
101
42.8
34.2
19.3
0
6004
pg
82.5
87.2
99.3
95.2
0
0
10.2
0
101
91.2
99.3
95.2
0
0
10.2
0
() = DL
[] = EMPC
Reviewer
Date
D2-6
-------
25-f
20 ~
15-
pg
10-
ITEF-TEQ
Project ID: 110249.2,001.04
P3290
0ND=0;EMPC=0
13ND=0;EMPC=EMPC
DND=DU2;EMPC=0
• ND=DU2; EMPC=EMPC
QND=DL; EMPC=EMPC
D2-7
-------
Totals
Project ID: 110249.2.001.04
P3290
0 Total PCDD/Fs (ND=0; EMPC=0)
DTotal PCDD/Fs (ND=0; EMPC=EMPC)
Q Total PCDD/Fs {2378-X ND=DL; EMPC=EMPC)
D2-8
-------
% Rec.
Mean Recoveries of Extraction Standards (N=7)
Project ID: 110249.2.001.04
P3290
EIMean
OStd. Dev.
D2-9
-------
Mean Recoveries of Sampling Standards (N=7)
Project ID: 110249.2.001.04
P3290
0 Mean DStd. Dev.
120
100
% Rec. 60
D2-10
-------
Sample ID: 0_1551_MB001 Method 23
Client Data
Name: MRI
Project ID: 1 1 0249.2.001 .04
Date Collected: n/a
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCOD
1,2,3,4,7.8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6.7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3.6,7,8-HxCOF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2.3,4,6,7.8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCOFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ (ND=DL/2)
Cone.
pg
ND
ND
ND
ND
ND
ND
12.1
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
12,1
0.0121
3.44
Sample Data
Matrix: Air
Weight/Volume: 1
DL
pg
1.82
4.38
4.7
4.31
4.3
2.8
1.37
2.11
1.95
0.64
0.562
0.591
0.725
1.02
1.27
3.19
1.82
4.38
4.43
2.8
1.37
2.03
0.624
1.13
EMPC
pg
12.1
0.0121
3.44
Laboratory Data
Project No.: P3290 Date Received: n/a
Sample ID: 0_1551_MB001 Date Extracted: 28Aug03
QC Batch No.: 1551 Date Analyzed: 08 Sep 03
Qualifier
A
ITEF
ITEF
Recoveries
ES
74.1
75.4
79.2
79.2
79.2
82.3
79.6
87.2
76.2
76.2
76.7
76.7
76.7
76.7
81.7
81.7
80.8
SS
98.8
101
98.2
98.2
98.2
98
98
98.8
101
101
102
102
102
102
98
98
98
AS
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
79.9
|| ALTA ANALYTICAL PERSPECTIVES
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 910 794-1 61 3
Fax:910794-3919
e-mail: yt@ultratrace.com
web: www.ultratrace.com
Checkcode: 3357
Reviewer
Date %x
'53
D2-11
-------
Sample ID: 1015 BLANK Method 23
Client Data
Name: MRI
Project ID: 1 10249.2,001 .04
Date Collected: 20 Aug 03
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7.8-PeCDF
1,2,3.4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7.8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4.7,8,9-HpCDF
OCDF
Totals & TEQs
TCODs
PeCDDs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ (ND=DL/2)
Cone.
pg
ND
ND
ND
ND
ND
11.5
90.5
ND
ND
ND
ND
ND
ND
ND
9.92
ND
ND
ND
ND
9.52
23.5
ND
ND
27.6
9.92
167
0.305
3.94
Sample Data
Matrix: Air
Weight/Volume: 1
DL
pg
1.78
3.05
3.09
2.83
2.82
1.59
2.6
2.39
<5
<5
<5
0.934
0.924
<10
1.78
3.05
1.59
2.49
EMPC
pg
13.1
171
0.305
3.94
Laboratory Data
Project No.: P3290 Date Received: 22 Aug 03
Sample ID: P3290_1 551 _001 Date Extracted: 28 Aug 03
QC Batch No.: 1551 Date Analyzed: 08Sep03
Qualifier
A
A
A
ITEF
ITEF
Recoveries
ES
82.2
85.8
88.7
88.7
88.7
88.3
87.7
82.1
86.1
86.1
88.4
88.4
88.4
88.4
87.2
87.2
88.6
SS
99.1
100
96.7
96.7
96.7
97.7
97.7
99.1
100
100
98.9
98.9
98.9
98.9
97.7
97.7
97.7
AS
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
87.8
1 • AI_TA ANALYTICAL PERSPECTIVES
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 910 794-1 61 3
Fax: 910 794-3919
e-mail: yt@ultratrace.com
web: www.ultratrace.com
Ctieckcode: 3888
Reviewer
Date
-Wj
D2-12
-------
Sample ID: 2009 Method 23
Client Data
Name: MR!
