United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-00-015
April 2000
AIR
&EPA
Final Report
Manual Testing and Continuous
Emissions Monitoring
Lime Kiln No. 4
Baghouse Inlet and Stack
Dravo Lime Company
Saginaw, Alabama
v
Mr
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FINAL REPORT
MANUAL TESTING AND CONTINUOUS EMISSIONS MONITORING
LIME KILN NO. 4 BAGHOUSE INLET AND STACK
DRAVO LIME COMPANY
SAGEVAW, ALABAMA
EPA Contract No. 68-D-98-004
Work Assignment No. 3-03
Prepared for:
Mr. Michael L. Toney (MD-19)
Work Assignment Manager
SCGA, EMC, OAQPS
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
April 2000
P:\S523\nNRJTS\DRAVO\REPORTORAVOFIN.WPD
Submitted by
PACIFIC ENVIRONMENTAL SERVICES, INC.
5001 S. Miami Blvd., Suite 300
Post Office Box 12077
Research Triangle Park, NC 27709-2077
(919) 941-0333
FAX (919) 941-0234 y $
Region 5, Library (PL-12J)
77 West Jackson Bpufevard, 12th Floor
Chicago, II 60604-3590
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DISCLAIMER
This document was prepared by Pacific Environmental Services, Inc. (PES) under EPA
Contract No. 68-D-98-004, Work Assignment No. 3-03. This document has been reviewed
following PES' internal quality assurance procedures and has been approved for distribution. The
contents of this document do not necessarily reflect the views and policies of the U.S.
Environmental Protection Agency (EPA). Mention of trade names does not constitute
endorsement by the EPA or PES.
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
2.1 EMISSIONS TEST LOG 2-1
2.2 PCDDs/PCDFs TEST RESULTS 2-1
2.3 HYDROGEN CHLORIDE, AMMONIA, AND CATIONS TEST RESULTS 2-3
2.4 CONTINUOUS EMISSION MONITORS 2-3
3.0 PROCESS DESCRIPTION 3-1
4.0 SAMPLING LOCATIONS 4-1
4.1 KILN NO. 4 BAGHOUSE INLET 4-1
4.2 KILN NO. 4 BAGHOUSE OUTLET 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 LOCATION OF MEASUREMENT SITES AND SAMPLE/VELOCITY
TRAVERSE POINTS 5-2
5.2 DETERMINATION OF STACK GAS VOLUMETRIC FLOW RATE 5-2
5.3 DETERMINATION OF STACK GAS OXYGEN AND CARBON
DIOXIDE CONTENT 5-2
5.4 DETERMINATION OF STACK GAS MOISTURE CONTENT 5-4
5.5 DETERMINATION OF PCDDs/PCDFs 5-4
5.6 DETERMINATION OF TOTAL HYDROCARBONS 5-6
5.7 DETERMINATION OF HYDROGEN CHLORIDE, AMMONIA, AND
CATIONS 5-6
5.8 DETERMINATION OF HCL (INSTRUMENTAL METHOD) 5-8
6.0 QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES
AND RESULTS 6-1
6.1 CALIBRATION OF APPARATUS 6-1
6.2 ON-SITE MEASUREMENTS 6-4
6.3 LABORATORY ANALYSES 6-6
111
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TABLE OF CONTENTS (Concluded)
APPENDIX A RAW FIELD DATA
Appendix A. 1 Raw Field Data, Kiln No. 4 Baghouse Inlet
Appendix A.2 Raw Field Data, Kiln No. 4 Baghouse Outlet
APPENDIX B LABORATORY ANALYTICAL DATA
Appendix B. 1 Laboratory Analytical Data, Method 23
Appendix B.2 Laboratory Analytical Data, Method 26A
APPENDIX C COMPUTER SUMMARIES AND EXAMPLE CALCULATIONS
APPENDIX D CALIBRATION DATA
APPENDIX E PARTICIPANTS
APPENDIX F PROCES S DATA
APPENDIX G TEST METODS
Appendix G. 1
Appendix G.2
Appendix G.3
Appendix G.4
Appendix G.5
Appendix G.6
Appendix G.7
Appendix G.8
EPA Method 1
EPA Method 2
EPA Method 3A
EPA Method 4
EPA Method 23
EPA Method 25A
EPA Method 26A
EPA Proposed Method 322
IV
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LIST OF TABLES
TABLE 2.1 EMISSIONS TEST LOG, DRAVO LIME COMPANY -
SAGINAW, ALABAMA MARCH 28, 1998 2-2
TABLE 2.2 PCDDs/PCDFs SAMPLING AND STACK GAS PARAMETERS
KILN NO. 4 BAGHOUSE INLET AND OUTLET, DRAVO LIME
COMPANY - SAGINAW, ALABAMA 2-5
TABLE 2.3 PCDDs/PCDFs CONCENTRATIONS AND EMISSION RATES KILN NO. 4
BAGHOUSE INLET AND OUTLET DRAVO LIME COMPANY -
SAGINAW, ALABAMA 2-6
TABLE 2.4 PCDDs/PCDFs CONCENTRATIONS AND 2378-TCDD TOXIC
EQUIVALENT CONCENTRATIONS ADJUSTED TO 7 PERCENT
OXYGEN KILN NO. 4 BAGHOUSE INLET AND OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA 2-7
TABLE 2.5 HCL AND AMMONIA SAMPLING AND STACK GAS PARAMETERS
KILN NO. 4 BAGHOUSE INLET, DRAVO LIME COMPANY -
SAGINAW, ALABAMA 2-8
TABLE 2.6 HCL, AMMONIA, AND CATIONS CONCENTRATIONS AND
EMISSION RATES, KILN NO. 4 BAGHOUSE INLET, DRAVO LIME
COMPANY - SAGINAW, ALABAMA 2-9
TABLE 2.7 HCL AND AMMONIA SAMPLING AND STACK GAS PARAMETERS
KILN NO.4 BAGHOUSE OUTLET, DRAVO LIME COMPANY -
SAGINAW, ALABAMA 2-10
TABLE 2.8 HCL, AMMONIA, AND CATIONS CONCENTRATIONS AND
EMISSION RATES, KILN NO. 4 BAGHOUSE OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA 2-11
TABLE 2.9 HCL AND THC CONCENTRATIONS AND EMISSION RATES
KILN NO. 4 BAGHOUSE OUTLET, DRAVO LIME COMPANY -
SAGINAW, ALABAMA 2-12
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LIST OF TABLES (Concluded)
Page
TABLE 3.1 SUMMARY OF OPERATING PARAMETERS 3-2
TABLE 5.1 SUMMARY OF SAMPLING METHODS
DRAVO LIME COMPANY - SAGINAW, ALABAMA 5-1
TABLE 6.1 SUMMARY OF TEMPERATURE SENSOR CALIBRATION DATA 6-2
TABLE 6.2 SUMMARY OF PITOT TUBE DIMENSIONAL DATA 6-3
TABLE 6.3 SUMMARY OF DRY GAS METER AND ORIFICE
CALIBRATION DATA 6-4
TABLE 6.4 SUMMARY OF CALIBRATION GAS CYLINDERS 6-5
TABLE 6.5 SUMMARY OF EPA METHODS 23 AND 26A FIELD SAMPLING
QA/QC DATA 6-8
TABLE 6.6 SUMMARY OF EPA METHOD 23 STANDARDS RECOVERY
EFFICIENCIES 6-10
TABLE 6.7 SUMMARY OF EPA METHOD 26A ANION SPIKES AND DUPLICATE
ANALYSIS 6-11
TABLE 6.8 SUMMARY OF EPA METHOD 26A CATION SPIKES AND
DUPLICATE ANALYSIS 6-12
TABLE 6.9 SUMMARY OF EPA METHOD 26A FIELD BLANK ANALYSIS 6-12
VI
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LIST OF FIGURES
Figure 1.1 Key Personnel and Responsibility for Field Testing at Dravo Lime
Company - Saginaw, Alabama 1-3
Figure 3.1 Kiln No. 4 Process Flow Schematic, Dravo Lime Company -
Saginaw, Alabama 3-3
Figure 4.1 Kiln No. 4 Baghouse Inlet Test Location, Dravo Lime Company -
Sagmaw, Alabama 4-2
Figure 4.2 Kiln No. 4 Baghouse Outlet Test Location, Dravo Lime Company -
Saginaw, Alabama 4-3
Figure 4.3 Kiln No. 4 Baghouse Outlet Sample Point Locations, Dravo Lime
Company - Saginaw, Alabama 4-4
Figure 5.1 CEMS Sampling and Analysis System 5-3
Figure 5.2 EPA Method 23 Sampling Train 5-5
Figure 5.3 EPA Method 26A Sampling Train 5-7
Figure 5.4 Proposed EPA Method 322 CEM Sampling System 5-9
Vll
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1.0 INTRODUCTION
The U.S. Environmental Protection Agency (EPA) Emission Standards Division (BSD) is
investigating the lime manufacturing industry to identify and quantify hazardous air pollutants
(HAPs) emitted from lime kilns. BSD requested that EPA's Emissions, Monitoring and Analysis
Division (EMAD) conduct the required testing. EMAD issued a work assignment to Pacific
Environmental Services, Inc. (PES) to conduct "screening" tests to collect emissions data as
specified in the ESD test request. The planning and initial preparation activities of the program
were conducted through EPA Contract No. 68-D7-0002, Work Assignment No. 0/005.
Remaining preparation, testing, and generation of the Draft Final Report were completed under
EPA Contract No. 68-D7-0002, Work Assignment No. 1/007. Generation of the Final Report,
incorporating EPA's comments on the Draft Final Report, was completed under EPA Contract
No. 68-D-98-004, Work Assignment No. 3-03.
The primary objective was to characterize HAP emissions from Lime Kiln No. 4 at Dravo
Lime Company's facility located in Saginaw, Alabama. The "screening"tests were conducted to
quantify the uncontrolled and controlled air emissions of hydrogen chloride (HC1), total
hydrocarbons (THC), and polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans
(PCDDs/PCDFs). The basic test methods employed were US EPA Test Methods 1 (sample point
location), 2 (velocity and volumetric flow), 3 A (oxygen and carbon dioxide concentration), 4
(moisture content), 23 (PCDDs/PCDFs), 25A (total hydrocarbon concentration), and 26A
(hydrogen chloride). Simultaneous testing was performed at the inlet to the baghouse and at the
stack. Additional analyses of the HC1 train reagents were conducted to quantify the content of
ammonia (NH4) and aluminum, calcium, magnesium, potassium, and sodium cations. Cybelle M.
Brockman of Research Triangle Institute (RTI), Durham, North Carolina recorded plant
operational data during testing. This work was conducted under a separate work assignment
issued to RTI by EPA ESD.
PES used four subcontractors for this effort: Air Pollution Characterization and Control
Inc. (APCC), of Toland, Connecticut; Triangle Laboratories, Inc. (TLI), of Durham, North
Carolina; Research Triangle Institute, and Atlantic Technical Services, Inc. (ATS), of Chapel Hill,
North Carolina. APCC was tasked with the quantification of HC1, oxygen, carbon dioxide, and
THC concentrations at the baghouse inlet and stack using Continuous Emission Monitors
(CEMs). During testing at the facility previous to Dravo (four lime kilns were tested during the
same mobilization), the CEM system was contaminated with a process liquor which rendered the
HC1 analyzer inoperable. Extensive onsite repairs were made to the CEM sampling system and to
the HC1 analyzer. At the direction of the WAM, PES used EPA Method 26A for HC1
quantification instead of the Draft Method 322 so the HC1 data could be collected. TLI provided
analytical services for the analysis of the PCDDs/PCDFs. RTI provided analytical services for the
analysis of the HC1, NH4, and additional cations, and ATS provided technical support for
1-1
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preparation of the Quality Assurance Project Plan (QAPP), Site Specific Test Plan (SSTP), for
reduction of the test data, and for preparation of the Draft Final Report.
The field testing program organization and major lines of communication are presented in
Figure 1.1. The PES Project Manager (PM) communicated directly with the EPA Work
Assignment Manager and coordinated all of the on-site testing activities.
1-2
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I
Dravo Lime Company
Environmental Manager
Lisa A. Potts
(412)995-5547
I
EPA/EMC
Work Assignment Manager
Michael L. Toney
(919)541-5247
1
EPA/ESD
Lead Engineer
Joseph P. Wood
(919)541-5466
PES
Program Manager
JohnT. Chehaske
(919)941-0333
BSD Contractor
Research Triangle Institute
CybeUe M. Brockman
(919)990-8654
PfiS
Coiporate QA/QC Officer
Jeffery L. Van Atten
(703)471-8383
PES
Project Manager
Franklin Meadows
(919)941-0333
Pretest Site Survey
PES
SSTP
PES
Subcontractor
Atlantic Technical Sevices, Inc.
QAPP
PES
Subcontractor
T
Held Testing
PES
Analysis
PES
Report Preparation
PES
Atlantic Technical Services, Inc.
Subcontractor
Air Pollution
Characterization & Control, Ltd
Subcontractor
Triangle Laboratories, Inc.
Subcontractor
Research Triangle Institute
Subcontractor
Atlantic Technical SenVces, Inc.
Figure 1.1 Key Personnel and Responsibility for Field Testing at Dravo Lime Company - Saginaw, Alabama
1-3
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2.0 SUMMARY OF RESULTS
This section provides summaries of the testing conducted at the Dravo Lime Company in
Saginaw, Alabama. The following text and tables summarize the dates and times of the sampling
runs, the parameters of the baghouse inlet and stack gas streams, and the concentrations and mass
emission rates of the target pollutants.
2.1 EMISSIONS TEST LOG
All testing at Dravo Lime Company's Kiln No. 4 was conducted on March 28, 1998.
Table 2.1 presents the emissions test log. The test log summarizes the run number designations,
target pollutants, run times, and down time durations. One Method 23 sampling run was
conducted simultaneously at the baghouse inlet and the stack locations. After the Method 23 runs
were completed, three pair of Method 26A sampling runs were completed. Each pair of Method
26A runs consisted of one run and the inlet location and one run at the outlet.
The inlet sample line was contaminated at the facility tested previously to Dravo, therefore
no CEM data was collected at the baghouse inlet location. CEM data consisting of O2, CO2, and
THC concentrations were collected at the outlet location during the Method 23 sampling runs.
Repairs to the HC1 analyzer were completed during the afternoon of March 28. The analyzer was
calibrated, and system QA/QC checks were conducted. Instrumental HC1 data was collected
starting shortly before the end of the second Method 26 A sampling run. HC1 data was collected
for slightly less than two hours at the stack location. No instrumental HC1 data was collected at
the baghouse inlet location.
2.2 PCDDs/PCDFs TEST RESULTS
PES employed EPA Method 23 for the measurement of PCDDs and PCDFs. The results
of the PCDD/PCDF testing are presented in Tables 2.2 through 2.4. PCDDs/PCDFs results are
presented as 1) actual concentrations and mass emission rates, 2) concentrations adjusted to
7 percent (%) O2, and 3) concentrations adjusted to 7 % O2 and 2378 tetra-chlorinated dibenzo-/>-
dioxin (TCDD) toxic equivalent basis. Due to the process upset described previously, no CEM
data was available for the quantification of O2 and CO2 content at the baghouse inlet. Therefore,
O2 and CO2 concentrations of 10.6 and 19.2 % were assumed based upon the outlet values.
These concentrations should be representative of the concentrations of the diluents at the inlet
location. Adjustment of the congeners to a 2378 toxic equivalent basis was conducted using the
Toxic Equivalency Factor (TEF) values developed by the NATO Committee on the Challenges of
Modern Society, August 1988.
2-1
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TABLE 2.1
EMISSIONS TEST LOG
DRAVO LIME COMPANY - SAGEVAW, ALABAMA
MARCH 28,1998
Run No.
Pollutant
Run Time
Downtime,
Minutes
Kiln No. 4 Baehouse Inlet
I-M23-4
I-M26A-4
I-M26A-5*
I-M26A-6
PCDDs/PCDFs
HC1
HC1, NH4, and Cations
HC1
Kiln No. 4 Baehouse Outlet
O-M23-4
O-M3A-4
O-M25A-4
O-M26A-4
O-M26A-5*
O-M26A-6
O-M322-4
PCDDs/PCDFs
02, C02
THC
HC1
HC1, NH4, and Cations
HC1
HC1 (GFC/IR)
1042-1355
1430-1530
1635-1735
1801-1901
13
0
0
0
1044-1346
1040-1340
1040-1340
1432-1532
1638-1738
1802-1902
1725-1910
2
0
0
0
0
0
15
* At the request of the WAM, the impinger solutions of the second inlet and outlet runs were analyzed to
determine the catches of ammonia and cations (aluminum, calcium, maganesium, potassium, and
sodium)
2-2
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The Method 23 sample fractions consisted of a sample train front-half solvent rinse, a
paniculate filter, a back-half solvent rinse, and an XAD*-2 sorbent resin module. During analysis,
each of the sample fractions was extracted, concentrated, combined, and analyzed using a Gas
Chromatograph with a Mass Spectrometer detector (GC/MS), according to the procedures
outlined in Method 23. During analysis, the combined sample extract was separated with a DB-5
capillary column. Where the results of that analysis indicated the presence of 2378-TCDF
congeners, the analysis was confirmed using a DB-225 capillary column.
The results of the analyses indicated the presence of several congeners that were qualified
as Estimated Maximum Possible Concentrations, or EMPCs. From time to time during the
Method 23 analyses, a peak elutes at the position expected for a particular congener, but the peak
fails validation based on the theoretical split of chlorine isotopes. That is to say that the number
of Cl35 isotopes and the number of Cl37 isotopes attached to the PCDDs/PCDFs congeners should
agree with the C135/C137 ratio found in nature. For each congener, this ratio must agree within
15%. If the mass ratio of chlorine isotopes does not agree with the natural chlorine isotope ratio,
then the peak is flagged as an EMPC.
The values presented as "Total PCDDs" are the sum of the "12346789 OCDD"
polychlonnated dibenzo-p-dioxin and all of the dioxins labeled "Total"; "Total PCDFs" values are
the sum of the "12346789 OCDF" polychlonnated dibenzofuran and all of the furans labeled
"Total". "Total PCDDs + Total PCDFs" values are the sum of the "Total PCDDs" and "Total
PCDFs" values. Values that have been qualified as being EMPC have been included in the sums.
Concentrations and emission rates based on or including EMPC values are denoted by braces
2.3 HYDROGEN CHLORIDE, AMMONIA, AND CATIONS TEST RESULTS
The results of the Method 26A are presented in Tables 2.5 and 2.6 for the Kiln No. 4
baghouse inlet. Table 2.5 summarizes the baghouse inlet flue gas parameters, and Table 2.6
summarizes the concentrations and emission rates of the target pollutants. The impinger catches
from the second Method 26A sampling run (I-M26A-5) were analyzed to determine the catch
weights of ammonia (as NH4), aluminum, calcium, maganesium, potassium, and sodium in
addition to chlorides. Table 2.6 presents two mass emission rates for chlorides, as HC1 and as Cl.
The target parameter during analysis is the concentration of chlorine ions in the impinger catches;
therefore, the calculated in-stack concentration of HC1 and Cl is the same. The mass emission
rate of HC1 is slightly greater because the formula weight of HC1 is slightly more than that of Cl
(36.47 Ib/lb-mol vs. 34.45 Ib/lb-mol). Stack gas parameters and mass emission rates for the
Method 26A sampling runs conducted at the outlet are presented in Tables 2.7 and 2.8.
2.4 CONTINUOUS EMISSION MONITORS
As stated previously, limited CEMs data for HC1 and THC were collected at the baghouse
outlet only. THC, O2, and CO2 concentrations were monitored during the Method 23 sampling
2-3
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run, while the instrumental HCI monitoring was performed during the third Method 26A (run
O-M26A-6). The THC and HCI results are presented in Table 2.9. The concurrent Method 26A
(run O-M26A-6) air stream moisture and flow rate data were used to calculate the HCI emission
rate, while the concurrent Method 23 outlet (run O-M23-4) air stream moisture and flow rate
were used to calculate the emission rate ofTHC.
Proposed Method 322 calls for the analysis of a matrix spike for HCI so that the integrity
of the sampling and analysis system for HCI can be ascertained. After calibration of the HCI
sampling system with the appropriate standards, the flue gas is sampled to determine the baseline
concentration of the HCI. After the baseline concentration is established, a known quantity of
HCI is injected into the sampling system, and the analyzer should report the concentration of the
HCI in the effluent stream plus the contribution of the HCI from the matrix spike injection. The
allowable tolerance for the matrix spike is ± 30% from the predicted value. During the matrix
spike procedures conducted on the sampling system at Dravo Lime Company, the spikes were
never measured by the analyzer, which is to say that the baseline HCI concentrations recorded by
the analyzer did not change when the HCI spike gas was introduced into the system.
The probable cause for the failure of the matrix spike procedure was the presence of finely
divided lime dust which was collected on the heated filter in the CEM stack interface module.
The caustic lime dust had the effect of neutralizing the acidic HCI that was added to the sampling
system during the matrix spike injection. During normal sampling of the stack gas, HCI was
detected because the HCI and lime dust were in a state of equilibrium in the effluent gas.
However, the addition of HCI into the matrix may have forced a response in the equilibrium
condition which resulted in the absorption of additional HCI by the lime dust. Based on this
theory, the results of the HCI testing are most likely representative of the HCI concentrations in
the effluent gas streams, or should any bias exist, are most likely biased low.
2-4
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TABLE 2.2
PCDDs/PCDFs SAMPLING AND STACK GAS PARAMETERS
KILN NO. 4 BAGHOUSE INLET AND OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Total Sampling Time, minutes
Average Sampling Rate, dscfin '
Sample Volume:
dscfb
dscmc
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume d
CO2 Concentration, % by Volume d
Moisture, % by Volume f
Exhaust Gas Volumetric Flow Rate:
acfmf
dscfrn"
dscmm B
Isokinetic Sampling Ratio, %
I-M23-4
03/28/98
180
0.710
127.805
3.619
472
10
20
4.5
162,000
80,100
2,270
100.1
O-M23-4
03/28/98
180
0.745
134.157
3.799
348
10.6
19.2
4.5
131,000
80,300
2,270
103.0
' Dry standard cubic feet per minute at 68° F (20° C) and 1 atm.
b Dry standard cubic feet at 68° F (20° C) and 1 atm.
c Dry standard cubic meters at 68° F (20° C) and 1 atm.
d In-stack oxygen and carbon dioxide concentrarions assumed to due to CEM malfunction.
' Estimated.
f Actual cubic feet per minute at exhaust gas conditions.
8 Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
2-5
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TABLE 2.3
PCDDs/PCDFs CONCENTRATIONS AND EMISSION RATES
KILN NO. 4 BAGHOUSE INLET AND OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
CONGENER
DIOXmS:
2378 TCDD
Total TCDD
12378 PeCDD
Total PeCDD
123478 HxCDD
123678 HxCDD
123789 HxCDD
Total HxCDD
1234678 HpCDD
Total HpCDD
12346789 OCDD
Total PCDDs
FURANS:
2378 TCDF
Total TCDF
12378 PeCDF
23478 PeCDF
Total PeCDF
123478 HxCDF
123678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1 234678 HpCDF
1234789 HpCDF
Total HpCDF
12346789 OCDF
Total PCDFs
Total PCDDs + PCDFs
CONCENTRATION m
(ng/dscm, as measured)
I-M23-4
(0.000829)
0.00553
(0.00111)
{0.000829}
(0.00166)
(0.00138)
(0.00138)
0.00276
0.00221
0.00553
0.0111
{0.0257}
0.0387
0.718
0.0111
0.0111
0.105
0.00276
0.00221
0.00221
(0.00111)
0.0138
0.00193
(0.00193)
0.00193
(0.00553)
(0.845)
(0.870)
O-M23-4
(0.00105)
(0.00105)
(0.00158)
(0.00158)
(0.00211)
(0.00184)
(0.00184)
{0.00237}
{0.00263}
{0.00263}
0.0132
(0.0208)
(0.00132)
0.0447
(0.00105)
(0.00105)
0.00263
(0.00132)
(0.00132)
(0.00158)
(0.00158)
0.00211
(0.00184)
(0.00263)
(0.00211)
(0.00263)
(0.0542)
(0.0750)
EMISSION RATE "
Oig/hr)
I-M23-4
(0.113)
0.752
(0.150)
{0.113}
(0.226)
(0.188)
(0.188)
0.376
0.301
0.752
1.50
{3.50}
5.27
97.8
1.50
1.50
14.3
0.376
0.301
0.301
(0.150)
1.88
0.263
(0.263)
0.263
(0.752)
(115)
(118)
O-M23-4
(0.144)
(0.144)
(0.215)
(0.215)
(0.287)
(0.251)
(0.251)
{0.323}
{0.359}
{0.359}
1.80
(2.84)
(0.180)
6.10
(0.144)
(0.144)
0.359
(0.180)
(0.180)
(0.215)
(0.215)
0.287
(0.251)
(0.359)
(0.287)
(0.359)
(7.40)
(10.2)
* Nanogram per dry standard cubic meter at 20°C and 1 atm.
b Micrograms per hour.
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
2-6
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TABLE 2.4
PCDDs/PCDFs CONCENTRATIONS AND 2378-TCDD TOXIC EQUIVALENT
CONCENTRATIONS ADJUSTED TO 7 PERCENT OXYGEN
KILN NO. 4 BAGHOUSE INLET AND OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
CONGENER
DIOXINS:
2378 TCDD
Total TCDD
12378 PeCDD
Total PeCDD
123478 HxCDD
123678 HxCDD
123789 HxCDD
Total HxCDD
1234678 HpCDD
Total HpCDD
12346789 OCDD
Total PCDDs
FURANS:
2378 TCDF
Total TCDF
12378PeCDF
23478 PeCDF
Total PeCDF
123478 HxCDF
123678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1234678 HpCDF
1234789 HpCDF
Total HpCDF
12346789 OCDF
Total PCDFs
Total PCDDs + PCDFs
CONCENTRATION •
(ng/dscm, adjusted to 7 percent O,)
I-M23-4
(0.00106)
0.00705
(0.00141)
{0.00106}
(0.00211)
(0.00176)
(0.00176)
0.00352
0.00282
0.00705
0.0141
{0.0328}
0.0493
0.916
0.0141
0.0141
0.134
0.00352
0.00282
0.00282
(0.00141)
0.0176
0.00247
(0.00247)
0.00247
(0.00705)
(1.08)
(1.11)
O-M23-4
(0.00142)
(0.00142)
(0.00213)
(0.00213)
(0.00284)
(0.00249)
(0.00249)
(0.00320)
(0.00355)
(0.00355)
(0.0178)
(0.0281)
(0.00178)
0.0604
(0.00142)
(0.00142)
0.00355
(0.00178)
(0.00178)
(0.00213)
(0.00213)
0.00284
(0.00249)
(0.00355)
(0.00284)
(0.00355)
(0.0732)
(0.101)
2378-TCDD
Toricity
Equivalence Factor
1.000
0.500
0.100
0.100
0.100
0.010
0.001
Total PCDDs TEQ
0.100
0.050
0.500
0.100
0.100
0.100
0.100
0.010
0.010
0.001
Total PCDFs TEQ
Total TEQ
2378 TOXIC EQUIVALENCIES
(ng/dscm, adjusted to 7 oercent O,^
I-M23-4
(0.00106)
(0.000705)
(0.000211)
(0.000176)
(0.000176)
0.0000282
0.0000141
(0.00237)
0.00493
0.000705
0.00705
0.000352
0.000282
0.000282
(0.000141)
0.0000247
(0.0000247)
(0.00000705)
(0.0138)
(0.0162)
O-M23-4
(0.00142)
(0.00107)
(0.000284)
(0.000249)
(0.000249)
(0.0000355)
(0.0000178)
(0.00332)
(0.000178)
(0.0000710)
(0.000710)
(0.000178)
(0.000178)
(0.000213)
(0.000213)
(0.0000249)
(0.0000355)
(0.00000355)
(0.00180)
(0.00513)
Nanogram per dry standard cubic meter at 20°C and 1 atm and corrected to 7 percent oxygen.
() Not Detected. Value shown is the detection limit and is included in totals.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
2-7
-------
TABLE 2.5
HCL AND AMMONIA SAMPLING AND STACK GAS PARAMETERS
KILN NO. 4 BAGHOUSE INLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Total Sampling Time, minutes
Average Sampling Rate, dscfm •
Sample Volume:
dscfb
dscmc
Average Exhaust Gas Temperature, °F
02 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfmd
dscfm '
dscmm'
Isokinetic Sampling Ratio, %
I-M26A-4
03/28/98
60
0.537
32.197
0.912
488
10*
20*
4.7
147,400
71,300
2,019
103.9
[JUM26A-5
03/28/98
60
0.531
31.844
0.902
497
10*
20*
4.5
159,700
76,700
2,170
103.7
I-M26A-6
03/28/98
60
0.536
32.149
0.910
516
10*
20*
4.8
165,400
77,700
2,200
103.4
Average
0.534
32.063
0.908
501
-
-
4.7
157,500
75,200
2,130
103.6
' Dry standard cubic feet per minute at 68° F (20° C) and 1 atm.
b Dry standard cubic feet at 68° F (20° C) and 1 atm.
c Dry standard cubic meters at 68° F (20° C) and 1 atm.
d Actual cubic feet per minute at exhaust gas conditions.
° Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
Esdmated oxygen and carbon dioxide values, based upon values observed at outlet location.
2-8
-------
TABLE 2.6
HCL, AMMONIA, AND CATIONS
CONCENTRATIONS AND EMISSION RATES
KILN NO. 4 BAGHOUSE INLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Clock Time, 24-hr clock
Chlorides as HC1
ppmvd "
Ib/hr b
Chlorides as Cl
ppmvd a
lb/hrb
Ammonia
ppmvd "
lb/hrb
Aluminum, Al
ppmvd '
lb/hrb
Calcium, Ca
ppmvd "
lb/hrb
Magnesium, Mg
ppmvd a
lb/hrb
Potassium, K
ppmvd "
lb/hrb
Sodium, Na
ppmvd a
lb/hrb
I-M26A-4
03/28/98
1430-1530
1.72
0.696
1.72
0.677
5.54
1.11
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
I-M26A-5
03/28/98
1635-1735
3.02
1.32
3.02
1.28
8.19
1.77
(0.0119)
(0.00382)
0.0965
0.0462
0.0204
0.00593
0.00649
0.00303
0.0556
0.0153
I-M26A-6
03/28/98
1801-1901
2.58
1.14
2.58
1.11
7.31
1.60
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
Average
2.44
1.05
2.44
1.02
7.01
1.49
(0.0119)
(0.00382)
0.0965
0.0462
0.0204
0.00593
0.00649
0.00303
0.0556
0.0153
* Parts Per Million by Volume Dry.
b Pounds per hour.
() Not Detected. Detection limit values enclosed in parentheses ().
#N/A The impinger catches from the first and the third runs were not analyzed for cation content.
2-9
-------
TABLE 2.7
HCL AND AMMONIA SAMPLING AND STACK GAS PARAMETERS
KILN NO, 4 BAGHOUSE OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Total Sampling Time, minutes
Average Sampling Rate, dscfm '
Sample Volume:
dscfb
dscm c
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfrn"
dscfm'
dscmm'
Isokinetic Sampling Ratio, %
O-M26A-4
03/28/98
60
0.735
44.116
1.249
352
10.6
19.2
4.8
131,000
80,100
2,270
101.8
O-M26A-5
03/28/98
60
0.730
43.822
1.241
349
10.6
19.2
4.5
130,000
79,700
2,260
101.6
O-M26A-6
03/28/98
60
0.743
44.602
1.263
358
10.6
19.2
5.1
132,000
79,900
2,260
103.2
Average
0.736
44.180
1.251
353
10.6
19.2
4.8
131,000
79,900
2,260
102.2
* Dry standard cubic feet per minute at 68° F (20° C) and 1 atm.
b Dry standard cubic feet at 68° F (20° C) and 1 atm.
c Dry standard cubic meters at 68° F (20° C) and 1 atm.
d Actual cubic feet per minute at exhaust gas conditions.
' Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
2-10
-------
TABLE 2.8
HCL, AMMONIA, AND CATIONS
CONCENTRATIONS AND EMISSION RATES
KILN NO. 4 BAGHOUSE OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Clock Time, 24-hr clock
Chlorides as HC1
ppmvd a
lb/hrb
Chlorides as Cl
ppmvd a
lb/hrb
Ammonia
ppmvd "
lb/hrb
Aluminum, Al
ppmvd a
lb/hrb
Calcium, Ca
ppmvd a
lb/hrb
Magnesium, Mg
ppmvd a
lb/hrb
Potassium, K
ppmvd a
lb/hrb
Sodium, Na
ppmvd "
lb/hrb
O-M26A-4
03/28/98
1432-1532
1.39
0.633
1.39
0.615
7.86
1.77
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
O-M26A-5
03/28/98
1638-1738
1.65
0.745
1.65
0.724
7.87
1.76
0.0116
0.00388
0.141
0.0700
0.0264
0.007967
(0.00238)
(0.00116)
0.0250
0.00712
O-M26A-6
03/28/98
1802-1902
2.07
0.938
2.07
0.912
9.43
2.12
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
#N/A
Average
1.70
0.772
1.70
0.750
8.38
1.88
0.0116
0.00388
0.141
0.0700
0.0264
0.007967
(0.00238)
(0.00116)
0.0250
0.00712
* Parts Per Million by Volume Dry.
b Pounds per hour.
() Not Detected. Detection Limit values enclosed in parentheses 0-
#N/A The impinger catches from the first and the third runs were not analyzed for cation content.
2-11
-------
TABLE 2.9
HCL AND THC CONCENTRATIONS AND EMISSION RATES
KILN NO. 4 BAGHOUSE OUTLET
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Run No.
Date
Clock Time, 24-hr clock
Total Sampling Time, minutes
O2 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Volumetric Flow Rate, dscfin d
Hydrogen Chloride:
Formula Weight, Ib/lb-mole
Concentration, ppmvw c
Concentration, ppmvd f
Concentration, ppmvd @ 7% O2 E
Emission Rate, Ib/hr h
Total Hydrocarbons (as methane):
Formula Weight, Ib/lb-mole
Concentration, ppmvw e
Concentration, ppmvd f
Concentration, ppmvd @ 7% O2 E
Emission Rate, Ib/hr h
Total Hydrocarbons (as propane):
Formula Weight, Ib/lb-mole
Concentration, ppmvw e
Concentration, ppmvd f
Concentration, ppmvd @ 7% O2 8
Emission Rate, Ib/hr h
M25A-O-4
03/28/98
1040-1340
180
10.6
19.2
4.5"
80,300
36.47
i
j
i
_ i
16.04
6.3
6.6
8.9
1.3
44.08
2.1
2.2
3.0
1.2
M322-O-4
03/28/98
1725-1910
90
10.6"
19.2 a
5.1°
79,900
36.47
7.1
7.5
10.1
3.4
16.04
i
i
i
- '
44.08
i
_ i
- '
- '
1 Diluent concentrations estimated based upon data collected during sampling run M25A-O-4
b Moisture concentration based upon data collected during sampling run M23-O-4
c Moisture concentration based upon data collected during sampling run M26A-O-6
d Dry standard cubic feet per minute at 68* F (20* C) and 1 atm.
' Parts per million by volume wet.
f Parts per million by volume dry.
g Parts per million by volume dry corrected to 7% O2
h Pounds per hour.
1 No data was acquired during the test period.
2-12
-------
3.0 PROCESS DESCRIPTION
Kiln No. 4 at Dravo Lime Company is an inclined rotating kiln. Limestone is charged at
the back end of the kiln through a preheater and tumbles toward the front end of the kiln via
gravity and the rotating motion of the kiln. Combustion air and fuel, which consists of pulverized
coal and coke, enter at the front end of the kiln. Combustion products are removed from the kiln
by an induced draft (ED) fan and pulled through the preheater and a series of multiclones and are
discharged to the atmosphere through a reverse-air baghouse and the stack. Ambient air is
introduced at the inlet to the preheater when the exhaust gas temperature at this location exceeds
a certain temperature.
Process data were recorded by the ESD contractor during testing. The data were
recorded from computer screens in the kiln control room; the recorded data were measured with
instruments already in place and used by the plant for process control of the kilns. A summary of
process operations during the testing is presented in Table 4.1. Individual recordings of process
parameters may be found in the appendix.
Except for opacity, the recorded process parameters varied only slightly during testing - as
indicated by the low values of percent relative standard deviation (% RSD) in Table 1. The %
RSD for opacity was high because of the 40 percent opacity recording at 2:43 pm; as seen in
Table 2, this opacity recording was extremely high compared to previous recordings, and those
that followed. The start-up of Method 26 testing (which occurred around this time) may have
interfered with the opacity monitor. No other process anomalies occurred during testing.
The plant does not measure the pressure drop across the baghouse (one of the process
parameters listed in the test plan for recording). The plant does measure the static pressure
downstream of the fan (just prior to the baghouse); the static pressure at this location was
recorded during testing and had an average value of 8.3 inches of water. The testing crew took
five measurements of the static pressure at the outlet test location (just downstream of the
baghouse); the measurements were taken during Method 23 and 26 testing (one measurement per
run) and during the velocity traverse. The five measurements ranged from -0.47 to -0.53 inches
of water; the average was -0.50 inches of water. The pressure drop from downstream of the fan
to the outlet test location was 7.8 inches of water. A typical value of the pressure drop across the
baghouse was not reported in the plant's questionnaire or mentioned during the pre-test site
survey.
During testing, Kiln No. 4 produced a high calcium lime from limestone which was
quarried on-site. The plant does not measure limestone feed rate or lime production rate. Plant
3-1
-------
personnel were asked whether or not they knew the production during testing, and they replied
no. Consequently, the production level during testing is not known.
Little information is available to determine if values of the other recorded parameters were
typical of normal operation. The only relevant parameters reported in the plant's questionnaire
were the exhaust temperature at the exit of the kiln (2000 degrees Fahrenheit [°F]), the inlet
temperature to the baghouse (435 °F), the ratio of coal and coke to lime (0.20 tons of coal and
coke per ton of lime), and the design capacity of the kiln (900 tons of lime per day). The reported
temperatures are consistent with those recorded during testing. The average coal and coke feed
rate during testing was 6.20 tons per hour, which was below the range of coal feed rates cited
during the pre-test site survey (6.4 to 6.6 tons of coal per hour). Based on the average coal and
coke feed rate during testing, and the reported coal and coke to lime ratio, the plant produced
approximately 31 tons of lime per hour during testing. This translates into approximately 744
tons of lime per day (assuming the kiln operates 24 hours per day), which is less than the design
capacity of 900 tpd reported in the plant's questionnaire.
TABLE 3.1
SUMMARY OF OPERATING PARAMETERS
Parameter
Fuel Feed Rate, tph
Kiln Speed, rpm
Preheater Inlet
Temperature, "F
Baghouse Inlet
Temperature, °F
Baghouse Static
Pressure, in. H2O
Stack Gas Opacity
Mean
6.20
1.37
2002
466
8.3
5.4
% RSD
2.19
0.714
0.4371
1.09
7.0
16
Minimum
5.96
1.36
1985
460
7.1
4.3
Maximum
6.54
1.38
2025
482
9.3
8
3-2
-------
Combustion
Air
Pulverized
coal & coke
Lime
Limestone
aghouse
Inlet
Test
Location
Figure 3.1 Kiln No. 4 Process Flow Schematic, Dravo Lime Company - Saginaw Alabama
3-3
-------
4.0 SAMPLING LOCATIONS
As stated previously, source sampling was conducted to determine uncontrolled and
controlled emissions of HC1, PCDDs/PCDFs, cations, and total hydrocarbons from Lime Kiln
No. 4 located at Dravo Lime Company's Saginaw, Alabama facility. Testing was conducted at
the inlet of the baghouse and at the Kiln No. 4 stack. Descriptions and schematic diagrams of the
test locations are presented below.
4.1 KILN NO. 4 BAGHOUSE INLET
The Kiln No. 4 baghouse inlet measurement site was located in an 84-inch inside diameter
(ID) round, vertical duct, 38 inches (0.5 duct diameters) downstream of the nearest flow
disturbance (90° bend) and 300 inches (3.6 duct diameters) upstream of the fan inlet.
According to EPA Method 1 criteria, this site required 24 sample traverse points. Only
one sample port was available for isokinetic testing, and because of a lack of clearance for the
Method 23 sampling train behind the port, isokinetic sampling was conducted at a single point in
the center of the duct. Prior to the test, a velocity traverse was conducted through the port which
indicated a uniform velocity profile. The center point of the duct approximated the average air
stream velocity. A schematic of the sampling location is depicted in Figure 4.1.
4.2 KILN NO. 4 BAGHOUSE OUTLET
The baghouse stack measurement site was located in an 83.25-inch inside diameter (ID)
round, vertical duct, 432 inches (5.2 duct diameters) downstream of the nearest flow disturbance
(breeching) and 617 inches (7.4 duct diameters) upstream of the nearest flow disturbance (the
exhaust to the atmosphere). Only two ports were available for testing. Because the Method 322
sampling probe occupied one of the test ports, the Method 23 sampling was performed using only
one port. According to EPA Method 1 criteria, this site required a total of 12 sample traverse
points; because only one axis was used, the 12 points were located along one of the perpendicular
diameters. Figure 4.2 shows a simplified schematic of the inlet measurement site and Figure 4.3
shows the sample traverse point locations.
A check for the presence of non-parallel flow was conducted as specified in Section 2.4 of
EPA Method 1. The results of the cyclonic flow check showed an average yaw angle (a) of 2.2
degrees which was well within the Method 1 criterion of 20 degrees; therefore, the sampling
location was considered suitable for isokinetic sampling.
4-1
-------
3" Sample Port
Multiclone
Discharge
Method 23 Sampling Port
CEM Sampling Port
Catwalk
Figure 4.1 Kiln No. 4 Baghouse Inlet Test Location, Dravo Lime Company - Saginaw,
Alabama
4-2
-------
617"
432"
From Baghouse •
Sampling Ports
(1 for Method 23
1 for CEMs)
Figure 4.2 Kiln No. 4 Baghouse Outlet Test Location, Dravo Lime Company - Saginaw,
Alabama
4-3
-------
Traverse
Point
No.
1
2
3
4
5
6
7
8
9
10
11
12
Distance
From Inside
Wall (in.)
1.7
5.6
9.8
14.7
20.8
29.6
53.6
62.4
68.5
73.4
77.7
81.5
Figure 4.3 Kiln No. 4 Baghouse Outlet Sample Point Locations, Dravo Lime Company
Saginaw, Alabama
4-4
-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES
Source sampling was performed at the baghouse inlet and the Kiln No. 4 stack to
determine the concentrations and mass emission rates of PCDDs/PCDFs, HCI, and total
hydrocarbons. Table 5.1 presents a summary of the sampling and analytical methods that were
used to quantify the target compounds. The following text provides brief descriptions of the
sampling and analysis procedures that were employed.
TABLE 5.1
SUMMARY OF SAMPLING METHODS
DRAVO LIME COMPANY - SAGINAW, ALABAMA
Test Method
EPA Method 1
EPA Method 2
EPA Method 3 A
EPA Method 4
EPA Method 23
EPA Method 26A
EPA Method 26A
Proposed Method 322
Parameter
Sample Point Location
Velocity and Flow
Oxygen, Carbon Dioxide
Moisture
PCDDs/PCDFs
HCI, Ammonia
Aluminum, Calcium,
Maganesium, Potassium,
Sodium
HCI
Measurement Principle
Linear Measurement
Differential Pressure,
Thermocouple
Paramagnetic and NDIR
Continuous Analyzers
Gravametric
Gas Chromatograph / Mass
Spectrometry
Ion Chromatograph
Inductively Coupled Plasma /
Atomic Emission Spectroscopy
Gas Filter Correlation / Infra Red
5-1
-------
5.1 LOCATION OF MEASUREMENT SITES AND SAMPLE/VELOCITY
TRAVERSE POINTS
EPA Method 1, "Sample and Velocity Traverses for Stationary Sources," was used to
establish velocity and sample traverse point locations at the baghouse outlet. The process
ductwork and locations of measurement sites and traverse points are discussed in Section 4.0 of
this document.
5.2 DETERMINATION OF STACK GAS VOLUMETRIC FLOW RATE
EPA Method 2, "Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S
Pitot Tube)," was used to determine exhaust gas velocity. A Type S Pitot tube, constructed
according to Method 2 criteria and having an assigned coefficient of 0.84, was connected to an
inclined-vertical manometer and used to measure the velocity pressure (Ap). The stack gas
temperature was also recorded at each traverse point using a Type K thermocouple. The average
gas velocity was calculated from the average square root of the velocity pressure, average stack
gas temperature, air stream molecular weight, and absolute outlet pressure. The volumetric flow
rate is the product of velocity and the cross-sectional area of the duct/outlet at the sampling
location.
5.3 DETERMINATION OF STACK GAS OXYGEN AND CARBON DIOXIDE
CONTENT
The CEM system was housed in the APCC Environmental Monitoring Laboratory
positioned near the baghouse outlet. Stack gas was drawn from the outlet through a heated
Teflon* sample line (320 °F nominal) and sample conditioning system (except the THC sample) to
remove moisture from the gas stream. A leakless Teflon* diaphragm pump then drew the sample
through an unheated dry Teflon* sample line and pumped it through a manifold under slightly
positive pressure with a bypass to the atmosphere. CO2 and O2 samples were continuously drawn
from this manifold to their respective analyzers. A heated sample was introduced directly to the
THC analyzer. All CEM data was recorded using a Tracor/Westronics 3000 automatic digital
data logger. All data was monitored by a TracerAVestronics 3000 digital data logger which
recorded using its integral color printer. Trends were monitored using the strip chart mode with
averages printed digitally for 5-minute intervals and/or the test period. Emissions data was
"sampled" by the data logger at 5-second intervals. Figure 5.1 shows a schematic of the system.
EPA Method 3 A, "Determination of Oxygen and Carbon Dioxide Concentrations in
Emissions from Stationary Sources (Instrumental Analyzer Procedure)," was used to determine
the O2 and CO2 concentrations at the baghouse outlet location. A Horiba CMA 321 analyzer was
used to monitor O2 and CO2 concentrations. Oxygen was measured using the paramagnetic
analytical technique. The analyzer was operated on a range of 0 - 25 percent and calibrated using
zero nitrogen and oxygen-in-nitrogen calibration standards of 11.1 and 20.2 percent. CO2 was
5-2
-------
Slack
Wall
Heated Filter
Sample By-Pass
Vent
Figure 5.1 CEMs Sampling and Analysis System
-------
measured using the principle of infra-red absorption. The analyzer was operated on a range of
0-40 % by volume and calibrated with carbon dioxide standards of 11.0 and 20.4 %. Radiation
absorbed by CO2 in the sample cell produces a capacitance change in the detector which is
proportional to the CO2 concentration. Calibration gas standards were prepared according to the
EPA Traceability Protocol.
5.4 DETERMINATION OF STACK GAS MOISTURE CONTENT
EPA Method 4, "Determination of Moisture Content in Stack Gases," was used to
determine the air stream moisture content. EPA Method 4 was performed in conjunction with
each EPA Method 23 and Method 26A test run. At the baghouse inlet single-point isokinetic
sampling was conducted. At the baghouse outlet multi-point, isokinetic sampling was conducted.
Condensed moisture was determined by recording pre-test and post-test weights of the impingers,
reagents, and silica gel. Due to weighing problems for run I-M23-4 at the baghouse inlet, no
condensed moisture weight is available; for calculation purposes, the moisture percent measured
by the Method 23 run at the outlet (0-4) was used as an estimate for the moisture percent for run
I-M23-4.
5.5 DETERMINATION OF PCDDs/PCDFs
EPA Method 23, "Determination of Polychlorinated Dibenzo-P-Dioxins and
Polychlorinated Dibenzofurans from Stationary Sources," was used to collect dioxins and furans
at each location. In addition, the proposed rules amending Method 23 as published in the Federal
Register, Volume 60, No. 104, May 31, 1995 were incorporated. These proposed rules correct
existing errors in the method, eliminate the methylene chloride rinse, and clarify the quality
assurance requirements of the method.
At the baghouse outlet, a multi-point integrated sample was extracted isokinetically from
the traverse points shown in Section 4.0; at each traverse point, sampling was performed for
15 minutes for a total run time of 180 minutes. At the baghouse inlet, the single sampling point
was sampled for 180 minutes, with readings taken every 10 minutes.
The EPA Method 23 samples were extracted through a glass nozzle, a heated glass-lined
probe, a precleaned and heated glass fiber filter, a water cooled condenser coil and an adsorbent
trap containing approximately 40 g of XAD®-2 adsorbent resin. The EPA Method 23 sampling
train is shown in Figure 5.2.
TLI prepared the filters and adsorbent traps and performed the analyses. The samples
were extracted and analyzed according to EPA Method 23 and the above mentioned proposed
rules amendment. The sample components (filter, XAD*, and rinses) were Soxhlet extracted and
combined. The sample was then split with half being archived and the other half analyzed.
Analysis was performed on a high resolution Gas Chromatograph with a high resolution Mass
Spectrometer detector.
5-4
-------
Burton Hook
Nozzle
Gas
Flow .,
TypeS
Pilot Tube
Gas
Exit
Temperature
Sensor
Condenser
Stack
Wall
Healed Glass
Liner
Temperature
Sensor
Inclined Recirculation
Manometer PumP
Temperature
..Sensors
ai.
'
t
111 • Ice MII
|||IWater|||l
ll|Bath Ml
ll'l ll'l
Empty 100 ml HPLC Water Empty Silica Gel
Inclined
Manometer
Vacuum
Pump
Vacuum
Line
Figure 5.2 EPA Method 23 Sampling Train
-------
5.6 DETERMINATION OF TOTAL HYDROCARBONS
EPA Method 25 A, "Determination of Total Gaseous Organic Concentration using a Flame
lonization Analyzer," was used to determine total hydrocarbon concentrations at the Kiln No. 4
stack. A VIG Industries Total Hydrocarbon Analyzer, which utilizes a flame ionization detector
(FID), was used to measure hydrocarbons. Approximately 5.0 liters per minute (1pm) of sample
gas was drawn from the source through a heated Teflon* sample line. The sample gas was drawn
through a heated filter and valves by a heated pump. The sample gas was introduced into the FID
chamber and any hydrocarbons in the sample were ionized by a hydrogen flame. The flame was
positioned between two charged plates, and the associated electric field induces the migration of
the ions towards the charged plates. The ion migration resulted in the genera- tion of a current
directly proportional to the amount of hydrocarbons present in the sample.
The analyzer was calibrated using methane calibration gas standards. THC concentrations
are in presented on a methane basis. In addition THC concentrations have been presented as
propane multiplying the methane result by a factor of three.
5.7 DETERMINATION OF HYDROGEN CHLORIDE, AMMONIA, AND CATIONS
EPA Method 26 A "Determination of Hydrogen Chloride Emissions from Stationary
Sources," was used to measure the chloride and ammonia concentrations in the gas streams at the
baghouse inlet and outlet locations. In addition, the impinger contents from the second run at
each location were analyzed for the following cations - aluminum, calcium, potassium,
magnesium, and sodium.
A sample was extracted isokinetically through a glass nozzle, probe liner, a Quartz fiber
filter maintained at greater than 250°F, and a series of impingers. The first and second impingers
were each charged with 100 milliliters of 0.1 N sulruric acid, the third and fourth impingers were
each charged with 100 milliliters of 0.1 N sodium hydroxide, and the fifth impinger contained a
known mass, approximately 200 grams, of silica gel. A schematic of this train is presented in
Figure 5.3.
Pre- and post-test leak checks were conducted on the Method 26A sampling train to
guard against dilution of the collection sample with ambient air. Prior to testing, the train was
leak checked at a system vacuum of at least fifteen inches of mercury, and after each test, the train
was leak checked at the highest system vacuum observed during the test. The maximum
acceptable leakage rate is 0.02 cftn, and all leak checks that were performed met this criteria.
After each test, the impinger contents were recovered, placed into labeled polypropylene
sample bottles, and transported to the analytical laboratory for chlorides, ammonia, and cations
content analysis. The impinger solutions were recovered and analyzed by ion chromatography for
the ammonia and chlorides, and ICP for the cations (aluminum, calcium, magnesium, potassium,
and sodium). The samples were analyzed by the Center for Environmental Measurement and
Quality Assurance of the Research Triangle Institute located in Research Triangle Park, North
Carolina.
5-6
-------
Lfl
Type S Pilol Tube
Figure 5.3 EPA Method 26A Sampling Train
-------
5.7 DETERMINATION OF HCL (INSTRUMENTAL METHOD)
Proposed EPA Method 322, "Measurement of Hydrogen Chloride Emissions from
Portland Cement Kilns by GFC/IR," was used to monitor HC1 emissions at the stack. The stack
gas sample was extracted from the sampling location and transported to the HC1 analyzer (a
Perkin Elmer (PE) MCS-100) through a heated sample probe, heated sample line, and a heated
sample pump. Sampling components were maintained at a minimum temperature of 375°F. A
heated three-way valve was attached to the probe assembly to allow for sampling of stack gas or
for the introduction of HC1 calibration standards. The sample exited the pump and passed
through a heated rotameter and into the analyzer containing the gas filter correlation infrared
spectrometer (GFC/IR). Hydrogen chloride in the sample cell attenuates an infrared light source.
The intensity of the attenuated beam is measured by a detector positioned at the end of the cell.
The amount of HC1 in the sample gas stream is related to the amount of light attenuated. A
schematic of this system is presented in Figure 5.4.
5-8
-------
Haatsd Preb«
(mln. 375'F) H*»t«4 Filter Box
Thrs*-way vary*
Uiw
PM-10
Cyclon
Microprocessor
DDDD DDQDD
Qss Filter Correlation
Intrsrsd Analyzer
Figure 5.4 Proposed EPA Method 322 CEM Sampling System
5-9
-------
-------
6.0 QUALITY ASSURANCE/QUALITY CONTROL
PROCEDURES AND RESULTS
This section describes the specific QA/QC procedures employed by PES in performing this
series of tests. The procedures contained in the "Quality Assurance Handbook for Air Pollution
Measurement Systems, Volume III, Stationary Source Specific Methods," EPA/600/R-94/038c,
and in the reference test methods served as the basis for performance for all testing and related
work activities in this project.
6.1 CALIBRATION OF APPARATUS
The preparation and calibration of source sampling equipment is essential in maintaining
data quality. Brief descriptions of the calibration procedures used by PES follow.
6.1.1 Barometers
PES used aneroid barometers which are calibrated against a station pressure value,
corrected for elevation, reported by a nearby National Weather Service Station.
6.1.2 Temperature Sensors
Bimetallic dial thermometers and Type K thermocouples were calibrated using the
procedure described in Calibration Procedure 2a of EPA/600/R-94/038c. Each temperature
sensor was calibrated over the expected range of use against an ASTM 3C or 3F thermometer.
Table 6.1 summarizes the type of calibrations performed, the acceptable levels of variance, and
the results. Digital thermocouple displays were calibrated using a thermocouple simulator having
arangeofO-2400°F.
6.1.3 Pitot Tubes
Type S pitot tubes constructed to EPA Method 2 specifications were used. Pitot tubes
meeting these specifications are assigned to a baseline coefficient to 0.84 and need not be
calibrated. The dimensional criteria and results for each pitot tube used are summarized in
Table 6.2.
6-1
-------
TABLE 6.1
SUMMARY OF TEMPERATURE SENSOR CALIBRATION DATA
Temp.
Sensor I.D.
4E
7D
MB-10
RMB-15
Usage
Stack Gas
Stack Gas
Dry Gas
Meter Inlet
Outlet
Dry Gas
Meter Inlet
Outlet
Temperature, *R
Reference
534
498
663
799
500
534
666
800
493
536
666
492
536
666
493
534
668
493
534
668
Sensor
534
498
662
800
501
534
665
801
494
536
665
494
537
665
495
534
670
493
535
668
Difference
(%)
0.0%
0.0%
-0.15%
0.13%
0.20%
0.0%
-0.15%
0.12%
0.20%
0.0%
-0.15%
0,40%
0.19%
-0.15%
0.40%
0.0%
0.30%
0.0%
0.19%
0.0%
Criteria
(%)
<±1.5%
<±1.5%
<±1.5%
<±1.5%
-------
TABLE 6.2
SUMMARY OF PITOT TUBE DIMENSIONAL DATA
Measurement
«i
Oj
Pi
P2
Y
e
A
Z
w
Dt
A/2D,
Criteria
<10°
<10°
<5°
<5°
-
-
-
<, 0.125 in.
< 0.03125 in.
0.1875" < Dt<: 0.375"
1.05D,< A< 1.50Dt
Acceptable
Assigned Coefficient
Results
Pitot Tube
Identification
4E
0
1
1
3
0
1
0.973
0
0.017
0.375
1.30
Yes
0.84
7D
3
3
1
1
1
0
0.931
0.016
0.0
0.375
1.24
Yes
0.84
6-3
-------
6.1.4 Differential Pressure Gauges
PES used Dwyer inclined/vertical manometers to measure differential pressures. The
differential pressures measurements included velocity pressure, static pressure, and meter orifice
pressure. Manometers were selected with sufficient sensitivity to accurately measure pressures
over the entire range of expected values. Manometers are primary standards and require no
calibration.
6.1.5 Dry Gas Meters and Orifices
The EPA Method 23 and Method 26A dry gas meters and orifices were calibrated in
accordance with Sections 5.3.1 and 5.3.2 of EPA Method 5. This procedure involves direct
comparison of the metered volume passed through the dry gas meter to a reference dry test meter.
The reference dry test meter is calibrated annually using a wet test meter. Before its initial use in
the field, the metering system was calibrated over the entire range of operation, as specified in
EPA Method 5. After field use, a calibration check of the metering system was performed at a
single intermediate setting based on the previous field test. Acceptable tolerances for the dry gas
meter correction factor (y) and orifice calibration factor (AH@) are ± 0.02 and ± 0.20 from
average, respectively. The calibration check of the dry gas meter correction factor must agree
within 5 percent of the correction factor generated during the annual calibration. The results for
the gas meters and orifices used in this test program are summarized in Table 6.3.
TABLE 6.3
SUMMARY OF DRY GAS METER AND ORIFICE CALIBRATION DATA
Meter
No.
MB-10
RMB-15
Dry Gas Meter Correction Factor
(Y)
Pre-test
1.021
1.000
Post-test
0.985
1.002
% Diff,
-3.6
0.2
EPA Criteria
±5%
±5%
Reference Orifice Pressure
(AH@, in. H2O)
Average
1.72
1.56
Range
1.59 - 1.79
1.56-1.56
EPA Criteria
1.72 ±0.20
1.56± 0.20
6.2 ON-SITE MEASUREMENTS
The on-site QA/QC activities include:
6.2.1 Measurement Sites
Prior to sampling, the stack and inlet duct were checked dimensionally to determine
measurement site locations, location of velocity and sample test ports, inside stack/duct
dimensions, and sample traverse point locations. Inside stack/duct dimensions were checked
6-4
-------
through both traverse axes to ensure uniformity of the stack/duct inside diameter. The inside
stack/duct dimensions, wall thickness, and sample port depths were measured to the nearest 1/16
inch.
6.2.2 Velocity Measurements
All velocity measurement apparatus were assembled, leveled, zeroed, and leak-checked
prior to use and at the end of each determination. The static pressure was determined at a single
point near the center of the stack or duct cross-section.
6.2.3 Method 3A (Stack Gas Composition^ / Method 25A
The field QA/QC activities for Method 3A and Method 25A included the use of EPA
Protocol calibration gases during pretest calibration error tests, system bias checks, and response
time tests; and post-test zero and calibration drift determinations. Table 6.4 lists the calibration
gas cylinder numbers, concentrations, and expiration dates. Calibration error tests, system bias
checks, calibration drift checks, and response time checks are shown in Appendix D. All pre- and
post-test calibrations and bias checks were well within the method specifications.
TABLE 6.4
SUMMARY OF CALIBRATION GAS CYLINDERS
Cylinder Number
AO 18685
AO 18704
AO 18749
A017718
CC79006
SX-27307
CC46103
CC84096
CC84096
CC60029
CC60029
Contents
10.7 ppm HC1 in nitrogen
26.0 ppm HC1 in nitrogen
37.6 ppm HC1 in nitrogen
101 ppm HC1 in nitrogen
29.97 ppm CH4 in nitrogen
51.1 ppm CH4 in nitrogen
84.8 ppm CH4 in nitrogen
10.99 % CO2 in N2/O2/CO2
11.05%O2inN2/O2/CO2
20.2 % CO2 in N2/O2/CO2
20.4%02inN,/0,/CO,
Expiration Date
08-26-98
08-12-98
08-25-98
08-12-98
11/4/97
08-20-99
3/5/97
03-02-01
03-02-01
04-03-99
04-03-99
6-5
-------
6.2.4 Moisture
The EPA Method 23 and Method 26A sampling trains were used to determine the flue gas
moisture content. During sampling, the exit gas of the last impinger was maintained below 68°F
to ensure complete condensation of flue gas water vapor. The total moisture was determined
gravimetrically using an electronic platform balance with 0.1 gram sensitivity. The XAD*
adsorbent module from the EPA Method 23 sampling train was also weighed and its weight
included in the moisture catch.
6.2.5 Method 23 and Method 26A
Table 6.5 summarizes the EPA Method 23 and Method 26A critical field sampling QA/QC
measurements made and the EPA's acceptability criteria. All pre- and post-test sample train leaks
met the acceptance criteria. The isokinetic sampling rates for all runs deviated by no more than
4% from 100%, thereby meeting the method criteria of 90-110%.
Due to plant operational issues, a field blank for the EPA Method 23 sample train was not
collected.
6.2.6 EPA Proposed Method 322
The HC1 sampling and analysis system was calibrated with a zero gas and three upscale
gas standards, corresponding to 10.7, 26, and 37.6 ppm HC1 in nitrogen. The response of the
analyzer was within 7.5% of span, as specified by the method, for all calibration standards with
the exception of the high-level gas. The calibration error for the high-level gas was 11.8% of
span, which means that HC1 concentrations in this range of the calibration curve would be over-
estimated by approximately 12%. However, the average concentration during the sampling run
was 7.1 ppm HC1, which is in the region of the calibration curve that was well characterized. The
response of the sampling system to the 10.7 ppm HC1 standard was within 3% of the instrument
span.
As stated previously, the HC1 sampling system did not respond to the injection of the HC1
spike gases. The effect of this failure is described in Section 2 of this document. Because of the
failure of the matrix spikes, the HC1 data collected at this facility is most likely biased low.
6.3 LABORATORY ANALYSES
6.3.1 EPA Method 23 PCDDs/PCDFs
Prior to the field testing program, TLI prepared PES' XAD*-2 adsorbent traps and
precleaned the glass fiber filters. TLI's laboratory QA/QC program consisted of adding
isotopically labeled standards to each sample at various stages of the project to determine
recovery efficiencies. The following types of standards were used:
6-6
-------
Surrogate Standards were spiked in the TLI laboratory on the XAD*-2 resin prior to the
field sampling program. Recovery efficiencies for these surrogate compounds provided a
measure of the sample collection efficiency and an indication of any analytical matrix
effects.
Internal Standards were spiked in the TLI laboratory after the field sampling program and
prior to sample extraction. Recovery efficiencies for these compounds were used in
quantifying the actual PCDDs/PCDFs isomers measured in the samples.
Alternate Standards were spiked in the TLI laboratory after the field sampling program
and prior to sample extraction. Recovery of these compounds indicated the extraction
efficiencies.
Recovery Standards were added in the laboratory after extraction just prior to GC/MS
analysis.
6-7
-------
TABLE 6.5
SUMMARY OF EPA METHODS 23 AND 26A FIELD SAMPLING QA/QC DATA
Site
Kiln 4 Baghouse
Inlet
Kiln 4 Baghouse Outlet
Run No.
I-M23-4
I-M26A-4
I-M26A-5
I-M26A-6
O-M23-4
0-M26A-4
0-M26A-5
0-M26A-6
Pre-Test Leak Rate
(acfm)
0.001 @ 15" Hg
0.002 @ 15" Hg
0.001 @15"Hg
0.001 @17"Hg
0.003 @20"Hg
0.005 @ 15" Hg
0.005 @ 15" Hg
0.003 @ 15" Hg
Post-Test Leak
Rate (acfm)
0.0_@_"Hg
0.002 @ 17" Hg
0.0_@_"Hg
0.001 @ 16" Hg
0.004@ 12" Hg
0.003 @ 15" Hg
0.002 @ 05" Hg
0.002 @ 12" Hg
EPA
Criteria
(acfm)
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
Isokinetic
Sampling
Ratio
(%)
100.4
103.9
103.7
103.4
103.0
101.8
101.6
103.2
EPA Criteria
(%)
90-1 10%
90-110%
90-110%
90-110%
90-110%
90-110%
90-110%
90-110%
6-8
-------
Table 6.6 summarizes the recovery efficiencies for the various standards and the respective
quality control limits. The recovery efficiencies for the XAD* blank and samples were all within
the method QC limits. Refer to TLI's case narrative for their discussion of any quality control
anomalies.
One of the Method 23 sample handling requirements is to keep the samples under ice.
The field sample recovery technician during this effort, Michael D. Maret, personally packed the
XAD resin traps with ice packs and personally delivered the samples to TLI on April 1, 1998.
This statement is made in rebuttal to the TLI custodian lab report; TLI was informed of this
discrepancy but has not responded as of the time of the preparation of this final report.
6.3.2 EPA Method 26A Hydrogen Chloride. Ammonia, and Cations
Tables 6.7 and 6.8 summarize the QC results from the Method 26A laboratory analyses
performed by Research Triangle Institute. All QC results are within generally accepted criteria,
with the exception of the sodium (Na) duplicate results as shown in Table 6.8. However, because
of the low concentration of Na (less than twice the detection limit), it is considered to be within
the variability of the instrument.
The field blank results are presented in Table 6.9. Note that the Ca, Mg, and Na results
are of significant magnitude (> 50% of sample) in comparison to the sample catches. Refer to
Appendix B.2 for a comparison of the blank and sample catches. This could indicate that the
sample catches do not represent the amount of Ca, Mg, and Na native to the air stream.
6-9
-------
TABLE 6.6
SUMMARY OF EPA METHOD 23 STANDARDS RECOVERY EFFICIENCIES
FULL SCREEN ANALYSIS
Internal Standards
2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF
1,2,3,7,8-PeCDD
1,2,3,6,7,8-HxCDF
1,2,3,6,7,8-HxCDD
1,2,3,4,6,7,8-HpCDF
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
Surroeate Standards
2,3,7,8-TCDD
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,4,7,8-HxCDD
1,2,3,4,7,8,9-HpCDF
Alternate Standards
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDF
CONFIRMATION ANALYSIS
Internal Standards
2,3,7,8-TCDF
Percent Recovery
TLI
M23
Blank
65.8
67.9
68.6
99.4
68.1
78.7
83.7
92.5
83.0
87.9
106
108
114
90.1
84.5
81.8
69.2
M23-I-4
60.6
53.7
63.2
69.5
72.2
70.5
65.5
68.4
40.3
88.9
96.0
92.2
93.2
76.0
76.1
75.6
56.1
M23-O-4
79.7
64.1
70.7
68.3
80.5
95.3
74.4
87.2
93.8
91.8
89.7
93.4
83.8
104
87.0
86.1
75.5
RB1-4
66.0
59.9
62.5
76.1
81.6
97.6
82.8
101
115
83.8
101
82.5
82.5
95.2
87.7
89.1
*
QC Limits
40-130%
40-130%
40-130%
40-130%
40-130%
40-130%
25-130%
25-130%
25-130%
70-140%
70-140%
70-140%
70-140%
70-140%
40-130%
40-130%
40-130%
* Confinnation analysis was not necessary on these samples since no TCDF's were detected in the full screen analysis.
6-10
-------
TABLE 6.7
SUMMARY OF EPA METHOD 26A ANION SPIKES
AND DUPLICATE ANALYSIS
Sample ID
Recovery Efficiency. %
QA-MED
QA-LOW
QA-MED
EPA-3909 b
NH4 QA-1
NH4 QA-2
EPA-3177"
M26A-I-6-A SPIKE
M26A-O-6-A SPIKE
Duplicate Analysis c
M26A-O-2-A
M26A-O-2-A DUPLICATE
Percent Difference
M26A-O-1-A
M26A-O-1-A DUPLICATE
Percent Difference
0
99.0
99.0
100.0
103.4
naa
naa
naa
100.4
naa
0.043 mg/L
0.044 mg/L
2.3
naa
na'
naa
NH4
na'
naa
naa
naa
96.9
93.6
91.4
naa
96.6
naa
naa
naa
0.019 mg/L
0.018 mg/L
5.3
a na = not applicable
b Quality assurance samples prepared by the EPA.
c Duplicate analyses were performed by the laboratory on samples collected at
another lime kiln facility during the same mobilization.
6-11
-------
TABLE 6.8
SUMMARY OF EPA METHOD 26A CATION SPIKES AND
DUPLICATE ANALYSIS
Sample ID
Recovery Efficiency. %
M26A-O-2A SPIKE*
Duplicate Analysis
M26A-O-5-ADUP
M26A-O-5-A
Percent Difference
K+
85.0
<4.8ug
<4.8ug
0.0
Ca+
91.8
277 ug
291 ng
-4.8
Mg*
96.2
32.3 ,ig
33.1 ug
-2.4
Na+
96.4
40.4 ug
29.6 ug
36.5
L AT
104
15.1 ug
16.1 ug
-6.2
* The matrix spike was performed by the laboratory on a sample collected at another lime
kiln facility during the same mobilization.
TABLE 6.9
SUMMARY OF EPA METHOD 26A FIELD BLANK ANALYSIS
Analyte
ci-
NH;
K+
Ca+
Mg+
Na+
AT
M26A-FB-2-A Catch
0.41 mg
0.20 mg
<3.5ng
80.8 ng
10.2 \ig
27.0 ^g
-------
APPENDIX A
RAW FIELD DATA
-------
Appendix A. 1
Raw Field Data - Kiln No. 4 Baghouse Inlet
-------
Plant:
Date:
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
At-
Sampling Location: IMLET To
Inside of Far Wall to Outside of Nipple: 3.S" + B<\'
Inside of Near Wall to Outside of Nipple (Nipple Length): 3.5.
Stack I.D.: S4" _
Distance Downstream from Flow Disturbance (Distance B):
_ inches / Stack I.D. - _ dd
Distance Upstream from Fbw Disturbance (Distance A):
_ inches / Stack I.D. -
Calculated Bv: /?
dd
\
c
•••^••^••H
{
!
4
^
t*
4
1
Schematic of
Sampling Location
Traverse
Point
Number
/
2
3
4
S
^
7
/?
•&k~7
,nB
• /77
.25D
-354
,4W
,7£O
. 823
• 8AZ
.333
.y '^
^3^
^7 ^8
£,&.£
72 s/^
77 5^
*/.%
^5 ^
-------
GAS VELOCITY AND VOLUMETRIC FLOW RATE
/
Plant: r)R^vo - SA^I^A^J MU^T Date: 3-28 -ty
Sampling Lo
Run*1. /)fgi
Barometric F
Moisture, %:
Stack Dimen
Wet Bulb, °F
TravtrM
Point
Numb«r
1
-2.
3
y
£
4,
7
&
q
10
//
/2
cation: |ML£-T TO B^6,uou*>^: Clock Time: 4-'3<9
^7;*, an/ l/'e./osJ-fv Onerstors: /^/etid.
ressure, in. \
/
Ha: 3^.^ Static Pressure, in. I-UO: -3on ««.c>
Molecular wt . Drv: Pitot Tube. CD: 0 , 8 4
sion, in. Diameter or Sidi
': Dry!
Velocity
H*ad
h.H20
x £* *" ^^
^S t tP -^^
*^.
A / ^^
0.B5
D.8&
h.&£
D.Zto
D.&L
0.8B
t> .$1,
' A .62.
O.B1
£P-
Stack
T«mp.
°F
Mfi TFK>
^CCLKO^
3££
Vo£
¥3t>
y&6
471
V77
VA7
Vt,t>
¥t>f
T«- 44B
B1: *4" Side 2:
3ulb.°F:
Md - (O.MxSCOj) •(• (O.S2x%02) 4 (0.28x%Ny
Md - (0.44x /2- ) + (O.S2X f ) + (0.28 x 7? )
Md- J-*-2d
100 100
M* - 33. (*~7
Pi- ^7,2? ln.Hg
«P-
— I T»(°R)
V« - 85.48X Cpx ^P X y pJ7jj; —
Vi - 65,49 x{ }x{ )x\/ •• —
V.- tt/«
A.- ft2
Cte-VtxAsxBOi/m
Qs- x X60
Qs • ACfnn
ltd 100
c-
-r*
-------
FIELD DATA SHEET
Plant Z)/?AvQ
'j
Sampling Location /A
Run Number: T-jn?3-
Pretest Leak Bate: o
TT>
Date:
cfrn
Sample Type:
Pbar:
CO2:
3 Operator:
Ps: i
02.
-3o"
Y^-t.ezi
Nozzle ID: p.2 ±> Thermocouple
^Filter*:
> Y: .
Assumed Bws
Meter Box #:
<-£
in. Hg.
Pretest Leak Check: Pitot:
Orsat:
Probe LengtoVType: 5'£/*<>* Pilot #:
Stack Diameter: 1* *81" As:
Post-Test Leak Rate:^
231
19
J/o
. 56
D.&B
3-°Z
477
5t
IOZ
/J'.SI
733.02-
Sf
/3.S
2. a
2.17.
483
/co
7*6. Z>0
0,*4
2.3?
/0V
/J-25
JL&&
49A
2Z.&
/CO
/oz
'2*.
*>.&!>
234
<*/
/Ol
!&L
13:55
fl.BL
3,01
l.o/
VA>
l/fe- c>c.iry
->3/$
r.JM
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
Run
Date:
Sample Box No.:
Job No.: iBo/2 - Coz.
Sample Location:
ample Type:
/l
r/W
ample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
MoisturelDatal
Impinger
No.
Contents
165-4
Initial
Volume, ml
Initial
Weight, grams
Final
Net
XA0
{<*>
<\yu}{ *
Total
Comments:
-------
FIELD DATA SHEET
Plant
Sampling Location lv>t.er -TO
Run Number: £-2le,A--4 Date:
Pretest Leak Rate: 0.002. elm @ IS in. Hg.
Pretest Leak Check: Pitot: s Orsat: _
Sample Type:
Pbar:
CO2:
A Operator: P
Ps: r.
Probe Length/Type: 5'
Pilot #:
Stack Diameter: 7'- Bt1' As:
Nozzle ID: 0,211 Thermocouple #. *}-£__
Assumed Bws: £ Filter #:
Meter Box #: f>lft|D Y: J^£/^TAH@: /.
3f
(.0
OochTJm.
(244iour
dock)
/y.jo
SW
7&/.LO
7/7. 23
7&4. 4?
741. Zt>
its. 1,1
14 Z.^
361. i,rft
IIAA&
^i2.44l
7i&rsA/4 ASA
Velocity
HMd (Ap)
inHZO
Orifice Pressure Dffter«ntJal
(AH) in H2O
Desired
Actual
Stack
Temp.
(Ts)
Temperature
°F
Probe
Fitter
Impinger
Temp.
°F
Dry Gas Meter Temp.
Inlet
(Tmln0F)
Outlet
(Tmout°F)
Pump
Vacuum
On-Hg)
Y/////////////////////////////////////////////////. Y/////////.
0.8Z
t.&7
*.&3
0.W
0.9 AT
/.,$
/./IT
/.//
///
/.//
/.rt
/,//
/./3
2J>4
J1
LB
<*&
t>8
U
HI
<*-!
107
•>iAC.T.
/O/
77
/&>
??
W
18
-------
MULTI-METALS SAMPLE RECOVERY DATA
z;
Plant:
Run No.: MA?ol-JT-4.
Date:
Sample Box No.:
Job No.:
Sample Location:
Sample Type: US
Sample Recovery Person: 1/frUVH
Container Description
Volume, ml
Sealed/Level Marked
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
A/
[Co
r
Total
Comments:
-------
Plant: Zfowo -
FIELD DATA SHEET
Sample Type: r^xfaA. Operator: £
Y-
Sampling Location /MLe-r
Run Number: 3~-j&A • Date
TO
CO2:
02:
Nozzle ID: p.:
Assumed Bws:
Meter Box #:
Thermocouple
Filter #:
Pretest Leak Rate: *.<*>/ cfm @ /i5~ in. Hg.
Pretest Leak Check: Pitot: •" Great:
Probe Length/Type: .5 '
Stack Diameter: -7'
Pilot #:
As:
Y: j^&f€ AH@:
Post-Test Leak RateXg-*g cfm @
in. Hg.
Post-Test Leak Check: Pitot:
Orsat:
TravwM
PoJnl
NumlMf
O
Sivr^Mng
Tim*
(mln)
0
5
/o
f$
20
2.S
30
35
/<,:
/7.'os
/•?-'/o
J7.-/S
/7.-20
/?'2S
/7.'30
/7-'3S
Gu Meter
Rvadino
(Vm)ns
g\2.~1l4
815 .10
S(R.4f
B2\. W
&23A+
A7A.47
B32L .1 1
^4-.g/
*M.€L
W>.3I
543. l(
«<^5.^IZ
7f
A.8f
o&l
0.tt
0,8?>
0.&2.
*.B A
/.t>*f
/.0(*
/.0-7
/.£>8
S.OB
/,61
/.0?
/.04
;.o¥
/,<>£
/,e>-?
/.//
£ FblMT
4?7
W2-
461
447
^6
502-
¥
52
£3
53
£•*>
$<+
$5
-rf
ISoKtK
f3
^3
^V
H
16
11,
15
1*
It,
46
STXCCvl.
^
fV
f-/
7Y
ff
ff
f/
^3
f^
f^
^^
fV
L.y
7
£
4
A
8,S
f
7.5-
yo
/a.^
//
/^
/3
/V
T7S-
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant: \/ti>W u.*tf
Date: 5 (it fat
Sample Location:
Sample Type: I
/)
Sample Box No.:
RunNo.:VW2/cA-T-r
JobNo.:fr'2.-06L
D/te.ta/^ /MLL-r
& .fefA /fe^ 76 A-
Sample Recovery Person: j/Ui^K
Container
Description Volume, ml
1
2
3
Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
4
5A
5B
5C
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
Nitric Rinse - Impinger No. 4
KMNO4/H2O Rinse - Impingers 5 & 6
HCI Rinse - Impingers 5 & 6
tpsfsipp
MoisturerData
Impinger
No.
\
2
I
-------
FIELD DATA SHEET
Dl 1 T-x «— I/ \ <-L
riant: ^ftfwo ' bA^iiJflw Idt-rJ ~j Samp
Sampling Location )ML£T T° ^>A.«*V\o»A*>fe: Pbar:
Run Number:
le Type: /^^feA Ope
J^. S Ps: -3
rator: P.^/e&eL-
O " MiC>
X-2tA.-t, Date: 3-2-8 -^S CO2: j-i. O2: q
Pretest Leak Rate: 0,00/ cfm® /? in. Hg. Probe Length/Type: s ' 6k<& Pilot #: +£
Pretest Leak Check: Pitot: \/ Orsat: Stack Diameter: -
Traverw
Potit
Numbw
0
Sanding
TbM
(rein)
0
&
/A
/<
30
/
/$:&(,
/*>.//
/8-'/(>
S8'2/
/8-3t>
/&:•*/
/8'3t,
/£:
/1 '•£>/
7' = 6'flv As: 36.^
95-^-"^-
Gas Meter
Reading
(Vm)fl3
^y^.z^
844. n
85 (.13
38&'T$
&£D^/&
/} r *j f"3 jf"1
&t&£.f O^?
86^,1,?-
^5/3Z.
87/,t>&
873.17
07<9.fi2.^
TeiTftt&i t^A
Velocity
Head(Ap)
inHZO
Orifice Pressure Differential
(AH) in H20
Desired
Actual
Stack
Temp.
(Ts)
Nozzle ID: /». 2./ "7 Thermc
Assumed Bws: S Filter #
Meter Box #: MRIO Y: M*l
>couple #:
tfg-
rtTAHfS): l.O tf ^t
t^ * O ^
#.#y
0,82.
Ot%t-
&'£&
O/SS'
4,87
&tf
£>'&b
£ ^o^/ou(,
/' <3S"
/,//
/.&
/'/y
/ '/ &
fZ> X-7-^
/./$•"
/.e>&
/,07
/ 0%
/.o6
X,
A/^
/,/£>
/A/A,^.fc/
5^
5^/4
.573
.5/2
.-5X/
.IYJT
£?~/d.
^*/
<&*/3
of= 2X
4,7
G^
C=>7
,^5
6^
67
66
6?S
&£*
1L
97
B_T./<,A<_
Pump
Vacuum
(ki.Hg)
'/////
&.6>
8 6
£,S
/o
10. -5
II
sz
/3
/5"
/5^5
/^>
V-
f
AVm-
AH-
Ti-
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
Run No.: lO»?6/4-j
Date:
/£L_
Sample Box No.:
Job No.: ficrt -an-
Sample Location:
Sample Type: (X'
\W
entM
Sample Recovery Person:
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1.2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C IHCI Rinse - Impingers 5 & 6
i . sssssgfi!rue-^^^iiySSj
MoisturelDatas
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
774-0
34*1
Total
Comments:
-------
Appendix A.2
Raw Field Data - Kiln No. 4 Baghouse Outlet
_ _. i
*>5s&fc""*--*v' ****^«*i
&»3ca5r-gae M.- rr -*r2i»i|
tv^sssasG"
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
Plant:
Date:
Sampling Location: RA/J/ICI^L. Oj-RjJr" ~_ E * I
Inside of Far Wall to Outside of Nipple: 90 "
Inside of Near Wall to Outside of Nipple (Nipple Length):.6.
Stack I.D.: £3 ty
Distance Downstream from Fbw Disturbance (Distance B):
*•' ^1 inches / Stack I.D. « Z. 1 dd
Distance Upstream from Flow Disturbance (Distance A):
^•V f.H inches/StackI.D. - "7.V dd
Calculated By:
Schematic of
Sampling Location
Traverse
Point
Number
1
2
3
4
5
(*
1
^
9
)0
\\
I1~
Fraction
of
Length
O.ozi
0.^61
o. US
0 /77
a. 1-fo
&' 35 (*
^•^^
0. ~)<0
0 -%21
0 .%%?-
0^33
0.^
Length
(inches)
^ty
\
!
(
•^
Product of
Columns 2 & 3
(To nearest 1/8")
M
56
**$
11.1
&•$
^,c
53-6
&,^
6.^
1S^
^7 7
^
Nipple
Length
(inches)
^^/V
r
\
iX
Traverse Point
Location
(Sum of Col. 4 & 5)
«&
y^ %
/6 ^
2-A&.
^7^
36 ^
C6 ^
/,^^
TSfy
<i
W fe
^^/
-------
50
•g
« 40
-------
GAS VELOCITY ,CYCLONIC, AND VOLUMETRIC FLOW RATE
Plant:
!/<= A.
Sample Location:
Run No.:
Pbar, in. Hg:
Moist, %:
i. 5
5.
Stack Dimension, in. Dia. 1:
Wet Bulb, °F:
25
Date:
Clock Time:
Operators:
Static Pressure, in. H20: — ,3C?
Pitot Tube, Cp: ,%fj
Dia. 2:
Dry Bulb, °F:
Traverse
Point
Number
I
7
/
1>
H
*,
L,
-7
%
3
ID
>l
11
Velocity
Head. in.
H,O
•^
•°\L
^0
,«t/
•16
-01
•Ob
.13
.-82
.
-------
•
3*
FIELD DA IA SHEET
Plant: Dr&\J0 - &\«
Run Number: O -M
i<.«-\. Sample Type: /^
^nu42- Oi.--H.-A- - t'U'f
1 '^^~~
Date: *3-2g>-q&
Pbar:
CO2:
2^.S
7t~
i-23 Operator: 77) /wi
Ps: -. S(
O2 : V
Nozzle ID:
Pretest Leak Rate: . OO3 cfrn @ ;y? in. Hg.
Pretest Leak Check: PHot: S Orsat: —
Probe LengoVType: 7'
Slack Diameter: 33 Z5 As:
Pilot #:
Assumed Bws: .v
Meter Box 4
Post-Test Leak Rate: , o
r*
Thermocouple
Filter #:
ts- Y:
cfm @ ^ in. Hg.