Project ID: 110249.2.001.04
Date Collected : 1 4 Aug 03
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2.3.4,7.8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCOD
OCDD
2.3.7,8-TCDF
1,2,3,7,8-PeGDF
2,3.4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2.3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1, 2,3,4 ,6,7,8-HpCDF
1,2.3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ (ND=DL/2)
Cone.
pg
8.17
5.24
ND
ND
6.1
28
164
4.21
EMPC
8.18
9.91
8.89
EMPC
ND
26.6
ND
11.2
149
104
90.3
60.3
83.8
69.5
59.9
38.9
831
18.5
19
Sample Data
Matrix: Air
Weight/Volume: 1
DL
pg
[Ra=0.864]
3.02
<5
0.627
1.27
EMPC
pg
6.02
8.95
156
109
89
85.5
71.9
876
19.7
20.1
Laboratory Data
Project No.: P3290 Date Received: 22 Aug 03
Sample ID: P3290_1 55 1JW2 Date Extracted: 28 Aug 03
QC Batch No.: 1551 Date Analyzed: 08Sep03
Qualifier
A
A
A
A
A
A
A
A
A
A
A
A
ITEF
ITEF
Recoveries
ES
84.7
87.5
88.6
88.6
88.6
90.9
90.6
86.2
86.3
86.3
88.2
88.2
88.2
88.2
89.6
89.6
89.3
SS
97.9
99.7
97
97
97
98.1
98.1
97.9
99.7
99.7
98.7
98.7
98.7
98.7
98.1
98.1
98.1
AS
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
90.3
1 • ALTA ANALYTICAL. PERSPECTIVES
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 910 794-161 3
Fax:910794-3919
e-mail: yt@ultratrace.com
web: www.ultratrace.com
Checkcode; 4463
Reviewer
Date
D2-13
-------
Sample ID: 1009 Method 23
Client Data
Name: MR!
Project ID: MRI
Date Collected: n/a
Analyte
2.3,7,8-TCDO
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6.7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7.8-HpCDD
OCDD
2.3,7,8-TCDF
1, 2,3,7 .B-PeCDF
2,3,4,7,6-PeCDF
1,2,3,4,7,8-HxCDF
1,2.3,6.7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2.3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ
-------
Sample ID: 3009 Method 23
Client Data
Name: MRI
Project ID: 110249.2.001.04
Date Collected : 1 5 Aug 03
Analytc
2,3,7,8-TCDD
1.2,3,7,8-PeCDD
1,2.3.4.7.8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1, 2,3,4,6,7 ,8-HpCDD
OCDD
2,3.7.8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3.6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3.4J,8,9-HpCDF
OCDF
Totals & TEQs
TCODs
PeCODs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ (ND=DL/2)
Cone.
pg
6.39
NO
NO
ND
ND
23.9
172
9.11
ND
10.3
9.58
8.01
8.18
ND
24.9
5.12
18.7
104
54.5
29.3
53.5
61.2
60.8
59.6
42.9
657
15.7
17.8
Sample Data
Matrix: Air
Weight/Volume: 1
DL
P9
[Ra=0.787]
<5
3.84
<5
<5
<5
0.733
EMPC
pg
113
66.1
49.2
80.4
71.1
61.6
728
15.7
17.8
Laboratory Data
Project No.; P3290 Date Received: 22 Aug 03
Sample ID: P3290_1551_003 Date Extracted: 28 Aug 03
QC Batch No.: 1551 Date Analyzed: 08Sep03
Qualifier
A
A
A
A
A
A
A
A
A
A
ITEF
ITEF
Recoveries
ES
82.4
82.9
86.9
86.9
86.9
91.9
90.9
83.9
83.6
83.6
84.7
B4.7
84.7
84.7
90.3
90.3
90.1
SS
102
106
100
100
100
103
103
102
106
106
104
104
104
104
103
103
103
AS
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
87.3
I| AUTA ANALYTICAL PERSPECTIVES
•
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 910 794-1613
Fax:910794-3919
e-mail: yt@ulfratrace.com
web: www.ultratrace.com
Checkcode: 4973
Reviewer
Date
D2-15
-------
Sample ID: 4004 Method 23
Client Data
Name: MR!
Project ID: 1 1 0249.2.001 .04
Date Collected: 1 8 Aug 03
Analyte
2,3,7,8-TCDD
1 ,2,3,7,8-PeCDD
1. 2.3,4,7 ,8-HxCDD
1 .2,3.6,7,8-HxCDD
1 ,2,3,7,8,9-HxCDD
1 ,2.3.4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1 .2,3.7,8-PeCDF
2,3,4,7,8-PeCDF
1,2.3,4,7,8-HxCDF
1,2,3,S.7.S-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1, 2.3,4,6,7, B-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDDs
HpCDOs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ (ND-DL/2)
Cone,
pg
5.78
6.1
ND
ND
13.2
58.9
811
EMPC
5.59
8.85
9.47
8.41
8.38
ND
24.4
5.91
18.5
103
DO C
83.6
116
137
55.6
57.9
60.6
44.6
1,490
19.2
19.9
Sample Data
Matrix: Air
Weight/Volume: 1
DL
pg
[Ra=0.691]
3.49
<5
<5
EMPC
pg
3.89
120
O7 (^
87,9
66.5
69.9
64.6
1,540
19.6
20.3
Laboratory Data
Project No.: P3290 Date Received: 22 Aug 03
Sample ID: P3290_1551_004 Date Extracted: 28 Aug 03
QC Batch No.: 1551 Date Analyzed: 08 Sep 03
Qualifier
A
A
A
A
A
A
A
A
A
A
A
A
ITEF
ITEF
Recoveries
ES
87
90
92.2
92.2
92.2
96.3
99.9
87.6
89.1
89.1
92.2
92.2
92.2
92.2
95.5
95.5
98.9
SS
97.9
99.4
98.9
98.9
98.9
97.7
97.7
97.9
99.4
99.4
99.4
99.4
99.4
99.4
97.7
97.7
97.7
AS
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
91.8
• I ALTA ANALYTICAL PERSPECTIVES
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 91 0794-1 61 3
Fax:910794-3919
e-mail: yt@ultratrace.com
web: www.ultratrace.com
Checkcode: 5462
Reviewer
Date
D2-16
-------
Sample ID: 5004 Method 23
Client Data
Name: MRI
Project ID: 1 10249.2.001 .04
Date Collected: 19 Aug 03
Analyte
2,3,7,8-TCDD
1. 2,3J .8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDO
1,2,3.4.6,7.8-HpCDD
OCDD
2,3,7,8-TCDF
1. 2,3,7 ,B-PeCDF
2,3,4,7,8-PeCDF
1.2,3,4,7.8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCOF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDS
PeCDDs
HxCDDs
HpCDDs
TCDFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=Q)
TEQ (ND=DU2)
Cone.