Post-Test Leak Check: Pilot: ]/ Orsat:
Traverse
Point
Numb*
J_
^1
/o
Sampling
Tkn*
(irin)
90
120
/TO
aockTim*
(244io
dock)
V.U,
Gaa Meter
Reading
(Vm)«3
Velocity
Head (Ap)
inH20
OriSce Preasure Differmtial
(AH) In H2O
Desired
Actual
Stack
Temp.
Temperature
°F
Probe
RtM
Impinger
Temp.
Op
Dry Gas Meter Temp.
Inlet
(Tmln0F)
Oullet
(Tm out°F)
Pump
Vacuum
On. Hg)
.55
-9
,13
Kb
•vA
2,0
2.0
\-5
ffc
TL> 0
2.0
HI
T-S8-
T-JO
95
-TV
3" v
'M-
10
rf.
6?
11
AVm=
AH
Ti=
2.
3-
2.
J3L
_Z
7
so
-Ti
•ft-
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
T
Run No.:
Date: 3/7S/4&
Sample Box No.:
Job No.: flo\i-
Sample Location:
Sample Type:
tffl
"23
Sample Recovery Person: iA/0/1
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMN04/H20 Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
- Wufek*
Initial
Volume, ml
Initial
Weight, grams
Final
Net
£.0
c
(.6
4
Total
Comments:
-------
FIELD DATA SHEET
r /
Plant:
"jHx^O - ^WNx--~ Sample Type: h- ^,A Operator: T4/^A
Sampling Location fivfe^ C>J{\j\ - fa -> 4 Pbar: 2f
Pretest Leak Rate: , oC>5" cfm @ /5" in
Pretest Leak Check: Pitot: jx- Orsat: —
Traverse
Point
Number
£>
/
Z
2>
^
5
u
7
5
*
<0
i<
a
Sampling
Time
(min)
O
5"
/o
/5
2-5
30
HO
$o
eg,
(eO
(24-hour
dock)
W32
HZ!
lLl^^
iWl
\L\tft
$S~\
I&&Z-
i£>7
Wt,
x,n
tfy-i.
\§V^
\fa^
Hg. Probe Length/Type. -) ' <^/b#$ Pftot #
~>D
Stack Diameter: <23. ?5 As:
•
Gas Meter
Reading
IslQ.WO
^5. 1
C.16,0
fl/^36»
0^/5.^
6^1.^
o53.3
^^.c,
u^0t ^
(J«^J>
LU.5
.-ML.5
Velocity
Head (Ap)
inH2O
//////////
, Thermo
Assumed Bws: ,o5 Filter*
Meter Box »:/^8^ Y: ^£
Post-Test Leak Rate: .o&5
Post-Test Leak Check: Pitot:
Temperature
°F
Probe
Fitter
Impinger
Temp.
°F
couple #:
: A/4 -
1J>
^V53
35/
352-
Otfx
^^^
3if3
3^5
25/
25-0
•3SO
fj
"^=0
2^ro
-L#>
Z5/
'o
2&
2$l
152,
^•7
5-7
vS"-T
^*1
5&
11
?/
q-j
**£.
*1Z.
*} 2
/O
/O
X?
;<>>
/&
1
#
IA
10
lO
$
T5-
Tm=
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
/(Lfnfo
Run No.:
Date:
Sample Box No.:
Job No.: Hot I - 6PZ^
Sample Location:
(\'Cr
u*r
Sample Type: U&
"26$
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMN04/H20 Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
)ingers 5 &6
"•.-•" : :• '.^ rfSs., y^; •'-v--.--.''.^ -^T^.;-.-. ^.~-CyK^j'''ci»-v.?'--:''§^v'.':Iy'-?.-V^'- . -'.s^y^Stfes^f^sfa^l;
initial Weight, grams
Impinger
No.
Contents
Initial
Volume, ml
Initial
Final
Net
6. I
0.\
S"
G4SZ
Total
Comments:
-------
FIELD DATA SHEET
Plant: pA/-. »o -
Sampling Location feWnya
Run Number: Q-l&A-S Date:
Pretest Leak Rate: fo05 cfm @ _/5
Pretest Leak Check: Pftot: ./ Orsat:
Sample Type: j^
Pbar: a^. 5"
CO2: />-'
Ps.
O2:
in. Hg.
Probe Length/Type:
Stack Diameter: r
Operator: T^/g^
- .fl
Pftot #: 10
As:
v~
Nozzle ID: . 2S6 Thermocouple
Assumed Bws: .,?5 Filter #: 7e<;»^
Y:
Meter Box #:,
Post-Test Leak Rate: ,2. c^" @ S in. Hg.
Post-Test Leak Check: Pftot: >/ Orsat: —
Traverse
Point
Number
O
/
z
3
4
5
6
7
f?
?
>0
n
il-
SampHng
Tim*
(mtn)
0
S
10
/5
2O
25
3£>
35
^
45
50
55
<^>
QockTime
(24-hour
dock)
JIA9)
n.K's
\\>^
IG53
Iflo3
n?>
nw
Gas Meter
Reading
(Vm)ft3
Gil.. 3^0
|,«0 ,0
u\\.%
(rf^.O
^7.. 8
IJXL,.^
nW)'\
-T63-5
icn.i
TI.Z.
i5C?
^e-o
34<}
050
350
?^>
35-0
2 So
7£O
1^
2^t
t.U'V
•J,*\U
14 ^
2^
ASOI
ioz.
/o?
73
1T~
\0
9o
9/
U
^3
^^
73
93
f*
^^
3
3
•2>
3
1
i.
2.
1.
^
3
3
J
-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
Date: 5
JLbw t^
M°(£ r\
Sample Box No.:
Run No.: {/V76^ ' O^
Job No.: |2o/ ? - OoZ,
Sample Location: U$6/feH<$£ O^TL-c/*"
Sample Type: US trfW I^o7(u? 264-
Sample Recovery Person: (/Yl$tH
Container Description Volume, ml
Sealed/Level Marked
1
2
3
Filter No.(s)
Acetone Rinse
Nitric Rinse
4
5A
5B
5C
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
Nitric Rinse - Impinger No. 4
KMN04/H20 Rinse - Impingers 5 & 6
HCI Rinse -
Impinger
No.
\
I
1
A
r
Total
Impingers 5 & 6
Contents
&. 1 l-lz-^4-
O'l ik&A
O.I MA
6 I Ajc-
^ GL
D/
Oil
Initial
Volume, ml
m>
\CU
(u?
/^
-
Weight, grams
Initial
W4
^^.r
6>'^^
^gj
6/fl.l
•^6^^
^£
Net
Comments:
-------
FIELD DATA SHEET
Plant:
TVAVD- ANu^^o- Sample Type: i/*- ?6fl Operator: TA/^ 4
— „.,. _, _.
Sampling Low
Run Number:
ition S^K*^ (VMjV - ^^ Pbar: If.^ Ps: - •
1
n
Q
^
ID
,\
KU
Sampling
Time
(min)
ft
J0
/£
20
15
"JjD
35
^0
*fe
50
r^
L»tf
Clock Time
dock)
lft)l
Ifol
/^/2^
^ il
»S^i.
/&Zl
/S32_
/*^7
/^^2.
)$*i~J
its*.
Ifrg-j
ftfiT-
Hg. Probe Length/Type: -/'Gfc/y Pftot #: 7D
— Stack Diameter: 7325 As:
Gas Meter
Reading
(Vm)ft3
"112. 1 1O
7Z1.0
Ill.O
735T2.
~7S9-2-
")-v3.O
"7^!«. °i
7 50.. i.
^^, 2-
1^ -2-
"/^/ 'T
-7^3. 7 °*V
Velocity
Head(Ap)
inH2O
Orifice Pressure Differential
(AH) in H2O
Desired
Actual
Stack
Temp.
(Ts)
Nozzle ID: , 2523 Thermocouple #: ID
Assumed Bws: i0j- Filter #:
Meter Box #: ^a /^ Y: . rT£
Tcft/,
- ^H@: /?7
Post-Test Leak Rate: fOf> ? cfm @tZ~
Post-Test Leak Check: Pftot: \f Orsa
Temperature
°F
Probe
Biter
Impinger
Temp.
°F
Dry Gas Meier Temp.
Inlet
{Tmln0F)
Outlet
(TmoutPF)
in. Hg.
t: —
Pump
Vacuum
(ln.Hg)
^////////y /////////
°IC)
(7o
•«5
,-15
•C»8
/l*«
,55
,60
,75
-7.5
/72
•7Z
2.6
2.5"
2.-Y
/. i
1,1
/-1
/• 5
LI
2^\
2-J
t.o
2.5
?.JT
2.^7
?v\
'•^
/. ^
/. -5
/7
2v!
•2,1
^v5fe
35©
359
t35"^
3^J
1J&E.
<**&•>•
x3^z_
^^V
7 ^r
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-------
MULTI-METALS SAMPLE RECOVERY DATA
Plant:
Run No.:
Date:
Sample Box No.:
Sample Location:
Sample Type:
fclfl*
26
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
1
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H20 Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
tvl
vl XI /4,
-------
MULTI-METALS SAMPLE RECOVERY DATA
lant:
Run No.:|1rt?6/l -
Date:
Sample Box No.:
Job No.: fat -
Sample Location:
\
O
UTLET-
Sample Type: IK
1M&-
Sample Recovery Person:
Container Description
Volume, ml Sealed/Level Marked
Filter No.(s)
Acetone Rinse
Nitric Rinse
Nitric Rinse - Imp. 1 ,2,3, + Back 1/2 Filter
5A
Nitric Rinse - Impinger No. 4
5B
KMNO4/H2O Rinse - Impingers 5 & 6
5C
HCI Rinse - Impingers 5 & 6
Impinger
No.
Contents
Initial
Volume, ml
Initial
Weight, grams
Final
Net
0.\ Kl
"t
0. 1 Kf
O.I
-i M
Total
Comments:
-------
Table A-2
HCi Emission Measurementsa Ume Kiln
Dravo Ume Company
Saglnaw, Alabama
3/28/98
Time
Date
Kiln No. 4
10:40-10:55
10:55-11:10
11:10-1125
1125-11:40
11:40-11:55
11:55-12:10
12:10-1225
1225-12:40
12:40-12:55
12:55-13:10
13:10-1325
1325-13:40
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
Inlet/Outlet
HCI
ppmW
«*S
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Average
Kiln No. 4
1725-17:40
17:40-17:55
17:55-18:10
18:10-1825
1825-18:40
18:55-19:10
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
3/28/98
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Average
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
7.8
6.8
6.9
7.3
6.9
6.6
7.1
THC
pprnW
<**T
7.0
6.8
6.6
6.9
6.6
6.5
6.4
6.2
5.9
5.8
5.6
5.7
6.3
O2
%
CO2
%
w
10.8
10.6
10.6
10.6
10.5
10.6
10.6
10.5
10.5
10.5
10.5
10.5
10.6
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
n/a
19.6
19.8
19.2
18.9
19.0
18.9
19.1
19.4
19.2
19.1
19.0
19.0
19.2
n/a
n/a
n/a
n/a
n/a
n/a
-------
-------
APPENDIX B
LABORATORY ANALYTICAL DATA
-------
Appendix B.I
Method 23 Analytical Report
-------
CASE NARRATIVE
Analysis of Samples for the Presence of
Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans by
High-Resolution Chromatography / High-Resolution Mass Spectrometry
Method 23 (6/93)
Date:
Client ID:
P.O. Number:
TLI Project Number:
April 21,1998
Pacific Environmental Services
104-98-0159
45399
This report should only be reproduced in full. Any partial reproduction of this report requires permission from
Triangle Laboratories, Inc.
Rev. 11/19/97
Triangle Laboratories, Inc.
801 Capitola Drive P.O. Box 13485
Durham, NC 27713-4411 Research Triangle Park, NC 27709-3485
919-544-5729 Fax* 919-544-5491
oca
-------
Triangle Laboratories, Inc. April 21,1998
Case Narrative 45399
Overview
The sample(s) and associated QC samples were extracted and analyzed according to
procedures described in Method 23 (6/93). Any particular difficulties encountered during
the sample handling by Triangle Laboratories will be discussed in the QC Remarks section
below. This report contains results only from the Method 23 dioxin/furan analyses of the
M23 sample(s).
Quality Control Samples
A laboratory method blank, identified as the TLI M23 Blank, was prepared along with the
samples.
Quality Control Remarks
This release of this particular set of Pacific Environmental Services analytical data by
Triangle Laboratories was authorized by the Quality Control Chemist who has reviewed
each sample data package following a series of inspections/reviews. When applicable,
general deviations from acceptable QC requirements are identified below and comments
are made on the effect of these deviations upon the validity and reliability of the results.
Specific QC issues associated with this particular project are:
Sample receipt: Twelve M23 sample(s) were received from Pacific Environmental
Services in good condition on April 01, 1998 at ambient temperature and stored in a
refrigerator at 4 °C. On the sample labeled M23-0-1-2, acetone was marked through and
toluene was written above it. On the sample labeled M23-0-1-3, toluene was marked
through and acetone was written above it. Neither of these labels agreed with the clients'
chain of custody.
Sample Preparation Laboratory: None
Mass Spectrometry: None
Data Review: Sample M23-O-1 indicated low internal standard recoveries. However, the
signal-to-noise ratio is above ten-to-one in all cases and all standards are valid for
quantitation. TCDF was the only analyte detected in this sample and is below Target
Detection Limit (TDL).
-------
Triangle Laboratories, Inc. April 21,1998
Case Narrative 45399
Other Comments: No 2,3,7,8-substituted target analytes were detected in the TLI Blank
above the target detection limit (TDL).
The analytical data presented in this report are consistent with the guidelines of EPA
Method 23 (6/93). Any exceptions have been discussed in the QC Remarks section of
this case narrative with emphasis on their effect on the data. Should Pacific
Environmental Services have any questions or comments regarding this data package,
please feel free to contact our Project Scientist, Rose West, at 919/544-5729 ext. 270.
For Triangle Laboratories, Inc.,
Released by
Girgis Mikhael
Report Preparation Chemist
The total number of pages in the data package is
-------
TRIANGLE LABORATORIES, INC.
LIST OF CERTIFICATIONS AND ACCREDITATIONS
ENVIRONMENTAL
American Association for Laboratory Accreditation. Accredidation pending. Certificate
Number 0226-01. Accreditation for technical competence in Environmental Testing.(Including
Waste Water, Sol/Haz Waste- Pulp/Paper, and Air Matrices) Parameters are AOX/TOX. and
Dioxin/Furan. Method 1613 for Drinking Water.
State of Alabama, Department of Environmental Management Expires December 31. 1SS8.
Laboratory I.D. # 40950. Dioxin in drinking water.
State of Alaska, Department of Environmental Conservation. Expires December 21. 19S8.
Certificate number OS-00397. Dioxin in drinking water.
State of Arizona, Department of Health Services. Expires May 26. 1998. Certificate 3AZ0423.
Drinking Water for Dioxin, Dioxin in WW and S/H Waste.
State of Arkansas, Department of Pollution Control and Ecology. Expires February 18, 1999.
Pulp/paper, soil, water, and Hazardous Waste for Dioxin/Furan; AOX/TOX, Volatiles, Semi-
volatiles, and Metals.
State of California, Department of Health Services. Expires August 31, 1999. Certificate
#1922. Selected Metals in Waste Water, Volatiies, Semi-volatiles, and Dioxin/furan in WW and
Sol/Haz Waste. Dioxin in drinking water.
State of Connecticut, Department of Health Services. Expires September 30, 1999.
Registration #PH-0117. Dioxin in drinking water. . . •
Delaware Health and Social Services. Expires December 31,1998. Certificate #NC 140. Dioxin
in drinking water.
Florida Department of Health and Rehabilitative Services. Expires June 30, 1998. Dioxin in
DW. Drinking Water ID HRS# 87424. Metals, Extractable Organics (GC/MS), PesticSdes/PCB's
(GC) and Volatiles (GC/MS) in Environmental Samples. Environmental water ID HRS# E87411.
fUviMd 3019* RM
y.certificNcertlistmem
-------
Hawaii Department of Health. Expires March 1, 1999. Dioxin in drinking water. "Accepted"
status for regulatory purposes.
Idaho Department of Health and Welfare. Expires December 31, 1998. Dioxin in drinking
water.
State of Kansas, Department of Health and Environment Expires January 31, 1999.
Environmental Analyses/Non portable Water and Solid and Hazardous Waste. Method 1613 for
drinking water. ID #"s - Drinking water and/or pollution control - E-215. Solid or Hazardous Waste -
E-1209.
Commonwealth of Kentucky, Department for Environmental Protection. Expires
December 31,1998. ID#90060: Dioxin in drinking water.
Maryland Department of Health and Mental Hygiene. Expires September 30, 1998.
Certification #235. Drinking water by Method 1613A.
State of Michigan, Department of Public Health. Expires June 3, 1998. Drinking water by
Method 1613.
Mississippi State Department of Health. No expiration date. Dioxin in drinking water.
Montana Department of Health and Environmental Services. Expires December 31, 1998.
Dioxin in drinking water.
State of New Jersey, Department of Environmental Protection and Energy. Expires June 30,
1998. ID #67851. BNAs and Volatiles. Dioxin in drinking water.
State of New Mexico, Environment Department Recertification pending. Dioxin in drinking
water.
New York State Department of Health. Expires April 1, 1998. ID #11026. Environmental
Analyses of non-potable Water, Solid and Hazardous Waste. Method 1613 in DW.
• •
State of North Carolina, Department of Environment Health and Natural Resources Expires
August 31,1999. Certificate # 37751. Djpxin in drinking water.
State of North Carolina, Department of Environment Health, and Natural Resources,
Division of Environmental Management Expires December 31, 2000. Certificate # 485.
Metals, pesticides & PCBs, semi-volatiles and volatiles; TCLP.
North Dakota State Department of Health and Consolidated Laboratories. Expires
December 31,1998. Certificate # R-076. Effective October 4,1993. Dioxin in drinking water.
Revised 3/2/98 RM
yrcertificNcertlistmem
-------
State of West Virginia, Department of Health. Expires December 31, 1998. Certificate No.
9923(C). Dioxin in drinking water.
State of Wisconsin, Department of Natural Resources. Expires August 31,1998. Laboratory
ID Number 999869530. Certification for the following categories of Organics: Purgeable,
Base/Neutral, Acid, PCBs, and Dioxin. Expires November 14, 1999. Laboratory ID 999869530.
Dioxin in drinking water.
PHARMACEUTICAL
Drug Enforcement Agency (DEA). Expires November 30, 1998. Registration number
RT01195835. Controlled substance registration for schedules 1,2,3,3N,4,5.
N.C. Department of Human Resources. Expires October 31,1998. Registration number
NC-PT 0000 0031. North Carolina controlled substances registration. Application submitted for
renewal.
Food & Drug Administration (FDA) Registration. Expires June 1998. ID #s 001500 1053481.
Annual registration of drug establishment. Annual registration of drug establishment.
OTHER
Clinical Laboratory Improvement Amendments (CLIA) Registration. Expires May 30, 1999.
ID # 34D0705123. Department of Health & Human Services, Health Care Rnancing
Administration.
U.S. EPA Large Quantity Hazardous Waste Generator. No expiration date. EPA ID
#NCD982156879. Permit indicates that the laboratory is a large generator of hazardous waste.
North Carolina General License for Radiation Protection. No. expiration date. License No.
032-875-OG. The general license applies only to radioactive material contained in devices which
have been manufactured and labeled in accordance with specific requirements.
ftevtod 3/2/98 RM
y:certific\certlistmem
-------
DOCUMENT
CONTROL
Trfangto Laooratorits, Inc.
801 Capitol* Drtv* P.O. Box 13485
Durham. NC 277134411 R*~rcii Trtangb Pvk, HC 27709-3485
919-S44-S729 F*X * 919-544-5491
-------
[/PACIFIC ENVIRONMENTAL SERVICES. INC.
CQMPXf «
Central Park West
5001 South Miami Boulevard, P,O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
Chain of Custody Record
>Jed Mum IProject Name
1012.002 1 US EPA Lime Kiln Screening - Alabama Lime
mpnrv:
Abematny. Gay. Maret. Phoenix, Slegal
Date
3/23/98
3/23/98
3/23/98
3/23/98
3/24/98
3/24/98
3/24/98
3/24/98
3/26/98
3/26/98
3/26/98
3/26/98
3/28/98
3/28/98
3/28/98
3/28/98
•V23/98
3/23/98
3/23/98
Time
Field Sample IO
M23-M-1
M23-I-1-2
M23-I-1-3
M23-I-1-4
M23-I-2-1
M23-I-2-2
M23-I-2-3
M23-I-2-4
M23-I-3-1
M23-I-3-2
M23-I-3-3
M23-I-3-4
M23-I-4-1
M23-I-4-2
M23-I-4-3
M23-I-4-4
M23-O-M
M23-O-1-2
M23-O-1-3
Sample Description
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Analysis Requested
,V>
«&
•*»
^0
*
•
•
•
•
•
•
•
•
•
*
•
•
•
•
•
*
«
•
JJ\
u,
c*
sj
cw
•
•
•
•
•
•
•
*
•
•
•
•
•
•
•
•
•
*
•
Remarks
4/1/98
Pagel of 3 Pages
-------
oz>
SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
Chain of Custody Record
r012.002
US EPA Lime Kiln Screening - Alabama Lime
wnpwfK
Abemathy, Gay, Maret, Phoenix. Sfegal
Date
3/23/98
3/24/98
3/24/98
3/24/98
3/24/98
3/26/98
3/26/98
3/26/98
3/26/98
3/28/98
3/28/98
3/28/98
3/28/98
3/23/98
3/23/98
3/23/98
3/23/98
3/24/98
3/24/98
Time
Field Sample ID
M23-O-1-4
M23-O-2-1
M23-O-2-2
M23-0-2-3
M23-O-2-4
M23-O-3-1
M23-O-3-2
M23-O-3-3
M23-O-3-4
M23-O-4-1
M23-O-4-2
M23-O-4-3
M23-O-4-4
M23-FB-1-1
M23-FB-1-2
M23-FB-1-3
M23-FB-1-4
M23-FB-2-1
M23-FB-2-2
Sample Description
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Analysis Requested
_VN
§
«_l
PV-
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
V/N
£
0
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
Remarks
i
FIELD BLANK 1
FIELD BLANK 1
FIELD BLANK 1
FIELD BLANK 1
FIELD BLANK 2
FIELD BLANK 2
4/1/98
Page 2 of 3 Pages
-------
u
PACIFIC ENVIRONMENTAL SERVICES. INC.
Centraf Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Chain of Custody Record
oJedNom [Project Name
1012.002 I US EPA Lime Kiln Screening - Alabama Lime
mptora:
Abemathy, Gay, Marat, Phoenix, Stegal
Date
3/24/98
3/24/98
3/26/98
3/26/98
3/26/98
3/26/98
3/27/98
3/27/98
3/27/98
3/27/98
Time
Field Sample ID
M23-FB-2-3
M23-FB-2-4
M23-FB-3-1
M23-FB-3-2
M23-FB-3-3
M23-FB-3-4
M23-RB-1
M23-RB-2
M23-RB-3
M23-RB-4
elinquished by: (Signature)
_ . _ fl
•flnqujaiMfftby: (Stfnature)
Dale/Time
Dale/Time
'%K
Sample Description
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Container No. 1 - Filter
Container No. 2 - Train Acetone Rinse
Container No. 3 - Train Toluene Rinse
Container No. 4 - XAD Sorbent Resin
Received by: (Signature)
Recely^d-forlalfEyj (Signature)
^!fl\/ J
£^2w^S ^p*^
Analysis Requested
Vx
§
•O
o~
*
•
•
•
•
•
•
•
•
»
J^
Tt
O
Q*>
•
•
•
•
•
•
•
*
*
•
Relinquished by: (Signature)
Date/Time
Remarks
FIELD BLANK 2
FIELD BLANK 2
FIELD BLANK 3
FIELD BLANK 3
FIELD BLANK 3
FIELD BLANK 3
REAGENT BLANK
REAGENT BLANK
REAGENT BLANK
REAGENT BLANK
Received by: (Signature)
REMARKS
4/1/98
Page 3 of 3 Pages
-------
Custody Seal : Absent Sample Seals: Absent
Chain of Custody : Present Container...: Intact
Sample Tag* i Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SMO Forms : N/A
IORATORIES, INC. -- LOG IN RECORD/CHAIN OF
TLI
Cli
Project Number 4S399 Book
ent: PES03 - Pacific Environmental Services '
204
Date Received j 04/01/98 j &fli£-^ ^stf^**"^ P*9*
Ice Chest/Box NO COOLANT Carrier and Number j ^ 92
|TLI Number Client Sample ID Matrix) To L
|mR/HiCPM Client COC ID * Location | Date
J204-92-1A M23-I-1-1 FILTER) j)/J
| M23-I-1-1 C02 j Ji
\ . J......7
|204-92-lB M23-I-1-2 ACETONE RINSE)
| M23-I-1-2 C02 j
|204-92-lC M23-I-1-3 TOLUENE RINSE)
| M23-I-1-3 C02 j
J204-92-1D M23-I-1-4 XAD|
| M23-I-1-4 C02 j
|204-92-2A M23-I-2-1 FILTER)
| M23-I-2-1 C02 j
|204-92-2B M23-I-2-2 ACETONE RINSE)
| M23-I-2-2 C02 j
|204-92-2C M23-I-2-3 TOLUENE RINSE)
| M23-I-2-3 C02 j
i : 1 —
(204-92-2D M23-I-2-4 XAD)
| M23-I-2-4 C02 j
|204-92-3A M23-I-3-1 FILTER)
| M23-I-3-1 C02 j
|204-92-3B M23-I-3-2 ACETONE RINSE)
| M23-I-3-2 C02 j
|204-92-3C M23-I-3-3 TOLUENE RINSE)
| M23-I-3-3 C02 j
|204-92-3D M23-I-3-4 XADJ
| M23-I-3-4 C02 j
|204-92-4A M23-I-4-1 FILTER)
| M23-I-4-1 C02 j
| j i
AS
/Init
^
1
1
|204-92-4B M23-I-4-2 ACETONE RINSE) UrfV,
| M23-I-4-2 C02 j [\t\\1
To STORAGE
Date/Init
U*
J
....
1
;
[
| To LAB
Date/Init
, ,,
To STORAGE
Date/Init
| To LAB
Date/Init
-
To STORAGE
Date/Init
j
1 1
| To LAB
Date/Init
1 1
To STORAGE
Date/Init
| DISPOSED
Date/Init
•
1 1
— ! 1
1 1
1 1
1
1
| Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE WAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE WAS
| ' MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AGGREED WITH CLIENT'S COC
1
| Archive Remarks: .1
-------
"TRIANGLE LABORATORIES, INC. -- IAKJ in Kc.\.unu/,.,,„*
Custody Seal i Absent Sample Seals: Absent
Chain of Custody : Present Container...: Intact
Sample Tag* : Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SMO Forms • N/A
Ice Cheat/Box NO COOLANT
M
|TLI Number Client Sample ID Matrix) To I
|mR/H:CPM. Client COC ID • Location | Dat«
M
s/Init
|204-92-4C M23-I-4-3 TOLUENE RINSE) ¥,////
| M23-I-4-3 C02 | >* W/ty
|204-92-4D M23-I-4-4 XAD|
| M23-I-4-4 C02 j
|204-92-5A M23-0-1-1 FILTER)
| M23-0-I-1 C02 j
II
1
|204-92-5B M23-0-1-2 TOLUENE RINSE)
| M23-O-1-2 C02 |
§|
1
|204-92-5C M23-0-1-3 ACETONE RINSE)
| M23-0-I-3 C02 j
I j
|204-92-5D M23-0-1-4 XAD)
| M23-0-1-4 C02 j
|204-92-£A M23-0-2-1 FILTER)
| M23-0-2-1 C02 j
I)
1
|204-92-CB M23-O-2-2 ACETONE RINSE)
| M23-O-2-2 C02 j
• |
1 1
|204-92-CC M23-O-2-3 TOLUENE RINSE)
| M23-0-2-3 C02 j
1 1
'1 1
|204-92-6D M23-0-2-4 XAD)
| M23-0-2-4 C02 j
»|
1
|204-92-7A M23-O-3-1 FILTER)
| M23-0-3-1 C02 I
(j
1
|204-92-7B M23-0-3-2 ACETONE RINSE)
| M23-0-3-2 C02 j
It
_ . . |
|204-92-7C M23-0-3-3 TOLUENE RINSE)
| M23-0-3-3 C02 j J
»i 1
1 . J,
|204-92-7D M23-0-3-4 XAD) I/V VI ,
| M23-0-3-4 C02 j ^* 7/T/'0»
TLI Project Number 45399 BOOK
Client: PES03 - Pacific Environmental Services ' •
204
Date Received 04/01/9B BvJtf^ S j£*-~~ — T P«9«
! ! x>%t^*> ~-*5i-™^
Carrier and Number j 92
To STORAGE
Date/Init
*J
1
1
1
l>
| Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH
| • MARKED THROUGH HITH ACETONE WRITTEN ABOVE FOR SAMPLE
1
| Archive Remarks:
VI
(U,
1
| To IAB
Date/Init
-
To STORAGE
Date/Init
| To LAB
Date/Init
To STORAGE
Date/Init
| To LAB
Date/Init
To STORAGE
Date/Init
_ . .
| DISPOSED
Date/Init
• •
•
AND TOLUENE WRITTEN ABOVE IT; TOLUENE HAS
M23-O-1-3; NEITHER AGGREED HITH CLIENT'S COC.
•Form Revised 05/27/1997 -- Page 2 OF 4>
-------
"TRIANGLE IJVnORATORIPS. INC. -- UX5 IN RECORD/CHAIN OF CUSTODY^
Custody Seal i Absent Sample Seals: Absent
Chain of Custody i Present Container...: Intact
Sample Tags : Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SHO Forms : N/A
TLI Project Number 45399 | Book
Client: PES03 - Pacific Environmental Services ' 'j
. | 204
Date Received , 04/01/98 j By^ ^ oS^^\ •*•
Ice Chest /Box NO COOLANT Carrier and Number j j 92
|TLI Number Client Sample ID Matrix) To I
|nR/H:CPM Client COC ID • Location . | Dati
J204-92-8A M23-0-4-1 FILTER) I/I
| M23-0-4-1 C02 j ^
|204-92-8B M23-O-4-2 ACETONE RINSE)
| M23-0-4-2 C02 j
1 |
|204-92-8C M23-O-4-3 TOLUENE RINSE)
| H23-0-4-3 C02 j
| j
|204-92-8D M23-O-4-4 XAD)
| H23-0-4-4 C02 j
1 1
|204-92-9A M23-FB-I-1 FILTER)
| M23-FB-1-1 C02 j
1 I
|204-92-9B M23-FB-1-2 ACETONE RINSE)
| M23-FB-1-2 C02 j
1 1
|204-92-9C M23-FB-1-3 TOLUENE RINSE)
| • M23-FB-1-3 C02 |
|204-92-9D M23-FB-1-4 XAD|
| M23-FB-1-4 C02 j
|204-92-10A M23-FB-2-1 FILTER)
| M23-FB-2-1 C02 j
I
>l 1
|204-92-10B M23-FB-2-2 ACETONE RINSE)
| M23-FB-2-2 C02 j
II
i
|204-92-10C M23-FB-2-3 TOLUENE RINSE)
| M23-FB-2-3 C02 j
Ij
1
(204-92-10D M23-FB-2-4 XAD|
jj M23-FB-2-4 C02 j
»|
i
(204-92-11A M23-FB-3-1 FILTER)
| M23-FB-3-1 C02 j
1 1
JtB
s/Init
A/i'
(204-92-11B M23-FB-3-2 ACETONE RISE) \l J\ 1
| M23-FB-3-2 C02 | V I/1/'? f\
To STORAGE
Date/Init
I//464
)
r
1
/
/
1
\
\
|
j
| To LAB
Date/Init
-
To STORAGE
Date/Init
To LAB
Date/Init
To STORAGE
Date/Init
•
| TO LAB
Date/Init
•
To STORAGE
Date/Init
1 1
| DISPOSED
Date/Init
•
t
| Receiving Remarks: ON SAMPLE LABEL:M23-O-l-2, ACETONE HAS MARKED THROUGH AND TOLUENE WRITTEN ABOVE IT; TOLUENE WAS
| MARKED THROUGH WITH ACETONE WRITTEN ABOVE FOR SAMPLE M23-O-1-3; NEITHER AOGREED HITH CLIENT'S COC.
1
| Archive Remarks:
=Forro Revised 05/27/199-7 -- Page 3 OF 4
-------
=TRIANGLE LABORATORIES, INC. -- LOG IK RECORD/CHAin ur wuo
Custody Seal i Absent Sample Seals: Absent
Chain of Custody i Present Container...: Intact
Sample Tags : Absent
Sample Tag Numbers: Not Listed on Chain of Custody
SMO Forms : N/A
TLI Project Number 4S399 | oom ,
Client: PES03 - Pacific Environmental Services ' j
j 204
1 |
Date Received 04/01/98 By fit- S S^W
i i ./ Ot/V JCTC4
i -...- — ....
Ice Chest/Box NO COOLANT Carrier and Number |
TLI Number Client Sample ID Matrix
•R/H.-CPM. Client COC ID • Location
204 -93 -11C M23-FB-3-3 TOLUENE RINSE
M23-FB-3-3 C02
204-92-110 M23-FB-3-4 XAD
M23-FB-3-4 C02
204-92-12A M23-RB-1 FILTER
M23-RB-1 C02
204-92-12B M23-RB-2 ACETONE RINSE
M23-RB-2 C02
204-92-12C M23-RB-3 TOLUENE RINSE
M23-RB-3 C02
204-92-120 M23-RB-4 XAD
H23-RB-4 C02
I To LAB
Date/lnit
^
AM,
-
.
To STORAGE
Date/lnit
^
i
-------
TRIANGLE LABORATORIES, INC.
SAMPLE TRACKING AND PROJECT MANAGEMENT FORM
ADMINISTRATIVE INFORMATION
TLI Proj#: 45399- Samples: 12 TurnAround.: 21 Day(s)
Prod Code: D23451 Matrix.: M23 Hold Time..: 30 Day(s)
DetectLim: 0.05 ng Type...: A Start Date.: 04/02/98
Recvd..: 04/01/98 Ship By : 04/21/98
DWL Due Dt.: 04/09/98
Analyte List.: Tetra-Octa CDDs/CDFs
Method : Method 23 : T-O, Toluene Combined
Client Proj..: r012.002/Lime Kiln
Client : Pacific Environmental Services (PES03)
P.O. No : 104-98-0159 Collect Dt/Tm: SeeCOC
Contact : Mike Maret Phone : 919-941-0333
Proj . Mgr. . . . : Rose West Fax : 919-941-0234
Sample Origin: AL
• -SPECIAL INSTRUCTIONS / QA REQUIREMENTS --
Prep Project: 04228 Prespike Standard: USF-CS
Prespike Amount..: 4.Ong
Extraction Exp...: 04/22/98
----------- ........ ------- REPORTING REQUIREMENTS
Reporting Format: Report Option II
See MILES for Instructions/Communications.
: kj^tV-UttJ'
Completed by: j^t-tt' _ DATE:
Reviewed by: KVo _ DATE: ~"L-1/ (PMGT0197)
-------
' PROJECT COMMUNICATION TRACKING FORM
TU Project Number:
Use this form to record all exchanges of information between production units as well as personnel
handling this project Decisions, corrective actions and recommendations must also appear on this
tracking document
Date Name
Comment / Decision / Resolution / Action / Observation
PES03-Pacific Environmental Services
M23-I-3-4
R r~o j ©o^t- : -4-5399
2O4-—92—-3D
t-Mabama Lime - R012.002
afctoe. ' '
' 4laBarch Trtwgte Par*. Worth Carolina
module
TLI PH'.-jrrr 104223
DATE. •.;?-••"--:..-:
.SPIKE 'ns?Tc ;< us?
?RE?SI ' T;- ' AC
PAOI.'IC ^rJlR
PES03-P»cific Environmental Services
M23-I-4-4.
2O-4-—92 —
/US EPA Ume Mh Screening - At
i Pacific EnvkuuuBflttftSvticaa
fltesearch Triangle Park, North
-^- 03-17-98
* USF-S
ENVIRONMENTAL
-------
PES03-Pacific Environmental Services
M23-0-1-4
Pr-ojoc-t. : 4-5399
20-4-—92 —5D
US 9A Un» Kfti Screening - Alabama Lime - R012.002
jTitangtoParte, North Carolina
*unMail23-O-1 [M*
' MB. M23-O-1<4 XAD sorbent moduia
Triangle Laboratories, Inc
TLI PROJECT #04223
DATS: 03-17-98
SPIKE: USF.-C & USF-S
PREPSD BYfAC
PACIFIC ENVIRONMENTAL
PES03-Pacific Environmental Services
M23-0-2-4
Rr-ojeo-t : 4-5399
2O4-—9 2—6 D
^^ — — i III Lf ^ J •
\ if8 ?A Ume ^ Scrcentag-Alabama LJme - R012 002 Wa 0 <*
f Padlic Enviponn»rtal Sgvkaea. lae.
f. Research Triangte Pane. North
I Run No. M23rO-2
•4 XAD soi
Triangle Laboratories, Inc.
TLI PROJECT #04223
DATE: 03-17-98
SPIKE: USF-rC & USF-S
SPIKER »$MBfo .i
PREPED BY AC ' • x
PACIFIC ENVIROLM^KTAL
«?0-
Triangle Laboratories, inc.
TLI PROJECT #04228
DATE: 03-17-98 TLI BLANK
SPIKE: USF-C & USF-S
SPIKER
.PREPED BY AC
PACIFIC ENVIRONMENTAL
17
-------
PROJECT COMMUNICATION TRACKING FORM
page of
TU Project Number:
Use this form to record all exchanges of information between production units as wed as personnel
handling this project. Decisions, corrective actions and recommendations must also appear on this
tracking document
Date Name
Comment / Decision / Resolution / Action / Observation
$ ,^
10
i) JJrHcr
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0
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-------
' PROJECT COMMUNICATION TRACKING FORM
TU Project Number:
page _ of -
Use this form to record all exchanges of information between production units as well as personnel
handling this project. Decisions, corrective actions and recommendations must also appear on this
. ' tracking document
)ate Name
Comment / Decision / Resolution / Action / Observation
<- r
tU?J
tzl
z
-------
Date:
Time i
04/03/98
11:41
Sample
• crd TLI_Number. .
000 TLI Blank
001
002
003
004
005
006
007
008
009
010
Oil
012
013
014
204-92-1A-D
204-92-2A-D
204-92-3A-D
204-92-4A-D
204-92-5A-D
204-92-6A-D
204-92-7A-D
204-92-8A-D
204-92-9A-D
204-92-10A-D
204-92-11A-D
204-92-12A-D
TLI LCS
TLI LCSD
Wet Lab MM5/PUF Observations
Project: 45399
TLI M23 Blank
M23-I-1
M23-I-2
M23-I-3
M23-I-4
M23-0-1
M23-0-2
M23-0-3
M23-0-4
M23-FB-1
M23-FB-2
M23-FB-3
M23-RB-1-4
TLI LCS
TLI LCSD
F.
No
0
1
1
1
1
1
1
1
1
1
1
1
1
0
0
XAD
Color
WHITE
WHITE
NHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
Filter
Color
NA
GREY
GREY
GREY
BROWN
WHITE
WHITE
GREY
GRAY
WHITE
WHITE
WHITE
WHITE
NA
NA
Glass Wool PUF
Color . . - - Color .
NA
WHITE
WHITE
WHITE
WHITE
WHITE
NHITE
WHITE
WHITE
WHITE
WHITE
WHITE
WHITE
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
. . . . Odor
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
NONE
Air
0 No.
04228
04228
04228
04228
04228
04228
04228
04228
04228
04228
04228
04228
04228
NA
NA
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIQKAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGHAM
WHIGKAM
WHIGHAM
Date Tir
04/03 10:59 F
04/03 10:59 f
04/03 10:59 P
04/03 10:59 P
04/03 10:59 F
04/03 10:59 P
04/03 10:59 F
04/03 10:59 P
04/03 10:59 P
04/03 10:59 F
04/03 10:59 F
04/03 10:59 1
04/03 10:59 F
04/03 10:59 F
04/03 10:59 F
... s
•* End of Report
-------
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-------
| TRIANGLE LABORATORIES, IMC.
| Dioxin Sample Preparation Tracking 1 Management Perm
| Project: 45399 Client: Pacific Environn
| Solvent (a) /Acid(s) : '*\i,t+t- / / Method: Method 23: T-Or Toluen*
| Lot Numbers: »f sft& ^tA^f 1 / Extraction Date: O*f / O/ faf
1 SS Spike: M! cone: . ng/Ml 1 f*- 1 iTMJ | /
1 MS Spike; 0 M! cone: 0.0000 ng/Ml I Qv /V & | S"6 7* i | 5" ^f
1 LCS Spike: 0 M! cone: 0.0000 ng/Ml I t/^£ ~I \ i^JP-M/ | f*
| OPR Spike: 20 ftl cone: _0.01_ ng/Ml I £Z / *j£ /^J | J2 / " /^* | '/ /
| | TLI / | GROSS | SAMPLE | \\ : j&A^, t\ : l^o.^, 1>
|S#.crd| SAMPLE / CLIENT | WEIGHT | SIZE | .0-1 nq/Ml | *« nq/Ml | d 1
1 I ID / SAMPLE ID I Before After 1 ,q / ml I Y" Ml 1 l nq/Ml | • Con<
Ml I 7^ Ml 1 ' Vol
1 . / (Any Le
| |Any L«
| |Any Lc
•bv^&~5&
,^\^ X
I |Any t
1 1 yes/
1 |Any I
1 1 yes/
1 l*ny 1
1 1 yes,
1 (Any
1 l*ny
ross weight of sample container + sample before/after aliquot removal.
mments:
72
Initials:
Date:
tt both SPIXER AND OBSERVER mat be entered.
Term - dross Height not provided for WATER
— RBV 05/27/97 (PSTN
-------
PACE 1 OF I
TRIANGLE LABORATORIES, INC.
DIOXIN SAMPLE EXTRACTION and CLEANUP TRACKING FORM
TLI Project No.: 45399
Ext Stt.crd
TLI Number
x1 |
>- 1 £-
A |
k ! £ IV-
009
204-92-9A-D
;»»»»««s»:s«a»«aso««» + «»«»««»»+ »»«»»^fc» + *mmm9mmm + mmmmmmmm+mmmmmmmm + mmmmmmmm + mmmmmmmm+mmmmmmmm+mmmmmmmm+m'&mi^'m'mm+aim
Enter the procedure number below into the box at the top of each column to signify the step performed.
Initial and date each sample for each numbered procedure performed.
* ...... PROCEDURE ---- SOP.#. .v.. DETAILS (circle)
EXTRACTION
<2>> SPIKE AFTER EXT'N
/fj) ADD TRIDECANE
CM ROTOVAP
(5T) COMBINE
£j) SOLVENT EXCHANGE
(tip CLEANUP
/$)) TRANSFER
10) ADDITIONAL CLEANUP
11) FINAL TRANSFER
TimeOn _ : _ Time Off _ : _
Jar / Sep Funnel / Steam Di«t / Cont LL / ASE / Haste Dilution
Other_
Heptane tot#_
SP 2SOJ / DSP 225 / DSP 115 / DSP 215 / DSP 267 / Other'
Mod. DSP 260 / DSP 225 / DSP 115 / DSP 215 / DSP 267 / DSP260(10g)
Comments:
..Rev 11/25/97 (PSTKF 4).
*
4
-------
PAGE 2 OP 2
TRIANGLE LABORATORIES, INC.
DIOXIN SAMPLE EXTRACTION and CLEANUP TRACKING FORM
TLI Project No.: 45399
Ext S#.crd and I'l ' «7 ' "X ' U ' <"" ' J 1 '/ ^ /J '"^-? '*^" ' G
TLI Number | J~ \ £- \ ^ 1 /^ 1 ^ 1 ' *> \ \0 \ [4. \ ' 1 V | /
010 tft^ 1 (jpfcj
204-92-10A-D l0W(o3M ' jU\
on 1 I
204-92-llA-D | |
012 | 1 |
204-92-12A-D | 1 |
*"] *
013 | |
TLI LCS | L \
014 l-fl^ |
TLI LCSD Ic'fyk^Aft 1
1 %!$<$ ' i V'<^i$'£'*fel^''$/3rf! ^'S'-^'i^fr i ily
i / i i 1,1,1,1 i if
ii i i i i / i i i
+ . 1 ..+ + + L..+ L..+... i..-+ 4-. -* *
1 ] 1 1 _ 1 I 1 1 1 / 1 / 1 1
II 1 1 | 1 / 1 1 / 1 1
1 1 1 1 . 1 / 1 1 1 f 1 if
' i ' ' ' / ' J ' J ' ^ ' 1
1 ii '^- ' - ' v * AI v ' § &y$$ u/
yi(y i i ' w ' (/ ' WJft ' vjf
1 1 T 1 1 1 I I II l,SV
1 1 1 1 ! 1 1 1 1 1 \\
I 1 I 1 1 1 1 1 1 1 1
I 1 I I 1 1 1 1 1 1 1
! I 1 I 1 1 III
1 I 1 1 1 1 III
1 1 1 1 1 1 III
1 I 1 1 1 1 III
1 1 1 1 1 1 III
1 1 1 1 1 1 III
Enter the procedure number below
Initial and date each sample for
ft PROCEDURE.... SOP.#. .V.
/l) EXTRACTION
into the box at the top of each column to signify the step performed.
each numbered procedure performed.
. DETAILS (circle)
Time On : . Time Off :
goxhle^)/ Jar / Sep Funnel / Steam Dist / Cont LL / ASE / Haste Dilution
SPIKE AFTER EXT'N
I ADD TRIDECANE Lot* T&l I '£'I/
'4PROTOVAP
COMBINE
IV^/LIP. DETERM.
CLEANUP
( TRANSFER
10) ADDITIONAL CLEANUP
11) FINAL TRANSFER
1-2.1 '
20*/80% (50%/50%) 5mL/20mL Other_
Iso-Octane Lott ^7"77/^f Heptane Lot#_
260^ / DSP 225 / DSP 115 / DSP 215 / DSP 267 / Other
Mod. DSP 260 / DSP 225 / DSP 115 / DSP 215 / DSP 267 / DSP260U-Og)
Comments:
.......Rev ll/2S/!»7 (PSTMI
-------
PAGE 1 OF 1
TRIANGLE LABORATORIES, INC.
Transfer Chain-of-Custody Form
Project 45399
Transfer From: DWLH5 To: DMS5
Released by:
Accepted by:
MILES. ID
45399- -000
45399- -001
45399- -002
45399- -003
45399- -004
45399- -005
45399- -006
45399- -007
45399- -008
45399- -009
45399- -010
45399- -Oil
45399- -012
45399- -013
45399- -014
Initials . .
\*J^
TLI No
TLI Blank
204-92-1A-D
204-92-2A-D
204-92-3A-D
204-92-4A-D
204-92-5A-D
204-92-6A-D
204-92-7A-D
204-92-8A-D
204-92-9A-D
204-92-10A-D
204-92-11A-D
204-92-12A-D
TLI LCS
TLI LCSD
Date Time ^ . .
\>V /C /^V ? :*Vc?
Cust . Id
TLI M23 Blank
M23-I-1
M23-I-2
M23-I-3
M23-I-4
M23-0-1
M23-0-2
M23-0-3
M23-0-4
M23-FB-1
M23-FB-2
M23-FB-3
M23-RB-1-4
TLI LCS
TLI LCSD
Additional comments or instructions:
-XfrCOC (Rev 11/01/94)--
-------
PAGE 1 Or 2
Method: Method 23: T-0. Toluene Combined
TRIANGLE LABORATORIES, INC.
HR GC/BRMS ANALYSIS
| Required Detection Limit: 0.05 ng | PROJECT: 45399
| SAMPLE INFORMATION RS Cone
| 1ST COLUMN 2ND COLOMN 20 Ml • 100.0 PG/fil
| | TLI / I GC/MS FILENAME 1 CONFIRM | CONFIRM FILENAME (OSF-RS
j.Qtt rrA\ SIMPLE ID / CLIENT | COLUMN: Jfaj 1 1 COLUMN: 9 fit*?,, 1 VOLUME
| | / SAMPLE ID | II ISOLN i
| OSF-RS (ANALYSIS
|ntIT. | COMMENTS
D (DATE |
| | TLI Blank | II 1 ^ 3£A '^T^'
| | 204-92-1A-0 I II 1 /
looi i M23-i-i i\^Vt>l Of"l" ' V 'fTclir/j/ '
| | 204-92-2A-D I II I
t-^rf $/C lo i P^j. 1 ^ ^ Y"
| | 204-92-3A-0 I II 1
1
1
1
1
1
1
* T
| | 204-92-4A-D I II III
/ 1 \1 1 III
| | 204-92-5A-D I II 1
|005 | M23-0-1 | "T^V t^^ 1 V 1 p^ y 1
| 204-92-SA-D | ' \J ' '
|006 M23-0-2 | \t\\f\. W~> \ J I - 1
| 204-92-7A-D | I I 1
(007 M23-0-3 | 5^'^'1-'^0'5 1 V 1 BO.? '
| 204-92-8A-D I I v I 1
|008 M23-0-4 i $1*5 l^OW 1 f 'Ptjilt,/^ '
| 204-92-9A-D I II 1
|009 M23-FB-1 | $ ^ 1/^0 1 | N | f> ^13^ 1
| | 204-92-10A-D , I ' V ' OdFlP/A '
|010 | M23-FB-2 | y^-^t^*^ 1 f 1 Klfi'-^O '
1
!
i
i
1
i
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i
i
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| | 204-92-llA-D | ' V ' /7/v ' «^«^ | Wl / |
|011
Comments:
M23-FB-3
I «3U^ | W> /
??» !.Cc3i*-...!*K.
I1"* Type: X
Spike File: SPMIT204
Act of Extract: 50%
---REV 03/07/95 (PSTHF
-------
PAGE 2 OF 2
Method: Method 23: T-0. Toluene Combined
Required Detection Limit: 0.05 ng
TRIANGLE LABORATORIES, IMC.
HR GC/HRMS ANALYSIS
(PROJECT: 45399 |
SAMPLE IMFORMATION
1ST COLUMN 2ND COLUMN
RS Cone
20 fil • 100.0 PC/Ml
| TLI / | GC/MS FILENAME | CONFIRM | CONFIRM FILENAME (OSF-RS
l.crd) SAMPLE ID / CLIENT | COLDMU: _ | ICOLOMN; DbT\,\ |VOLDHE
| / SAMPLE ID | || ISOLN 10
(USF-RS (ANALYSIS
(IMIT. (COMMBMTS
(DATE |
204-92-12A-D
I TLI LCS
3 I
M23-RB-1-4
TLI LCS |
I
TLI LCSD
TLI LCSD
Comments:
Type: A
Spike Pile: SPMIT204 \
I
Ant of Extract: 50% (
•—REV 03/07/95 (PSTMP «)--»
27
-------
Run Log
Instrument ID Column Type Co|umn IP p|ot Name
^,£, £HV5 ^^fcMHf ~t,rti.(? m MniK-U-?
^L^- M/.yrtl
Signature Data
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" Dated initials required
srvr1/qa/fc>rms/hnunlog.doc (02/05197)
ConCal Due:
ConCal Due:
Page:
-------
inangie uiuuiaiuima, UK..
Run Log '
Instrument IP
Column Type
Column IP
Plot Name
Ini. Vol.
Acquisition
Signature
Filename
Date*
Time*
Project*
Sample*
No.
Client Sample ID
Syr
332
Operatoi/Date
Comments*
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lo.
tu
tu
Jx
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fj
MTtu
.iiflfi
- ft -
M
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** Pated initials required
srvrVqa/forma/hnunlog doc (02/05/97)
ConCal Pue:
ConCal Pue:
Page:
-------
Instalment IP
10T
Column Type
.ftfe'?
Column ID
Plot Name
Ini. Vol.
cquisition
/63a
^^^^^M__M^MnHM^MgMHgHHHMHBI^Vi^^^^H^^BV«"^^^^^^^^ "
Transcribed from chromatographic data
" Dated initials required
5rvr1/qa/forms/hmjnlog.doc (02/05/97)
MukfeiM
"1
'M'iU/U*/
»r
flU-V^i
ConCal Pue:
ConCal Due:
G/C
Page:
-------
uauoraiones, inc.
Run Log
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" Dated initials required
6fvr1/qa/fofms/hrtunlog doc (02/05/97)
ConCal Due: j -fT
ConCalDue:
-------
ttu I i /I 'vv ty~T^"'
Transcribed from chromatographic data
n_i~ J I^liixla ranll\ror\
ConCal
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doc (02rt»97)
Pane:
-------
inangie LJ "xx aim tea, mo.
F Log
Instrument ID Column Tvoe Column ID Plot Name Inj Vol
"=?OtLX ^v3t-^ >r# &<£•*> V Tc?-*- J.ffJi
Ml
Acquisition
/J^>& &l*-\
y^jt~,^\^.
GtC
j/rffg
Signature Date
Transcribed from chromatographic data
•* Dated initials required
srvrl/qa/lbnnB/hminlog.doc (02/05/07)
ConCal Due:
ConCal Due:
-------
r\ui i uuy
Instrument ID Column Type Column IP
PMName
InLVQL
Acquisit
Signature
Transcribed from chromatographic data
Dated initials required
Mvrl/qartbfms/hminlog.doc (02/0»07)
Dua:
G/C
Date
Page
2
-------
M BMi
Triangle Laboratories, Inc.
Run Log
Instrument ID Column Type Column ID Plot Name Inj. Vol. Acquisition
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Dated initials required
-
ConCalDue:
ConCalDue:
-------
Triangle Laboratories, Inc.
Run Log
Instrument ID Column Type Column ID
"3o? 7}£t? f -M-^QQ^S
Plot Name
-r-f {
Ini. Vol. Acquisition Q/G
U(Jt jL-_ iffitfi*
Signature Date
Filename
Date*
Time*
Project #
Sample*
No.
Client Sample ID
Syr
332
Operator/Date
Comments*
^
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html
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Transcribed from chromatographic data
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sivrl/qa/forms/hrrunlofl.doc (02106197)
jf
Null
mi
8-
M *lnhl
v/n/if
ConCal Due:
ConCal Due:
38
ir
-------
SAMPLE
DATA
Triangle Laboratories, me.
901 Capltota Drive P.O. Box 13485
Durham, NC 277134411 Research Triangle f
919*44-5729 Fax i 919444-5491
37
-------
TRIANGLE LABORATORIES OF RTF, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
Page 1
04/21/98
:===========;
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
U980780
TLI M23 Blank
ng
04/03/98
04/15/98
U
XAD
Soxhlet
(0.002)
(0.002)
(0.003)
(0.002)
(0.002)
(0.003)
0.01 J
{0.004}J
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.002)
(0.003)
(0.002)
(0.002)
.(0.002)
(0.003)
{0.004}
(0.002)
(0.002)
(0.002)
W981017
M23-I-1
ng
04/03/98
04/16/98
W
M23
Soxhlet
(0.03)
(0.05)
(0.06)
(0.06)
(0.06)
(0.09)
(0.1)
0.05
(0.03)
(0.04)
(0.04)
(0.04)
(0.04)
(0.05)
(0.06)
(0.08)
(0.1)
(0.03)
(0.05)
(0.06)
(0.09)
0.09
{0.06}
(0.04)
(0.06)
B
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 87.9 83.3
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 106 89.3
13C12-HXCDF 478 108 78.3
114 75.5
90.1 83.6
13C12-HxCDD 478
13C12-HpCDF 789
Other Standards Percent Recovery Summary (% Rec)
13C12-HxCDF 789 84.5 82.4
13C12-HXCDF 234 81.8 114
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 65.8 71.2
13C12-2378-TCDD 67.9 78.1
W981018
M23-I-2
ng
04/03/98
04/16/98
W
M23
Soxhlet
(0.04)
(0.07)
(0.09)
(0.08)
(0.08)
(0.1)
{0.29}
1.5
0.21
0.21
0.10 J
{0.05} J
(0.06)
(0.07)
{0.05} J
(0.1)
(0.1)
0.25
{0.11}
0.07
(0.1)
12.1
2.7
0.33
{0.05}
84.7
88.8
81.0
75.6
85.1
90.3
78.2
73.1
74.0
T981957
M23-I-3
ng
04/03/98
04/18/98
T
M23
Soxhlet
(0.003)
(0.004)
(0.007)
(0.007)
(0.007)
(0.01)
{0.03} JB
0.02 B
(0.003)
(0.003)
{0.007}J
{0.004}J
(0.004)
(0.005)
0.009 J
(0.008)
(0.02)
0.01
(0.004)
(0.007)
(0.01)
0.11
0.02
0.01
0.009
84.9
94.9
87.6
90.8
68.1
80.1
94.0
76.6
71.7
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham. North Carolina 27713
Printed: 11:2304/21;
-------
TRIANGLE LABORATORIES OF RTP, INC. Page 2
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
Data File U980780 W981017 W981018 T981957
Sample ID TLI M23 Blank M23-I-1 M23-I-2 M23-I-3
Units ng ng ng ng
Extraction Date 04/03/98 04/03/98 04/03/98 04/03/98
Analysis Date 04/15/98 04/16/98 04/16/98 04/18/98
Instrument U W W T
Matrix XAD M23 M23 M23
Extraction Type Soxhlet Soxhlet Soxhlet Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123 68.6 68.5 64.9 72.6
13C12-PeCDD 123 99.4 71.8 68.3 80.1
13C12-HxCDF 678 68.1 119 87.9 101
13C12-HxCDD 678 78.7 115 93.0 93.2
13C12-HpCDF 678 83.7 115 100.0 99.8
13C12-HpCDD 678 92.5 116 107 101
13C12-OCDD 83.0 103 95.4 65.6
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713 Printed-11 '23 \
Phone. (819* 544-5729 • Fax: '91 Q\ «
-------
TRIANGLE LABORATORIES OF RTP, INC. Page 3
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
=====================================================================================
Data File T981958 T981959 T981960 S982305
Sample ID M23-I-4 M23-O-1 M23-O-2 M23-O-3
Units ng ng ng ng
Extraction Date 04/03/98 04/03/98 04/03/98 04/03/98
Analysis Date 04/18/98 04/18/98 04/18/98 04/18/98
Instrument T T T S
Matrix M23 M23 M23 M23
Extraction Type Soxhlet Soxhlet Soxhlet Soxhlet
Analytes
2378-TCDD (0.003) (0.01) (0.006) (0.006)
12378-PeCDD (0.004) (0.02) (0.009) (0.009)
123478-HxCDD (0.006) (0.02) (0.01) (0.01)
123678-HxCDD (0.005) (0.02) (0.01) (0.01)
123789-HxCDD (0.005) (0.02) (0.01) (0.009)
1234678-HpCDD 0.008 J (0.03) 0.01 J (0.01)
OCDD 0.04 JB (0.05) {0.03} JB (0.02)
2378-TCDF 0.34 {0.02} B 0.03 B {0.007}JB
12378-PeCDF 0.04 J (0.01) (0.006) (0.006)
23478-PeCDF 0.04 J (0.01) (0.006) (0.006)
123478-HxCDF 0.01 J (0.01) (0.008) (0.006)
123678-HxCDF 0.008 J (0.01) (0.007) (0.006)
234678-HxCDF 0.008 J (0.01) (0.009) (0.007)
123789-HxCDF (0.004) (0.01) (0.01) (0.008)
1234678-HpCDF 0.007 J (0.02) {0.01} J (0.01)
1234789-HpCDF (0.007) (0.02) (0.02) (0.01)
OCDF (0.02) (0.04) (0.03) (0.01)
TOTAL TCDD 0.02 0.03 0.08 (0.006)
TOTAL PeCDD {0.003} (0.02) 0.03 (0.009)
TOTAL HxCDD 0.01 (0.02) (0.01) (0.01)
TOTAL HpCDD 0.02 (0.03) 0.01 (0.01)
TOTAL TCDF 2.6 {0.02} 0.25 {0.007}
TOTAL PeCDF 0.38 {0.01} 0.02 (0.006)
TOTAL HxCDF 0.05 (0.01) {0.007} (0.007)
TOTAL HpCDF 0.007 (0.02) {0.01} (0.01)
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 88.9 92.6 87.1 96.7
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 96.0 107 98.8 102
13C12-HXCDF 478 92.2 91.3 91.0 97.4
13C12-HxCDD 478 93.2 99.4 .95.9 96.5
13C12-HpCDF 789 76.0 84.8 82.2 95.2
Other Standards Percent Recovery Summary (% Rec)
13C12-HxCDF 789 76.1 38.5 V 66.8 62.9
13C12-HxCDF 234 75.6 39.2 V 73.2 65.3
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 60.6 22.9 V 57.4 54.8
13C12-2378-TCDD 53.7 22.3 V 54.3 49.0
Triangle Laboratories, Inc.® Analytical Services Division
-------
TRIANGLE LABORATORIES OF RTF, INC. Page 4
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
= = = ====== = = = = = ===== = ======= = ===============:========================:=======:======:=====
Data File T981958 T981959 T981960 S982305
Sample ID M23-I-4 M23-O-1 M23-O-2 M23-O-3
Units ng ng ng ng
Extraction Date 04/03/98 04/03/98 04/03/98 04/03/98
Analysis Date 04/18/98 04/18/98 04/18/98 04/18/98
Instrument T T T S
Matrix M23 M23 M23 M23
Extraction Type Soxhlet Soxhlet Soxhlet Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123 63.2 25.6 V 54.4 55.4
13C12-PeCDD 123 69.5 31.3 V 62.6 59.7
13C12-HxCDF 678 72.2 35.4 V 74.0 63.9
13C12-HXCDD 678 70.5 36.3 V 71.9 72.6
13C12-HpCDF 678 65.5 33.7 67.7 54.3
13C12-HpCDD 678 68.4 38.7 77.0 65.5
13C12-OCDD 40.3 25.1 47.7 63.1
Triangle Laboratories, Inc.® Analytical Services Division
801 Capftola Drive • Durham, North Carolina 27713 Printed-11 -23 04/21/98
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
TRIANGLE LABORATORIES OF RTP, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
Page 5
04/21/98
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
===============
S982306
M23-0-4
ng
04/03/98
04/18/98
S
M23
Soxhlet
:=================
S982307
M23-FB-1
ng
04/03/98
04/18/98
S
M23
Soxhlet
=================
S982308
M23-FB-2
ng
04/03/98
04/18/98
S
M23
Soxhlet
===================
S982309
M23-FB-3
ng
04/03/98
04/18/98
S
M23
Soxhlet
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
(0.004)
(0.006)
(0.008)
(0.007)
(0.007)
{0.01} J
0.05 JB
0.02 JB
(0.004)
(0.004)
(0.005)
(0.005)
(0.006)
(0.006)
(0.007)
(0.01)
(0.01)
(0.004)
(0.006)
{0.009}
{0.01}
0.17
0.01
0.008
(0.008)
(0.003)
(0.005)
(0.005)
(0.005)
(0.004)
(0.005)
(0.006)
(0.002)
(0.004)
(0.004)
(0.003)
(0.003)
(0.004)
(0.004)
(0.004)
(0.005)
(0.004)
(0.003)
(0.005)
(0.005)
(0.005)
(0.002)
(0.004)
(0.004)
(0.005)
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 91.8 93.5
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 89.7 106
13C12-HXCDF 478 93.4 90.4
13C12-HXCDD 478 83.8 92.9
13C12-HpCDF 789 104 110
Other Standards Percent Recovery Summary (% Rec)
13C12-HXCDF 789 87.0 84.9
13C12-HXCDF 234 86.1 87.4
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 79.7 74.4
13C12-2378-TCDD 64.1 63.1
(0.004)
(0.005)
(0.006)
(0.006)
(0.006)
(0.006)
(0.009)
0.005 JB
(0.004)
(0.004)
(0.004)
(0.004)
(0.004)
(0.004)
(0.005)
(0.006)
(0.006)
(0.004)
(0.005)
(0.006)
(0.006)
0.005
(0.004)
(0.004)
(0.005)
92.1
107
84.6
85.0
82.6
85.6
87.6
70.4
66.2
(0.003)
(0.005)
(0.005)
(0.005)
(0.005)
(0.006)
(0.008)
(0.002)
(0.004)
(0.004)
(0.004)
(0.003)
(0.004)
(0.004)
(0.005)
(0.006)
(0.006)
(0.003)
(0.005)
(0.005)
(0.006)
(0.002)
(0.004)
(0.004)
0.008
93.8
99.6
83.7
90.3
85.4
88.0
87.6
63.8
63.4
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Printed: 11:23 04/21
-------
TRIANGLE LABORATORIES OF RTP, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
=================================================
Data File
Sample ID
S982306
M23-0-4
S982307
M23-FB-1
S982308
M23-FB-2
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
ng
04/03/98
04/18/98
S
M23
Soxhlet
ng
04/03/98
04/18/98
S
M23
Soxhlet
ng
04/03/98
04/18/98
S
M23
Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123 70.7
13C12-PeCDD 123 68.3
13C12-HXCDF 678 80.5
13C12-HXCDD 678 95.3
13C12-HpCDF 678 74.4
13C12-HpCDD 678 87.2
13C12-OCDD 93.8
,1
.6
70.
83
72.8
91.7
80.5
106
119
72
95
96
104
102
133
114
Page 6
04/21/98
S982309
M23-FB-3
ng
04/03/98
04/18/98
S
M23
Soxhlet
64.2
74.3
84.5
97.8
82.6
99.2
104
Triangle Laboratories, Inc.® Analytical Services Division
8QT CapiJoJa Drive • Durham, North Carolina 27713
Printed: 1123 04/21/98
-------
Data File
Sample ID
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
= - = = = = = = = = ==a = ss
Analytes
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD .
2378-TCDF
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
TOTAL TCDD
TOTAL PeCDD
TOTAL HxCDD
TOTAL HpCDD
TOTAL TCDF
TOTAL PeCDF
TOTAL HxCDF
TOTAL HpCDF
TRIANGLE LABORATORIES OF RTP, INC.
Sample Result Summary for Project 45399
Method MIT2 Analysis (DB-5)
=— =— ==— =— =— =— — —— — sss===sss=assssss=ssss
S982310
M23-RB-1-4
ng
04/03/98
04/18/98
S
M23
Soxhlet
(0.003)
(0.004)
(0.004)
(0.004)
(0.004)
(0.004)
(0.005)
(0.002)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.003)
(0.004)
(0.004)
(0.003)
(0.004)
(0.004)
(0.004)
(0.002)
(0.003)
(0.003)
(0.004)
Page 7
04/21/98
Other Standards Percent Recovery Summary (% Rec)
37C1-TCDD 83.8
Other Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 234 101
13C12-HxCDF 478 82.5
13C12-HxCDD 478 82.5
13C12-HpCDF 789 95.2
Other Standards Percent Recovery Summary (% Rec)
13C12 -HxCDF 789 87 .7
13C12-HXCDF 234 89.1
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 66.0
13C12-2378-TCDD 59.9
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 2771 3
Printed: 1 1 :23 04/21,
-------
TRIANGLE LABORATORIES OF RTF, INC. Page 8
Sample Result Summary for Project 45399 04/21/98
Method MIT2 Analysis (DB-5)
Data File S982310
Sample ID M23-RB-1-4
Units ng
Extraction Date 04/03/98
Analysis Date 04/18/98
Instrument S
Matrix M23
Extraction Type Soxhlet
Internal Standards Percent Recovery Summary (% Rec)
13C12-PeCDF 123
13C12-PeCDD 123
13C12-HXCDF 678
13C12-HXCDD 678
13C12-HpCDF 678
13C12-HpCDD 678
13C12-OCDD
62.5
76.1
81.6
97.6
82.8
101
115
{Estimated Maximum Possible Concentration}, (Detection Limit).
Triangle Uboretories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713 Printed: 11 -23 04/21/98
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
TRIANGLE LABORATORIES, INC.
Sample Result Summary for Project 45399
Method 23X (DB-225)
=========-====================================================
Data File P981305 P981306 P981307
Sample ID TLI M23 Blank M23-I-1 M23-I-2
Units
Extraction Date
Analysis Date
Instrument
Matrix
Extraction Type
Analytes
2378-TCDF
ng
04/03/98
04/16/98
P
XAD
(0.005)
ng
04/03/98
04/16/98
P
M23
ng
04/03/98
04/16/98
P
M23
{0.007}JB
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 69.2 80.4
0.51
73.5
Page 1
04/20/98
P981308
M23-I-3
ng
04/03/98
04/16/98
P
M23
{0.007JJB
79.7
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North CaroHna 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:3804/20/l
-------
TRIANGLE LABORATORIES, INC.
Sample Result Summary for Project 45399
Method 23X (DB-225)
==========================================================:
Data File
Sample ID
Units
Extractior
Analysis Date
Instrument
Matrix
Page 2
04/20/98
P981309
M23-I-4
ng
Date 04/03/98
ate 04/16/98
P
M23
Type
P981310
M23-0-1
ng
04/03/98
04/16/98
P
M23
P981311
M23-O-2
ng
04/03/98
04/16/98
P
M23
======================
P981312
M23-O-3
ng
04/03/98
04/16/98
P
M23
Analytes
2378-TCDF
0.14
(0.01)
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 56.1 21.4 V
0.01 JB
54.0
(0.007)
60.0
Triangle Laboratories, Inc.® Analytical Services Division
801 Capftola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 21:38 04/20/98
-------
TRIANGLE LABORATORIES, INC. Page 3
Sample Result Summary for Project 45399 04/20/98
Method 23X (DB-225)
=====================================================================================
Data File P981317 P981319
Sample ID M23-0-4 M23-FB-2
Units ng ng
Extraction Date 04/03/98 04/03/98
Analysis Date 04/17/98 04/17/98
Instrument P P
Matrix M23 M23
Extraction Type
Analytes
2378-TCDF (0.005) (0.005)
Internal Standards Percent Recovery Summary (% Rec)
13C12-2378-TCDF 75.5 73.7
{Estimated Maximum Possible Concentration}, (Detection Limit).
Triangle Laboratories, Inc.® Analytical Sendees Division
801 Capftola Drive • Durham, North Carolina 27713 Printed: 21:38 04/20/
Phone: (919) 544-5729 • Fax: (919) 544-5491
-------
Method 8290 Sample Calculations:
Analyte Concentration
The concentration or amount of any analyte is calculated using the following expression.
Where:
Ap
RRF(a,=
w
Ap * RRF!a) * W
concentration or amount of a given analyte
integrated current for the characteristic ions of the analyte
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume
Detection Limits
The detection limit reported for a target analyte that is not detected or presents an analyte
response that is less than 2.5 times the background level is calculated by using the
following expression. The area of the analyte is replaced by the noise level measured in a
region of the chromatogram clear of genuine GC signals multiplied by an empirically
determined factor. The detection limits represent the maximum possible concentration of
a target analyte that could be present without being detected.
2 * 2.5 * (F * H) * Q*
Where:
DL(0)
2.5
F
H
RRF(0)
w
W
estimated detection limit for a target analyte
minimum response required for a GC signal
an empirical number that approximates the area to height ratio for a
GC signal. (F = 3.7 for all dioxin/furan analyses)
height of the noise
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume
Rev. 11/19/97
49
-------
Data Flags
In order to assist with data interpretation, data qualifier flags are used on the final reports.
Please note that all data qualifier flags are subjective and are applied as consistently as
possible. Each flag has been reviewed by two independent Chemists and the impact of the
data qualifier flag on the quality of the data discussed above. The most commonly used
flags are:
A *B' flag is used to indicate that an analyte has been detected in the laboratory method
blank as well as in an associated field sample. The 'B* flag is used only when the
concentration of analyte found in the sample is less than 20 times that found in the
associated blank. This flag denotes possible contribution of background laboratory
contamination to the concentration or amount of that analyte detected in the field sample.
An '£' flag is used to indicate a concentration based on an analyte to internal standard
ratio which exceeds the range of the calibration curve. Values which are outside the
calibration curve are estimates only.
An T flag is used to indicate labeled standards have been interfered with on the GC
column by coeluting, interferem peaks. The interference may have caused the standard's
area to be overestimated. All quantitations relative to this standard, therefore, may be
underestimated.
A ' J' flag is used to indicate a concentration based on an analyte to internal standard ratio
which is below the calibration curve. Values which are outside the calibration curve are
estimates only.
A TR' flag is used to indicate that a GC peak is poorly resolved. This resolution problem
may be seen as two closely eluting peaks without a reasonable valley between the peak
tops, overly broad peaks, or peaks whose shapes vary greatly from a normal distribution.
The concentrations or amounts reported for such peaks are most likely overestimated.
A *Q' flag is used to indicate the presence of QC ion instabilities caused by quantitative
interferences.
An 'RO' flag is used to indicate that a labeled standard has an ion abundance ratio that is
outside of the acceptable QC limits, most likely due to a coeluting interference. This may
have caused the percent recovery of the standard to be overestimated. All quantitations
versus this standard, therefore, may be underestimated.
An'S' flag indicates that the response of a specific PCDD/PCDF isomer has exceeded the
normal dynamic range of the mass spectrometer detection system. The corresponding
signal is saturated and the reported analyte concentration is a 'minimum estimate'. When
the 'S' qualifier is used in the reporting of 'totals', there is saturation of one (not
Data Rap P»ge 1 of2
Rev. 11/19/97
-------
necessarily from a specific isomer) or more saturated signals for a given class of
compounds.
A 'U' flag is used to indicate that a specific isomer cannot be resolved from a large, co-
eluting interferent GC peak. The specific isomer is reported as not detected as a valid
concentration cannot be determined. The calculated detection limit, therefore, should be
considered an underestimated value.
A 'V flag is used to indicate that, although the percent recovery of a labeled standard may
be below a specific QC limit, the signal-to-noise ratio of the peak is greater than ten-to-
one. The standard is considered reliably quantifiable. All quantitations derived from the
standard are considered valid as well.
An 'X' flag is used to indicate that a pentachlorodibenzofuran (PCDF) peak has eluted at
the same time as the associated diphenyl ether (DPE) and that the DPE peak intensity is at
least ten percent of the total PCDF peak intensity. Total PCDF values are flagged 'X' if
the total DPE contribution to the total PCDF value is greater than ten percent. All PCDF
peaks that are significantly influenced by the presence of DPE peaks are either reported as
"estimated maximum possible concentration (EMPC) values without regard to the isotopic
abundance ratio, or are included in the detection limit value depending on the analytical
method.
51
-------
Method 23 Sample Calculations:
Analyte Concentration
The concentration or amount of any analyte is calculated using the following expression.
Where:
AC
Ap
Qp
RRF(0)
W
Amt<0, =
Ap * RRF(a) * W
amount of a given analyte, expressed in nanograms (ng) or picograms
(Pg).
integrated current for the characteristic ions of the analyte
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume (W = 1.0 for Method 23 samples)
Detection Limits
The detection limit reported for a target analyte that is not detected or presents an analyte
response that is less than 2.5 times the background level is calculated by using the
following expression. The area of the analyte is replaced by the noise level measured in a
region of the chromatogram clear of genuine GC signals multiplied by an empirically
determined factor. The detection limits represent the maximum possible concentration of
a target analyte that could be present without being detected.
2 * 2.5 * (F * H) * Q*
Where:
DL(0)
2.5
F
H
W
Ap * RRF,0) * W
estimated detection limit for a target analyte, expressed in ng or pg
minimum response required for a GC signal
an empirical number that approximates the area to height ratio for a
GC signal. (F = 3.7 for all dioxin/furan analyses)
height of the noise
integrated current of the characteristic ions of the corresponding
internal standard
amount of internal standard added to the sample before extraction
mean analyte relative response factor from the initial calibration
sample weight or volume
Rev. 11/19/97
-------
TLI Project: 45399
Client Sample: TLI M23 Blank
Method 23 PCDD/PCDF Analysis (a)
Analysis File: U980780
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
XAD
TLI Blank
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
II
04/03/98
04/15/98
n/a
U980780
ML
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMTT204
UF51058
U980771
n/a
n/a
n/a
AnaJytes
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
1,2,3,4,6,7,8,9-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
U,3,4,6,7,8,9-OCDF
Totate •;: :;-;?.:::- • V- ;,:;.>•
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Amt, (ng)
ND
ND
ND
ND
ND
ND
001
V/.V/ X
EMPC
ND
ND
ND
ND
ND
4 ~ U
ND
ND
ND
IT I-/
ND
'•=::-••. ''•;.•""••. Amt (n^
ND
ND
ND
ND
EMPC
ND
ND
ND
OL* - EMPO ^ '=" «s IM»^:
0.002
0.002
ooni
U.UUj
0.002
0.002
0.003
Oo<
.CO
0.004
0.002
0.002
0.002
0.002
0 009
0.002
0009
V/.Uv^
OO09
v.VAy^
0.003
ffelmbef Dt EMPC • «,;
0.002
0.002
0.002
0.003
0.004
0.002
0.002
0.002
"O* ^B^t'v' f v*J^ ^^i^^to^.
*rV ^Tl* fS^ J-^f9CKy '
~
—
38:23 J —
J_
^ *
^^^
~— —
'tl^/Trff|ag»'
•••-
••" ' '
~
—
—
—
Page 1 of2
Mmj-SR vlM.LAKSC.HjOO
Triangle Laboratories, lnc.«
801 Capltola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/20/98
53
-------
TLI Project:
Client Sample:
45399
TLI M23 Blank
Method 23 PCDD/PCDF Analysis (a)
Analysis File: U980780
Internal Standards
»C,2-2,3J,8-TCDF
»C,j-2,3,7,8-TCDD
13C,;-l,2,3,7,8-PeCDF
'3C,:-l,2,3,7,8-PeCDD
13C,:-1.23,6,7,8-HxCDF
13C,2-l,2,3,6,7,8-HxCDD
13Cr-1.2,3,4,6,7,8-HpCDF
13Ci:-l,2,3,4,6,7,8-HpCDD
"Ci:-U,3,4,6,7,8,9-OCDD
Surrogate Standards (Type A)
l3C12-2,3,4,7,8-PeCDF
13Cr.-l,2,3,4,7,8-HxCDF
13C,2-l,2,3,4,7,8-HxCDD
'3C,:-l,2,3,4>7,8,9-HpCDF
Other Statidtaro::;i: | '^^ '• : v £•:
37CU-2,3,7,8-TCDD
Alternate Stances (Type Aj
13Cp.-l,2,3,7,8,9-HxCDF
13Ci;-2,3,4,6,7,8-HxCDF
Recovery Standards
13C12-1,2,3,4-TCDD
'3r,,-1.2.3.7.8.9-HxCDD
, Anit« (ng)-?..
2.6
2.7
2.7
4.0
2.7
3.1
3.3
3.7
6.6
^Am£>g)
4.2
4.3
4.6
3.6
>•''•"•• AttjL.(ftg)
3.5
^HAmt^-{ng)
3.4
3.3
'
-7-^ ^v_^7"
;^"'^%R«COVWqg. •%
65.8
67.9
68.6
99.4
68.1
78.7
83.7
92.5
83.0
% Recovery
106
108
114
90.1
%r*K*veiy;
87.9
v;% Recovery
84.5
81.8
-Wr-
QC Limits
40%-130%
40%- 130%
40%-130%
40%-130%
40%-130%
40%- 130%
25%-130%
25%-130%
25%-130%
QCLlmtts
40%-130%
40%- 130%
40%-1307o
25%- 130%
''.'.''*•• ~- •{
40%- 130%
QC Limits
40%-130%
40%-130%
-,'--irrr-
*$£&&$&
•>• •£ f?'-ty ^-dCxws ftrsSv^
0.77
0.81
1.48
1.50
0.50
1.23
0.39
1.00
0.87
"-' Ralte
1.46
0.49
1.22
0.42
-
;^ Rafe--
0.50
0.50
' /' RalH»-"
0.82
1.20
%x ft3* N> *"^^-x^E^%KEK
•A 3r l^Bv ^sr*. ^ ^"* ' ?s * ^•^•SJW* %
23:21
24:07
27:32
28:38
31:15
31:57
34:04
35:03
38:22
frr frfegs
28:17
31:10
31:53
35:30
, at ^JFfegs
24:08
- &;?.•.•• ;--xFkgs
32:30
31:46 .
-^- ,fJT '^^-^ta^s
23:55
32:16
Data Reviewer,
Page 2 of 2
04/20/98
MinLPSRvlM.LAltSa.llA
Triangle Laboratories, lnc.«
801 Cap'rtola Drive • Durham, North Carolina 27713
(919) 544-5729 • Fax: (919^ 544-5491
Printed: 13:40 04/20/9)
-------
Initial
Data Review By:
Calculated Noise Area:
4.07
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirement*.
Page No.
04/20/98
Listing of 0980780B.dbf
Matched OC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
D
320-322
37C1-TCDD
328
323
13C12-TCDD
332-334
332-334
PeCDF
340-342
0.65-0.89
DC NL 0:00 RO 0.62
23:22 RO 0.45
1 Peak
0.65-0.89
DC NL 0:00 RO 1.96
DC WL 22:13 0.76
22:54 0.87
23:21 0.77 27,
23:49 RO 0.99
3 Peaks 27,
0.65-0.89
DC NL 0:00 RO 0.63
DC SN 23:20 RO 3.39
D SN 24:08 RO 0.43
DC SN 24:21 RO 1.36
DC SN 24:30 RO 1.70
0 Peaks
DC NL 0:00
22:37
24:08 18
2 Peaks 18
0.65-0.89
DC NL 0:00 RO 2.10
22:53 RO 1 . 12
23:55 0.82 28
24:07 0.81 21
24:29 0.79
4 Peaks 49
1.32-1.78
DC NL 0:00 RO 0.84
DC SN 25:29 RO 2.89
DC SN 25:48 RO 0.72
DC SN 26:05 RO 0.47
15.06
32.25 14.03
32.25
6.21
318.34
121.02 56.22
052.70 11,732.50
69.14 38.57
242.86
4.90
8.18
18.85
2.60
2.16
0.00
1.39
17.02 17.02
,717.10 18,717.10
,734.12
13.54
104.54 66.07
,009.20 12,615.40
.268.95 9,538.45
318.23 140.18
,700.92
TCDD / P*CDF Follows ~
4.33
5.38
3.36
3.64
0.844-1.086
0.000
31.51 1.001 2378-TCDF AN J
0.957-1.043
0.000
0.951
64.80 0.981
15,320.20 1.000 13C12-2378-TCDF ISO
39.06 1.020
0.878-1.050
0.000
0.968
1.001 2378-TCDD AN
1.010
1.016
0.917-1.083
0.000
0.938
1.001 37C1-TCDD CLS
0.917-1.083
0.000
59.06 0.949
15,393.80 0.992 13C12-1234-TCDD RSI
11,730.50 1.000 13C12-2378-TCDD IS1
178.05 1.015
0.917-1.068
0.000
0.926
0.937
0.947
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 13:40 04/2CV98
-------
Page No.
04/20/98
Listing of O980780B.dbf
Matched GC Peak* / Ratio
/ Ret. Tin*
Compound/
H_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Nam*.. ID.. Flags.
340-342
i3C12-FeCDF
352-354
352-354
PeCDD
356-358
D
D
356-358
13C12-PeCDD
368-370
368-370
HxCDF
374-376
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
D
DC
D
DC
DC
DC
DC
DC
DC
DC
DC
DC
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
NL
7
NL
SN
SN
SN
SN
SN
SN
WH
WH
0
NL
4
NL
SN
SN
SN
26:26 RO
26:39 RO
26:49
26:58 RO
27:10 RO
28:11
28:17 RO
28:25
29:14 RO
29:20 RO
Peaks
1..
0:00
26:38
27:10
27:32
27:51
28:17
28:38
29:16
Peaks
1.
0:00 RO
26:55 RO
27:32 RO
27:39
28:17
28:36 RO
29:05 RO
29:22 RO
29:38 RO
Peaks
1.
0:00 RO
27:32
28:38
28:46
29:00 RO
1 Peaks
1
0:00
31:11
31:53 RO
31:56 RO
0.16
0.57
1.43
0.43
0.52
1.73
2.08
1.50
0.99
0.72
32-1.78
1.46
1.49
1.34
1.48 21.
1.53
1.46 22.