pg
EMPC
6.78
ND
8.89
EMPC
77.1
1,220
5.3
ND
7
EMPC
ND
EMPC
ND
12.9
ND
ND
62.5
99.3
136
179
44.6
34.8
19.2
12.9
1,820
10.4
11.1
Sample Data
Matrix; Air
Weight/Volume: 1
DL
pg
[Ra=0.97]
3.83
4.45
<5
1.16
2.78
<10
EMPC
P9
4.36
15.4
6.32
5.41
89.2
103
151
48.1
41.2
35.6
1,890
17.5
18.1
Laboratory Data
Project No.: P3290 Date Received: 22 Aug 03
Sample ID: P3290J551_005 Date Extracted: 28 Aug 03
QC Batch No.: 1551 Date Analyzed: 09Sep03
Qualifier
A
A
A
A
A
A
A
A
A
ITEF
ITEF
Recoveries
ES
60.8
63.5
64.5
64.5
64.5
67.6
68
62.2
63.7
63.7
62.9
62.9
62.9
62.9
66.9
66.9
67,4
SS
100
102
102
102
102
99.2
99.2
100
102
102
104
104
104
104
99.2
99.2
99.2
AS
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
65.8
|| ALTA ANALYTICAL. PERSPECTIVES
•
2714 Exchange Drive
Wilmington
North Carolina 28405
USA
Tel: 910 794-1 61 3
Fax:910794-3919
e-mail: yt@ultratrace.com
web: www.uttratrace.com
Checkcode: 2818
Reviewer
Date
D2-17
-------
Sample ID: 6004 Method 23
Client Data
Name: MRI
Project ID: 1 1 0249.2.001 .04
Date Collected; 20 Aug 03
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7.8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCQF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4.6.7,8-HxCDF
1.2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Totals & TEQs
TCDDs
PeCDDs
HxCDOs
HpCDDs
TCOFs
PeCDFs
HxCDFs
HpCDFs
Total PCDD/Fs
TEQ (ND=0)
TEQ
-------
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)
-------
9.3.1 Batch CSS
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 CSS is initiated at the same instant as the XAD/PUF
cartridges are prepared for sampling.
One Batch CSS 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 CSS's are prepared to provide front- and back-
end calibration verifications for all the samples as well as reinjections when necessary.
The Batch CSS 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 BCSs (M8290B), click
here.
• In order to use the front- and back-end Batch CSSs
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-l
-------
(ES, CS/SS, JS, NS) are prepared from new primary
stock standards with a minimum of one verification
per year.
93.1.1.2 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.
A ls x, A ls -4 - laboratory source
A A
a x
A 1S y A 1S -1 1
^-x A ^-ES •* - independent
where:
Axls = the area of the unlabeled analyte from the
laboratory source
AESls = the area of the labeled extraction standard
from the laboratory source
AX1S = the area of the unlabeled analyte from the
independent source
AES'S = the area of the labeled extraction standard
from the independent source
a 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.
E-2
-------
J NOTE: It is highly recommended that the above
I 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.
. is ^ laboratory source
Ass x AES -4 independent
where:
ASS s = the area of the sampling standard from the
laboratory source
AES'S = the area of the labeled extraction standard
from the laboratory source
ASsls = the area of the sampling standard from the
independent source
AES'S = the area of the labeled extraction standard
from the independent source
a 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.
"t NOTE: When the SS are used as cleanup standards for "
j non-air matrices, replace SS by CS and ES by
i JS in the expression above. '
E-3
-------
9.3.1.1.5 The RPDs between the front- and back-end Batch CS3s
should remain within
9.3.1.1.5.1
9.3.1.1.5.2
Ten percent for the unlabeled compounds
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. .6.1 Twenty percent for the unlabeled compounds
9.3.1. .6.2 Thirty-five percent for the non-air matrices labeled
ES compounds
9.3.1. .6.3 Fifty percent for air matrices labeled ES compounds
9.3.1. .6.4 Twenty percent for air's labeled SS, and
9.3.1. .6.5 Thirty percent for non air's labeled CS compounds
9.3.1. .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-4
-------
9.3.1.2 At the beginning and end of each 12-hour period during which
samples are analyzed, an aliquot of the Batch CSS 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-5
-------
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-6
-------
RRFs used to report the sample analytes. The pseudo-
RRFs 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 Axor 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-7
-------
Table Insert 1:
Batch CS3 PD Requirements
Based on Traditional RRFs
("A" to "C" Types)
Type
A
B
Ci
C2
Analytes
Ax vs ES
ES vs JS
CS vs JS
(non air)
SS vs. ES
(air)
Requirement
±20%
±35% non air
±50% for air0
±35%
±20%
Failure Possible Cause3'0
1 . Calibration out
2. Spiking error
1 . Calibration out
2. Spiking error
1 . Calibration out
2. Spiking error
1 . Calibration out
2. Spiking error
Failure Level
1. PD-3
2. PD-l/PD-2
1. PD-3
2. PD-l/PD-2
1. PD-3
2. -
1. PD-3
2. PD-l/PD-2
Suggested
Corrective Action
1 . New Calibration
2. New Standards/New
Extraction
1 . New Calibration
2. New Standards/New
Extraction
1 . New Calibration
2. Affects other Types
1 . New Calibration
2. New Standards/New
Extraction/New
Sampling4
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 CSS 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-S
-------
Table Insert 2:
Batch CS3 PD Requirements
Based on Pseudo-RRFs
("D" to "G" Types)
Type
D
Ei
E2
Fi
G2
Analytes3
Ax vs. CS/SS
Ax vs. JS
(non air)
Ax vs. JS
(air)
ES vs. CS
(non air)
SS vs. JS
(air)
Requirement
±25%
±35%
±50%
±20%
±50%
a) Pseudo-RRFs are limited to analytes, for
which an analogous/homologous standard is
available:
13,
2,3,7,8-TCDD (Ax) vs. 1JCi2-l,2,3,4-
TCDD (JS)
2,3,4,7,8-PeCDF (Ax) vs. 13Ci2-
1,2,3,4,6-PeCDF (CS)
13Ci2-l,2,3,7,8-PeCDD
1,2,3,4,7-PeCDD (CS)
13Ci2-l,2,3,7,8-PeCDD (ES) vs. 13Ci2-
Do not consider pairs such as OCDD
13
(Ax) vs. 1JCi2-l,2,3,4,6,8,9-HpCDF
13
(SS) or 1JCi2-l,2,3,4,7-PeCDD (CS or
13
SS) vs. 1JCi2-l,2,3,4,6,7-HxCDD (JS)
E-9
-------
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
Ax
-
-
-
ES
Y
-
-
CS
Y
Y
-
JS
Y
Y
Y
"PD Requirements Decision Matrix"—Defective Ax Spiking
(use ICAL RRFs)
Ax
ES
CS
Ax
-
-
-
ES
N
-
-
CS
N
Y
-
JS
N
Y
Y
"PD Requirements Decision Matrix" - Defective JS Spiking
(use BCS3 RRFs)
percent recovery measurements for CS & ES affected, not the analytes
Ax
ES
CS
Ax
-
-
-
ES
Y
-
-
CS
Y
Y
-
JS
N
N
N
"PD Requirements Decision Matrix"—Defective CS Spiking
(use BCS3 RRFs)
percent recovery measurements for CS affected, not the analytes
Ax
ES
CS
Ax
-
-
-
ES
Y
-
-
CS
N
N
-
JS
Y
Y
N
"PD Requirements Decision Matrix"—Defective ES Spiking
(Levels PD-1 or PD-2)
Ax
ES
CS
Ax
-
-
-
ES
N
-
-
CS
Y
N
-
JS
Y
N
Y
E-10
-------
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
Ax
-
-
-
ES
Y
-
-
SS
Y
Y
-
JS
Y
Y
Y
"PD Requirements Decision Matrix"—Defective Ax Spiking
(use ICAL RRFs)
Ax
ES
SS
Ax
-
-
-
ES
N
-
-
SS
N
Y
-
JS
N
Y
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
Ax
-
-
-
ES
Y
-
-
SS
Y
Y
-
JS
N
N
N
"PD Requirements Decision Matrix"—Defective SS Spiking
(use BCS3 RRFs)
percent recovery measurements for SS affected, not the analytes
Ax
ES
SS
Ax
-
-
-
ES
Y
-
-
SS
N
N
-
JS
Y
Y
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
Ax
-
-
-
ES
N
-
-
SS
Y
N
-
JS
Y
N
Y
E-ll
-------
Appendix F
BCS3 Performance Criteria
-------
ANALYTICAL PROCEDURE
ALTA ANALYTICAL PERSPECTIVES
PRIMARY HIGH-RESOLUTION CONCENTRATION CALIBRATION SOLUTIONS
(Regular Initial Calibration for 8290B)
Concentrations In pg / id.