1.66
1.58
45,
32-1.78
0.69
0.59
1.08
1.72
1.77
2.08
0.93
0.36
1.17
32-1.78
0. 98
1.64
1.50 16
1.53 1
3.03
17
.05-1.43
1.30
1.07
0.71
0.25
1.07
5.74
1.65
2.50
5.91
4.61
5.99
4.95
4.95
2.50
0.00
3.27
515.16 308.00
43.38 24.88
926.89 13,102.30
168.38 101.84
359.52 13,285.30
44.32 27.66
65.71 40.27
123.36
\nf*r\f> t D^/^f^A T?i^1 1 Ai*f«
'vv.Ur / r«v,UU r Oiiows - —
1.83
5.26
15.14
3.13
15.90
3.70
4.28
2.37
6.70
0.00
2.39
28.72 17.85
,427.29 9,847.36
,424.21 860.99
13.36 15.88
.893.58
PeCDD / KxCDF Follows --
10.44
8.09
4.15
3.16
0.960
0.968
0.974
0.979
0.987
1.024
1.027 23478-PeCDF
1.032
1.062
1.065
0.855-1.145
0.000
207.16 0.967
18.50 0.987
8,824.59 1.000 13C12-PeCDF 123
66.54 1.012
9,074.22 1.027 13C12-PeCDF 234
16.66 1.040
25.44 1.063
0.928-1.022
0.000
0.940
0.362
0.96d
0.988
0.999 12378-PeCDD
1.016
1.026
1.035
0.860-1.140
0.000
10.87 0.962
6,579.93 1.000 13C12-PeCDD 123
563.22 1.005
5.24 1.013
0.959-1.047
0.000
0.998 123478-HXCDF
1.020
1.022
AN
IS2
SUR1
AN
I S3
AN
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919} 544-5729 e Fax: (919\ 544-5491
Printed: 13:40 04/20
-------
Page No.
04/20/98
Listing of 0980780B.db£
Matched GC Peaks / Ratio
/ Ret. Tine
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Mane..
ID.. Flags.
D
374-376
13C12-HXCDF
384-386
334-336
HxCDD
390-392
D
D
390-392
isc 12 -HXCDD
402-404
402-404
HpCDF
408-410
408-410
13C12-HpCDF
418-420
418-420
DC SN 32:04 !
DC SN 32:07 1
DC SN 32:11
DC SN 32:29
D SN 32:31
DC WH 32:55
0 Peaks
DC NL 0 : 00
30:10
30:18
31:10
31:15
31:46
32:30
6 Peaks
DC NL 0:00
D SN 31:10
D SN 31:16
DC SN 31:47
DC WH 32:30
0 Peaks
DC NL 0:00
31:22
31:53
31:57
32:16
4 Peaks
DC NL 0:00
DC SN 34:06
DC SN 35:27
DC SN 35:36
DC WH 35:43
0 Peaks
DC NL 0:00
34:04
35:30
2 Peaks
RO
RO
RO
RO
RO
0.
RO
1.
RO
RO
RO
RO
RO
1.
RO
0
RO
RO
RO
RO
0
RO
0.34
2.02
3.67
0.73
1.11
0.42
43-0.59
1.27
0.45
0.47
0.49 19,
0.50 22,
0.50 24,
0.50 19,
86,
05-1.43
0.83
1.95
2.30
3.01
8.36
05-1.43
1.03
1.17
1.22 15
1.23 19
1.20 24
59
.88-1.20
2.42
2.70
1.08
3.00
2.77
.37-0.51
0.60
0.39 16
0.42 12
28
1.64
2.93
2.53
6.20
11.58
3.54
0.00
11.01
211.83 66.19
252.65 80.95
894.83 6.563.63
345.35 7,415.55
229.50 8.099.80
282.44 6,456.14
216.60
IvOTlP / Uv^"An V/
-------
Pag* No.
04/20/98
Listing of U980780B.dbf
Matched OC Peaks / Ratio / Ret. Tim*
Compound/
M_Z QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Are*.Peak.2.. Rel.RT Compound. Maine. . ID.. Flags.
Above: HpCDF / HpCDD Follows
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
OCDF
442-444
442-444
OCDD
458-460
458-460
0.88-1.20
DC NL 0:00 RO 0.36 1.61
DC WL 34:03 RO 2.59 10.38
DC SN 34:38 RO 4.74 2.33
0 Peaks 0.00
0.88-1.20
DC NL 0:00 RO 1.38 13.63
34:21 RO 1.30 80.62
35:03 1.00 16,382.49
2 Peaks 16,463.11
51.37
8,187.87
0.975-1.005
0.000
0.971
0.988
0.971-1.029
0.000
39.52 0.980
8,194.62 1.000 13C12-HpCDD 678 IS7
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0:
34:
34:
35:
35:
35:
35:
35:
36:
38:
40
40
40
00
34
39
03
29
37
48
54
:54
:51
: 39
:46
:55
0.'
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
76-
0.
1.
0.
1.
1.
1.
1.
0,
2,
0
2
1
1
1.02
97
05
72
89
15
35
10
.63
.02
.35
.08
.91
.18
DC NL
0.76-1.02
0:00 RO 2.18
38:23 0.86
1 Peak
2.10
37.20
37.20
10.07
Above: HpCDD / Octa-CDD and CDF Follows
4.97
1.78
4.16
10.05
6.41
3.74
4.16
6.99
3.59
1.34
1.49
1.08
2.91
10.05
5.32
896-1.104
0.000
0.901
0.903
0.914
0.925
0.928
0.933
0.936
0.962
1.013
1.060
1.063
17.20
1.066
0.896-1.104
0.000
20.00 1.000 OCDD
AN
13C12-OCDD 0.76-1.02
470-472 DC NL 0:00 RO 2.50 1.91
38:22 0.87 22,056.70
470-472 1 Peak 22,056.70
10,248.60
0.995-1.004
0.000
11,808.10 1.000 13C12-OCDD
1S8
Column Description.
•Why Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
..RT. -Retention Tine (muss)
Rat.l -Ratio of M/M+2 Ions
OK
-RO»Ratio Outside Limits
WL-Below Retention Time Window A-Peak Added
Rel.RT- Relative Retention Time
•** End of Report
WH-Above Retention Tine Window
SN-Below Signal to Noise Level
-------
ile:0980780 #1-893 Acq:15-APS-199B 20:48tSl CC SI+ Voltiya SIS 70S Nairn*:3276
03.9016 T:2 BSOB(256,30,-3.0) PKD(9,5, 3, 0.10\, 13104.0,1.00\,r,T) Xxp:NDB5tJS
TRIANGLE LABS TmxttTLI M23 BLANK TLH45399
00\ A1.10E5
20} 00 21:00 22,00 23:00 24:00
Fil»,0980780 tl-893 Acq:15-APR-1998 20:48:51 CC 11+ Volttgm SIX 70S Noi»»:5246
305.8987 Tt2 BSVB(2S6,30,-3.0) PKD(9,S,3, 0.10\,20984 .0,1. 00\,r,T) Exp:HDB5US
TRIANGLE LABS TertiTLI K23' BLANK TLIH5399
1004 A3.1515
20:00 21:00 22:00 2.5:00 24:00
rile:U980780 #1-893 Aeq:15-APR-1998 20:48:51 GC EI+ Voltage SIR 70S Noiae:3441
315.9419 F:2 BSUB(256,30, -3.0) PKD(9,5,3, 0.10\,13764 .0,1. 00\,ff T) Elp-.SDBSOS
TRIANGLE LABS T*xt:TLI H23 BLANK TLI#4S399
100\
80;
40
20:
A1.J.7E8
20:00 21:00, 22:00 23:00 24:00
rile:U980780 #1-893 Ac
-------
ril*iU980780 tl-893 Acqtl5-APX-1998 20:48(51 6C XI+ Volttye SIX
70S Jtol««>1065
319.8965 Ti2 BSUB(256,30,-3 .0) PKD(7, 5,3,0 . 10\,4260. 0,1. 00\,r,T) XxptODBSUS
TRIANGLE LASS TfJCtiTLI M23 BLANK TLIt45399
1001
80:
60:
40.
' j
20. 1
', '
A1.57X5
\
_3.or4
A3. 82X4 '•
A'''viywi->/irl — A/kJffw WM l-/v\.A^jjuv'"'y
22:00 ' ' 23:00 ' ' 24:00
rileiU980780 tl-893 Acqtl5-APX-1998 20:48:51 GC KI+ Volttg* SIX
2.4X4
1.8X4
1.2X4
5.9X3
O.OfO
25 tOO ' ' Time
70S Xoif*il687
321.8936 Tt2 BSUB(256, 30, -3.0) PXD(7r5,3, 0.10%, 6748. 0,1 . 00%, J-, T; XzptNDBStTS
TRIANGLE LABS T«xt:TLJ H23 BLANK TLIt45399
1001
80:
60:
40.
20:
\ / ^^^
•N i f j ** 5^^^ ^4 & ^i
^•y ' Hu J\M^r^'Wic — jyivwv/rww ^v
22:00 , 23 .-00 24:00
ril»sO980780 tl-893 Acq:15-APR-1998 20:48:51 GC EH- Volt aye SIX
12X5 -5.5X4
•
|
L Aj 22X4
li. h J J1 * r A
v¥VVWL/*V/^_Av#v u VVA^*^/^ v
.4.4X4
.3.3X4
.2.2X4
.1 . 1X4
25:00 Tiae
70S Noif»t8036
331.9368 r-.2 BSUB(256, 30, -3. 0) PXD( 7,5, 3, 0.10%, 32144.0,1 . 00\,r,T) KxptNDBSUS
TRIANGLE LABS TeztiTLI M23 BLANK TLIt45399
1001
sol
60:
40.
20.
0'
A1.26EB
-3.0X7
L»5.54r7
1
} U
V
.2.4X7
_1 . 81T7
.1.2X7
.6.0E6
• 0 . OEO
22:00 23^00 24 i 00 25:00 ' ' Tijie
rileiU980780 tl-893 Acq:15-APX-1998 20:48:51 SC XI+ Voltage SIX 70S Hoi ft -.3 8 27
333.9338 T-.2 BSVB(2S6,30, -3 .0) PKZ( 7,5,3, 0.10%, 15308. 0,1 . 00%, T,
TRIANGLE LABS Tejct:TEI M23 BLANK TLIt45399
1001
801
60'.
40.
20.
0
A1.54r8
A
L.
(I
i
1
J w
T; Exp:NVB5US
3 . 6E7
17X8
A
\
\
V
.2.9X7
.2.1X7
.1.4X7
.7.2X6
• 0 . OEO
' 22:00 ' ' 23:00 24iflO 25^00 ' Time
ril»>U980780 tl-893 AcqilS-APR-1998 20i48,51 GC XI* Voltage SIX 70S Jtoif»i696
327.8847 T: 2 BSUB(256, 30, -3 , 0) PKD(7 , 5 ,3 , 0 . 10\, 2784 .0,1 .00\, r, T) Exp:NDB5US
TRIANGLE LABS TextsTLI M2 3.' BLANK TLH45399
100.
80.
60.
40.
20
0
\ A1
<
•
1
' 22«00 ' 23^00 24:0
|7£8 _4.4r7
V
.3.5E7
.2.6X7
.1 . 8X7
.8.8X6
0.0X0
0 25:00 ' ' ' Ti»«
ril«sU980780 tl-893 Acg: 15-APS-1998 20:48:51 GC EI+ Volttge SIX 70S
330.9792 Tt2 Exp:NDB5US
TRIANGLE LASS TmxttTLI M23 BLANK TLIt45399
100
80
60
40
20
0
}^~_ 3i>*3 22, or' '22:J1 ".54 ^LiiH'f*. £f»51c
: Virv-/^rv^-^>^*-
-------
il*:t7980780 »l-893 Acg:15-APK-1998 20:48)51 CC XX+ Voltage SIS 70S Noiae: 131^7
39.8597 rt2 BSOB(256,30,-3.0) PKD(7,5,3,0,10\,5268.0,1.00\,r,T) XxpiMDtSUS
TRIANGLX LABS TerttTLI M23 BLANK TLH45399
26:00 27:00 28:00 29:00
ile:U980780 tl-893 Aeq:15-APR-1998 20:48:51 CC XI+ Volt*?* SIS 70S Noi*e:1568
41.8567 F:2 BSUB(256,30,-3.0) PKD(7,5,3,0.10\, 6272.0,1. 00\,r,T) Xxp:NDBSOS
TRIANBLX LABS TeJtttTLI M23 BLANK TLIH5399
004 *?•
001
80:
60.
40:
20:
A6.
A3.78X4
80:
so:
40:
20:
7E4
A6.08E4
A6.B9E4
26:00 27:00 28:00
File:O980780 tl-893 Acq: 15-APR-1998 20:48:51 GC EI+ Voltage SIR 70S Noia0:971
51.9000 T:2 BSUB(256, 30, -3.0) PKD(7, 5,3, 0.10%, J884. 0,1. 00\,r,T) Exp:NDBSOS
TRIANGLE LABS Text:TLI M23 BLANK TLIt4S399
1001 A1.31E8 A1.33E8
80:
60:
29:00
40:
20:
L V
25:00 27:00 28:00
File:U980780 tl-893 Acq:15-APR-1998 20:46:51 GC EI+ Voltage SIR 70S Noiae:666
353.8970 T:2 BSUB(256t 30, -3 . 0) PKD(7, 5,3,0.10\,2664 .0,1.00\,F,T) Exp:NDB5US
TKI ANGLE LABS TeitiTLI M23 BLANK TLI#45399
29-00
1001
80:
40:
201
A8.82E7
26:00 27:00 28:00
File:U980780 tl-893 Acq:15-APR-1998 20:48:51 GC EI+ Voltage SIR 70S
330.9792 T:2 ExpsNDBSDS
TRIANGLE LABS Text:TLI H23 BLANK TLIt45399
29:00
1001
80:
60.
40:
20:
o:
25: 31 2547 26:09
27:00
27:45
-------
>C9'43~Arj(-4yy0 ju:*ui3ji sc *if voltage SIM /us aoiuetSSS
55.8546 Ti2 BSUB(256,30,-3.0) PKD(5,5,3,0.05\,2220.0,1.00\,f,T) Xxp:HDSSUS
TXIAOGLX LASS TextiTLI H23 BLANK TLIt45399
°°* "'I™ A6.37X4
27100 28'tOO 29:00
Til*,0980780 41-693 Aoq:lS-APS-1998 20,48,51 CC XH- Voltage SIX 70S Hoif0,801
57.8516 T:3 BSU3(256,30,-3.0) PXD(5,5,3,0.05%,3204.0,1.00\,T,T) XxptSDBSUS
TRIANGLE LASS TexttTLX H23 BLANK TLI»45399
100\ AS.40X4
80.
60.
40.
20.
0.
27:00 28:00 29:00
rile:0980780 tl-893 AcqslS-APB-1998 20:48:51 GC XI+ Voltage SIS 70S ttoiae:727
'67.8949 T:2 BSUB(256,30, -3 .0) FKD(5, 5,3, 0. 05\,2908. 0,1. 00\,r, T) £xp:HDBSOS
TRIANGLE LABS Text:TLI M23 BLANK TLH45399
A9.85E7
80.
60.
40.
27,00 28:00 29:00
File:0980780 tl-893 Acq:15-APS-1998 20:48:51 CC XI* Voltage SIS 70S Koife:740
369.8919 T:2 BSUB(256,30,-3.0) PKD(5, 5,3,0. 05\,2960.0,1.00\,T,T) ExptXDBSUS
TJtIANSLE LABS TextiTLI M23 BLANK TLHH5399
100\ A6.J8E7
so:
eo:
40.
201
0.
rr
-r
>.63X6
^V
27iOO 28iOO
File:U980780 tl-893 Acq:15-APS-1998 20:48:51 CC XI + Voltage SIS 70S
330.9792 T:2 Xxp:KDB5US
TSIAltSLX LABS TextiTLI H23 BLANK TLH4S399
29:00
10<&
80.
60.
40.
20.
0.
27:00
2.4X4
1. 9X4
.1. 4X4
.9. 5E3
14.7X3
0.0X0
Time
3. 0X7
2.4X7
.1. 8X7
.1.2X7
.6.1X6
.0.0X0
Time
.2.0X7
.1.6X7
.1.2X7
.7.9X6
.4.0X6
.0.0X0
Time
12r5.7X7
.4.6X7
.3.4X7
.2.3X7
.1.1X7
27\00
at t oo
39 1 00
.0.0X0
Time
-------
-------
,J.eiUyau/aO tl-113 Acq:15-APM-lS98 20:48:51 GC EI+ Volt*y» SIX 70S tfoil»,2614
89.8156 f,3 BSUB(256,30, -3.0) HO>{ 7,3, 3,0.10\, 10456.0,1.00\,T,T) IxptXDBSUS
XHIANGLS LASS T«jct>3ZZ H23 BLAHX TLI145399
001 A1.39E5
30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32,24
ile:U980780 01-413 Acq:15-APB-1998 20:48:51 GC SI+ Voltcgr* SJJt 705 No±f»:3167
91.8127 Ti3 BSU*(256,30,-3.0) fKD<7,5,3,0.10\,12668.0,1.00\,FrT) XxptXDBSVS
TSIANGLX LABS TtacttTLI H23 BLANK TLH45399
001 A6.14X4
30t36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24
rile:U980780 tl-413 AcgilS-APR-1998 20:48:51 GC EI+ Voltage SIS 70S Noia«:4424
01.8558 f:3 BSUB(256, 30r-3 .0 ) PKD(7t 5, 3, 0.10\,17696. 0,1. 00\,r,T) Eip:HDB5CS
TBI ANGLE LABS TeltiTLI M23 BLANK TLI#45399
001 A1.J3E8
AS. 73f4
AS.99f4 A1.30S4
32,36
32:36
80.
eo:
40.
20:
Al.OSES
30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36
rile,0980780 41-413 Acq:15-APS-1998 20:48:51 GC EI+ Voltage SIX 70S tfoia«:4307
403.8529 T:3 BSUB(256, 30, -3. 0) PKD(7, 5 ,3, 0.10\, 17228 .0,1. 00\, F,T) Ejfp:KDBSas
TRIANGLE LABS T«Jt:OXI H23 BLANK TLI#45399
1001 A1.11ES
801
eo:
40.
20J
A8.55E7
30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00
rilmt0980780 01-413 Acq:15-APR-1998 20:48:51 GC ZX+ Volttya SIX 70S
392.9760 T:3 ExptHOBSVS
TBIANGLE LABS T»xt:TLI H23 BLAKK TLH45399
100* 30t38 . 30:57 31:06 31:24
BO:
eo:
40.
20.
0.
4.1E7
.3.2E7
.2.4E7
.1. 6E7
.8.1E6
.O.OEO
Tim*
.3.4X7
.2. 7X7
.3. 0X7
.1.3X7
.6.7X6
32:12 32:24
32:36
.0.0X0
Tim
33,19 "*3033,3B
30,36 30:48 31:00 31:12 31:24 31,36 31,48 32tOO 32:12 32,34 32,36
.3.5X7
.3.0X7
.1.5X7
.1.0X7
.5.0X6
0.0X0
-------
He,0980780 tl-662 Acqil5-APX-1998 20t48t51 GC CI+ Voltmgm SIX 70S Nairn*t2930
07.7818 T:4 BSUt(256,30,-3.0) PXD(7,5,3,0.10\, 11680.0,1.00\,r,T) XxptNDBSUS
\IARGLE LASS Tart;IXJ M23 SLANT TLIH5399
00*
80J A9-t9E4 II A1.72X4
34,00 34,12 34,24 34,36 34,48 35,00 35,12 35,24 35,36
ile:V960780 tl-662 AcqilS-APX-1998 20t48i51 GC XI+ Volttym SIX 70S Noit»,1203
09.7789 F,4 BSUB(256,30,-3.0) PKD( 7, 5,3,0.10\,4812.0,1.00\,F,T) ExptKDBSUS
TXIAtKLX LASS TextiTLI H23 BLAH* TLIf45399
00\ A5.88X4
sol
40:
sol
ol
34,00 34,12 34,24 34,36 34,48 35:00 35,12 35,24 35,36
rile:V980780 tl-662 AcqtlS-APX-1998 20:48:51 GC EX+ Voltage SIS 70S Hoif»,1898
17.8253 T:4 BSUB(2S6, 30,-3.0) PJO>(7,5,3, 0.10\, 7592. 0,1.00\,T, I) Exp:NDBSOS
TRIANGLE LABS TextiTLI M23 BLANK TLIt45399
1001 A4.74E7
.4.3X4
.3.414
.2.5E4
.1. 7X4
.8.4X3
0.0X0
35,48 36,00
A3
..2.6E4
.2.1X4
.1. 6X4
.1.1E4
.5.3X3
35,48
60:
40:
201
0.
A3.61E7
34:00 34:12 34:24 34:36 34:48 35:00 35:12 35,24 35:36
rile,O980780 tl-662 Acq:15-APX-1998 20:48:51 GC EH- Voltage SIR 70S Noiae:3168
419.8220 r,4 BSUS(256,30,-3.0) PKD( 7, 5,3, 0.10\,12672. 0,1. 00\,F, T) EzpiNDBSUS
TRIANGLE LABS TextlTLI H23 SLANT TLI#45399
1004 A1.20E8
35,48
80J
601
401
0.
A8.52E7
34:00 34:12 34:24 34,36 34:48 35:00 35:12 35,24
rile:O980780 tl-662 Acq:15-APS-1998 20:48:51 GC EI+ Voltay* SIB 70S
430.9729 T-.4 Exp:KDB5US
TSIAlfGLE LABS Text:TLI H23 BLANK TLI#45399
35:36
35,48
1003
aol
34:05 34,16
34,00 34,12 34,24 34:36 34,48 35', 00 35', 12 35:24
rile,,0980780 tl-662 Acqil5-APK-1998 20:48:51 GC XI* Voltage SIS 70S
479.7165 T>4 EJCpsHDBSOS
TJtlAVSLX LABS Teat:TLI H23 BLANK TLIt45399
351 05
35,36
35,48
34100
34,12
34134
34136
34,48
35:00
35,12
35,24
35,36
35,48
36:
O.OEO
00 Time
-.1.1X7
la.5X6
.5.7X6
.2.8E6
36,00 Tim»
-3.4E7
.2.7E7
.2.0E7
.1.4X7
.6.8X6
36.
0.0X0
00 Time
•.O.OEO
36:00 Timm
.0X0
36', 00 Timm
-------
riJ.e:PS80/80 fl-t>til AOJ:li-AfM-J.yya 20,48,51 CC XI* Volcagr* SIM 70S BOJ.*»:409
423.7766 T>4 BSW>(256,30,-3.0) PXD(7,5,3,0.10\,1636.0,1.00\,r,T) XxptHDBSaS
XXIJUKLf LABS Tmxt'.TLI M23 BLAST TLIH5399
ion
34>12 34,18 34,24 34,30 34,36 34,42 34,48 34,54 35,00 35,06 35,12 35,18 35,24 35,30
rll»:U980780 41-662 Aoy:15-APS-1998 20,48,51 CC XI+ Volt*?* SIX 70S Hoif»>1133
425.7737 T:4 BSUB(256,30, -3.0) PKV(7, 5,3,0.10\,4532.0,1. 00\,r,T) XzptHDBSUS
TRIANGLE LABS TmitiTLI H23 BLANK TLIH5399
1003,
80.
60.
40.
201
AS.12X4
1. 8X4
.1.5X4
34,12 34,18 34:24 34:30 34:36 34:42 34,48 34:54 35:00 35:06 35,12 35:18 35:24 35:30
rile:U980780 tl-662 AcqilS-APX-1998 20,48:51 CC EI+ Voltmyf SIX 70S Noise,4602
435.8169 P:4 BSUB(256,30,-3.0) PKD(7,5,3,0.10\,18408.0,1,00\,f,T) Exp:NDBSOS
TRIANGLE LABS TextilLI H23 BLANK TLH45399
100* AS.19X7
BO:
eo:
40.
4-0.010
Tim,
20.
O.OEO
34': 12 34', 18 34', 24 34', 30 34': 36 34': 42 34:48 34:54 35': 00 35:06 35:12 35:18 35:24 35:30 Tim
.1.8E7
-1.3E7
.8.9X6
.4.5E6
Tile:U980780 tl-662 AcgilS-APK-1998 20:48:51 CC EI+ Voltage SIS 70S Koitf.3339
437.8140 T:4 BSW>(256,30, -3.0) PKD(7, 5,3, 0.10%, 13356.0,1.00\,r,T) ErpiHDBSOS
TRIANGLE LABS TeJCt.-IXJ H23 SLANT TLH45399
10Q\ A8.19E7
80J
tfo:
40.
20.
34:12 34:18 34:24 34:30 34:36 34:42 34:48 34:54 35,00 35:06 35:12 35:18 35:24 35,30
ril»:U980780 tl-662 Aoq:15-APS-1998 20:48:51 CC XI+ Volt*?* SIX 70S
430.9729 T,4 ExpiNDBSUS
TEIAWCLJE LABS T*xt:TLI M23 BLANK TLH45399
34il6 _ A . ,^.,r 34$50 -- - tc.tt -_ ^1.717
.2.2X7
.1.8X7
.1.3X7
'.8.9X6
.4.4X6
.0.0X0
Tim
80.
60.
40.
20.
0.
35115
35128
34:12 34:18 34:24 34,30 34:36 34,42 34,48 34\54 35,00 35:06 35:12 35:18 35:24 35:30
.1.3X7
-1. 0X7
'.6.6X6
.3.3X6
.0.0X0
Mm
-------
CD
-------
.1«>C79007B0 tl-663 Acqsl5-Qf*-1998 20:49:51 GC EI+ VoltMffU SI* 70S
57.7377 f>4 tSU*(256, 30,-3.0) fXD{7, 5,3, 0.10\,4844.0,1.00\,r,T) Xip:ltDB5US
TRIANGLE LASS TmxtiTLX M33 BLAST TLI«4S399
00\ Al. 72X5
80:
60.
40.
20.
38,12 38il8 38:24 38:30 38t36 38:42
lla:0980780 il-662 Aeqtl5-AfX-1998 20:48:51 CC XI+ Voltage SIX 70S Koif1:556
59.7348 rt4 3SUS(2S6,30,-3.0) PKD(7, 5,3,0.10\,2224.0,1.00\,f,T) XxptHDBSaS
XXIANGLX LASS TmxtiTLI H23 SLANT TLH45399
004 A2.00E5
80.
60.
40.
20.
38i48
5.3X4
4.3X4
3.2X4
2.1X4
.1.1X4
.0.0X0
Tim,
.5.1X4
.4.1X4
.3.1X4
.2.1E4
.1. 0X4
0.0X0
38:12 38:18 38:24 38:30 38:36 38:42
file>(7980780 tl-662 Adjil5-AfS-1998 20:48:51 SC El* Voltage SIR 70S Koia»sl263
69.7779 Ts4 BSO3(256, 30, -3 . 0) PKD(7,5,3, 0.10\, 5052. 0,1.00%, JT, T) ExptUDSSUS
TXTANSLS LABS T*xt:TLI M23 BLANK TLH4S399
1001 Al.
so:
60.
40.
20:
38:48
38:12 38:18 38:24 38:30 38:36 38:42
Til»:U9B07aO tl-662 Acq:1S-APR-1998 20:48:51 GC XI+ Voltage SIX 70S HoiffsSOS
471.7750 T:4 BSUB(256, 30, -3 . 0) PKD(7, 5,3, 0 .10\,2020. 0,1.00%, r, T) ExpiKDBSCfS
TXIANGLE LABS Text:TLI M23 BLANK TLI#45399
1001 Al.
38,48
38,18 . 38:24 38:30 38':36 38:42
Ml»tV980780 tl-662 AcqtlS-AfX-1998 20:48:51 GC EI+ Voltage SIR 70S
430.9729 F:4 Exp:NDB5US
TXIANGLX LABS T*xt:TLI M23 BLANK TLI945399
38:48
so:
60.
40.
20.
2.0X7
1. 6X7
1.2X7
.8.2X6
.4.1X6
.0.0X0
Tim
2.3X7
1.9X7
1.4X7
19.3X6
4.7E6
0.0X0
Tim
.1. 6X7
.1.3X7
.9.7X6
'.6.3X6
.3.2X6
0.0X0
38 12
38:18
38:24
38:30
38:36
38142
38:48
-------
a
a
Peak Locate Examination:15-APR-1998:20:47 File:U980780
Experiment:NDB5US Function:2 Reference:PFK
-------
TLI Project- 45399 Method 23 TCDD/TCDF Analysis (DB-225)
Client Sample: TLI M23 Blank Analysis File: P981305
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
" *~
_•»•••_•••••-•• «»^ ™
| Analytes
r012.002/Lime Kiln
XAD
TLI Blank
1.000
n/a
DB-225
•;•.'• Amt. (n
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
rvoS«t-:
/ /
04/03/98
04/16/98
n/a
U980780
BJG
;-*«*:K»
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
«i*^;:;;x%
SPC2NF04
PF24098
P981302
n/a
n/a
n/a
'j^flT''--: '• ';-: Ffeioft
2,3,7,8-TCDF
Internal Standard
,^—^—».^^—«^^—^«^-—•p~—~^~^™
'3C,:-2,3,7,8-TCDF
Recovery Standard
»C,2-1,2,3,4-TCDD
ND
0.005
Amt. (ng)
2.8
40%-130%
0.75
22:23
0.78
21:17
Ffegs
Data Reviewer
04/2(V98
Page 1 of 1
Triangle Laboratories, Inc.*
801 CapKola Drive • Durham. North Carolina 27713
DKona- /Q1 Q\ K.AA-KT3O • Cav /Q1 ON
CaVJ'SR T2XU. LARS 6.U X
Printed: 21:27 04/20/9
-------
Data Review By:
Calculated Noise Area: 0.13
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/20/98
Listing of P981305B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why . .RT. OX Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
304-306
0.65-0.89
DC NL 0:00 RO 1.00
0 Peaks
0.14
0.00
0.790-1.102
0.000
13C12-TCDF
316-318
316-318
13C12-TCDD
332-334
332-334
DC
DC
DC
DC
DC
NL 0:
WL 20:
WL 21:
22:
SN 23:
WH 24:
0.
00 RO
58
14
23
02 RO
25
65-
1.
0.
0.
0.
1.
0.
0.89
13
88
75
75
40
87
1 Peak
- M
DC
NL 0
19
21
21
22
0
:00 RO
: 54 RO
:00
.65-0.39
1.
1.
0
22
04
.78
: 17 0.78
:00
0
.75
4 Peaks
0.14
0.81
2.19
257.47 110.10
0.27
2.62
257.47
Above: TCDF / TCDD Follows -
0.16
0.42
181.15
276.72
1.45
459.74
0.25
79.63
121.27
0.62
0.955-1.045
0.000
0.937
0.949
147.37 1.000 13C12-2378-TCDF ISO
1.029
1.091
0.905-1.095
0.000
0.24 0.948
101.52 1.000 13C12-2378-TCDD IS1
155.45 1.013 13C12-1234-TCDD RSI
0.83 1.048
Column Description "Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es) WL-Below Retention Time Window A-Peak Added
..RT. -Retention Time (mm:ss) WH-Above Retention Time Window K-Peak Kept
Rat.l -Ratio of M/M+2 Ions SN-Below Signal to Koise Level D-P«ak Deleted
OK -RO=Ratio Outside Limits
-------
File:P981305 #1-1006 Acq: 16-APS-1998 15:42:39 EI+ VoltMfff SIM
303.9016 Exp:DB225
70P
TRIANGLE LASS Text .-HI H23 BLANK TLI §45399
1003
95l
90l
as'-
801
75l
70l
65'
601
551
501
45l
40l
35l
301
2Sl
20l
15\
101
Si
ol
22
31 : 59
I 21:21 •},.'•»»
i A. /A it A I , I i
I rN Km\A iU
IT INI^V \\w
»' ny i
V
}Jl. v<>-
22:09
\
Ll 1 1
fVl
V r KJ
24
22
\
J
Mn
V i
VK .»Tf- ;?.»>
Mu
•34 33
,
i in
n
i Wr
Vff(fef<
21 bo' 21\'l2 '21\24 ' 21:36' 2l':48 22:00 22': 12 22\24 ' 22\ 36 22
23,14
1
•49 1 33
** 33:07 \
\ \ 1
1 1 1
L rtl iJi
\M\ P
WW y
pi n
1 i '
-.»
:38
23:53
!)
1
': 48 23 \ 00 23 ': 12 23 s 24
|
fL23:44 (1 1 I/I
mWfl^
ly|i ' '
1
9.1E2
.8.7E2
.8.2E2
7.8E2
.7.3E2
.6.8E2
.6.4E2
9 or?
.5.5E2
.5.0E2
.4.6E2
.4.1E2
.3.6E2
-3.2E2
.2. 7E2
-2.3E2
'.1 . 8E2
-.1 . 4E2
•-9.1E1
'-.4.6E1
'• 0 . OEO
2J ': 36 ' 23 '• 48 24 • 00 Time
File:P981305 #1-1006 Acq:16-APR-1998 15:42:39 EI+ Voltage SIR 70?
315.9419 Exp:DB225
TRIANGLE LABS Tart.-IXI M23 BLANK TLI#45399
100^
95.
90\
851
ao-
75.
70.
65.
60.
55.
50.
45.
40.
35.
30
35
30
IS
10
5
0
--
., .
.r
-^~^^
21:00 21:12 31t34 21\36 2 1^4 8
22:23
,
j \
J \^_
32': 00 '32\'l2 22t34 '32:36 3
2>4t 23tbb 23112 23i
24
2.5E5
-2.4E5
-2.2E5
:2.1E5
'.2.0E5
-1.9E5
'.1 . 7E5
.1 . 6E5
Ll . 5E5
.1 . 4E5
-1.2E5
.1 . 1ES
.1 . OE5
.B.7E4
.7.SE4
.6.2E4
.5.0E4
.3 . 7E4
.2.SE4
.1.2X4
33': 3 6 33': 4 8 24 00 Tim
-------
18:00 19:00 20:00 21:00 22,00 23:00
rile:P961305 tl-1006 Ac 00
18:00 19:00 - 20:00 21:00 22:00 23:00
'ile:P9B1305 #1-1006 Acq:16-APS-1998 15:42:39 EI+ Voltage SIR 70P Noise:47
315.9419 BSDB(256f30,-3.0) PKX>(5, 3, 1, 0.10\,188. 0, 0. 00%, F,F) Elp:DB225
TRIANGLE LABS Teit-.TLI M23 BLANK TLH45399
1004
BO:
eo:
40:
201
24 : 00
IB:00 19:00 20:00 21:00 22:00 23:00
F±le:P9B1305 #1-1006 Acqrl6-APR-1998 15:42:39 EI+ Voltage SIS 70P Noiae:42
317.9389 BSUB(256,30,-3.0) PKD(5, 3,1, 0.10%, 168. 0, 0 . 00*, f, T) Exp:DB225
TRIANGLE LABS T&xf.TLI H23 BLANK TLI#45399
1001 A1.47E6
80J
60J
401
201
0.
24:00
18:00 19:00 , • 20:00 21:00 22:00 23:00
File:P981305 tl-1006 Acq:16-APR-1998 15:42:39 EI+ Voltage SIX 70P
375.8364 Exp:DB225
TRIANGLE LABS Text:TLI M23 SLANT TLH45399
24:00
O.OEO
25:00 Time
0 . OEO
2S\00 Tim,
J.2.5ES
-2.0E5
.1.5E5
-9.9E4
'.5.0E4
.O.OEO
25': 00 Tim
..3.3E5
.2.6E5
.2.0E5
.1.3E5
.6.6E4
.O.OEO
25:00 Tim
18:00
15:00
20:00
ai> oo
22 tOO
23 tOO
24100
0*0
25:00 Tim
-------
'ilf:P9813O5 91-1006 Aoq:16-APR-1998 15:42:39 Sir Voltfy* SIX 7OP lfoif*:10
19.8965 BSOB(256,30,-3.0) PKD( 5,3,1,0.10\,160.0,0.00\,F,F) Xxp:DB225
TXIAKSLE LASS TaxtsTLI M23 BLANK TLH45399
001
19:00 30 i 00 21:00 22:00 23:00
ile:P981305 01-1006 Acq: 16-APK-1998 15:43i3S EI+ Voltay* SIS TOP tioi*e:34
21.8936 BSUB(256,30,-3.0) PKD( 5 , 3, 1 , 0 . 10\, 136 .0,0 .00\,F,F) Exp:DB225
TRIANGLE LABS TextiTLI M23 BLAST TLHH5399
003, „„« no A325.27
A41S.70
40:
20L
19:00 20:00 2l':00 22:00 23:00
File:P981305 #1-1006 Acq:16-APS-1998 15:42:39 EI+ Voltage SIS 70P Koiae:47
27.8847 BSUB(256,30,-3.0) PKD(5,3,1,0,10\,188.0,0.00\,F,r> Exp:DB225
TRIANGLE LABS Text:TLI M23 BLANK TLI#45399
10 01 A1.75E6
801
so:
40:
20:
24:00
24 : 00
r4.3E5
'.3.5E5
'.2.6E5
.1. 7E5
.8.7E4
19:00 20:00 21:00 22:00 23:00
rile:P981305 #1-1006 Acqil6-APS-1998 15:42:39 EI+ Voltage SIR 70P Noise:54
331.9368 BSUB(256,30,-3.0) PKD(5,3,1,0.10\,216.0,0.00\,F,F) Elp:DS225
TRIANGLE LABS Text-.TLI H23 SLANT TLI*45399
lOOi, A1.21E6
24 : 00
.0. OEO
Time
80J
60:
401
20.
A7.96E5
2.9E5
.2.3E5
'.1. 8E5
-1.2E5
.S.9E4
19:00 20:00 21:00 22:00 23:00
riletP981305 tl-1006 Acqrl6-APR-1998 15>42t39 EI+ Voltage SIR 70P Koi*»:43
333.9338 BSUB(256,30,-3.0) PXD(5,3rl,0.10\,172.0,0.00\,T,r) EJCp:DB225
TRIANGLE LABS Tart.-TLJ H23 BLANK TLH45399
1001 A1.S5E6
24:00
.O.OEO
Tim
80.
60.
40.
20.
Al.02X6
19:00
20,: 00
2ltOO
22:00
23:00
24100
.3. 7E5
'-3.0E5
.2.2E5
.1.5E5
'.7.4X4
0.0X0
Tim
-------
rile:P981305 #1-1006 Acq: 16-APS-199S 15:42:39 EH-
303.9016 Exp:DB225
TRIANGLE LABS Text .-Til H23 BLAKK TLI445399
100*
80: ,
60:
40:
20:
o-
18:52 lg.3620:01
7:54 I II 1 j 30:59
^^^^
r " if M »Vy ^ > ^* r^sTT ~ T^ luM Vv*U rV^r "T^a
18:00 ' ' ' 19:00 20100 21:00
Voltage SIX 70P
, rn22:24 ...4
21-381l IL "{""i14. 23:53 24:28
^ji • jo i i n t 1 j hi I 11 tti
lAAJi^* AjAi/vvf Ui ..L/w/l flkilk j^lAwWLV**Wi/
ivjr«vv^M|fTiFU Vr'|\^Ui>'WVr T»I"W"Vw v^vyv v»>vf
.9.412
.7.5E2
.5 . 6E2
.3.7E2
.1.9E2
O.OEO
22:00 23 loo ' 24:00 ' ' 25:00 Ti«e
rile.-PS81305 #1-1006 Aoq:16-APS-1998 15:42:39 EI+ Voltage SIS 70P
315.9419 Exp:DB22S
TRIANGLE LASS Text: TLI H23 BLANK TLI #45399
100J
80:
60:
40:
20:
c:
18:00 19.' 00 20 .-00 ' 2ll-00
22:23 2.5E5
J \
.2.0E5
.1.5E5
.l.OES
.5.0E4
• 0 . OEO
22:00 2.3 : CO 24:00 25:00 Tijne
File; ;P9 813 05 #1-1006 Acg:16-APJ?-1998 15:42:39 EI+ Voltage SIX 70P
319.8965 Exp:DB225
TRIANGLE LABS Text: TLI H23 BLANK IXI#45399
1004 17:59 __ -,„.„.:
so:
60:
40:
20:
o:
^:57 19 3e 20:20 — ;" ,
V^M\j\Mvvki J'JVwwAV'yljiWixL JiJli/Wi. \i**(\\ (L
rt "y-^ ' i M'r^'V yW^'V^ «'*YtySflih/y|fTAw/fl*'^V uu V\
18. -00 15 1-00 20. -00 ' 21:00
24:25 8.8E2
1:2421-49 32'24 23:2i 34l01 /111
M!M - i it JLii/lii/U Lli j MlOl^ AMJli«*/^iuUJLir vtJU(\»W
nVw^.U^Vn*y W r\j^/AiiV|T^^ i"vy*"
•-7.1E2
'-5.3E2
.3.5E2
Ll . 8E2
; 0 . OEO
22.- 00 23.' 00 24 !• 00 ' 25.' 00 riffle
File:P981305 #1-1006 Aciy.-16-APX-1998 15.-42.-39 EI+ Voltage SIR 70?
331.9368 Exp:DB225
TRIANGLE LASS Text: TLI H23 BLANK TLI #45399
1005
80J
50:
40.
20.
D
21
21:00
ft
JU
18.' 00 19.' 00 20ioO 21 .' 00
17 2.9E5
L
I.2.3E5
•
Ll . 8E5
:i.2E5
L5.9E4
22 .-00 23 1-00 241-00 25:00 Tiae
File:P981305 #1-1006 Ac
-------
fl;P981385
Ref, lass 292,9825 Peak top
Height .87 volts Span 288 ppi
Systei file roe
Dka file naie
Resolution
Group number
lonlzatlon
Switching
Ref, lasses 292.9625,
A 292.9825
8 383.9816
D 315.9419
E 317.9389
F 319.8965
6 321.8936
H 327.8847
I 338.9792
J
K
L
H
1
El*
VOLTAGE
388.9761
338.9792
331.9368
333.9338
375.8364
Channel I 338,9792 Peak top
Height ,87 wits Span 288 ppi
-------
Pages 77 through 159 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project: 45399
Client Sample: M23-I-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: T981958
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-4A-D
1.000
n/a
DB-5
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
04/01/98
04/03/98
04/18/98
n/a
U980780
HLM
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
TT51308
T981946
n/a
n/a
n/a
Analytes
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
1,2,3,4,6,7,8,9-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
1,2,3,4,6,7,8,9-OCDF
Totals
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
. Amt. (ng)
ND
ND
ND
ND
ND
0.008
0.04
0.34
0.04
0.04
0.01
0.008
0.008
ND
0.007
ND
ND
Amt (ng)
0.02
FJvlPC
0.01
0.02
2.6
0.38
0.05
0.007
*V&^ jt^ r 7J-SMPC - Ballo
0.003
0.004
0.006
0.005
0.005
1.00
0.84
0.80
1.52
1.43
1.28
1.40
1.14
0.004
0.90
0.007
0.02
•Number ^^\..&^^J^^:^/:^^
2 0.04
0.003
2
2
14 2.6
10 0.46
5
1
fIT
36:49
40:23
25:26
29:25
30:07
32:52
32:58
33:27
35:49
^ii^V^v ;
Ffcg*
J_
JB_
J_
J_
J_
J_
J_
jZ
•rvfte^s.
—
_
Page 1 of 2
Mm.PSRvl.04. LARS 6.11.00
Triangle Laboratories, Inc.®
RD1 Canrtnla Drix/P • Hnrham Mnrth
Printer)-
rU/9O/QR
-------
- >•• '
Fadficfii
TLI Project: 45399
Client Sample: M23-I-4
internal Standards . •" V-;:^:: ,;,
13C,:-2,3,7,8-TCDF
13C,2-2,3,7,8-TCDD
13C,:-l,2,3,7,8-PeCDF
3C,:-l,2,3,7,8-PeCDD
13C,2-l,2,3,6,7,8-HxCDF
13Cp_-l,2,3,6,7,8-HxCDD
3C,2-l,2,3,4,6,7,8-HpCDF
13Cp.-l,2,3,4,6,7,8-HpCDD
13Cp-l,2,3,4,6,7,8,9-OCDD
Surrogate Standards (Type A)
13C,:-2,3,4,7,8-PeCDF
'3Cp-1.2,3,4,7,8-HxCDF
13C,2-l,2,3,4,7,8-HxCDD
13Cp-l,2,3,4,7,8,9-HpCDF
Other Standard
37CL,-2,3,7,8-TCDD
Alternate Standards (Type A>
3Cr_-l,2,3,7,8,9-HxCDF
13C,:-2,3,4,6,7,8-HxCDF
Recovery Standards
!3C,:-1,2,3,4-TCDD
"Cr.-l,2,3,l,S,9-HxCDD
Antf. :{hg)
2.4
2.1
2.5
2.8
2.9
2.8
2.6
2.7
3.2
Amt. (ng)
3.8
3.7
3.7
3.0
Arrrt. (ng)
3.6
Amt. (ng)
3.0
3.0
H§J<^4*&' iSjp
tWifdjlM6iu&
Method 23 PCDD/PCDF Analysis (a)
Analysis File: T981958
% Recovery
60.6
53.7
63.2
69.5
72.2
70.5
65.5
68.4
40.3
% Recovery
96.0
92.2
93.2
76.0
% Recovery
88.9
% Recovery
76.1
75.6
".,:' •;.- - •'.... •• . -.v . .
QC Limits
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
QC Limits
40%- 130%
40%- 130%
40%- 130%
25%-130%
QC Limits
40%- 130%
QC Limits
40%- 130%
40%- 130%
.-.'xVy.vV -::. :
Rsdtki
0.75
0.81
1.45
1.51
0.50
1.22
0.43
1.02
0.86
Ralfo
1.46
0.50
1.21
0.42
Ratio
0.50
0.51
Ratio
0.81
i ?ft
Jeff-' - Flags ,, \
25:23
26:07
29:24
30:26
32:58
33:38
35:48
36:49
40:22
y-' ; fft '•'•"f/V-'i^fafgS.' ^
30:06
32:52
33:34
37:18
flT .: , Ftags
26:09
•;:i«TV.:V:: Flags};;
34:12
33:26
:<:vlfc.<;;2i;frags.::F
25:56
Data Reviewer
04/20/98
Page 2 of2
MmJ>SR T! M. LAKS 6.11 X»
Triangle Laboratories, Inc.®
801
•Durham Mnr»hr.at*\lina077fs
-------
Initial
..Oat*..
Data Review By:
Calculated Noise Area:
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
0.18
Page No.
04/20/98
Listing of T981958B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why . ,RT. OK Ratio Total . Area ... Area. Peak. 1. . Area . Peak . 2 . . Rel.RT Compound . Name .. ID.. Flags.
TCDF
304-306
DC
304-306
NL 0:
22:
22:
22:
23:
23:
24:
24:
24:
24:
25:
25:
25:
26:
26
27
0.
00 RO
09
41
56
20
39
04
21
39
:59
14
26
: 52
:04
:18 RO
:10
65-0.89
1.29
0.79
0.80
0.78
0.81
0.78
0.79
0.78
0.80
0.79
0.76
0.80
0,79
0.71
0.93
0.73
15 Peaks
0.868-1.077
0.
31.
15.
9.
113.
58.
54.
51.
42.
39.
18.
70.
24.
11.
2.
2.
546.
42
91
39
97
69
73
12
26
33
68
34
71
89
35
41
13
91
14.
6.
4.
50.
25.
23.
22.
18.
17.
7.
31.
10.
4.
1.
0.
04
85
38
76
69
82
54
81
49
93
46
95
73
27
90
17.
8.
5.
62.
33.
30.
28.
23.
22
10
39
13
6
1
1
87
54
59
.93
.04
.30
.72
.52
.19
.41
.25
.94
.62
.36
.23
0.
0.
0.
0.
0.
0.
0.
0,
0,
0
0
1
1
1
1
1
000
873
.894
,903
,919
,932
.948
.959
.971
.984
.994
.002 2378-TCDF
.019
.027
.036
.070
J
AN
J
J
13C12-TCDF
316-318
316-318
0.65-0.89
DC NL 0:00 RO 1.35
0.961-1.039
0.35
24:58
25:23
25:51
3 Peaks
0.89
0.75
0.86
iVin
2.55
676.36
3.27
682.18
\ro- Trnp / Trn
1.20
290.19
1.51
1.35 0.984
386.17 1.000
1.76 1.018
0.000
0.984
1.000 13C12-2378-TCDF ISO
TCDD
320-322
320-322
D
D
DC
DC
DC
DC
D
D
DC
NL
SN
SN
SN
SN
SN
SN
5
0
23
23
24
25
25
25
25
26
26
26
26
:00
:33
:56
:57
-.12
:23
:35
:58
:03
:09
:17
:29
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
65-
1.
0
0.
0,
0.
2
0
0
0
0
1
0
•0.89
,17
80
,48
.61
.24
.18
.31
.90
.95
.51
.05
.82
Peaks
0.
1.
0.
1.
0.
0,
0
0
0
0
0
0
5
,21
.73
.69
.70
.23
.30
.28
.53
.74
.85
.35
.93
.79
0.77
0.30
0.74
0.40
0.42
0.896-1.045
0.000
0.96 0.902
0.62 0.916
1.21 0.955
0.965
0.972
0.980
0.994
0.42 0.997
1.001 2378-TCDD
1.006
0.51 1.014
J
J
J
AN
Triangle Laboratories, Inc.® Analytical Services Division
Pj>nitfi!a Hriuo » nurfeam Nl/trth P.amlino 97713
-------
Page No. 2 Listing of T981958B.dbf
04/20/98 Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total .Area. .. Area. Peak. 1 .. Area . Peak . 2 . .
37C1-TCDD 0.
328 DC NL 0:00 0.13
24:46 2.29 2.29
26:09 428.41 428.41
26:32 2.38 2.38
328 3 Peaks 433.08
13C12-TCDD 0.65-0.89 0.
332-334
332-334
PeCDF
340-342
A
M
340-342
13C12-PeCDF
552-354
352-354
?eCDD
156-358
A
DC NL 0:
25:
26:
26:
00
56
07
28
RO 1.
0.
0.
0.
3 Peaks
DC NL 0:
DC WL 27:
27:
28:
28:
28:
28:
29:
29:
29:
29:
29:
29:
30:
30:
DC SN 30:
DC SN 30:
31:
00
13
24
24
33
42
52
02
07
19
25
34
42
07
14
28
33
05
1.32-
RO 0.
RO 0.
RO 1.
1.
1.
1 .
1.
RO 1.
1.
1.
1.
RO 1.
1.
1.
1.
RO 1.
1.
RO 1.
98
81
81
89
1
1.78
86
45
25
35
46
62
51
25
34
33
52
31
49
43
48
20
33
91
14 Peaks
0.83
753.51
463.61
7.87
,224.99
337.
206.
3.
.35
,91
.71
416.16
256.70
4.16
Rel.RT Conpound . Name . . ID..
924-1.076
0.000
0.948
1.001 37C1-TCDD CLS
1.016
924-1.076
0
0
1
1
.000
.993 13C12-1234-TCDD RSI
.000 13C12-2378-TCDD IS1
.013
Flags
•BAor\w w»»1 1 _..•«.
0.20
1.07
7.42
4.88
23.55
5.29
2.64
2.22
2.71
1.12
7.11
2.68
5.06
6.78
3.54
0.39
0.35
0.84
75.84
4.
2.
13.
3.
1.
1.
1.
0.
4.
1.
3.
3.
2.
0.
51
80
98
27
59
35
55
64
29
63
03
99
11
63
1.32-1.78
DC NL 0:
28:
29:
29:
30:
31:
00
30
24
40
06
03
RO 1.
1 .
1.
1.
1.
1.
5 Peaks
DC NL 0:
28:
DC SN 29:
00
37
08
1.32-
RO 1.
RO 0.
RO 0.
22
35
45
44
46
54
1
1.78
00
73
38
0.18
1.67
588.63
5.46
567.36
1-60
,164.72
0.18
0.31
0.16
0.
348.
3.
336.
0.
96
18
.22
.42
,97
0.
3.61
2.08
9.57
2.02
1.05
1.08
1.16
0.48
2.82
1.24
2.03
2.79
1.43
0.33
0.
0.71
240.45
2.24
230.94
0.63
926-1.063
0
0
0
0
0
0
0
0
0
0
1
1
1
1
1
1
1
1
864
0
0
1
1
1
1
.000
.926
.932
.966
.971
.976
.982
.988
.990
.997
.001 12378-PeCDF AN
.006
.010
.024 23478-PeCDF AN
.028
.036
.039
.057
-1.136
.000
.969
.000 13C12-PeCDF 123 IS2
.009
.024 13C12-P6CDF 234 SUR1
.056
J
J
J
J
J
J
J
J
J
J
J
J
J
-
0,
,19
0.
0.26
936-1.021
0
0
0
.000
.940
.957
J
iangle Laboratories, Inc.® Analytical Services Division
H Capitola Drive • Durham, North Carolina 27713
ir>rwa- fQ1 O\
Printed: 15:39 04/20/98
-------
Page No.
04/20/98
Listing of T981958B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak. 2. . Rel.RT Compound.Kane.. ID.. Flags.
0.965
0.970
0.976
0.984
0.990
1.001 12378-PeCDD
1.004
356-358
13Cl2-PeCDD
368-370
368-370
HxCDF
374-376
374-376
13C12-HXCDF
384-386
384-386
HxCDD
390-392
390-392
D SN
DC SN
DC SN
DC SN
D SN
D SN
DC SN
DC WH
1
DC NL
2
DC NL
DC SN
DC SN
DC SN
5
DC NL
8
DC NL
DC SN
DC SN
DC WH
2
29:22
29:31 RO
29:42
29:56
30:08
30:27 RO
30:34 RO
31:11 RO
Peak
1.:
0:00 RO
30:26
30:35
Peaks
1.
0:00 RO
31:54
32:03
32:12
32:21 RO
32:52
32:58
33:05
33:27
Peaks
0.
0:00 RO
31:53
32:02
32:52
32: 58
33:26
33:49 RO
33:55 RO
34:12
Peaks
1
0:00 RO
32:52
33:03
33:58 RO
34:01 RO
34:12 RO
! Peaks
1.59
1.26
1.77
1.40
1.48
1.16
1.18
6.33
32-1.78
1.25
1.51
1.44
05-1.43
1.00
1.10
1.07
1.37
1.00
1.28
1.40
1.35
1.14
43-0.59
1.09
0.51
0.57
0.50
0.50
0.51
0.33
0.66
0.50
.05-1.43
0.90
1.32
1.42
0.61
0.27
0.64
0,75
0.39
0.36
0.48
0.82
0.61
0.21
0.08
0.31
0.16
358.85
36.59
395.44
0.38
0.63
2.21
0.45
0.31
1.55
1.20
0.40
0.90
6.49
0.17
3.36
2.16
426.02
480.37
474.12
1.10
1.12
370.48
1,758.73
0.33
0.58
0.46
0.31
0.07
0.38
1.04
AN
1.025
215.94
21.61
Follows
0.33
1.14
0.87
0.70
0.48
1.14
0.78
141.90
160.93
160.01
0.37
0.49
123.09
Follows
0.33
0.27
0.869-1.131
0.000
142.91 1.000 13C12-P6CDD 123 IS3
14.98 1.005
0.963-1.045
0.000
0.30 0.968
1.07 0.972
0.977
0.981
0.68 0.997 123478-HXCDF AN
0.50 1.000 123678-HXCDF AN
1.004
0.42 1.015 234678-HxCDF AN
J
J
0.879-1.121
0.000
2.22 0.967
1.38 0.972
284.12 0.997 13C12-HXCDF 478 SUR2
319.44 1.000 13C12-HXCDF 678 IS4
314.11 1.014 13C12-HXCDF 234 ALT2
1.11 1.026
0.74 1.029
247.39 1.037 13C12-HXCDF 789 ALT1
0.25
0.19
0.958-1.013
0.000
0.977
0.983
1.010 123789-HxCDD
1.011
1.017
AN
Triangle Laboratories, Inc.® Analytical Services Division
1 K'
-------
Page No .
04/20/98
Listing of T981958B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z .... QC . Log Omi t Why
HpCDF
408-410
M
408-410
13C12-HpCDF
418-420
418-420
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
OCDF
442-444
442-444
OCDD
458-460
.RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2. . Rel.RT Compound.Name.. ID.. Flags.
.998 13C12-HXCDD 478 SUR3
.000 13C12-HXCDD 678 IS5
.009 13C12-HXCDD 789 RS2
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
1.05-1.43
NL 0:00 RO 0.77
33:03 RO 0.70
33:34 1.21
33:38 1.22
33:56 1.20
34:22 RO 0.82
34:25 RO 0.50
6 Peaks
0.88-1 .20
NL 0:00 1.09
35:49 0.90
1 Peak
0.37-0.51
NL 0:00 RO 1.15
35:48 0.43
SN 36:13 RO 0.17
37:18 0.42
2 Peaks
0.88-1.20
NL 0:00 RO 1.50
36:05 0.90
36:49 1.00
2 Peaks
0.88-1.20
NL 0:00 1.13
36:49 1.02
37:14 RO 0.86
2 Peaks
0.76-1 .02
NL 0:00 0.82
WL 35:41 RO 0.50
WL 35:57 RO 1.67
WL 36:02 RO 0.57
SN 40:35 RO 1.37
0 Peaks
0.76-1.02
NL 0:00 1.00
40:02 RO 0.23
40:23 0.84
0.36
0.90
280.38
359.75
506.53
0.96
0.89
1,149.41
0.23
0.59
0.59
0.19
245.39
0.49
134.79
380.18
WTI("" pip /
rlpt_ LJr 1
0.16
0.55
0.40
0.95
0.32
210.51
0.61
211.12
0.20
0.13
0.11
0.08
0.36
0.00
0.20
1.44
1.03
0.28
73.79
40.11
Follows
0.26
0.20
106.11
0.31
0.996-1.047
0.000
0.31 1.000 1234678-HpCDF
AN
0.944-1.112
0.000
171.60 1.000 13C12-HpCDF 678 IS6
1.012
94.68 1.042 13C12-HpCDF 789 SUR4
0.976-1.005
0.000
0.29 0.980 J
0.20 1.000 1234673-HpCDD AN' J
0.973-1.027
0.000
104.40 1.000 13C12-HpCDD 678 IS7
0.36 1.011
Follows
0.68
0.47
0.901-1.099
0.000
0.884
0.891
0.893
1.005 OCDF-
0.901-1.099
0.000
2.90 0.992
0.56 1.000 OCDD
AN
AN
Triangle Laboratories, Inc.® Analytical Services Division
301 Capitola Drive • Durham, North Carolina 27713
-------
Page No. 5 Listing of T981958B.dbf
04/20/98 Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.PeaX.1.. Area.Peak.2.. Rel.RT Confound.Name.. ID.. Flags.
458-460 2 Peaks 2.47
13C12-OCDD 0.76-1.02 0.996-1.004
470-472 DC NL 0:00 RO 1.10 0.19 0.000
40:22 0.86 167.16 77.42 89.74 1.000 13C12-OCDD IS8
DC WH 40:46 RO 0.44 0.64 1.010
470-472 1 Peak 167.16
Column Description "Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es) WL-Below Retention Time Window A-Peak Added
..RT. -Retention Time (mm:ss) WH-Above Retention Time Window K-Peak Kept
Rat.1 -Ratio of M/M+2 Ions SN-Below Signal to Noise Level D-Peak Deleted
OK -RO=Ratio Outside Limits
-------
File:T98195B #1-720 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR
303.9016 F:2 BSVB(256,30,
TRIANGLE LABS Text:M23-I
1001
SOJ
•
60J
I
401
201
0'
AS.
A A6.85E4
A yv/v_ J
23:00'
70T Noise: 156
-3.0) PKD(9,5,5,0.05\,624.0,1.00l,FeT) Exp:KDB5US
-4 TLI#45399
OSES
ft
A2.25E5
A2.38E5 A
A A \
lA A JTr
241-00
IKT. TIKE - 06s 59
AJ.
Al . 75F5
A]
-A/
25:00
File:T981958 #1-720 Acq -.IB-APR- 199 8 06:59:26 EI+ Voltage SIR
305.8987 F:2 BSUB(256,30,
15E5
f\
\ A1.10E5
A 4 . 73E4
/\ ~ -
.1 . OES
18.0E4
'-.6.0E4
'.4.0E4
.2. or 4
O.OEO
26:00 27.' 00 Time
70T Noise: 118
-3.0) PTD(9,5,5,0.05\,472.0r1.00\,F,T) Exp:NDBSas
TRIANGLE LABS Teit:M23-I-4 TLI#45399
1003
aoj
;
60J
•
40:
•
2ol
0'
A6.
AA8.54E4
/Vvv J
'iJ-Oo'
29E5
ft
A2.87E5
A3.30E5A3.03E5 A
A A /
CA A A-
24-00
XKT. TTME - 05:55
r 1 . 3E5
A3 . 53Z5
A2.22r5
i
/
25 1-00
File:T981958 #1-720 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR
315.9419 F:2 BSUB<256,30,
-3.0; PKDf9, 5, 5,0.054,
TRIANGLE LABS Teit:M23-I-4 TLIH45399
1004
8CJ
6CJ
401
201
ol
23!- oo
24:00
\
\ Al . 39E5
\ /\!6.62Z4
V 7V /\ ^ _
_1 . OE5
-7.6E4
-5.0E4
-2.5E4
O.OEO
26:00 27:00 ' Tiae
70T Noise: 137
548. 0,1. 00%, F, T) Exp:NDB5US
INJ. TIME = 06:59
"1
;
25.' Ofl'
File:T981958 #1-720 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR
317.9389 F:2 BSUB(256,30,
-3.0) PKD(9,5,5,O.OS\,
TRIANGLE LABS Text:M23-I-4 TLI#45399
1004
80 1
601
401
201
o"
23 .-00
24 .-00
396. 0,1. 00%, F
!E6 7.4E5
L5.5E5
-4.5E5
.3 . OE5
-1.5E5
0 . OEO
,
26:00 27:00 Ti«e
70T Noise: 99
,T) Exp:NDB5US
INJ. TIME = 06:59
A3.
1
25:00'
File:T98195S #1-720 Acq: 1B-APR-1998 06:59:26 EI+ Voltage SIR
330.9792 F:2 Exp-.tfDBSVS
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
80.
60.
40.
20.
0.
22 ; 3 J 23 1 00
2jT00
23:35 24:3
241-00
025:02^
'25\00
File:T98195B #1-720 Acq: IB-APR- 1998 06:59:26 EI+ Voltage SIR
375.8364 Fi2 Elp:NDB5US
i
TRIANGLE LABS Text:H23-I.-4 TLI #45399
1003
80.
60.
40.
20.
0.
22 143 I-JL?*"
/1A ^. y\* '\A, yU'U I A
v\F"^ v v
23:00
16E6 1.0E6
V
.8. OES
-6.0E5
-4. OES
.2. OES
O.OEO
'261-00 27.' 00' ' ' ' Tiae
70T
INJ. TIME = 06. -5P
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"
.1.2E6
.9.1E5
.6. OES
.3. OES
• o . OEO
'26:00 27.' 00 ' ' ' Tiae
70T
INJ. TIME - 06:59
t 25r-25 _!.»«?
24
2J.-25
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26:00 27:00 Time
-------
ile.-T98.l958 #1-720 Acq: 1B-APR-199B 06:59:26 EI+ Voltage SIX 70T Jfoi«ei71
19.8965 F:2 BSOB(256,30,-3.0) PKD(7, 5,3,0.05\,284.0,1.00\,r,T) KxpiBDBSUS
TRIANGLE LABS Text:M23-I-4 TLH4S399 IJKT. TIME - 06:59
001
80:
60J
40:
A7.41E3
A2.991.3
A3.70E3
1.97E3 A4.15E3
^
C2.3E3
.1. 9E3
.1.4E3
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.4.6E2
24:00 25:00 26:00 27:00
rile.-T981958 #1-720 Acg.-18-APJ?-1998 06:59:26 EI+ Voltage SIX 70T Noime:59
21.8936 F:2 BSUB(2S6,30,-3.0) PKD(7,5,3, 0.05\,236.0,1.00\,F,T) Efp-.KDBSUS ,d
TRIANGLE LABS Tert:M23-I-4 TLI#45399 JWT. TIME - 06:59 '
001 - :
24:00 25:00 26:00
File:T98195S #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noise:465
31.9368 T:2 BSUB(256,30, -3.0) PKD( 7, 5, 3, 0 . 05%, 1860 . 0,1. 00%, F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME * 06:
1001 A3.37E6
27.- 00
59
80.
60.
40.
20.
2.07E6
I V
24:00 25:00 26:00 27:00
rile.-TSSlSSS #1-720 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noiae:236
333.9338 T: 2 BSUB{ 256, 30,.-3 .0 ) PKD( 7, 5, 3, 0 . 05%,944 . 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME ' 06:59
1001 A4.16E6
80:
60:
40:
20:
0:
2.57E6
24:00 25:00 26:00 27:00
file:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR TOT Koiae:67
327.8847 F:2 BSUB( 256, 30, -3 . 0) PKD( 7, 5, 3, 0 . 05t,268 . 0, 1. 00\,F, T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399 JKT. TIME * 06:59
1001 A4.28E6
80:
60:
40:
20:
0:
24:00 25:00 26:00
JTile:T981958 *1-720 Acg:lfl-APJ!-1998 06:59:26 EH- Voltage SIX 70T
330.9792 JT.-2 Exp:NDB5DS
TRIANGLE LABS Text:M23-I-4 TLI#45399 IKT. TIME
27:00
1001
80:
60:
40:
20:
o:
23:36
24:02
24:30
06:59
S.-J2 26; 54
Time
1 ,- •)/ , «/
I(- ''"'V -x T
_9.4rs
L7.5E5
L5.6E5
-3 . 8E5
.1.9E5
O.OEO
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1.2E6
9.3E5
7. OE5
4.7E5
.2.3E5
O.OEO
Time
.1.2E6
.9.4E5
.7.0E5
.4.7E5
.2.3E5
.O.OEO
Tim,
.1.5E6
.1.2E6
.9.1E5
.6.0E5
.3.015
24:00
25s 00
26:00
27:00
o.oro
Ti*e
-------
File:T981958 #1-720 AcqslS-APR-1998 06:59:26 XI+ Voltage SIR 701 KOiae>60
339.8597 F:2 BSUB(256, 30, -3. 0) PXD( 7,5,3, 0. OS\,240.
TRIANGLE LABS Text:M23-I-4 TLI#4S399
1004 A1.40E5
•
ao:
60:
40:
•
20:
0:
/
AS.
A j
A A, / I A A1.3SE4 I
A /V \J\ ^-yw J
28:00 29:00
0,1.00%,^, T) Exp:NDB5US
XJTJ. TIME « 06:59
3 . 5E4
04E4
ft A3.99E4
\ A3.03E4 A
-2.8E4
-2.1E4
.1.4E4
-7.0E3
30:00 31:00 Time
File:T981958 #1-720 Acq -.18 -APR- 19 9 8 06:59:26 EI+ Voltage SIR 701 K>iae:68
341.8567 F:2 BSOB! 256, 30, -3 .0) PJO)f 7,5,3, 0. 05%,272.
TRIANGLE LABS Text:M23-I-4 TLI#45399
1001
aej
60:
40:
20:
0.
0,1.00\,F,T) Exp:m>S5US
IKJ. TIME ' 06:59
C2.SE4
AA3.42E4 A2.79E4
A1.08E4 \ A2.03E4 A
28^: 00 29: 00
-.2.0E4
-1.5E4
'.1.0E4
-5.0E3
• 0 . OF.O
30:00 31:00 Time
File:T981958 #1-720 Acq : 18-APR-1998 06:59:26 EI+ Voltage SIR 701 Noise:56
351.9000 F:2 BSDB<25'6, 30, -3 . 0) PKD( 7, 5, 3 , 0 . 051,224 .
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
80:
60:
40:
20:
0 '
0,1.00\,r,T) Exp-.NDBSUS
IlfJ. TIME = 06:59
A3.48E6 A3.36E6 1.1E6
j
28:00 29:00
ft
1 / V
-8.4E5
'-6.3E5
-4.2E5
-2.1E5
• 0 . OF.O
30 1-00 '31:00 ' ' Time
File:T981958 #1-720 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR 701 Noise:47
353.8970 F:2 BSUBI256, 30, -3 .0 ) PKD( 7, 5, 3, 0. 05*,18S.
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
80:
60:
40:
20:
ol
0,1.00%,r,r; Exp:NDB5US
INJ. TIME = 05:59
A2.40E6 A2.^1E6 ^7 . 3E5
1
28-00 29:00
I / V
'-5.8E5
'-4.4E5
-2.9E5
-1.5E5
O .OF.O
30.' 00 31:00 Time
FiIe:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIS 701
330.9792 F:2 Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
;
.
60:
40:
20:
0:
27:38 27:5528:09 • 28_j_31 28:55 29:10
28:00 291-00
INJ-. TIME = 06:59
29:33 29^5.230:08 30:4330:59 1 . 5E6
— \T~ '
.1.2E6
-9.2ES
•-6.1E5
-3.1E5
30:00 31:00 Tt»»
File:T98195B #1-720 Acq:18-APR-1998 06:59:26 £1+ Voltage SIR 701
409.7974 F:2 Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
80:,
60.
40:
20:
0:
i 28:59
1 r
A 2?:35 , 1 , i 29
^/ »J^ j f8,'06 A ,„ „. nflA^/
^\j^^^k^^ wvvl/
20:00 29:00
JWJ. TIME - 06:59
30:26 1.0E3
I .
I 1 31:12
I" 30.A 30{46 i
1 iii i ,AAJ»iill A UK J liJLj^U
l^^^^wvyifw vv^l/l^r1^ ^
•
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-6.2E2
-4.1E2
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1 1 1 | 1 1 1 1 1 1 | | | 1 - . wv
30:00 31:00 Time
-------
'ile:T981958 #1-720 Acq:18-APR-199B 06:59:26 EH- Voltage SIS 70T Hoiae:56
55.8546 F:2 BSUB(256,30, -3. 0) PKD(7,5,3, 0. 05\,224. 0,1. 00\,r,T) Exp-.HDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME - 06:59
28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 31:24
File:T981958 #1-720 Acq:18-APR-199S 06:59:26 EI+ Voltage SIX 70T Noiae:53
357.8516 F:2 BSUB(256, 30, -3 . 0) PKD(7,S,3, 0. 05\,212. 0, 1. 00\,F, T) Exp-.NDBSUS
TRIANGLE LABS Teit:M23-I-4 TLI#45399 IJW. TIME - 06:59
1004
001
so:
601
401
•20-
0.
A4.61E3
A3.75E3
VVN
Al.90E3
1.24E3
-1.2E3
-9.9E2
.7.4E2
-4.9E2
.2.5E2
O.OEO
Time
A2.01E3
A3.29E3
28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 31:24
File:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIX 70T Noiae:49
367.8949 F:2 BSUB(256, 30,-3. 0) PKE(7, 5,3, 0 . 05%, 196. 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME = 06:59
1004 A2-16E6
flOj
60:
40:
20:
2.16E5
.5.3E5
.3.9E5
.2. 6E5
11. 3E5
.O.OEO
28[:48 29^.00 29\12 29\24 29': 36 29\48 30\00 30\12 30': 24 30:36 30\48 31: 00 31:12 31': 24 Time
F±le:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noiae:42
369.8919 F:2 BSUB(256, 30, -3 . 0) PKD(7, 5,3, 0 . 05%, 168 . 0, 1. 00\,F, T) Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME - 06:59
1004 A1.43E6
SOJ
to:
20 L
-4.4E5
-3.SE5
'.2. 6E5
.1.7E5
.8.7E4
1.50ES
O.OEO
28:36' 28:48' 29:00 29:12 29:24' 29:36 29\48 30:00 30:12' 30':24 30:36 3o':48' 3l':00' 3l':12 3l':24 Time
File:T981958 #1-720 Acq:18-APR-1998 06:59:26 EH- Voltage SIR 70T
330.9792 T:2 ExptHSSSVS
TRIA
1003,
80.
60.
401
20.
0
NGLE LABS Teit:M23-I-4 TLH45399 INJ. TIME " 06:59
28:42 28:55 29:1029:21 29:33 29:52 30:0830:1830:29 30:43 30:59
^ V/ " ~~^
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1.5*6
-1.2E6
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28:36 28:48 29:00 39tl2. 29:24 29:36 29:48 30:00 30:12 30,24 30:36 30:48 31:00 31:12 31:34 Tim.
-------
rile:T9819S8 #1-425 Acq:18-APK-1998 06:59:26 EI+ Voltage SIX 70T NoiseilOS
73.8208 F:3 BSUBf256,30, -3. 0) PKD(7,5,3, 0. 05\,420. 0,1. 00\,F, T) Exp:JIDB5US
TRIANGLE LABS T6JCt:M23-I-4 TLI#45399 ZXJ. TIME ' 06:59
.1004 A1.}4E4
31 ':48' 32:bo' 32:12 ' 32:24 ' 32:36 ' 32: 48 ' 33:00 33:12 33:24
File:T981958 #1-425 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Soiae:104
375.8178 F:3 BSUB(256, 30,-3.0) PKD(7,5,3, 0. 05\,416. 0,1. 00\,F, T) Exp:ltDB5OS
TRIANGLE LABS Text:M23-I-4 TLI#45399 IJW. TIME - 06:5*
1004 A1.Q7E4
8 01
601
401
201
Ol
O.OEO
3424 3436 34 48 Tiae
31:48 32:00 32':12 32:24 32:36 32':48 33:00 33\12 33:24 33:36 33':48 34:00 34:12 34:24 34:36 34 48
F±le:T981958 #1-425 Acq:1B-APR-1998 06:59:26 EI+ Voltage SIR 70T Noise:62
383.8639 F:3 BSUBf 256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 051,248 . 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Tejct:M23-I-4 TLI#45399 INJ. TIME - 06:59
-O.OEO
Time
100*
401
Al . 61E6
50E6
A1.23E6
5.3E5
-4.3E5
:3.2E5
•.2.1E5
.1. 1E5
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:T981958 #1-425 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noise:S7
385.8610 F:3 BSUBf 256, 30, -3 . 0) PKDf 7, 5, 3, 0 . 05%, 228 . 0, 1. 00\,F, T) Exp-.NDBSUS
TRIANGLE LABS Tezt:M23-I-4 TLI#45399 INJ. TIKE = 06:59
1004 A3.19E6 A3.J.4E6
sol
34
:o. OEO
48 Time
601
401
201
Ol
A2.47E6
1. OE6
.8.3E5
.6.2E5
-4.1E5
.2.1E5
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36
File:T981958 #1-425 Acq: 18-APR-1998 06:59:26 EI+ Voltage SIR 70T
392.9760 F:3 Ezp-.NDBSVS
TRIANGLE LABS Text:H23-I-4 TLI#45399 IWJ. TIME » 05:59
100*. 31jS8 32:2132:3132:42 32:58 33:17 33.27 33.40 34:0034:12 34:27
801
601
401
201
Ol
34
.O.OEO
48 Time
-7.2E5
-5.SE5
.4.3E5
.2.9E5
.1.4E5
O.OEO
31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34:36 34 48 Time
File:T981958 #1-425 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T
445.7555 F:3 Ezp:mB5aS
TRIANGLE LABS Teit:H23-I-4 TLI#45399 INJ. TIME - 06:59
33:57
31-48 32so 32-.2 32i34 32:3632[:48' 33'tO 33il2
33\ 36 ' 33'i48 ' 34 1 00 ' 34:12' 34't24'
34s36
.O.OEO
34 48 Time
-------
------- OCR error (C:\Conversion\JobRoot\000004IG\tiff\2000EW0P.tif): Unspecified error
-------
423.7766 T:4 BSUB<256, 30, -3.0) PKD(7,5,3, 0.05\,248. 0,1. 00\,T, T) Exp:KDB5US
TRIANGLE LABS Tezt:M23-I-4 TLI#45399 INJ. TIKE - 06s59
100$ A2.8E3
A2.03E3
80J
36':00 36:06 36': 12 35:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00
F±le:T981958 #1-629 Acq:18-APR-1998 06:59:26 EI+ Voltage SIX 70T Noise:39
425.7737 F:4 BSUB(256, 30,-3 .0 ) PKD( 7, 5, 3, 0 . 05%, 156. 0, 1. 00%, T, T) Ezp:]tDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399 IKJ. TIME - 06:59
8.SE2
.6.8E2
.5.1E2
3.4E2
.1. 7E2
37:06 37:12 37:18
1001
80:
60J
40:
20:
o:
A2.93E3
A2. 2E3
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:T981958 #1-629 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noise:86
435.8169 F:4 BSVB<256, 30, -3 . 0) PKD(7, 5, 3, 0 . 05%, 344 . 0, 1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI445399 INJ. TIME = 06:59
1001 A1.06E6
so:
eo:
40:
201
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00
File:T981958 #1-629 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noise:75
437.8140 F:4 BSUB( 256, 30,-3.0 ) PKD(7, 5 , 3 , 0. 05\, 300 . 0 , 1.00\,F,T) Ejcp:JfDB5US
TRIANGLE LABS Text:M23-I-4 TLIH45399 INJ. TIME - 06:59
1003, A1.04E6
80.
60.
40.
20.
37:06 37:12 37:18
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:T981958 #1-629 Acq:18-APX-1998 06:59:26 EI+ Voltage SIR 70T
430.9729 F:4 Exp:NDB5OS
TRIANGLE LABS Tezt:M23-I-4 TLI#45399 INJ. TIME - 06:59
100A- 36_±01 36L06 . ^ 36:23 36:32 36:4036:46 36:58 37:10 37:17
80.
60.
40.
20.
0.
.8.0E2
.6.4E2
.4.8E2
.3.2E2
.1. 6E2
.O.OEO
Time
.2.6E5
.2.1E5
.1. 6ES
.1. OE5
.5.2E4
36:00 36:06 36:12 36:1» 36:24 36:30 36t36 36t42 36:46 36:54 37tOO 37s06 37:12 37:18
.2.5E5
.2.0E5
.1. 5E5
.1. OE5
.5.1E4
.O.OEO
Time
.4.9E5
.4.0E5
.3. OE5
.2.0E5
.9.9E4
.O.OEO
Time
-------
File:T981958 #1-629 Ac?:18-AP.R-1998 06:59:
441.7428 F:4 BSUB( 256, 30, -3 . 0 ) PKD(7,5,3,0
TRIANGLE LABS Tezt:H23-I-4 TLI#45399
1003
901
801
701
601
501
401
301
20.
10.
.
36:00 37.' 00 38.' 00
rile.-T981958 #1-629 Acq:l 8-APR-199S 06:59:
443.7399 F:4 BSUB(256, 30, -3 .0 ) PKD(7,5,3,0
TRIANGLE LABS Text:M23-I-4 TLI#45399
1001
901
801
701
601
501
401
301
201
101
36.- 00 37:00 3SiO£)
File:T981958 #1-629 Acq:18-APR-1998 06:59:
430.9729 F:4 Exp:NI>B5DS
TRIANGLE LABS Text:M23-I-4 TLI#45399
1003
901
a 01
701
601
501
401
30.
I^^*^*^^^^~\/v~M^^-J*^^^
20\
10J
36^00 371-00 38^00
File:T981958 #1-629 Acq:18-APR-1998 06:59:
513.6775 F:4 Exp-.NDBSOS
TRIANGLE LABS Tejct:M23-I-4 TLIH45399
1003
90.
601
7°~
60_
50.
40J
30J
201
101
01
35420 35:52 ,, ,0
3 1 36:52 37:39 t .
nWJV^\v'WVA^^^Ly<^^/4A«^^w'^^iM'Lv^^
36:00 371-00 3sToO
26 EI+ Voltage SIR 70T Noise :44
.051,176. 0,1.00\,F,T) ExpiSDBSOS
ZKJ. TIKE »
— ** r
39iob ' ' ' 40:00
26 EI+ Voltagre SIR 70T Hoiae:
06:59
p.2.1E4
.1 . 9E4
.1 . 7E4
il . 5E4
-1.3E4
.1.1E4
iB.5E3
.6.4E3
L4.3E3
.2.1E3
O.OEO
41:00 42:00 Time
53
.051, 212. 0,1. 001, F,T) Eip:lTDB5US
IJfJ. TIME *
39:00 40:00
26 EI+ Voltage SIR 70T
INJ. TIME *
38:28 39:35 40:03
39:00 40:00
26 El-*- Voltage SIR 70T
nrj. TIME •
06:59
1 . 6E4
.1 . 4E4
-1.3E4
.1 . 1E4
.9 . 6E3
-8.0E3
-6.4E3
-4.8E3
.3.2E3
.1 . 6E3
41:00 42:00 Time
06:59
2 41:29 42:30 p5.0E5
yfjf/^1- — J-'\*V^VJ n .Jr lf-lf^f^\n^.^r^
.4.5E5
-4.0E5
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- o . nrn
41:00 42:00 Tine
'
06:59
r4.2E3
41,43
•J*M*to«+&»*J~h**isJ<^
39:00 40; 00
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L3.4E3
-2.9E3
-2.5E3
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n /•••/)
41:00 42:00 Time
17!=;
-------
'ile:T9B195B #1-6SS Acq:lB-Aflt-199B 06:59:26 £1+ Voltage Six 70f Ooiae:4B
57.7377 T:4 BSUB(256,30, -3. 0) PKD( 7, 5, 3, 0. 05%, 192. 0,1.00\,F, T) Exp:tO)S5OS
TRIANGLE LABS Text:M23-I-4 TLHH5399 INJ. TIME - 06:59
1001 A4.69E3
40:18 40:24 40:30 40:36 40:42
rile:T981958 #1-629 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T Noiae:50
459.7348 F:4 BSUB( 256, 30,-3 .0 ) «CD(7, S, 3, 0. 05%,200. 0,1. 00*, T, T) Exp:NDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIKE - 06:55
1001 A5.61E3
so:
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20.
40:48
~T
~r
~r
40:18 40:24 40:30 40:36 40':42
File:T981958 #1-629 Acq:18-APK-1998 06:59:26 EH- Voltage SIS 70T Noise:57
469.7779 F:4 BSUB(256, 30,-3 . 0 ) PKD(7, 5, 3, 0 . 05%, 228 . 0,1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLI#45399 INJ. TIME = 06:59
1004 A7.74E5
80J
60J
40.
20.
40:48
40:18 40:24 40:30 40:36 40:42
File:T9B1958 #1-629 Acq: 1S-APR-1998 06:59:26 EI+ Voltage SIR 70T No±ae:49
471.7750 F:4 BSUB( 256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 196. 0, 1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:M23-I-4 TLIK45399 INJ. TIME = 06.-59
1001 A8<)7E5
eo:
eo;
40.
20:
40:48
40:18 40:24 40:30 40:36 40:42
rile:T98195a 01-629 Actj:18-AfR-1998 06:59:26 Eli- Voltage SIS 70T
430.9729 F:4 Exp-.NDBSUS
TRIANGLE LABS Text:M23-I-4 TLI#45399 ISJ. TIME -
40:48
06:59
1.3E3
1. 1E3
8.1E2
S.4E2
2. 7E2
O.OEO
Time
1.4E5
.1. 1E5
.8.6E4
.5.7E4
.2.9E4
.O.OEO
Time
.1. 7E5
.1.4E5
.1. OE5
.6.9E4
.3.4E4
.O.OEO
Time
OOJ
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60.
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30.
0
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fc
40.' Ifl 40:24 40i30 40ijfi 40.' 42 40:48
_4 . 7E5
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-1.9ES
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Time
-------
fl'T981948
Channel I 338,9792 Peak top
Height ,78 wits Span 288 ppi
Systea file nace
Data filename
Resolution
Group nuaber
lonization aode
Pitching
Ref, tasses 292,3825,
fl 233 J 331
K 332
L 334
I 348
N 342
0 352
P 354
9 356
R 358
B 384
386
D 316
E 318
F 328
G 322
H 328
I 331
I
El*
VOLTflGE
416,9768
S 368
T 378
U 376
V 418
tef.'iass 416,9768 Peak top
Height ,17volts Span 288ppi
t~l 1*1
-------
File:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T
339.8597 F:2 Exp:NDB5US
Sample Text:M23-I-4 TLI#45399 INJ. TIME = 06:59 File Text:M23-I-
100% A4.29E4
60J
401
20J
4 TLI#»
1.3E4
L1.1E4
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341.8567 F:2 Exp:NDB5US
Sample Text:M23-I-4 TLI#45399 INJ. TIME = 06:59 File Text:M23-I-
100% A2.82E4
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28:42 28:48 28:54 29:00 29:06 29:12 29:18 29:24 29:30 29:36 29:42 29:48 29:54 30:00 Time
File:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T
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File:T981958 #1-720 Acq:18-APR-1998 06:59:26 EI+ Voltage SIR 70T
367.8949 F:2 Exp:NDB5US
Sample Text:M23-I-4 TLI#45399 INJ. TIME = 06:59
100* 27;51
27:40
60J
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-------
O\ 00 O
p..p..p..
O O 10 CTl O
w w w td w
*» *» Ui yi ui H
ISf
-------
TLI Project: 45399
Client Sample: M23-I-4
Method 23 TCDD/TCDF Analysis (DB-225)
Analysis File: P981309
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23 Date Received:
204-92-4A-D Date Extracted:
Date Analyzed:
1.000
n/a
DB-225
Dilution Factor:
" Blank File:
Analyst:
04/01/98
04/03/98
04/16/98
n/a
U980780
ML
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPC2NF04
PF24098
P981302
n/a
n/a
n/a
Analytes
Anrt.
(ng) . •:;*•• 0t>': =?:?.•.
•V:?»qv£<
-l^feM'j
TT>.xv:Ffe$* .-;
:,3,7,8-TCDF
0.14
0.76
22:24
Internal Standard
Amt. (ng)
% Recovery QCPmite
Ffe^S
!C,:-2.3,7,8-TCDF
2.2
56.1
40%-130%
0.77
22:23
Recovery Standard
Irtergs
Ci:-l,2,3,4-TCDD
0.81
21:17
Data Reviewer
04/20/98
Page 1 of 1
•iangle Laboratories, Inc.®
)1 Caprtola Drive • Durham, North Carolina 27713
lone: (919) 544-5729 • Fax: (919) 544-5491
C2NFJ>SR T102. LARS 6.11 JOO
Printed: 21:28 04/20/98
-------
Initial
Date..
Data. Review By:
Calculated Noise Area:
0.13
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page Mo.
04/20/98
Listing of P981309B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2. . Rel.RT Compound.Na
ID.. Flags.
TCDF
304-306 DC NL 0:
17:
18:
18:
19:
19:
19:
19:
19:
20:
20:
20:
20:
20:
20:
21:
21:
21:
21:
21:
22:
0.65-0.89
00 RO 1.
51
51
58
06
17
33
43
52
01
08
11
32
37
59
04
14
28
40
52
17
22:24
22:37
22:
23:
23:
;57
:05
:50
24:32
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
11
75
74
77
72
74
75
75
74
74
73
83
67
89
76
77
73
77
81
74
79
0.76
0.85
0,
,71
0.74
0
.70
0.70
304-306 26 Peaks
13C12-TCDF
316-318 DC NL 0
DC WL 20
22
23
DC WH 24
0.
13.
39.
10.
13.
7.
6.
8.
2.
29.
3.
4.
11.
6.
19.
1.
13.
9.
0.
5.
4.
14.
4.
3.
10.
3
16
77
31
91
26
82
14
51
78
63
56
08
74
84
32
63
90
50
85
21
50
01
.64
.11
.99
.08
0.75
249
.84
5.
16.
4.
5.
3.
2.
3.
1.
12.
1.
1 .
4.
3.
8.
0.
5.
4.
0.
2.
1.
6.
2.
1.
4.
1 ,
0.
92
66
75
55
32
63
64
18
61
50
85
72
22
35
71
87
14
38
21
99
06
13
29
67
,27
.31
7.
22.
6.
7.
4.
3.
4.
1.
17.
2.
2.
7.
3.
10.
0.
8.
5.
0.
3.
0.790-1.102
85
65
16
71
50
51
87
60
02
06
23
02
62
97
92
03
36
47
00
2.51
7.95
2.51
1.82
6.
1.
.32
.81
0.44
0.65-0.89
:00
:59
:23
:03
:26
RO 1
0
0
RO 1
0
316-318 2 Peaks
13C12-TCDD
332-334 DC NL 0
19
21
.10
.72
.77
.37
.77
» W.»»«. .
0
0
394
0
5
394
m/TY
.18
.91
.06
.48
.49
.54
v I nv*
0.65-0.89
:00
:53
:01
RO 1
0
0
.50
.80
.78
0
0
290
.14
.54
.21
171
0
.22
.37
222
0
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
000
797
842
847
853
862
873
881
888
894
899
902
917
921
937
941
949
959
968
0.977
0.
1.
1.
.996
,001 2378-TCDF AN
.010
1.025
1.
.031
1.065
1
.096
0.955-1.045
.84
.27
0
0
1
1
1
.000
.937
.000 13C12-2378-TCDF ISO
.030
.092
DD Follows —
0
127
.24
.00
0
163
0.
.30
.21
905
0
0
1
-1.095
.000
.946
.000 13C12-2378-TCDD IS1
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
: 21:98(WJ>n/QR
-------
Page No.
04/20/98
Listing o£ P981309B.dbf
Hatched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak. 2. . Rel.RT Compound.Name.. ID.. Flags.
332-334
21:17 0.81
22:00 RO 0.91
4 Peaks
522.68
2.02
815.45
233.35
1.04
289.33 1.013 13C12-1234-TCD0 RSI
1.14 1.047
Column Description.
"Why" Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es)
..RT. -Retention Time (mn:ss)
Rat.l -Ratio of M/M+2 Ions
OK -RO=Ratio Outside Limits
Rel,RT-Relative Retention Time
*** End of Report *»'
WL-Below Retention Time Window
WH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
\fileiP9B1309 tl-1006 Acq:16-Alt>s-19!)tl JJJ.-M.-5fl El* Voltage SIX 70P
303.9016 ExpsDB22S
TRIANGLE LABS Text:M23-I-4 TLII45399
10
21 2l': 12 2l': 24
' 21\te' 22': 00 22': 12 22\24 ' 22': 36' 22\4B 2300
23t:24 ' '23\'36 iJ'-48
rile:P981309 #1-1006 Acq:16-APR-1998 19:51:58 EI+ Voltage SIR 70P
315.9419 Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI#4S399
2 .23
SOJ
80.
75.
70.
65.
60.
55.
50:
45.
40.
3Sl
30.
25
20
15
10
5
24 i 00 Tia
4.1E5
3.9E5
3.7E5
3.SE5
3.3E5
3.1E5
2.9E5
2.7E5
.2.5E5
.2.2E5
.2.0E5
.1. 8E5
.1. 6E5
-1.4E5
.1.2E5
':!. OE5
.8.2E4
.6.1E4
.4.1E4
.2.0E4
.0.010
21 00 111 12'21124' 21136' 21:48 22tOO 22tl2 32\24 22t36 23t48 23tOO 23tl2 23i24 23t36 23>4t 24*00
-------
file:PS81309 #1-10O6 Acqsl6-APX-19S8 19i51:5B EI+ Voltage SIS 7 OP Koif»t4U
303.9016 BSU3(2S6,30,-3.0) MCDf 5,3,1, 0.10\,192. 0,0. 00\,r,r) ExpiDB225
TX I ANGLE LABS Text:H23-I-4 TLI#4S399
1004 A1.67XS
*°-
'
'•
6°~ A1'l E A8~
"-,
1 i 1 *'•"*'
;ll MyAA 1H J
J5E4
i i A6.06E4
lt.HE4 A M.67X4
(I A A2.21E4 A
/\ A A/ n \ A1.27E4
\J\lv^J\ A/ vyv /u V .A ^
.4.6E4
-3 . 7ff4
-2.8E4
.1 . 8JE4
-9.2E3
O.OEO
18:00 19.' 00 20:00 21:00 22:06 23:06 24:00 25:00 Time
File:P981309 #1-1006 Acq:16-APR-1998 19:51:58 EI+ Voltage SIR 70P Noise -.44
305.8987 BSUB(256,30,-3.0) PKD(S, 3, 1, Q.10\, 176.0,0 .00\,T,T) Exp:DB225
TRIANGLE LABS Tert:M23-I-4 TLI#45399
1004 A2.26E5
^
1
so: A1 • ; OE5
I A1.10E5
•
40:
' A 1 A7.02E4
ll t JV I A
^11 JMFftAA IV i
18:00 19\00 . 20:00 21
i A7.95E4
A /I A6.32E4
A5.36E4 /I «
(I A A3.00J4 A
A A A \ A1.81E4
W/UV^A /Yl/vWv A r
.6.2E4
_5 . OE4
-3.7E4
-2.5E4
_1 . 2E4
O.OEO
:00 ' ' ' 221-06 ' 23 .-00 24 .-00 ' ' 25 .-00 Tiaie
File:P981309 #1-1006 Acq: 16 -APR- 199 8 19:51:58 EI+ Voltage SIR 70P Noiae:S7
315.9419 BSUB(256,30,-3.0) PTH(5,3, 1, 0.10%,228. 0,0. 00%,f, T) Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI#45399
1004
so:
so:
40:
20:
0'
18:00 19:00 ' 20 !• 00 21
Al . 71£S
1
J 1
4. IBS
13.3^5
:2.4E5
.1.SJF5
-8.2E4
O.OEO
1-00 ' 22.-00 ' ' 23.-00 ' ' ' 24-00 ' ' ' 2s!oO Time
file:P981309 #1-1006 Acq:16-APR-1998 19:51:58 EI+ Voltage SIR 70P Noise:52
317.9389 BSUB(256,30,-3.0) ?KD( 5,3, 1, 0 .10\,208 .0,0 .00\,r,F) EJCp:DB225
TRIANGLE LABS Text:M23-I-4 TLIH5399
1003
so:
so:
40:
20:
0'
A2.23ES
H
5.4E5
.4.4E5
.3 . 3E5
.2.2E5
.1 . li'S
0 .OEO
18:06 15:00 < 20:00 21:00 22:06 23:00 24:06 25:00 Time
rile:P981309 #1-1006 Acqs.l6-APR-1998 19:51:58 EH- Voltage SIS 70P
375.8364 Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI #45399
100417:55
80. |
so_ 18:20
40. 1 *°'°»
20 JWLi^^U*^^ . «:« 33:34. 24,02 34:39
0- ,
•^wvrv^^*»yvj"^j-^r*jv^-nj^"/-A^^---»-/~k'V^^
-3.3E3
-2.6E3
.2.0E3
.1 . 3E3
-6.5E2
' o . ana
18:00 15:00 , 20:00 2llo6 22:00 23<06 24»00 ' ' 25^00 Time
-------
'ile.-PSBUOS #1-1006 Acq:lS'-At>S-19SB 19:51:58 tl+ Voltage Sit 7OP Nbi»e:51
119.8965 BSUB(2S6,30,-3.0) PKD( 5,3,1, 0.10\,204.0,0.00\,f,T) Exp:DB225
TRIANGLE LABS TextsM23-I-4 TLH45399
1001
15:00 20:00 21:00 22:00 23:00
File:P981309 #1-1006 Acq:16-APR-1998 19:51:58 ZI+ Voltage SIS 70P Noise:57
321.8936 BSU3(256,30,-3.0) PKD(5,3,1, 0.10\,228.0,0. 00\,F,F) KipsDB225
TRIANGLE LABS TeJtt:M23-I-4 TLI#45399~
1001
15:00 20:00 21:00 22:00 23:00
File:P981309 #1-1006 Acq:16-APX-1998 1S.-51.-58 EI+ Voltage SIS 70P Noiae:54
327.8847 BSOB( 256,30,-3 .0 ) PKD(5, 3, 1, 0.10\,216. 0, 0. 00\,T,T) Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI#45399
1004 A2.78E6
so:
60J
20;
OJ
19:00 20:00 21:00 22:00 23:00
Tile:P981309 #1-1006 Acqtl6-APX-1998 19:51:58 ri+ Voltage SIS 70P Noiae:61
331.9368 BSUB(256,30,-3.0) PKD(5, 3, 1, 0 .10%, 244 . 0, 0 . 00\,F, F) Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI#45399
1004
801
601
401
20J
19:00 20:00 21:00 22:00 23:00
FilesP9S1309 #1-1006 Acq-.16-APR-1998 19:Sis58 EI+ Voltage SIS 70P Noiae:42
333.9338 BSOS(256,30, -3. 0) PKD( 5, 3,1,0.10\,168.0,0.00\,F,F) Eip:DB225
TRIANGLE LABS Text:M23-I-4 TLII4S399
1001
00.
601
401
20.
0.
19\00
20(00
24:00
24:00
24 : 00
O.OEO
Time
34:00
O.OEO
Tiae
7.7E5
.6.1E5
.4.6E5
.3.1E5
.1. 5.T5
.O.OEO
Tiae
6.2E5
5.0E5
3.7E5
.2.5E5
.1. 2E5
.O.OEO
Time
^7.6E5
-6.1E5
'-4.6E5
',3.0E5
11.515
21100
i | i
22:00
1 1—i 1 i
23:00
2
-------
Tile:P9ai309 #1-1006 Acq:16-APS-1998 19:51:58 EI+ Voltage SIS 70P
303.9016 Eip:DB225
TRIANGLE LABS Text:M23-I-4 TLH45399
1004 18; 51
aoj
60': II 30:01
40:
20:
ol
18:00 19:00 20:00 21:00 32:00 23:00
File:P981309 #1-1006 Acq:16-APS-1998 19:51:58 EI+ Voltage SIS 70P
315.9419 Elp:DB225
TRIANGLE LABS Text:M23-I-4 TLH45399
1004 22; 23
80:
60:
40:
20:
20:59
22:24
9:1719:43
AA
23:05
23:50
/v
4.7E4
.3. 8E4
.2.8E4
ll. 9S4
.9.4E3
24:00
.O.OEO
25:00 Tine
4.1E5
:3.3E5
.2.5E5
.1. 6E5
.8.2E4
18:00 19:00 20:00 21:00 22:00 23:00
File:P981309 #1-1006 Acq:16-APR-1998 19:51:58 EI+ Voltage SIR 70P
319.8965 Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLI#4S399
18:41
24: 00
25:
O.OEO
00 Time
18':00 19:00 20:00 21:00 221-00 2J1-00
File:P981309 #1-1006 Acq: 16-APR-1998 19:51:58 EI+ Voltage SIS 70P
331.9368 Exp:DB225
TRIANGLE LABS Text:M23-I-4 TLIV45399
100S,
80:
60:
40:
20:
18:00 19:00 20:00 21:00 221-00 231-00
File:P9S1309 #1-1006 Acq:16-APR-1998 19:51:58 EI+ Voltage SIR 70P
292.9825 Exp:DB225
TRIANGLE LABS Text-.M23-I-4 TLIV45399
803
SO:
40:
20:
0.
24 : 00
21
1
"1
24:00
23:45 24:15
25.
^.O.OEO
: 00 Time
6.2E5
-5.0E5
.3. 7E5
.2. 5E5
.1. 2E5
O.OEO
00 Tint
1. OE6
-8.2E5
.6.115
.*.ij;5
.3.OES
18:00 19:00 20:00 21:00 22:00 23:00
File:P981309 #1-1006 Acg:16-APK-1998 19:51:58 EI+ Voltage SIS 70P
330.9792 Exp:DB22S
TRIANGLE LABS Text:M23-I-4 TLIM5399
O.OEO
24:00
25:00 Time
18:00
19:00
20:00
21100
32tOO
231 00
24:00
O.OEO
25': 00 Ti*<
187
-------
Pages 188 through 268 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project: 45399
Client Sample: M23-O-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982306
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
Analytes
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
1,2,3,4,6,7,8,9-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
1,2,3,4,6,7,8,9-OCDF
Totals
Fotal TCDD
Fotal PeCDD
rotal HxCDD
fotal HpCDD
fotal TCDF
fotal PeCDF
fotal HxCDF
fotal HpCDF
r012.002/Lime Kiln
M23 Date Received: 04/01/98 Spike File- SPMIT204
204-92-8A-D Date Extracted: 04/03/98 ICal: SF51078
Date Analyzed: 04/18/98 ConCal: S982303
1.000 Dilution Factor: n/a % Moisture: n/a
n/a Blank File: U980780 % Lipid: n/a
DB-5 Analyst: DL % Solids: n/a
• -• • Amt. (ng) • ,-: .-at. vr ^SWH^r? •/••>-. • • 'j^*^&i&^"'l*fc'<-
ND 0.004
ND 0.006
ND 0.008
ND 0.007
ND 0.007
F*MPP r\ f\-\
cavir\_ U.U1 J
°-05 0.95 40:44 jil
°-02 0.69 25:18 JB
ND 0.004
ND 0.004
ND 0.005
ND 0.005 '
ND 0.006
ND 0.006
ND 0.007
Mn n m
nu U.U1
ND 0.01
Amt (ng) Murobef Dt EMPC : • ^ ; ^ f Ftegs- 1
ND 0.004
ND 0.006
EMPC 0.009
EMPC 0.01 .
0-17 8 0.20
0-01 1 0.02
0.008 1
ND 0.008
Page 1 of 2
Mm_PSR »!*«, LARS «J 1 SO.
Triangle Laboratories, Inc.®
301 Capitola Drive • Durham, North Carolina 27713
'hone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 11:08
-------
TLI Project: 45399
Client Sample: M23-O-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982306
Internal Standards
13C12-2,3,7,8-TCDF
13Ci:-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDF
IJCl2-l,2,3,7,8-PeCDD
C12-l,2,3,6,7,8-HxCDF
->Ci2-l,2,3,6,7,8-HxCDD
13Ci2-l,2.3,4,6,7.8-HpCDF
13C,2-l,2,3,4,6,7,8-HpCDD
13C12-1,2,3,4,6,7,8,9-OCDD
Surrogate Standards (Type A)
13C,:-2,3,4,7,8-PeCDF
13Cr-l,2,3,4,7,8-HxCDF
13Cp-l,2,3,4,7,8-HxCDD
13Cp-l,2,3,4,7,8,9-HpCDF
Other Standard
37Cl4-2,3,7,8-TCDD
Alternate Standards (Type A)
I3C,2-l,2,3,7,8,9-HxCDF
13C,2-2,3,4,6,7,8-HxCDF
Recovery Standards
13C12-1,2,3,4-TCDD
13Cr_-l,2,3,7,8,9-HxCDD
Ami: (ng)
3.2
2.6
2.8
2.7
3.2
3.8
3.0
3.5
7.5
AmL (ng)
3.6
3.7
3.4
4.2
AtnL (ng)
3.7
Amt. (ng)
3.5
3.4
<> ^ftfreawf^f
f. Sf
79.7
64.1
70.7
68.3
80.5
95.3
74.4
87.2
93.8
vv,;%;Recovery:.
89.7
93.4
83.8
104
% Recovery
91.8
• ::% Recovery
87.0
86.1
QC Limits
f 1- f s
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
<3CLIm^
40%-130%
40%- 130%
40%-130%
25%-130%
QC Limits
40%-130%
QC Limits
40%- 130%
40%- 130%
<;TRa»»-';
-if"*
0.72
0.79
1.55
1.47
0.50
12.0
0.42
1.01
0.87
I, v^kii|:
1.50
0.50
1.21
0.43
#**::=••: =:.^.
&#**&>•?&
0.50
0.50
Ratio
0.80
1.26
.-%$"-''"< Flags
f.f S V f f
25:15
25:58
29:11
30:13
32:45
33:28
35:46
36:52
40:44
;;-«T/-;i®^a^:.;-,
29:53
32:40
33:24
37:23
"'.:rirr,--^:vtH^v-
25:59
.^|^/>:^^5»^;-
34:04
33:16
RT &ags
25:47
33:48
Data Reviewer
Page 2 of2
04/21/98
Umj>SR T! J04. LARS «.H Oi
Triangle Laboratories, Inc.®
Hrh/a • Durfiam Mnrfh
11 -ftfl ftA/01 /Qfl
-------
Initial
.. Date..
Data Review By:
Calculated Noise Area:
0.19
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
Page No.
04/21/98
Listing of s982306B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
M
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
D
320-322
37C1-TCDD
328
328
13C12-TCDD
332-334
DC NL 0:00
22:09
22:39
22:55
23:15
23:36
23:58
24:13
24:33
24:51
25:06
25:18
11 Peaks
DC NL 0:00
DC WL 24:14
24:51
25:15
25:41
3 Peaks
DC NL 0:00
d SN 23:27
DC SN 23:39
DC SN 24:15
DC SN 24:23
DC SN 25:16
0 Peaks
0.
RO
RO
RO
RO
0.
RO
RO
RO
RO
0.
RO
RO
RO
RO
RO
65-0.89
2.
0.
0.
0.
0.
0.
0.
0.
1.
0.
1.
0.
65-
1.
0.
0.
0.
1.
25
78
88
80
88
88
79
85
01
98
05
69
0.89
00
96
59
72
10
65-0.89
1.
0.
1.
0.
2.
2.
20
86
22
17
00
33
0.21
5.26
2.84
1.33
8.74
5.31
5.47
3.50
2.73
1 .98
1.04
3.66
41.86
0.25
0.81
2.00
644.64
1.91
648.55
TPDF / TC
i v- ur 1 i\.
0.18
0.54
0.16
0.05
0.11
0.21
0.00
2
1
0
4
2
2
1
1
1
0
1
0
269
1
.31
.33
.59
.08
.48
.42
.61
.56
.10
.62
.49
.87
.10
.19
2
1
0
4
2
3
1
1
1,
0.
2
1.
375.
1.
0.873-1.075
0.
.95 0.
.51 0.
.74 0.
.66 0.
.83 0.
.05 0.
.89 0.
.54 0.
.12 0.
.59 0.
.17 1.
0.960-
0.
0.
.47 0.
.54 1.
.08 1.
000
877
897
908
921
935
949
959
972
984
994
002 2378-TCDF AN
1.040
000
960
984
000 13C12-2378-TCDF ISO
017
J
J
J
J
J
J
J
J
J
J
J
'
0.899-
0.
0.
0.
0.
0.
0.
1.046
000
903
911
934
939
973
0.923-1.077
DC NL 0:00
24:37
25:59
26:22
26:39
4 Peaks
DC NL 0:00
0.
RO
0.12
2.57
347.08
0.27
0.36
350.28
2
347
0
0
.57
.08
.27
.36
.65-0.89
2.
73
0.19
0.
0.
1.
1.
1.
000
948
001 37Cr-TCDD CLS
015
026
0.923-1.077
0.
000
riangle Laboratories, Inc.® Analytical Services Division
01 Capitola Drive • Durham, North Carolina 27713
hone: (919),544-57^LlFax: (919) 544-5491
Printed: 11:09 04/21/98
9*71
-------
Page No.
04/21/98
Listing of S982306B.dbf
Hatched GC Peaks / Ratio
/ Ret. Time
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
332-334
PeCDF
340-342
DC
DC
DC
DC
DC
d
DC
DC
DC
DC
4
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
24:
25:
25:
26:
Pea
0:
27:
28:
28:
28:
29:
29:
29:
30:
30:
30;
30:
48
47
58
17
iks
00
12
12
21
50
06
21
54
02
22
:30
:45
1.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
0.
0.
0.
0.
32-
0.
1.
0.
1.
0.
0.
0.
0
4
0
0
0
87
80
79
76
&V\mr
•1.78
75
00
86
59
.39
.37
.92
.94
.30
.90
.47
.50
1.
563.
398.
5.
968.
8. rtv-nr
1 L \~UJJ
0.
0.
0.
i.
0.
0.
0.
0.
0.
0.
0.
0.
78 0.83
57 249.74
20 175.28
33 2.31
88
15
72 0.44
31
40 0.86
20
12
38
49
26
15
13
07
0.95 0.
313.83 0.
222.92 1.
3.02 1.
0.928-
0.
0.44 0.
0.
0.54 0.
0.
0,
1.
1
1
1
1
1
955
993 13C12-1234-TCDD RSI
000 13C12-2378-TCDD IS1
012
•1.063
.000
932
.966
,971
.988
.997
.006
.025 23478-PeCDF AN
.029
.041
.045
.054
J
J
340-342
2 Peaks
2.12
13C12-PeCDF
352-354
352-354
PeCDD
356-358
356-358
DC NL 0:
28:
DC SN 28:
29:
29:
29:
30:
1.
00 RO
20
47 RO
11
28
53
52 RO
32-
1
1
0
1
1
1
0
5 Peaks
DC NL 0
DC SN 29
DC SN 30
1.
:00 RO
: 11
:13 RO
32
0
1
1
-1.78
.00
.33
.54
.55
.32
.50
.94
-1.78
.80
.77
.10
0 Peaks
0.
1.
0.
428.
2.
373.
0.
15
77 1.01
35
94 260.76
,18 1.24
.83 224.49
.79 0.48
0.863-
0
0.76 0
0
168.18 1
0.94 1
149.34 1
0.51 1
-1.13
.000
.971
.986
.000
.010
.024
.058
807.51
0
0
0
0
.13
.36
.18
.00
0.937
0
0
1
-1.02
.000
.966
.000
000 13C12-PeCDF 123 IS2
13C12-PeCDF 234 SUR1
AN
13C12-PeCDD
368-370
368-370
HXCDF
374-376
1.32-1.78
DC NL 0:00 RO 1.13
0.15
0.868-1.132
0.000
DC
DC
SN 29:09
30:13
30:21
2 Peaks
NL 0:00
1.44
1.47
1.43
1.05-1.43
1.33
0.39
229.78 136.91
19.46 11.46
249.24
0.21
0.965
92.87 1.000 i:
8.00 1.004
0.963-1.048
0.000
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham. North Carolina 27713
-------
Page No.
04/21/98
Listing of S982306B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... OC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
D
374-376
13C12-HXCDF
384-386
384-386
HxCDD
390-392
390-392
13C12-HXCDD
402-404
402-404
HpCDF
408-410
D
DC
d
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
DC
SN
SN
SN
SN
SN
1
NL
SN
SN
SN
SN
SN
7
NL
SN
SN
WH
WH
WH
1
NL
SN
SN
4
NL
SN
SN
31:41
31:51
32:40
32:45
33:05
33:16
Peak
0:00
31:42
31:50
32:40
32:45
32-58
33:06
33:16
33:27
33:35
33:42
34:04
34:18
Peaks
0:00
32:03
32:39
32- 50
33:59
34:03
34:06
Peak
0:00
32:51
33:24
33:28
33:48
34:04
34:12
Peaks
0:00
35:47
36:23
RO
RO
RO
RO
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
1.
RO
RO
RO
RO
1
RO
RO
0
RO
RO
0.91
1.
1.
1
2
1.
,29
,00
,00
.50
.05
0.
0.
0.
0.
0.
0.
0.
18
71 0.40
45
40
09
39
71
43-0.59
0
0
0
0
0
0
0
0
1
0
1
0
0
05
1
1
1
1
0
1
2
.05
1
1
1
1
1
0
1
.88
1
1
0
.89
.66
.66
.50
.50
.35
.15
.50
.84
.63
.60
.50
.23
-1.43
.20
.25
.65
.26
.67
.67
.17
-1.43
.33
.18
.21
.20
.20
.28
.67
-1.20
.36
.05
.77
0.
1.
1.
284.
299.
0.
0.
316.
0.
0.
0.
257.
0.
1,161.
27
98 0.87
51 0.66
12 94.61
43 100.38
33
21
87 105.51
29
.29
.15
28 85.88
74 0.25
93
0.
0.31 0.
0.
1.
1.
1.
967
973
997 123478-HxCDF
000 123678-HxCDF
010
016 234678-HxCDF
AN
AN
AN
0.878-1.122
0.
1,31 0.
1.00 0.
189.51 0.
199.05 1.
1.
1.
211.36 1.
1.
1.
1.
171.40 1.
1.10 1.
000
968
972
997 13C12-HXCDF 478
000 13C12-HXCDF 678
007
Oil
016 13C12-HXCDF 234
021
025
029
040 13C12-HXCDF 789
047
SUR2
IS4
ALT2
ALT1
• HxCDF / HxCDD Fol 1 ows •- — —
0
0
0
0
0.
0
0
0
.22
.09
.58 0.43
.43
.07
.13
.13
.58
0.958-
0.
0.
0.26 0.
0.
1.
1.
1.
•1.014
000
958
976
981
015
017
019
0.970-1.030
0
0
197
256
291
0
0
747
0
1
0
.21
.98 0.53
.91 108.18
.92 140.31
.70 159.10
.20
.34
.51
n / Uv^i^nv t?rtl i /-iu«
.22
.23
.20
0.
0.45 0.
89.73 0.
116.61 1,
132.60 1
1
1.
.000
.982
.998 13C12-HXCDD 478
.000 13C12-HXCDD 678
.010 13C12-HXCDD 789
.018
.022
-
SUR3
IS5
RS2
0.997-1.051
0
1
1
.000
.000 1234678-J$>CDF
.017
AN
Triangle Laboratories, Inc.® Analytical Services Division
101 Caprtola Drive • Durham, North Carolina 27713
'hone:
Printed: 11:09 04/21^87
-------
Page No.
04/21/98
Listing of S982306B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... QC.Log Omit Why . .RT. OK Ratio Total.Area... Area.Peak.1. . Area.Peak.2. . Rel.RT Compound.Name.. ID.. Flags.
408-410
13C12-HpCDF
418-420
418-420
HpCDD
424-426
MX
424-426
13C12-HpCDD
436-438
436-438
OCDF
442-444
442-444
OCDD
458-460
MK
458-460
13C12-OCDD
470-472
470-472
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
SN 36:29 RO
SN 36:36 RO
SN 36:40 RO
0 Peaks
0.
NL 0:00 RO
35:46
37:23
2 Peaks
0.
NL 0:00 RO
36:53 RO
1 Peak
0.
NL 0:00
36:52
1 Peak
0
NL 0:00
SN 38:02
SN 39:36
SN 40:55
0 Peaks
0
NL 0:00
40:44
1 Peak
0
NL 0:00
40:44
1 Peak
2.43
1.57
1.50
37-0.51
0.95
0.42
0.43
88-1.20
0.77
1.42
88-1.20
1.07
1.01
.76-1.02
1.00
0.83
0.85
0.91
.76-1.02
0.88
0.95
.76-1.02
1.00
0.87
0.14
0.14
0.24
0.00
0.27
183.77 54.11
153.17 45.69
336.94
Ur\f*r\f? 1 Ur^nn Wr*1 1 /tuc — •
np<_ \jc i np4. LJU f o i. x ows
0.20
0.49 0.34
0.49
0.29
188.22 94.75
188.22
0.20
0.11
0.24
0.21
0.00
0.15
1.85 0.90
1.85
0.16
274.79 127.71
274.79
1.020
1.023
1.025
0.944-1.112
0.000
129.66 1.000 13C12-HpCDF 678
107.48 1.045 13C12-HpCDF 789
0.976-1.005
0.000
0.24 1.000 1234678-HpCDD
0.973-1.027
0.000
93.47 1.000 13C12-HpCDD 678
0.902-1.098
0.000
0.934
0.972
1.005
0.902-1.098
0.000
0.95 1.000 OCDD
0.996-1.004
0.000
147.08 1.000 13C12-OCDD
IS6
SUR4
AN
IS7
AN
IS8
Column Description "Why Code Description OC Log Desc.
H_Z -Nominal Ion Hass(es)
..RT. -Retention Time (ran.-ss)
Rat.l -Ratio of M/M+2 Ions
OK -RO=Ratio Outside Limits
Rel.RT-Relative Retention Time
*** End of Report
WL-Below Retention Time Window A-Peak Added
HH-Above Retention Time Window
SN-Below Signal to Noise Level
-------
Tile:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noil* : 133
303.9016 F:2 BSOB( 256,30, -3.0) PJO)(9, 5,5,0 .05\,532. 0,1. 00\,r,T) Exp:KDB5US
TRIANGLE LABS Text:TLIt45399 M23-0-4 IKJ. TIME - 12:12
1001
80:
60:
A4 08E4
1
A A1.33E4 . M «•«« „ ,OM
4Q-\\ !\ ' /'I II A A1.10E4 ""'j!
atl_ A^5!j VLrlAy^
23\00 24. -00 25:00 26:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EH- Voltage SIR 70S Noise: 61
305.8987 F:2 BSUBf 256, 30, -3 . 0) PKD(9, 5,5, 0. 05\,244. 0,1. 00\,F, T) Ezp:lO>B5US
TRIANGLE LASS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
1003
sol
sol
40.
201
o-
A4 . 66E4
n
A ,7 ei^ A3.05E4 A2.17E4
A XM !\A*-f9*4 A.
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1 J VjTL_ J \J \ J \jj V^^S^y LurA^J V^-_-V\A.r4
23:00 24 \00 25\00 26^00
File:S982306 #1-746 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise: 69
315.9419 F:2 BSUB( 256 , 30, -3 . 0 ) PKD(9 , 5 , 5 , 0 . 05\, 276 .0 , 1 . 00\,F,T) Exp:NDB5US
TRIANGLE LABS Text :TLI#45399 M23-O-4 INJ. TIKE = 12:12
1001
80:
601
40:
20:
ol
A2.69E6
'
1 I
23(:00 24\00 25:00 26:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noiae:68
317.9389 F:2 BSUBf 256, 30, -3 . 0) PKD(9 , 5 , 5 , 0 .05\, 272 .0 , 1 . 00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME - 12:12
1001
aol
601
401
20 j
ol
A3.76E6
'
'
J V
2J.-00 24\ 00 25:00 26:00
File:S9S2306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
330.9792 F:2 Ezp:NDB5C7S
TRIANGLE LABS Text: TLI#45399 M23-0-4 INJ. TIME - 12:12
'alV^^^^--^^
eo:
4ol
2ol
ol
23 : 00 24 !• 00 25*: 00 26: 00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
375.8364 F:2 Exp:NDB5US
TRIANGLE LASS Text: TLI#4S399 M23-0-4 Utj. TIME - 12-12
1001
80.
60:
401
2bl
ol
t
C7.3E3
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11.513
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27: 00 Time
1 . OE4
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27:00 Time
-------
Tile:S9B2306 tl-746 Acq:18-APR-1998 12:09:23 XI + Voltage SIS 70S Noime:61
319.8965 F:2 BSUB(256f 30, -3.0) PXD(7,S,3
,0.05%,244.0,1.00%,r,T; Exp:NDB50S
TRIANGLE LABS Text:TLI#45399 M23-O-4
1003
801
60.
40.
20.
0
N
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1
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llil . 09E3 M
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241-00
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12:12
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26\ 00
'•-9.8E2
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'.4.9E2
'-2.5E2
• n nrn
27:00 Tiae
File:S982306 #1-746 Acq:18-APS-1998 12:09:23 EI+ Voltage SIX 70S Noise: 50
321.8936 F:2 BSUB(256,30, -3 .0 ) PKV(7,5r 3,0. 05%,200.0,1. 00%,
TRIANGLE LABS Text:TLI#45399 M23-0-4
1001
•
80^
'.
601
'•
401
201
,
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J.
F,T) Exp:KDB5US
JK7. TIME -
A2.82E3
Al.
1
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/ Irv^Wlf
24 • 00
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A2.30E3
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27:00 Time
File:S982306 #1-746 Acq:18-APR-199S 12:09:23 EI+ Voltage SIR 70S Noiae:152
331.9368 F:2 BSUB( 256 , 30, -3 . 0 ) PKD( 7, 5, 3, 0 . 05\, 608 . 0,1 . 00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-4
1001
80J
601
401
201
0'
24 1- 00
A2.50E
1*1
I I
25 1-00
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6
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261-00
12:12
r6.9E5
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27:00 Time
File:S982306 #1-746 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:56
333.9338 F:2 BSUB( 256 , 30, -3 . 0 ) PKD( 7, 5, 3, 0 . OS\,224 . 0, 1 . 00%,
TRIANGLE LABS Text:TLI#45399 M23-0-4
1003
801
601
401
201
01
F, T) Exp:NDB5US
INJ-. TIME -
A3.14E6
12:12
C8.7E5
\\A2.23E6
(
24 1- 00
25l
00
1 V
ft
y V
26:00
,7.0£5
.5.2E5
.3.5E5
.1 . 7E5
O.OEO
27:00 Time
File:S982306 #1-746 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S 3foiae:58
327.8847 F:2 BSUB ( 256, 30, -3 . 0) PKD< 7, 5, 3, 0 . 05\,232. 0, 1 . 00%,
TRIANGLE LABS Text:
1001
flOJ
60.
40.
20.
0
24 1- 00
File :S9 823 06 #1-746
TLI#45399 M23-0-4
•
A.
251-00
F, T) Exp:NVB5US
INJ. TIME -
? 47E6
j V
26\00
12:12
rl . OE6
.B.OE5
.6.0E5
.4 . OE5
.2.0E5
27:00 ' ' ' Ti»e
Acq:18-APR-1998 12:09:23 EI+ Voltage SIS 70S
330.9792 F:2 ExpsSDBSUS
TRIANGLE LABS Text:
1001
BO.
60.
40.
20.
0
/-
23 : 54
24 1- 00
TLI#45399 M23-0-4
25.-
15
^4^1724,3424^58 ^/^4Z>™_^
>^~V
k
25:00
I«7. TIME -
S 26:05 26sl9
^•w^,.^- N * .i^-— v^-^.
26-00
12:12
26-38 1-9F6
A 27:09
^*^^y ^\vx^x~*^^^*'^ -v"--. iV.. ^
.1.5E6
.1.1E6
.7.4E5
.3.7E5
• o . OEO
-i 1 1 1 1 i <
27:00 Time
-------
file}S982306 #1-746 AcgilB-APK-1998 12:09:23 EH- Voltage SIX 70S Hoiae:46
339.8597 F:2 BSDB(256, 30, -3. 0) PKD(7,5,3,0.05\,184.0,1.00\,f,T) ErpsmSSOS
TRIANGLE LABS Text:TLI#4S399 M23-O-4 HfJ. TIME - 12:12
100$ A8 (3E3
8CJ
60J
40:
201
^L^^~~^*^£V UWWKA
20:00 29': 00 30:00
Tile:S9B2306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIS 70S Koiaei62
341.8567 F:2 BSUB(256, 30,-3 .0 ) PKD( 7, 5,3, 0 . 05%,248 . 0,1. 00\,T, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME " 12:12
100$ A5.45E3
31: 00
2.6E3
2.1E3
1. 6E3
1.1E3
S.3E2
O.OEO
Time
28:00 29:00 30:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:45
351.9000 F:2 BSU3(256, 30, -3 . 0) PJCDf 7, 5, 3, 0 . 05%, 180 . 0, 1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME « 12:12
100$ A2.61E6
31 : 00
gQj
40
201
A2.24E6
28:00 29:00 JO:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:43
353.8970 F:2 BSVB( 256 , 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 1 72. 0,1. 00%, F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
100$ A1.68E6
A1.49E6
80J II t
601
401
31: 00
Oi , / V J V
1 1 1 1 1 1 1 ' i—'i i i 4 >-|
28:00 29:00 30:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
330.9792 F:2 Exp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-4
100$
SO:
40:
20:
0.
12:12
31\00
30:53 31_: 10
28:00 29:00 3o': 00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
409.7974 F:2 Exp:KDB5US
TRIANGLE LABS Text:TLI#4S399 M23-O-4 INJ. TIME - 12:12
100$
27:42 28-00
31 \ 00
60
40:
20:
oj
j - 28:26 28:42
AW^v^JWIW^l^V^^
29'sOO
30':00
31\00
.8.3E5
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Tiae
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.4.3E5
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Time
.1. 9E6
.1.516
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Time
.1. 6E3
.1.3E3
.9.8E2
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.3.3X2
.0.0X0
Time
977
-------
. n-746 Acq:lB-APR-199B 12:09:33 Xl-t- Voltage SIX 70S Noiaei42
55.8546 F:2 BSUB(256,30,-3. 0) PKD(7,5,3,0.05\,168.0,1.00\rrrT) Exp:HDB5VS
TRIANGLE LABS Text:TLI#45399 M23-O-4 XWJ. TIME - 12:12
ile:S982306 #1-746 Acq:18-APX-1998 12:09:23 EI+ Voltage SIR 70S Soiae-.SO
57.8516 F:2 BSUB(256, 30, -3. 0) PKD( 7,5, 3, 0. OS\,200. 0,1 .00\,F,T) Exp-.NDBSUS
TRIANGLE LABS Text :TLH4 5399 M23-0-4 XKJ. TIMS - 12:12
004
381: 34' 28': 36' 28': 48' 29:bo' 29': 12' J29:i<' 29\ 36' 29': 48
3:12 30:24 -ff 30\48' 31:00
O.OEO
31:12 Time
25 1- j«t ' 29:48
30:12' Jbl-
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 3(
ile:S982306 #1-746 Acq: 18-APR-199S 12:09:23 EI+ Voltage SIR 70S Noiae:47
67.8949 F:2 BSVB<256, 30,-3 .0 ) PKD( 7, 5, 3, 0 . 05%, 188 . 0, 1. 00\,F, T) Exp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME - 12:12
004 A1.37E6
80 L
eo:
40:
20 L
-o
28.-.Z4 ' 28\ 36 2B:4e
1.0EO
Time
-3.6E5
~2.7E5
.1.8E5
.8.9E4
1.15E5
O.OEO
Tim
29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:41
369.8919 F:2 BSUB(256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 164 . 0, 1. 00*,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
1004 A9.29E5 ^3.1E5
801
601
401
201
28': 24' 20136 ' 28:48' 29': 00 ' 29': 12' '29\24' 29': 36' 29\48 30:00 30:12 30':24 30:36 30:48 31:00 31:12
T
8.00E4
.2.5E5
'.1.9E5
'-1.2E5
'.6.2E4
.O.OEO
Tim:
File:S982306 #1-746 Acq:18-APK-1998 12:09:23 EI+ Voltage SIR 70S
330.9792 F:2 Exp:«DB5VS
TRIANGLE LABS TextsTLI#4S399 M23-O-4 INJ. TIME '
100* 29:19
28:47 29:06 / \ >V 29:54 30i°9 30:21
12:12
801
601
401
201
0.
28:33
30:53
28:24
29s 24 29 36
30\ 00 ' 30\12 30\34 30\36
.O.OEO
31:00 31:12 Tim
.1.9E6
-1.5E6
.1.1E6
•-7.4E5
-------
File:S982306 #1-465 Acq:18-APX-1998 12:09:23 EI+ Voltage SIR 70S Noias:58
373.8208 F:3 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,232.0,1.00\,r,T) £xp;«DB5CS
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
1004 A3.97E3
31:36 31:48 32:00 32:12 32:24 32:36 32:48 J3.-00 33:12 33:24 33:36' 33\48 34\00
File:S982306 #1-465 Acq:18-APX-1998 12:09:23 EI+ Voltage SIX 70S Noise:44
375.8178 F-.3 BSUB(256, 30, -3.0) PKD(7, 5,3, 0. 05\,176. 0,1. 00\,F, T) Ezp-.mBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME ' 12:12
100* A3. 1E3
34:24 34 36
File:S982306 #1-465 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:80
383.8639 F:3 BSUB(256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 320 . 0, 1. OOl,F, T) Exp-.NDBSOS
TRIANGLE LABS Text:TLI#45399 H23-0-4 INJ. TIME - 12:12
1003. A9.46E5 A1.06E6
801
601
401
201
01
A8.59E5
T
'
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:35 33:40 34:00 34:12 34:24 34':36
File:S982306 #1-465 Acq: 1S-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:89
385.8610 F-.3 BSVB( 256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 05%, 356. 0, 1. 00\,F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIKE = 12:12
I0°* A1.99E6 A2.11E6
801
601
401
201
01
A1.71E6
31:36 31:48 32:00 32-12 32':24 32:36 32\48 33':00 33':12 33':24 33:36 33:48 34:00 34:12 34:24 34:36
File:S982306 #1-465 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S
392.9760 F:3 Exp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 H23-O-4 INJ. TIME - 12-12
1003, Jj.50,,.^ 33:05 33,1933,31 ^ 3^,51 3<;
801
601
401
201
01
3i.'3s'3i.'48'32.'o0132;-i2'32.'24'32.'36132i48'33.'bo' jjlii'33.'24 ' 33.'35 ' 33.'*8 ' 34ioo'
8E5
3E5
7E5
1E5
7E4
OEO
Time
7E5
6E5
4E5
3E5
1E5
OEO
Time
5E5
9ES
1E5
4E5
File:S982306 #1-465 Acq:18-APX-1998 12:09:23 EI+ Voltage SIX 70S
445.7555 F:3 Ezp-.NDBSVS
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME
1004 ( 33:02
32,tt 32-IIO i i5.->c 33:39
34:12 34:24 34:36
.OEO
Tim<
12:12
31,36 31:48 32:00 32',12 32',24 32:36 32,48 33\00 33\12 33\24 33\ 36 ' 33>48 34-00
34\'l2 3424
34\ 36
.OEO
Time
-------
>ile:S9B2306 Vl-465 Acq:ia-APR-199B 12:09:23 BI+ Volttye Slit 70S Noi*e:6l
38S.8156 T:3 BSDB(256,30, -3.0} P1O>(7,S,3,0.05\,244.0,1.00\,F,T) ExpsODBSOS
TRIANGLE LABS Text:TLI#4S399 M23-0-4 INJ. TIME - 12:12
1004 A4.29E3
BO:
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48
Tile:S982306 #1-465 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noiae:49
391.8127 T:3 BSUB( 256, 30, -3.0) PKD( 7, S, 3 , 0,05\, 196.0,1.00\,F,T) Exp:NDB5US
TRIANGLE LABS Text:TLI*4S399 M23-O-4 INJ. TIME - 12:12
1004 A2.58E3
34
.O.OEO
'34'iia Time
^1.1E3
32:12 32:24 32:36 32':48 33':00 33:12 33':24 33:36 33:48
F±le:S982306 #1-465 Acq:18-APR-1998 12:09:23 EI+ Voltage SIS 70S Noiae:58
401.8558 F:3 BSUB(256, 30,-3 .0 ) PKOf 7, 5, 3, 0 . 05%, 232. 0, 1. 00\,T, T) Exp:tWB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME - 12:12
1003, A1.59E6
34:00 34:12
801
601
401
201
A1.40E6
32:12 32:24 32:36 32:48 33:00 33:12 33':24 33:36 33:48
File:S982306 #1-465 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noiae:44
403.8529 F.-3 BSUB(256, 30, -3. 0) PKD( 7, 5,3, 0. 054, 1 76. 0, 1. 00\,P, T) Exp-.NDBSUS
TRIANGLE LABS Text:TLI#45399 M23-0-4 IlfJ. TIME » 12:12
1003, A1.33E6
34 : 00
34:12
80.
60.
40.
20.
Al.17E6
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36
r±leiS982306 #1-465 Acqsl8-APR-1998 12:09:23 EI+ Voltage SIR 70S
392.9760 F:3 Exp:KDB5US
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
33:48 34:00
34:12
.O.OEO
Time
.4.3E5
.3.5E5
.2.6E5
.1. 7E5
.8.6E4
.0 .OEO
Tiae
.3.5E5
.2.8E5
.2.1E5
.1. 4E5
.7.1E4
.O.OEO
Time
1001
80.
60.
40.
20.
0
a a . ft£ 9 9 • C 7
32:14 32:22 32:33 32:48 */\s^~ _j^J^_-^ 33:31 -jj«O^^v^_._ 3^y?* _^^
k
32\12 32\24 32\36 32\48 33\00 33\12 ' ' 33\24 ' '33\36 ' '33\48 ' ' 34\00 ' '34\12
-8.SE5
16.8E5
15.1ES
L3.4E5
.1 . 7E5
Time
-------
File:;S982306 #1-569 Acq:18-APS-1998 12:09:23 EI+ VoZtaffa SIX 70S Hbi««:75
407.7818 F:4 BSUB(256,30, -3.0) PKD(7, 5,3,0. 05\,300.0,1.00\,r,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 H23-0-4 XMT. TIME - 12:12
1004
35:48 36:00 36:12 36:24 36:36 36:46 37:00 37:12 37:24
rile:S982306 #1-569 Acq:18-APS-1998 12:09:23 EI+ Voltage SIR 70S Koine: 57
409.7789 F:4 BSUB(2S6, 30,-3'.0) PKD(7,5,3, 0. 05\,228. 0,1. 00\,I, T) Exp:NDBSaS
TRIANGLE LABS Text:TLI#4S399 M23-O-4 IKJ. TIKE - 12:12
1004A6.04E3
37:36 37:48
80:
60:
40:
20:
0:
Al.26E3
A954.65
A1.29E3
A2.
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:S982306 #1-569 Acq:1S-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:89
417.8253 F:4 BSUBf 256, 30, -3 . 0 ) PKD< 7, 5, 3, 0 . 05%, 356 . 0, 1. 00%,f, T) Ezp:NDB5US
TRIANGLE LABS Text: TLI#45399 M23-0-4 INJ. TIKE = 12:12
1004 A5.41E5
37:36
37:48
80:
60:
40:
20:
o:
A4.57E5
35:48 36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24
File:S982306 #1-569 Acq:18-APR-1993 12:09:23 EI+ Voltage SIR 70S Ndise:96
419.8220 F:4 BSUB(256,30,-3'.0 ) PKD( 7, 5, 3, 0. 05%, 384 . 0,1. 00%,F, T) Exp:NDB5US
TRIANGLE LABS Text: TLI#45399 M23-O-4 INJ. TIKE = 12:12
1004 Al..
37:36
37:48
80:
60:
40:
20:
o:
OE6
A1.07E6
35:48 36:00 36:12 36:24 36:36 36:48 37:00
File:S982306 #1-569 Acq:18-APR-199B 12:09:23 EI+ Voltage SIR 70S
430.9729 F:4 Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ.
1004 35:45 _35^55 36:17 36L30 36:41 . 36:54 . .37;
• ^sy/sx**"% x"1*^ "" ^^^'VWx^-^gv js^>*>^ __ ~~ ~
80J
60J
40J
20:
OJ
37:1^ 37:24
37:36
37:48
TIME
06
12:12
37:23
35:48 36:00 36:12 36:24 36:36 36:48 37:00 ' '37\12 ' '37\24
File:S982306 #1-569 Acq: 18-AfR-1998 12:09:23 EH- Voltage SIS 70S
479.7165 F:4 Exp:SDB5VS
TRIANGLE LABS Text:TLIf45399 M23-0-4 IKJT. TIME - 12:12
1004
'37\48
=O.OEO
Time
.1. 3E3
.1.1E3
.8.0E2
.5.3E2
.2.7E2
. 0. OEO
Time
.1.1E5
.9.1E4
.6.8E4
.4.6E4
.2.3E4
. 0. OEO
Time
.2.7E5
.2.2E5
.1. 6E5
.1.1E5
.5.4E4
.O.OEO
Time
.5.1E5
.4.0E5
.3.0E5
.2.0E5
.1.0E5
.O.OEO
Time
35:48 36:00 36:12 36:24 36:36
281
-------
I
lie:S931301 #1-569 Acqsia-Afs-iS98 12:09iJJ EH- vo.LCag* SIM /us itoiam:52
23.7766 Ft4 BSUB(256,30, -3.0) PKD(7,5,3, 0. OS\,204.0,1.00\,r, T) ExpsXDBSVS
TRIANGLE LABS Text:TLI#45399 H23-O-4 X1TJ. TIME - 12:12
001 A2.91E3
36:00 36':06 36':12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982306 tl-569 Acq:18-APR-1998 12:09:23 EI+ Voltage SIX 70S Hoiae:66
25.7737 F:4 BSUB(256,30, -3. 0) PKD(7,5,3, 0. 05\,264. 0,1. 00\,T,T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 ~ UKT. TIKE - 12:12
10Q1 A1.91E3
1.1E3
8.4E2
6.3E2
4.2E2
2.1E2
O.OEO
Time
36:00 36:06 36:12 36:18 36:24 36':30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
File:S982306 #1-569 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noiae:73
35.8169 F:4 BSUB( 256, 30,-3 . 0 ) PKD( 7, 5, 3, 0 . 051,292. 0, 1. 00\,F, T) Exp-.NVBSUS
TRIANGLE LABS Text:TLI»45399 M23-0-4 INJ. TIME - 12:12
1004 A9.17E5
8 01
601
401
201
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06
'ile:S982306 #1-569 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:68
437.8140 F:4 BSUB( 256 , 30 ,-3 . 0 ) PKD( 7, S, 3 , 0 . OS*, 272 .0 , 1. 00\, F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 M23-O-4 INJ. TIME = 12:12
1001 A9.35E5
eo:
eo:
401
20.
37:12 37:18
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54
File:S982306 tl-569 Acq:18-APR-199B 12:09:23 EI+ Voltage SIR 70S
430.9729 F:4 Exp:NDB5US
TRIANGLE LABS Text:TLIt45399 M23-0-4
37:00 37:06 37:12 37:18
O.OEO
Time
.1. 7E5
.1. 3E5
.1. OE5
.6. 7E4
.3.3E4
.O.OEO
Time
.1. 7E5
.1.3E5
.9.9E4
.6.6E4
.3.3E4
.O.OEO
Time
1003
80.
60.
40.
20.
0.
IK7. TIME -
36:54
\ ' ' ' ' ' | ' ' ' i ' I i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i I i i i
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
.5.1E5
-4.0E5
13.OE5
L2.0E5
.1. OE5
O.OEO
Tim.
-------
File:S982306 #1-5*9 Acq: 18-APR-1998 12:09:23 EI+ Voltage SIR 70S J*oi««:52
441.7428 F:4 BSUB(256, 30, -3 . 0) PKD(7, 5,3,0. 05\,208. 0,1. 00\,F,T) ExpiHDBSUS
TRIANGLE LABS TeJCt:TLI#45399 M23-0-4 XJfJ. TIME - 12:12
1004 -2.SE4
901
a 01
701
60.
50.
40.
301
20.
10.
36.-OC ' ' ' 37:00 ' ' 3S.'oO
File:S982306 #1-569 Acg:18-APJ!-1998 12:09:
443.7399 F:4 BSUB(256, 30, -3 . 0) PKH(7,5,3,0
TRIANGLE LABS Text:TLI#45399 M23-0-4
IOCS
901
801
701
601
501
401
301
201
10\ A1.51E3
P " *-" ~ -*• * f*!^ ^ A ^ * " tth • * T f~
39:00 40:00 41 : 00 42:00
23 EI+ Voltage SIR 70S Noiae:50
.05%, 200. 0,1. 00\,F,T) ExpiNDBSUS
INJ. TIKE * 12:12
.M.r-s 1^ A rt * - - - ^^ Lmrt ' ^T.» - - *
36:00 ' ' ' J7.-00 ' ' ' 3e':00 ' 39:00 40.' 00 4l': 00 ' ' 42:00
File:S982306 #1-569 Acq: 18-APK-1998 12:09:23 EI+ Voltage SIR 70S
430.9729 F:4 Exp:iTDB5VS
TRIANGLE LABS Text:TLI#45399 M23-0-4 INJ. TIME - 12:12
100\ 36 30 37-06 38:28 39:11 39:37 40:22 4Q ^ 41-46
90\l\^^^y4^^^^
801
701
601
50J
40J
301
201
10.
0
36:00 J7.-00 Jfll-00
File:S982306 #1-569 Acq:lB-APK-199B 12:09.
513.6775 F:4 Exp:KDB5US
TRIANGLE LABS Text:TLH45399 H23-O-4
1004
90j
80J
70J
601
501
401
"1 35:55 3'[" 37:\0 37:48 38,14
2OQ**^~~t~jJ*J^-*rJ^^
10\
36\00 J7:00 3B-00
J9.-00 40:00 41:00 42:00
2J EI+ Voltage SIR 70S
INJ. TIME ' 12:12
39:15 *2:11
38:52 \ i 1 10:07 41:11 1
t^^L^J^L^^^
39:00 40:00 41:00 ' 42: 00
.2.2E4
.2 . OE4
_1 . 7E4
_1 . 5r4
_1.2£4
.9.9E3
.7.4E3
:4.9r3
L2.5Z3
_o.oro
Tiffle
_1 . 8E4
.1.6E4
-1.5E4
-1.3E4
.1.1E4
-9.1E3
-7.3E3
-5.5E3
-3.6E3
Ll . 8E3
Time
-5.2E5
-4.7E5
-4.2E5
.3.7E5
-3.1E5
-2.6E5
-2.1E5
.1.6E5
.1 . OE5
-5.2E4
'• 0 . OEO
Tine
C-4.3E3
.3.9E3
.3.4E3
.3 . OE3
.2.6E3
-2.1E3
.1 . 7E3
.1.3E3
-8.6E2
.4.3X2
.O.OEO
Time
283
-------
40-36 40:42 40':48 40:54 41:00 41:06
File:S982306 #1-555 Acq:18-APR-1998 12:09:23 11+ Voltage SIS 70S Koiee:39
59.7348 F:4 BSUB(256, 30, -3. 0) PKD(7, 5,3, 0 . 05\, 156.0, 1.00\,F, T) Exp-.SDBSUS
TRIANGLE LABS Text:TLI*45399 M23-0-4 INJ. TIME - 12:12
1001 A1.S5E3 A2.55E3
'JLle:S982306 01-569 Acq:18-APR-1998 12sliSs23 EI+ VoJ.tage SIS 70S Noise:37
57.7377 T:4 BSDB( 256,30, -3. 0) PKD(7,5,3,0.051,148.0,1.00*,r,T) ExpsNDXSUS
TRIANGLE LABS Text:TLH45399 M23-O-4 IK7. TIME - 12:12
001 A8.99E3
41:12
40 36 40:42 40:48 40:54 41:00 41:06
File:S982306 #1-555 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S Noise:41
469.7779 F:4 BSUB(256, 30,-3 . 0) PJO>( 7, 5, 3, 0 . 05\, 164 . 0,1. 00*, F, T) Elp:NDB5US
TRIANGLE LABS TextiTLI#45399 H23-O-4 INJ. TIKE - 12:12
1001
41:12
40-36 40-42 40:48 40:54 41:00 41:06
File:S982306 #1-569 Acq: 18-APR-199B 12:09:23 EI+ Voltage SIR 70S Noise:39
471.7750 F:4 BSUBf 256 , 30,-3 .0 ) PKD( 7, 5, 3, 0 . 05%, 156 . 0, 1. 00%, F, T) Exp:NDB5US
TRIANGLE LABS Text:TLI#45399 H23-O-4 JJW. TIME «• 12:12
1001 Al.
41:12
40:36 40':42 40:48 40:54 41': 00 41:06
File:S982306 #1-565 Acq:18-APS-1998 12:09:23 EI+ Voltage SIR 70S
430.9729 F:4 ExptXDBSUS
TRIANGLE LABS TeJct:TLI»45399 M23-0-4 TK7. TIME - 12:12
1001 40_iJJ 40±S6 41_:OS
80.
60.
40.
20.
41:12
.O.OEO
Time
1.2E3
9.6E2
7.2E2
4.8E2
2.4E2
.O.OEO
Time
.1.2E5
.9.3E4
.7.0E4
.4. 7E4
.2.3E4
.O.OEO
Tiot*
1.3E5
LIES
8.0E4
5.4E4
40 36
O.OEO
Tim
5.1E5
4.0E5
3.0E5
2.0ES
1. OE5
40:42
40:48
40:54
41:00
41:06
41112
.0.0*0
Tim
-------
Charrel I 338,9782 Peak top
Height ,33 volts Span 288 ppi
Systei file naie
Data file naie
Resolution
Group nuibef
lonlzation nde
Pitching
Ref, lasses 292,9825,
R 293 J 331
KB5US
fl;S982384
B 384
C 386
D 316
E 318
F 328
G 322
H 328
I 331
K 332
I 334
R 348
N 342
0 352
P 354
8 356
R
2
El*
VOLTflGE
416,9768
S 368
T 378
U 376
V 418
Ref, lass 416.9768 Peak top
Height .88 volts .Span 288 ppi
285
-------
r-
i
File:S982306 #1-746 Acq:18-APR-199B 12:09:23 EI+ Voltage SIR 70S
303.9016 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4 INJ. TIME =
100%
12:12 File Text:TLI#45399 M23»
24100 25:00 26:00 Time
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
305.8987 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4 INJ. TIME = 12:12 File Text:TLI#45399 M23»
100%
0
24:00
25:00
26:00
Time
-------
t-
oo
CM
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
303.9016 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4 INJ. TIME =
12:12 File Text:TLI#45399 M23»
^4.1E3
25:00 26:00 27:00
File:S982306 #1-746 Acq:18-APR-1998 12:09:23 EH- Voltage SIR 70S
305.8987 F:2 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4 INJ. TIME =
100%,
28:00
Time
25:00
2e!oo
27^00
12:12 File Text:TLI#45399 M23»
5.8E3
L5.2E3
L4.6E3
L4.0E3
L3.5E3
L2.9E3
L2.3E3
L1.7E3
L1.2E3
L5.8E2
JO-
28:00
Time
-------
File:S982306 #1-569 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
423.7766 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-0-4 INJ. TIME =
10 OS,
A3.42E3
12:12 File Text:TLI#45399 M23»
2. OE3
L1.8E3
L1.6E3
L1.4E3
L1.2E3
L9.8E2
17.8E2
L5.9E2
L3.9E2
L2.OE2
36:00 37:00 38:00
File:S982306 #1-569 Acq:18-APR-1998 12:09:23 EI+ Voltage SIR 70S
425.7737 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4 INJ. TIME =
lOOi A2.36E3
39! oo
O.OEO
Time
12:12 File Text:TLI#45399 M23»
1.6E3
36.-00
-------
File:S982306 #1-569 Acq:18-APR-1998 12
457.7377 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-0-4
100%
09:23 EI+ Voltage SIR 70S
INJ. TIME =
A8.98E3
39:48 40:00 40:12 40:24
File:S982306 #1-569 Acq:18-APR-1998 12
459.7348 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4
100%
12:12 File Text:TLI#45399 M23>
.-1.8E3
40:36 40:48 41:00 41:12
09:23 EI+ Voltage SIR 70S
41:24 41:36
Time
INJ. TIME =
A9.47E3
12:12 File Text:TLI#45399 M23»
r_2.0E3
39148 40:00 40il2 40i24
File:S982306 #1-569 Acq:18-APR-1998 12
469.7779 F:4 Exp:NDB5US
Sample Text:TLI#45399 M23-O-4
100%
80J
60 j
40J
20J
40:36 40:48 41:00 41:12
09:23 EI+ Voltage SIR 70S
41:24 41:36
.O.OEO
Time
INJ. TIME =
OJ
40:44
12:12 File Text:TLI#45399 M23»
1.2E5
L9.4E4
L7.0E4
L4.7E4
2.3E4
39:48 40:00 40:12 40:24 40:36 40:48 41:00 41:12 41:24
41:36
LO.OEO
Time
-------
TLI Project: 45399
Client Sample: M23-O-4
Method 23 TCDD/TCDF Analysis (DB-225)
Analysis File: P981317
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-8A-D
1.000
n/a
DB-225
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Blank File:
Analyst:
04/01/98
04/03/98
04/17/98
n/a
U980780
KB
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPC2NfF04
PF24098
P981314
n/a
n/a
n/a
Analyses
2,3,7,8-TCDF
Internal Standard
l3C12-2,3,7,8-TCDF
•;::"::.f ."•'•.;;•: Amtj-'(ng) Qt.
ND
1 :; : v Ami* (05
3.0
Recovery Standard ','•'.'.. : :
0.005
,\ : ".... .J;..: ILimfts::;
40%-130%
... ...::.,:,:.,. -j- ^v:-,,::-.
BaW:/:r .?;•;
=>:^Afe;'4--;:
0.76
^yMio-.,yi:
;«T-V.:/-
$%'&-.
22:23
•«l-:-v;
::^Ng«,/
:^FI^;.-.''
^flags' •
13C,:-1,2,3,4-TCDD
0.80 21:16
Data Reviewer.
Page 1 of 1
04/20/98
Triangle Laboratories, Inc.®
801 Cap'rtola Drive • Durham, North Carolina 27713
Printed: 21:29 04/20/98
-------
Initial
..Date...
Data Review By:
Calculated Noise Area:
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirements.
0.11
Page No.
04/20/98
Listing of P981317B.dbf
Matched GC Peaks / Ratio / Ret. Time
Compound/ -
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
TCDF
304-306
304-306
0.65-0.89
DC
DC
DC
DC
DC
DC
DC
NL 0:
17:
SN 17:
18:
18:
19:
19:
19:
19:
20:
SN 20:
SN 20:
SN 20:
20
21
SN 22
SN 22
00 RO
51
57 RO
50
59 RO
06 RO
•17 RO
33
:42
:01 RO
:06 RO
:11 RO
:31 RO
:59 RO
:14
:15 RO
:24 RO
0.
0.
3.
0.
1.
1.
1 ,
0
0
0
0
0
0
0
0
0
1
90
85
00
,66
.05
.02
.07
.85
.71
.63
.17
.47
.25
.42
.81
.50
.78
10 Peaks
0.
1.
0.
1.
0.
0.
0.
0.
0.
0.
0.
0
0
0
0
0
0
7
18
26
04
33
39
.94
,25
.50
.72
.99
,02
.18
.18
.34
.56
.07
.16
.28
0.
0.
0.
0.
0.
0.
0.
0.
o.
0
58
53
23
,54
15
.23
,30
.43
.15
.25
0,
0,
0.
0.
0,
0.
0
0
0
0
0.789-1.101
.68
,80
.22
.53
.14
.27
.42
.68
.36
.31
0.000
0.797
0.802
0.841
0.848
0.853
0.862
0.873
0.880
0.894
0.898
0.902
0.917
0.937
0.949
0.994
1.001 2378-TCDF
J
J
J
J
J
J
J
J
AM
13C12-TCDF
316-318
316-318
0.65-0.89
DC NL 0:00 RO
DC WL 20:59 RO
22:23
23:02 RO
DC WH 24:25
2 Peaks
1.20
0.58
0.76
1.25
0.68
0.18
0.44
225.41
0.28
2.82
225.69
97.46 127.95
0.20 0.16
0.955-1.045
0.000
0.937
1.000 13C12-2378-TCDF ISO
1.029
1.091
Above: TCDF / TCDD Follows
13C12-TCDD
332-334
332-334
0.65-0.89
DC NL 0:00 RO
19:53 RO
21:00
21:16
22:00 RO
4 Peaks
1.22
1.42
0.79
0.80
0.97
0.16
0.34
154.37
222.13
1.08
377.92
0.27
67.90
98.53
0.59
0.19
86.47
123.60
0.61
0.905-1.095
0.000
0.947
1.000 13C12-2378-TCDD IS1
1.013 13C12-1234-TCDD RSI
1.048
riangle Laboratories, Inc.® Analytical Services Division
01 Caprtola Drive • Durham, North Carolina 27713
hone: (919) 544-5729 • Fax: (919} 544-5491
Printed: 21:29
-------
Page No. 2 Listing of P9813X7B.dbf
04/20/98 Matched GC Peaks / Ratio / Ret. Time
Compound/
M_Z.... gc.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Compound.Name.. ID.. Flags.
Column Description "Why* Code Description QC Log Desc.
M_Z -Nominal Ion Mass(es) WL-Below Retention Time Window A-Peak Added
..RT. -Retention Time (mnuss) WH-Above Retention Tine Window K-Peak Kept
Rat.l -Ratio of M/M+2 Ions SK-Below Signal to Noise Level D-Peak Deleted
OK -RO=Ratio Outside Limits
-------
ro
CD
-------
#1-1006 Acq:17-APR-lyye UJ:4J.:J.1 CI+ vox cage SIS 7OP NoiaeitO
03.9016 BSUB(256,30,-3.0) PXD(S,3rl,0.10\,lB4.0rO.OO\,T,T) Xlp:DB225
TRIANGLE LABS Text:M23-0-4 TLI*45399
001 A4.36E3
18:00 19:00 30:00 31:00 33100 23s00
File:P981317 #1-1005 Acq:17-APR-1998 02:41:14 EI+ Voltage SIR TOP Noiae:48
05.8987 BSUB(256,30,-3.0) PKD(5,3, 1,0.10\,193.0,0.00\,F,F) Xxp:DB225
TRIANGLE LABS Text:M23-0-4 TLI#4S399
001 ., A6.78E3
-1.9E3
24:00
'.O.OEO
25:00 Time
Al.20E3
1.84E3 I A611426
18:00 19:00 20:00 21:00 22:00 23:00
File:P981317 #1-1006 Acq:l7-APR-1998 02:41:14 EI+ Voltage SIR 70P Noiae:61
15.9419 BSUB(256,30,-3.0) PKD(5, 3, 1, 0.10%, 244 . 0, 0. 0
-------
file:P9B1317 #1-1006 Acq:17-APs-199B 02:41:14 K+ Voltage SIS 70P Xoiie:44
319.8965 BSUB(256,30,-3.0) PKD(5,3,1, 0.10\,176. 0,0.00%,r,T) Xxp:DB225
TRIANGLE LABS Text:M23-0-4 TLI#45399
-1001
15.-00 .20:00 21tOO 22:00 23:00
File:P981317 01-1006 Acq:17-APR-1998 02:41:14 ZI+ Voltage SIS 70P Noiae:62
321.8936 BSUB(256,30,-3.0) PXD(5, 3,1, 0.10\,248. 0,0. 00\,T,F) Exp:DB225
TRIANGLE LABS Teit:M23-0-4 TLI#45399
1S.-00 20:00 21:00 22.-OC 23:00
File:P981317 #1-1006 Acq:17-APK-1998 02:41:14 EI+ Voltage SIS 70P Noiae:48
327.8847 BSUB(256, 30,-3. 0 ) PKD(5, 3,1, 0.10%, 152. 0, 0. 00\,F ,F) Exp:DB225
TRIANGLE LABS Text:M23-0-4 TLI#45399
1004 A1.48E6
BO:
60-
401
20 L
15.-00 201-00 21.' 00 22 .-co''23\ 00
File:P981317 #1-1006 Acq:17-APR-1998 02:41:14 EI+ Voltage SIS 70P Noiae:57
331.9368 BSUB(256,30,-3.0) PKD(5, 3,1, 0.10%,228. 0, 0. 00*, F,F) Exp:DB225
TRIANGLE LABS Teit:M23-0-4 TLI#45399
A9.85E5
80.
60.
40.
20.
T
T
19:00 20:00 21:00 22:00 23:00
File:P981317 #1-1006 Acq:17-APR-1998 02:41:14 EI+ Voltage SIR 70P Noise:47
333.9338 BSUB(256,30, -3. 0) PKD(5,3,1, 0.10\,188.0,0.00\, F,F) Xxp:DB22S
TRIANGLE LASS Text:M23-O-4 TLH45399
A1.24E6
BO:
so;
40.
20.
o.
A8.6SES
19:00
20100
21:00
22s 00
23\00
24:00
.O.OEO
Tim,
24:00
Time
r3.8E5
.3.1ES
.2. 3E5
.1. 5E5
-7.7E4
i I >
24:00
O.OEO
Time
24\00
.2.1ES
.1. 6E5
.1. OE5
-S.2E4
.O.OEO
Tim,
-3.3E5
.2.6X5
.2.0E5
.1.3X5
.6.5X4
I I "T-
24 tOO
.0.0X0
Tim
-------
.File:
303.5
THIAA
100]
40i,
201
P981317 #1-1006 Acq: 17 -APR- 1998 02:41:14 EH- Voltagrc SIK 70P
016 Exp:DB225
1GLE LABS TextiM23-0-4' IXI#453S5
20:01
/L^^AjyiAJXX1^^
18:00 15:00 20:00 21:00 22:00 231-00 24. -00
File:PS81317 #1-1005 Acg:17-APB-15S8 02:41:14 XI+ Voltage SI* 70P
315.S41S Exp:DB22S
TRIANGLE LABS TextiM23-O-4 TLI#45399
1004 32^23
80:
60:
40:
20:
oi
Tile
319.
TSIA.
1003
801
401
201
oi
Tile
331.
TSIA
1004
80^
60:
40:
20.
0.
Fil«
252.
TKIt
1003
80.
60.
40.
20.
0
Fil.
330
TRI<
100
80
60
40
20
0
• :
11
.2.7X3
.2.2X3
.1 . 6X3
.1.1X3
.5.4X2
.0.0X0
25 00 Time
-2.3E5
Jsioo 15:00 20:00 21:00 22:00 23:00 24:00 25:
.•PS81317 #1-1006 Acq:17-APS-1998 02:41:14 EI+ Voltage SIS 70P
8965 Elp:DB225
NGLE LASS Text:M23-O-4 TLI#45399
^^^^
18\00 IS: 00 20:00 21:00 22:00 23:00 24:00
•.P981317 #1-1006 Acq:17-APR-1998 02:41:14 EI+ Voltage SIR 70P
9368 Ezp:DB225
NGLE LABS Text :M23 -0-4 TLI #45399
21:16
21:00
1
Jill
18:00 15:00 20:00 21:00 22:00 23:00 24:00
:PSfllJ17 #1-1006 Acg:17-APJ?-lSS8 02:41:14 EI+ Voltage SIS 70P
9825 Elp:DB225
\NGLE LABS Text:H23-0-4 TLI#45399
k 15:3115:57 20:26 20:55 21:3422:02 22:4623:1423:40
~^ ^^^^-^^v-^r^-^-v^^^ ^ ~Y V*^"
.
.1 . 8X5
.1.4X5
.5.2X4
.4.6X4
0.0X0
00 Time
_1.2X3
-.9 . 2X2
L6.SX2
^4.6X2
L2.3X2
10. 0X0
25 00 Time
2.6E5
12 . 1X5
11 . 6X5
11 . 0X5
15.2X4
10. 0X0
25 00 Time
,.^.-3 . 8E5
18:00 15:00 • 20:00 21:00 22:00 23:00 24:00 25
B.-PS81317 #1-1006 Jcg:17-APK-lP58 02:41:14 EI+ Voltage SIR 70P
.9792 Exp:DB225
WGLE LABS Tejct:M23-O-4 TLI #4 5399
L^vM^V^^A^V^^^^
18:00 15:00 20:00 21:00 22.' 00 231-00 24:00
as
•.3.0E5
.2.3E5
.1 . 5E5
.7.6E4
O.OEO
00 Time
4.1JW
L3 . 315
.2.5E5
.1 . 6E5
.8.2X4
O.OEO
00 Time
-------
lonlzatlon lode
Switching
, lasses 292,9825,
fef , lass 292,9825 Peak top
Height ,86 volts Span 288 ppi
Systei file naie
Data file naie
Resolution
fl=P971317
ft 232,9825
B 383,9816
C 385,8987
D 315,9419
E 317,9389
F 319,8965
6 321,8936
H 327,8847
I 338,9792
J
K
L
H
1
El*
VOLTflGE
388,9761
338.9792
331,9368
333,9338
$5,8364
Channel I 338,9792 Peak top
Height .86 volts Span 288 ppi
-------
Pages 298 through 357 from the Triangle Laboratories, Inc. analytical report
have been excluded by PES since these pages present results for samples
collected at another lime kiln facility during the same mobilization.
-------
TLI Project: 45399
Client Sample: M23-RB-1-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982310
Client Project:
Sample Matrix:
TLI ID:
Sample Size:
Dry Weight:
GC Column:
r012.002/Lime Kiln
M23
204-92-12A-D
1.000
n/a
DB-5
Date Received: 04/01/98
Date Extracted: 04/03/98
Date Analyzed: 04/18/98
Dilution Factor n/a
Blank File: U980780
Analyst: DL
Spike File:
ICal:
ConCal:
% Moisture:
% Lipid:
% Solids:
SPMIT204
SF51078
S982303
n/a
n/a
n/a
Aralytes •.
-*U '*." s -\.s VJtatf.
(ng^llS'^^fe^^^^^iEMP^^
£__! ^..MM^N k^ ' - -'-^fe*
SrHOl^^l^ffli
ffj ^ ^ .- <;„ <.>^N.^''^^M
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1^,3,6,7,8-HxCDD
U,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1^,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
lZ3,4,7,8,9-HpCDF
1,2,3,4,6,7,8,9-OCDF
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.003
0.004
0.004
0.004
0.004
0.004
0.005
0.002
0.003
0.003
0.003
0.003
0.003
0.003
0.003
0.004
0.004
i^*^ : ,; ™^~*^ Jte&jift^
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
ND
ND
ND
ND
ND
ND
ND
ND
0.003
0.004
0.004
0.004
0.002
0.003
0.003
0.004
Page 1 of 2
MR2J>SR VIM. LARS 6.114)0
Triangle Laboratories, Inc.®
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28
-------
TLI Project: 45399
Client Sample: M23-RB-1-4
Method 23 PCDD/PCDF Analysis (a)
Analysis File: S982310
13C,j-2.3,7,8-TCDF
13Ci:-Z3,7,8-TCDD
13C,:-1.2,3,7,8-PeCDF
»Cp-l,2.3,7,8-PeCDD
13C13-U23,6,7,8-HxCDF
l3Cl:-1.2,3,6,7,8-HxCDD
»Cp-1.23,4,6,7,8-HpCDF
13Cp_-l,2,3,4,6,7,8-HpCDD
»C,:-1.2,3,4,6,7,8,9-OCDD
'3C12-13,4,7,8-PeCDF
13C,rl.2,3,4,7,8-HxCDF
"Cp-1.2,3,4,7,8-HxCDD
»Cp-l,2,3,4,7,8,9-HpCDF
13C,2-1.2,3,7,8,9-HxCDF
13C,:-2,3,4,6,7,8-HxCDF
Recovery Standards
«C,rU2,3,4-TCDD
'3Cp.-l,2,3,7,8,9-HxCDD
2.6
2.4
2.5
3.0
3.3
3.9
3.3
4.0
9.2
66.0
59.9
62.5
76.1
81.6
97.6
82.8
101
115
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
40%-130%
25%-130%
25%-130%
25%-130%
0.71
0.80
1.57
1.48
0.50
121
0.42
1.01
0.85
25:14
25:57
29:10
30:13
32:44
33:27
35:44
36:52
40:42
4.0
3.3
3.3
3.8
101
82.5
82.5
95.2
40%-130%
40%-130%
40%-130%
25%-130%
0.50
120
0.43
29:52
32:38
33:22
37:22
3.5
3.6
0.79
1.19
25:46
33:47
Data Reviewer.
Page 2 of2
04/20/98
Mrn_PSR »IXR LARS 6.1UK
Triangle Laboratories, Inc.®
801 Capftola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/20/9J
n e- n
-------
Initial
Date..
Data Review By:
Calculated Boise Area: 0.10
The Total Area for each peak with an ion abundance ratio outside
ratio limits has been recalculated according to method requirement*.
Page No.
04/20/98
Listing of S982310B.dbf
Hatched GC Peaks / Ratio / Ret. Tim*
Compound/
H_Z QC.Log Omit Why . ,RT. OK Ratio Total. Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Confound.Name.. ID.. Flags.
TCDF
304-306
304-306
13C12-TCDF
316-318
316-318
TCDD
320-322
D
320-322
37C1-TCDD
328
328
13C12-TCDD
332-334
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
DC
DC
DC
NL
0
NL
WL
WL
4
NL
SN
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
0:00
Peaks
0:00
23:15
24:12
24:31
24:50
25:14
25:40
Peaks
0:00
23:26
23:34
23:43
23:53
24:12
24:26
24:46
25:30
25:44
25:59
Peaks
0.
RO
0.
RO
RO
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
65-0.89
1.
23
0
0
.23
.00
65-0.89
1.
1.
0.
0.
0.
0.
0.
00
46
71
88
71
71
86
0
0
12
1
3
434
1
440
m/*rv
65-0.89
0.
4.
0.
0.
0.
0.
0.
1.
1.
3.
0.
90
00
43
67
40
83
18
00
20
75
37
0
0
0
0
0
0
0
0
0
0
0
0
.28
.42
.07
.05 0.49
.00 1.25
.08 180.06
.90 0.88
.03
f i ffy^nn QM! i r^*m
.18
.04
.07
.10
.05
.11
.07
.39
.09
.07
.16
.00
0.873-1.075
0.
000
0.960-1.040
0.
0.
'0.
0.56 0.
1.75 0.
254.02 1.
1.02 1.
0.899-
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
1.
000
921
959
972
984
000 13C12-2378-TCDF
017
1.046
000
903
908
914
920
933
942
954
983
992
001 2378-TCDD
ISO
AN
0.923-1.077
DC
DC
DC
NL
SN
4
NL
0:00
24:35
25:07
25:58
26:10
27:27
Peaks
0:00
24:46
25:46
25:57
0.
RO
RO
0
1
0
240
0
0
242
.13
.40 1.40
.12
.64 240.64
.28 0.28
.16 0.16
.48
65-0.89
1.
0.
0.
0.
27
94
79
80
0
1
458
302
.27
.54 0.82
.13 202.61
.52 134.10
0.
0.
0.
1.
1.
1.
000
947
968
001 37C1-TCDD
008
058
CLS
0.923-1.077
0.
0.87 0.
255.52 0.
168.42 1.
000
954
993 13C12-1234-TCDD
000 13C12-2378-TCDD
RSI
IS1
riangle Laboratories, Inc.® Analytical Services Division
31 Capitola Drive • Durham, North Carolina 27713
hone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/20/98
-------
Pag* No.
04/20/98
Listing of S982310B.dbf
Hatched QC Peaks / Ratio / Ret. Tin*
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.RT Confound.
NUM.. ID.. Flags.
332-334
PeCDF
340-342
340-342
13C12-PeCDF
352-354
352-354
PeCDD
356-358
356-358
13C12-PeCDD
368-370
368-370
HXCDF
374-376
26:17
4 Peaks
DC NL 0:00
DC SN 29:20
DC SN 29:30
DC SN 29:39
DC SN 29:45
DC SN 29:54
DC SN 30:08
0 Peaks
DC NL 0:00
28:19
28:47
29:10
29:20
29:27
29:52
30:14
30:49
8 Peaks
DC NL 0:00
DC SN 29:37
DC SN 29:49
0 Peaks
DC NL 0:00
29:07
29:17
30:13
30:20
DC SN 30:45
4 Peaks
DC NL 0:00
DC SN 31:50
DC SN 32:15
DC SN 32:20
DC SN 33:02
0.
89
1.32-1.78
RO 1.00
1.75
RO 0 . 17
RO 0.50
RO 0.60
RO 0.73
RO 0.38
1.32-1.78
RO
RO
RO
RO
RO
1.
RO
RO
RO
1.
RO
RO
RO
RO
1.
RO
RO
RO
RO
RO
1.
1.
1.
1.
0.
1.
1.
1.
1.
11
51
80
57
89
34
53
09
00
kW«*_ .
4.
766.
0.
0.
0.
0.
0.
0.
0.
0.
0.
18.
0.
308.
1.
2.
301.
0.
0.
633.
44
63
/
/
13
11
12
05
10
13
05
00
16
55
89
06
28
78
10
41
92
99
2.09
2.35
1.
013
0.928-1.063
0.000
1.006
1.011
1.017
1.020
1.025 23478-PeCDF AN
1.033
0.863-1.137
0.000
11.
0.
188.
0.
1.
182.
0.
0.
15
63
06
78
59
19
25
56
7.40
0.35
120.00
0.88
1.19
118.91
0.23
0.56
0,
0,
.971
.987
1.000 13C12-PeCDF 123 IS2
1.
1,
1
1
1
.006
.010
.024 13C12-PeCDF 234 SUR1
.037
.057
32-1.78
1.
2.
1.
,00
,00
,22
0.
0.
0.
0.
13
.13
,18
.00
32-1.78
0.
1,
2,
1
1
2
.89
.00
.74
.48
.44
.11
0.
0.
0,
208
17
0
226
•o*y*TM
.13
.48
.59
.19
.71
.23
.97
r\ I
05-1.43
0
2
0
0
1
.90
.00
.67
.33
.50
0
0
0
0
0
.16
.16
.04
.02
.04
0.
29
0.63
124.24
10.45
0.
0.
0.29
0.23
83.95
7.26
937-1.022
0
0
0
.000
.980
.987
868-1.132
0
0
0
1
1
1
.000
.964
.969
.000 13C12-PeCDD 123 IS3
.004
.018
0.
963-1.048
0
0
0
0
1
.000
.973
.985
.988
.009
Triangle Laboratories, Inc.® Analytical Services Division
801 Caprtola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28
04/20/901
-------
Page No.
04/20/98
Listing of S982310B.dbf
Matched GC Peaks / Ratio / Ret.
Tin
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.1.. Area.Peak.2.. Rel.BT Conpound.Name.. ID.. Flags.
374-376
13C12-HXCDF
384-386
384-386
HxCDD
390-392
D
390-392
13C12-HXCDD
402-404
402-404
HpCDF
408-410
D
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
DC
DC
DC
DC
DC
DC
DC
DC
DC
d
SN
WH
WH
0
ML
SN
SN
SN
SN
8
NL
SN
SK
SN
SN
SN
SN
SN
SN
SN
0
NL
6
NL
SN
SN
33:05
34:34
34:38
Peaks
0:00
31:40
31:47
32:38
32:44
32:58
33:01
33:03
33:15
33:29
33:32
34:03
34:22
Peaks
0:00
32:26
32:34
32:38
32:43
32:49
32:58
33:03
33:09
33:17
Peaks
0:00
32:50
33:22
33:27
33:47
34:01
34:13
Peaks
0:00
35:50
35:55
RO
RO
0.
RO
RO
1.
38
0.40
3.
,50
0.
0.
0.
0.