Unlabeled Analytes
2,3,7,8-TCOD
2,3,7,8-TCDF
1,2,3,7,8-PeCOD
1.2.3.7,B-P»CDF
2,3,4,7,B-PeCDF
1,2.3,4,7,8-HxCDD
1,2,3,6,7.8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3.4,7,8-HxCDF
1, 2,3,6,7,8- HxCOF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCOF
1.2,3,4,6,7,8-HpCDO
1.2,3,4,8,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDD
OCDF
Extraction Standard*
1:>Cl2-2,3,7,8-TCDD
">C,2-2,3.7,8-TCDF
'3C,2-1,2,3,7,8-PeCDD
"C,i-1 ,2.3,7,8-PeCDF
"C,,-2,3,4,7,8-PeCDF
"C,,-1,2,3,4,7,8-HxCDD
13C.r1,2,3,6,7,8-HxCDD
13C.r1,2,3,7,8,9-HxCDD
'3C,2-1,2,3,4,7,8-HxCDF
l3C,,-1,2,3,6,7,8-HxCDF
13C,r2,3,4,6,7,8-HxCDF
l:lC,2-1,2,3,7,8,9-HxCDF
!3C,2-1 ,2,3,4,6,7,8-HpCDD
"C.,-1, 2,3,4,6,7, 8-HpCDF
1!>C,:-1,2.3,4,7,8,9-HpCDF
"C,2-OCDD
13C,rOCDF
.Jeafiiin/SampIinQ Stand^fd^
!'Clj-2,3,7,8-TCDD
1JC,j-1,2,3,4,7-PeCDD
"C,z -1 ,2,3,4,6-PeCDF
"C,2-1.2,3,4.6,9-HxCDF
13C12-1 2,3,4,6,8,9-HpCDF
Injection Standards
I;lCir1,2,3,4-TCDD
13C12-1,2,3,4-TCDF
"C12-1,2,3.4,6,7-HxCDD
cso
0-25
026
125
1,25
1.25
1,25
125
1,25
1.25
1,25
1.25
1.25
1.25
1.25
1.2S
2.S
2.5
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
200
200
100
too
100
too
100
100
100
CS1
0,5
0,5
2.5
2.5
2,6
2.5
25
2.5
2.5
25
2.5
25
25
25
2.5
5
5
100
100
too
too
too
too
100
100
100
100
100
100
100
100
100
200
200
05
100
100
100
100
too
too
100
CS2
2
2
10
10
10
10
10
10
10
10
10
10
10
10
10
20
20
100
100
100
100
100
100
100
100
100
too
100
100
too
too
100
200
200
2
100
too
100
100
100
100
100
CS3
10
10
50
50
50
50
50
50
50
50
50
50
SO
50
50
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
too
200
zoo
10
100
100
100
100
100
100
100
CS4
40
40
200
200
200
200
200
200
200
200
200
200
200
200
200
400
400
100
100
100
100
100
100
100
100
100
too
100
100
100
100
100
200
200
40
100
100
100
100
100
100
100
CSS
200
200
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
2000
2000
100
100
100
100
too
100
100
100
100
100
100
100
100
100
100
200
200
200
100
100
100
100
100
100
100
CS6
500
500
2500
2500
2500
2500
2600
2500
2500
2SOO
2500
2SOO
2500
2500
2500
5000
5000
100
100
100
100
100
100
100
100
100
100
too
100
100
100
too
200
200
too
100
100
100
100
100
100
AP-CM-5, Page 1 of 3
F-l
-------
ANALYTICAL PROCEDURE
ALTA ANALYTICAL PERSPECTIVES
Calibration Solutions for Method 23
Compound PCDD/PCDF
Calibration Standards
2,3,7,8-TCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDD
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDO
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
1 ,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDD
OCDF
Internal Standards
"0,2-2,3,7,8-1000
13C,r2,3(7,8-TCDF
)3C,j-1, 2,3,7,8-PeCDD
"0,2-1 ,2,3,7,8-PeCDF
I3Ci2-1,2,3.6,7.8-HxCDD
"0,2-1, 2,3,6,7,8-HxCDF
"C,2-1, 2,3,4,6,7,8-HpCDD
"0,2-1, 2,3,4,6,7,8-HpCDF
13C,2-OCDD
'3C,2-OCDF
Surrogate Standards
37a,-2,3,7,8-TCDD
I3Cir2,3,4,7,8-PeCDF
"C,2-1,2,3,4,7,8-HxCDD
13C,2-1,2,3,4,7,8-HxCDF
"C,?-1,2,3,4,7,8,9-HpCDF
Recovery Standards