19
04
04
00
43-0.59
0.87
0.60
0.54
0.50
0.50
RO
RO
RO
0.23
0.27
0.18
0.50
RO
RO
0.42
0.69
0.51
RO
1.
0.67
1
* W ..u. .
05-1.43
1.29
RO
RO
RO
RO
RO
RO
RO
RO
3
1
1
2
1
0
0
0
2
.00
.00
.00
.13
.20
.60
.70
.75
.44
0.
3.
6.
254.
303.
0.
0.
0.
327.
0.
0.
259.
0.
.156.
23
47 1 . 37
79 2.39
40 84.46
42 101.46
18
09
18
85 109.60
56 0.19
20
19 87.04
32 0.14
00
1.011
1.056
1.058
0.878-1.122
0.000
2.30 0.967
4.40 0.971
169.94 0.997 13C12-HXCDP 478
201.96 1.000 13C12-HXCDF 678
1.007
1.009
1.010
218.25 1.016 13C12-HXCDP 234
0.45 1.023
1.024
172.15 1.040 13C12-HXCDF 789
0.21 1.050
SUR2
ISA
ALT2
ALT1
0.
0.
0.
0.
0.
16
04
07
25
18
0.22
0.05
0.13
0.05
0.20
0.958-1.014
0.000
0.970
0.974
0.976
0.978
0.981
0.986
0.988
0.991
0.995
0.00
1.
RO
RO
RO
05-1.43
1
1
1
1
1
1
1
.56
.46
.20
.21
.19
.39
.94
0.20
1 . 57 1 . 02
199.35 108.74
262.94 143.85
291.63 158.76
0.86 0.50
0.38 0.33
0.970-1.030
0.000
0.70 0.982
90.61 0.998 13C12-HXCDD 478
119.09 1.000 13C12 -HXCDD 678
132.87 1.010 13C12-HXCDD 789
0.36 1.017
0.17 1.023
SOR3
IS5
RS2
756.73
0,
RO
RO
HxCDI
.88-1.20
0
2
0
.81
.75
.90
0
.26
0.08
0.40
0.997-1.051
0.000
1.003
1.005
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 20:28 04/30/98
-------
Pag* No.
04/20/98
Lilting of S982310B.dbf
Matched GC P«aXa / Ratio / R«t. Tim*
Compound/
M_2 QC.Log Omit Why . .RT. OK Ratio Total. Ar«a... Ar«a.P«ak.l.. Ar«a.P«*k.2.. tel.KT CoapouDd.Ham*.. ID.. Flags.
408-410
0 Peaks
0.00
13C12-HpCDF
418-420
418-420
HpCDD
424-426
424-426
13C12-HpCDD
436-438
436-438
OCDF
442-444
442-444
OCDD
458-460
458-460
13C12-OCDD
470-472
470-472
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
DC
NL
3
NL
SN
SN
0
NL
2
NL
HL
SN
SN
SN
SN
SN
SN
SN
SN
SN
0
NL
SN
SN
SN
SN
SN
0
NL
1
0:00
35:44
36:07
37:22
P«aka
0:00
36:13
37:02
0.
RO
37-0.51
0.93
0.42
RO
0.95
0.43
0.22
204.45 60.09
0.32 0.21
155.83 46.84
0.944-1.112
0.000
144.36 1.000 13C12-HpCDF 678
IS6
0.22 1.011
108.99 1.046 13C12-HpCDF 789
SUR4
360.60
0.
RO
RO
RO
88-1.20
1.25
4.50
0
.67
nfrrwwr I ft^f^fW f w** www ~
0.16
0.04
0.08
0.976-1.005
0.000
0.982
1.005
Peaka 0 . 00
0:00
36:04
36:52
Peaks
0:00
36:37
37:50
37:55
38:01
38:38
38:43
38:50
39:08
39:15
39:18
Peaka
0:00
40:41
40:54
40:54
41:06
41:12
Peak*
0:00
40:42
Peak
0.
88-1.20
1
0
1
.14
.94
.01
0.30
2.41 1.17
217.46 109.39
0.973-1.027
0.000
1.24 0.978
108.07 1.000 13C12-HpCDD 678
IS7
219.87
0.
RO
RO
RO
RO
RO
RO
RO
RO
RO
RO
0.
RO
RO
RO
RO
RO
0.
RO
U^-TM
PV / e\~ •> • — ^nn •*»*) /T»
76-1.02
1
0
0
3
1
0
2
0
0
0
0
.00
.75
.75
.50
.67
.40
.00
.19
.71
.10
.31
0
0
0
0
0
0
0
0
0
0
0
0
.16
.19
.13
.04
.17
.04
.OS
.06
.11
.02
.08
.00
76-1.02
1
6
0
0
0
0
.00
.50
.75
.43
.50
.50
0
0
0
0
0
0
0
.16
.04
.06
.06
.08
.02
.00
76-1.02
1
0
.13
.85
0
.15
337.69 154.89
337
.69
0.902-1.098
0
0
0
0
0
0
0
0
0
0
0
.000
.900
.930
.932
.934
.949
.951
.954
.962
.964
.966
0.902-1.098
0
1
1
1
1
1
.000
.000 OCDD
.005
.005
.010
.012
AN
0.996-1.004
0
182.80 1
.000
.000 13C12-OCDD
IS8
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitola Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 2028 04/20/98
-------
Fag* No. 5 Listing of S982310B.dbf
04/20/98 Matched OC Peaks / Ratio / Ret. Tin*
Compound/
M_Z.... QC.Log Omit Why ..RT. OK Ratio Total.Area... Area.Peak.l. . Area.Peak.2.. Rel.RT Compound.Nam*.. ID.. Flags.
Column Description 'Why Cod* Description QC Log D*»c.
M_Z -Nominal Ion Mass(es) WL-Below Retention Tine Window A-Peak Added
..RT. -Retention Tin* (nmtss) WH-Above Retention Time Window X-Peak Kept
Rat.l -Ratio of M/M+2 Ions SH-Below Signal to Hois* Level D-Peak Deleted
OK -RO»Ratio Outside Limits
-------
ril*:S982310 tl-746 Aoq:18-APR-1998 15:13:36 SI+ Voltmg* SIX 70S
303.9016 r:2 BSOB(256,30,-3.0) TXD(9,5,S,0.05%,312.0,1.00\,f,T)
TKIKKGLE LABS T*xtiTLI*45399 M23-XB-1-4 IKT. TIMS - 15,16
1001
2.3(00 24(00 25,00 26(00
rilm:S982310 #1-746 Acq 11B-APX-1998 15:13:36 XI+ VoltMgm SIX 70S Nairn*:63
305.8987 T:2 BSUB(256,30,-3.0) FXD(9,5,5,0.05\f252.0,1.00\,T,T) ExptSDBSUS
TXIANGLE LABS T*xt:XLIt45399 K23-XB-1-4 XK7. 2XKB - 15(16
1001 A4.J2X3
23:00 24:00 25,00
ril*:S982310 tl-746 Acqsl8-APX-1998 15:13t36 EH- VoltAge SIX 70S Noi»e:81
315.9419 Ts2 BSUB(256, 30, -3.0) PJO>(9, 5,5,0.051,324.0,1.00\rf,T) Xxp:SDB5OS
TRIANGLE LABS T*xtsTLH4S399 M23-RB-1-4 IKT. TIKE - 15(16
1001 A1.90X6
80:
60:
40:
20:
o:
23:00 • 24:00 25(00 26(00
Til*:S9823lQ tl-746 AcqsLS-APR-1998 15:13:36 EI+ Voltmg* SIX 70S Soii9t7S
317.9389 F:2 BSUB(256,30,-3.0) PXD(9,5,5,0.OS\,312.0,1.00\,T,T) ExpiNDBSUS
TRIANGLE LABS T*xtiTLH45399 M23-XB-1-4 IKT. TIME - 15(16
1001 A2.54X6
80:
60:
40:
20:
o:
~r
-r
~r
23,00 24,00 25 .-00
Pile:3982310 tl-746 AcqtlS-APX-1998 15:13:36 EH- VoltMg* SIX 70S
330.9792 T:2 ExpilWBSUS
TRJANGir LABS Text:TLItt5399 H23-S3-1-4 IXJ. TIKE -
25114
^.24:25
1001
80:
60:
40:
20:
o:
26:00
15,16
-T
T
rr
23:00 24(00 25(00
ril*iS982310 tl-746 Acq:lt-APX-1998 15*13:36 XI* VoltMy* SIX 70S
375.8364 T:2 ExpiNDtSVS
TXIAJfSLE LABS T*lt:TLIt45399 M23-U-1-4 IKT. TIKE -
1001
26,00
15:16
00:
60:
40:
20:
0:
22,41
22,25
25,45
27(00
27(00
27:00
.0.0X0
Hm*\
27\00"
2«,22 a6, 46 27,09
23 i 00
44t00
25(00
26(00
27(00
5.2X5
,4.2X5
.3.1X5
.2.1X5
.1.0X5
.O.OZO
Tim*
.7.3X5
.5.8X5
.4.4X5
.2.9X5
.1.5X5
.0.0X0
Tim*
.8.5X5
.6.4X5
.4.2X5
.2.1X5
.0.0X0
Tim,
l.»X3
.1.4E3
.1.1X3
.7.1X2
.3.5X2
9.0X0
Tim*
3(
-------
Fila:S982310 tl-746 Acqtl8-APR-1998 15tl3t36
rj> Volt*o» srjf 70S Xoi*ei43
319.8965 r>2 BSUB(256,30,-3.0) PXD(7,5,3,0.05\,172.0,1.00\,r,T) XxptBDMSUS
TRIANGLX LABS ToxttTLIf 45399 K23-XB-1-4
1001
80:
60:
40:
20:
A3. 1813
A1.15E3
24:00 25:00
Fil*iS982310 tl-746 Acqil8-APR-1998 15tl3t36
IKJ. TIME •
A2.79IT3
jl
lAQ5Mw
26:00
IJ* Volttgm SIR 70S Hoi*ei52
15:16
-7.6*2
A1.57E3
UM|V^^
L6.XE2
14.6X2
'.3.1E2
'-1.5X2
• n arn
27<00 Timm
321.8936 Ti2 BSUB(256, 30, -3.0) PJ3>(7,S,3,O.OS\,208.0,1.00\,T,T) XxpiKDBSUS
TRIANGLE LABS TexttTLIt45399 M23-X3-1-4
100]
80;
60.
40:
20:
a-
A626.47
A2.21X3
UKT. TIME •
JU.87W
u* .tryt''
15 1!6
ft,tfY> °' '
M'L W/^/^?
'TVj-fr J^*idk*j\^l" *<3?'°sl( .A , 1.
24:00 25:00
File:S982310 tl-746 Acq:18-APR-1998 15:13:36
Sa/wir/VS9 823 10 tl-746 Aoq:18-APR-1998 15:13,36
330.9792 tt2 ExpsNDBSUS
TRIANGLE LABS Text:TLIt45399 M23-RB-1-4
1001
80.
60.
40.
20J
0:
„ „ ' 25,
"- - ^-ii~?A-j2iAj£? ** •' *2_^J___'v/
-v^-^- . -wx_^-^-XV
. ..
24:00 25:00
IW7. TIME -
A2.41E6
i C
' 26iOO
XH- Voltmgm SIX 70S
IKJ. TIME •
14 25i48 26 04
X,^v££j^£._xs^. y\
*1-'"1 I^'LJI»I'"» ^^^/^ \^A*^^V ^ A^
2«ioO
15:16
-6.7X5
.5.3X5
.4 . 0X5
.2.7X5
.1.3X5
27 1 00 Time
15:16
•\f • 77 ^ * J.£D
v^^*r~
.8.5X5
.6.4X5
.4.2X5
.2.1X5
27:00 ' !!••
366
-------
\TilmtS982310 tl-746 Acq,18-AFX-1998 15:13:36 XH- Volt*y* SIX 70S Hoimmt39
339.8S97 f,2 BSUB(256, 30, -3. 0) PXD( 7,5,3,0.05\,1S6.0,l.OO\,T,T) Xxp:«DB5OS
TSIAIKLX LUS T»xttXLIt45399 K23-U-1-4 ZXT. TIME - 15.15
IOC
38,00 39100 30tOO
rll»,S982310 tl-746 Acq,18-APX-199B 15,13,36 XH- VoltMyt 81* 70S Ho±*mt41
341.8567 r,2 BSVB(256,30, -3.0) PXD(7,5,3,0.OS\,16t .0,1.00\,T,T) XxptXDBSUS
TRIANGLE LUS T*Xt:TLH4S399 H23-XS-1-4 ZK7. TIMS -
1001
28tQO 39i00 30tOO
TilftS982310 41-746 Acq,18-APM-1998 15,13:36 X+ Voltig* SIM 70S Soit*,49
351.9000 f:2 SSUB(256, 30»-3. 0) PB>(7, 5,3,0.051,196.0,1.00\,r,T) XxptSPfSOS
TRIANGLE LABS Text:TLH45399 H23-RB-1-4 UU. TJMS - 15ilff
31,00
ion
so:
60:
40:
20:
o:
Al.
8E6
28,00 39tOO 30,00
ril»sS982310 tl-746 Acq,18-APX-1998 15:13,36 H+ Voltage SIX 70S B6im»,44 '
353.8970 r,2 BSOB(2S6, 30, -3. 0) PKD( 7,5, 3,0 .OS\,176.0,1.00\fT.,T) ExptKDSSOS
TSIANSLE LABS T*xt,TLI44S399 H33-SB-1-4 XK7. ITMT • 15>15
31:00
1003
so:
60:
40:
20:
o:
A1.20K6
28,0039,00 30iOO
rilf,S982310 tl-746 Acq:18-APS-1998 15:13:36 XI+ Voltage SIX 70S
330.9792 T,2 ExptNVBSVS
TRIANGLE LABS T*xt:TLIt45399 M23-SB-1-4 INJ. TlttX -
1001
Sl'iOO
15:16
80:
60:
40:
20:
0:
27,20
29,00 30:00
ril»iS982310 tl-746 Acq,18-APS-1998 15,13t36 H+ Volt*g* SIX 70S
409.7974 r,2 Exp,m>B5OS
aiAOGLX LABS T*xt,TLIt45399 H23-XB-1-4 OKT. TIME -
100\ 29146
80:
60:
40:
20:
o:
15,16
31:00
31 02
IBiOO
29\00
J0I00
Sl',00
5. 7K5
4.6X5
3.4X5
,2.3X5
.1.1X5
.0.0X0
£!••
.3.815
.3.0X5
.2.3X5
.1.5X5
.7.6X4
.0.0X0
Tim*
.1.1X6
.8. 7X5
.6.6X5
.4.4X5
.2.2X5
.0.0X0
Time
.1. 8X3
.1.4X3
.1. 1X3
,7.1X2
.3.5X2
.0.0X0
Timo
-------
0.0*0
28:24 28':36"28:48' 29':b6 29:12' 29:24 ' 29\ 36 "29\4» "st'iOO ' 30*12' 3b':24 ' So'i 36' 30t48' Jl'iOO 3l'il2 Tim
•ile:S982310 fl-746 Acq:18-APX-1998 15:13:36 EI+ Voltmge SIX 70S XOiie:39
357.8516 T:2 BSOB(256,30, -3.0) PKD(7,5,3,0.051,156.0,1.00\,r,T) Exp:BDB5US
TXIAWBLE LABS Text:TLIf45399 M23-XB-1-4 BET. TIMX '15:16
1001 ^5.3X2
fl-746 Acg:18-APX-l998 15:13:36 B* Voltag* SI* JOS
55.8546 T:2 BSOB(256,30, -3.0) PKD(7,S,3,O.OS\,152.0,1.00\,r,T) XxptmtSOS
TXIAJKLE LABS Text:TLIf45399 M23-XB-1-4 OKT. TIMX - 15ilff
A2.20E3
80.
60.
40.
20.
A456.62
ro.oxo
29': 12 29': 24 ' '29\'36 '2a\4B"3oYoO 30\12 3o':24' 3o':36 30':4e' Jl:b6' 31:12 Tim*
r±l*:S982310 fl-746 Acq:18-APX-1998 15:13:36 XH- Voltage SIX 70S HOime:42
367.8949 T:2 BSOB(256,30, -3.0) PKD(7,5,3,0.05\,168.0,1.00\,r,T) XxptKDBSUS
TXIAHGLE LABS Text:TLIf45399 M23-SB-1-4 OCT. TIME " 15:16
1001 A1.24I6
00:
6o:
40.
20:
OSES
.4.0X5
13.2X5
.2.4X5
.1. 6E5
.7.9X4
0.0X0
28t24 ' 2B\36 28t48 29tOO.> 29:12 29s24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 Ti»«
rll*:S982310 fl-746 Adj:18-APX-1998 15:13:36 fl+ Volt«gr» SIS 70S Xoi*»>44
369.8919 Tt2 BSUB(256, 30, -3.0) PKD(7, 5,3, 0.051,176.0,1.00\,r,T) XxptNDBSUS
TXIASSLE LABS Text:TLIt45399 M23-RB-1-4 IKT. TIKE - 15»15
10 0\ At.40X5 ,.2.7X5
80.
60.
40.
20.
7.26X4
.2.2X5
.1. 6X5
.1.1X5
.5.4X4
0.0X0
28:24'28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 Ti*<
rile:S982310 fl-746 Acq:18-APX-1998 15:13:36 EI+ Voltaff* SIX 70S
330.9792 T:2 XxptSDBSOS
TXIAJKLE LABS Tert:TLIf45399 H23-XB-1-4 UC7. TIME - 15:16
1001
"J0«50 31:07
80.
60.
40.
20.
.8.7X5
.6.6X5
.4.4X5
.2.2X5
0.0X0
28:24 28:36 28:48 29:00 29:12 29:24 29:36 29:48 30:00 30:12 30:24 30:36 30:48 31:00 31:12 Time
368
-------
'ile:S982310 tl-465 Aaq:18-APX-1998 15:13,36 XI + Voltag* SIS 70S Boi*»:44
73.8208 rs3 BSOB(256,30, -3.0) PKD(7,5,3,0.05\, 176.0,1.00\,r,T) ExpiHDBSUS
TRIANGLE LABS T*xt:TLH45399 M23-X3-1-4 OKT. TIME " IStlf
10MA530.26
31:36 31t48 32iOO 32tl2 32t24 32t36 32t48 33tOO 33,It 33,24 33,36 33i48 34iOO 34>12 34',24 34',36
rll»:S982310 tl-465 Aoqtl8-APX-1998 15*13,36 XH- Voltage SIX 705 *>i*mi48
375.8178 Tt3 BSWI(256r30, -3.0) PKD(7,5,3,0.OS\, 192.0,1.00\,T,T) KxptXDBSas
TXIAJKLX LABS T*xtiTLIH5399 H23-XB-1-4 OCT. TOtf - 15,16
ion
31:36 31:48 32,00 32,12 32:24 32:36 32:48 33,00 33:12 33:24 33,36 33,48 34,00 34:12 34,24 34:36
rile:S982310 tl-465 Aoj:18-APX-1998 15,13,36 EI+ Voltigw SIX 70S Bain:66
383.8639 f:3 BSffB(256, 30, -3. 0) PXD(7,5,3, 0.051,264.0,1.00\,r,T) IxptXDBSVS
TRIANGLE LABS T*xt:TLIt45399 H23-XB-1-4 ZX7. TIME - 15:16
A1.41E3 A180.60
481.48
1001
80:
40:
20:
o:
A1.01E6
A1.10I6
A8.70X5
31':36 31,48 32:00 32:12 32:24 32:36 32:48 33,00 33:12 33:24 33:36 33:48 34:00 34:12 34:24 34,36
ril»:S982310 tl-465 Acqtl8-APX-1998 15:13:36 tl+ Volt*g» SIX 70S Hoimti74
385.8610 F,3 BSUB(2S6,30,-3.0) PKD(7,5,3,0.05\,296.0,1.00\,T,T) KjcptHDBSVS
TEIASGLX LABS T*xt,TLH45399 M23-BB-1-4 OUT. Ufa ' 15,16
1004 A2.Q2E6 A2.J.8E6
80:
eo:
40:
20:
o:
Al.72E6
5,
.4,
'.3,
:2.
.1.
34,24 34,36
31,36 31:48 32,00 32,12 32,24 32,36 32,40 33,00 33:12 33:24 33,36 33,48 34,00 34,12
ril»,S982310 tl-465 Acq,18-APR-1998 15,13,36 EI+ Voltag* SIS 70S
392.9760 r,3 Sxp,NDB5US
TRIANGLE LABS T*xt,TLH45399 K23-XB-1-4 XXT. TOO; - 15:16
1003
80:
60:
40:
20:
31,36 31t48 32tOO 32,12 32:24 32,36 32,48 33,00 33il2 33,24 33,36\33i4ia' 34,00 34\ 12 34',24 34\36
rilm:S982310 il-465 Acq,18-APX-1998 15,13,36 11+ Volta?* SIX 70S
445.7555 ft3 ExptNBBSUS
TRIANGLE LABS T*xtiTLH45399 K23-XB-1-4 XJK7. TIKE - 15,16
34108
l*ii«' 32:1432:24 32:37 32,52 j^^L^jL?!" 33'*7ff^3J^^J*-34i27
*~" '>-^^V—vVV^m^JVV*A^~V -W*~ .A^L^v-u^^vV"
r-S
.4
.3
.2
.1
0
OEO
Time
0X5
4X5
8X5
2E5
9E4
.0X0
Time
8E5
7E5
.5E5
.3X5
.2E5
.OEO
Time
.4X5
.3X5
.2X5
.2E5
.1X5
.OEO
100]
80:
60:
40:
20:
0:
31:50
32:06
32,26
32,55
32,47 I ",07
33,25
3,37 33:48
34,28
31:36 31,48 32,00 32:12 32,24 32,36 32:48 33:00 33,12 33:24 33:36 33:48 34,00 34,12 34,24 34:36
6E3
3E3
7X2
5X2
.2X2
.0X0
Tlmi
36
-------
fUe:S98S310 H-4S5 Acq:lB-APx-19SB 15.-I3.Jf H+ Voltmg* Sit 70S Hoim.,44
389.8156 T:3 BSUB(256,30, -3. 0) PXD(7,5, 3,0.05\,176.0,1.00\,r,T) Xxp:JO)B5US
TRIANGLE LABS T»xt:TLIt45399 M23-XB-1-4 OJ. TIMX - 15tl6
1001 A3.22X3
32:12 32,24 32i36 32i48 33iOO 33tl2 33i24 33>36 33i48 34tOO 34tl2
T±l»tS982310 tl-465 AcqtlB-APS-1998 15:13:36 11+ Volt*g» SIX 70S *oi**s36
391.8127 F:3 BSUB(256,30,-3.0) PKD(7,5,3,0.05\,144.0,1.00\,r,T) Xxp:HDB5US
TRIANGLE LABS T»xttTLH45399 H23-SS-1-4 OCT. THIS » 15:16
1001 Al. 2E3
80.
60.
40.
20.
32,12 32t24 32:36 32i48 33,00 33:12 33:24 33:36 33:48
rile,S982310 H-465 AcqtlS-APX-1998 15:13:36 II + Volt*y» SIX 70S Boi*»:68
401.8558 r:3 BSUS(256,30,-3.0) fXD(7,5,3,0.05\,272.0,1.00\,r,T) XxpiKDBSUS
TRIANGLE LABS T»xtiTLIf45399 H23-RB-1-4 1X7. ZZME - 15ilff
1001 A1.59E6
7.1X2
5.7X2
4.3X2
2.8X2
1. 4X2
.0.0X0
34100 34112
80.
eo:
40.
20.
A1.44X6
32:12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48
File:S982310 tl-465 Acq:ia-APX-1998 15:13:36 EI+ Volttgm SIX 70S tfoim»:43
403.8529 T:3 BSUB(256,30^-3.0) PKD(7, 5,3, 0.05\,172.0,1.00\,T,T) fxpsSDBSUS
TXIANGLS LABS Text:TLH45399 M23-XB-1-4 JXT. TZMC • 15:16
A1.33E6
34tOO 34t12
ao:
so:
40:
20.
OJ
32,12 32:24 32:36 32:48 33:00 33:12 33:24 33:36 33:48 34:00
rile,S982310 tl-465 Acq, IB-APR-1998 15:13:36 XI+ Volt*g» SIX 70S
392.9760 r,3 XxpiKDBSVS
TRIANGLE LABS TeJCt:TLIt4S399 M23-XB-1-4 ZK7. TIME - 15.16
1001
32,14 32,24 32,37 32i52 ~_^V_ #»•" 33,37
"v^-Aj
ao.
so:
40.
20:
o:
34:12
'32,12 '32,24 ' '32:36 32',48 ' 33\66 ' '33\12 ' '33,24 ' '33\36 ' 33,48 ' 34',00
34:12
4.1X5
3.3X5
2.5X5
1. 6X5
.8.2X4
0.0X0
Time
3. 4X5
2.8X5
2.1X5
1.4X5
6.9X4
0.0X0
Time
5.4X5
4.3X5
3.2X5
2.2X5
1.1X5
0.0X0
Time
370
-------
ile,S982310 #1-569 Aeq,18~APX-1998 15,13,36 XI+ Volttg* SIR 70S Woif*,64
07.7818 F,4 BSUB(256,30,-3.0) PXD( 7,5, 3, 0.05%, 256.0,1.00%,?, I) XxptMDSSUS
TXIANCLE 1JUS Text, TLH4 5399 M23-ja-l-4 Off. TIME - 15iltf
003
sol
35',48 36': 00 36,12 36:24 36,36 36,48 37,00 37,12 37,24 37,36 37,48
T±l»iS982310 tl-569 Aoq,18-APX-1998 15,13,36 EI+ Volt*g» SIX 70S moif»,79
09.7789 T,4 SSVS(256,30,-3.0) PKD(7 ,5,3,0.05\,316,0,1.00\,T,T) fxpiHDBSUS
TRIANGLE LASS Ttat,TLIt45399 M23-XS-1-4 OKT. TIME - 15,16
100*
35,48 36,00 36,12 36,24 36,36 36,48 37,00 37,12 37,24
rilt,S982310 tl-569 Acq:18-APX-1998 15,13,36 EH- Volttg* SIX 70S Boim»i69
417.8253 T,4 BSO3(256,30, -3. 0) PKD(7,5,3,0.05\,276.0,1.00\,T,T) JEzpiNDBSOS
TRIANGLE LASS T*xt:TLH45399 M23-XS-1-4 HKT. TIME - 15,16
1003LA6.01E5
50:
40:
201
A859.32
A^^^^
37,36 37,48
00:
tfO:
40.
20:
A4.68E5
35,48 36,00 36,12 36,24 36,36 36,48 37,00 37,12 37,24
ril*:S982310 tl-569 Acq:18-APK-1998 15:13,36 EH- Voltage SIX 70S Hoimmi74
419.8220 r,4 SSUS(256,30,-3.0) PXS(7,5, 3, 0. OS\,296.0,1. 00\,T,T) ExptODSSUS
TSIAHBLE LASS T9Xt,TLIf4'5399 M23-XS-1-4 OCT. TIME " 15,16
1003LA1.44E6
37,36 37,48
80:
50:
40:
20:
AI.0515
37,24
35,48 36,00 36,12 36,24 36,36 36,48 37,00 37,12
rilf,S982310 tl-569 Acq,18-APX-1998 15,13,36 EH- Volt*y» SIX 70S
430.9729 F,4 ExpiNDBSUS
TRIANGLE LASS Tert.-ZXIM5.3SS H23-RB-1-4 UKT. TIME - 15,16
100]
80:
50:
40:
20.
37,36 37,48
35,48 36,00 36,12 36,24 36,36 36,48 37,00 37,12
rilf ,3982310 H-S69 Acqil8-APX-1998 15,13,36 EI+ Voltage SIB 70S
479.7155 F,4 Exp,KDBSOS
TRIANGLE LASS TmxtiTLH45399 M23-XS-1-4 ISJ. TIME * 15,16
100\
36,11
37,24 37,36 37,48
80:
50:
40:
20:
o:
36,22
36,54
37*16
\35s51
36:07
36,3.
37105
37,411
1. 8E3
1.5E3
.1.1E3
.7.412
.3.7E2
.0.0X0
.1.2E5
.9.7E4
.7.3E4
.4.9E4
.2.414
O.OEO
Tim
^3.0X5
.2.4X5
.1. 8X5
.1.2X5
.5.9X4
O.OEO
35,48
36:00 36,12 36,24 36,36 36,48
37,00
37,12 37:24 37,36 37,48
3.6X5
2.9X5
.2.2X5
.1. 5X5
.7.3X4
.0.0X0
Time
.1. 7X3
.1.4X3
.1. 0X3
.6.8X2
.3. 4X2
.0.0X0
Tim*
-------
Tile:S9W310 #1-569 Acq:18-AfS-1998 1S:1J:J6 K-t- Volbty. Sit 70S
423.7766 Ts4 BSOB(256,30, -3. 0) PKD(7,5,3,O.OS\,204.0l1.00\,r,T) Xxp:lO>B5US
TXIASGLE LASS T*xt:TLH4S399 M23-SB-1-4 IJKT. TIMS - 15tl6
1003, A3.97X3
so:
60.
40.
20.
36,00 36:06 36:12 36,18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37t06 37tl2 37:18
rilt:S982310 41-569 AtnjilS-APX-1998 15,13:36 EH- Voltage SIS 70S Moif»:39
425.7737 T:4 BSOB(256r30,-3.0) PKD(7, 5,3 , 0.05\, 156.0,1.00\,T,T) XxptXDBSUS
TXI ANGLE LASS Text :TLH4 5399 M23-SB-1-4 ZIK7. TIME - 15s 16
1001
ao:
36,00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
ril»iS982310 #1-569 Acq:18-APK-1998 15:13:36 EI+ VoZtag* SIS 70S KOifft78
435.8169 T:4 3SUB(256,30,-3.0) PXD(7,5,3, 0.05%,312.0,1.00\,T, T) Elp:KDB5US
TRIANGLE LABS Text:TLIt4S399 M23-XB-1-4 IUJ. TIME - 15:16
1001 A1.Q9E6
80.
60.
40.
20.
0..
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37:12 37:18
Flle:S9B2310 fl-569 Acq:18-APX-1998 15:13:36 EI+ Voltage SIS 70S Hoist: 70
437.8140 T:4 BSUB(256,30,'-3.0) PXL(7,5,3,0. 05\,280. 0,1,00\,T, T) Ezp:m>B5US
TRIANGLE LASS Text:TLI*45399 M23-SB-1-4 IK7. TIME - 15:16
1004 Al.
80J
50:
40:
20:
36:00 36:06 36il2 36:18 36:24 36:30 36:36 36:42 36:48 36:54 37:00 37:06 37112 37:18
FU.»:S982310 H-569 Acq,lS-APS-1998 15:13:36 EI+ Voltage SIX 70S
430.9729 t:4 ExpsNDBSUS
TRIANGLE LASS TfXtiTLI*4S399 M23-KB-1-4 IJKT. TIME ' 15:16
36:0836:14 . Jtfl<1 36L53 .37L08 37,19
80.
60.
40.
20.
1.2E3
9. 8E2
7.4E2
4.9E2
.2.5E2
.0.0X0
T±mm\
36:00 36:06 36:12 36:18 36:24 36:30 36:36 36t42 36:48 36:54 37tOO 37:06 37\12 37\18
0.0X0
Tim*
.1. 6X5
.1.3X5
.9. 7X4
.6.5X4
.3.2X4
.0.0X0
Time
.1. 6X5
.1.3X5
.9. 5X4
.6.3X4
.3.2X4
.0.0X0
T±m»
.3.5X5
.2.8X5
.2.1X5
.1.4X5
.7.0X4
.0.0X0
Timm
3^»O
< d
-------
1 ile,S9823l6 U-569 Acq:l8-AP*-l996 13,13,31 11+ Volttg* SIM 70S Jtoi*«.4l 1
441.7428 T»4 SSOS(256,30,-3.0) PXD(7 , 5,3,0 .05\, 164 .0,1. 00\,T,T) ErpsJQWSOS
TXIAKSLX LASS T**tiTLZ*45399 H33-XS-1-4 IKT. TIME • 15(10
004 -.2.4X4
901
801
701
601
501
401
301
201
10:
rum
443.
TXIAi
lOOi
901
801
701
601
501
401
301
201
10J
nit
430.
TXIA
1003
901
801
701
fol
501
401
30;
20;
10.
0
Tilt
513.
TXIf
loot
90.
80.
70.
60.
50.
40.
30.
20.
10.
0.
. . . - _ j.
36:00 ' 37:00 38,00 39,00 40,00 41:00 42:00
-.5982310 H-569 Acq:18-APX-1998 15,13,36 XI* Volt»g» SIX 70S tfoimmi41
7399 T:4 SSUS(256,30,-3.0) fJX>(7 , 5,3,0 .05\, 164 .0,1. 00\,T,T) XlptKDBSOS
NGLX LASS yat:TLH45399 K23-XS-1-4 IKT. TIMX - 15,16
- i •• - f- -r r -•] r1 <•
1 .. ... IL
36,00 ' 37:00 38:00 39:00 40:00 ' 41iOO ' ' 42\00
,3982310 H-569 Aeqil8-APX-1998 15:13:36 EH- Voltaya SIS 70S
9729 Tt4 XJCptJO>S5as
VGLX LASS Tmxt:TLIHS399 H33-XS-1-4 IKT. TIMX - 15,16
^^^V^A^v^^
36:00 37:00 38s 00 39:00
,2982310 tl-569 Aeq:18-APX-1998 15:13:36 SI+ Voltage
6775 f,4 XxptltDSSUS
OKLX LASS T»XtiTLIt4S399 H23-XS-1-4
f'd6 L 37'34 39(06 ^ 3»03
«te & _/rt\ii _ Jl» fvH ^j^t^A *L^nA^Lt _^_ fLJLi^j^TJ^ jVYA^AALlrftfflUifi
l*v^A^l^^T^J™"*^ '^^^M^ft^vvV^Tp**^^>w^v>1*r^V^^V^v^'**^v^^^^^'
iff loo jrlob ' * ' jaioo ' ' ' isloo
SIR 70S
IKT. TIMX
39i49 40,16
40<00
41:00 ' 45*00
15.16
-JLv-^j^iUflk,«^^^^
41 100 42'tOO
.2.2X4
.1.9X4
.1.7X4
.1.4X4
.1.3X4
.9.6X3
.7.3X3
.4.8X3
.3.4X3
0.0X0
Time
-1.7X4
J..6X4
.1 . 4X4
.1.3X4
.1.0X4
.8.7X3
.7.0X3
.5.3X3
.3.5X3
J..7X3
Tim*
-3.6X5
'•.3.3X5
'.2.9XS
.3.6X5
.2.2X5
.1.8X5
il.SXS
11.1X5
.7.3X4
.3.6X4
0.0X0
-3.8X3
.3.5X3
.3.1X3
.2. 7X3
.3.3X3
.1.9X3
.1.5X3
.1.2X3
-.7.7X3
.3.8X2
0.0X0
Tim»
-------
rile>S99231Q #1-569 Aoq:18-AfS-lS98 15:11:16 EI+ VoltMfft SIX 70S MoimeiJS
457.7377 Ti4 BSOB(256,30, -3.0) PXD(7,5,3, 0. 05%, 156. 0,1. 00\,r,T) ExptUDBSUS
TXIANGLX LABS T*xt:TLI#45399 M23-SB-1-4 IJKT. TIME - 15:16
1001 A1.34X3
80.
60.
40.
20.
40i36 40:42 40:48 40:54 41:00 41:06
F±l»tS982310 #1-569 Acq:18-APS-1998 15:13:36 XT* Voltlf* SIS 70S Soite:38
459.7348 T:4 BSUB(256,30r-3.0) PH>(7, 5,3, 0.05\, 152.0,1. 00\,F,T) XxpsHDBSOS
TRIANGLE LABS Text:TLI#45399 H23-SB-1-4 IJKT. TIKE - 15:16
A245.59
80.
60.
40.
20.
40 36 40:42 40:48 40:54 41,00 41:06
File :S9 83310 il-569 Acqtl8-APS-1998 15:13:36 EI+ Voltafff SIS 70S Hoi ft-.43
469.7779 f:4 BSUS(256,30,-3.0) PXD(7,5,3,0.05\,172.0,1.00\,f,T) ExpsXDBSUS
TXIAXGLX LABS T*xt:TLH45399 H23-U-1-4 JWJ. TIME - 15:16
1001 A1.5.5E6
ao:
50:
40.
20:
40 36 40:42 - 40:48 40:54 41:00 41:06
rile:S982310 #1-569 Acq:18-APS-1998 15:13:36 EI+ Voltage SIX 70S Hoima:41
471.7750 T-.4 BSUB(256,30^-3:0) PXD(7,5,3, 0.05\,164. 0,1. 00\,r,T) Exp:NDB5DS
TRIANGLE LABS Text:TLIt4S399 M23-SB-1-4 TWJ. TIME - 15:16
10 OS A1.J3E6
40 36 40:42 40:48 40:54 41:00 41,06
ril»:S982310 #1-569 Acq: 18-ATB-199I 15:13,36 EH- Voltay* SIX 70S
430.9729 F:4 ExpiNDBSOS
TRIANGLE LABS Text:TLI#45399 M23-U-1-4 ZtTJ. TIME - 15sIff
1001
80.
60.
40.
lit 00
41s 08
40 36
40:42
40:48
40 > 54
41:00
41 i Off
41112
41112
41112
41:12
.3.5X2
'.2.8X2
12.JJS2
.1.4X2
.6.9X1
0.0X0
,.2. 7E2
.2.2X2
.1. 6X2
.1.1X2
.5.5X1
.0.0X0
Timt
1.7X5
.1.3X5
'.9.9E4
.6.6X4
'.3.3X4
0.0X0
Tint
-1.9X5
.1.5X5
-1.2XS
'.7.7X4
'-3.9E4
.0.0X0
Time
3.5X5
2.8X5
2.1X5
1.4X5
7.0X4
0.0X0
Time
-------
CO
-------
CALIBRATION
DATA
*01Capfloto0rfv»
Durh*m,NC 27713-4411
919-544-5729
P.O. Box 13485
Fix i 919444-5491
-------
Initial Calibration Summary for UPS 1058
Analysis Data : 01/05/98
Instrument : U
Analytes
Total MCDF
Total MCDD
Total DCDF
Total BCDD
Total TriCDF
Total TriCDD
1368-TCDF
2378-TCDF
TOTAL TCDF
1363-TCDD
1379-TCDD
2378-TCDD
TOTAL TCDD
12373-PeCEF
23473-PeCDF
•TOTAL PeCDF
12373-PeCDD
TOTAL PeCDD
123478-KxCD?
123678-HxCDF
234678-HxCDF
123789-HxCDF
TOTAL HxCDF
'123478-HxCDD
123673-HxCDD
123739-HxCDD
TOTAL HxCDD
1234678-HpCDF
1234789-HpCDF
TOTAL HpCDF
1234678-HpCDD
TOTAL HpCDD
OCDF
OCDD
Other Standards
37C1-TCDD
13C12-PeCDF 234
13C12-HxCDF 478
13C12-HxCDF 234
13C12-HxCDF 789
13C12-HxCDD 478
13C12-HpCDF 789
RF SD
0.000 0.000
0.000 0.000
0.000 0.000
0.000 0.000
0.000 0.000
0.000 0.000
1.298 0.073
1.240 0.132
1.240 0.132
0.715 0.032
0.360 0.021
1.240 0.160
1.240 0.160
1.051 0.090
1.019 0.073
1.025 0.084
1.32 0.125
1.32 0.125
l.OC 0.074
1.25 0.089
0.935 0.082
0.870 0.047
1.029 0.071
0.755 0 .051
0.975 0.079
0.941 0.063
0.894 0.064
1.413 0.098
1.095 0.071
1.252 0.084
0.995 0.051
0.995 0.051
1.377 0.070
1.103 0.080
%RSD
100%
100%
100%
100%
100%
100%
6%
11%
11%
4%
6%
13%
13%
9%
8%
8%
9%
9%
7%
7%
3%
5%
7%
7%
8%
7%
7%
7%
6%
7%
5%
5%
5%
7%
RF
SD
1.001 0.056
0.966 0.010
0.825 0.042
0.902 0.043
0.695 0.042
0.732 0.024
0.802 0.016
%RSD
6%
1%
5%
5%
6%
3%
2%
»m*m
RT
21:26
24:36
22:46
23:10
25:19
28:33
29:14
29:34
32:01
32:07
32:26
33:22
RT/LO
4:35
5:18
11:35
12:18
15:35
17:
23:
24:
24:
25:
23:
18
35
18
32
34
06
RT/HI Ratiol Ratio2
18:35
19:18
19:35
20:18
22:35
23:
30:
31:
32:
33:
36:
18
35
18
32
24
06
0.
0.
0.
0.
0.
0.
0.
1.
1.
1.
1.
1.
1.
745
743
744
776
786
737
781
525
520
523
530
530
232
1.245
1.
1.
.252
.252
1.262
32:42
32:47
33:05
35:00
36:31
36:01
39:47
39:35
RT
25:19
29:14
32:01
32:35
33:21
32:42
36:30
28
30
32
35
35
:47
:59
:00
:34
:34
RT/LO
23
26
:18
:32
32:59
36
38
40
43
43
:47
:59
:00
:34
:34
RT/HI
27
30
38
:18
:32
:59
1.257
1
1
1
1
1
1
1
1
0
0
.211
.234
.232
.060
.049
.055
.023
.023
.891
.836
Ratiol Ratio2
1
0
0
0
1
0
.498
.509
.508
.504
.214
.431
N
0
0
0
0
0
0
6
6
6
6
6
6
6
5
Q
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
N
6
6
6
6
6
6
6
Page
Triangle Laboratories, Inc.® Analytical Services Division
801 Capttola Drive • Durham. North Carolina 27713
Printed: 15
-------
%RSD
4%
4%
7%
8%
3%
2%
2%
2%
7%
Recovery Standards RF SD %RSD
13C12-1234-TCDD l.OQQ O.QQO 0%
13C12-HxCDD 789 1.000 0.000 0%
*** End of Report *»*
Cateroal Standards
L3C12-2378-TCDF
L3C12-2378-TCDD
L3C12-PeCDP 123
L3C12-PeCDD 123
13C12-HXCDF 678
13C12-HxCDD 678
13C12-HpCDF 678
13C12-HpCDD 678
13C12-OCDD
RF
1.467
1.118
1.142
0.590
1.346
0.995
0.822
0.726
0.545
SD
0.053
0.049
0.075
0.045
0.033
0.017
0.013
0.011
0.038
RT
24:35
25:18
28:32
29:34
32:06
32:47
34:59
36:00
39:34
RT/LQ
23:35
23:18
24:32
25:34
28:06
31:47
32:59
35:00
37:34
RT/HI
25:35
27:18
32:32
33:34
36:06
33:47
38:59
37:00
41:34
Ratio 1
0.755
0.807
1.478
1.506
0.506
1.216
0.434
1.018
0.861
Ratio2
RT
25:08
33:05
RT/LO RT/HI
Ratio1
0.812
1.210
Ratio2
H
6
6
6
6
6
6
6
6
6
N
6
6
Page
fangte Laboratories, toc^ Anatytfcsi Services Division
1 CaptobOriv«*Duri«fn. North Cuofca 27713
ena: (919) 544-5729 • Fax: (919) 544-5491
Printed: 15.16
O ( <
-------
Continuing Calibration for 0980771
Init Calibration.
ICal Date
Analyte Sunmazy
Name
Total MO2F
Total MCDD
Total DCDF
Total DCDD
Total TriCDF
Total TriCDD
1368-TCDF
2378-TCDF
TOTAL TCDF
1368-TCDD
1379-TCDD
2378-TCDD
TOTAL TCDD
12378-PeCDF
23478-PeCDF
TOTAL PeCDF
12378-PeCDD
TOTAL PeCDD
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
• DI* XHStjrxnBWXt
: UF51058
• 01/05/98
Sti
i.Conc
.. : O
.
10.00
ICal Delta
RF Ratio RT RT Rel. RT RF RF %D
It2 Lo/High
0.000 3:22 0.000 0.000 100.0%
17:22
0.000 4:08 0.000 0.000 100.0%
18:08
0.000 10:22 0.000 0.000 100.0%
18:22
0.000 11:08 0.000 0.000 100.0%
19 : 08
0.000 14:22 0.000 0.000 100.0%
21:22
0.000 16:08 0.000 0.000 100.0%
1.285
1.227
1.227
0.702
0.321
1.125
1.125
1.081
1.056
1.069
1.250
1.250
1.210
1.267
1.053
1.031
0.76
0.77
0.76
0.79
0.78
0.78
0.78
1.51
1.49
1.50
1.61
1.61
1.26
1.24
1.28
1.30
22 : 08
19:43 19:55 0.8524
25:22
23:23 1.0007
21:12 21:24
25:20
21:50
24:09
25:16 27:34
29:26
28:18
26:35 28:39
29:17
30:00 31:10
32:44
31:17
31:46
32:30
Page 1
0.8867
0.9047
1.0007
1.0006
1.0272
1.0000
0.9968
1.0005
1.0160
1.0394
1.298 -0.013
1.240 -0.013
1.240
0.715
0.360
1.240
1.240
1.051
1.019
1.035
1.333
1.333
1.007
1.253
0.985
0.870
-0.013
-0.013
-0.039
-0.115
-0.115
0.030
0.037
0.034
-0.083
-0.083
0.203
0.014
0.068
0.161
-1.0%
-1.1%
-1.1%
-1.9%
-10.3%
-9.3%
-9.3%
2.9%
3.6%
3.2%
-6.2%
-6.2%
20.2%
1.1%
6.9%
18.5%
Triangle Laboratories, Inc.® Analytical Service* Division
801 Capitola Drive • Durham. North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 14:20 04/15/9
-------
Date: 04/13/98
TOTAL HxCDF
123 47 8 -HxCDD
123678-HxCDD
123789-HxCDD
TOTAL HxCDD
1234678-HpCDF
123 47 8 9 -HpCDF
TOTAL HpCDF
1234678-HpCDD
TOTAL HpCDD
OCDF
OCDD
TRXANQUe UABORATOfUKS OF RTF, IMC.
Continuing Calibration Cor U980771
1.140 1.27 1.029 0.111
0.878 1.21 30:31 31:53 0.9979 0.765 0.113
32:24
0.916 1.22 31:58 1.0005 0.976 -0.060
0.910 1.22 32:16 1.0099 0.941 -0.031
0.901
1.377
1.115
1.246
1.008
1.008
1.279
1.001
1.21
1.06
1.06
1.06
1.02
1.02
0.91
0.87
33:
35:
34:
35:
34:
42:
34:
42:
54
41
10
13
23
23
23
23
34:05
35:31
35:04
38:34
38:24
1.0005
1.0426
1.0005
1.0048
1.0004
Other Standard Summary
Name
37C1-TCDD
13C12-PeCDF 234
13C12 -HxCDF 478
13C12-HXCDF 234
13C12 -HxCDF 789
13C12 -HxCDD 478
13C12 -HpCDF 789
RF
0.972
0.932
1.005
0.977
0.834
0.939
0.866
Ratio
112
RT
RT
Rel. RT
0.894
1.410
1.096
1.253
0.995
0.995
1.377
1.108
ICal
RF
0.007
-0.033
0.019
-0.007
0.013
0.013
-0.098
-0.107
Delta
RF
10.8%
14.8%
-6.1%
-3.3%
0.
-2.
1.
-0.
1.
1.
-7.
-9.
%D
8%
3%
7%
6%
3%
3%
1%
6%
Lo/High
22:08
1.47
0.51
0.50
0.49
1.20
0.42
26
23
31
32
:08
:33
:33
:04
24:09
28:17
31:10
31:46
32:30
31:53
35:31
1.0007
1.0266
0.9968
1.0160
1.0394
0.9979
1.0426
1.001
0.966
0.825
0.902
0.695
0.732
0.802
-0.029
-0.034
0.180
0.075
0.139
0.207
0.064
-2
-3
21
8
20
28
8
.9%
.5%
.9%
.3%
.0%
.3%
.0%
.38:04
Internal Standard Summary
Name RF Ratio
1&2
13C12-2378-TCDF 1.484 0.76
ICal
Rel. RT RF
13C12-2378-TCDD
13C12-PeCDF
1.121 0.81
1.085 1.49
RT RT
Lo/High
22:22 23:22 1.0000
24:22
22:08 24:08 1.0000
26:08
23:33 27:33 1.0000
31:33
Page 2
Delta
RF
%D
1.467 0.017 1.2%
1.118 0.003 0.2%
1.142 -0.057 -5.0%
Triangle Laboratories, Inc.® Analytical Services Division
801 Capitoia Drive • Durham, North Carolina 27713
Phone: (919) 544-5729 • Fax: (919) 544-5491
Printed: 14:20 04/1
VfC
-------
13C12-P«CDD 123
13C12-HXCDF S78 1.289 0.51
13C12-HXCDD 678 1.043 1.23
13C12-HpCDF 678 0.879 0.43
13C12-HJ?CDD 678 0.741 1.06
13C12-OCDD 0.569 0.88
Continuing Calibration for 0980771
0.607 1.46 24:39 28:39 1.0000 0.590 0.017 2.8%
32:39
27:16 31:16 1.0000 1.346 -0.057 -4.3%
35:16
30:57 31:57 1.0000 0.995 0.048 4.8%
32:57
32:04 34:04 1.0000 0.822 0.057 6.9%
38:04
34:03 35:03 1.0000 0.726 0.015 2.1%
36:03
38:12 38:23 1.0000 0.545 0.024 4.3%
38:32
Recovery Standard Sunmary
Name RF Ratio
1*2
13C12-1234-TCDD 1.000 0.82
13C12-HXCDD 789 1.000 1.20
ICal
Ral. RT RF
RT RT
Lo/High
23:56 0.9917
32:15 1.0094
Delta
RF
1.000 0.000
1.000 0.000
%D
0.0%
0.0%
QC Front End Check:
1.5693
Page
Triangle Laboratories, Inc.® Analytical Services Division
801 CapHola Drive • Durham, North CaroBna 27713
Phone: <919) 544-5729 • Fax: (919) 544-5491
Printed: 1420 04/1 &
-------
Appendix B.2
Method 26A Analytical Reports
-------
TECHNICAL REPORT
Client: Pacific Environmental Services, Inc.
Purchase Order No.: 104-98-0175
RTI Project No.: 7048-03E
Date: April 23,1998
By
KateK.Luk
Research Triangle Institute
Post Office Box 12194
3040 Cornwallis Road
Research Triangle Park, NC 27709
(919) 541-6569
Submitted to:
Frank Phoenix
Pacific Environmental services, Inc.
5001 South Miami Blvd., Suite 300
RIP, NC 27709-2077
/RTI
-------
INTRODUCTION
Six impinger samples were received under Purchase No. 104-98-0175 on April 9,
1998 for K, Ca, Mg, Na, and Al analyses .
ANALYSIS
The samples were analyzed as follows:
Digestion Method - None
Instrumentation - Leemans Plasma Spec ICP and V.G. Plasma Quad P2
ICP/MS
Measurement Method - ICP/ AES
QA/QC - Duplicates, spikes, blanks, and calibration check solutions
were used
RESULTS
See Tables 1-4
COMMENTS
No problems encountered.
SAMPLE CUSTODY
Samples will be kept for 3 months after report is delivered.
Page 1 of3
/RTI
-------
RTI Project No.: 7048-03E
Samples: Impinger Samples
Company: PES (P.O.* 104-98-0175)
Anatyte: Trace metals
Method of Analysis: ICP
Sample Received Date: 4-9-98
Analysis Date: 4-16-98
Report Date: 4-23-98
Table 1. Results for Impinger Samples
Sample
M26A-I-2-A
M26A-O-2-A
M26A-FB-1-A(inlet)
M26A-I-5-A
M26A-O-5-A
Total
Volume
ml
371
493
241
227
269
K
ug
8.87
78.9
<4.3
9.51
<4.8
Ca
ug
150
233
63.6
145
291
Mg
ug
30.1
45.8
12.5
18.6
33.1
Na
ug
151
119
75.0
47.9
29.6
Al
ug
<20
<27
<13
<12
16.1
M26A-FB-2-A(inlet) 197 < 3.5 80.8 10.2 27.0 <11
Detection Limit: K - 0.018 ug/mL
Ca - 0.003 ug/mL
Mg - 0.001 ug/mL
Na- 0.065ug/mL
Al - 0.054 ug/mL
Page 2 of 3
-------
RTI Project No.: 7048-03G
Samples: QC for Impinger Samples
Company: PES (P.O.* 104-98-0175)
Analyte: Trace metals
Method of Analysis: ICP
Sample Received Date: 4-9-98
Analysis Date: 4-16-98
Report Date: 4-23-98
Sample
QC
QC Epected
QC
QC Expected
Table 2. Calibration Check Sample
K
ug/mL
Measured
Ca
ug/mL
Measured
Mg
ug/mL
Measured
Na
ug/mL
Measured
At
ug/mL
Measured
0.0432
0.0500
0.0497
0.0500
2.05
2.00
1.01
1.00
2.06
2.00
10.0
10.0
2.10
2.00
5.12
5.00
10.1
10.0
20.1
20.0
Sample
RTI-Blk
M26-O-2A SPK
SPK Expected
% SPK Recovery
Table 3. Results of Blank and Spike Analysis
K, ug/mL Ca, ug/mL Mg, ug/mL Na, ug/mL Al, ug/mL
Measured Measured Measured Measured Measured
< 0.018
0.340
0.400
85.0
< 0.003
0.459
0.500
91.8
< 0.001
4.81
5.00
96.2
< 0.065
2.41
2.50
96.4
< 0.054
5.22
5.00
104
Sample
M26-O-5-A DUP
Table 4. Results of Duplicate Analysis
K, ug Ca, ug Mg, ug Na, ug Al, ug
Measured Measured Measured Measured Measured
<4.8
277
32.3
40.4
15.1
Page 3 of 3
-------
TECHNICAL REPORT
Client: Pacific Environmental Services
Purchase Order No.: 104-98-0175
RTI Project No.: 91C-7048-03E
Date: April 21,1998
By
Eva D. Hardison
Research Triangle Institute
Post Office Box 12194
3040 Comwallis Road
Research Triangle Park, NC 27709
(919)541-5926
Submitted to:
Frank Phoenix
Pacific Environmental Services
5001 South Miami Blvd., Suite 300
Research Triangle Park, NC 27709
/RTI
-------
INTRODUCTION
Seven impinger samples were received under Purchase Order No. 104-98-0175 on April
9,1998 for analysis of chloride and ammonium ions.
ANALYSIS
The samples were analyzed on a Dionex Model DX-500 Ion Chromatograph using
conductivity detection and data reduction by Dionex PeakNet software. Chloride ion
was analyzed using a Dionex AS12A anion separator column and ammonium ion was
analyzed using a Dionex CS12 cation separator column. Quality control samples
prepared by RTI and quality assurance samples prepared by the Environmental
Protection Agency (EPA) were used to verify the calibrations. A sample matrix spike
and a duplicate were also analyzed.
RESULTS
See spreadsheets.
COMMENTS
No problems were encountered.
SAMPLE CUSTODY
Samples will be kept for 3 months after the report is delivered.
Page 1 of 1
/RTI
-------
Analysis of Implnger Absorbing Solutions for Cl and NH4
Pacific Environmental Services
PES P.O.* 104-98-0175
RTI Project No. 91C-7048-03E
/
Sample Receipt Date: 4/9/98
Sample Analysis Date: 4/15/98; 4/20/98
Report Date: 4/20/98
Sample ID Cl, ug/mL DF Vol, mL Cl, mg
\
NH4.ug/mL DF Vol.mL NH4,mg
M26A-I-4-A 0.102 100 226 2.31 4-38 0.670 25 226 3.79
M26A-I-5-A 0.177 100 227 4.02 *M4 0.976 25 227 5.54
M26A-I-6-A 0.153 100 226 3.46 *• Sfc 0.883 25 226 4.99
M26A-0-4-A 0.107 100 239 2.56 *. U5 1.232 25 239 7.36
M28A-O-5-A 0.112 100 269 3.01 3.10 1.089 25 269 7.32
M26A-O-6-A 0.163 100 236 3.85 * .°ld> 1.514 25 236 8.93
M26A-FB-2-A 0.021 100 197 0.41 0.041 25 197 0.20
-------
QA/QC for
Analysis of Implnger Absorbing Solutions for Cl and NH4
Pacific Environmental Services
Sample Receipt Date: 4/9/98
Sample Analysis Date: 4/15/98; 4/20/98
Report Date: 4/20/98
Cl, exp.
Sample ID mg/L
QA/QC:
QA-MED 0.500
QA-LOW 0.200
QA-MED 0.495
EPA-3909 0.502
NH4 QA-1 NA
NH4 QA-2 NA
EPA-3177 NA
Spikes:
M26-I-6-A 1/100 DIL
Spike 0.553
M26A-O-6-A 1/25 DIL
Spike
Duplicates:
M26A-O-2-A 1/100 DIL
M26A-O-2-A DUP 1/100 DIL
M26A-O-1-A 1/25 DIL
M26A-O-1-A DUP 1/25 DIL
Cl, found
mg/L % Rec.
0.495 99.0
0.198 99.0
0.495 100.0
0.519 103.4
NA
NA
NA
0.153
0.555 100.4
0.043
0.044
NH4, exp. NH4, found
mg/L mg/L
NA NA
NA NA
NA NA
NA NA
5.000 4.844
0.500 0.468
0.444 0.406
1.514
2.514 2.428
0.019
0.018
V.Rec.
96.9
93.6
91.4
96.6
-------
APPENDIX C
COMPUTER SUMMARIES AND EXAMPLE CALCULATIONS
-------
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 1 of 6
Y
AH
Astatic
Ts
C02
02
N2
C
Ap
0
'P
1/2
Vws,d
1-BWS
Md
Ms
Vs
A
Qa
QS
Q»(cmm)
I
RUN NUMBER
RUN DATE
RUNTIME
I-M23-4
3/28/98
1042-1355
MEASURED DATA
Meter Box Correction Factor 1.021
Avg Meter Orifice Pressure, in. H20 2.07
Barometric Pressure, inches Hg 29.50
Sample Volume, ft3 133.796
Average Meter Temperature, °f 99.08
Stack Static Pressure, inches H20 -30.00
Average Stack Temperature, "F 472
Carbon Dioxide content, % by volume 19.2
Oxygen content, % by volume 10.6
Nitrogen content, % by volume 70.2
Pitot Tube Coefficient 0.84
Average Square Root Ap, (in. H20)1/2 0.9333
Sample Run Duration, minutes 180
Nozzle Diameter, inches 0.250
CALCULATED DATA
Nozzle Area, ft2 0.00034
Standard Meter Volume, dscf 127.805
Standard Meter Volume, dscm 3.619
Stack Pressure, inches Hg 27.29
Estimated Moisture, % by volume 4.50
Standard Water Vapor Volume, ft3 6.022
Dry Mole Fraction 0.955
Molecular Weight (d.b.), Ib/lb-mole 31.50
Molecular Weight (w.b.), lb/lb«mole 30.89
Stack Gas Velocity, ft/s 70.5
Stack Area, ft2 38.48
Stack Gas Volumetric flow, acfm 162,732
Stack Gas Volumetric flow, dscfm 80,260
Stack Gas Volumetric flow, dscmm 2,273
Isokinetic Sampling Ratio, % 99.9
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 2 of 6
RUN NUMBER
RUN DATE
RUN TIME
I-M23-4
3/28/98
1042-1355
EMISSIONS DATA
DIOXINS:
2378 TCDD
ng Catch, ng (0.003)
ng/dscm Concentration, ng/dscm, as measured (0.000829)
ug/hr Emission Rate, ug/hr (0.113)
Total TCDD
ng Catch, ng 0.02
ng/dscm Concentration, ng/dscm, as measured 0.00553
ug/hr Emission Rate, ug/hr 0.754
12378 PeCDD
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00111)
ug/hr Emission Rate, ug/hr (0.151)
Total PeCDD
ng Catch, ng . {0.003}
ng/dscm Concentration, ng/dscm, as measured {0.000829}
ug/hr Emission Rate, ug/hr {0.113}
123478 HxCDD
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00166)
ug/hr Emission Rate, ug/hr (0.226)
123678 HxCDD
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00138)
ug/hr Emission Rate, ug/hr (0.188)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 3 of 6
RUN NUMBER
RUN DATE
RUN TIME
I-M23-4
3/28/98
1042-1355
EMISSIONS DATA -Continued
DIOXINS - Continued
123789 HxCDD
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00138)
ug/hr Emission Rate, ug/hr (0.188)
Total HxCDD
ng Catch, ng 0.01
ng/dscm Concentration, ng/dscm, as measured 0.00276
ug/hr Emission Rate, ug/hr 0.377
1234678 HpCDD
ng Catch, ng 0.008
ng/dscm Concentration, ng/dscm, as measured 0.00221
ug/hr Emission Rate, ug/hr 0.301
Total HpCDD
ng Catch, ng 0.02
ng/dscm Concentration, ng/dscm, as measured 0.00553
ug/hr Emission Rate, ug/hr 0.754
QCJ2Q
ng Catch, ng 0.04
ng/dscm Concentration, ng/dscm, as measured 0.0111
ug/hr Emission Rate, ug/hr 1.51
Total PCDD
ng Catch, ng {0.093}
ng/dscm Concentration, ng/dscm, as measured {0.0257}
ug/hr Emission Rate, ug/hr {3.50}
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 4 of 6
RUN NUMBER
RUN DATE
RUN TIME
I-M23-4
3/28/98
1042-1355
EMISSIONS DATA - Continued
FURANS
2378 TCDF
ng Catch, ng 0.14
ng/dscm Concentration, ng/dscm, as measured 0.0387
ug/hr Emission Rate, ug/hr 5.28
Total TCDF
ng Catch, ng 2.6
ng/dscm Concentration, ng/dscm, as measured 0.718
ug/hr Emission Rate, ug/hr 98.0
12378PeCDF
ng Catch, ng 0.04
ng/dscm Concentration, ng/dscm, as measured 0.0111
ug/hr Emission Rate, ug/hr 1.51
23478 PeCDF
ng Catch, ng 0.04
ng/dscm Concentration, ng/dscm, as measured 0.0111
ug/hr Emission Rate, ug/hr 1.51
Total PeCDF
ng Catch, ng 0.38
ng/dscm Concentration, ng/dscm, as measured 0.105
ug/hr Emission Rate, ug/hr 14.3
123478 HxCDF
ng Catch, ng 0.01
ng/dscm Concentration, ng/dscm, as measured 0.00276
ug/hr Emission Rate, ug/hr 0.377
() Not Detected. Value shown is the detection Hmit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 5 of 6
RUN NUMBER
RUN DATE
RUN TIME
I-M23-4
3/28/98
1042-1355
EMISSIONS DATA - Continued
Furans - Continued
123678 HxCDF
ng Catch, ng 0.008
ng/dscm Concentration, ng/dscm, as measured 0.00221
ug/hr Emission Rate, ug/hr 0.301
234678 HxCDF
ng Catch, ng 0.008
ng/dscm Concentration, ng/dscm, as measured 0.00221
ug/hr Emission Rate, ug/hr 0.301
123789 HxCDF
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00111)
ug/hr Emission Rate, ug/hr (0.151)
Total HxCDF
ng Catch, ng 0.05
ng/dscm Concentration, ng/dscm, as measured 0.0138
ug/hr Emission Rate, ug/hr 1.88
1234678 HpCDF
ng Catch, ng 0.007
ng/dscm Concentration, ng/dscm, as measured 0.00193
ug/hr Emission Rate, ug/hr 0.264
1234789 HpCDF
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00193)
ug/hr Emission Rate, ug/hr (0.264)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Inlet
Page 6 of 6
RUN NUMBER
RUN DATE
RUN TIME
I-M23-4
3/28/98
1042-1355
EMISSIONS DATA - Continued
Furans - Continued
Total HpCDF
ng Catch, ng 0.007
ng/dscm Concentration, ng/dscm, as measured 0.00193
ug/hr Emission Rate, ug/hr 0.264
QCDF
ng Catch, ng (0.02)
ng/dscm Concentration, ng/dscm, as measured (0.00553)
ug/hr Emission Rate, ug/hr (0.754)
Total PCDF
ng Catch, ng (3.057)
ng/dscm Concentration, ng/dscm, as measured (0.845)
ug/hr Emission Rate, ug/hr (115)
Total PCDD + PCDF
ng Catch, ng ' (3.15)
ng/dscm Concentration, ng/dscm, as measured (0.870)
ug/hr Emission Rate, ug/hr (119)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 26A - HCI
Kiln No. 4 Baghouse Inlet
Page 1 of 2
p
'static
Y
•bar
vm
AP1/2
AH
Tm
Ts
V,c
CO2
02
N2
CP
0
Dn
An
Vm(std)
Vm(std)
Qm
PS
BWS
Vwstd
1-BW,
Md
Ms
V,
A
Qa
Qs
Qs
I
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches H20
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Ap, (in H2O)1'2
Avg Meter Orifice Pressure, in. H2O
Average Meter Temperature, °F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ib/lb-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
I-M26A-4
3/28/98
1430-1530
-30.00
1.021
29.50
33742
0.9110
1.10
98.3
488
33.6
19.20
10.60
702
084
60
0.217
0.000257
32.197
0.912
0.537
27.29
4.7
1 582
0.953
31.50
30.86
69.4
38.48
147,378
71,314
2,019
103.7
I-M26A-S
3/28/98
1635-1735
-30.00
1.021
29.50
33.138
0.9055
1.07
944
497
31.9
19.20
10.6
70.2
0.84
60
0.217
0.000257
31.844
0902
0.531
27.29
45
1 502
0955
31 50
30.89
69.3
38.48
160,007
76,841
2,176
103.5
I-M26A-6
3/28/98
1801-1901
-30.00
1.021
29.50
33.556
0.9280
1 11
96.1
516
34.2
19.20
10.60
70.2
0.84
60
0.217
0.000257
32.149
0.910
0.536
27.29
4.8
1.610
0.952
31 50
30.85
71.8
38.48
165,684
77,822
2,204
103.2
Average
-30.00
1.021
29.50
33.479
0.9148
1 09
96.3
501
33.2
19.2
10.6
70.2
0.84
60
0.217
0.000257
32.063
0.908
0.534
27.29
4.7
1.564
0.953
31.50
30.87
70.2
38.48
157,689
75,326
2,133
103.5
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 26A • HCI
Kiln No. 4 Baghouse Inlet
Page 2 of 2
Fw,
^pprnvd
EHCI
Fw,
ppmvd
EC,
Fw.
^ ppmvd
^NH4
Fw,
*-* ppmvd
EA,
FWI
^ ppmvd
Eca
Fw,
^ ppmvd
EMg
Fw,
Cppmvd
EK
Fwi
^ ppmvd
EN.
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
Chlorides as HCI
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Chlorides as Cl
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Ammonia
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Aluminum. Al
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Calcium. Ca
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Magnesium. Mg
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Potassium. K
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Sodium. Na
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate. Ib/hr
I-M26A-4 I-M26A-5 I-M26A-6
3/28/98 3/28/98 3/28/98
1430-1530 1635-1735 1801-1901
2.38
36.47
1.72
0.696
2.31
35.45
1.72
0.677
3.79
1804
5.54
1.11
#N/A
26.98
#N/A
#N/A
#N/A
4008
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
4.14
36.47
3.02
1.32
4.02
35.45
3.02
1.28
5,54
18.04
8.19
1.77
(12)
26.98
(0.0119)
(0.00383)
145
40.08
0.0965
0.0463
18.6
24.31
0.0204
0.00594
9.51
39.10
0.00649
0.00304
47.9
22.99
0.0556
0.0153
3.56
36.47
2.58
1.14
3.46
35.45
2.58
1.11
4.99
18.04
7.31
1.60
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
Average
3.36
36.47
2.44
1.05
3.26
35.45
2.44
1.023
4.77
18.04
7.01
1.49
(12)
26.98
(0.0119)
(0.00383)
145
40.08
0.0965
0.0463
18.6
24.31
0.0204
0.00594
9.51
39.10
0.00649
0.00304
47.9
22.99
0.0556
0.0153
() - Not Detected
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Y
AH
Pbar
vm
Tm
"static
Ts
Vlc
C02
02
N2
CP
AP1*
©
Dn
An
Vm(std)
Vm(std)
PS
Bws
Vws,d
1-BWS
Md
Ms
Vs
A
Qa
Q.
^"»(anm)
I
Kiln # 4 Baghouse Outlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H20
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, °F
Stack Static Pressure, inches H2O
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Average Square Root Ap, (in. H2O)1/2
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Stack Pressure, inches Hg
Moisture, % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), lb/lb«mole
Molecular Weight (w.b.), Ib/Ib«mole
Stack Gas Velocity, tt/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio. %
O-M23-4
3/28/98
1044-1346
1.000
1.99
29.50
140.622
88.2
-0.51
348
134.4
19.2
10.6
70.2
0.84
0.8517
180.0
0.250
0.00034
134.157
3.799
29.46
4.5
6.326
0.955
31.50
30.89
57.6
37.80
130,734
80,274
2,273
103.0
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Outlet
Page 2 of 6
RUN NUMBER
RUN DATE
RUN TIME
O-M23-4
3/28/98
1044-1346
EMISSIONS DATA
DIOXINS:
2378 TCDD
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00105)
pg/hr Emission Rate, pg/hr (0.144)
Total TCDD
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00105)
pg/hr Emission Rate, pg/hr (0.144)
12378PeCDD
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00158)
pg/hr Emission Rate, pg/hr (0.215)
Total PeCDD
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00158)
pg/hr Emission Rate, pg/hr (0.215)
123478 HxCDD
ng Catch, ng . (0.008)
ng/dscm Concentration, ng/dscm, as measured (0.00211)
pg/hr Emission Rate, pg/hr (0.287)
123678 HxCDD
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00184)
pg/hr Emission Rate, pg/hr (0.251)
() Not Detected. Value shown is the detection limit and is included in toUls.
{} Estimated Maximum Possible Concentration. EMPC values a1^ included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Outlet
Page 3 of 6
RUN NUMBER
RUN DATE
RUN TIME
O-M23-4
3/28/98
1044-1346
EMISSIONS DATA -Continued
DIOXINS - Continued
123789 HxCDD
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00184)
ug/hr Emission Rate, ug/hr (0.251)
Total HxCDD
ng Catch, ng {0.009}
ng/dscm Concentration, ng/dscm, as measured {0.00237}
ug/hr Emission Rate, ug/hr {0.323}
1234678 HpCDD
ng Catch, ng {0.01}
ng/dscm Concentration, ng/dscm, as measured {0.00263}
pg/hr Emission Rate, pg/hr {0.359}
Total HpCDD
ng Catch, ng {0.01}
ng/dscm Concentration, ng/dscm, as measured {0.00263}
ug/hr Emission Rate, ug/hr {0.359}
QC_D_D_
ng Catch, ng 0.05
ng/dscm Concentration, ng/dscm, as measured 0.0132
ug/hr Emission Rate, ug/hr 1.80
Total PCDD
ng Catch, ng (0.079)
ng/dscm Concentration, ng/dscm. as measured (0.0208)
pg/hr Emission Rate, ug/hr (2.84)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Outlet
Page 4 of 6
RUN NUMBER
RUN DATE
RUN TIME
O-M23-4
3/28/98
1044-1346
EMISSIONS DATA - Continued
FURANS
2378 TCDF
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00132)
pg/hr Emission Rate, ug/hr (0.180)
Total TCDF
ng Catch, ng 0.17
ng/dscm Concentration, ng/dscm, as measured 0.0447
pg/hr Emission Rate, ug/hr 6.10
12378PeCDF
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00105)
ug/hr Emission Rate, ug/hr (0.144)
23478 PeCDF
ng Catch, ng (0.004)
ng/dscm Concentration, ng/dscm, as measured (0.00105)
ug/hr Emission Rate, ug/hr (0.144)
Total PeCDF
ng Catch, ng 0.01
ng/dscm Concentration, ng/dscm, as measured 0.00263
ug/hr Emission Rate, ug/hr 0.359
123478 HxCDF
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00132)
ug/hr Emission Rate, ug/hr (0.180)
() Not Detected. Value shown is the detection limit and is included hi totals.
/ \ PctimataH Maximum Possible Concentration EMPC vafiK:. _::: included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Outlet
Page 5 of 6
RUN NUMBER
RUN DATE
RUN TIME
O-M23-4
3/28/98
1044-1346
EMISSIONS DATA - Continued
Furans - Continued
123678 HxCDF
ng Catch, ng (0.005)
ng/dscm Concentration, ng/dscm, as measured (0.00132)
ug/hr Emission Rate, ug/hr (0.180)
234678 HxCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00158)
ug/hr Emission Rate, ug/hr (0.215)
123789 HxCDF
ng Catch, ng (0.006)
ng/dscm Concentration, ng/dscm, as measured (0.00158)
ug/hr Emission Rate, ug/hr (0.215)
Total HxCDF
ng Catch, ng 0.008
ng/dscm Concentration, ng/dscm, as measured 0.00211
ug/hr Emission Rate, ug/hr 0.287
1234678 HpCDF
ng Catch, ng (0.007)
ng/dscm Concentration, ng/dscm, as measured (0.00184)
ug/hr Emission Rate, ug/hr (0.251)
1234789 HpCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00263)
ug/hr Emission Rate, ug/hr (0.359)
() Not Detected. Value shown is the detection limit and is included in totals.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
-------
Summary of Stack Gas Parameters and Test Results
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 23 - PCDDs/PCDFs
Kiln # 4 Baghouse Outlet
Page 6 of 6
RUN NUMBER
RUN DATE
RUN TIME
O-M23-4
3/28/98
1044-1346
EMISSIONS DATA - Continued
Furans - Continued
Total HpCDF
ng Catch, ng (0.008)
ng/dscm Concentration, ng/dscm, as measured (0.00211)
ug/hr Emission Rate, (jg/hr (0.287)
OCDF
ng Catch, ng (0.01)
ng/dscm Concentration, ng/dscm, as measured (0.00263)
ug/hr Emission Rate, ug/hr (0.359)
Total PCDF
ng Catch, ng (0.206)
ng/dscm Concentration, ng/dscm, as measured (0.0542)
ug/hr Emission Rate, pg/hr (7.40)
Total PCDD + PCDF
ng Catch, ng (0.285)
ng/dscm Concentration, ng/dscm, as measured (0.0750)
ug/hr Emission Rate, ug/hr (10.2)
() Not Detected. Value shown is the detection limit and is included in totals.
{} Estimated Maximum Possible Concentration. EM PC values are included in totals.
-------
Summary of Stack Gas Paranwtere and Test Results
Air Emissions Screening Test
Dravo Lime Company - Saglnaw, Alabama
US EPA Test Method 26A - HCI
Kiln No. 4 Baghouse Outlet
Page 1 of 2
"static
r
Pfcar
vm
Ap"2
AH
Tm
Ts
V,c
CO2
02
N2
CP
©
Dn
An
»m(sld)
Vm(std)
Qm
PS
Bws
Vwstd
1-Bw.
Md
Ms
V8
A
Qa
Qs
Qs
I
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches H2O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Ap, (in. H2O)1G
Avg Meter Orifice Pressure, in. H20
Average Meter Temperature, °F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pitot Tube Coefficient
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ib/lb-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfrn
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
O-M26A-4
3/28/98
1432-1532
-0.53
1.000
29.50
46.613
0.8536
2.03
92.6
352
46.9
19.20
10.60
70.2
0.84
60
0.250
0.000341
44.116
1.249
0.735
29.46
4.8
2.208
0.952
31.50
30.85
57.9
37.80
131,380
80,103
2,268
101.8
0-M26A-5
3/28/98
1638-1738
-0.47
1.000
29.50
46.498
0.8467
2.01
94.9
349
44.3
19.20
10.6
70.2
0.84
60
0.250
0.000341
43.822
1.241
0.730
29.47
4.5
2.085
0.955
31.50
30.88
57.3
37.80
130,038
79,736
2,258
101.6
O-M26A-6
3/28/98
1802-1902
-0.47
1.000
29.50
46.964
0.8567
2.06
90.8
358
50.5
19.20
10.60
70.2
0.84
60
0.250
0.000341
44.602
1.263
0.743
29.47
5.1
2.377
0.949
31.50
30.81
58.4
37.80
132,462
79,877
2,262
103.2
Average
-0.49
1.000
29.50
46.692
0.8523
2.03
92.8
353
47.2
19.2
10.6
70.2
0.84
60
0.250
0.000341
44.180
1.251
0.736
29.46
4.8
2.223
0.952
31.50
30.85
57.9
37.80
131,293
79,905
2,263
102.2
-------
Summary of Stack Gas Parameters and Test Results
Air Emissions Screening Test
Dravo Lime Company - Saginaw, Alabama
US EPA Test Method 26A - HCI
Kiln No. 4 Baghouse Outlet
Page 2 of 2
Fw>
Cppmvd
EHCI
Fw.
Cppnwd
EC.
FWI
^ppmvd
ENI-M
Fw.
Cppmvd
Ew
Fwt
^ppmvd
ECa
Fw.
Cppmvd
EMfl
Fw.
^ppcnvd
EK
Fw.
Cppmvd
EN.
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
Chlorides as HCI
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Chlorides as Cl
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Ammonia
Target Catch, mg
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Aluminum. Al
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Calcium. Ca
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Magnesium. Mg
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Potassium. K
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
Sodium. Na
Target Catch, ug
Formula Weight, Ib/lb-mol
Concentration, ppm by volume
Emission Rate, Ib/hr
O-M26A-4 O-M26A-5 O-M26A-6
3/28/98 3/28/98 3/28/98
1432-1632 1638-1738 1802-1902
2.63
36.47
1.39
0.633
2.56
35.45
1.39
0.615
7.36
18.04
7.86
1.77
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
3.10
36.47
1.65
0.745
3.01
35.45
1.65
0.724
7.32
18.04
7.87
1.76
16.1
26.98
0.0116
0.00388
291
40.08
0.141
0.0700
33.1
24.31
0.0264
0.00797
(4.8)
39.10
(0.00238)
(0.00116)
29.6
22.99
0.0250
0.00712
3.96
36.47
2.07
0.938
3.85
35.45
2.07
0.912
8.93
18.04
9.43
2.12
#N/A
26.98
#N/A
#N/A
#N/A
40.08
#N/A
#N/A
#N/A
24.31
#N/A
#N/A
#N/A
39.10
#N/A
#N/A
#N/A
22.99
#N/A
#N/A
Average
3.23
36.47
1.70
0.772
3.14
35.45
1.70
0.750
7.87
18.04
8.38
1.88
16.1
26.98
0.0116
0.00388
291
40.08
0.141
0.0700
33.1
24.31
0.0264
0.00797
(4.8)
39.10
(0.00238)
(0.00116)
29.6
22.99
0.0250
0.00712
() - Not Detected
-------
Example Calculations
Dravo Lime Company - Saginaw, Alabama
US EPA Method 23-PCDD/PCDF
(Using Data from Run O-4)
Note: Discrepancies may exist between the computer generated reported results, which use
more significant figures, and the values manually calculated from the displayed values.
1. Volume of dry gas sampled corrected to standard conditions of 68 °F, 29.92 in. Hg, ft3.
V
m(std)
17.64VmY
bar
AH
13.6
460 + t
m(std)
= (17.64)(140.622)(1.000)
29.5
1.992
13.6
I 460 + 88.17 )
V , = 134.157 dscf
m(std)
2. Volume of dry gas sampled corrected to standard conditions of 68 °F, 29.92 in. Hg, m3
Vm(std)m3 = Vm(std)(0.028317)
= (134.157)(0.028317)
dscm
3. Volume of water vapor at standard conditions, ft3.
Vw(,td) = 0.04707VU
Vw(,td) = (0.04707)(134.4)
w(,td)
scf
-------
4. Moisture content in stack gas.
B*" (V ( «n + V , *n]
B = 6.326
ws 134.157+ 6.326
Bws = 0.0450
5. Dry molecular weight of stack gas, Ib/lb-mol.
Md = 0.44 (%CO2) + 0.32 (%O2) + 0.28 (%N2 +%CO)
M, = U.44(iy.2) + O.i2(l0.b) + U.28 (/0.2 +0)
Md = 31.50 Ib/lbmol
6. Molecular weight of stack gas, Ib/lb-mol.
Ms = 31.50(1 -0.0450) + 18(0.0450)
M - 31.50(0.9550) + 18(0.0450)
Ms = 30.0825 + 0.810
Ms = 30.89 Ib/lbmol
-------
7. Absolute stack gas pressure, in. Hg.
p
p _ p + static
s - bar
Ps . 29.5 +
13.6
Ps - 29.46 inches Hg
8. Stack velocity at stack conditions, fps.
v = 85.49 C
avg
ts+460
~M^
v = (85.49)(0.84)(0.8517)
\
(348.3 + 460)
(30.89) (29.46)
9. Isokinetic Variation.
vs = 57.64 fps
/ol -
460) (17.32)
(vs)(Dn2)(0)(Ps)(l-Bws)
0/ol = (134.157) (348.3->-460) (17.32)
(57.64) (0.250)2 (180) (29.46) (1-0.0450)
= 103.0
-------
10. Stack gas volumetric flow rate at stack conditions, acfrn.
Qs = (60) (A) (vs)
Qs = (60) (37.80) (57.64)
Qs = 130,734 acfin
11. Dry stack gas volumetric flow rate at standard conditions, dscfin
= 17.64 O —
^S x.
= (17-64) (130,734) | ——] (1-0.0450)
348.3+460 V '
= 80'274 dscfin
12. Dry stack gas volumetric flow rate at standard conditions, dscmm.
Qs(std)m'/min = Qs(std) °'028317
fa = (80'274> (0-028317)
= 2'273
-------
13. Pollutant (2378 TCDD) concentration, ng/dscm.
ng/dscm =
*m(std)m3
,. < 0.004
ng/dscm =
3.799
ng/dscm = < 0.00105 ng/dscm
14. Pollutant (2378 TCDD) concentration, ng/dscm adjusted to 7 percent oxygen.
ng/dscm@7%O, = (ng/dscm) •
2 (20.9 - %02)
ng/dscm@7%O, = (< 0.00105) —
2 (20.9 - 10.6)
ng/dscm@7%O2 = < 0.00142 ng/dscm@7%O2
15. Pollutant (2378 TCDD) emission rate, ng/hr.
(60) (ng) (Qsfstd.)
do3) (vm(std))
= (60) (< 0.004) (80,274)
(103) (134.157)
/ug/hr = < 0.144
-------
APPENDIX D
CALIBRATION DATA
-------
4E
PACIFIC ENVIRONMENTAL SERVICES, INC.
4700 Duke Drive,
Suite 150
Mason, Ohio 45040
Phone:(513)398-2556
Fax (513) 398-3342
www.pes.com
Pitol Tube Number:
Effeclive Length:
4E
49*
Pilot Tube Openings Damaged?
Pitot Tube Assembly Level?
a | = 0_
P. = L
Y = 0
z = A sin Y =
w = A sin 6 =
0
0.0170
PA =
PB =
D,=
Date:
Calibrated By:
YES
' YES I
°(< 10°)
' N0 '
NO
a 2 =
6=
1
cm (in.) 0.32 cm ( < 1/8 in.)
cm (in.) 0.08 cm ( < 1/32 in.)
0.487 cm (in.)
0.486
0.375
cm (in.)
cm (in.)
12/23/97
S. Simon
0.973
(8)
The types of face-opening misalignment shown above wll not affect the baseline value of Cp(s) so
tongas °S and °S Is less than or equal to 1O*. a, end a, Is less than or equal to 6', z Is less than or
equal too.32 cm (1/8 in.), and w is less than or equal to O.OB cm( 1/32 In.) (referancel 1.O In
Assigned Pitot Coefficient, Cp:
0.84
'« 10°)
Pitot Tube Calibration Form
1998 Yearly Calibration
-------
7D
PACIFIC ENVIRONMENTAL SERVICES, INC.
4700 Duke Drive.
Suite 150
Mason, Ohio 45040
Phone:(513)398-2556
Fax (513) 398-3342
www.pes.com
Pilot Tube Number: 7D Date:
Effective Length: 84.5" Calibrated By:
Pilot Tube Openings Damaged? YES | NO \
Pilot Tube Assembly Level? | YES | NO
a , = 3 °(< 10°) a 2 =
P, = l °«5°) p2 =
Y= 1 6=0 A =
z = A sin Y = 0.016 cm (in.) 0.32 cm ( < 1/8 in.)
w = A sin 6 = 0 cm (in.) 0.08 cm ( < 1/32 in.)
PA = 0.466 cm (in.)
12/23/97
S. Simon
3 °(< 10°)
1 °(<5°)
0.931
Pfl =
0.465
cm (in.)
Dt =
0.375
cm (in.)
£F7
(a)
"Rio types of face-opaning miBalioirmttnt shown abov* v/t\ not affect th* bas«ln« valu* of Q3(s) mo
long as <*, and "aim lass than or equal to 1O*. a< and a> I* less than or equal to 9*, z Is lass than or
equal to O.32 cm (1/8 In.), andw Is lass than or equal to O.OB om(1O2 In.) (reference-! 1.O tn
Pitot Tube Calibration Form
1998 Yearly Calibration
-------
*.*> VAKVAiWAA A
PACIFIC ENVIRONMENTAL SERVICES.INC.
4700 Duke Drive,
Suite 150
Mason, Ohio
Phone: (513) 398-2556
Fax: (513)3983342
www.pes.com
TEMPERATURE SENSOR CALIBRATION DATA
FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
4E
DATE:
12/23/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. "F:
29.52
74
REFERENCE:
Mercury-in-glass:
Other
'CALIBRATOR:
ASTM-3F
G.Gay
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Mot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
74
38
203
339
Thermocouple
Potentiometer
Temperature.°F
74
38
202
340
Temperature
Difference,"
%
o!oo
0.00
0.15
0.13
Type of calibration used.
"f ref temp 8F+46QWtest thermometer temp flF+46(H
X100
reftemp,'Ff460
100<1.S%
Comments:
STACK THEFMOCOUPLE CALIBRATION FORM
1998 Yeariv Calibration
-------
PACIFIC ENVIRONMENTAL SERVICES.INC.
4700 Duke Drive,
Suite 150
Mason, Ohio
Phone: (513) 398-2556
Fax: (513) 3983342
www.pes.com
TEMPERATURE SENSOR CALIBRATION DATA
FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
7D
DATE:
12/23/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29.52
74
REFERENCE:
Mercury-in-glass:
Other:
"CALIBRATOR:
ASTM-3F
G. Gay
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
74
40
206
340
Thermocouple
Potentiometer
Temperature,°F
74
41
205
341
Temperature
Difference,"
%
0.00
0.20
0.15
0.13
"Type of calibration used.
b(ref. temD°F+460Wtestthermometertemp.°F+460) X100
reftemp,°F+460
100<1.5%
Comments:
STACK THERMOCOUPLE CALIBRATION FORM 1998 Yearly Calibration
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F ~i
Sensor Type
Length
Reference Temp. Sensor:
Barometric Pressure, "Hg -z,-?, c/
Date
^•L^r
"
a
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
£5
b\tL
wlv^
,
Temp. °F
Ref.
Sensor
n
1<*
•1^<~
Test
Sensor
34-
!(•
wsr
1
.
•
Temp.
Diff. %
o
Within
TJmfaa
Y/N
Calibrated
By
% Temp. Diff
(Ref'
460) - ( Teat Teinp. * 460)
(Ref. Temp. + 460)
x 10Q
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. eF 7
Reference Temp. Sensor:
Sensor Type JfC-Tc. • Length I
Barometric Pressure, "Eg "? ^
Date
Vlo-ftt
j»
«'
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
/
A-i/t
{*»"-
M*-o
•
Temp. °F
Ref.
Sensor
3^
?<*
-Z^>c.
Test
Sensor
3f-
17
zo^-
Temp.
DifT. %
.*foc.
./*<.
./So
•
Within
T.itnifjB
Y/N
y
Y
y
Calibrated
By
]Utt»
^^
tifc
*
Temp. Diff
(Ref' Ten*>
460)
. Temp. * 460)
x 100 * 1.5
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F
feM - \
"7-
Reference Temp. Sensor:
.,
Sensor Type K~TC Length
Barometric Pressure, "Hg
t '
*
Date
>i*-f!r
C(
>'
'
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
\C
\V^"S
\u&
'
% Temp. Diff
(J?ef •
40) ' ( Teat
460)
(Ref. Temp. + 460)
x 100 s 1.5 %
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No. DCM-oof Sensor Type K-Tc • Length t,
Ambient Temp. °F "7^* Barometric Pressure, "Hg •sa.T*
n»M»<««A nPAvnn Cancn*>»
>y
AliJUHCUl &«Uf»« »• ___^_
Reference Temp. Sensor:
Date
i'l%'c|y
/,
••
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
(C«=.
&**
H°^'
Temp. °F
Ref.
Sensor
S3
•7-t
z.oU
Test
Sensor
3.3
•7.i"
•tOK
Temp.
Diff. %
o
. 1*7
o
Within
TJmHg
Y/N
y
Y
Y
Calibrated
By
Ai^>
Vu^
Hu\
^
% Temp. Tiff - (*ef * Tezap : 4!0) " ( TeSt ***' * 460)
^ r=C3r renp. •*• 460)
100 s 1.5 %
-------
From: "Paul Siegel"
Organization: Pacific Environmental Services
To: Estewart@rtp.pes.com
Date sent: Wed, 5 Aug 1998 21:04:52 -0500
Subject: Alabama Lime Kiln Testing
Priority: normal
Mr. Stewart,
All pre and post leak-checks performed during the Alabama lime kiln
testing program were less than 0.020 cubic feet during a one minute
period. All pre-test leak-checks were conducted under a minimum of 15
inches of vacuum. All post-test leak-checks were conducted at a
vacuum rate of 1 inch greater than the highest vacuum measured during
the sample run. If you have any questions or need any additional
comments, please call or e-mail.
Paul Siegel
Emil Stewart — 1 — Thu, 6 Aug 1998 12:18:59
-------
1of2
PACIRC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park. North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
Date:
PM,, in Hg'
9/1/97
30.16
Calibrator. Tom McDonald
Meter Box No.: MB-10
Reference Meter Correction Factor 1.0049 (8/28/96)
AH = 0.5
Trial
1
2
3
Trial
Duration
(min)
19
19
19
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
994.409
1001.982
1009.513
Final
(ft3)
1001.982
1009.513
1017.050
Net
(ft3)
7.573
7.531
7.537
Meter Temperatures
Initial, Inlet
CF)
74
77
80
Final, Inlet
CF)
78
80
81
Avg. Inlet
(°F)
76
78.5
80.5
Initial, Outlet
CF)
73
75
77
inal, Outte
CF)
75
77
78
Avg. Outlet
CF)
74
76
77.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
600.523
608.185
615.801
Final
(ft3)
608.185
615.801
623.430
Net
(ft3)
7.662
7.616
7.629
Meter Temperature
Initial
CF)
72
74
76
Final
CF)
74
76
77
Avg.
CF)
73
75
76.5
Meter Box
Correction
Factor
Y
1.019
1.019
1.021
Reference
Orifice Press
AH0
(in. H20)
1.71
1.74
1.74
AH = 0.75
Trial
1
2
3
Trial
Duration
(min)
15
15
15
Dry Gas Meter MB-10
Gas Volume
initial
(ft3)
17.220
24.350
31.563
Final
(ft3)
24.350
31.563
38.780
Net
(ft3)
7.130
7.213
7.217
Meter Temperatures
Initial, Inlet
CF)
80
82
82
Final, Inlet
CF)
82
83
83
Avg. Inlet
CF)
81
82.5
82.5
Initial, Outlet
CF)
78
79
79
inal, Outte
CF)
79
79
81
Avg. Outlet
CF)
78.5
79
80
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
623.622
630.833
638.141
Final
(ft3)
630.833
638.141
645.425
Net
(ft3)
^7.211
7.308
7.284
Meter Temperature
Initial
CF)
77
78
78
Final
CF)
77
78
78.5
Avg.
CF)
77
78
78.25
Meter Box
Correction
Factor
Y
1.020
1.021
1.018
Reference
Orifice Press
AH0
(in. H2O)
1.82
1.77
1.79
AH= 1.0
Trial
1
2
3
Trial
Duration
(min)
10
10
10
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
38.946
44.490
50.050
Final
(ft3)
44.490
50.050
55.585
Net
(ft3)
5.544
5.560
5.535
Meter Temperatures
Initial, Inlet
CF)
81
83
84
Final, Inlet
CF)
83
84
84
•Avg. Inlet
CF)
82
83.5
84
Initial, Outlet
CF)
60
80
80
inal, Outte
CF)
80
80
80
Avg. Outlet
CF)
80
80
80
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft8)
645.614
651.220
656.829
Final
(ft3)
651.22
656.829
662.435
Net
(ft3)
5.606
5.609
5.606
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
Y
1.019
1.018
1.023
Reference
Orifice Press
AH0
(in. H20)
1.79
1.78
1.78
-------
2 of 2
PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park. North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
AH = 2.0
Trial
1
2
3
Trial
Duration
(min)
10
10
10
Dry Gas Meter MB-10
Gas Volume
Initial
(ft3)
55.868
63.519
71.182
Final
^
63.519
71.182
78.845
Net
(^
7.651
7.663
7.663
Meter Temperatures
Initial. Inlet
CF)
84
86
86
Final, Inlet
CF)
86
86
87
Avg. Inlet
CF)
85
86
86.5
Initial, Outlet
CF)
81
81
81
mat. Outle
CF)
81
81
81
Avg. Outlet
CF)
81
81
81
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
662.729
670.472
678.244
Final
(ft3)
670.472
678.244
686.010
Net
(ft3)
7.743
7.772
7.766
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
T
1.021
1.025
1.024
Reference
Orifice Press
AH0
(in. HaO)
1.87
1.86
1.86
AH = 4.0
Trial
1
2
3
Trial
Duration
(min)
8
8
8
Dry Gas Meter MB-10
Gas Volume
Initial
^
79.058
86.620
94.185
Final
(ft3)
86.620
94.185
101.754
Net
(ft3)
7.562
7.565
7.569
Meter Temperatures
Initial, Inlet
CF)
85
87
89
Final, Inlet
CF)
88 •
89
89
Avg. Inlet
CF)
86.5
88
89
Initial, Outlet
CF)
81
82
82
inal, Outle
CF)
82
82
82
Avg. Outlet
CF)
81.5
82
82
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
686.208
693.895
701.558
Final
(ft3)
693.895
701.558
709.244
Net
(ft3)
7.687
7.663
7.686
Meter Temperature
Initial
CF)
78
78
78
Final
CF)
78
78
78
Avg.
CF)
78
78
78
Meter Box
Correction
Factor
r
1.023
1.021
1.025
Reference
Orifice Press
AHQ
(in. H20)
2.44
2.45
2.43
Calibration
Results
AH | Y | AH0
0.50
0.75
1.0
2.0
4.0
1.020 1.73
1.020 1.79
1.020 1.78
1.023 1.86
1.023 2.44
Dry Gas Meter MB-10 on 09/01/97
Meter Box Calibration Factor
Meter Box Reference Orifice Pressure
1.021
1.92
1Q_09Q17.x1s
Priittarl- R/-KVOB
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Posttest Dry Gas Meter Calibration Form (English Units)
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date: 572/98 P^, in Hg
1.021
16
1.0077
29.94 Calibrator D. Holzschuh
Meter Box No.
MB-10
AH= 1.41
Trial
1
2
3
Duration
(min)
15
8
8
Dry Gas Meter
Initial
(ft3)
902.1
912.624
917.493
Final
(ft3)
912.624
917.993
923.154
Net
(ft3)
10.524
5.369
5.661
Initial, Inlet
(°F)
75
76
76
Final, Inle
(°F)
76
76
76
Avg. Inlet
(°F)
75.5
76
76
Initial, Outlet
(°F)
74
74
74
Final, Outlet
(°F)
74
74
74
Avg. Outlet
CF)
74
74
74
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
320.645
331.244
336.545
Final
(ft3)
331.244
336.545
341.865
Net
(ft3)
10.601
5.301
5.32
Meter Temperature
Initial
(°F)
75
72
73
Final
(°F)
75
73
73
Avg.
(°F)
75
72.5
73
Meter Box
Correction
Factor
y
1.011
0.996
0.947
Reference
Orifice Press
AHe
(in. H2O)
1.59
1.79
1.78
10 09017.xls
PostTest050298
6/10/98
-------
1of2
Central Park West
5001 South Miami Boulevard. P.O. Box 12077
f -=f- -a -..-----I i-..-\*:.3j rcesearcn i nangie Kane, norm Carolina 27709-2077
O PACIFIC ENVIRONMENTAL SERVICES, INC. (919)941-0333 FAX: (919) 941-0234
' A^W'::\ •;'^'- :V'::'«aii«3FSp^
Date:
PO.T, in Hg
10/13/97 Calibrator. MMD
29.86
Meter Box No.:
Reference Meter Correction Factor
RMB-15
1.0077
(10/5/97)
AH = 0.5
Trial
1
2
3
Trial
Duration
(min)
15
13
12
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
48.833
54.722
59.821
Final
(ft3)
54.722
59.821
64.544
Net
(ft3)
5.889
5.099
4.723
Meter Temperatures
Initial, Inlet
CF)
73
78
80
Final, Inlet
CF)
77
80
83
Avg. Inlet
CF)
75
79
81.5
Initial, Outlet
(°F)
72
74
76
inal, Outte
CF)
75
76
77
Avg. Outlet
(°F)
73.5
74.5
76.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
34.044
39.829
44.843
Final
(ft3)
39.829
44.843
49.463
Net
(ft3)
5.785
5.014
4.620
Meter Temperature
Initial
CF)
70
71
71
Final
CF)
70
70
71
Avg.
CF)
70
70.5
71
Meter Box
Correction
Factor
T
0.997
1.001
0.999
Reference
Orifice Press
AH0
(in. H20)
1.86
1.86
1.86
AH = 0.75
Trial
1
2
3
Trial
Duration
(min)
8
21
13
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
69.524
73.327
83.322
Final
(ft3)
73.327
83.322
89.571
Net
(ft3)
3.803
9.995
6.249
Meter Temperatures
Initial, Inlet
CF)
74
77
78
Final, Inlet
CF)
74
83
82
Avg. Inlet
CF)
74
80
80
Initial, Outlet
CF)
77
76
78
inal, Outle
CF)
75
77
74
Avg. Outlet
CF)
76
76.5
76
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
54.365
58.108
67.912
Final
(ft3)
58.108
67.912
74.036
Net
(ft3)
3.743
9.804
6.124
Meter Temperature
Initial
CF)
72
72
73
Final
CF)
72
73
73
Avg.
CF)
72
72.5
73
Meter Box
Correction
Factor
7
0.996
0.997
0.995
Reference
Orifice Press
AH0
(in. H20)
1.91
1.91
1.88
AH = 1.0
Trial
1
2
3
Trial
Duration
(min)
19
8
16
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
89.777
100.214
104.614
Final
(ft3)
100.214
104.614
113.404
Net
(ft3)
10.437
4.400
8.790
Meter Temperatures
Initial, Inlet
CF)
82
85
85
Final. Inlet
CF)
86
87
88
Avg. Inlet
CF)
84
86
86.5
Initial, Outlet
CF)
79
81
82
inal, Outle
CF)
80
81
83
Avg. Outlet
CF)
79.5
81
82.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
74.254
84.440
88.743
Final
(ft3)
84.44
88.743
97.302
Net
(ft3)
10.186
4.303
8.559
Meter Temperature
Initial
CF)
73
73
73
Final
CF)
73
73
73
Avg.
CF)
73
73
73
Meter Box
Correction
Factor
T
0.997
1.002
1.000
Reference
Orifice Press
AH0
(in. H20)
1.92
1.91
1.92
Printed- R/KVQft
-------
2 Of 2
Q PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919)941-0333 FAX: (919) 941-0234
AH = 2.0
Trial
1
2
3
Trial
Duration
(min)
9
7
7
Gas Volume
Initial
(ft3)
13.863
20.884
26.372
Final
20.884
26.372
31.871
Net
7.021
5.488
5.499
DryGasMeterRMB-15
Meter Temperatures
Initial, Inlet
CF)
87
90
90
Final, Inlet
CF)
91
92
93
Avg. Inlet
CF)
89
91
91.5
Initial, Outlet
CF)
83
84
84
inal, Outle
CF)
83
84
84
Avg. Outlet
CF)
83
84
84
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(tt3)
97.749
104.591
109.929
Final
(ft3)
104.591
109.929
115.281
Net
(ft3)
6.842
5.338
5.352
Meter Temperature
Initial
CF)
73
73
73
Final
CF)
73
73
74
Avg.
CF)
73
73
73.5
Meter Box
Correction
Factor
T
1.001
1.002
1.002
Reference
Orifice Press
AH0
(in. H20)
1.90
1.89
1.88
AH = 4.0
Trial
1
2
Trial
Duration
(min)
6.5
15.5
DryGasMeterRMB-15
Gas Volume
Initial
(ft3)
32.371
39.484
Final
(ft3)
39.484
56.484
Net
(ft3)
7.113
17.000
Meter Temperatures
Initial, Inlet
CF)
92
93
Final, Inlet
CF)
94
97
Avg. Inlet
CF)
93
95
Initial, Outlet
CF)
85
87
inal, Outle
CF)
85
87
Avg. Outlet
CF)
85
87
Trial
1
2
Reference Meter
Gas Volume
Initial
(ft3)
15.775
22.732
Final
(ft3)
22.732
39.287
Net
(ft3)
6.957
16.555
Meter Temperature
Initial
CF)
73
73
Final
CF)
74
73
Avg.
CF)
73.5
73
Meter Box
Correction
Factor
Y
1.004
1.005
Reference
Orifice Press
AH0
(in. H20)
1.92
1.92
Calibration Results
| AM
0.50
0.75
1.0
2.0
4.0
T
0.999
0.996
1.000
1.002
1.004
AHC
1.86
1.90
1.92
1.89
1.92
Dry Gas Meter RMB-15 on 10/13/97
Meter Box Calibration Factor
Meter Box Reference Orifice Pressure
< — Two Trial Average
1.000
1.90
-------
'PACIFIC ENVIRONMENTAL SERVICES, INC.
Posttest Dry Gas Meter Calibration Form (English Units)
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date: 5/2/98 Pb», in Hg
1.000
12
1.0077
29.94 Calibrator: D. Holzschuh
Meter Box No.
MB-15
AH= 1.41
Trial
1
2
3
Duration
(min)
8
8
11
Dry Gas Meter
Initial
(ft3)
776.09
781.709
787.439
Final
(ft3)
781.709
787.439
795.344
Net
(ft3)
5.619
5.730
7.905
Initial, Inlet
(T)
71
73
73
Final, Inle
(°F)
73
73
73
Avg. Inlet
(°F)
72
73
73
Initial, Outlet
(°F)
69
70
71
Final, Outlet
CF)
70
71
71
Avg. Outlet
CF)
69.5
70.5
71
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
343.209
348.9
354.597
Final
(ft3)
348.9
354.597
362.414
Net
(ft3)
5.691
5.697
7.817
Meter Temperature
Initial
CF)
72
72
72
Final
CF)
72
72
72
Avg.
CF)
72
72
72
Meter Box
Correction
Factor
y
1.015
0.998
0.993
Reference
Orifice Press
AH0
(in. H2O)
1.56
1.56
1.56
15J0137.xto
PostTest50298
6/10/98
-------
REFERENCE METER CALIBRATION
ENGLISH REFERENCE METER UNITS
Baronet He Pretiure 29.82
Meter Tw 1.00000
K ( deg R/fnchet Hg) 17.64
Dry Gaa Meter
Tlae Pressure Meter Readings
(•in) (In. N20)
20.50
5.00
13.00
8.50
27.50
26.50
14.00
15.50
12.50
23.50
17.50
15.00
32.00
35.Cr>
15.00
•8.000
•8.000
•8.000
-5.400
-5.400
-5.400
•3.800
•3.800
-3.800
-2.400
-2.400
-2.400
-1.600
•1.600
-1.600
Initial
742.719
768.193
774.402
790.575
798.821
825.423
850.983
861.899
953.219
962.970
976.611
986.740
995.413
1008.596
1022.986
DGN Serial * 6841495
Date 10/5/97 FUeneM: F:\DATAFILE\CALIBRAT\CAL NEMJ.DSKVDGMJIEF,
Revised: 06/08/95
(DGM) Temperature Vet Test Meter (VTM) DGM Coefficient Flow
Voluw Initial Final Meter Readings VoluM Temp Coefficient Variation Rate
Final (cubic feet) (deg F) (deg F)
768.193
774.402
790.575
798.821
825.423
850.983
861.899
873.960
962.970
976.611
986.740
995.413
1008.596
1022.986
1029.158
25.474
6.209
16.173
8.246
26.602
25.560
10.916
12.061
9.751
13.641
10.129
8.673
13.183
14.390
6.172
78.0
79.0
79.0
79.0
79.0
80.0
81.0
81.0
86.0
86.0
87.0
87.0
88.0
89.0
89.0
79.0
79.0
79.0
79.0
80.0
81.0
81.0
82.0
86.0
87.0
87.0
88.0
89.0
89.0
90.0
Initial
671.890
697.180
703.325
719.309
727.485
753.809
779.025
789.820
879.651
889.205
902.599
912.545
921.069
934.025
948.175
Final (cubic feet) (deg F) Yds Vds-(Avg.Yds) (CFM)
697.180
703.325
719.309
727.485
753.809
779.025
789.820
801.740
889.205-
902.599
912.545
921.069
934.025
948.175
954.255
25.290
6.145
15.984
Max Yds - Mln
Average
8.176
26.324
25.216
Max Yds - Nln
Average
10.795
11.920
9.554
Max Yds - Nln
Average
13.394
9.946
8.524
Max Yds - Min
Average
12.956
14.150
6.080
77.0 1.016
77.0 1.013
77.0 1.012
Yds •0.003626886 Must
Yds -1.013636253 Must
77.0 1.009
77.0 1.008
77.0 1.006
Yds -0.002262496 Must
Yds •1.007525980 Must
77.0 1.006
77.0 1.006
78.0 1.004
Yds -0.002245979 Must
Yds •1.005164785 Must
78.0 1.003
78.0 1.004
78.0 1.006
Yds -0.002785363 Must
Yds -1.004591811 Must
78.0 1.006
78.0 1.007
78.0 1.010
0.002 1.208
0.000 1.204
-0.002 1.204
to no greater than 0.030
to between 0.95 to 1.05
0.001 0.942
0.000 0.938
-0.001 0.932
to no greater than 0.030
to between 0.95 to 1.05
0.001 0.755
0.001 0.753
-0.001 0.747
to no greater than 0.030
to between 0.95 to 1.05
-0.001 0.557
0.000 0.556
0.002 0.556
to no greater than 0.030
to between 0.95 to 1.05
-0.002 0.396
0.000 0.395
0.002 0.396
Max Yds - Mln Yds -0.004205886 Must to no greater than 0.030
Average Yda -1.007822494 Must to between 0.95 to 1.05
Overall Average Yds -1.007748265
I certify that the above Dry Ces Meter was calibrated in accordance with E.P.A. Method 5 , paragraph 7.1 ;CFR 40 Part 60.
using the Precision Wet Test Meter f 11AE6, which In turn was calibrated using the Aoerlcan Bell Prover f 3785.
certificate * F107. wfylcX Is traceable to the National Bureau of Standards (N.I.S.T.).
Signature
Date
-S~'f 7
-------
REFERENCE METER CALIBRATION
ENGLISH REFERENCE METER UNITS
Baraaatric Pressure 29.73
Meter Yw 1.00000
t ( dag R/lnchM Hg) 17.64
OGN Serial
Oat*
6841495
8/28/96
Fid
Revised:
F:\DATAFILE\CALI8RAT\CAL NEHU.OSKXDGM REF.
06/08/95
Tine Pressure Meter Readings
(•in) (in. H20) Initial Final
6.00 -6.60 374.451 381.901
24.00 -6.60 381.901 411.424
8.00 -6.60 411.424 421.233
10.00
35.00
16.50
12.50
14.00
58.50
16.50
42.00
66.50
15.90
13. SO
35.00
-4.00 421.233 430.675
-4.00 430.675 464.147
-4.00 464.147 479.992
-2.80 479.992 489.698
-2.80 489.698 500.594
-2.80 500.594 546.063
-1.60 574.496 583.672
-1.60 590.619 614.123
-1.60 614.123 651.520
-1.00 651.520 657.572
•1.30 657.572 663.065
-1.30 663.365 677.274
Dry Gas Mater (DCN) Temperature
Volume Initial Final
(cubic feet) (deg F) (deg F)
7.450 73.0 76.0
29.523 74.0 76.0
9.809 76.0 76.0
Uet Test Meter (UTM) OGN Coefficient Flow
Meter Readings Volume Tenp Coefficient Variation Rate
Initial Final (cubic feet) (deg F) Yds Yds-(Avg.Yds) (CFM)
496.572 503.987 7.415 77.0 1.007 -0.004 1.207
503.987 533.471 29.484 77.0 1.011 0.000 1.200
533.471 543.279 9.808 77.0 1.015 0.004 1.197
9.442
33.472
15.845
9.706
10.896
45.469
9.176
23.504
37.397
6.052
5.493
14.209
76.0
77.0
77.0
78.0
78.0
78.0
79.0
80.0
80.0
81.0
82.0
82.0
77.0 543.279 552.761
77.0 552.761 585.965
78.0 585.965 601.625
78.0 601.625 611.270
78.0 611.270 622.061
79.0 622.061 667.125
79.0 695.390 704.530
80.0 711.429 734.785
81.0 734.785 771.901
32.0 771.901 777.994
82.0 777.994 783.400
32.0 783.400 797.515
Max Yds - Nin Yds «0.007489914 Mutt to no greater than 0.030
Average Yds «1.011058546 Must to between 0.95 to 1.05
9.482 77.0 1.013 0.009 0.926
33.204 77.0 1.002 -0.003 0.926
15.660 77.0 0.999 -0.006 0.927
Max Yds - Nin Yds "0.014197179 Must to no greater than 0.030
Average Yds -1.004786738 Must to between 0.95 to 1.05
9.645 77.0 1.003 0.002 0.754
10.791 77.0 0.999 -0.002 0.753
45.064 77.0 1.001 0.000 0.752
Max Yds - Min Yds » 0.00338145 Must to no greater than 0.030
Average Yds »1.000808891 Must to between 0.95 to 1.05
9.140 77.0 1.004 0.000 0.541
23.356 77.0 1.003 0.000 0.543
37.116 77.0 1.003 0.000 0.545
Max Yds - Min Yds •0.000835063 Must to no greater than 0.030
Average Yds *1.003302205 Must to between 0.95 to 1.35
5.393
K'.TIS
78.0
78.0
78.0
1.016
0.994
1.003
•5.011
•0.010
0.001
0.396
0.390
0.393
10.113 10.U I.UU3 -M.UUI U.JVJ
Max 'os - Min fds *0.321724294 Must to no grnter than -3.030
Average Yds »1.004344616 Must to between 0.95 to 1.35
Overall Average fds *1.004860199
! certify that the above Dry Gas Meter was calibrated in accordance with 5.P.A. Method 5 . paragraoh 7.1 ,-CFR 40 Part 60,
using the Precision Uet rest Meter * 11AE6, which in :urn *as calibrated using the Aswrican Sell Prover 4 3785,
certificate 4 ?107, -4i^ch is traceable to the National Bureau ?f Stanoaros (H.i.S.T.:.
Signature
71
-------
Mon««Mo ?*LmiumnHtniB*-rt*iiiterHOOK+.MaaaM
KNuMMtWOiMM
ZEROOAS
LOW RANGE
MID RANGE
HK3H RANGE
KNnMFlMlO
ZERO GAS
LOW RANGE
MM) RANGE
HMH RANGE
KM.MMMI.
ZEROOAS
LOW RANGE
MO RANGE
KIN>f4P»Mlli
ZEROOAS
LOW RANGE
MM* OAMAB
flKHMWC
I^M^Bl^^M
KMI04MIMCI
ZEROOAS
LOW RANGE
MM) RANGE
UMftl O*\ftlA0t
HUI» 1 IrWWK
ACTUAL OONC
0
10.7
20
97*
MM
ACTUALOONC
0
10.7
20
37.1
-»
18
T)
g
-------
Table C-5
Saglnaw Kiln #4
Continuous Emissions Monitoring Data Sheet
EPA Method* 3A, 6C, 7E, 10, and 25A
28-Mar-98
INLET
Analyzer
OxygMi
Range
Gas Cone.
0-25%
zero
upscale
0.0
11.1
PraTest
SysxCaL
0.4
11.3
Cat. Bias
% of Span
1.6%
0.8%
POStTMt
Sy*.CaL
0.4
11.3
Cal.BiM
% of Span
1JB%
OJS%
Drift
% of Span
OJO%
0.0%
Carbon Dioxide;
0-40%
zero
0.0
0.2
03%
0.2
03%
0.0%
upscale
11.0
10.7
•0.8%
-0.8%
0.0%
Total Hydrocarbon
0-100ppm
zero
0.0
2.9
0.4
04%
23%
upscale
51.1
53.1
2.0%
53.5
15%
Analyzar Canbnrtton Chaefc
15%
13%
Analyzer
O2 High
O2 Mid
O2 zero
CO2Hbh
CO2Mid
CO2zero
THCHigh
THCMid
THCHigh
THCzero
Gas Cone.
20.2
11.1
0.0 '
20.4
11.0
0.0
84.8
51.1
30.0
0.0
Response
20.1
11.4
0.4
2a3
10.8
02
83.5
53.1
312
za
Error
•040%
120%
1JSO%
•0.25%
•047%
030%
•1JO%
2jOO%
221%
2JO%
-------
snit
Scott Specialty Gases
"pped 1290 COMBERMERE STREET
From: TROY MI 48083
Phone: 248-585-2950
CERTIFICATE OP
Pax: 248-589-2134
ANALYSIS
PACIFIC ENVIRONMENTAL SERVICES
JOHN POWELL
C/0 AIR POLUTION.C & C LT-
60 INDUSTRIAL PARK RD W.
TOLLAND CT 06084
PROJECT #: 05-23193-001
P0#: 104-98-0125
ITEM #: 0502243202 5A
DATE: 2/25/9A
CYLINDER #: A018685
FILL PRESSURE: 2000 PSI
ANALYTICAL ACCURACY: +/-5%
PRODUCT EXPIRATION: 8/26/1998
BLEND TYPE : CERTIFIED WORKING STD
GAS
COMPONENT
HYDROGEN CHLORIDE
NITROGEN
COHC MOLBS
10.
ANALYSIS
(MOLES)
PPM
BALANCE
10.7
PPM
BALANCE
CERTIFIED WORKING STANDARD
ANALYST:
-------
Scott Specialty Gases
Lpped
From:
1290 COMBERMERE STREET
TROY MI 48083
Phone: 248-589-2950
CERTIFICATE OF
Fax: 248-589-2134
ANALYSIS
PACIFIC ENVIRONMENTAL'SERVICES
JOHN POWELL
C/O AIR POLUTION C i C LT '
60 INDUSTRIAL PARK RD W.
TOLLAND CT 06084
PROJECT #: 05-9.3193-002
PO#: 104-98-0125
ITEM #: 0502243202 5A
DATE: 2/13/98
CYLINDER #: A018704
FILL PRESSURE: 2ftOO PSI
ANALYTICAL ACCURACY: +/-5%
PRODUCT EXPIRATION: 8/12/1998
BLEND TYPE : CERTIFIED WORKING STD
. REQUESTED GAS
COMPONENT . ' CONC MOLES
HYDROGEN CHLORIDE ~2T! PFM~"
NITROGEN ' . BALANCE
ANALYSIS
(MOLES)
26.0
PPM
BALANCE
CERTIFIED WORKING.STANARD
ANALYST:
-------
Scott Specialty
snipped
From: ?•
1290 CCMBERMERE STREET
TROY * MI 48083
Phone: 248-589-2950
CERTIFICATE OF
Fax: 248-589-2134
ANALYSIS
PACIFIC ENVIRONMENTAL SERVICES
JOHN POWELL
C/0 AIR POLUTION C & C LT
60 INDUSTRIAL PAWK TZD W.
TOLLAND CT 06084
PROJECT #: 05-23193-003
P0#: 104-98-0125
ITEM #: 0502243202 5A
DATE: 2/25/98
CYLINDER #: A018749
FILL PRESSURE: 200Q PSI
ANALYTICAL ACCURACY: +/-5*
PRODUCT EXPIRATION: 8/25/1998
BLEND TYPE :
COMPONENT
HYDROGEN CHLORIDE
NITROGEN
WORKING STD
REQUESTED GAS
CONG MOLES
40.
PPM
BALANCE
ANALYSIS
(MOLB6)
37
PPM
BALANCE
CERTIFIED WORKING STANDARD
ANALYST:
S -..f.
''
-------
Scott Specialty Gases
uppcd
Prom:
1290 COMBERMERE STREET
TROY MI 48083
Phone: 248-589-2950
CERTIFICATE OP
Fax: 248-589-2134
ANALYSIS
PACIFIC ENVIRONMENTAL SERVICES
JOHN POWELL
C/0 AIR POLUTION C & C LT
60 INDUSTRIAL PARK RD W.
TOLLAND ' CT 06084
PROJECT #: 05-23193-004
PO#: 104-98-0125
ITEM #: 05022430 5A
DATE: 2/12/98
CYLINDER #: A017718
FILL PRESSURE: 2000 PSI
ANALYTICAL ACCURACY: +/-5%
PRODUCT EXPIRATION: 8/12/1998
BLEND TYPE : CERTIFIED WORKING STD
REQUESTED GAS
COMPONENT CONG MOLHS _
HYDROGEN CHLORIDE 100. PPM 10l"
NITROGEN BALANCE
ANALYSIS
(MOLBS)
PPM
BALANCE
CERTIFIED WORKING STANDARD
ANALYST:
-------
ChnMnCTOttlQ
PhonE C2Q3) 29V£B7
• •"" ^^ IB^WF, *«nf^MK0
FAX:
CERTIFICATE OF ANALYSIS
Date:
Record Number
Customer Name:
Purchase Order f:
Grade of Product
Cylinder Number
CC79006
11/4/97
3350
Airya* Chechir*
127383
Primary Standard
Component
Methane
Nitrogen
Required
Concentration
30ppm
Balance
Actual
29.97 ppm
Balance
Uncertainty Of Analytical Result
Approval S'»onafi«
C?
-------
Q*/99'97 00:43
CERTIFICATE OF ANALYSIS CALMAT0X
CIISTOMIfeA&CO Welding^ ladutdtlStgrty
SX^37307
«CRMDffCKs 109-31*46
CXLMAl1 DAXLY • 3
AFXLVSBDATE: IftOft*
KXPTRATtOM DATE: V20V99
5L2ppm
COKC:
CO19&
JUfiCK STAXIIABIK
BXVUODiCBis
CYURDERf:
SRM-1750
SX-20007
MITHOPty
1.140S-04-T1
StttUJL**
MCASU
LASTCALIBfiATlOJfc
31S1A9U13
OC*PID
8/20/96
THIS CERnnCATlON WAS PERPCRMEDACDORDINOTO STANDARDCPERATlNGPItOCEDURES AND 15
TRACEABLE TO AN NOT STAMDASD.
ANALYST
PAJE
TJf/Pr vn
nne
-------
»
CMMlCIQMIO
PHone (203) 2SMK7
FAX (203)250^42
CERTIFICATE OF ANALYSIS
Date:
Customer Name:
Address:
03-5-97 -'Record Number
NORTHEAST AIRGAS CHESHIRE
Purchase Order*: 98537
Grade of Product: Primary Standard
Cylinder Number
CC46103
Component
METHANE
NITROGEN
^Required
^Concentration
85 PPM
BALANCE
1087
• \
Actual g
Concentration
84.8 PPM
BALANCE
Uncnrtairrty of Analytical Result: ± 1 %
I
I
-------
Airqas Specialty Gases
325 McCwrirtCnit
ChaMttCTOttiO
Certificate of Anah
Kec*
Cylinder No:
Cylinder Pressure:
Certification Date
4149
CC84096
2000
37S98"
Purchase Order*
Expiration Date:
Laboratory:
139680
3/2/01
Cheshire, CT
ReferencfiLStandanUnformatton:
Type Component
GMIS Carbon Dioxide
GMIS Oxygen
Cyf. fiumbar
CC34977
CC19914
CfiDCBOtCBflOQ
14.08%
20.08%
Instrumentation;
' Instrumant/Modet/Saflal No.
Rosenwunt/NGA200Qffiacfc#1
Sarvomex/2447701/488
lytica
it PrlnefnlB
NDIR
Pa/magnetic
Analytical Methodology does not require correction for analytical interferences.
Certified Concentrations;
;;:i:;-;):!::;:::;::'
F«w*jn:»«2£ •;•!•;•
-------
NATIONAL SPECIALTY GASES
630 UNrHJD DRIVE
DURHAM, NC
277J3
,
REFERENCE!: U-4M3I
EXP. CATC: 4/3.99 .
METHOD: ANALYZED A
1993O-1 THIS STANDARD SHOl
COMPONENT: CARBON DIC
STANRARD
SRMf 14738
CYL.lt CLM64SI -
CONC 14.01*
INSTRUMENT) ROSEMOUNT
MODEL* IN
SERIAL* 2000411
LASTCAL.: 3/21/W
MBANOONC:' 30
REPLICATE COKC.
DATE: 4WI/96
20J %
20.1 %
20.2 %
(9I9)M
CERTIFICATE OF ANALYSIS '
CYLINDER * CC6WM
LAST ANALVS.S DATE: 4/3/96
EPA PROTOCOL MIXTURES
rvurREssuRfc IOOOPSIG P.O.* 11771
CUSTOMER: CONNECTICUT AIROAS
.0 NOT BE USED WHEN ITS OAS PRESSURE IS BELO^ 1.0 MEOAPASCALS (1 5C- PSK>).
ODE
MMR
..2H W- 0.2%
DATE:
COMPONENT! OXYIKV
STANDARD
SUM*: 2&M |
CYL,* ^ CLM«7^7
CONC: 20.72%)
1NSTIUMCNT: BEdMJlN PARAMAGNETIC
MODfL*: 755 1
SERIAL* 1001419]
LASTCAL.: ^^ 4/lM •
[MEAN CONC: ;
(REPLICATE CONC. i
DATE 4/3/9* ;
20.4 %
20.4 %
205 %
BALANCE OAS: NtTOOOEN
REPUCATBDATA
DATE: 4/3/96
Z 0 R
R 14.0 Z
Z 0 C
ANALWT: 'YY\G^~l
MM W At MATVOML fMC&BLTVQMl
14.1 C 20J
0 C 20.i
20J R 14.!
RE
PLICATE DATA
DATE: 40/96
Z 0
R 394
Z 0
20.4M *.'• 0.3%
DATE:
| RCPUCATB DATA
It 394 C 390
Z 0 C 392
C 390 R 394
3- ZERO C-CANMDXTB R-REFEKENCB \A ^Ifl I
(APPROVED BY: /5BUAA'^
Mixcmo*ic|
(Nitw-imj
• IWtHMEL •
-------
APPENDIX E
PARTICIPANTS
-------
PROJECT PARTICIPANTS
Name
Affiliation
Responsibility
Michael L. Toney
Franklin Meadows
Frank J. Phoenix
Troy Abernathy
Paul Siegel
Gary Gay
Mike Maret
Cybelle Brockman
Eric Dithrich1
Terry Thomasson1
USEPA, Emission Measurement Center
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Pacific Environmental Services, Inc.
Research Triangle Institute
APCC
APCC
Work Assignment Manager
Project Manager
Task Manager
Site Leader/Console Operator
Site Leader/Console Operator
Sampling Technician
Sampling Technician/Sample Recovery
Process Data Recorder
CEM Team Leader
CEM Sampling Technician
1 Subcontractor to Pacific Environmental Services, Inc.
-------
APPENDIX F
PROCESS DATA
-------
RESEARCH TRIANGLE INSTITUTE
/RTI
Center for Environmental Analysis / Environmental Engineering Program
December 14, 1998
TO: Joseph Wood, ESD/MICG (MD-13)
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
FROM: Cybele Brockmann, RTI
SUBJECT: Process data recorded during emissions testing at
Dravo's plant in Saginaw, Alabama, March 28, 1998
REFERENCE: Information Gathering and Analysis for the Lime
Manufacturing Industry NESHAP
EPA Contract 68-D6-0014
ESD Project 95/06
RTI Project 7035-027
Attached is a finalized process description and summary of
process data recorded during emissions testing at Dravo's plant
in Saginaw, Alabama March 28, 1998. The memo was finalized based
on comments received by Lisa Potts, environmental manager for
Dravo Lime Company.1
3040 Cornwallis Road • Post Office Box 12194 • Research Triangle Park, North Carolina 27709-2194 USA
Telephone 919 990-8603 • Fax 919 990-8600
-------
1.0 Process Description
The following is a brief process description of Kiln 4. See
the attached pre-test site survey memo for a more detailed
process description.
Figure 1 is a schematic of Kiln 4. The kiln is an inclined
rotating kiln. Limestone enters at the back end of the kiln (the
highest point of incline) through a preheater, and tumbles toward
the front end of the kiln via gravity and the rotating motion of
the kiln. Combustion air and fuel, which consists of pulverized
coal and coke, enter at the front end of the kiln. Combustion
exhaust exits at the back end of the kiln through the preheater.
Exhaust from the preheater passes through multiclones, a
fan, a reverse-air baghouse, and a stack, from which it is
discharged to the atmosphere. As noted in the pre-test site
survey, ambient air is mixed in with the exhaust at the inlet to
the preheater when the exhaust temperature at this location
exceeds a certain temperature.
2.0 Process Monitoring
Kiln 4 was tested on March 28, 1998. Process data were
recorded during testing. The data were recorded from computer
screens in the kiln control room; the recorded data were measured
with instruments already in place and used by the plant for
process control of the kilns.
Table 1 is a statistical summary of the process data
recorded during testing. Table 2 displays all of process data
recorded during testing. Except for opacity, the recorded
process parameters varied only slightly during testing - as
indicated by the low values of percent relative standard
deviation (% RSD) in Table 1. The % RSD for opacity was high
because of the 40 percent opacity recording at 2:43 pm; as seen
in Table 2, this opacity recording was extremely high compared to
previous recordings, and those that followed. The start-up of
Method 26 testing (which occurred around this time) may have
interfered with the opacity monitor. No other process anomalies
occurred during testing.
The plant does not measure the pressure drop across the
baghouse (one of the process parameters listed in the test plan
for recording). The plant does measure the static pressure
downstream of the fan (just prior to the baghouse); the static
pressure at this location was recorded during testing and had an
average value of 8.3 inches of water. The testing crew took five
-------
measurements of the static pressure at the outlet test location
(just downstream of the baghouse); the measurements were taken
during Method 23 and 26 testing (one measurement per run) and
during the velocity traverse. The five measurements ranged from
-0.47 to -.53 inches of water; the average was - 0.50 inches of
water. The pressure drop from downstream of the fan to the
outlet test location was 7.8 inches of water. A typical value of
the pressure drop across the baghouse was not reported in the
plant's questionnaire or mentioned during the pre-test site
survey.
During testing, kiln 4 produced a high calcium lime from
limestone which was quarried on-site. The plant does not measure
limestone feed rate or lime production rate. Plant personnel
were asked whether or not they knew the production during testing
and they replied no. Consequently, the production level during
testing is not known.
Little information is available to determine if values of
the other recorded parameters were typical of normal operation.
The only relevant parameters reported in the plant's
questionnaire were the exhaust temperature at the exit of the
kiln (2000 degrees Fahrenheit [° F] ) , the inlet temperature to
the baghouse (435 ° F), the ratio of coal and coke to lime (0.20
tons of coal and coke per ton of lime), and the design capacity
of the kiln (900 tons of lime per day) .2 The reported
temperatures are consistent with those recorded during testing.
The average coal and coke feed rate during testing was 6.20 tons
per hour, which was below the range of coal feed rates cited
during the pre-test site survey (6.4 to 6.6 tons of coal per
hour). Based on the average coal and coke feed rate during
testing, and the reported coal and coke to lime ratio, the plant
produced approximately 31 tons of lime per hour during testing;
this translates into approximately 744 tons of lime per day
(assuming the kiln operates 24 hours per day), which is less than
the design capacity of 900 tpd reported in the plant's
questionnaire.3
-------
Table 1. Statistical Summary of Recorded Data for Kiln 4 at Dravo's Plant In Saglnaw, AL.
Recorded 3/28/98 from 10:40 am to 7:00 pm Mean % RSD Minimum Maximum * Recordings
Coal/coke, tph 6.20 2.19 5.96 6.54 28.00
Kiln speed, rpm 1.37 0.714 1.36 1.38 28
Inlet Temperature to preheater, deg F 2002 0.4371 1985 2025 28
Inlet Temperature to baghouse, deg F 466 1.09 460 482 28
opacity, %* 5.4 16 4.3 8 28.0
Static pressure at inlet to baghouse,'H20 8.3 7.0 7.1 9.3 23
tph = tons per hour
rpm = rotations per minute
%RSD = relative standard deviation as a percentage of the mean
•Opacity statistics do not include 40% opacity measurement at 2:43 pm
-------
Table 2. Process Data Collected from Kiln 4 at Dravo's Saglnaw Plant on 3-28-98.
Time
10:40 AM
10:56 AM
11:10 AM
1 1 :25 AM
1 1 :40 AM
1 1 :55 AM
12:10 PM
12:25 PM
12:40 PM
12:55 PM
1:10PM
1 :25 PM
1 :40 PM
1 :58 PM
2:43 PM
3:01 PM
3:16 PM
3:30 PM
4:39 PM
4:55 PM
5:10 PM
5:25 PM
5:40 PM
5:58 PM
6:15 PM
6:30 PM
6:46 PM
7:00 PM
Lime
Produced
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
HICAL
Coal/coke,
tph
6.24
6.28
6.20
6.21
6.28
6.22
6.18
6.21
6.19
6.23
6.19
6.20
6.21
6.21
6.02
6.22
6.16
596
6.01
6.52
5.98
6.35
6.23
6.20
6.30
613
6.54
5.98
Inlet T to
Kiln rpm preheater, deg F
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.36
1.38
1.38
1.38
1.38
1.38
1.38
1.38
1.38
1.38
1.38
1.36
1.36
1.36
1.36
1.36
2000
2001
2001
1997
1998
2000
1998
1998
2004
2002
2007
2010
2011
2025
2001
1992
2002
1999
2002
1989
2012
1985
2011
1987
2012
1989
2007
2006
Inlet T to
bh, deg F
464
466
461
464
463
461
463
463
460
462
460
462
467
464
466
467
465
461
465
465
469
466
470
470
472
472
476
482
Static pressure at inlet
opacity, % to bh, "H20
4.3
4.3
4.3
4.3
4.6
4.6
5.1
5.1
5.1
5.1
5.4
5.4
5.1
5.4
40.0
5.4
5.4
5.4
5.4
6.4
6.7
5.4
6.0
5.4
6.0
8.1
6.4
6.0
9
7.9
7.8
7.6
9
7.8
8.4
9.3
8.9
8.8
8.2
7.1
8.3
7.8
7.7
8.1
8.6
8.3
7.5
8.3
9
8.7
8.6
At 2'43 PM, Method 26 was getting started and may have interfered with the opacity monitor (resulting in the high reading).
The average and % RSD for opacity do not include the opacity reading at 2:43 pm
Acronyms
rpm = rotations per minute
tph = tons per hour
T = temperature
deg F = degrees Fahrenheit
P = pressure
bh = baghouse
HICAL = high calcium lime
Blank cells mean data were not recorded
-------
Limestone
To atmosphere
A
Preheater
Baghouse
D
ambient air (as needed for cooling)
combustion
A air
Lime
pulverized coal and
coke
A = Coal/coke feed rate measurement
B = Temperature measurement at inlet to preheater
C = Static pressure measurement
D = Temperature measurement at inlet to baghouse and inlet testing
E = Opacity Measurement
F = Outlet testing
dashed lines are gas flows
solid lines are material flows
Figure 1. Kiln 4 at Dravo's Saginaw, AL plant
-------
References
1. Docket item II-D-174. Letter, A. Potts, Dravo Lime Company,
to J. Wood, EPA:OAQPS:ESD:MICG, November 2, 1998, Comments
on the Draft Report of the Process Description and Operation
for Dravo's Saginaw, Alabama Facility.
2. Docket item. II-D-42 Letter and attachment, R. Henry, Dravo
Corporation, Dravo Lime Company, to J. Wood, EPA:MICG,
October 30, 1995, enclosing response to NLA/EPA voluntary
questionnaire for Longview plant.
3. Reference 2.
-------
APPENDIX G
TEST METHODS
-------
Appendix G.I
EPA Method 1
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 1 - Sample and Velocity Traverses for Stationary Sources
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. To aid in the representative measurement of
pollutant emissions and/or total volumetric flow rate from a
stationary source, a measurement site where the effluent stream is
flowing in a known direction is selected, and the cross-section of
the stack is divided into a number of equal areas. A traverse
point is then located within each of these equal areas.
1.2 Applicability. This method is applicable to flowing gas
streams in ducts, stacks, and flues. The method cannot be used
when: (1) flow is cyclonic or swirling (see Section 2.4), (2) a
stack is smaller than about 0.30 meter (12 in.) in diameter, or
0.071 m2 (113 in.2) in cross-sectional area, or (3) the measurement
site is less than two stack or duct diameters downstream or less
than a half diameter upstream from a flow disturbance.
The requirements of this method must be considered before
construction of a new facility from which emissions will be
measured; failure to do so may require subsequent alterations to
the stack or deviation from the standard procedure. Cases
involving variants are subject to approval by the Administrator,
U.S. Environmental Protection Agency.
2. PROCEDURE
2.1 Selection of Measurement Site. Sampling or velocity
measurement is performed at a site located at least eight stack or
duct diameters downstream and two -diameters upstream from any flow
disturbance such as a bend, expansion, or contraction in the stack,
or from a visible flame. If necessary, an alternative location may
be selected, at a position at least two stack or duct diameters
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross section, an equivalent diameter (De) shall
be calculated from the following equation, to determine the
upstream and downstream distances:
D = 2LW
e (L + W)
Eq. 1-1
Where
L = Length and W = width.
An alternative procedure is available for determining the
acceptability of a measurement location not meeting the criteria
above. This procedure,
determination of gas flow angles at the sampling points and
comparing the results with acceptability criteria, is described in
Section 2.5.
2.2 Determining the Number of Traverse Points.
2.2.1 Particulate Traverses. When the eight- and two-diameter
criterion can be met, the minimum number of traverse points shall
be: (1) twelve, for circular or rectangular stacks with diameters
(or equivalent diameters) greater than 0.61 meter (24 in.); (2)
eight, for circular stacks with diameters between 0.30 and 0.61
meter (12 and 24 in.); and (3) nine, for rectangular stacks with
equivalent diameters between 0.30 and 0.61 meter (12 and 24 in.).
When the eight- and two-diameter criterion cannot be met, the
minimum number of traverse points is determined from Figure 1-1.
Before referring to the figure, however, determine the distances
from the chosen measurement site to the nearest upstream and
downstream disturbances, and divide each distance by the stack
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 3
diameter or equivalent diameter, to determine the distance in terms
of the number of duct diameters. Then, determine from Figure 1-1
the minimum number of traverse points that corresponds: (1) to the
number of duct diameters upstream; and (2) to the number of
diameters downstream. Select the higher of the two minimum numbers
of traverse points, or a greater value, so that for circular stacks
the number is a multiple of 4, and for rectangular stacks, the
number is one of those shown in Table 1-1.
2.2.2 Velocity (Non-Particulate) Traverses. When velocity or
volumetric flow rate is to be determined (but not particulate
matter), the same procedure as that used for particulate traverses
(Section 2.2.1) is followed, except that Figure 1-2 may be used
instead of Figure 1-1.
2.3 Cross-Sectional Layout and Location of Traverse Points.
2.3.1 Circular Stacks. Locate the traverse points on two
perpendicular diameters according to Table 1-2 and the example
shown in Figure 1-3. Any equation (for examples, see Citations 2
and 3 in the Bibliography) that gives the same values as those in
Table 1-2 may be used in lieu of Table 1-2.
For particulate traverses, one of the diameters must be in a plane
containing the greatest expected concentration variation, e.g.,
after bends, one diameter shall be in the plane of the bend. This
requirement becomes less critical as the distance from the
disturbance increases; therefore, other diameter locations may be
used, subject to the approval of the Administrator.
In addition, for stacks having diameters greater than 0.61 m (24
in.), no traverse points shall be within 2.5 centimeters (1.00 in.)
of the stack walls; and for stack diameters equal to or less than
0.61 m (24 in.), no traverse points shall be located within 1.3 cm'
(0.50 in.) of the stack walls. To meet these criteria, observe the
procedures given below.
2.3.1.1 Stacks With Diameters Greater Than 0.61 m (24 in.), when
any of the traverse points as located in Section 2.3.1 fall within
2.5 cm (1.00 in.) of the
stack walls, relocate them away from the stack walls to: (1) a
distance of
2.5 cm (1.00 in.); or (2) a distance equal to the nozzle inside
diameter, whichever is larger. These relocated traverse points (on
each end of a diameter) shall be the "adjusted" traverse points.
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 4
Whenever two successive traverse points are combined to form a
single adjusted traverse point, treat the adjusted point as two
separate traverse points, both in the sampling (or velocity
measurement) procedure, and in recording the data.
2.3.1.2 Stacks With Diameters Equal To or Less Than 0.61 m (24
in.). Follow the procedure in Section 2.3.1.1, noting only that
any "adjusted" points should be relocated away from the stack walls
to: (1) a distance of 1.3 cm (0.50 in,); or (2) a distance equal to
the nozzle inside diameter, whichever is larger.
2.3.2 Rectangular Stacks. Determine the number of traverse points
as explained in Sections 2.1 and 2.2 of this method. From Table 1-
1, determine the grid configuration. Divide the stack cross-
section into as many equal rectangular elemental areas as traverse
points, and then locate a traverse point at the centroid of each
equal area according to the example in Figure 1-4.
If the tester desires to use more than the minimum number of
traverse points, expand the "minimum number of traverse points"
matrix (see Table 1-1) by adding the extra traverse points along
one or the other or both legs of the matrix; the final matrix need
not be balanced. For example, if a 4 x 3 "minimum number of
points" matrix were expanded to 36 points, the final matrix could
be 9 x 4 or 12 x 3, and would not necessarily have to be 6 x 6.
After constructing the final matrix, divide the stack cross-section
into as many equal rectangular, elemental areas as traverse points,
and locate a traverse point at the centroid of each equal area. The
situation of traverse points being too close to the stack walls is
not expected to arise with rectangular stacks. If this problem
should ever arise, the Administrator must be contacted for
resolution of the matter.
2.4 Verification of Absence of Cyclonic Flow. In most stationary
sources, the direction of stack gas flow is essentially parallel to
the stack walls. However, cyclonic flow may exist (1) after such
devices as cyclones and inertial demisters following venturi
scrubbers, or (2) in stacks having tangential inlets or other duct
configurations which tend to induce swirling; in these instances,
the presence or absence of cyclonic flow at the sampling location
must be determined. The following techniques are acceptable for
this determination. Level and zero the manometer. Connect a Type
S pitot tube to the manometer. Position the Type S pitot tube at
each traverse point, in succession, so that the planes of the face
openings of the pitot tube are perpendicular to the stack cross-
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 5
sectional plane; when the Type S pitot tube is in this position, it
is at "0° reference." Note the differential pressure (Ap) reading
at each traverse point. If a null (zero) pitot reading is obtained
at 0° reference at a given traverse point, an acceptable flow
condition exists at that point. If the pitot reading is not zero
at 0° reference, rotate the pitot tube (up to ±90° yaw angle) ,
until a null reading is obtained. Carefully determine and record
the value of the rotation angle (a) to the nearest degree. After
the null technique
has been applied at each traverse point, calculate the average of
the absolute values of a; assign a values of 0° to those points for
which no rotation was required, and include these in the overall
average. If the average value of a is greater than 20°, the
overall flow condition in the stack is unacceptable, and
alternative methodology, subject to the approval of the
Administrator, must be used to perform accurate sample and velocity
traverses. The alternative procedure described in Section 2.5 may
be used to determine the rotation angles in lieu of the procedure
described above.
2.5 Alternative Measurement Site Selection Procedure. This
alternative applies to sources where measurement locations are less
than 2 equivalent or duct diameters downstream or less than one-
half duct diameter upstream from a flow disturbance. The
alternative should be limited to ducts larger than 24 in. in
diameter where blockage and wall effects are minimal. A
directional flow-sensing probe is used to measure pitch and yaw
angles of the gas flow at 40 or more traverse points; the resultant
angle is calculated and compared with acceptable criteria for mean
and standard deviation.
NOTE: Both the pitch and yaw angles are measured from a line
passing through the traverse point and parallel to the stack axis.
The pitch angle is the angle of the gas flow component in the plane
that INCLUDES the traverse line and is parallel to the stack axis.
The yaw angle is the angle of the gas flow component in the plane
PERPENDICULAR to the traverse line at the traverse point and is
measured from the line passing through the traverse point and
parallel to the stack axis.
2.5.1 Apparatus.
2.5.1.1 Directional Probe. Any directional probe, such as United
Sensor Type DA Three-Dimensional Directional Probe, capable of
measuring both the pitch and yaw angles of gas flows is acceptable.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 6
(NOTE: Mention of trade name or specific products does not
constitute endorsement by the U.S. Environmental Protection
Agency.) Assign an identification number to the directional probe,
and permanently mark or engrave the number on the body of the
probe. The pressure holes of directional probes are susceptible to
plugging when used in particulate-laden gas streams. Therefore, a
system for cleaning the pressure holes by "back-purging" with
pressurized air is required.
2.5.1.2 Differential Pressure Gauges. Inclined manometers, U-tube
manometers, or other differential pressure gauges (e.g., magnehelic
gauges) that meet the specifications described in Method 2, Section
2.2.
NOTE: If the differential pressure gauge produces both negative
and positive readings, then both negative and positive pressure
readings shall be calibrated at a minimum of three points as
specified in Method 2, Section 2.2.
2.5.2 Traverse Points. Use a minimum of 40 traverse points for
circular ducts and 42 points for rectangular ducts for the gas flow
angle determinations. Follow Section 2.3 and Table 1-1 or 1-2 for
the location and layout of the traverse points. If the measurement
location is determined to be acceptable
according to the criteria in this alternative procedure, use the
same traverse point number and locations for sampling and velocity
measurements.
2.5.3 Measurement Procedure.
2.5.3.1 Prepare the directional probe and differential pressure
gauges as recommended by the manufacturer. Capillary tubing or
surge tanks may be used to dampen pressure fluctuations. It is
recommended, but not required, that a pretest leak check be
conducted. To perform a leak check, pressurize or use suction on
the impact opening until a reading of at least 7.6 cm (3 in.) H20
registers on the differential pressure gauge, then plug the impact
opening. The pressure of a leak-free system will remain stable for
at least 15 seconds.
2.5.3.2 Level and zero the manometers. Since the manometer level
and zero may drift because of vibrations and temperature changes,
periodically check the level and zero during the traverse.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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2.5.3.3 Position the probe at the appropriate locations in the gas
stream, and rotate until zero deflection is indicated for the yaw
angle pressure gauge. Determine and record the yaw angle. Record
the pressure gauge readings for the pitch angle, and determine the
pitch angle from the calibration curve. Repeat this procedure for
each traverse point. Complete a "back-purge" of the pressure lines
and the impact openings prior to measurements of each traverse
point.
A post-test check as described in Section 2.5.3.1 is required. If
the criteria for a leak-free system are not met, repair the
equipment, and repeat the flow angle measurements.
2.5.4 Calculate the resultant angle at each traverse point, the
average resultant angle, and the standard deviation using the
following equations. Complete the calculations retaining at least
one extra significant figure beyond that of the acquired data.
Round the values after the final calculations.
2.5.4.1 Calculate the resultant angle at each traverse point:
i = arc cosine [ (cosineY.^) (cosinePi) ]
Eq. 1-2
Where:
PI
resultant angle at traverse point i, degree.
yaw angle at traverse point i, degree.
pitch angle at traverse point i, degree.
2.5.4.2 Calculate the average resultant for the measurements:
-_ ER.
n
Where:
Eq. 1-3
Ra
n
average resultant angle, degree.
total number of traverse points.
2.5.4.3 Calculate the standard deviations:
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EMTIC TM-001
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E (R-
R)
(n-1)
Where :
standard deviation, degree.
2.5.5 The measurement location is acceptable if Ravg
< 10°.
Bj. 1-4
20° and S
2.5.6 Calibration. Use a flow system as described in Sections
4.1.2.1 and 4.1.2.2 of Method 2. In addition, the flow system
shall have the capacity to generate two test-section velocities:
one between 365 and 730 m/min (1200 and 2400 ft/min) and one
between 730 and 1100 m/min (2400 and 3600 ft/min) .
2.5.6.1 Cut two entry ports in the test section. The axes through
the entry ports shall be perpendicular to each other and intersect
in the centroid of the test section. The ports should be elongated
slots parallel to the axis of the test section and of sufficient
length to allow measurement of pitch angles while maintaining the
pitot head position at the test-section centroid. To facilitate
alignment of the directional probe during calibration, the test
section should be constructed of plexiglass or some other
transparent material. All calibration measurements should be made
at the same point in the test section, preferably at the centroid
of the test section.
2.5.6.2 To ensure that the gas flow is parallel to the central
axis of the test section, follow the procedure in Section 2.4 for
cyclonic flow determination to measure the gas flow angles at the
centroid of the test section from two test ports located 90° apart.
The gas flow angle measured in each port must be ±2° of 0°.
Straightening vanes should be installed, if necessary, to meet this
criterion.
2.5.6.3 Pitch Angle Calibration. Perform a calibration traverse
according to the manufacturer's recommended protocol in 5°
increments for angles from -60° to +60° at one velocity in each of
the two ranges specified above. Average the pressure ratio values
obtained for each angle in the two flow ranges, and plot a
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 9
calibration curve with the average values of the pressure ratio (or
other • suitable measurement factor as recommended by the
manufacturer) versus the pitch angle. Draw a smooth line through
the data points. Plot also the data values for each traverse
point. Determine the differences between the measured datavalues
and the angle from the calibration curve at the same pressure
ratio. The difference at each comparison must be within 2° for
angles between 0° and 40° and within 3° for angles between 40° and
60°.
2.5.6.4 Yaw Angle Calibration. Mark the three-dimensional probe
to allow the determination of the yaw position of the probe. This
is usually a line extending the length of the probe and aligned
with the impact opening. To determine the accuracy of measurements
of the yaw angle, only the zero or null position need be calibrated
as follows: Place the directional probe in the test section, and
rotate the probe until the zero position is found. With a
protractor or other angle measuring device, measure the angle
indicated by the yaw angle indicator on the three-dimensional
probe. This should be within 2° of 0°. Repeat this measurement
for any other points along the length of the pitot where yaw angle
measurements could be read in order to account for variations in
the pitot markings used to indicate pitot head positions.
BIBLIOGRAPHY
1. Determining Dust Concentration in a Gas Stream, ASME
Performance Test Code No. 27. New York. 1957.
2. DeVorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District. Los Angeles, CA. November
1963.
3. Methods for Determining of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
4. Standard Method for Sampling Stacks for Particulate Matter.
In: 1971 Book of ASTM Standards, Part 23. ASTM Designation D
2928-71. Philadelphia, PA. 1971.
5. Hanson, H.A., et al. Particulate Sampling Strategies for
Large Power Plants Including Nonuniform Flow. USEPA, ORD,
ESRL, Research Triangle Park, NC. EPA-600/2-76-170. June
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 10
6.
7.
8
10,
11
12
13,
14
1976.
Entropy Environmentalists, Inc. Determination of the Optimum
Number of Sampling Points: An Analysis of Method 1 Criteria.
Environmental Protection Agency. Research Triangle Park, NC.
EPA Contract No. 68-01-3172, Task 7.
Hanson, H.A., R.J. Davini, J.K. Morgan, and A.A. Iversen.
Particulate Sampling Strategies for Large Power Plants
Including Nonuniform Flow. USEPA, Research Triangle Park, NC.
Publication No. EPA-600/2-76-170. June 1976. 350 p.
Brooks, E.F., and R.L. Williams. Flow and Gas Sampling
Manual. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/2-76-203. July
1976. 93 p.
Entropy Environmentalists, Inc. Traverse Point Study.
Contract No. 68-02-3172. June 1977. 19 p.
EPA
Brown, J. and K. Yu. Test Report: Particulate Sampling
Strategy in Circular Ducts. Emission Measurement Branch.
Emission Standards and Engineering Division. U.S.
Environmental Protection Agency, Research Triangle Park, NC
27711. July 31, 1980. 12 p.
Hawksley, P.G.W., S. Badzioch, and J.H. Blackett. Measurement
of Solids in Flue Gases. Leatherhead, England, The British
Coal Utilisation Research Association. 1961. p. 129-133.
Knapp, K.T. The Number of Sampling Points Needed for
Representative Source Sampling. In: Proceedings of the Fourth
National Conference on Energy and Environment. Theodore, L.
et al. (ed). Dayton, Dayton Section of the American Institute
of Chemical Engineers. October 3-7, 1976. p. 563-568.
Smith, W.S. and D.J. Grove. A Proposed Extension of EPA
Method 1 Criteria. Pollution Engineering. XV (8):36-37.
August 1983.
Gerhart, P.M. and M.J. Dorsey. Investigation of Field Test
Procedures for Large Fans. University of Akron. Akron, OH.
(EPRI Contract CS-1651). Final Report (RP-1649-5) . December
1980.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 11
15. Smith, W.S. and D.J. Grove. A New Look at Isokinetic Sampling
Theory and Applications. Source Evaluation Society
Newsletter. VIII(3) :19-24 . August 1983.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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Table 1-1. CROSS-SECTION LAYOUT FOR
RECTANGULAR STACKS
-Number of traverse points
Matrix layout
9
12
16
20
25
30
36
42
49
3x3
4x3
4x4
5x4
5x5
6x5
6x6
7x6
7x7
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EMTIC TM-001
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TABLE 1-2
LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
(Percent of stack diameter from inside
wall to traverse point)
Traverse
Point
Number on a
Diameter
1
2
3
4
5 ....
6
7
8 ....
9
10 ....
11 ....
12 ....
13 ....
2
14
.6
85
.4
4
6.
7
25
.0
75
.0
93
.3
Number of traverse points on a diameter
6
4.
4
14
.6
29
.6
70
.4
85
.4
95
.6
8
3.
2
10
.5
19
.4
32
.3
67
.7
80
.6
89
.5
96
.8
10
2.6
8.2
14.
6
22.
6
34.
2
65.
8
77.
4
85.
4
91.
8
97.
4
12
2.1
6.7
11.
8
17.
7
25.
0
35.
6
64.
4
75.
0
82.
3
88.
2
93.
3
97.
9
14
1.8
5.7
9.9
14.
6
20.
1
26.
9
36.
6
63.
4
73.
1
79.
9
85.
4
90.
1
94.
3
16
1.6
4.9
8.5
12.
5
16.
9
22.
0
28.
3
37.
5
62.
5
71.
7
78.
0
83.
1
87.
5
18
1.
4
4 .
4
7.
5
10
.9
14
.6
18
.8
23
.6
29
.6
38
.2
61
.8
70
.4
76
.4
81
.2
20
1.
3
3.
9
6.
7
9.
7
11
2.
9
16
.5
20
.4
25
.0
30
.6
38
.8
61
.2
69
.4
75
.0
22
1.1
3.5
6.0
8.7
11.
6
14.
6
18.
0
21.
8
26.
2
31.
5
39.
3
60.
7
68.
5
24
1.1
3.2
5.5
7.9
10.
5
13.
2
16.
1
19.
4
23.
0
27.
2
32.
3
39.
8
60.
2
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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14 ....
15 ....
16 ....
17 ....
18 ....
19 ....
20 ....
21 ....
22 ....
23 ....
24 ....
98.
2
91.
5
95.
1
98.
4
85
.4
89
.1
92
.5
95
.6
98
.6
79
.6
83
.5
87
.1
90
.3
93
.3
96
.1
98
.7
73.
8
78.
2
82.
0
85.
4
88.
4
91.
3
94.
0
96.
5
98.
9
67.
7
72.
8
77 .
0
80.
6
83.
9
86.
8
89.
5
92.
1
94.
5
96.
8
98.
9
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EMTIC TM-001
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Duct Diameters Upstream from Flew Disturbance* (Distance A)
1.5 2.0
2.5
50 U
40
30
20
10
0
I I
Higher Number a fix-
Rectangular Stacks or Ducts
24 or 25
— " From Point of Any Type of
Disturbance (Bend. Expansion. C
I
20
.ontrvcbon, etc.
I
16
)
! I
t
T"
B
I M*a«urement
[_ Srt*
r-~
Disturb* nc«
V — I
™
™
Stack Diameter > 0.61 m (24 m.)
12
.or.'
Stack Diameter • 0 30 to 0.61 m (1 2-24 in )
I I I
I
345678
Duct Diameters Downstream from Flow Disturbance* (Distance B)
Figure 1-1. Minimum number of traverse points for
particulate traverses.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
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50
0.5
40 -
30 -
20 -
10 -
Duct Diameters Upstream from Flow Disturbance* (Distance A)
1.0 15 20
2.5
I I I I I '1
8 Higher Number is for
Rectangular Stacks or Ducts
16 Stack Dii
I
_^
j.
B
I
|
/Disturbance
Measurement
Site
Disturbance
V - — I
-
meter > 0.61 m (24 In.)
|
— * From Point of Any Type of
Disturbance (Bend. Expansion. Contraction, etc.)
Stack Diameter
I I I I I I
12
8or98 —
> 0.30 to 0.61 m (12-24 In )
I
345678
Duct Diameters Downstream from Row Disturbance* (Distance B)
10
Figure 1-2. Minimum number of traverse points for velocity
(nonparticulate) traverses.
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Traverse
Pant
1
2
3
4
5
6
Distance
% of dameter
44
147
295
705
853
956
Figure 1-3. Example showing circular stack cross section
divided into 12 equal areas, with location of traverse
points indicated.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 18
0
o
o
o
o
J
o
o
h 1
o
o
o
o
o
Figure 1-4 . Example showing rectangular stack cross section
divided into 12 equal areas, with a traverse point at centroid
of each area.
-------
STACK SAMPLING CYCLONIC FLOH
General
Conventional sampling procedures are not applicable to stacks with
cyclonic flow due to the presence of non-axial flow components. This
appendix describes a method for sampling stacks with cyclonic flow; I.e.
flow with tangential velocity components. Cyclonic flow may exist after
cyclones, tangential Inlets, or other configurations that may tend to
Induce swirling.
Several different approaches have been devised to minimize the biasing
effects of non-axial flow. The method discussed In this appendix
utilizes the alignment approach to reduce or eliminate the bias produced
by misalignment of the sampling nozzle and pltot tubes with the path of
the particles. Sampling results obtained with this method must be
reviewed for possible Inherent bias (see section entitled Accuracy
Considerations) to determine acceptability for any purpose.
Accuracy Considerations
As discussed 1n Chapter 5, small (light) particles tend to follow the
flow stream while Jarge (heavy) particles tend to be affected more by
their own Inertia than by the How stream. Due to the effects of tht
cyclonic condition and centrifugal action, components of radial velocity
should be Imparted to large particles, while small particles continue to
follow the flow stream. If the sampling ports are sufficiently down-
stream of the onset of cyclonic flow (at least two stack diameters),
large particles should have moved to the vicinity of the stack wall and
no longer have radial velocity components. For this reason, this method
does not consider components of radial velocity, and the term "total
velocity vector" refers to the resultant of the vertical (parallel to
the stack axis) velocity vector and the tangential velocity vector.
Although sampling by the alignment approach Is done 1n the direction of
flow of the stack gas at each sample point, bias may still be produced
1f the path of the particles Is not In the direction of flow. Small
particles follow the flow stream and large particles at the stack wall
have no radial velocity components so the only source of bias should be
large particles near the stack wall that may not be moving In the direc-
tion of flow, I.e. unequal tangential velocity components. An Indica-
tion of the distribution of large and small particles may be obtained by
conparlng the probe wash and cyclone catch to the filter and 1mp1nger
catch. Large particles that do not follow the now stream should be
caught In the probe and cyclone, while small particles should be caught
on the filter and In the 1mp1ngers. Such comparison may yield
-------
Information on possible bias 1n the sample since bias Is produced by
Urge particles, but should not be considered to be an accurate deter- -
n1 nation of particle size distribution. If the Urge particles Mere not
Bovlng In the direction of flow 1n the stack, the large/small particle
proportion 1n the sampling train may not be the save as In the stack.
If all particles are wring parallel to the direction of flow, no bias
should be produced.
If the pollutant 1s or behaves as a gas, no bias Is produced by par-
ticles novlng 1n directions other than parallel to the flow stream.
This method provides an accurate determination of velocity and flow
rate, which are requirements of gaseous sampling (Chapter 6). The
larger the proportion of the total catch that behaves as a gas (filter
and Inplngers), the greater the confidence In the sample being without
bias.
•
Detenrlnlng Cyclonic Flow •
The existence of cyIconic flow 1s determined by measuring the flow angle
at each sample point. The flow angle 1s the angle between the direction
of now and the axis of the stack. If the average of the absolute val-
ues of the flow angles 1s greater than 20*. cyclonic flow exists to such
an extent that special sampling procedures are necessary.
The direction of flow 1s determined by locating the pltot tube null posi-
tion at each sample point. The pltot tube null position at a sample
point 1s determined by rotating the pltot tubes around the axis of the
probe until a zero manometer reading 1s obtained. Advance knowledge of
the direction of the tangential flow component 1s helpful for the Ini-
tial rotation of the pltot tubes since the plane through the pltot tubes
must be perpendicular to the total velocity vector to obtain a null read-
Ing on the manometer. The angle between the plane through the pltot
tubes In the null position and the stack cross->sect1ona1 plane Is equal
In magnitude to the flow angle; the magnitude of the angle may be
measured with the pltot tubes In the null position or after the pltot
tubes have been rotated 90* Into the flow stream for velocity measure-
ment. A magnetic protractor-level 1s a convenient angle measuring de-
vice; scribe marks on the sample box with a pointer on the probe (or
vice-versa) may be satisfactory 1f proper alignment with the axis of the
stack and the plane of the pltot tubes Is maintained.
In some cases of cyclonic flow, the flew angle may be greater than 90*
at some sample points. Indicating flow back Into the stack at those
particular sample points. If the flow angle 1s greater than 90*, It 1s
recorded as 90* so that sample points with negative velocity are con-
sidered to have no vertical velocity (cos 90* • 0). The existence of
sample points with negative velocity may be determined with the pltot
tubes aligned with the flow stream; the manometer deflection will Indi-
cate the direction of flow.
-------
Sampling Procedure
•__^__B& _^____—«» ,
Standard 1sok1net1c sampling procedures (Chapters 4 and 5) are followed
except for adjustment of the sampling time and pi tot tube and nozzle
orientation at each sample point.
Preliminary Velocity Traverse and Calculations
Knowledge of the flow angles at all sampling points Is necessary to
Insure that the total sample time and total sample volume 1s adequate; •
therefore, flow angles are normally measured during the preliminary
velocity traverse. The complete set of angles should be measured In as
short a duration of time as possible In case the position of the flow
cyclone In the stack 1s changing with time. After the measurement of
flow angles 1s complete, a base sampling time for each sampling point 1s
selected. The actual sampling time at each sample point Is the base
sampling time multiplied by the cosine of the flow angle at that sample
point.
All preliminary procedures and calculations are performed with prelimi-
nary data as measured 1n the direction of flow similar to standard 1so-
kinetic sampling procedures. The actual sampling time at each sample
point (base time x cos a) 1s used 1n preliminary calculations. As
discussed earlier, If zero or negative flow exists at any sample point,
the now angle 1s recorded as 90* and the actual sampling time at that
sample point 1s zero (cos 90* • 0). The base time should be large
enough so that the total sample volume 1s adequate and that the sampling
time at the sample point with the shortest actual sampling time Is long.
enough to record data. Appendix 0 contains data forms for recording
angles and sampling times along with forms for standard stack sampling.
Sampling
Sampling 1s performed with the nozzle and pltot tubes oriented 1n the
direction of flow at each sampling point with 1sok1net1c conditions
maintained according to the AP measured 1n the flow stream. As dis-
cussed 1n the section on Accuracy Considerations, radial velocity
components are not considered since large particles should have no
radial velocity components. Since large particles should be concen-
trated near the stack wall, the accuracy of sampling at the outer points
1s of particular Importance. The precalculated sampling time at each
sampling point Is the base time multiplied by the cosine of the How
angle. For Instance, If the base sampling time 1s four minutes and the
How angle 1s 60* at one sample point, the actual sampling time at that
sample point Is two minutes (cos 60* • 0.5). It 1s suggested that
sampling at each sample point be started at some Increment of a minute
or that a timer be used for each sample point to avoid confusion with
various odd minutes and seconds. The flow may be stopped for short
-------
periods between sample points, but the off-time must not be so long that
the sample could be contaminated by particles entering the sampling
train while the flow 1s stopped.
In some cases of cyclonic flow, some sample points may have negative
flow or flow back Into the stack (flow angle > 9(f) rather than out the
stack. These sampling points are treated as points with zero flow and
zero actual sampling time. This situation may cause the results to be
biased high If some of the pollutant sampled at the sample points with
positive flow 1s also present at the sample points with negative flow.
Two separate samples may produce more accurate results In such a case -
one sample for positive flow and one sample for negative flow with the
numerical difference being the emission rate.
The field check of percent 1sok1net1c 1s made using actual parameters
measured during sampling; velocity 1s used as measured In the flow
stream and time 1s the sum of the adjusted (actual) sampling times for
the separate sample points. -The 1sok1net1c check could also be per-
formed by calculating the vertical velocity component at each sample
point and using the total base time as explained 1n the section on Data
Reduction, but this approach 1s considered too cumbersome for field use.
Data Reduction
Data reduction procedures must account for the differences between the
total velocity vectors (defined by a and AP) and the exiting components
of these vectors. Since the average exiting velocity mist be used to
calculate stack flow rate (ACFM or SCFM), effective stack height, and,
In turn, allowable emission rate and standard effective stack height,
data reduction procedures must average only the vertical components of
the total velocity vectors. Different data reduction approaches may
yield correct results; the data reduction procedures discussed 1n this
section are based on adjustment of Individual AP readings to correspond
to vertical velocity components. Standard data reduction procedures are
discussed 1n Chapter 8 and only the adjustments to the Input data neces-
sary to apply the standard procedures are discussed here.
Each field AP reading (as measured 1n the flow stream) 1s multiplied by
the square of the cosine of the flow angle («) corresponding to each AP
reading. Data reduction Input AP Is (cosz«) (field AP). Input sample
time per sample point 1$ the total base sampling time per sample point
and the total sampling time Input Is the total base time (base time)
(number of sample points). All other parameters are Input as measured.
The data sheets In Appendix 0 should be helpful In organizing cyclonic
flow data.
-------
CYCLONIC FLOW FIELD CALCULATION SHEET
Company Name_
Address
Data
Sampling Location
Tester
Base Test Time
Sanpl e
Point
•
.
\ng1e
*
Tint
•
f
Run I
*
AP
cos * ( $p)
Boa t
A?
•
cos* (VSJH
Run t
AP
co$ 4 (/Ep)
T««C Tint • eg« * (Baa* Tia«)
Average
Avertgt Apy
Avtragt
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Appendix G.2
EPA Method 2
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 2 - Determination of Stack Gas Velocity and Volumetric
Flow Rate (Type S Pitot Tube)
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. The average gas velocity in a stack is determined from the gas
density and from measurement of the average velocity head with a Type S
(Stausscheibe or reverse type) pitot tube.
1.2 Applicability. This method is applicable for measurement of the average
velocity of a gas stream and for quantifying gas flow.
This procedure is not applicable at measurement sites that fail to meet the
criteria of Method 1, Section 2.1. Also, the method cannot be used for direct
measurement in cyclonic or swirling gas streams; Section 2.4 of Method 1 shows
how to determine cyclonic or swirling flow conditions. When unacceptable
conditions exist, alternative procedures, subject to the approval of the
Administrator, U.S. Environmental Protection Agency, must be employed to make
accurate flow rate determinations; examples of such alternative procedures are:
(1) to install straightening vanes; (2) to calculate the total volumetric flow
rate stoichiometrically, or (3) to move to another measurement site at which the
flow is acceptable.
2. APPARATUS
Specifications for the apparatus are given below. Any other apparatus that has
been demonstrated (subject to approval of the Administrator) to be capable of
meeting the specifications will be considered acceptable.
2.1 Type S Pitot Tube. Pitot tube made of metal tubing (e.g., stainless steel)
as shown in Figure 2-1. It is recommended that the external tubing diameter
(dimension Dt, Figure 2-2b) be between 0.48 and 0.95 cm (3/16 and 3/8 inch).
There shall be an equal distance from the base of each leg of the pitot tube to
its face-opening plane (dimensions PA and E^, Figure 2-2b); it is recommended
that this distance be between 1.05 and 1.50 times the external tubing diameter.
The face openings of the pitot tube shall, preferably, be aligned as shown in
Figure 2-2; however, slight misalignments of the openings are permissible (see
Figure 2-3).
The Type S pitot tube shall have a known coefficient, determined as outlined in
Section 4. An identification number shall be assigned to the pitot tube; this
Prepared by Emission Measurement Branch EMTIC M-002
Technical Support Division, OAQPS, EPA
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
number shall be permanently marked or engraved on the body of the tube. A
standard pitot tube may be used instead of a Type S, provided that it meets the
specifications of Sections 2.7 and 4.2; note, however, that the static and impact
pressure holes of standard pitot tubes are susceptible to plugging in
particulate-laden gas streams. Therefore, whenever a standard pitot tube is used
to perform a traverse, adequate proof must be furnished that the openings of the
pitot tube have not plugged up during the traverse period; this can be done by
taking a velocity head (Ap) reading at the final traverse point, cleaning out the
impact and static holes of the standard pitot tube by "back-purging" with
pressurized air, and then taking another Ap reading. If the Ap readings made
before and after the air purge are the same (±5 percent) , the traverse is
acceptable. Otherwise, reject the run. Note that if Ap at the final traverse
point is unsuitably low, another point may be selected. If "back-purging" at
regular intervals is part of the procedure, then comparative Ap readings shall
be taken, as above, for the last two back purges at which suitably high Ap
readings are observed.
2.2 Differential Pressure Gauge. An inclined manometer or equivalent device.
Most sampling trains are equipped with a 10-in. (water column) inclined-vertical
manometer, having 0.01-in. H2O divisions on the 0- to 1-in. inclined scale, and
0.1-in. H20 divisions on the 1- to 10-in. vertical scale. This type of manometer
(or other gauge of equivalent sensitivity) is satisfactory for the measurement
of Ap values as low as 1.3 mm (0.05 in.) H20. However, a differential pressure
gauge of greater sensitivity shall be used (subject to the approval of the
Administrator), if any of the following is found to be true: (1) the arithmetic
average of all Ap readings at the traverse points in the stack is less than
1.3 mm (0.05 in.) H20; (2) for traverses of 12 or more points, more than 10
percent of the individual Ap readings are below 1.3 mm (0.05 in.) H20; (3) for
traverses of fewer than 12 points, more than one Ap reading is below 1.3 mm
(0.05 in.) H20. Citation 18 in the Bibliography describes commercially available
instrumentation for the measurement of low-range gas velocities.
As an alternative to criteria (1) through (3) above, the following calculation
may be performed to determine the necessity of using a more sensitive
differential pressure gauge:
Prepared by Emission Measurement Branch EMTIC M-002
Technical Support Division, OAQPS, EPA
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EMTIC TM-002 NSPS TEST METHOD Page 3
T =
. +K
W *• "
i = l
Where:
Api. = Individual velocity head reading at a traverse point, mm (in.)
H20.
n = Total number of traverse points.
K = 0.13 mm H20 when metric units are used and 0.005 in. H20 when
English units are used.
If T is greater than 1.05, the velocity head data are unacceptable and a more
sensitive differential pressure gauge must be used.
NOTE: If differential pressure gauges other than inclined manometers are used
(e.g., magnehelic gauges), their calibration must be checked after each test
series. To check the calibration of a differential pressure gauge, compare Ap
readings of the gauge with those of a gauge-oil manometer at a minimum of three
points, approximately representing the range of Ap values in the stack. If, at
each point, the values of Ap as read by the differential pressure gauge and
gauge-oil manometer agree to within 5 percent, the differential pressure gauge
shall be considered to be in proper calibration. Otherwise, the test series
shall either be voided, or procedures to adjust the measured Ap values and final
results shall be used, subject to the approval of the Administrator.