"C,2-1,2,3,4-TCDD
"Cti-1 ,2,3,4-TCDF
"C,2-1, 2,3,4,7,8,9-HxCDD
Alternate Standard
"0,2-1 ,2,3,7,8,9-HxCDF
Calibration Solutions (pg/uL)
CSO
0.25
0.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
1.25
2.5
2.5
100
100
100
100
100
100
100
100
100
100
60
60
60
60
60
100
100
100
100
CS1
0.50
0.50
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
5.0
5.0
100
100
100
100
100
100
100
100
100
100
60
60
60
60
60
100
100
100
100
CS2
1.0
1.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
10
10
100
100
100
100
100
100
100
100
100
100
80
80
80
80
80
100
100
100
100
CSS*
5.0
5.0
25
25
25
25
25
25
25
25
25
25
25
25
25
50
50
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
CS4
50
50
250
250
250
250
250
250
250
250
250
250
250
250
250
500
500
100
100
100
100
100
CS5
100
100
500
500
500
500
500
500
500
500
500
500
500
500
500
1000
1000
100
100
100
100
100
100 ; 100
100
100
100
100
120
120
120
120
120
100
100
100
100
100
100
100
100
140
140
140
140
140
100
100
100
100
CS6
500
500
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
5000
5000
100
100
100
100
100
100
100
100
100
100
160
160
160
160
160
100
100
100
100
AP-CM-5, Page 2 of 3
F-2
-------
ANALYTICAL PROCEDURE
ALT* ANALYTICAL PERSPECTIVES
List of First & Last Eluters present in the BCS3
£ti««t tOt Q.llSSJfceSl.jl rilccuuM! 0*e«lFt 5. 1 vi«lr 11
:~r:,,^,
2J»i1T
t.2.}.i,*, ?.»-8ti#i)e 49* it*'*' 1,3,3,4.5,IM-SBCCD n«J8 ^
1, ],«,«. 8- C-CW 2»v**^" l,S,),t,B-HM?»r 33i5* -^
1.3, J,4,«,B~*b«Ce? 14 *«Z''' i.a.l.T^S^S-IUClWf 37-5«-^
1,3, 1,4,4, ?.«-m«Cpf J»f^Vv» I.I. J.4. I,*,8»ltpCSSir 42 >t&**
AP-CM-5, Page 3 of 3
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. 2.
EPA-
4. TITLE AND SUBTITLE
Characterization of Dioxin Emissions From Sources That Use Ball Clays
Emission Test Report: Unimin Corporation, Gleason, TN
7. AUTHOR(S)
Clyde E. Riley, USEPA Mark B. Turner, RTI International
Mary Johnson, USEPA John Hosenfeld, Midwest Research Institute
Brian Shrager, USEPA
Robin Segal I, USEAP
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, NC 27711
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 2771 1
3. RECIPIENT'S ACCESSION
NO.
5. REPORT DATE
March 2010
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D-01-079
13. TYPE OF REPORT AND PERIOD COVERED
Final; March 20 10
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 ANALY3S
a. DESCRIPTORS
Dioxins/furans
Ball Clay
18. DISTRIBUTION STATEMENT
b. IDENTIFIERSOPEN ENDED TERMS
Air pollution control
Ball Clay
19. SECURITY CLASS (Report)
20. SECURITY CLASS (Page)
c. COSATI
Field/Group
21. NO. OF
PAGES
22. PRICE
EPA Form 2220-1 (Re/. 4-77)
-------
United States Office of Air Quality Planning and Publication No.
Environmental Protection Standards EPA-453/R-10-001
Agency Sector Policies and Programs March, 2010
Division
Research Triangle Park, NC
MRI-AED\UNIMIN TEST REPORT NON-CBI VERSION REVISED BY LIBRARY 3-24-10.DOC
------- |