2.3 Temperature Gauge. A thermocouple, liquid-filled bulb thermometer,
bimetallic thermometer, mercury-in-glass thermometer, or other gauge capable of
measuring temperature to within 1.5 percent of the minimum absolute stack
temperature. The temperature gauge shall be attached to the pitot tube such that
the sensor tip does not touch any metal; the gauge shall be in an interference-
free arrangement with respect to the pitot tube face openings (see Figure 2-1 and
also Figure 2-7 in Section 4). Alternative positions may be used if the pitot
tube-temperature gauge system is calibrated according to the procedure of Section
4. Provided that a difference of not more than 1 percent in the average velocity
measurement is introduced, the temperature gauge need not be attached to the
pitot tube; this alternative is subject to the approval of the Administrator.
2.4 Pressure Probe and Gauge. A piezometer tube and mercury- or water-filled
U-tube manometer capable of measuring stack pressure to within 2.5 mm (0.1 in.)
Hg. The static tap of a standard type pitot tube or one leg of a Type S pitot
tube with the face opening planes positioned parallel to the gas flow may also
be used as the pressure probe.
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EMTIC TM-002 NSPS TEST METHOD Page 4
2.5 Barometer. A mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See NOTE in Method 5,
Section 2.1.9.
2.6 Gas Density Determination Equipment. Method 3 equipment, if needed (see
Section 3.6), to determine the stack gas dry molecular weight, and Reference
Method 4 or Method 5 equipment for moisture content determination; other methods
may be used subject to approval of the Administrator.
2.7 Calibration Pitot Tube. When calibration of the Type S pitot tube is
necessary (see Section 4), a standard pitot tube for a reference. The standard
pitot tube shall, preferably, have a known coefficient, obtained either (1)
directly from the National Bureau of Standards, Route 70 S, Quince Orchard Road,
Gaithersburg, Maryland, or (2) by calibration against another standard pitot tube
with an NBS-traceable coefficient. Alternatively, a standard pitot tube designed
according to the criteria given in Sections 2.7.1 through 2.7.5 below and
illustrated in Figure 2-4 (see also Citations 7, 8, and 17 in the Bibliography)
may be used. Pitot tubes designed according to these specifications will have
baseline coefficients of about 0.99 ± 0.01.
2.7.1 Hemispherical (shown in Figure 2-4) ellipsoidal, or conical tip.
2.7.2 A minimum of six diameters straight run (based upon D, the external
diameter of the tube) between the tip and the static pressure holes.
2.7.3 A minimum of eight diameters straight run between the static pressure
holes and the centerline of the external tube, following the 90-degree bend.
2.7.4 Static pressure holes of equal size (approximately 0.1 D) , equally spaced
in a piezometer ring configuration.
2.7.5 Ninety-degree bend, with curved or mitered junction.
2.8 Differential Pressure Gauge for Type S Pitot Tube Calibration. An inclined
manometer or equivalent. If the single-velocity calibration technique is
employed (see Section 4.1.2.3), the calibration differential pressure gauge shall
be readable to the nearest 0.13 mm (0.005 in.) H20. For multivelocity
calibrations, the gauge shall be readable to the nearest 0.13 mm (0.005 in.) H20
for Ap values between 1.3 and 25 mm (0.05 and 1.0 in.) H20, and to the nearest
1.3 mm (0.05 in.) H20 for Ap values above 25 mm (1.0 in.) H20. A special, more
sensitive gauge will be required to read Ap values below 1.3 mm (0.05 in.) H20
(see Citation 18 in the Bibliography).
3. PROCEDURE
3.1 Set up the apparatus as shown in Figure 2-1. Capillary tubing or surge
tanks installed between the manometer and pitot tube may be used to dampen Ap
fluctuations. It is recommended, but not required, that a pretest leak-check be
conducted as follows: (1) blow through the pitot impact opening until at least
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EMTIC TM-002 NSPS TEST METHOD Page 5
7.6 cm (3 in.) H20 velocity pressure registers on the manometer; then, close off
the impact opening. The pressure shall remain stable for at least 15 seconds;
(2) do the same for the static pressure side, except using suction to obtain the
minimum of 7.6 cm (3 in.) H20. Other leak-check procedures, subject to the
approval of the Administrator, may be used.
3.2 Level and zero the manometer. Because the manometer level and zero may
drift due to vibrations and temperature changes, make periodic checks during the
traverse. Record all necessary data as shown in the example data sheet
(Figure 2-5) .
3.3 Measure the velocity head and temperature at the traverse points specified
by Method 1. Ensure that the proper differential pressure gauge is being used
for the range of Ap values encountered (see Section 2.2). If it is necessary to
change to a more sensitive gauge, do so, and remeasure the Ap and temperature
readings at each traverse point. Conduct a post-test leak-check (mandatory), as
described in Section 3.1 above, to validate the traverse run.
3.4 Measure the static pressure in the stack. One reading is usually adequate.
3.5 Determine the atmospheric pressure.
3.6 Determine the stack gas dry molecular weight. For combustion processes or
processes that emit essentially C02, 02, CO, and N2, use Method 3. For processes
emitting essentially air, an analysis need not be conducted; use a dry molecular
weight of 29.0. For other processes, other methods, subject to the approval of
the Administrator, must be used.
3.7 Obtain the moisture content from Reference Method 4 (or equivalent) or from
Method 5.
3.8 Determine the cross-sectional area of the stack or duct at the sampling
location. Whenever possible, physically measure the stack dimensions rather than
using blueprints.
4. CALIBRATION
4.1 Type S Pitot Tube. Before its initial use, carefully examine the Type S
pitot tube in top, side, and end views to verify that the face openings of the
tube are aligned within the specifications illustrated in Figure 2-2 or 2-3. The
pitot tube shall not be used if it fails to meet these alignment specifications.
After verifying the face opening alignment, measure and record the following
dimensions of the pitot tube: (a) the external tubing diameter (dimension Dt/
Figure 2-2b); and (b) the base-to-opening plane distances (dimensions PA and PB,
Figure 2-2b). If Dt is between 0.48 and 0.95 cm (3/16 and 3/8 in.), and if $
and PB are equal and between 1.05 and 1.50 Dc, there are two possible options:
(1) the pitot tube may be calibrated according to the procedure outlined in
Sections 4.1.2 through 4.1.5 below, or (2) a baseline (isolated tube) coefficient
value of 0.84 may be assigned to the pitot tube. Note, however, that if the
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EMTIC TM-002 NSPS TEST METHOD Page 6
pitot tube is part of an assembly, calibration may still be required, despite
knowledge of the baseline coefficient value (see Section 4.1.1).
If Dt, ^ , and ? are outside the specified limits, the pitot tube must be
calibrated as outlined in Sections 4.1.2 through 4.1.5 below.
4.1.1 Type S Pitot Tube Assemblies. During sample and velocity traverses, the
isolated Type S pitot tube is not always used; in many instances, the pitot tube
is used in combination with other source-sampling components (thermocouple,
sampling probe, nozzle) as part of an "assembly." The presence of other sampling
components can sometimes affect the baseline value of the Type S pitot tube
coefficient (Citation 9 in the Bibliography); therefore an assigned (or otherwise
known) baseline coefficient value may or may not be valid for a given assembly.
The baseline and assembly coefficient values will be identical only when the
relative placement of the components in the assembly is such that aerodynamic
interference effects are eliminated. Figures 2-6 through 2-8 illustrate
interference-free component arrangements for Type S pitot tubes having external
tubing diameters between 0.48 and 0.95 cm (3/16 and 3/8 in.). Type S pitot tube
assemblies that fail to meet any or all of the specifications of Figures 2-6
through 2-8 shall be calibrated according to the procedure outlined in Sections
4.1.2 through 4.1.5 below, and prior to calibration, the values of the
intercomponent spacings (pitot-nozzle, pitot-thermocouple, pitot-probe sheath)
shall be measured and recorded.
NOTE: Do not use any Type S pitot tube assembly which is constructed such that
the impact pressure opening plane of the pitot tube is below the entry plane of
the nozzle (see Figure 2-6B).
4.1.2 Calibration Setup. If the Type S pitot tube is to be calibrated, one leg
of the tube shall be permanently marked A, and the other, B. Calibration shall
be done in a flow system having the following essential design features:
4.1.2.1 The flowing gas stream must be confined to a duct of definite cross-
sectional area, either circular or rectangular. For circular cross sections, the
minimum duct diameter shall be 30.5 cm (12 in.); for rectangular cross sections,
the width (shorter side) shall be at least 25.4 cm (10 in.).
4.1.2.2 The cross-sectional area of the calibration duct must be constant over
a distance of 10 or more duct diameters. For a rectangular cross section, use
an equivalent diameter, calculated from the following equation, to determine the
number of duct diameters:
2LW
(L + W)
Eq. 2-1
Where:
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EMTIC TM-002 NSPS TEST METHOD Page 7
De = Equivalent diameter.
L = Length.
W = Width.
To ensure the presence of stable, fully developed flow patterns at the
calibration site, or "test section," the site must be located at least eight
diameters downstream and two diameters upstream from the nearest disturbances.
NOTE: The eight- and two-diameter criteria are not absolute; other test section
locations may be used (subject to approval of the Administrator) , provided that
the flow at the test site is stable and demonstrably parallel to the duct axis.
4.1.2.3 The flow system shall have the capacity to generate a test-section
velocity around 915 m/min (3,000 ft/min). This velocity must be constant with
time to guarantee steady flow during calibration. Note that Type S pitot tube
coefficients obtained by single-velocity calibration at 915 m/min (3,000 ft/min)
will generally be valid to ±3 percent for the measurement of velocities above 305
m/min (1,000 ft/min) and to ±5 to 6 percent for the measurement of velocities
between 180 and 305 m/min (600 and 1,000 ft/min). If a more precise correlation
between Cp and velocity is desired, the flow system shall have the capacity to
generate at least four distinct, time-invariant test-section velocities covering
the velocity range from 180 to 1,525 m/min (600 to 5,000 ft/min), and calibration
data shall be taken at regular velocity intervals over this range (see Citations
9 and 14 in the Bibliography for details).
4.1.2.4 Two entry ports, one each for the standard and Type S pitot tubes, shall
be cut in the test section; the standard pitot entry port shall be located
slightly downstream of the Type S port, so that the standard and Type S impact
openings will lie in the same cross-sectional plane during calibration. To
facilitate alignment of the pitot tubes during calibration, it is advisable that
the test section be constructed of plexiglas or some other transparent material.
4.1.3 Calibration Procedure. Note that this procedure is a general one and must
not be used without first referring to the special considerations presented in
Section 4.1.5. Note also that this procedure applies only to single-velocity
calibration. To obtain calibration data for the A and B sides of the Type S
pitot tube, proceed as follows:
4.1.3.1 Make sure that the manometer is properly filled and that the oil is free
from contamination and is of the proper density. Inspect and leak-check all
pitot lines; repair or replace if necessary.
4.1.3.2 Level and zero the manometer. Turn on the fan, and allow the flow to
stabilize. Seal the Type S entry port.
4.1.3.3 Ensure that the manometer is level and zeroed. Position the standard
pitot tube at the calibration point (determined as outlined in Section 4.1.5.1),
and align the tube so that its tip is pointed directly into the flow. Particular
care should be taken in aligning the tube to avoid yaw and pitch angles. Make
sure that the entry port surrounding the tube is properly sealed.
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EMTIC TM-002
NSPS TEST METHOD
Page 8
4.1.3.4 Read Apstd, and record its value in a data table similar to the one shown
in Figure 2-9. Remove the standard pitot tube from the duct, and disconnect it
from the manometer. Seal the standard entry port.
4.1.3.5 Connect the Type S pitot tube to the manometer. Open the Type S entry
port. Check the manometer level and zero. Insert and align the Type S pitot
tube so that its A side impact opening is at the same point as was the standard
pitot tube and is pointed directly into the flow. Make sure that the entry port
surrounding the tube is properly sealed.
4.1.3.6 Read Aps, and enter its value in the data table. Remove the Type S
pitot tube from the duct, and disconnect it from the manometer.
4.1.3.7 Repeat Steps 4.1.3.3 through 4.1.3.6 above until three pairs of Ap
readings have been obtained.
4.1.3.8 Repeat Steps 4.1.3.3 through 4.1.3.7 above for the B side of the Type
S pitot tube.
4.1.3.9 Perform calculations, as described in Section 4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the six pairs of Ap readings (i.e., three from side A and
three from side B) obtained in Section 4.1.3 above, calculate the value of
the Type S pitot tube coefficient as follows:
r =r
p(s) ^p(std)
\
AP
std
Where:
P(s)
-plstd)
Eg. 2-2
Type S pitot tube coefficient.
Standard pitot tube coefficient; use 0.99 if the
coefficient is unknown and the tube is designed according
to the criteria of Sections 2.7.1 to 2.7.5 of this
method.
ApBtd = Velocity head measured by the standard pitot tube, cm
(in.) H20.
Ap, = Velocity head measured by the Type S pitot tube, cm (in.)
H20.
4.1.4.2 Calculate Cp (side A), the mean A-side coefficient, and Cp (side B), the
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EMTIC TM-002 NSPS TEST METHOD Page 9
mean B-side coefficient; calculate the difference between these two average
values.
4.1.4.3 Calculate the deviation of each of the three A-side values of
Cp(a) from Cp (side A) , and the deviation of each B-side values of Cp(s) from
Cp (side B). Use the following equation:
Deviation = C -C (A or B)
P(s) P
Eq. 2-3
4.1.4.4 Calculate a, the average deviation from the mean, for both the A and B
sides of the pitot tube. Use the following equation:
o(side A or B) =
Eq. 2-4
4.1.4.5 Use the Type S pitot tube only if the values of o (side A) and o (side
B) are less than or equal to 0.01 and if the absolute value of the difference
between Cp (A) and Cp (B) is 0.01 or less.
4.1.5 Special Considerations.
4.1.5.1 Selection of Calibration Point.
4.1.5.1.1 When an isolated Type S pitot tube is calibrated, select a calibration
point at or near the center of the duct, and follow the procedures outlined in
Sections 4.1.3 and 4.1.4 above. The Type S pitot coefficients so obtained,
i.e., Cp (side A) and £ (side B) , will be valid, so long as either: (1) the
isolated pitot tube is used; or (2) the pitot tube is used with other components
(nozzle, thermocouple, sample probe) in an arrangement that is free from
aerodynamic interference effects (see Figures 2-6 through 2-8).
4.1.5.1.2 For Type S pitot tube-thermocouple combinations (without sample
probe), select a calibration point at or near the center of the duct, and follow
the procedures outlined in Sections 4.1.3 and 4.1.4 above. The coefficients so
obtained will be valid so long as the pitot tube-thermocouple combination is used
by itself or with other components in an interference-free arrangement (Figures
2-6 and 2-8).
4.1.5.1.3 For assemblies with sample probes, the calibration point should be
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EMTIC TM-002 NSPS TEST METHOD Page 10
located at or near the center of the duct; however, insertion of a probe sheath
into a small duct may cause significant cross-sectional area blockage and yield
incorrect coefficient values (Citation 9 in the Bibliography). Therefore, to
minimize the blockage effect, the calibration point may be a few inches off-
center if necessary. The actual blockage effect will be negligible when the
theoretical blockage, as determined by a projected-area model of the probe
sheath, is 2 percent or less of the duct cross-sectional area for assemblies
without external sheaths (Figure 2-10a), and 3 percent or less for assemblies
with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pitot tube-nozzle interference is
a factor (i.e., those in which the pitot-nozzle separation distance fails to meet
the specification illustrated in Figure 2-6A) , the value of Cp(s, depends upon the
amount of free-space between the tube and nozzle, and therefore is a function of
nozzle size. In these instances, separate calibrations shall be performed with
each of the commonly used nozzle sizes in place. Note that the single-velocity
calibration technique is acceptable for this purpose, even though the larger
nozzle sizes (>0.635 cm or 1/4 in.) are not ordinarily used for isokinetic
sampling at velocities around 915 m/min (3,000 ft/min), which is the calibration
velocity; note also that it is not necessary to draw an isokinetic sample during
calibration (see Citation 19 in the Bibliography).
4.1.5.3 For a probe assembly constructed such that its pitot tube is always used
in the same orientation, only one side of the pitot tube need be calibrated (the
side which will face the flow) . The pitot tube must still meet the alignment
specifications of Figure 2-2 or 2-3, however, and must have an average deviation
(a) value of 0.01 or less (see Section 4.1.4.4.)
4.1.6 Field Use and Recalibration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type S pitot tube (isolated or in an assembly) is used in the
field, the appropriate coefficient value (whether assigned or obtained by
calibration) shall be used to perform velocity calculations. For calibrated Type
S pitot tubes, the A side coefficient shall be used when the A side of the tube
faces the flow, and the B side coefficient shall be used when the B side faces
the flow; alternatively, the arithmetic average of the A and B side coefficient
values may be used, irrespective of which side faces the flow.
4.1.6.1.2 When a probe assembly is used to sample a small duct, 30.5 to 91.4 cm
(12 to 36 in.) in diameter, the probe sheath sometimes blocks a significant part
of the duct cross-section, causing a reduction in the effective value of Cp(t}.
Consult Citation 9 in the Bibliography for details. Conventional pitot-sampling
probe assemblies are not recommended for use in ducts having inside diameters
smaller than 30.5 cm (12 in.) (see Citation 16 in the Bibliography).
4.1.6.2 Recalibration.
4.1.6.2.1 Isolated Pitot Tubas. After each field use, the pitot tube shall be
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EMTIC TM-002 NSPS TEST METHOD Page 11
carefully reexamined in top, side, and end views. If the pitot face openings are
still aligned within the specifications illustrated in Figure 2-2 or 2-3, it can
be assumed that the baseline coefficient of the pitot tube has not changed. If,
however, the tube has been damaged to the extent that it no longer meets the
specifications of the Figure 2-2 or 2-3, the damage shall either be repaired to
restore proper alignment of the face openings, or the tube shall be discarded.
4.1.6.2.2 Pitot Tube Assemblies. After each field use, check the face opening
alignment of the pitot tube, as in Section 4.1.6.2.1; also, remeasure the
intercomponent spacings of the assembly. If the intercomponent spacings have not
changed and the face opening alignment is acceptable, it can be assumed that the
coefficient of the assembly has not changed. If the face opening alignment is
no longer within the specifications of Figure 2-2 or 2-3, either repair the
damage or replace the pitot tube (calibrating the new assembly, if necessary).
If the intercomponent spacings have changed, restore the original spacings, or
recalibrate the assembly.
4.2 Standard Pitot Tube (if applicable). If a standard pitot tube is used for
the velocity traverse, the tube shall be constructed according to the criteria
of Section 2.7 and shall be assigned a baseline coefficient value of 0.99. If
the standard pitot tube is used as part of an assembly, the tube shall be in an
interference-free arrangement (subject to the approval of the Administrator).
4.3 Temperature Gauges. After each field use, calibrate dial thermometers,
liquid-filled bulb thermometers, thermocouple-potentiometer systems, and other
gauges at a temperature within 10 percent of the average absolute stack
temperature. For temperatures up to 405°C (761°F), use an ASTM mercury-in-glass
reference thermometer, or equivalent, as a reference; alternatively, either
a reference thermocouple and potentiometer (calibrated by NBS) or thermometric
fixed points, e.g., ice bath and boiling water (corrected for barometric
pressure) may be used. For temperatures above 405°C (761°F), use an NBS-
calibrated reference thermocouple-potentiometer system or an alternative
reference, subject to the approval of the Administrator.
If, during calibration, the absolute temperature measured with the gauge being
calibrated and the reference gauge agree within 1.5 percent, the temperature data
taken in the field shall be considered valid. Otherwise, the pollutant emission
test shall either be considered invalid or adjustments (if appropriate) of the
test results shall be made, subject to the approval of the Administrator.
4.4 Barometer. Calibrate the barometer used against a mercury barometer.
5. CALCULATIONS
Carry out calculations, retaining at least one extra decimal figure beyond that
of the acquired data. Round off figures after final calculation.
5.1 Nomenclature.
A = Cross-sectional area of stack, m2 (ft2) .
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EMTIC TM-002
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Page 12
Water vapor in the gas stream (from Method 5 or Reference
Method 4), proportion by volume.
Pitot tube coefficient, dimensionless.
Pitot tube constant,
34.97
m
sec
(g/g-mole)(mmHg)
(mmH20)
1/2
for the metric system.
85.49
ft
sec
Ib/lb-mole) (in.Hgl
(°R) (in.HJD)
1/2
for the English system.
Molecular weight of stack gas, dry basis (see Section 3.6),
g/g—mole (Ib/lb-mole).
Molecular weight of stack gas, wet basis, g/g-mole (Ib/lb-
mole) .
= M(l-B) + 18.0B
PS
Eq. 2-5
Barometric pressure at measurement site, mm Hg (in. Hg)
Stack static pressure, mm Hg (in. Hg).
Absolute stack pressure, mm Hg (in. Hg),
w
bar
t.
Eq. 2-6
Standard absolute pressure, 760 nun Hg (29.92 in. Hg) .
Dry volumetric stack gas flow rate corrected to standard
conditions, dsm3/hr (dscf/hr).
Stack temperature, °C (°F).
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EMTIC TM-002
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Page 13
for metric.
Absolute stack temperature, °K (°R)
= 273 + t
= 460 + t.
Eg. 2-7
for English.
Ap
Eq. 2-8
Standard absolute temperature, 293°K (528°R).
Average stack gas velocity, m/sec (ft/sec).
Velocity head of stack gas, mm H20 (in. H20).
3,600= Conversion factor, sec/hr.
18.0 = Molecular weight of water, g/g-mole (Ib/lb-mole).
5.2 Average Stack Gas Velocity.
vs = KG (\/AP)
p p
avg
s (avg)
Eg. 2-9
5.3 Average Stack Gas Dry Volumetric Flow Rate.
Qsd = 3,600(l-Bws)vsA
"std
T P
s(avg) std
BIBLIOGRAPHY
1. Mark, L.S. Mechanical Engineers' Handbook. New York.
Co., Inc. 1951.
2. Perry. J.H. Chemical Engineers' Handbook. New York.
Eg. 2-10
McGraw-Hill Book
McGraw-Hill Book
-------
EMTIC TM-002 NSPS TEST METHOD Page 14
Co., Inc. 1960.
3. Shigehara, R.T., W.F. Todd, and W.S. Smith. Significance of Errors in
Stack Sampling Measurements. U.S. Environmental Protection Agency,
Research Triangle Park, N.C. (Presented at the Annual Meeting of the Air
Pollution Control Association, St. Louis, MO., June 14-19, 1970).
4. Standard Method for Sampling Stacks for Particulate Matter. In: 1971 Book
of ASTM Standards, Part 23. Philadelphia, PA. 1971. ASTM Designation
D 2928-71.
5. Vennard, J.K. Elementary Fluid Mechanics. New York. John Wiley and Sons,
Inc. 1947.
6. Fluid Meters - Their Theory and Application. American Society of
Mechanical Engineers, New York, N.Y. 1959.
7. ASHRAE Handbook of Fundamentals. 1972. p. 208.
8. Annual Book of ASTM Standards, Part 26. 1974. p. 648.
9. Vollaro, R.F. Guidelines for Type S Pitot Tube Calibration. U.S.
Environmental Protection Agency, Research Triangle Park, N.C. (Presented
at 1st Annual Meeting, Source Evaluation Society, Dayton, OH,
September 18, 1975.)
10. Vollaro, R.F. A Type S Pitot Tube Calibration Study. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park,
N.C. July 1974.
11. Vollaro, R.F. The Effects of Impact Opening Misalignment on the Value of
the Type S Pitot Tube Coefficient. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. October 1976.
12. Vollaro, R.F. Establishment of a Baseline Coefficient Value for Properly
Constructed Type S Pitot Tubes. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. November 1976.
13. Vollaro, R.F. An Evaluation of Single-Velocity Calibration Technique as a
Means of Determining Type S Pitot Tube Coefficients. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park, NC.
August 1975.
14. Vollaro, R.F. The Use of Type S Pitot Tubes for the Measurement of Low
Velocities. U.S. Environmental Protection Agency, Emission Measurement
Branch, Research Triangle Park, NC. November 1976.
15. Smith, Marvin L. Velocity Calibration of EPA Type Source Sampling Probe.
United Technologies Corporation, Pratt and Whitney Aircraft Division, East
Hartford, CT. 1975.
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EMTIC TM-002 NSPS TEST METHOD Page 15
16. Vollaro, R.F. Recommended Procedure for Sample Traverses in Ducts Smaller
than 12 Inches in Diameter. U.S. Environmental Protection Agency, Emission
Measurement Branch, Research Triangle Park, NC. November 1976.
17. Ower, E. and R.C. Pankhurst. The Measurement of Air Flow, 4th Ed. London,
Pergamon Press. 1966.
18. Vollaro, R.F. A Survey of Commercially Available Instrumentation for the
Measurement of Low-Range Gas Velocities. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
November 1976. (Unpublished Paper).
19. Gnyp, A.W., C.C. St. Pierre, D.S. Smith, D. Mozzon, and J. Steiner. An
Experimental Investigation of the Effect of Pitot Tube-Sampling Probe
Configurations on the Magnitude of the S Type Pitot Tube Coefficient for
Commercially Available Source Sampling Probes. Prepared by the University
of Windsor for the Ministry of the Environment, Toronto, Canada.
February 1975.
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EMTIC TM-002
NSPS TEST METHOD
Page 16
1.SO-2.54 em'
(0.75-1.0 in.)
7.62 cm (3 In )•
Tempentur* Senior
/ /
J L
Type S Pilot Tub*
* Suggested (Interference Free)
Prtot tube/ThermocoupIt Spicing
Figure 2-1. Type S pitot tube manometer assembly.
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EMTIC TM-002
NSPS TEST METHOD
Page 17
Traniveree
Tube Axil
Longitudinal
Tub* Axlt
PI
A-Slde Plane
B-Slde Plant
(b)
ll.
(c)
1.0S D,< P < 1.50 D,
PA-
(I) end vtow; (*c* optnlng plan*! perpendicular
to traiuvoree axtt,
(b) top view; lace opening planet penllel to
longitudinal axli.
(c) >lde view: both leg* of equal length end
centerltnei coincident when viewed from
bothaldei. Baaetn* ooefMent valuei ol
O.M mey be aaalgned to pilot tubee oon-
llnicted thh way
Figure 2-2. Properly constructed Type S pi tot tube.
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EMTIC TM-002
NSPS TEST METHOD
Page 18
2=17
•37
Ik'
i_
Figure 2-3. Types of face-opening misalignment that can result from field use
or improper construction of Type S pitot tubes. These will not affect the
baseline value of Cp(s) so long as a1 and a2 slO0, (J1 and 32 *5°, z sO.32 cm (1/8
in.) and w sO.08 cm (1/32 in.) (citation 11 in Bibliography).
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EMTIC TM-002
NSPS TEST METHOD
Page 19
Curv*d or
tared Junction
SUlic
HoUi
(-0.1D) '
Htmtaph.rtc.1 _
Figure 2-4. Standard pitot tube design specifications.
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EMTIC TM-002 HSPS TEST METHOD Page 20
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EMTIC TM-002
NSPS TEST METHOD
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PLANT
DATE
RUN NO. STACK DIA. OR
BAROMETRIC PRESS., mm Hg
DIMENSIONS, m (in.)
(in. Hg) CROSS SECTIONAL AREA, m2 (ft2).
OPERATORS
PITOT TUBE I.D. NO.
AVG. COEFFICIENT, Cp =
LAST DATE CALIBRATED
SCHEMATIC OF STACK
CROSS SECTION
Traverse
Pt. No.
Vel. Hd., Ap
mm ( in . ) H20
Stack Temperature
TS,
°C (°F)
Average
Ts,
°K (°R)
Pg
mm Hg
(in.Hg)
Up)1/2
Figure 2-5. Velocity traverse data.
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EMTIC TM-002
NSPS TEST METHOD
Page 22
| Ot Type S PHal Tube
d_
.D,1J-(XH
Sampling Nozzl*
A Bottom View, chowfng minimum pltot tube-fl«zta eeparation.
State Preeeure
Opening Plan*
Impact Praiaura
Opening Plan*
B Sid* View; to prav*nt ptot tub* from Interfering wttn gai
(low itraamUnat approachng th* noul*. the Impact pruiur*
opening plan* of the pttot tube *hal b* even with or above the
noule entry plan*
Figure 2-6. Proper pi tot tube-sampling nozzle configuration to prevent
aerodynamic interference; button-hook type nozzle; centers of nozzle and
pi tot opening aligned; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 23
T*mp*ntun Svnsor
Ty|)«5P».ITul»
I D, Tyn a nu TUI
SintpK Prt*t
Figure 2-7. Proper thermocouple placement to prevent interference; Dt
between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TBST METHOD
Page 24
Type SPKot Tub*
Sample Probe
Figure 2-8. Minimum pilot-sample probe separation needed lo prevenl
Interference; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 25
PITOT TUBE IDENTIFICATION NUMBER: DATE: CALIBRATED BY:
RUN NO.
1
2
3
RUN NO.
1
2
3
Average De
"A" SIDE CALIBRATION
cm H2O
(in H20)
cm H2O
(in H2O)
c
^*p , avg
(SIDE A)
C,,.,
"B" SIDE CALIBRATION
cm H20
(in H20)
"\7~\ a+~n i^n — rr
cm H2O
(in H20)
c
'-p.avg
(SIDE B)
3
EC - C
p(s) p(AorB)
1 = 1
— ^- MT T
viation a(AorB) ^
Cp(SideA) -Cp(SideB) -MustBe <;0 . 01
Deviation
CP(8) - CP(A)
Deviation
Cp,8, - CP(B)
stBe^O.Ol
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EMTIC TM-002 NSPS TEST METHOD Page 26
Figure 2-9. Pitot tube calibration data.
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EMTIC TM-002
NSPS TEST METHOD
Page 27
Figure 2-10. Projected-area models for typical pitot tube assemblies,
-------
Appendix G.3
EPA Method 3 A
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 3A • Determination of Oxygen and Carbon Dioxide Concentrations
1n Emissions froo Stationary Sources
(Instrumental Analyzer Procedure)
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability. This method 1s applicable to the determination of oxygen (02) and
carbon dioxide (C02) concentrations in emissions from stationary sources only when
specified within the regulations.
1.2 Principle. A sample is continuously extracted from the effluent stream: a
portion of the sample stream is conveyed to an instrumental analyzer(s) for
determination of 02 and CO. concentrations). Performance specifications and test
procedures are provided to ensure reliable data.
2. RANGE AND SENSITIVITY
Same as in Method 6C. Sections 2.1 and 2.2. except that the span of the monitoring
system shall be selected such that the average 02 or C02 concentration is not less than
20 percent of the span.
3. DEFINITIONS
3.1 Measurement System. The total equipment required for the determination of the Oj
or COs concentration. The measurement system consists of the same major subsystems as
defined 1n Method 6C. Sections 3.1.1, 3.1.2. and 3.1.3.
3.2 Span, Calibration Gas. Analyzer Calibration Error. Sampling System Bias. Zero
Drift. Calibration Drift. Response Time, and Calibration Curve. Same as in Method 6C.
Sections 3.2 through 3.8. and 3.10.
3.3 Interference Response. The output response of the measurement system to a
component in the sample gas. other than the gas component being measured.
4. MEASUREMENT SYSTEM PERFORMANCE SPECIFICATIONS
Same as in Method 6C. Sections 4.1 through 4.4.
Prepared by Emission Measurement Branch EMTIC TM-003A
Technical Support Division. OAQPS. EPA May 6. 1989
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EMTIC TM-003A NSPS TEST METHOD Page 2
5. APPARATUS AND REAGENTS
•
5.1 Measurement Systen. Any measurement system for 02 or CQ that meets the
specifications of this method. A schematic of an acceptable measurement system 1s
shown 1n Figure 6C-1 of Method 6C. The essential components of the measurement system
are described below:
5.1.1 Sample Probe. A leak-free probe of sufficient length to traverse the sample
points.
5.1.2 Sample Line. Tubing to transport the sample gas from the probe to the moisture
removal system. A heated sample line is not required for systems that measure the 02
or C02 concentration on a dry basis, or transport dry gases.
5.1.3 Sample Transport Line, Calibration Valve Assembly. Moisture Removal Systen,
Part1culate Filter. Sample Pump. Sample Flow Rate Control. Saaple Gas Manifold, and
Data Recorder. Same as in Method 6C. Sections 5.1.3 through 5.1.9. and 5.1.11. except
that the requirements to use stainless steel. Teflon, and nonreactlve glass filters do
not apply.
5.1.4 Gas Analyzer. An analyzer to determine continuously the Oj or COj concentration
in the sample gas stream. The analyzer must meet the applicable performance
specifications of Section 4. A means of controlling the analyzer flow rate and a
device for determining proper sample flow rate (e.g.. precision rotameter. pressure
gauge downstream of all flow controls, etc.) shall be provided at the analyzer. The
requirements for measuring and controlling the analyzer for measuring and controlling
the analyzer flow rate are not applicable if data are presented that demonstrate the
analyzer is insensitive to flow variations over the range encountered during the test.
5.2 Calibration Gases. The calibration gases for COj analyzers shall be C02 in ^ or
COz in air. Alternatively. COz/SDz. Oz/SOz. or (yoysOj, gas mixtures 1n NZ may be used.
Three calibration gases, as specified in Sections 5.3.1 through 5.3.4 of Method 6C.
shall be used. For 02 monitors that cannot analyze zero gas. a calibration gas
concentration equivalent to less than 10 percent of the span may be used in place of
zero gas.
6. MEASUREMENT SYSTEM PERFORMANCE TEST PROCEDURES
Perform the following procedures before measurement of emissions (Section 7).
6.1 Calibration Concentration Verification. Follow Section 6.1 of Method 6C. except
if calibration gas analysis is required, use Method 3 and change the acceptance
criteria for agreement among Method 3 results to 5 percent (or 0.2 percent by volume.
whichever 1s greater).
6.2 Interference Response. Conduct an Interference response test of the analyzer
prior to its initial use 1n the field. Thereafter, recheck the measurement system 1f
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EMTIC TM-003A NSPS TEST METHOD Page 3
changes are made 1n the instrumentation that could alter the Interference response
(e.g., changes in the type of gas detector). Conduct the interference response 1n
accordance with Section 5.4 of Method 20.
6.3 Measurement System Preparation, Analyzer Calibration Error. Response Time, and
Sampling System Bias Check. Follow Sections 6.2 through 6.4 of Method 6C.
7. EMISSION TEST PROCEDURE
7.1 Selection of Sampling Site and Sampling Points. Select a measurement site and
sampling points using the same criteria that are applicable to tests performed using
Method 3.
7.2 Sample Collection. Position the sampling probe at the first measurement point.
and begin sampling at the same rate as that used during the response time test.
Maintain constant rate sampling (i.e.. ±10 percent) during the entire run. The
sampling time per run shall be the same as for tests conducted using Method 3 plus
twice the average system response time. For each run. use only those measurements
obtained after twice the response time of the measurement system has elapsed to
determine the average effluent concentration.
7.3 Zero and Calibration Drift Test. Follow Section 7.4 of Method 6C.
8. QUALITY CONTROL PROCEDURES
The following quality control procedures are reconmended when the results of this
method are used for an emission rate correction factor, or excess air determination.
The tester should select one of the following options for validating measurement
results:
8.1 If both 02 and CQ are measured using Method 3A. the procedures described in
Section 4.4 of Method 3 should be followed to validate the 02 and CQ measurement
results.
8.2 If only Oj is measured using Method 3A. measurements of the sample stream2CO
concentration should be obtained at the sample by-pass vent discharge using an Orsat
or Fyrite analyzer, or equivalent. Duplicate samples should be obtained concurrent
with at least one run. Average the duplicate Orsat or Fyrite analysis results for
each run. Use the average C02 values for comparison with the20 measurements in
accordance with the procedures described in Section 4.4 of Method 3.
8.3 If only C02 is measured using Method 3A. concurrent measurements of the sample
stream C02 concentration should be obtained using an Orsat or Fyrite analyzer as
described in Section 8.2. For each run. differences greater than 0.5 percent between
the Method 3A results and the average of the duplicate Fyrite analysis should be
Investigated.
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EMTIC TM-003A NSPS TEST METHOD Page 4
9. EMISSION CALCULATION
9.1 For all C02 analyzers, and for Oz analyzers that can be calibrated with zero gas,
follow Section 8 of Method 6C. except express all concentrations as percent, rather
than ppm.
9.2 For Oj analyzers that use a low-level calibration gas 1n place of a zero gas.
calculate the effluent gas concentration using Equation 3A-1.
C.-C,,,
C-, - (C - C.) + C., Eq. 3A-1
c.-c0
Where:
Cgw - Effluent gas concentration, dry basis, percent.
C., - Actual concentration of the upscale calibration gas. percent.
Co, - Actual concentration of the low-level calibration gas. percent.
C. - Average of initial and final system calibration bias check
responses for the upscale calibration gas. percent.
C0 - Average of initial and final system calibration bias check
responses for the low level gas. percent.
U - Average gas concentration indicated by the gas analyzer, dry basis.
percent.
10. BIBLIOGRAPHY
Same as in Bibliography of Method 6C.
-------
Appendix G.4
EPA Method 4
^^-aW^*^^'
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 4 - Determination of Moisture Content
in Stack Gases
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. A gas sample is extracted at a constant rate from
the source; moisture is removed from the sample stream and
determined either volumetrically or gravimetrically.
1.2 Applicability. This method is applicable for determining the
moisture content of stack gas.
1.2.1 Two procedures are given. The first is a reference method,
for accurate determinations of moisture content (such as are needed
to calculate emission data). The second is an approximation
method, which provides estimates of percent moisture to aid in
setting isokinetic sampling rates prior to a pollutant emission
measurement run. The approximation method described herein is only
a suggested approach; alternative means for approximating the
moisture content, e.g., drying tubes, wet bulb-dry bulb techniques,
condensation techniques, stoichiometric calculations, previous
experience, etc., are also acceptable.
1.2.2 The reference method is often conducted simultaneously with
a pollutant emission measurement run; when it is, calculation of
percent isokinetic, pollutant emission rate, etc., for the run
shall be based upon the results of the reference method or its
equivalent; these calculations shall not be based upon the results
of the approximation method, unless the approximation method is
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
shown, to the satisfaction of the Administrator, U.S. Environmental
Protection Agency, to be capable of yielding results within 1
percent H20 of the reference method.
1.2.3 Note: The reference method may yield questionable results
when applied to saturated gas streams or to streams that contain
water droplets. Therefore, when these conditions exist or are
suspected, a second determination of the moisture content shall be
made simultaneously with the reference method, as follows: Assume
that the gas stream is saturated. Attach a temperature sensor
[capable of measuring to within 1°C (2°F)] to the reference method
probe. Measure the stack gas temperature at each traverse point
(see Section 2.2.1) during the reference method traverse; calculate
the average stack gas temperature. Next, determine the moisture
percentage, either by: (1) using a psychrometric chart and making
appropriate corrections if stack pressure is different from that of
the chart, or (2) using saturation vapor pressure tables. In cases
where the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternative methods, subject to the approval of the Administrator,
shall be used.
2. REFERENCE METHOD
The procedure described in Method 5 for determining moisture
content is acceptable as a reference method.
2.1 Apparatus. A schematic of the sampling train used in this
reference method is shown in Figure 4-1. All components shall be
maintained and calibrated according to the procedures in Method 5.
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 3
2.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
to prevent water condensation, and equipped with a filter, either
in-stack (e.g., a plug of glass wool inserted into the end of the
probe) or heated out-stack (e.g., as described in Method 5), to
remove particulate matter. When stack conditions permit, other
metals or plastic tubing may be used for the probe, subject to the
approval of the Administrator.
2.1.2 Condenser. See Method 5, Section 2.1.7, for a description
of an acceptable type of condenser and for alternative measurement
systems.
2.1.3 Cooling System. An ice bath container and crushed ice (or
equivalent), to aid in condensing moisture.
2.1.4 Metering System. Same as in Method 5, Section 2.1.8, except
do not use sampling systems designed for flow rates higher than
0.0283 m3/min (1.0 cfm). Other metering systems, capable of
maintaining a constant sampling rate to within 10 percent and
determining sample gas volume to within 2 percent, may be used,
subject to the approval of the Administrator.
2.1.5 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See
NOTE in Method 5, Section 2.1.9.
2.1.6 Graduated Cylinder and/or Balance. To measure condensed
water and moisture caught in the silica gel to within 1 ml or 0.5
g. Graduated cylinders shall have subdivisions no greater than 2
ml. Most laboratory balances are capable of weighing to the
nearest 0.5 g or less. These balances are suitable for use here.
2.2 Procedure. The following procedure is written for a condenser
system (such as the impinger system described in Section 2.1.7 of
Method 5) incorporating volumetric analysis to measure the
condensed moisture, and silica gel and gravimetric analysis to
measure the moisture leaving the condenser.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 4
2.2.1 Unless otherwise specified by the Administrator, a minimum
of eight traverse points shall be used for circular stacks having
diameters less than 0.61 m (24 in.), a minimum of nine points shall
be used for rectangular stacks
having equivalent diameters less than 0.61 m (24 in.), and a
minimum of twelve traverse points shall be used in all other cases.
The traverse points shall be located according to Method 1. The
use of fewer points is subject to the approval of the
Administrator. Select a suitable probe and probe length such that
all traverse points can be sampled. Consider sampling from
opposite sides
of the stack (four total sampling ports) for large stacks, to
permit use of shorter probe lengths. Mark the probe with heat
resistant tape or by some other method to denote the proper
distance into the stack or duct for each sampling point. Place
known volumes of water in the first two impingers. Weigh and
record the weight of the silica gel to the nearest 0.5 g, and
transfer the silica gel to the fourth impinger; alternatively, the
silica gel may first be transferred to the impinger, and the weight
of the silica gel plus impinger recorded.
2.2.2 Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater
than 0.021 m3/min (0.75 cfm) . When both moisture content and
pollutant emission rate are to be determined, the moisture
determination shall be simultaneous with, and for the same total
length of time as, the pollutant emission rate run, unless
otherwise specified in an applicable subpart of the standards.
2.2.3 Set up the sampling train as shown in Figure 4-1. Turn on
the probe heater and (if applicable) the filter heating system to
temperatures of about 120°C (248°F), to prevent water condensation
ahead of the condenser; allow time for the temperatures to
stabilize. Place crushed ice in the ice bath container. It is
recommended, but not required, that a leak check be done, as
follows: Disconnect the probe from the first impinger or (if
applicable) from the filter holder. Plug the inlet to the first
impinger (or filter holder), and pull a 380 mm (15 in.) Hg vacuum;
a lower vacuum may be used, provided that it is not exceeded during
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 5
the test. A leakage rate in excess of 4 percent of the average
sampling rate or 0.00057 m3/min (0.02 cfm), whichever is less, is
unacceptable. Following the leak check, reconnect the probe to the
sampling train.
2.2.4 During the sampling run, maintain a sampling rate within 10
percent of constant rate, or as specified by the Administrator.
For each run, record the data required on the example data sheet
shown in Figure 4-2. Be sure to record the dry gas meter reading
at the beginning and end of each sampling time increment and
whenever sampling is halted. Take other appropriate readings at
each sample point, at least once during each time increment.
2.2.5 To begin sampling, position the probe tip at the first
traverse point. Immediately start the pump, and adjust the flow to
the desired rate. Traverse the cross section, sampling at each
traverse point for an equal length of time. Add more ice and, if
necessary, salt to maintain a temperature of less than 20°C (68°F)
at the silica gel outlet.
2.2.6 After collecting the sample, disconnect the probe from the
filter holder (or from the first impinger) , and conduct a leak
check (mandatory) as described in Section 2.2.3. Record the leak
rate. If the leakage rate exceeds the allowable rate, the tester
shall either reject the test results or shall correct the sample
volume as in Section 6.3 of Method 5. Next, measure the volume of
the moisture condensed to the nearest ml. Determine the increase
in weight of the silica gel (or silica gel plus impinger) to the
nearest 0.5 g. Record this information (see example data sheet.
Figure 4-3), and calculate the moisture percentage, as described in
2.3 below.
2.2.7 A quality control check of the volume metering system at the
field site is suggested before collecting the sample following the
procedure in Method 5, Section 4.4.
2.3 Calculations. Carry out the following calculations, retaining
at least one extra decimal figure beyond that of the acquired data.
Round off figures after final calculation.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 6
2.3.1 Nomenclature.
Bws = Proportion of water vapor, by volume, in the gas stream.
Mw = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg) .
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 (mm Hg) (m3) / (g-mole) (°K) for
metric units and 21.85 (in. Hg) (ft3) / (Ib-mole) (°R) for
English units.
Tm = Absolute temperature at meter, °K (°R) .
Tstd = Standard absolute temperature, 293°K (528°R) .
Vm = Dry gas volume measured by dry gas meter, dcm (dcf).
AVm = Incremental dry gas volume measured by dry gas meter at
each traverse point, dcm (dcf).
Vm(std) = DrY 9as volume measured by the dry gas meter, corrected to
standard conditions, dscm (dscf).
= Volume of water vapor condensed, corrected to standard
conditions, scm (scf).
= Volume of water vapor collected in silica gel, corrected
to standard conditions, scm (scf).
Vf = Final volume of condenser water, ml.
Vi = Initial volume, if any, of condenser water, ml.
Wf = Final weight of silica gel or silica gel plus impinger, g.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 7
WA = Initial weight of silica gel or silica gel plus impinger,
g-
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml).
2.3.2 Volume of Water Vapor Condensed.
RT
V = (V ~V,)p std
f i w p M Ea. 4-1
std w ^
=K (V -V )
1 f i
Where :
Kx = 0.001333 m3/ml for metric units,
= 0.04707 ft3/ml for English units.
2.3.3 Volume of Water Collected in Silica Gel.
_ (Wf - W±) RTstd
v
wsg(std)
std w
(Wf - W±)
Where:
K2 = 0.001335 m3/g for metric units,
= 0.04715 ft3/g for English units,
2.3.4 Sample Gas Volume.
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 8
(P J (T )
V _ = V Y m 8td
m(std) m / p \ I rn \
V8tdp m Eq. 4-3
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 9
Where:
K3 = 0.3858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units,
NOTE: If the post-test leak rate (Section 2.2.6) exceeds the
allowable rate, correct the value of Vra in Equation 4-3, as
described in Section 6.3 of Method 5.
2.3.5 Moisture Content.
wc(std) wsg(std) Eq . 4-4
ws V +V +V
wc(std) wsg(std) m(std)
NOTE: In saturated or moisture droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be
made, one using a value based upon the saturated conditions (see
Section 1.2), and another based upon the results of the impinger
analysis. The lower of these two values of Bws shall be considered
correct.
2.3.6 Verification of Constant Sampling Rate. For each time
increment, determine the AVm. Calculate the average. If the value
for any time increment differs from the average by more than 10
percent, reject the results, and repeat the run.
3. APPROXIMATION METHOD
The approximation method described below is presented only as a
suggested method (see Section 1.2).
3.1 Apparatus. See Figure 4-4.
3.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 10
to prevent water condensation and equipped with a filter (either
in-stack or heated out-stack) to remove particulate matter. A plug
of glass wool, inserted into the end of the probe, is a
satisfactory filter.
3.1.2 Impingers. Two midget impingers, each with 30-ml capacity,
or equivalent.
3.1.3 Ice Bath. Container and ice, to aid in condensing moisture
in impingers.
3.1.4 Drying Tube. Tube packed with new or regenerated 6- to 16-
mesh indicating-type silica gel (or equivalent desiccant), to dry
the sample gas and to protect the meter and pump.
3.1.5 Valve. Needle valve, to regulate the sample gas flow rate.
3.1.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
3.1.7 Volume Meter. Dry gas meter, sufficiently accurate to
measure the sample volume to within 2 percent, and calibrated over
the range of flow rates and conditions actually encountered during
sampling.
3.1.8 Rate Meter. Rotameter, to measure the flow range from 0 to
3 liters/min (0 to 0.11 cfm).
3.1.9 Graduated Cylinder. 25-ml.
3.1.10 Barometer. Mercury, aneroid, or other barometer, as
described in Section 2.1.5 above.
3.1.11 Vacuum Gauge. At least 760-mm (30-in.) Hg gauge, to be
used for the sampling leak check.
3.2 Procedure.
3.2.1 Place exactly 5 ml water in each impinger. Leak check the
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 11
sampling train as follows: Temporarily insert a vacuum gauge at or
near the probe inlet; then, plug the probe inlet, and pull a vacuum
of at least 250 mm (10 in.) Hg. Note the time rate of change of
the dry gas meter dial; alternatively, a rotameter (0 to 40 cc/min)
may be temporarily attached to the dry gas meter outlet to
determine the leakage rate. A leak rate not in excess of 2 percent
of the average sampling rate is acceptable. NOTE: Carefully
release the probe inlet plug before turning off the pump.
3.2.2 Connect the probe, insert it into the stack, and sample at
a constant rate of 2 liters/min (0.071 cfm) . Continue sampling
until the dry gas meter registers about 30 liters (1.1 ft3) or
until visible liquid droplets are carried over from the first
impinger to the second. Record temperature, pressure, and dry gas
meter readings as required by Figure 4-5.
3.2.3 After collecting the sample, combine the contents of the two
impingers, and measure the volume to the nearest 0.5 ml.
3.3 Calculations. The calculation method presented is designed to
estimate the moisture in the stack gas; therefore, other data,
which are only necessary for accurate moisture determinations, are
not collected. The following equations adequately estimate the
moisture content, for the purpose of determining isokinetic
sampling rate settings.
3.3.1 Nomenclature.
B^ = Approximate proportion by volume of water vapor in the gas
stream leaving the second impinger, 0.025.
Bws = Water vapor in the gas stream, proportion by volume.
M« = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 12
Pscd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 [(mm Hg) (m3) ] / [ (g-mole) (°K) ]
for metric units and 21.85 [(in. Hg) (ft3) ] / [ (Ib-mole) (°R)]
for English units.
Tm = Absolute temperature at meter, °K (°R) .
Tstd = Standard absolute temperature, 293 °R (528°R) .
Vf = Final volume of impinger contents, ml.
Vi = Initial volume of impinger contents, ml.
Vm = Dry gas volume measured by dry gas meter, dcm (dcf) .
Vm(std) = Dry gas volume measured by dry gas meter, corrected to
standard conditions, dscm (dscf) .
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml) .
3.3.2 Volume of Water Vapor Collected.
w,
PstdMw Eq. 4-5
Where :
K! = 0.001333 m3/ml for metric units,
= 0.04707 ft3/ml for English units
3.3.3 Gas Volume .
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EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 13
Where:
v
m(std)
= V
std,
'std
Eq. 4-6
= K. Vm —
2 ffi T
K2 = 0.03858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units.
3.3.4 Approximate Moisture Content.
V
B
+ B
V +V wm
we m(std)
V
Eq. 4-7
V +V
we m(std)
•+(0.025)
4. CALIBRATION
4.1 For the reference method, calibrate the metering system,
temperature gauges, and barometer according to Sections 5.3, 5.5,
and 5.7, respectively, of Method 5. The recommended leak check of
the metering system (Section 5.6 of Method 5) also applies to the
reference method. For the approximation method, use the procedures
outlined in Section 5.1.1 of Method 6 to calibrate the metering
system, and the procedure of Method 5, Section 5.7, to calibrate
the barometer.
5. BIBLIOGRAPHY
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 14
1. Air Pollution Engineering Manual (Second Edition). Danielson,
J.A. (ed.). U.S. Environmental Protection Agency, Office of Air
Quality Planning and Standards. Research Triangle Park, NC.
Publication No. AP-40. 1973.
2. Devorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District, Los Angeles, CA. November 1963.
3. Methods for Determination of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
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EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 15
Cond«n««r.|c« 8«th Syltam Including SUIct Oil Tub*
method.
Figure 4-1. Moisture sampling train reference
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 16
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Figure 4-2. Field Moisture Determination Reference Method.
Plant
Location.
Operator.
Date
Run No.
Ambient temperature.
Barometric pressure.
Probe Length
SCHEMATIC OF STACK CROSS SECTION
Traverse
Pt. No.
Sampling
Time
(6) , min
Stack
Temperature
°C (°F)
Average
Pressure
differential across
orifice meter AH
mm (in. ) H20
Meter
Reading gas
sample
volume
m3 (ft3)
&vm
m3
(ft3)
Gas sample
temperature at
dry gas meter
Inlet
Tmin
°C(°F)
Outlet
TRW
°C(°F)
Temperature
of gas
leaving
condenser or
last
impinger
°C(°F)
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 18
Figure 4-3. Analytical data - reference method.
Impinger Silica gel
volume. ml weight, a
Final
Initial
Difference
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EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 19
L
Figure 4-4. Moisture Samping Train - Approximation Method,
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EMTIC TM-004
EMTIC NSPS TEST METHOD
Page 20
Figure 4-5. Field Moisture Determination - Approximation Method.
Location.
Test
Date
Operator
Barometric pressure.
Comments:
Clock Time
Gas volume
through
meter, (VJ ,
m3 (ft3)
Rate meter
setting mYmin
(ftVmin)
Meter
temperature
" C (° F)
-------
Appendix G.5
EPA Method 23
-------
6560-50
ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 60
[AD-FRL- ]
STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES
Appendix A , Test Method 23
AGENCY: Environmental Protection Agency (EPA).
ACTION: Proposed Rule.
SUMMARY: This rule amends Method 23, entitled
"Determination of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans from Stationary Sources," to
correct existing errors in the method, to eliminate the methylene
chloride rinse of the sampling train, and to clarify the quality
assurance requirements of the method.
DATES: Comments. Comments must be received on or before
(90 days after publication in the FEDERAL
REGISTER].
Public Hearing. If anyone contacts EPA requesting to speak
at a public hearing by (two weeks after
publication in the FEDERAL REGISTER), a public hearing will be
held on (four weeks after publication in the
FEDERAL REGISTER), beginning at 10:00 a.m. Persons interested in
attending the hearing should call Ms. Lala Cheek at
(919) 541-5545 to verify that a hearing will be held.
Request to Speak at Hearing. Persons wishing to present
-------
oral testimony must contact EPA by (two weeks
after publication in the FEDERAL REGISTER).
ADDRESSES: Comments. Comments should be submitted (in duplicate
if possible) to Public Docket No. A-94-2 at the following
address: U. S. Environmental Protection Agency , Air and
Radiation Docket and Information Center, Mail Code: 6102, 401 M
Street, SW, Washington, DC 20460. The Agency requests that a
separate copy also be sent to the contact person listed below.
The docket is located at the above address in Room M-1500
Waterside Mall (ground floor), and may be inspected from
8:30 a.m. to Noon and 1:00 to 3:00 PM, Monday through Friday.
The proposed regulatory text and other materials related to this
rulemaking are available for review in the docket or copies may
be mailed on request from the Air Docket by calling 202-260-7548.
A reasonable fee may be charged for copying docket materials.
Public Hearing. If anyone contacts EPA requesting a public
hearing, it will be held at EPA's Emission Measurement
Laboratory, Research Triangle Park, North Carolina. Persons
interested in attending the hearing or wishing to present oral
testimony should notify Ms. Lala Cheek (MD-19), U.S.
Environmental Protection Agency, Research Triangle Park, North
Carolina 27711, telephone number (919) 541-5545.
-------
Docket: A Docket, A-94-22, containing materials relevant to
this rulemaking, is available for public inspection and copying
between 8:30 a.m. and Noon and 1:00 and 3:00 p.m., Monday through
Friday, in at EPA's Air Docket Section (LE-131), Room M-1500
Waterside Mall (ground floor) 401 M Street, S.W., Washington,
D.C. 20460. A reasonable fee may be charged for copying.
FOR FURTHER INFORMATION CONTACT: Gary McAlister, Emission
Measurement Branch (MD-19), Emissions, Monitoring, and Analysis
Division, U.S. Environmental Protection Agency, Research Triangle
Park, North Carolina 27711, telephone (919) 541-1062.
SUPPLEMENTARY INFORMATION:
The proposed regulatory text of the proposed rule is not
included in this Federal Register notice, but is available in
Docket No. A-94-22 or by written or telephone request from the
Air Docket (see ADDRESSES). If necessary, a limited number of
copies of the Regulatory Text are available from the EPA contact
persons designated earlier in this notice. This Notice with the
proposed regulatory language is also available on the Technology
Transfer Network (TTN), one of EPA's electronic bulletin boards.
TTN provides information and technology exchange in various areas
of air pollution control. The service is free except for the
cost of the phone call. Dial (919) 541-5742 for up to a 14400
-------
bps modem. If more information on TTN is needed, call the HELP
line at (919) 541-5384.
I. SUMMARY
Method 23 was promulgated along with the New Source
Performance Standard for municipal waste combustors (Subpart Ea).
As promulgated, the method contained some errors. This action
would correct those errors and would clarify some of the existing
quality assurance requirements. In addition, the current
procedure requires rinsing of the sampling train with two
separate solvents which must be analyzed separately. Based on
data the Agency has collected since promulgation of Method 23, we
believe that one of these rinse steps and the resulting sample
fraction can be eliminated. This could save as much as $2000 per
test run in analytical costs.
II. THE RULEMAKING
This rulemaking does not impose emission measurement
requirements beyond those specified in the current regulations
nor does it change any emission standard. Rather, the rulemaking
would simply amend an existing test method associated with
emission measurement requirements in the current regulations that
would apply irrespective of this rulemaking.
III. ADMINISTRATIVE REQUIREMENTS
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A. Public Hearing
A public hearing will be held, if requested, to discuss the
proposed amendment in accordance with section 307(d)(5)of the
Clean Air Act. Persons wishing to make oral presentations should
contact EPA at the address given in the ADDRESSES section of this
preamble. Oral presentations will be limited to 15 minutes each.
Any member of the public may file a written statement with EPA
before, during, or within 30 days after the hearing. Written
statements should be addressed to the Air Docket Section address
given in the ADDRESSES section of this preamble.
A verbatim transcript of the hearing and written statements
will be available for public inspection and copying during normal
working hours at EPA's Air Docket Section in Washington, DC (see
ADDRESSES section of this preamble).
B. Docket
The docket is an organized and complete file of all the
information considered by EPA in the development of this
rulemaking. The docket is a dynamic file, since material is
added throughout the rulemaking development. The docketing
system is intended to allow members of the public and industries
involved to identify and locate documents readily so that they
may effectively participate in the rulemaking process. Along
-------
with the statement of basis and purpose of the proposed and
promulgated test method revisions and EPA responses to
significant comments, the contents of the docket, except for
interagency review materials, will serve as the record in case of
judicial review [Section 307(d)(7)(A)].
C. Executive Order 12291 Review
Under Executive Order 12291, EPA is required to judge
whether a regulation is a "major rule" and, therefore, subject to
the requirements of a regulatory impact analysis. This
rulemaking does not impose emission measurement requirements
beyond those specified in the current regulations, nor does it
change any emission standard. The Agency has determined that
this regulation would result in none of the adverse economic
effects set forth in Section 1 of the Order as grounds for
finding the regulation to be a "major rule." The Agency has,
therefore, concluded that this regulation is not a "major rule"
under Executive Order 12291.
D. Regulatory Flexibility Act
The Regulatory Flexibility Act (RFA) of 1980 requires the
identification of potentially adverse impacts of Federal
regulations upon small business entities. The RFA specifically
requires the completion of an analysis in those instances where
-------
small business impacts are possible. This rulemaking does not
impose emission measurement requirements beyond those specified
in the current regulations, nor does it change any emission
standard. Because this rulemaking imposes no adverse economic
impacts, an analysis has not been conducted.
Pursuant to the provision of 5 U.S.C. 605(b), I hereby
certify that the promulgated rule will not have an impact on
small entities because no additional costs will be incurred.
E. Paperwork Reduction Act
This rule does not change any information collection
requirements subject to Office of Management and Budget review
under the Paperwork Reduction Act of 1980, 44 U.S.C. 3501 et seq.
F. Statutory Authority
The statutory authority for this proposal is provided by
sections 111 and 301 (a) of the Clean Air Act, as amended: 42
U.S.C., 7411 and 7601(a).
LIST OF SUBJECTS
Air pollution control, municipal waste combustors,
polychorinated dibenzo-p-dioxins, sources.
-------
Date The Administrator
It is proposed that 40 CFR Part 60 be amended as follows:
1. The authority citation for Part 60 continues to read as
follows: Authority: Clean Air Act (42 U.S.C. 7401 [et seq.], as
amended by Pub. L 101-549).
2. Replace test Method 23 of Appendix A, with the
following:
Method 23 - Determination of Polychlorinated Dibenzo-p-dioxins
and Polychlorinated Dibenzofurans from Municipal Waste Combustors
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability. This method is applicable to the
determination of emissions of polychlorinated dibenzo-p-dioxins
(PCDD's) and polychlorinated dibenzofurans (PCDF's) from
municipal waste combustors. Calibration standards are selected
for regulated emission levels for municipal waste combustors.
1.2 Principle. A sample is withdrawn isokinetically from the
gas stream and collected in the sample probe, on a glass fiber
filter, and on a packed column of adsorbent material. The sample
cannot be separated into a particle and vapor fraction. The
PCDD's and PCDF's are extracted from the sample, separated by
high resolution gas chromatography (HRGC), and measured by high
8
-------
resolution mass spectrometry (HRMS).
2. APPARATUS
2.1 Sampling. A schematic of the sampling train is shown in
Figure 23-1. Sealing greases shall not be used in assembling the
train. The train is identical to that described in Section 2.1
of Method 5 of this appendix with the following additions:
-------
Oil Flow
alack wall
tamparatura
aanaor
! haatad glail llnar
I * ,
1
haat
u
d
>
,
pilot
manometer
t
tamparatura
aanaor
B»i txlt
Figure 23.1 Sampling Train
10
-------
11
-------
2.1.1 Nozzle. The nozzle shall be made of nickel, nickel-
plated stainless steel, quartz, or borosilicate glass.
2.1.2 Sample Transfer Lines. The sample transfer lines, if
needed, shall be heat traced, heavy walled TFE (1/2 in. OD with
1/8 in. wall) with connecting fittings that are capable of
forming leak-free, vacuum-tight connections without using sealing
greases. The line shall be as short as possible and must be
maintained at >I20°C.
2.1.1 Filter Support. Teflon or Teflon-coated wire.
2.1.2 Condenser. Glass, coil type with compatible fittings.
A schematic diagram is shown in Figure 23-2.
2.1.3 Water Bath. Thermostatically controlled to maintain the
gas temperature exiting the condenser at <.20°C (68°F) .
2.1.4 Adsorbent Module. Glass container to hold up to 40
grams of resin adsorbent. A schematic diagram is shown in Figure
23-2. Other physical configurations of the water-jacketed resin
trap/condenser assembly are acceptable. The connecting fittings
shall form leak-free, vacuum tight seals. A coarse glass frit is
included to retain the adsorbent in the water-jacketed sorbent
module.
2.1.5 Probe Liner. The probe liner shall be made of glass and
a Teflon ferrule or Teflon coated 0-ring shall be used to make
the seal at the nozzle end of the probe.
12
-------
2.2 Sample Recovery.
2.2.1 Fitting Caps. Ground glass, Teflon tape, or aluminum
foil (Section 2.2.6) to cap off the sample exposed sections of
the train and sorbent module.
2.2.2 Wash Bottles. Teflon, 500-mL.
13
-------
Flue
Gas
Flow
Sorbent Trap
f 20/15
Glut Sintered Disk
XAD-2
Water Jacket
Glass Wool Plug
Condenser
Cooling Coil
Water Jacket
20/15
Figure 23.2 Condenser and Adsorbent Trap
14
-------
15
-------
2.2.3 Probe Liner, Probe Nozzle, and Filter Holder Brushes.
Inert bristle brushes with precleaned stainless steel or Teflon
handles. The probe brush shall have extensions of stainless
steel or Teflon, at least as long as the probe. The brushes
shall be properly sized and shaped to brush out the nozzle, probe
liner, and transfer line, if used.
2.2.4 Filter Storage Container. Sealed filter holder, wide-
mouth amber glass jar with Teflon-lined cap, glass petri dish, or
Teflon baggie.
2.2.5 Balance. Triple beam.
2.2.6 Aluminum Foil. Heavy duty, hexane-rinsed (Do not use to
wrap or ship filter samples, because it may react with
particulate matter).
2.2.7 Metal Storage Container. Air tight container to store
silica gel.
2.2.8 Graduated Cylinder. Glass, 250-mL with 2-mL
graduations.
2.2.9 Glass Sample Storage Containers. Amber glass bottles
for sample glassware washes, 500- or 1000-mL, with leak free
Teflon-lined caps.
2.3 Analysis.
2.3.1 Sample Containers. 125- and 250-mL flint glass bottles
with Teflon-lined caps.
16
-------
2.3.2 Test Tubes. Glass.
2.3.3 Soxhlet Extraction Apparatus. Capable of holding 43 x
123 mm extraction thimbles.
2.3.4 Extraction Thimble. Glass, precleaned cellulosic, or
glass fiber.
2.3.5 Pasteur Pipettes. For preparing liquid chromatographic
columns.
2.3.6 Reacti-vials. Amber glass, 2-mL.
2.3.7 Rotary Evaporator. Buchi/Brinkman RF-121 or equivalent.
2.3.8 Kuderna-Danish Concentrator Apparatus.
2.3.9 Nitrogen Evaporative Concentrator. N-Evap Analytical
Evaporator Model III or equivalent.
2.3.10 Separatory Funnels. Glass, 2-liter.
2.3.11 Gas Chromatograph. Consisting of the following
components:
2.3.11.1 Oven. Capable of maintaining the separation column
at the proper operating temperature ±10°C and performing
programmed increases in temperature at rates of at least
40°C/min.
2.3.11.2 Temperature Gauges. To monitor column oven,
detector, and exhaust temperatures ±1°C.
2.3.11.3 Flow Systems. Gas metering system to measure sample,
fuel, combustion gas, and carrier gas flows.
17
-------
2.3.11.4 Capillary Columns. A fused silica column,
60 x 0.25 mm inside diameter (ID), coated with DB-5 and a fused
silica column, 30 m x 0.25 mm ID coated with DB-225. Other
column systems may be substituted provided that the user is able
to demonstrate, using calibration and performance checks, that
the column system is able to meet the specifications of Section
6.1.2.2.
2.3.12 Mass Spectrometer. Capable of routine operation at a
resolution of 1:10000 with a stability of ±5 ppm.
2.3.13 Data System. Compatible with the mass spectrometer and
capable of monitoring at least five groups of 25 ions.
2.3.14 Analytical Balance. To measure within 0.1 mg.
3. REAGENTS
3.1 Sampling.
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent
penetration) on 0.3-micron dioctyl phthalate smoke particles.
The filter efficiency test shall be conducted in accordance with
ASTM Standard Method D 2986-71 (Reapproved 1978) (incorporated by
reference - see §60.17).
3.1.1.1 Precleaning. All filters shall be cleaned before
their initial use. Place a glass extraction thimble and 1 g of
silica gel and a plug of glass wool into a Soxhlet apparatus,
18
-------
charge the apparatus with toluene, and reflux for a minimum of 3
hours. Remove the toluene and discard it, but retain the silica
gel. Place no more than 50 filters in the thimble onto the
silica gel bed and top with the cleaned glass wool. Charge the
Soxhlet with toluene and reflux for 16 hours. After extraction,
allow the Soxhlet to cool, remove the filters, and dry them under
a clean nitrogen (N2) stream. Store the filters in a glass petri
dishes and seal with Teflon tape.
3.1.2 Adsorbent Resin. Amberlite XAD-2 resin. Thoroughly
cleaned before initial use. Do not reuse resin. If precleaned
XAD-2 resin is purchased from the manufacturer, the cleaning
procedure described in Section 3.1.2.1 is not required.
3.1.2.1 Cleaning. Procedure may be carried out in a giant
Soxhlet extractor. An all-glass filter thimble containing an
extra-coarse frit is used for extraction of XAD-2. The frit is
recessed 10-15 mm above a crenelated ring at the bottom of the
thimble to facilitate drainage. The resin must be carefully
retained in the extractor cup with a glass wool plug and a
stainless steel ring because it floats on methylene chloride.
This process involves sequential extraction in the following
order.
Solvent Procedure
Water Initial Rinse: Place resin in a beaker,
19
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rinse once with HPLC water, and discard
water. Refill beaker with water, let
stand overnight, and discard water.
Water Extract with HPLC water for 8 hours.
Methanol Extract with methanol for 22 hours.
Methylene Chloride Extract with methylene chloride for 22
hours.
Methylene Chloride Extract with methylene chloride for 22
hours.
3.1.2.2 Drying.
3.1.2.2.1 Drying Column. Pyrex pipe, 10.2 cm ID by 0.6 m
long, with suitable retainers.
3.1.2.2.2 Procedure. The adsorbent must be dried with clean
inert gas. Liquid nitrogen from a standard commercial liquid
nitrogen cylinder has proven to be a reliable source for large
volumes of gas free from organic contaminants. Connect the
liquid nitrogen cylinder to the column by a length of cleaned
copper tubing, 0.95 cm ID, coiled to pass through a heat source.
A convenient heat source is a water-bath heated from a steam
line. The final nitrogen temperature should only be warm to the
touch and not over 40°C. Continue flowing nitrogen through the
adsorbent until all the residual solvent is removed. The flow
rate should be sufficient to gently agitate the particles, but
20
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not so excessive as to cause the particles to fracture.
3.1.2.3 Quality Control Check. The adsorbent must be checked
for residual methylene chloride (MeCl2) as well as PCDDs and
PCDFs prior to use. The analyst may opt to omit this check for
precleaned XAD-2.
3.1.2.3.1 MeClj Residue Extraction. Weigh a 1.0 g sample of
dried resin into a small vial, add 3 mL of toluene, cap the vial,
and shake it well.
3.1.2.3.2 MeCl2 Residue Analysis. Inject a 2 /xl sample of the
extract into a gas chromatograph operated under the following
conditions:
Column: 6 ft x 1/8 in stainless steel containing 10 percent
OV-101™ on 100/120 Supelcoport.
Carrier Gas: Helium at a rate of 30 mL/min.
Detector: Flame ionization detector operated at a sensitivity
of 4 x 10-11 A/mV.
Injection Port Temperature: 250°C.
Detector Temperature: 305°C.
Oven Temperature: 30°C for 4 min; programmed to rise at
40°C/min until it reaches 250°C; return to 30°C after 17
minutes.
Compare the results of the analysis to the results from the
reference solution. Prepare the reference solution by injecting
21
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4.0 jil of methylene chloride into 100 mL of toluene. This
corresponds to 100 fig of methylene chloride per g of adsorbent.
The maximum acceptable concentration is 1000 /xg/g of adsorbent.
If the adsorbent exceeds this level, drying must be continued
until the excess methylene chloride is removed.
3.1.2.3.3 PCDD and PCDF Check. Extract the adsorbent sample
as described in Section 5.1. Analyze the extract as described in
Section 5.3. If any of the PCDDs or PCDFs (tetra through hexa)
are present at concentrations above the target detection limits
(TDLs), the adsorbent must be recleaned by repeating the last
step of the cleaning procedure. The TDLs for the various
PCDD/PCDF congeners are listed in Table 1.
3.1.2.4 Storage. After cleaning, the adsorbent may be stored
in a wide mouth amber glass container with a Teflon-lined cap or
placed in glass adsorbent modules tightly sealed with glass
stoppers. It must be used within 4 weeks of cleaning. If
precleaned adsorbent is purchased in sealed containers, it must
be used within 4 weeks after the seal is broken.
3.1.3 Glass Wool. Cleaned by sequential immersion in three
aliquots of methylene chloride, dried in a 110°C oven, and stored
in a methylene chloride-washed glass container with a Teflon-
lined screw cap.
3.1.4 Water. Deionized distilled and stored in a methylene
22
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chloride-rinsed glass container with a Teflon-lined screw cap.
3.1.5 Silica Gel. Indicating type, 6 to 16 mesh. If
previously used, dry at 175° C (350°F) for two hours. New silica
gel may be used as received. Alternatively, other types of
desiccants (equivalent or better) may be used, subject to the
approval of the Administrator.
3.1.6 Chromic Acid Cleaning Solution. Dissolve 20 g of sodium
dichromate in 15 mL of water, and then carefully add 400 mL of
concentrated sulfuric acid.
3.1.7 HPLC Water.
3.2 Sample Recovery.
3.2.1 Acetone. Pesticide quality.
3.2.2 Toluene. Pesticide quality.
3.3 Analysis.
3.3.1 Potassium Hydroxide. ACS grade, 2-percent
(weight/volume) in water.
3.3.2 Sodium Sulfate. Granulated, reagent grade. Purify
prior to use by rinsing with methylene chloride and oven drying.
Store the cleaned material in a glass container with a Teflon-
lined screw cap.
3.3.3 Sulfuric Acid. Reagent grade.
3.3.4 Sodium Hydroxide. 1.0 N. Weigh 40 g of sodium hydroxide
into a 1-liter volumetric flask. Dilute to 1 liter with water.
23
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3.3.5 Hexane. Pesticide grade.
3.3.6 Methylene Chloride. Pesticide grade.
3.3.7 Benzene. Pesticide grade.
3.3.8 Ethyl Acetate.
3.3.9 Methanol. Pesticide grade.
3.3.10 Toluene. Pesticide grade.
3.3.11 Nonane. Pesticide grade.
3.3.12 Cyclohexane. Pesticide Grade.
3.3.13 Basic Alumina. Activity grade 1, 100-200 mesh. Prior
to use, activate the alumina by heating for 16 hours at 130°C.
Store in a desiccator. Pre-activated alumina may be purchased
from a supplier and may be used as received.
3.3.14 Silica Gel. Bio-Sil A, 100-200 mesh. Prior to use,
activate the silica gel by heating for at least 30 minutes at
180°C. After cooling, rinse the silica gel sequentially with
methanol and methylene chloride. Heat the rinsed silica gel at
50°C for 10 minutes, then increase the temperature gradually to
180°C over 25 minutes and maintain it at.this temperature for
90 minutes. Cool at room temperature and store in a glass
container with a Teflon-lined screw cap.
3.3.15 Silica Gel Impregnated with Sulfuric Acid. Combine 100
g of silica gel with 44 g of concentrated sulfuric acid in a
screw capped glass bottle and agitate thoroughly. Disperse the
24
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solids with a stirring rod until a uniform mixture is obtained.
Store the mixture in a glass container with a Teflon-lined screw
cap.
3.3.16 Silica Gel Impregnated with Sodium Hydroxide. Combine
39 g of 1 N sodium hydroxide with 100 g of silica gel in a screw
capped glass bottle and agitate thoroughly. Disperse solids with
a stirring rod until a uniform mixture is obtained. Store the
mixture in glass container with a Teflon-lined screw cap.
3.3.17 Carbon/Celite. Combine 10.7 g of AX-21 carbon with 124
g of Celite 545 in a 250-mL glass bottle with a Teflon-lined
screw cap. Agitate the mixture thoroughly until a uniform
mixture is obtained. Store in the glass container.
3.3.18 Nitrogen. Ultra high purity.
3.3.19 Hydrogen. Ultra high purity.
3.3.20 Internal Standard Solution. Prepare a stock standard
solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Internal Standards" in 10 mL of nonane.
3.3.21 Surrogate Standard Solution. Prepare a stock standard
solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Surrogate Standards" in 10 mL of nonane.
3.3.22 Recovery Standard Solution. Prepare a stock standard
25
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solution containing the isotopically labelled PCDD's and PCDF's
at the concentrations shown in Table 2 under the heading
"Recovery Standards" in 10 mL of nonane.
4. PROCEDURE
4.1 Sampling. The complexity of this method is such that, in
order to obtain reliable results, testers and analysts should be
trained and experienced with the procedures.
4.1.1 Pretest Preparation.
4.1.1.1 Cleaning Glassware. All glass components of the train
upstream of and including the adsorbent module, shall be cleaned
as described in Section 3A of the "Manual of Analytical Methods
for the Analysis of Pesticides in Human and Environmental
Samples." Special care shall be devoted to the removal of
residual silicone grease sealants on ground glass connections of
used glassware. Any residue shall be removed by soaking the
glassware for several hours in a chromic acid cleaning solution
prior to cleaning as described above.
4.1.1.2 Adsorbent Trap. The traps shall be loaded in a clean
area to avoid contamination. They may not be loaded in the
field. Fill a trap with 20 to 40 g of XAD-2. Follow the XAD-2
with glass wool and tightly cap both ends of the trap. Add 40 /xl
of the surrogate standard solution (Section 3.3.21) to each trap
for a sample that will be split prior to analysis or 20 A*l of the
26
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surrogate standard solution (Section 3.3.21) to each trap for
samples that will not be split for analysis (Section 5.1). After
addition of the surrogate standard solution, the trap must be
used within 14 days. Keep the spiked sorbent under refrigeration
until use.
4.1.1.3 Sampling Train. It is suggested that all components
be maintained according to the procedure described in APTD-0576.
4.1.1.4 Silica Gel. Weigh several 200 to 300 g portions of
silica gel in air tight containers to the nearest 0.5 g. Record
the total weight of the silica gel plus container, on each
container. As an alternative, the silica gel may be weighed
directly in the fifth impinger just prior to sampling.
4.1.1.5 Filter. Check each filter against light for
irregularities and flaws or pinhole leaks. Pack the filters flat
in a clean glass container or Teflon baggie. Do not mark filter
with ink or any other contaminating substance.
4.1.2 Preliminary Determinations. Same as Section 4.1.2
Method 5.
4.1.3 Preparation of Sampling Train.
4.1.3.1 During preparation and assembly of the sampling train,
keep all train openings where contamination can enter, sealed
until sampling is about to begin. Wrap sorbent module with
aluminum foil to shield from radiant heat of sun light. (NOTE:
27
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Do not use sealant grease in assembling the train.)
4.1.3.2 Place approximately 100 mL of water in the second and
third impingers, leave the first and fourth impingers empty, and
transfer approximately 200 to 300 g of preweighed silica gel from
its container to the fifth impinger.
4.1.3.3 Place the silica gel container in a clean place for
later use in the sample recovery. Alternatively, the weight of
the silica gel plus the fifth impinger may be determined to the
nearest 0.5 g and recorded.
4.1.3.4 Assemble the sampling train as shown in Figure 23-1.
4.1.3.5 Turn on the adsorbent module and condenser coil
recirculating pump and begin monitoring the adsorbent module gas
entry temperature. Ensure proper sorbent gas entry temperature
before proceeding and before sampling is initiated. It is
extremely important that the XAD-2 adsorbent resin temperature
never exceed 50°C because thermal decomposition and breakthrough
of surrogate standards will occur. During testing, the XAD-2
temperature must not exceed 20°C for efficient capture of the
PCDD's and PCDF's.
4.1.4 Leak-Check Procedure. Same as Method 5, Section 4.1.4.
4.1.5 Sampling Train Operation. Same as Method 5,
Section 4.1.5.
4.2 Sample Recovery. Proper cleanup procedure begins as soon
28
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as the probe is removed from the stack at the end of the sampling
period. Seal the nozzle end of the sampling probe with Teflon
tape or aluminum foil.
When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe. Remove the probe
from the train and close off both ends with aluminum foil. Seal
off the inlet to the train with Teflon tape, a ground glass cap,
or aluminum foil.
Transfer the probe and impinger assembly to the cleanup area.
This area shall be clean and enclosed so that the chances of
losing or contaminating the sample are minimized. Smoking, which
could contaminate the sample, shall not be allowed in the cleanup
area. Cleanup personnel shall wash their hands prior to sample
recovery.
Inspect the train prior to and during disassembly and note any
abnormal conditions, e.g., broken filters, colored impinger
liquid, etc. Treat the samples as follows:
4.2.1 Container No. 1. Either seal the filter holder or
carefully remove the filter from the filter holder and place it
in its identified container. Do not place the filter in aluminum
foil. Use a pair of cleaned tweezers to handle the filter. If
it is necessary to fold the filter, do so such that the
particulate cake is inside the fold. Carefully transfer to the
29
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container any particulate matter and filter fibers which adhere
to the filter holder gasket, by using a dry inert bristle brush
and a sharp-edged blade. Seal the container with Teflon tape.
4.2.2 Adsorbent Module. Remove the module from the train,
tightly cap both ends, label it, and store it on ice for
transport to the laboratory.
4.2.3 Container No. 2. Quantitatively recover material
deposited in the nozzle, probe transfer lines, the front half of
the filter holder, and the cyclone, if used, first, by brushing
while rinsing three times with acetone and then, by rinsing the
probe three times with toluene. Collect all the rinses in
Container No. 2.
Rinse the back half of the filter holder three times with
acetone. Rinse the connecting line between the filter and the
condenser three times with acetone. Soak the connecting line
with three separate portions of toluene for 5 minutes each. If
using a separate condenser and adsorbent trap, rinse the
condenser in the same manner as the connecting line. Collect all
the rinses in Container No. 2 and mark the level of the liquid on
the container.
4.2.4 Impinger Water. Measure the liquid in the first four
impingers to within 1 mL by using a graduated cylinder or by
weighing it to within 0.5 g by using a balance. Record the
30
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volume or weight of liquid present. This information is required
to calculate the moisture content of the effluent gas. Discard
the liquid after measuring and recording the volume or weight.
4.2.5 Silica Gel. Note the color of the indicating silica gel
to determine if it has been completely spent and make a mention
of its condition. Transfer the silica gel from the fifth
impinger to its original container and seal.
5. ANALYSIS
All glassware shall be cleaned as described in Section 3A of
the "Manual of Analytical Methods for the Analysis of Pesticides
in Human and Environmental Samples." All samples must be
extracted within 30 days of collection and analyzed within 45
days of extraction.
5.1 Sample Extraction. The analyst may choose to split the
sample extract after the completion of sample extraction
procedures. One half of the sample can then be archived. Sample
preparation procedures are given for using the entire sample and
for splitting the sample.
5.1.1 Extraction System. Place an extraction thimble (Section
2.3.4) , 1 g of silica gel, and a plug of glass wool into the
Soxhlet apparatus, charge the apparatus with toluene, and reflux
for a minimum of 3 hours. Remove the toluene and discard it, but
retain the silica gel. Remove the extraction thimble from the
31
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extraction system and place it in a glass beaker to catch the
solvent rinses.
5.1.2 Container No. 1 (Filter). Transfer the contents
directly to the glass thimble of the extraction system and
extract them simultaneously with the XAD-2 resin.
5.1.3 Adsorbent Cartridge. Suspend the adsorbent module
directly over the extraction thimble in the beaker (See Section
5.1.1). The glass frit of the module should be in the up
position. Using a Teflon squeeze bottle containing toluene,
flush the XAD-2 into the thimble onto the bed of cleaned silica
gel. Thoroughly rinse the glass module catching the rinsings in
the beaker containing the thimble. If the resin is wet,
effective extraction can be accomplished by loosely packing the
resin in the thimble. Add the XAD-2 glass wool plug to the
thimble.
5.1.4 Container No. 2 (Acetone and Toluene). Concentrate the
sample to a volume of about 1-2 mL using a Kuderna-Danish
concentrator apparatus, followed by N2 blow down at a temperature
of less than 37°C. Rinse the sample container three times with
small portions of methylene chloride and add these to the
concentrated solution and concentrate further to near dryness.
This residue contains particulate matter removed in the rinse of
the sampling train probe and nozzle. Add the concentrate to the
32
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filter and the XAD-2 resin in the Soxhlet apparatus described in
Section 5.1.1.
5.1.5 Extraction. For samples that are to be split prior to
analysis add 40 /xl of the internal standard solution
(Section 3.3.20) to the extraction thimble containing the
contents of the adsorbent cartridge, the contents of
Container No. 1, and the concentrate from Section 5.1.4.
Alternatively, 20 ptl of the internal standard solution
(Section 3.3.20) for samples that are not to be split prior to
analysis. Cover the contents of the extraction thimble with the
cleaned glass wool plug to prevent the XAD-2 resin from floating
into the solvent reservoir of the extractor. Place the thimble
in the extractor, and add the toluene contained in the beaker to
the solvent reservoir. Add additional toluene to fill the
reservoir approximately 2/3 full. Add Teflon boiling chips and,
assemble the apparatus. Adjust the heat source to cause the
extractor to cycle three times per hour. Extract the sample for
16 hours. After extraction, allow the Soxhlet to cool. Transfer
the toluene extract and three 10-mL rinses to the rotary
evaporator. Concentrate the extract to approximately 10 mL. If
decided to split the sample, store one half for future use, and
analyze the other half according to the procedures in Sections
5.2 and 5.3. In either case, use a nitrogen evaporative
33
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concentrator to reduce the volume of the sample being analyzed to
near dryness. Dissolve the residue in 5 mL of hexane.
5.2 Sample Cleanup and Fr&ctionation.
The following sample cleanup and fractionation procedures are
recommended. Alternative procedures may be utilized providing
acceptable identification criteria (Section 5.3.2.5) and
quantification criteria (Section 5.3.2.6) are met.
5.2.1 Silica Gel Column. Pack one end of a glass column,
20 mm x 230 mm, with glass wool. Add in sequence, 1 g silica
gel, 2 g of sodium hydroxide impregnated silica gel, 1 g silica
gel, 4 g of acid-modified silica gel, and 1 g of silica gel.
Wash the column with 30 mL of hexane and discard. Add the sample
extract, dissolved in 5 mL of hexane to the column with two
additional 5-mL rinses. Elute the column with an additional 90
mL of hexane and retain the entire eluate. Concentrate this
solution to a volume of about 1 mL using the nitrogen evaporative
concentrator (Section 2.3.9).
5.2.2 Basic Alumina Column. Shorten a 25-mL disposable
Pasteur pipette to about 16 mL. Pack the lower section with
glass wool and 12 g of basic alumina. Transfer the concentrated
extract from the silica gel column to the top of the basic
alumina column and elute the column sequentially with 120 mL of
0.5 percent methylene chloride in hexane followed by 120 mL of 35
34
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percent methylene chloride in hexane. Discard the first 120 mL
of eluate. Collect the second 120 mL of eluate and concentrate
it to about 0.5 mL using the nitrogen evaporative concentrator.
Transfer this extract with hexane to "13 mL tubes".
5.2.3 AX-21 Carbon/Celite 545 Column. Remove the bottom 0.5
in. from the tip of a 2-mL disposable Pasteur pipette. Insert a
glass fiber filter disk or glass wool plug in the top of the
pipette 2.5 cm from the constriction. Add sufficient
carbon/Celite™ mixture to form a 2 cm column (the 0.6 mL mark
column. Top with a glass wool plug. In some cases AX-21 carbon
fines may wash through the glass wool plug and enter the sample.
This may be prevented by adding a celite plug to the exit end of
the column. Pre-elute the column with 5 mL toluene, followed by 1
mL of a 50:50 methylene chloride/cyclohexane mixture, followed by
5 mL of hexane. Load in sequence, the sample extract in 1 mL
hexane, 2x0.5 mL rinses in hexane, 2 mL of 50 percent methylene
chloride in hexane and 2 mL of 50 percent benzene in ethyl
acetate and discard the eluates. Invert the column and elute in
the reverse direction with 13 mL of toluene. Collect this
eluate. Concentrate the eluate in a nitrogen evaporator at 45°C
to about 1 mL. Transfer the concentrate to a Reacti-vial using a
toluene rinses and concentrate to near dryness (less than 20
using a stream of N2. Store extracts at room temperature,
35
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shielded from light, until the analysis is performed.
5.3 Analysis. Analyze the sample with a gas chromatograph
coupled to a mass spectrometer (GC/MS) using the instrumental
parameters in Sections 5.3.1 and 5.3.2. Immediately prior to
analysis, add a 20 ^il aliquot of the recovery standard solution
from Table 2 to each sample. A 2 pi aliquot of the extract is
injected into the GC. Sample extracts are first analyzed using
the DB-5 capillary column to determine the concentration of each
isomer of PCDD's and PCDF's (tetra-through octa-). If 2,3,7,8-
TCDF is detected in this analysis, then analyze another aliquot
of the sample in a separate run, using the DB-225 column to
measure the 2,3,7,8 tetra-chloro dibenzofuran isomer. Other
column systems may be used, provided that it can be demonstrated
using calibration and performance checks that the column system
is able to meet the specifications of Section 6.1.2.
5.3.1 Gas Chromatograph Operating Conditions. The recommended
conditions are shown in Table 4.
5.3.2 High Resolution Mass Spectrometer.
5.3.2.1 Resolution. 10,000 resolving power or 100 ppm
mass/mass.
5.3.2.2 lonization Mode. Electron impact.
5.3.2.3 Source Temperature 250°C.
5.3.2.4 Monitoring Mode. Selected ion monitoring. A list of
36
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the various ions to be monitored is presented in Table 5.
5.3.2.5 Identification Criteria. The following identification
criteria shall be used for the characterization of
polychlorinated dibenzodioxins and dibenzofurans.
1. The integrated ion-abundance ratio (M/M+2 or M+2/M+4) shall
be within 15 percent of the theoretical value. The acceptable
ion-abundance ratio ranges (±15%) for the identification of
chlorine-containing compounds are given in Table 6. If the ion-
abundance ratio ranges are the outside those in Table 6, the
source has the option of using the results if the concentration
is determined using procedures in Section 9.3 or redoing the
analysis to eliminate the unacceptable ion-abundance ratio.
2. The retention time for the analytes must be within 3
seconds of the corresponding 13C-labeled internal standard or
surrogate standard.
3. The monitored ions, shown in Table 5 for a given analyte,
shall reach their maximum within 2 seconds of each other.
4. The identification of specific isomers that do not have
corresponding 13C-labeled standards is done by comparison of the
relative retention time (RRT) of the analyte to the nearest
internal standard retention time with reference (i.e., within
0.005 RRT units) to the comparable RRT's found in the continuing
calibration.
37
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5. The signal to noise ratio for all monitored ions must be
greater than 2.5.
6. The confirmation of 2, 3, 7, 8-TCDF shall satisfy all of
the above identification criteria.
7. Any PCDF coeluting (±2 s) with a peak in the corresponding
PCDPE channel, of intensity 10% or greater compared to the
analyte peak is evidence of a positive interference, the source
may opt keep the value to calculate CDD/CDF concentration or
conduct a complete reanalysis in an effort to remove or shift the
interference. If a reanalysis is conducted, all values from the
reanalyzed sample will be used for CDD/CDF concentration
calculations.
8. Set the mass spectrometer lock channels as specified in
Table 5. Monitor the quality control check channels specified in
Table 5 to verify instrument stability during the analysis. If
the signal varies by more than 25 percent from the average
response, results for all isomers at corresponding residence time
shall be invalid. The source has the options of conducting
additional cleanup procedures on the other portion of the sample
for split samples or diluting the original sample or following
other procedures recommended by the Administrator. When a
complete reanalysis is conducted, all concentration calculations
shall be based on the reanalyzed sample.
38
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5.3.2.6 Quantification. The peak areas for the two ions
monitored for each analyte are summed to yield the total response
for each analyte. Each internal standard is used to quantify the
indigenous PCDD's or PCDF's in its homologous series. For
example, the 13C12-2, 3 , 7, 8-tetra chlorinated dibenzodioxin is used
to calculate the concentrations of all other tetra chlorinated
isomers. Recoveries of the tetra- and penta- internal standards
are calculated using the 13C12-1, 2, 3 , 4-TCDD. Recoveries of the
hexa- through octa- internal standards are calculated using 13C12-
1,2,3,7,8,9-HxCDD. Recoveries of the surrogate standards are
calculated using the corresponding homolog from the internal
standard. When no peak is detected, the noise level, as measured
by the intensity of the noise in a clear zone of the
chromatogram, is used to calculate the detection limit. Tables
7, 8, and 9 summarize the quantification relationships for the
unlabeled analytes, internal standards and surrogate standards,
respectively.
6. CALIBRATION
Same as Method 5 with the following additions.
6.1 GC/MS System.
6.1.1 Initial Calibration. Calibrate the GC/MS system using
the set of five standards shown in Table 3. The relative
standard deviation for the mean response factor from each of the
39
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unlabeled analytes (Table 3) and of the internal and surrogate
standards shall be less than or equal to the values in Table 6.
The signal to noise ratio for the GC signal present in every
selected ion current profile shall be greater than or equal to
10. The ion abundance ratios shall be within the control limits
in Table 5.
6.1.2 Daily Performance Check.
6.1.2.1 Calibration Check. Inject 2 p.1 of solution Number 3
from Table 3. Calculate the relative response factor (RRF) for
each compound and compare each RRF to the corresponding mean RRF
obtained during the initial calibration. The analyzer
performance is acceptable if the measured RRF's for the labeled
and unlabeled compounds for the daily run are within the limits
of the mean values shown in Table 10. In addition, the ion-
abundance ratios shall be within the allowable control limits
shown in Table 6.
6.1.2.2 Column Separation Check. Inject 2 /zl of a solution of
a mixture of PCDD's and PCDF's that documents resolution between
2,3,7,8-TCDD and other TCDD isomers. Resolution is defined as a
valley between peaks that is less than 25 percent of the lower of
the two peaks. Identify and record the retention time windows
for each homologous series. Perform a similar resolution check
on the confirmation column to document the resolution between
40
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2,3,7,8 TCDF and other TCDF isomers.
6.2 Lock Channels. Set mass spectrometer lock channels as
specified in Table 5. Monitor the quality control check channels
specified in Table 5 to verify instrument stability during the
analysis.
7. QUALITY CONTROL
7.1 Sampling Train Collection Efficiency Check. Add 40 /*! of
the surrogate standards in Table 2 for samples split for analysis
or 20 £il of the surrogate standards for sample not split for
analysis to the adsorbent cartridge of each train before
collecting the field samples.
7.2 Internal Standard Percent Recoveries. A group of nine
carbon-labeled PCDDs and PCDFs representing the tetra- through
octachlorinated homologues, is added to every sample prior to
extraction. The role of the internal standards is to quantify
the native PCDD's and PCDF's present in the sample as well as to
determine the overall method efficiency. Recoveries of the
internal standards shall be between 40 to 130 percent for the
tetra- through hexachlorinated compounds while the range is 25 to
130 percent for the hepta- and octachlorinated homologues.
7.3 Surrogate Standard Recoveries. The five surrogate
compounds in Table 3 are added to the resin in the adsorbent
sampling cartridge before the sample is collected. The surrogate
41
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recoveries are measured relative to the internal standards and
are a measure of the sampling train collection efficiency. They
are not used to measure the native PCDD's and PCDF's. All
surrogate standard recoveries shall be between 70 and
130 percent. Poor recoveries for all the surrogates may be an
indication of breakthrough in the sampling train. If the
recovery of all standards is below 70 percent, the sampling runs
must be repeated. As an alternative, the sampling runs do not
have to be repeated if the final results are divided by the
fraction of surrogate recovery (on a homolog group basis) . Poor
recoveries of isolated surrogate compounds should not be grounds
for rejecting an entire set of samples.
7.4 Toluene QA Rinse. Report the results of the toluene QA
rinse separately from the total sample catch. Do not add it to
the total sample.
7.5 Detection Limits. Calculate the detection limits using
the equation in Section 9.8. If the detection limits meet the
Target Detection Limits (TDLs) in Table 1, then they are
considered acceptable. If the TDLs are not met, the impact of
the detection limits shall be calculated using the procedures in
Section 9.9. If the maximum potential value of the sum of the
summed detection limits is less then 50 percent of the emission
standard, the detection limits are acceptable. If the value is
42
-------
greater than 50 percent of the emission standard, then the
analysis and/or sampling and analysis must be repeated until
acceptable detection limits are obtained.
8. QUALITY ASSURANCE
8.1 Applicability. When the method is used to analyze samples
to demonstrate compliance with a source emission regulation, an
audit sample must be analyzed, subject to availability.
8.2 Audit Procedure. Analyze an audit sample with each set of
compliance samples. The audit sample contains tetra through octa
isomers of PCDD and PCDF. Concurrently analyze the audit sample
and a set of compliance samples in the same manner to evaluate
the technique of the analyst and the standards preparation. The
same analyst, analytical reagents, and analytical system shall be
used both for the compliance samples and the EPA audit sample.
8.3 Audit Sample Availability. Audit samples will be supplied
only to enforcement agencies for compliance tests. Audit samples
may be obtained by writing:
Source Test Audit Coordinator (MD-77B)
Quality Assurance Division
Atmospheric Research and Exposure Assessment Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
or by calling the Source Test Audit Coordinator (STAC) at (919)
43
-------
541-7834. The audit sample request must be made at least 30 days
prior to the scheduled compliance sample analysis.
8.4 Audit Results. Calculate the audit sample concentration
according to the calculation procedure provided in the audit
instructions included with the audit sample. Fill in the audit
sample concentration and the analyst's name on the audit response
form included with the audit instructions. Send one copy to the
EPA Regional Office or the appropriate enforcement agency and a
second copy to the STAC. The EPA Regional office or the
appropriate enforcement agency will report the results of the
audit to the laboratory being audited. Include this response
with the results of the compliance samples in relevant reports to
the EPA Regional Office or the appropriate enforcement agency.
9. CALCULATIONS
Same as Method 5, Section 6 with the following additions.
9.1 Nomenclature.
Aai = Integrated ion current of the noise at the retention time
of the analyte.
Acij = Integrated ion current of the two ions characteristic of
compound i in the jth calibration standard.
A*cij = Integrated ion current of the two ions characteristic of
the internal standard i in the jth calibration standard.
Acsi = Integrated ion current of the two ions characteristic of
44
-------
surrogate compound i in the calibration standard.
AA = Integrated ion current of the two ions characteristic of
compound i in the sample.
A*i = Integrated ion current of the two ions characteristic of
internal standard i in the sample.
Ars = Integrated ion current of the two ions characteristic of
the recovery standard.
Asi = Integrated ion current of the two ions characteristic of
surrogate compound i in the sample.
G! = Concentration of PCDD or PCDF i in the sample, pg/M3.
CT = Total concentration of PCDD's or PCDF's in the sample,
pg/M3.
DL = Detection limit, pg/sample.
DLhs = Detection limit for each homologous series, pg/sample.
DLsum = Sum of all isomers times the corresponding detection
limit, ng/m3.
Hai = Summed heights of the noise at the retention time of the
analyte in the two analyte channels.
mci = Mass of compound i in the calibration standard injected
into the analyzer, pg.
m*ci = Mass of labeled compound i in the calibration standard
injected into the analyzer, pg.
m*i = Mass of internal standard i added to the sample, pg.
45
-------
mrs = Mass of recovery standard in the calibration standard
injected into the analyzer, pg.
ms = Mass of surrogate compound in the sample to be analyzed,
pg.
msi = Mass of surrogate compound i in the calibration standard,
P9-
RRFi = Relative response factor for compound i.
RRFrs = Recovery standard response factor.
RRFS = Surrogate compound response factor.
vmistd)= Metered volume of sample run, dscm.
1000 = pg per ng.
9.2 Average Relative Response Factor.
A m
RRF = - cij " Eq. 23-1
ni=i A* m
cij ci
9.3 Concentration of the PCDD's and PCDF's.
i
C. = Eq. 23-2
A/ RRF. V
1 i n>_^
9.4 Recovery Standard Response Factor.
46
-------
RRFrs = -T Eq. 23-3
Ars md
9.5 Recovery of Internal Standards (R*)
A, m
R' = —x!00% Eg. 23-4
9.6 Surrogate Compound Response Factor.
A ; m .
RRF£ = £1- Eq. 23-5
9.7 Recovery of Surrogate Compounds (R,) .
si
R3 = — x!00% Eq. 23-6
9.8 Detection Limit (DL). The detection limit can be
calculated based on either the height of the noise or the area of
47
-------
the noise using one of the two equations.
Detection limit using height for the DB-225 column. Three and
one half times the height has been empirically determined to give
area.
2.5 (3.5 x ff .) m,
DL = Eq. 23-7
Detection limit using height for the DB-5 column. Five times the
height has been empirically determined to give area.
2.5 (5 x H .) mi
DL = Eq. 23-8
Ac', RRF.
Detection limit using area of the noise.
2.5 A mi
DL = —- Eq. 23-9
9.9 Summed Detection Limits. Calculate the maximum potential
value of the summed detection limits. If the isomer (group of
unresolved isomers) was not detected, use the value calculated
for the detection limit in Section 9.8 above. If the isomer
(group of unresolved isomers) was detected, use the value (target
48
-------
detection limit) from Table 1.
DLSu» = <13 DLTCDD + 16 DLTCO. + 12 DLPeCOO
+ 14 DL., _„+ 7 DL,,.._ + 12 D
E 23_10
2 DLHPCDD + 4 D
100°
Note: The number of isomers used to calculate the summed
detection limit represent the total number of isomers typically
separated and not the actual number of isomers for each series.
9.10 Total Concentration of PCDD's and PCDF's in the Sample.
Cr = EC, E<3- 23-i:L
i=l
Any PCDDs or PCDFs that are reported as not detected (below the
DL) shall be counted as zero for the purpose of calculating the
total concentration of PCDDs and PCDFs in the sample.
10. BIBLIOGRAPHY
1. American Society of Mechanical Engineers. Sampling for the
Determination of Chlorinated Organic Compounds in Stack
Emissions. Prepared for U.S. Department of Energy and U.S.
Environmental Protection Agency. Washington DC. December 1984.
25 p.
2. American Society of Mechanical Engineers. Analytical
49
-------
Procedures to Assay Stack Effluent Samples and Residual
Combustion Products for Polychlorinated Dibenzo-p-Dioxins (PCDD)
and Polychlorinated Dibenzofurans (PCDF). Prepared for the U.S.
Department of Energy and U.S. Environmental Protection Agency.
Washington, DC. December 1984. 23 p.
3. Thompson, J. R. (ed.). Analysis of Pesticide Residues in
Human and Environmental Samples. U.S. Environmental Protection
Agency. Research Triangle Park, NC. 1974.
4. Triangle Laboratories. Case Study: Analysis of Samples
for the Presence of Tetra Through Octachloro-p-Dibenzodioxins and
Dibenzofurans. Research Triangle Park, NC. 1988. 26 p.
5. U.S. Environmental Protection Agency. Method 8290 - The
Analysis of Polychlorinated Dibenzo-p-dioxin and Polychlorinated
Dibenzofurans by High-Resolution Gas Chromatography/
High-Resolution Mass Spectrometry. In: Test Methods for
Evaluating Solid Waste. Washington, DC. SW-846.
6. Personnel communications with R. L. Harless of U.S. EPA and
Triangle Laboratory staff.
50
-------
TABLE 23-1. TARGET DETECTION LIMITS (TDLs)
ANALYTE
TCDD/TCDF
PeCDD/PeCDF
HxCDD/HxCDF
HpCDD/HpCDF
OCDD/OCDF
TDL (pg/Sample Train)
50
250
250
250
500
TABLE 23-2. COMPOSITION OF THE SAMPLE FORTIFICATION AND RECOVERY
STANDARDS SOLUTIONS*
ANALYTE
CONCENTRATION (pg//iL)
Internal Standards
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDD
13C12 -1,2,3,6,7, 8 -HxCDD
13C12 -1,2,3,4,6,7, 8 -HpCDD
13C12-OCDD
13C12-2,3,7,8-TCDF
13C12-1,2,3, 7, 8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13C12-1,2,3,4,6,7, 8-HpCDF
100
100
100
100
100
100
100
100
100
Surrogate Standards
37Cl4-2,3,7,8-TCDD
13C12 -1,2,3,4,7,8 -HxCDD
13C12-2,3,4,7,8-PeCDF
13C12-l,2,3,4,7,8-HxCDF
13C12-1 , 2,3,4,7,8,9 -HpCDF
100
100
100
100
100
Recovery Standards
51
-------
13C12-1,2,3,4-TCDD
13C12-1 , 2,3,7,8,9 -HxCDD
100
100
'Calibration levels are specific for samples at
the MWC compliance standard level.
52
-------
TABLE 23-3. COMPOSITION OF THE INITIAL CALIBRATION SOLUTIONS
COMPOUND
SOLUTION NO.
CONCENTRATIONS (pg//xl)
1
2
3
4
5
UNLABELED ANALYTES
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-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-HxCDF
1,2,3,7,8,9-HxCDF
2,3,4,6,7,8-HxCDD
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
0.5
0.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
5
5
1
1
5
5
5
5
5
5
5
5
5
5
5
5
5
10
10
5
5
25
25
25
25
25
25
25
25
25
25
25
25
25
50
50
50
50
250
250
250
250
250
250
250
250
250
250
250
250
250
500
500
100
100
500
500
500
500
500
500
500
500
500
500
500
500
500
1000
1000
INTERNAL STANDARDS
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDD
13C12 -1,2,3,6,7,8 -HxCDD
13C12- 1 ,2,3,4,6,7, 8 -HpCDD
13C12-OCDD
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
53
-------
13C12-2,3f7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13C12- 1 ,2,3,4,6,7,8 -HpCDF
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
TABLE 23-3. (Continued)
COMPOUND
SOLUTION NO.
CONCENTRATION (pg//il)
1
2
3
4
5
SURROGATE STANDARDS
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
13C12 - 1 , 2 , 3 , 4 , 7 , 8 - HxCDD
13C12- 1 ,2,3,4,7,8 -HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
60
60
60
60
60
80
80
80
80
80
100
100
100
100
100
120
120
120
120
120
140
140
140
140
140
RECOVERY STANDARDS
13C12-1,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
100
100
100
100
100
100
100
100
100
100
54
-------
TABLE 23-4. RECOMMENDED GC OPERATING CONDITIONS
Column Type
DB-5
DB-225
Length (m)
i.d. (mm)
Film Thickness
Carrier Gas
(A«n)
Carrier Gas Flow (mL/min)
60
0.25
0.25
Helium
1-2
30
0.25
0.25
Helium
1-2
Injection Mode
<-- splitless -->
Valve Time (min)
2.5
2.5
Initial Temperature (° C)
Initial Time (min)
Rate 1 (deg. C/min)
Temperature 2 (deg. C)
Rate 2 (deg. C/min)
Final Temperature (deg. C)
150
0.5
60
170
3
300
130
2.5
50
170
4
250
55
-------
TABLE 23-5. ELEMENTAL COMPOSITIONS AND EXACT MASSES OF THE IONS
MONITORED BY HIGH RESOLUTION MASS SPECTROMETRY FOR PCDD's AND PCDF's
DESCRIPTOR
NUMBER
2
3
ACCURATE
MASS
292.9825
303.9016
30.5.8987
315.9419
317.9389
319.8965
321.8936
327.8847
330.9792
331.9368
333.9339
339.8597
341.8567
351.9000
353.8970
355.8546
357.8516
367.8949
369.8919
375.8364
409.7974
373.8208
375.8178
383.8639
385.8610
389.8157
391.8127
392.9760
ION
TYPE
LOCK
M
M+2
M
M+2
M
M+2
M
QC
M
M+2
M+2
M+4
M+2
M+4
M+2
M+4
M+2
M+4
M+2
M+2
M+2
M+4
M
M+2
M+2
M+4
LOCK
ELEMENTAL COMPOSITION
C,Fn
C12H435C14O
C12H435C13C137O
13C12H435C140
13C12H435C1337C10
C12H435C1402
C12H435C1337C1O2
C12H437C1402
C,F13
13C12H435C1402
13C12H435C137C102
C12H335C1437C10
C12H335C1337C120
13C12H335C1437C10
13C12H335C1337C120
C12H335C1337C102
C12H335C1337C1202
13C12H335C1437C102
13C12H335C1337C1202
C12H435C1537C10
C12H335C1637C10
C12H235C1537C1O
C12H235C1437C120
13C12H23SC160
13C12H235C1537C10
C12H235C1537C1O2
C12H235C1437C1202
C9F15
ANALYTE
PFK
TCDF
TCDF
TCDF(S)
TCDF(S)
TCDD
TCDD
TCDD(S)
PFK
TCDD(S)
TCDD(S)
PeCDF
PeCDF
PeCDF (S)
PeCDF (S)
PeCDD
PeCDD
PeCDD (S)
PeCDD (S)
HxCDPE
HpCPDE
HxCDF
HxCDF
HxCDF (S)
HxCDF (S)
HxCDD
HxCDD
PFK
56
-------
401.8559
403.8529
445.7555
430.9729
M+2
M+4
M+4
QC
13C12H235C1537C102
13C12H235C1437C120
C12H235C1637C120
C9F17
HxCDD(S)
HxCDD(S)
OCDPE
PFK
TABLE 23-5.
(Continued)
DESCRIPTOR
NUMBER
ACCURATE
MASS
407.7818
409.7789
417.8253
389.8157
391.8127
392.9760
401.8559
403.8529
445.7555
430.9729
407.7818
409.7789
417.8253
419.8220
423 .7766
425.7737
435.8169
437.8140
479.7165
430.9729
441.7428
443.7399
457.7377
459.7348
469.7779
ION
TYPE
M+2
M+4
M
M+2
M+4
LOCK
M+2
M+4
M+4
QC
M+2
M+4
M
M+2
M+2
M+4
M+2
M+4
M+4
LOCK
M+2
M+4
M+2
M+4
M+2
ELEMENTAL DESCRIPTION
C12H35C1637C1O
C12H35C1537C12O
13C12H35C170
C12H235C1537C1O2
C12H235C1437C1202
C9F15
13C12H235C1537C102
13C12H235C1437C120
C12H235C1637C120
C9F17
C12H35C1637C10
C12H35C1537C12O
13C12H35C170
13C12H35C1637C10
C12H35C1637C1O2
C12H35C1537C12O2
13C12H35C1637C102
13C12H35C1537C1202
C12H35C1737C120
C9F17
C1235C1737C10
C1235C1637C120
C1235C1737C102
C1235C1637C1202
13C1235C1737C102
ANALYTE
HpCDF
HpCDF
HpCDF (S)
HxCDD
HxCDD
PFK
HxCDD (S)
HxCDD (S)
OCDPE
PFK
HpCDF
HpCDF
HpCDF (S)
HpCDF (S)
HpCDD
HpCDD
HpCDD (S)
HpCDD (S)
NCPDE
PFK
OCDF
OCDF
OCDD
OCDD
OCDD(S)
-------
471.7750
513.6775
442.9728
M-t-4
M+4
QC
13C1235C1637C1202
C1235C1837C1202
^-10^17
OCDD(S)
DCDPE
PFK
35C1 = 34.968853
The following nuclidic masses were used:
H = 1.007825 0 = 15.994914 C = 12.000000
13C = 13.003355 37C1 = 36.965903 F = 18.9984
S = Labeled Standard
QC = Ion selected for monitoring instrument stability during the
GC/MS analysis.
-------
TABLE 23-6. ACCEPTABLE RANGES FOR ION-ABUNDANCE RATIOS OF PCDD'S AND
PCDF's
Number of
Chlorine
Atoms
4
5
6
6a
7b
7
8
Ion Type
M/M+2
M+2/M+4
M+2/M+4
M/M+2
M7M+2
M+2/M+4
M+2/M+4
Theoretical
Ratio
0.77
1.55
1.24
0.51
0.44
1.04
0.89
Control Limits
Lower
0.65
1.32
1.05
0.43
0.37
0.88
0.76
Upper
0.89
1.78
1.43
0.59
0.51
1.20
1.02
-------
TABLE 23-7. UNLABELED ANALYTES QUANTIFICATION RELATIONSHIPS
ANALYTE
2,3,7,8-TCDD
Other TCDD's
INTERNAL STANDARD USED
13C12- 2,3,7,8-TCDD
13C12-2,3,7,8-TCDD
1,2,3,7,8-PeCDD
Other PeCDD's
13C12-l,2,3,7,8-PeCDD
13C12-l,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
Other HxCDD's
13C12 -1,2,3,6,7,8 -HxCDD
13C12 -1,2,3,6,7,8 -HxCDD
13C12- 1 ,2,3,6,7,8 -HxCDD
13C12-1 , 2,3,6,7, 8-HxCDD
1,2,3,4,6,7,8-HpCDD
Other HpCDD ' s
13C12-1 , 2,3,4,6 , 7, 8-HpCDD
13C12 - 1 , 2 , 3 , 4 , 6 , 7 , 8 -HpCDD
OCDD
13C12-OCDD
2,3,7,8-TCDF
Other TCDF ' s
13C12-2,3,7,8-TCDF
13C12-2,3,7,8-TCDF
1,2,3,7, 8-PeCDF
2,3,4,7,8-PeCDF
Other PeCDF's
13C12-l,2,3,7,8-PeCDF
13C12-1,2,3,7, 8-PeCDF
13C12-l,2,3,7,8-PeCDF
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
Other HxCDF's
13C12 -1,2,3,6,7,8 -HxCDF
13C12-1 , 2,3,6,7,8 -HxCDF
13C12-1, 2 ,3,6,7, 8-HxCDF
13C12 -1,2,3,6,7,8 -HxCDF
13C12-l,2,3,6,7,8-HxCDF
1,2,3,4,6,7,8-HpCDF
13C12-l,2,3,4,6,7,8-HpCDF
-------
1,2,3,4,7,8,9-HpCDF 13C12-1, 2, 3 , 4, 6 , 7, 8-HpCDF
OCDF
13
Cia-l,2,3,4,6,7,8-HpCDF
-------
TABLE 23-8. INTERNAL STANDARDS QUANTIFICATION RELATIONSHIPS
INTERNAL STANDARD
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDD
13C12-l,2,3,6,7,8-HxCDD
13C12-l,2,3,4,6,7,8-HpCDD
13C12-OCDD
13C12-2,3,7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13C12 - 1 , 2 , 3 , 6 , 7 , 8 -HxCDF
13C12 -1,2,3,4,6,7,8 -HpCDF
STANDARD USED DURING PERCENT
RECOVERY DETERMINATION
13C12-1,2,3,4-TCDD
13C12-1,2,3,4-TCDD
13C12-1,2,3,7,8, 9-HxCDD
l3Cia-l,2,3,7,8,9-HxCDD
13C12 -1,2,3,7,8, 9 -HxCDD
13C12-1,2,3,4-TCDD
13C12-1,2,3,4-TCDD
13C12 -1,2,3,7,8,9 -HxCDD
13C12- 1 ,2,3,7,8,9 -HxCDD
TABLE 23-9. SURROGATE STANDARDS QUANTIFICATION RELATIONSHIPS
SURROGATE STANDARD
37Cl4-2,3,7,8-TCDD
13C12-2,3,4/7/8-PeCDF
13C12-1,2,3,4,7, 8 -HxCDD
13C12-1 , 2,3,4,7 , 8 -HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
STANDARD USED DURING PERCENT
RECOVERY DETERMINATION
13C12-2,3,7,8-TCDD
13C12-l,2,3,7,8-PeCDF
13C12 -1,2,3,6,7,8 -HxCDD
13C12-l,2,3,6,7,8-HxCDF
13C12 -1,2,3,4,6,7,8 -HpCDF
-------
TABLE 23-10. MINIMUM REQUIREMENTS FOR INITIAL AND DAILY CALIBRATION
RESPONSE FACTORS
COMPOUND
UNLABELED
2,3,7,8-TCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDD
1,2,3,7,8-PeCDF
1,2,4,5,7,8-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-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
OCDD
OCDF
SURROGATE
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
13C12 -1,2,3,4,7,8 -HxCDD
13C12-1 , 2,3,4,7 , 8-HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
RELATIVE RESI
INITIAL
CALIBRATION
(RSD)
ANALYTES
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
STANDARDS
25
3ONSE FACTORS
DAILY
CALIBRATION
{% DIFFERENCE)
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
25
-------
Thermocouple^
-8-Type Pilot
/ Filter Holder
Thermocouple—jr-i
^Thermocouple Thermocouple
^ f Check Valvt
XAD-2Trap
Stack Wall
Pilot
Manometer
RaclroulatlbnPump Wa(9r Knockout 100ml HPLC Watar
Implnoar §g§
Valva
Silica Gel
(300 grams)
Vacuum Una
Main Valve
Alr-Tlghl
Pump
Figure 5-1. CDD/CDF Sampling Train Configuration
-------
Condenser
Flu* Gas Flow •
Sorbent Trap
(Q
h
(D
•20/18
37cm-
8 mm Glass Cooling Coll
To Suit-
Water Jacket Cooling Coll
Glee? Wool Plug Water Jacket XAD-2 Olaw Sintered Disk
(78 Qrams)
FIGURE 2. CONDENSER AND SORBENT TRAP FOR COLLECTION OF GASEOUS PCDDs AND
PCDFs
-------
Appendix G.6
EPA Method 25A
-------
Appendix G.6
EPA Method 25A
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
N8PS TEST METHOD
METHOD 25A-DBTERMINATION OF TOTAL GASEOUS ORGANIC
CONCENTRATION USING A FLAME IONIZATION ANALYZER
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total gaseous
organic concentration of vapors consisting primarily of alkanes, alkenes, and/or
arenes (aromatic hydrocarbons). The concentration is expressed in terms of
propane (or other appropriate organic calibration gas) or in terms of carbon.
1.2 Principle. A gas sample is extracted from the source through a heated
sample line, if necessary, and glass fiber filter to a flame ionization analyzer
(FIA) . Results are reported as volume concentration equivalents of the
calibration gas or as carbon equivalents.
2. Definitions
2.1 Measurement Systems. The total equipment required for the determination
of the gas concentration. The system consists of the following major subsystems:
2.1.1 Sample Interface. That portion of the system that is used for one or more
of the following: sample acquisition, sample transportation, sample
conditioning, or protection of the analyzer from the effects of the stack
effluent.
2.1.2 Organic Analyzer. That portion of the system that senses organic
concentration and generates an output proportional to the gas concentration.
2.2 Span Value. The upper limit of a gas concentration measurement range that
is specified for affected source categories in the applicable part of the
regulations. The span value is established in the applicable regulation and is
usually 1.5 to 2.5 times the applicable emission limit. If no span value is
provided, use a span value equivalent to 1.5 to 2.5 times the expected
concentration. For convenience, the span value should correspond to 100 percent
of the recorder scale.
2.3 Calibration Gas. A known concentration of a gas in an appropriate diluent
gas.
2.4 Zero Drift. The difference in the measurement system response to a zero
level calibration gas before and after a stated period of operation during which
no unscheduled maintenance, repair, or adjustment took place.
Prepared by Emission Measurement Branch EUtlC TM-25A
Technical Support Division, OAQPS, EPA June 23, 1993
-------
EMTIC TM-25A EMTIC NSPS TEST METHOD Page 2
2.5 Calibration drift. The difference in the measurement system response to
a midlevel calibration gas before and after a stated period of operation during
which no unscheduled maintenance, repair or adjustment took place.
2.6 Response Time. The time interval from a step change in pollutant
concentration at the inlet to the emission measurement system to the time at
which 95 percent of the corresponding final value is reached as displayed on the
recorder.
2.7 Calibration Error. The difference between the gas concentration indicated
by the measurement system and the known concentration of the calibration gas.
3. Apparatus.
A schematic of an acceptable measurement system is shown in Figure 25A-1.
The essential components of the measurement system are described below:
3.1 Organic Concentration Analyzer. A flame ionization analyzer (PIA) capable
of meeting or exceeding the specifications in this method.
3.2 Sanple Probe. Stainless steel, or equivalent, three-hole rake type.
Sample holes shall be 4 mm in diameter or smaller and located at 16.7, 50, and
83.3 percent of the equivalent stack diameter. Alternatively, a single opening
probe may be used so that a gas sample is collected from the centrally located
10 percent area of the stack cross-section.
3.3 Sample Line. Stainless steel or Teflon * tubing to transport the sample
gas to the analyzer. The sample line should be heated, if necessary, to prevent
condensation in the line.
3.4 Calibration Valve Assembly. A three way valve assembly to direct the zero
and calibration gases to the analyzers is recommended. Other methods, such as
quick-connect lines, to route calibration gas to the analyzers are applicable.
3.5 Particulate Filter. An in-a tack or an out-of-stack glass fiber filter is
recommended if exhaust gas particulate loading is significant. An out-of-stack
filter should be heated to prevent any condensation.
* Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
3.6 Recorder. A strip-chart recorder, analog computer, or digital recorder for
recording measurement data. The minimum data recording requirement is one
measurement value per minute, Note: This method is often applied in highly
explosive areas. Caution and care should be exercised in choice of equipment and
installation.
4. Calibration and Other Oases.
Oases used for calibrations, fuel, and combustion air (if required) are
-------
EMTIC TM-25A BMTIC NSPS TEST METHOD Page 3
contained in compressed gas cylinders. Preparation of calibration gases shall
be done according to the procedure in Protocol No. 1, listed in Citation 2 of
Bibliography. Additionally, the manufacturer of the cylinder should provide a
recommended shelf life for each calibration gas cylinder over which the
concentration does not change more than ±2 percent from the certified value. For
calibration gas values not generally available (i.e., organics between 1 and 10
percent by volume), alternative methods for preparing calibration gas mixtures,
such as dilution systems, may be used with prior approval of the Administrator.
Calibration gases usually consist of propane in air or nitrogen and are
determined in terms of the span value. Organic compounds other than propane can
be used following the above guidelines and making the appropriate corrections for
response factor.
4.1 Fuel. A 40 percent Hj/60 percent NZ gas mixture is recommended to avoid
an oxygen synergism effect that reportedly occurs when oxygen concentration
varies significantly from a mean value.
4.2 Zero Oas. High purity air with less than 0.1 parts per million by volume
(pptnv) of organic material (propane or carbon equivalent) or less than 0.1
percent of the span value, whichever is greater.
4.3 Low-level Calibration Oas. An organic calibration gas with a concentration
equivalent to 25 to 35 percent of the applicable span value.
4.4 Mid-level Calibration Oas. An organic calibration gas with a concentration
equivalent to 45 to 55 percent of the applicable span value.
4.5 High-level Calibration Oas. An organic calibration gas with a
concentration equivalent to 80 to 90 percent of the applicable span value.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than ±3 percent of the span value.
5.2 Calibration Drift. Less than ±3 percent of span value.
5.3 Calibration Error. Less than ±5 percent of the calibration gas value.
6. Pretest Preparations
6.1 Selection of Sampling Site. The location of the sampling site is generally
specified by the applicable regulation or purpose of the test; i.e., exhaust
stack, inlet line, etc. The sample port shall be located at least 1.5 meters or
2 equivalent diameters upstream of the gas discharge to the atmosphere.
6.2 Location of Sample Probe. Install the sample probe so that the probe is
centrally located in the stack, pipe, or duct and is sealed tightly at the stack
port connection.
-------
BMTIC TM-25A EMTIC NSPS TEST METHOD Page 4
6.3 Measurement System Preparation. Prior to the emission test, assemble the
measurement system following the manufacturer's written instructions in preparing
the sample interface and the organic analyzer. Make the system operable.
FIA equipment can be calibrated for almost any range of total organics
concentrations. For high concentrations of organics (>1.0 percent by volume as
propane) modifications to most commonly available analyzers are necessary. One
accepted method of equipment modification is to decrease the size of the sample
to the analyzer through the use of a smaller diameter sample capillary. Direct
and continuous measurement of organic concentration is a necessary consideration
when determining any modification design.
6.4 Calibration Error Test. Immediately prior to the test series, (within 2
hours of the start of the test) introduce zero gas and high-level calibration gas
at the calibration valve assembly. Adjust the analyzer output to the appropriate
levels, if necessary. Calculate the predicted response for the low-level and
mid-level gases based on a linear response line between the zero and high-level
responses. Then introduce low-level and mid-level calibration gases successively
to the measurement system. Record the analyzer responses for low-level and mid-
level calibration gases and determine the differences between the measurement
system responses and the predicted responses. These differences must be less
than 5 percent of the respective calibration gas value. If not, the measurement
system is not acceptable and must be replaced or repaired prior to testing. No
adjustments to the measurement system shall be conducted after the calibration
and before the drift check (Section 7.3). If adjustments are necessary before
the completion of the test series, perform the drift checks prior to the required
adjustments and repeat the calibration following the adjustments. If multiple
electronic ranges are to be used, each additional range must be checked with a
mid-level calibration gas to verify the multiplication factor.
6.5 Response Tim* Test. Introduce Zero gas into the measurement system at the
calibration valve assembly. When the system output has stabilized, switch
quickly to the high-level calibration gas. Record the time from the
concentration change to the measurement system response equivalent to 95 percent
of the step change. Repeat the test three times and average the results.
7. Emission Measurement Test Procedure
7.1 Organic Measurement. Begin sampling at the start of the test period,
recording time and any required process information as appropriate. In
particular, note on the recording chart periods of process interruption or cyclic
operation.
7.2 Drift Determination. Immediately following the completion of the test
period and hourly during the test period, reintroduce the zero and mid-level
calibration gases, one at a time, to the measurement system at the calibration
valve assembly. (Make no adjustments to the measurement system until after both
the zero and calibration drift checks are made.) Record the analyzer response.
If the drift values exceed the specified limits, invalidate the test results
preceding the check and repeat the teat following corrections to the measurement
-------
EMTIC TM-25A EMTIC NSPS TEST METHOD Page 5
system. Alternatively, recalibrate the test measurement system as in Section 6.4
and report the results using both sets of calibration data (i.e., data determined
prior to the test period and data determined following the test period) .
8. Organic Concentration calculations
Determine th^ average organic concentration in terms of ppmv as propane or
other calibration gas. The average shall be determined by the integration of the
output recording over the period specified in the applicable regulation. If
results are required in terms of ppmv as carbon, adjust measured concentrations
using Equation 25A-1.
Where:
Cc • Organic concentration as carbon, ppmv.
C^.," Organic concentration as measured, ppmv.
K • Carbon equivalent correction factor.
K - 2 for ethane.
K - 3 for propane.
K m 4 for butane.
K » Appropriate response factor for other organic calibration
gases.
9. Bibliography
1. Measurement of Volatile Organic Compounds-Guideline Series. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-450/2-78-041. June 1978. p. 46-54.
2. Traceability Protocol for Establishing True Concentrations of Oases
Used for Calibration and Audits of Continuous Source Emission
Monitors (Protocol No. 1). U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory. Research Triangle
Park, NC. June 1978.
3. Gasoline Vapor Emission Laboratory Evaluation-Part 2. U.S.
Environmental Protection Agency, Office of Air Quality Planning and
Standards. Research Triangle Park, NC. BMB Report No. 75-OAS-6.
August 1975.
-------
KMTIC TM-25A
EMTIC NSPS TEST METHOD
Page 6
Prob*
Oigwto
Aralyur
Pump
Stack
Figure 25A-1. Organic Concentration Measurement System.
-------
Appendix G.7
EPA Method 26A
-- __ ..-
-------
Method 26A - Determination of Hydrogen Halide and Halogen Emissions
from Stationary Sources - Isokinetic Method
1. APPLICABILITY, PRINCIPLE, INTERFERENCES, PRECISION, BIAS, AND
STABILITY
1.1 Applicability. This method is applicable for
determining emissions of hydrogen halides (HX) [hydrogen chloride
(HC1), hydrogen bromide (HBr), and hydrogen fluoride (HF)] and
halogens (X2) [chlorine (C12) and bromine (Br2) ] from stationary
sources. This method collects the emission sample isokinetically
and is therefore particularly suited for sampling at sources,
such as those controlled by wet scrubbers, emitting acid
particulate matter (e.g., hydrogen halides dissolved in water
droplets). [Note: Mention of trade names or specific products
does not constitute endorsement by the Environmental Protection
Agency.]
1.2 Principle. Gaseous and particulate pollutants are
withdrawn isokinetically from the source and collected in an
optional cyclone, on a filter, and in absorbing solutions. The
cyclone collects any liquid droplets and is not necessary if the
source emissions do not contain them; however, it is preferable
to include the cyclone in the sampling train to protect the
filter from any moisture present. The filter collects other
particulate matter including halide salts. Acidic and alkaline
-------
absorbing solutions collect the gaseous hydrogen halides and
halogens, respectively. Following sampling of emissions
containing liquid droplets, any halides/halogens dissolved in the
liquid in the cyclone and on the filter are vaporized to gas and
collected in the impingers by pulling conditioned ambient air
through the sampling train. The hydrogen halides are solubilized
in the acidic solution and form chloride (Cl') , bromide (Br') ,
and fluoride (F") ions. The halogens have a very low solubility
in the acidic solution and pass through to the alkaline solution
where they are hydrolyzed to form a proton (H+), the halide ion,
and the hypohalous acid (HC1O or HBrO). Sodium thiosulfate is
added to the alkaline solution to assure reaction with the
hypohalous acid to form a second halide ion such that 2 halide
ions are formed for each molecule of halogen gas. The halide ions
in the separate solutions are measured by ion chromatography
(1C). If desired, the particulate matter recovered from the
filter and the probe is analyzed following the procedures in
Method 5. [Note.- If the tester intends to use this sampling
arrangement to sample concurrently for particulate matter, the
alternative TeflonR probe liner, cyclone, and filter holder
should not be used. The TeflonR filter support must be used.
The tester must also meet the probe and filter temperature
requirements of both sampling trains.]
-------
1.3 Interferences. Volatile materials, such as chlorine
dioxide (C102) and ammonium chloride (NH4C1) , which produce
halide ions upon dissolution during sampling are potential
interferents. Interferents for the halide measurements are the
halogen gases which disproportionate to a hydrogen halide and an
hypohalous acid upon dissolution in water. The use of acidic
rather than neutral or basic solutions for collection of the
hydrogen halides greatly reduces the dissolution of any halogens
passing through this solution. The simultaneous presence of both
HBr and C12 may cause a positive bias in the HC1 result with a
corresponding negative bias in the C12 result as well as
affecting the HBr/Br2 split. High concentrations of nitrogen
oxides (NOX) may produce sufficient nitrate (NO3") to interfere
with measurements of very low Br~ levels.
1.4 Precision and Bias. The method has a possible
measurable negative bias below 20 ppm HC1 perhaps due to reaction
with small amounts of moisture in the probe and filter. Similar
bias for the other hydrogen halides is possible.
1.5 Sample Stability. The collected Cl' samples can be
stored for up to 4 weeks for analysis for HCl and C12-
1.6 Detection Limit. The in-stack detection limit for HCl
is approximately 0.02 /ig per liter of stack gas; the analytical
detection limit for HCl is 0.1 /zg/ml. Detection limits for the
-------
other analyses should be similar.
2. APPARATUS
2.1 Sampling. The sampling train is shown in Figure 26A-1;
the apparatus is similar to the Method 5 train where noted as
follows:
Teflon or Quartz
Filler
Dry Ou Vacuum
Meter Pump
Figure 26A-1. Sampling Train
-------
2.1.1 Probe Nozzle. Borosilicate or quartz glass;
constructed and calibrated according to Method 5, Sections 2.1.1
and 5.1, and coupled to the probe liner using a TeflonR union; a
stainless steel nut is recommended for this union. When the
stack temperature exceeds 210°C (410°F) , a one-piece glass
nozzle/liner assembly must be used.
2.1.2 Probe Liner. Same as Method 5, Section 2.1.2, except
metal liners shall not be used. Water-cooling of the stainless
steel sheath is recommended at temperatures exceeding 500°C.
TeflonR may be used in limited applications where the minimum
stack temperature exceeds 120 °C (250 °F) but never exceeds the
temperature where Teflon" is estimated to become unstable
(approximately 210 °C).
2.1.3 Pitot Tube, Differential Pressure Gauge, Filter
Heating System, Metering System, Barometer, Gas Density
Determination Equipment. Same as Method 5, Sections 2.1.3,
2.1.4, 2.1.6, 2.1.8, 2.1.9, and 2.1.10.
2.1.4 Cyclone (Optional). Glass or TeflonR . Use of the
cyclone is required only when the sample gas stream is saturated
with moisture; however, the cyclone is recommended to protect the
filter from any moisture droplets present.
2.1.5 Filter Holder. Borosilicate or quartz glass, or
-------
TeflonR filter holder, with a TeflonR filter support and a
sealing gasket. The sealing gasket shall be constructed of
TeflonR or equivalent materials. The holder design shall provide
a positive seal against leakage at any point along the filter
circumference. The holder shall be attached immediately to the
outlet of the cyclone.
2.1.6 Impinger Train. The following system shall be used
to determine the stack gas moisture content and to collect the
hydrogen halides and halogens: five or six impingers connected
in series with leak-free ground glass fittings or any similar
leak-free noncontaminating fittings. The first impinger shown in
Figure 26A-1 (knockout or condensate impinger) is optional and is
recommended as a water knockout trap for use under high moisture
conditions. If used, this impinger should be constructed as
described below for the alkaline impingers, but with a shortened
stem, and should contain 50 ml of 0.1 N H2S04. The following two
impingers (acid impingers which each contain 100 ml of 0.1 N
H2SO4) shall be of the Greenburg-Smith design with the standard
tip (Method 5, Section 2.1.7). The next two impingers (alkaline
impingers which each contain 100 ml of 0.1 N NaOH) and the last
impinger (containing silica gel) shall be of the modified
Greenburg-Smith design (Method 5, Section 2.1.7). The
condensate, acid, and alkaline impingers shall contain known
-------
quantities of the appropriate absorbing reagents. The last
impinger shall contain a known weight of silica gel or equivalent
desiccant. Teflon" impingers are an acceptable alternative.
2.1.7 Ambient Air Conditioning Tube (Optional). Tube
tightly packed with approximately 150 g of fresh 8 to 20 mesh
sodium hydroxide-coated silica, or equivalent, (Ascarite IIR has
been found suitable) to dry and remove acid gases from the
ambient air used to remove moisture from the filter and cyclone,
when the cyclone is used. The inlet and outlet ends of the tube
should be packed with at least 1-cm thickness of glass wool or
filter material suitable to prevent escape of fines. Fit one end
with flexible tubing, etc. to allow connection to probe nozzle
following the test run.
2.2 Sample Recovery. The following items are needed:
2.2.1 Probe-Liner and Probe-Nozzle Brushes, Wash Bottles,
Glass Sample Storage Containers, Petri Dishes, Graduated Cylinder
or Balance, and Rubber Policeman. Same as Method 5, Sections
2.2.1, 2.2.2, 2.2.3, 2.2.4, 2.2.5, and 2.2.7.
2.2.2 Plastic Storage Containers. Screw-cap polypropylene
or polyethylene containers to store silica gel. High-density
polyethylene bottles with Teflon screw cap liners to store
impinger reagents, 1-liter.
2.2.3 Funnels. Glass or high-density polyethylene, to aid
-------
in sample recovery.
2.3 Analysis. For analysis, the following equipment is
needed:
2.3.1 Volumetric Flasks. Class A, various sizes.
2.3.2 Volumetric Pipettes. Class A, assortment, to dilute
samples to calibration range of the ion chromatograph (1C).
2.3.3 Ion Chromatograph. Suppressed or nonsuppressed, with
a conductivity detector and electronic integrator operating in
the peak area mode. Other detectors, a strip chart recorder, and
peak heights may be used.
3. REAGENTS
Unless otherwise indicated, all reagents must conform to the
specifications of the Committee on Analytical Reagents of the
American Chemical Society (ACS reagent grade). When such
specifications are not available, the best available grade shall
be used.
3.1 Sampling.
3.1.1 Water. Deionized, distilled water that conforms to
American Society of Testing and Materials (ASTM) Specification D
1193-77, Type 3.
3.1.2 Acidic Absorbing Solution, 0.1 N Sulfuric Acid
(H2S04) . To prepare 1 L, slowly add 2.80 ml of concentrated H2SO4
to about 900 ml of water while stirring, and adjust the final
-------
volume to 1 L using additional water. Shake well to mix the
solution.
3.1.3 Alkaline Absorbing Solution, 0.1 N Sodium Hydroxide
(NaOH). To prepare 1 L, dissolve 4.00 g of solid NaOH in about
900 ml of water and adjust the final volume to 1 L using
additional water. Shake well to mix the solution.
3.1.4 Filter. Teflon" mat (e.g., PallflexR TX40HI45)
filter. When the stack gas temperature exceeds 210 °C (410 °F) a
quartz fiber filter may be used.
3.1.5 Silica Gel, Crushed Ice, and Stopcock Grease. Same
as Method 5, Sections 3.1.2, 3.1.4, and 3.1.5, respectively.
3.1.6 Sodium Thiosulfate, (Na2S2O33'5 H20) .
3.2 Sample Recovery.
3.2.1 Water. Same as Section 3.1.1.
3.2.2 Acetone. Same as Method 5, Section 3.2.
3.3 Sample Analysis.
3.3.1 Water. Same as Section 3.1.1.
3.3.2 Reagent Blanks. A separate blank solution of each
absorbing reagent should be prepared for analysis with the field
samples. Dilute 200 ml of each absorbing solution (250 ml of the
acidic absorbing solution, if a condensate impinger is used) to
the same final volume as the field samples using the blank sample
of rinse water. If a particulate determination is conducted,
-------
collect a blank sample of acetone.
3.3.3 Halide Salt Stock Standard Solutions. Prepare
concentrated stock solutions from reagent grade sodium chloride
(NaCl), sodium bromide (NaBr), and sodium fluoride (NaF). Each
must be dried at 110°C for 2 or more hours and then cooled to
room temperature in a desiccator immediately before weighing.
Accurately weigh 1.6 to 1.7 g of the dried NaCl to within 0.1 mg,
dissolve in water, and dilute to 1 liter. Calculate the exact
Cl~ concentration using Equation 26A-1.
j*g ClVml = g of NaCl x 103 x 35.453/58.44 Eq. 26A-1
In a similar manner, accurately weigh and solubilize 1.2 to 1.3 g
of dried NaBr and 2.2 to 2.3 g of NaF to make 1-liter solutions.
Use Equations 26A-2 and 26A-3 to calculate the Br" and F"
concentrations.
/ig BrVml = g of NaBr x 103 x 79.904/102.90 Eq. 26A-2
Hg F-/ml = g of NaF x 103 x 18.998/41.99 Eq. 26A-3
Alternately, solutions containing a nominal certified
concentration of 1000 mg/L NaCl are commercially available as
convenient stock solutions from which standards can be made by
appropriate volumetric dilution. Refrigerate the stock standard
solutions and store no longer than 1 month.
3.3.4 Chromatographic Eluent. Same as Method 26, Section
3.2.4.
-------
4. PROCEDURE
Because of the complexity of this method, testers and
analysts should be trained and experienced with the procedures to
ensure reliable results.
4.1 Sampling.
4.1.1 Pretest Preparation. Follow the general procedure
given in Method 5, Section 4.1.1, except the filter need only be
desiccated and weighed if a particulate determination will be
conducted.
4.1.2 Preliminary Determinations. Same as Method 5,
Section 4.1.2.
4.1.3 Preparation of Sampling Train. Follow the general
procedure given in Method 5, Section 4.1.3, except for the
following variations:
Add 50 ml of 0.1 N H2S04 to the condensate impinger, if
used. Place 100 ml of 0.1 N H2S04 in each of the next two
impingers. Place 100 ml of 0.1 N NaOH in each of the following
two impingers. Finally, transfer approximately 200-300 g of
preweighed silica gel from its container to the last impinger.
Set up the train as in Figure 26A-1. When used, the optional
cyclone is inserted between the probe liner and filter holder and
located in the heated filter box.
4.1.4 Leak-Check Procedures. Follow the leak-check
-------
procedures given in Method 5, Sections 4.4.1 (Pretest Leak-
Check), 4.1.4.2 (Leak-Checks During the Sample Run), and 4.1.4.3
(Post-Test Leak-Check).
4.1.5 Train Operation. Follow the general procedure given
in Method 5, Section 4.1.5. Maintain a temperature around the
filter and (cyclone, if used) of greater than 120 °C (248 °F) .
For each run, record the data required on a data sheet such as
the one shown in Method 5, Figure 5-2. If the condensate
impinger becomes too full, it may be emptied, recharged with
50 ml of 0.1 N H2S04, and replaced during the sample run. The
condensate emptied must be saved and included in the measurement
of the volume of moisture collected and included in the sample
for analysis. The additional 50 ml of absorbing reagent must
also be considered in calculating the moisture. After the
impinger is reinstalled in the train, conduct a leak-check as
described in Method 5, Section 4.1.4.2.
4.1.6 Post-Test Moisture Removal (Optional). When the
optional cyclone is included in the sampling train or when
moisture is visible on the filter at the end of a sample run even
in the absence of a cyclone, perform the following procedure.
Upon completion of the test run, connect the ambient air
conditioning tube at the probe inlet and operate the train with
the filter heating system at least 120 °C (248 °F) at a low flow
-------
rate (e.g., AH = 1 in. H2O) to vaporize any liquid and hydrogen
halides in the cyclone or on the filter and pull them through the
train into the impingers. After 30 minutes, turn off the flow,
remove the conditioning tube, and examine the cyclone and filter
for any visible moisture. If moisture is visible, repeat this
step for 15 minutes and observe again. Keep repeating until the
cyclone is dry. [Note: It is critical that this is repeated
until the cyclone is completely dry.]
4.2 Sample Recovery. Allow the probe to cool. When the
probe can be handled safely, wipe off all the external surfaces
of the tip of the probe nozzle and place a cap loosely over the
tip. Do not cap the probe tip tightly while the sampling train
is cooling down because this will create a vacuum in the filter
holder, drawing water from the impingers into the holder. Before
moving the sampling train to the cleanup site, remove the probe,
wipe off any silicone grease, and cap the open outlet of the
impinger train, being careful not to lose any condensate that
might be present. Wipe off any silicone grease and cap the
filter or cyclone inlet. Remove the umbilical cord from the last
impinger and cap the impinger. If a flexible line is used
between the first impinger and the filter holder, disconnect it
at the filter holder and let any condensed water drain into the
first impinger. Wipe off any silicone grease and cap the filter
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holder outlet and the impinger inlet. Ground glass stoppers,
plastic caps, serum caps, TeflonR tape, ParafilmR, or aluminum
foil may be used to close these openings. Transfer the probe and
filter/impinger assembly to the cleanup area. This area should
be clean and protected from the weather to minimize sample
contamination or loss. Inspect the train prior to and during
disassembly and note any abnormal conditions. Treat samples as
follows:
4.2.1 Container No. 1 (Optional; Filter Catch for
Particulate Determination). Same as Method 5, Section 4.2,
Container No. 1.
4.2.2 Container No. 2 (Optional; Front-Half Rinse for
Particulate Determination). Same as Method 5, Section 4.2,
Container No. 2.
4.2.3 Container No. 3 (Knockout and Acid Impinger Catch for
Moisture and Hydrogen Halide Determination). Disconnect the
impingers. Measure the liquid in the acid and knockout impingers
to ±1 ml by using a graduated cylinder or by weighing it to ±0.5
g by using a balance. Record the volume or weight of liquid
present. This information is required to calculate the moisture
content of the effluent gas. Quantitatively transfer this liquid
to a leak-free sample storage container. Rinse these impingers
and connecting glassware including the back portion of the filter
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holder (and flexible tubing, if used) with water and add these
rinses to the storage container. Seal the container, shake to
mix, and label. The fluid level should be marked so that if any
sample is lost during transport, a correction proportional to the
lost volume can be applied. Retain rinse water and acidic
absorbing solution blanks and analyze with the samples.
4.2.4 Container No. 4 (Alkaline Impinger Catch for Halogen
and Moisture Determination). Measure and record the liquid in
the alkaline impingers as described in Section 4.2.3.
Quantitatively transfer this liquid to a leak-free sample storage
container. Rinse these two impingers and connecting glassware
with water and add these rinses to the container. Add 25 mg of
sodium thiosulfate per ppm halogen-dscm of stack gas sampled.
[Note: This amount of sodium thiosulfate includes a safety
factor of approximately 5 to assure complete reaction with the
hypohalous acid to form a second Cl~ ion in the alkaline
solution.] Seal the container, shake to mix, and label; mark
the fluid level. Retain alkaline absorbing solution blank and
analyze with the samples.
4.2.5 Container No. 5 (Silica Gel for Moisture
Determination). Same as Method 5, Section 4.2, Container No. 3.
4.2.6 Container Noe. 6 through 9 (Reagent Blanks). Save
portions of the absorbing reagents (0.1 N H2S04 and 0.1 N NaOH)
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equivalent to the amount used in the sampling train; dilute to
the approximate volume of the corresponding samples using rinse
water directly from the wash bottle being used. Add the same
ratio of sodium thiosulfate solution used in container No. 4 to
the 0.1 N NaOH absorbing reagent blank. Also, save a portion of
the rinse water alone and a portion of the acetone equivalent to
the amount used to rinse the front half of the sampling train.
Place each in a separate, prelabeled sample container.
4.2.7 Prior to shipment, recheck all sample containers to
ensure that the caps are well-secured. Seal the lids of all
containers around the circumference with Teflon" tape. Ship all
liquid samples upright and all particulate filters with the
particulate catch facing upward.
4»3 Sample Preparation and Analysis. Note the liquid
levels in the sample containers and confirm on the analysis sheet
whether or not leakage occurred during transport. If a
noticeable leakage has occurred, either void the sample or use
methods, subject to the approval of the Administrator, to correct
the final results.
4.3.1 Container Nos. 1 and 2 and Acetone Blank (Optional;
Particulate Determination). Same as Method 5, Section 4.3.
4.3.2 Container No. 5. Same as Method 5, Section 4.3 for
silica gel.
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4.3.3 Container Nos. 3 and 4 and Absorbing Solution and
Water Blanks. Quantitatively transfer each sample to a
volumetric flask or graduated cylinder and dilute with water to a
final volume within 50 ml of the largest sample.
4.3.3.1 The 1C conditions will depend upon analytical
column type and whether suppressed or nonsuppressed 1C is used.
Prior to calibration and sample analysis, establish a stable
baseline. Next, inject a sample of water, and determine if any
Cl", Br~, or F" appears in the chromatogram. If any of these ions
are present, repeat the load/injection procedure until they are
no longer present. Analysis of the acid and alkaline absorbing
solution samples requires separate standard calibration curves;
prepare each according to Section 5.2. Ensure adequate baseline
separation of the analyses.
4.3.3.2 Between injections of the appropriate series of
calibration standards, inject in duplicate the reagent blanks and
the field samples. Measure the areas or heights of the Cl", Br~,
and F~ peaks. Use the average response to determine the
concentrations of the field samples and reagent blanks using the
linear calibration curve. If the values from duplicate
injections are not within 5 percent of their mean, the duplicate
injection shall be repeated and all four values used to determine
the average response. Dilute any sample and the blank with equal
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volumes of water if the concentration exceeds that of the highest
standard.
4.4 Audit Sample Analysis. Audit samples must be analyzed
subject to availability.
5. CALIBRATION
Maintain a laboratory log of all calibrations.
5.1 Probe Nozzle, Pitot Tube, Dry Gas Metering System,
Probe Heater, Temperature Gauges, Leak-Check of Metering System,
and Barometer. Same as Method 5, Sections 5.1, 5.2, 5.3, 5.4,
5.5, 5.6, and 5.7, respectively.
5.2 Ion Chromatograph. To prepare the calibration
standards, dilute given amounts (1.0 ml or greater) of the stock
standard solutions to convenient volumes, using 0.1 N H2SO4 or
0.1 N NaOH, as appropriate. Prepare at least four calibration
standards for each absorbing reagent containing the three stock
solutions such that they are within the linear range of the field
samples. Using one of the standards in each series, ensure
adequate baseline separation for the peaks of interest. Inject
the appropriate series of calibration standards, starting with
the lowest concentration standard first both before and after
injection of the quality control check sample, reagent blanks,
and field samples. This allows compensation for any instrument
drift occurring during sample analysis. Determine the peak
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areas, or height, of the standards and plot individual values
versus halide ion concentrations in jig/ml. Draw a smooth curve
through the points. Use linear regression to calculate a formula
describing the resulting linear curve.
6. QUALITY CONTROL
Same as Method 5, Section 4.4.
7. QUALITY ASSURANCE
7.1 Applicability. When the method is used to demonstrate
compliance with a regulation, a set of two audit samples shall be
analyzed.
7.2 Audit Procedure. The currently available audit samples
are chloride solutions. Concurrently analyze the two audit
samples and a set of compliance samples in the same manner to
evaluate the technique of the analyst and the standards
preparation. The same analyst, analytical reagents, and
analytical system shall be used both for compliance samples and
the Environmental Protection Agency (EPA) audit samples.
7.3 Audit Sample Availability. Audit samples will be
supplied only to enforcement agencies for compliance tests.
Audit samples may be obtained by writing the Source Test Audit
Coordinator (MD-77B), Quality Assurance Division, Atmospheric
Research and Exposure Assessment Laboratory, U.S. Environmental
Protection Laboratory, Research Triangle Park, NC 27711 or by
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calling the Source Test Audit Coordinator (STAC) at
(919) 541-7834. The request for the audit samples should be made
at least 30 days prior to the scheduled compliance sample
analysis.
7.4 Audit Results. Calculate the concentrations in mg/dscm
using the specified sample volume in the audit instructions.
Include the results of both audit samples, their identification
numbers, and the analyst's name with the results of the
compliance determination samples in appropriate reports to the
EPA regional office or the appropriate enforcement agency.
(NOTE: Acceptability of results may be obtained immediately by
reporting the audit results in mg/dscm and compliance results in
total ^ig HCl/sample to the responsible enforcement agency.) The
concentrations of the audit samples obtained by the analyst shall
agree within 10 percent of the actual concentrations. If the
10 percent specification is not met, reanalyze the compliance
samples and audit samples, and include initial and reanalysis
values in the test report. Failure to meet the 10 percent
specification may require retests until the audit problems are
resolved.
8. CALCULATIONS
Retain at least one extra decimal figure beyond those
contained in the available data in intermediate calculations, and
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round off only the final answer appropriately.
8.1 Nomenclature. Same as Method 5, Section 6.1. In
addition :
1 Bx- = Mass concentration of applicable absorbing
solution blank, ng halide ion (Cl~, Br", F')/ml,
not to exceed 1 /zg/ml which is 10 times the
published analytical detection limit of 0.1 /xg/ml
(It is also approximately 5 percent of the mass
concentration anticipated to result from a one
hour sample at 10 ppmv HCl . )
C = Concentration of hydrogen halide (HX) or halogen
(X2) , dry basis, mg/dscm.
mjjx = Mass of HCl, HBr, or HF in sample, ug.
mX2 = Mass of C12 or Br2 in sample, ug .
Sx- = Analysis of sample, ug halide ion (Cl~, Br", F"
Vs = Volume of filtered and diluted sample, ml.
8.2 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. See data sheet (Figure 5-2 of Method 5) .
8.3 Dry Gas Volume. Calculate Vn(Btd) and adjust for
leakage, if necessary, using the equation in Section 6.3 of
Method 5.
8.4 Volume of Water Vapor and Moisture Content. Calculate
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the volume of water vapor Vw(std) and moisture content Bws from the
data obtained in this method (Figure 5-2 of Method 5); use
Equations 5-2 and 5-3 of Method 5.
8.5 Isokinetic Variation and Acceptable Results. Use
Method 5, Sections 6.11 and 6.12.
8.6 Acetone Blank Concentration, Acetone Wash Blank Residue
Weight, Particulate Weight, and Particulate Concentration. For
particulate determination.
8.7 Total jig HC1, HBr, or HF Per Sample.
TCHX = K Vs (Sx- - Bx.) Eq. 26A-4
where: KHC1 = 1.028 (/ig HCl/Vg-mole) / (/xg Cl~/ng-mole) .
IW = 1.013 (/xg HBr//xg-mole)/ (/ig Br-//*g-mole) .
KHF = 1.053 (jug HF//Kj-mole) / (/ig F-/ng-moIe) .
8.8 Total ng C12 or Br2 Per Sample.
mX2 = Vs (Sx- - Bx-) Eq. 26A-5
8.9 Concentration of Hydrogen Halide or Halogen in Flue
Gas.
C = K itW^/V^sta, Eq. 26A-6
where: K = 10'3 mg//xg
8.10 Stack Gas Velocity and Volumetric Flow Rate.
Calculate the average stack gas velocity and volumetric flow
rate, if needed, using data obtained in this method and the
equations in Sections 5.2 and 5.3 of Method 2.
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9. BIBLIOGRAPHY
1. Steinsberger, S. C. and J. H. Margeson. Laboratory and
Field Evaluation of a Methodology for Determination of Hydrogen
Chloride Emissions from Municipal and Hazardous Waste
Incinerators. U.S. Environmental Protection Agency, Office of
Research and Development. Publication No. 600/3-89/064.
April 1989. Available from National Technical Information
Service, Springfield, VA 22161 as PB89220586/AS.
2. State of California Air Resources Board. Method 421 -
Determination of Hydrochloric Acid Emissions from Stationary
Sources. March 18, 1987.
3. Cheney, J.L. and C.R. Fortune. Improvements in the
Methodology for Measuring Hydrochloric Acid in Combustion Source
Emissions. J. Environ. Sci. Health. A19_{3): 337-350. 1984.
4. Stern, D.A., B.M. Myatt, J.F. Lachowski, and K.T.
McGregor. Speciation of Halogen and Hydrogen Halide Compounds in
Gaseous Emissions. In: Incineration and Treatment of Hazardous
Waste: Proceedings of the 9th Annual Research Symposium,
Cincinnati, Ohio, May 2-4, 1983. Publication No. 600/9-84-015.
July 1984. Available from National Technical Information
Service, Springfield, VA 22161 as PB84-234525.
5. Holm, R.D. and S.A. Barksdale. Analysis of Anions in
Combustion Products. In: Ion Chromatographic Analysis of
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Environmental Pollutants, E. Sawicki, J.D. Mulik, and
E. Wittgenstein (eds.). Ann Arbor, Michigan, Ann Arbor Science
Publishers. 1978. pp. 99-110.
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Appendix G.8
EPA Proposed Method 322
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(PROPOSED) TEST METHOD 322 - MEASUREMENT OF HYDROGEN CHLORIDE
EMISSIONS FROM PORTLAND CEMENT KILNS BY GFCIR
1.0 Applicability and Principle
1.1 Applicability. This method is applicable to the
determination of hydrogen chloride (HC1) concentrations in
emissions from portland cement kilns. This is an instrumental
method for the measurement of HC1 using an extractive sampling
system and an infrared (IR) gas-filter correlation (GFC)
analyzer. This method is intended to provide the cement industry
with a direct interface instrumental method. A procedure for
analyte spiking is included for quality assurance. This method
is considered to be self-validating provided that the
requirements in section 9 of this method are followed.
1.2 Principle. A gas sample is continuously extracted from
a stack or duct over the test period using either a source-level
hot/wet extractive subsystem or a dilution extractive subsystem.
A nondispersive infrared gas filter correlation (NDIR-GFC)
analyzer is specified for the measurement of HC1 in the sample.
The total measurement system is comprised of the extractive
subsystem, the analyzer, and the data acquisition subsystem.
Test system performance specifications are included in this
method to provide for the collection of accurate, reproducible
data.
1.3 Test System Operating Range. The measurement range
(span) of the test system shall include the anticipated HC1
concentrations of the effluent and spiked samples. The range
should be selected so that the average of the effluent
measurements is between 25 and 75 percent of span. If at any
time during a test run, the effluent concentration exceeds the
span value of the test system, the run shall be considered
invalid.
2.0 Summary of Method
2.1 Sampling and Analysis. Kiln gas is continuously
extracted from the stack or duct using either a source level,
hot/wet extractive system, or an in-situ dilution probe or heated
out-of-stack dilution system. The sample is then directed by a
heated sample line maintained above 350°F to a GFC analyzer
having a range appropriate to the type of sampling system. The
gas filter correlation analyzer incorporates a gas cell filled
with HC1. This gas cell is periodically moved into the path of
an infrared measurement beam of the instrument to filter out
essentially all of the HC1 absorption wavelengths. Spectral
filtering provides a reference from which the HC1 concentration
of the sample can be determined. Interferences are minimized in
the. analyzer by choosing a spectral band over which compounds
such as CO2 and H2O either do not absorb significantly or do not
match the spectral pattern of the HC1 infrared absorption.
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2.2 Operator Requirements. The analyst must be familiar
with the specifications and test procedures of this method and
follow them in order to obtain reproducible and accurate data.
3.0 Definitions
3.1 Measurement System. The total equipment required for
the determination of gas concentration. The measurement system
consists of the following major subsystems:
3.1.1 Sample Interface. That portion of a system used for
one or more of the following: sample acquisition, sample
transport, sample conditioning, or protection of the analyzers
from the effects of the stack gas.
3.1.2 Gas Analyzer. That portion of the system that senses
the gas to be measured and generates an output proportional to
its concentration.
3.1.3 Data Recorder. A strip chart recorder, analog
computer, or digital recorder for recording measurement data from
the analyzer output.
3.2 Span. The upper limit of the gas concentration
measurement range displayed on the data recorder.
3.3 Calibration Gas. A known concentration of a gas in an
appropriate, diluent gas (i.e., N2) .
3.4 Analyzer Calibration Error. .The difference between the
gas concentration exhibited by the gas analyzer and the known
concentration of the calibration gas when the calibration gas is
introduced directly to the analyzer.
3.5 Sampling System Bias. The sampling system bias is the
difference between the gas concentrations exhibited by the
measurement system when a known concentration gas is introduced
at the outlet of the sampling probe and the known value of the
calibration gas.
3.6 Response Time. The amount of time required for the
measurement system to display 95 percent of a step change in gas
concentration on the data recorder.
3.7 Calibration Curve. A graph or other systematic method
of establishing the relationship between the analyzer response '
and the actual gas concentration introduced to the analyzer.
3.8 Linearity. The linear response of the analyzer or test
system to known calibration inputs covering the concentration
range of the system.
3.9 Interference Rejection. The ability of the system to
reject the effect of interferences in the analytical measurement
processes of the test system.
4.0 Interferences
4.1 Sampling System Interferences. An important
consideration in measuring HC1 using an extractive measurement
system is to ensure that a representative kiln gas sample is
delivered to the gas analyzer. A sampling system interferant is
a factor that inhibits an analyte from reaching the analytical
instrumentation. Condensed water vapor is a strong sampling
system interferant for HC1 and other water soluble compounds.
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"Cold spots" in the sampling system can allow water vapor in the
sample to condense resulting in removal of HC1 from the sample
stream. The extent of HC1 sampling system bias depends on
concentrations of potential interferants, moisture content of the
gas stream, temperature of the gas stream, temperature of
sampling system components, sample flow rate, and reactivity of
HC1 with other species in the gas stream. For measuring HC1 in a
wet gas stream, the temperatures of the gas stream and sampling
system components and the sample flow rate are of primary
importance. In order to prevent problems with condensation in
the sampling system, these parameters must be closely monitored.
4.1.1 System Calibration Checks. Performing these
calibration checks where HC1 calibration gas is injected through
the entire system both before and after each test run
demonstrates the integrity of the sampling system and capability
of the analyzer for measuring this water soluble and otherwise
unstable compound under ideal conditions (i.e., HC1 in N2) .
4.1.2 Analyte Spiking Checks. For analyte spiking checks,
HC1 calibration gas is quantitatively added to the sample stream
at a point upstream of the particulate filter and all other
sample handling components both before and after each test run.
The volume of HC1 spike gas should not exceed 10 percent of the
total sample volume so that the sample matrix is relatively
unaffected. Successfully performing these checks demonstrates
the integrity of the sampling system for measuring this water
soluble and reactive compound under actual sample matrix
conditions. Successfully performing these checks also
demonstrates the adequacy of the interference rejection
capability of the analyzer. (See section 9.3 of this method.)
4.2 Analytical Interferences. Analytical interferences are
reduced by the GFC spectroscopic technique required by the
method. The accuracy of HC1 measurements provided by some GFC
analyzers is known to be sensitive to the moisture content of the
sample. This must be taken into account in order to acquire
accurate results. These analyzers must be calibrated for the
specific moisture content of the samples.
5.0 Safety
This method may involve sampling at locations having high
positive or negative pressures, or high concentrations of
hazardous or toxic pollutants, and cannot address all safety
problems encountered under these diverse sampling conditions. It
is the responsibility of the tester (s) to ensure proper safety
and health practices, and to determine the applicability of
regulatory limitations before performing this test method.
Because HC1 is a respiratory irritant, it is advisable to limit
exposure to this compound.
6.0. Equipment and Supplies
Note: Mention of company or product names does not
constitute endorsement by the U. S. Environmental Protection
Agency.
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6.1 Measurement System. Use any GFC measurement system for
HC1 that meets the specifications of this method. All sampling
system components must be maintained above the kiln gas
temperature, when possible, or at least 350°F. The length of
sample transport line should be minimized and sampling rate
should be as high as possible to minimize adsorption of HC1. The
essential components of the measurement system are described in
sections 6.1.1 through 6.1.12.
6.1.1 Sample Probe. Glass, stainless steel, Hastalloy1*, or
equivalent, of sufficient length to traverse the sample points.
The sampling probe shall be heated to a minimum of 350°F to
prevent condensation. Dilution extractive systems must use a
dilution ratio such that the average diluted concentrations are
between 25 to 75 percent of the selected measurement range of the
analyzer.
6.1.2 Calibration Valve Assembly. Use a heated, three-way
valve assembly, or equivalent, for selecting either sample gas or
introducing calibration gases to the measurement system or
introducing analyte spikes into the measurement system at the
outlet of the sampling probe before the primary particulate
filter.
6.1.3 Particulate Filter. A coarse filter or other device
may be placed at the inlet of the probe for removal of large
particulate (10 microns or greater). A heated (Balston® or
equivalent) filter rated at 1 micron is necessary for primary
particulate removal, and shall be placed immediately after the
heated probe. The filter/filter holder shall be maintained at
350°F or a higher temperature. Additional filters at the inlet
of the gas analyzer may be used to prevent accumulation of
particulate material in the measurement system and extend the
useful life of components. All filters shall be fabricated of
materials that are nonreactive with HC1. Some types of glass
filters are known to react with HC1.
6.1.4 Sample Transport Lines. Stainless steel or
polytetrafluoroethylene (PTFE) tubing shall be heated to a
minimum temperature of 350°F (sufficient to prevent condensation
and to prevent HC1 and NH3 from combining into ammonium chloride
in the sampling system)-to transport the sample gas to the gas
analyzer.
6.1.5 Sample Pump. Use a leak-free pump to pull the sample
gas through the system at a flow rate sufficient to minimize the
response time of the measurement system. The pump components
that contact the sample must be heated to a temperature greater
than 350°F and must be constructed of a material that is
nonreactive to HC1.
6.1.6 Sample Flow Rate Control. A sample flow rate control
valve and rotameter, or equivalent, must be used to maintain a
constant sampling rate within ±10 percent. These components must
be heated to a temperature greater than 350°F. (Note: The
tester may elect to install a back-pressure regulator to maintain
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the sample gas manifold at a constant pressure in order to
protect the analyzer(s) from over-pressurization, and to minimize
the need for flow rate adjustments.)
6.1.7 Sample Gas Manifold. A sample gas manifold, heated
to a minimum of 350°F, is used to divert a portion of the sample
gas stream to the analyzer and the remainder to the by-pass
discharge vent. The sample gas manifold should also include
provisions for introducing calibration gases directly to the
analyzer. The manifold must be constructed of material that is
nonreactive to the gas being sampled.
6.1.8 Gas Analyzer. Use a nondispersive infrared analyzer
utilizing the gas filter correlation technique to determine HC1
concentrations. The analyzer shall meet the applicable
performance specifications of section 8.0 of this method. (Note:
Housing the analyzer in a clean, thermally-stable, vibration free
environment will minimize drift in the analyzer calibration.)
The analyzer (system) shall be designed so that the response of a
known calibration input shall not deviate by more than ±3 percent
from the expected value. The analyzer or measurement system
manufacturer may provide documentation that the instrument meets
this design requirement. Alternatively, a known concentration
gas standard and calibration dilution system meeting the
requirements of Method 205 of appendix M to part 51 of this
chapter, "Verification of Gas Dilution Systems for Field
Calibrations" (or equivalent procedure), may be used to develop a
multi-point calibration curve over the measurement range of the
analyzer.
6.1.9 Gas Regulators. Single stage regulator with cross
purge assembly that is used to purge the CGA fitting and
regulator before and after use. (This purge is necessary to
clear the calibration gas delivery system of ambient water vapor
after the initial connection is made, or after cylinder
changeover, and will extend the life of the regulator.) Wetted
parts are 316 stainless steel to handle corrosive gases.
6.1.10 Data Recorder. A strip chart recorder, analog
computer, or digital recorder, for recording measurement data.
The data recorder resolution (i.e., readability) shall be 0.5
percent of span. Alternatively, a digital or analog meter having
a resolution of 0.5 percent of span may be used to obtain the
analyzer responses and the readings may be recorded manually. If
this alternative is used, the readings shall be obtained at
equally-spaced intervals over the duration of the sampling run.
For sampling run durations of less than 1 hour, measurements at
1-minute intervals or a minimum of 30 measurements, whichever is
less restrictive, shall be obtained. For sampling run durations
greater than 1 hour, measurements at 2-minute intervals or a
minimum of 96 measurements, whichever is less restrictive, shall
be obtained.
6.1.11 Mass Flow Meters/Controllers. A mass flow meter
having the appropriate calibrated range and a stated accuracy of
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±2 percent of the measurement range is used to measure the HC1
spike flow rate. This device must be calibrated with the major
component of the calibration spike gas (e.g., nitrogen) using an
NIST traceable bubble meter or equivalent. When spiking HC1,. the
mass flow meter/controller should be thoroughly purged before and
after introduction of the gas to prevent corrosion of the
interior parts.
6.1.12 System Flow Measurement. A measurement device or
procedure to determine the total flow rate of sample gas within
the measurement system. A rotameter, or mass flow meter
calibrated relative to a laboratory standard to within ±2 percent
of the measurement value at the actual operating temperature,
moisture content, and sample composition (molecular weight) is
acceptable. A system which ensures that the total sample flow
rate is constant within ±2 percent and which relies on an
intermittent measurement of the actual flow rate
(e.g., calibrated gas meter) is also acceptable.
6.2 HC1 Calibration Gases. The calibration gases for the
gas analyzer shall be HC1 in N2. Use at least three calibration
gases as specified below:
6.2.1 High-Range Gas. Concentration equivalent to 80 to
100 percent of the span.
6.2.2 Mid-Range Gas. Concentration equivalent to 40 to 60
percent of the span.
6.2.3 Zero Gas. Concentration of less than 0.25 percent of
the span. Purified ambient air may be used for the zero gas by
passing air through a charcoal filter or through one or more
impingers containing a solution of 3 percent H2O2.
6.2.4 Spike Gas. A calibration gas of known concentration
(typically 100 to 200 ppm) used for analyte spikes in accordance
with the requirements of section 9.3 of this method.
7.0 Reagents and Standards
7.1 Hydrogen Chloride. Hydrogen Chloride is a reactive gas
and is available in steel cylinders from various commercial gas
vendors. The stability is such that it .is not possible to
purchase a cylinder mixture whose HC1 concentration can be
certified at better than ±5 percent. The stability of the
cylinder may be monitored over time by periodically analyzing
cylinder samples. The cylinder gas concentration must be
verified within 1 month prior to the use of the calibration gas.
Due to the relatively high uncertainty of HC1 calibration gas
values, difficulties may develop in meeting the performance
specifications if the mid-range and high-range calibration gases
are not consistent with each other. Where problems are
encountered, the consistency of the test gas standards may be
determined: (1) by comparing analyzer responses for the test
gases with the responses to additional certified calibration gas
standards, (2) by reanalysis of the calibration gases in
accordance with sections 7.2.1 or 7.2.2 of this method, or (3) by
other procedures subject to the approval of EPA.
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7.2 Calibration Gas Concentration Verification. There are
two alternatives for establishing the concentrations of
calibration gases. Alternative No. 1 is preferred.
7.2.1 Alternative No. 1. The value of the calibration
gases may be obtained from the vendor's certified analysis within
1 month prior to the test. Obtain a certification from the gas
manufacturer that identifies the analytical procedures and date
of certification.
7.2.2 Alternative No. 2. Perform triplicate analyses of
the gases using Method 26 of appendix A to part 60 of this
chapter. Obtain gas mixtures with a manufacturer's tolerance not
to exceed ±5 percent of the tag value. Within 1 month of the
field test, analyze each of the calibration gases in triplicate
using Method 26 of appendix A to part 60 of this chapter. The
tester must follow all of the procedures in Method 26 (e.g., use
midget impingers, heated Pallflex TX40H175 filter (TFE-glass
mat), etc. if this analysis is performed. Citation 3 in section
13 of this method describes procedures and techniques that may be
used for this analysis. Record the results on a data sheet.
Each of the individual HC1 analytical results for each
calibration gas shall be within 5 percent (or 5 ppm, whichever is
greater) of the triplicate set average; otherwise, discard the
entire set and repeat the triplicate analyses. If the average of
the triplicate analyses is within 5 percent of the calibration
gas manufacturer's cylinder tag value, use the tag value/-
otherwise, conduct at least three additional analyses until the
results of six consecutive runs agree within 5 percent (or 5 ppm,
whichever is greater) of the average. Then use this average for
the cylinder value.
7.3 Calibration Gas Dilution Systems. Sample flow rates of"
approximately 15 L/min are typical for extractive HC1 measurement
systems. These flow rates coupled with response times of 15 to
30 minutes will result in consumption of large quantities of
calibration gases. The number of cylinders and amount of
calibration gas can be reduced by the use of a calibration gas
dilution system in accordance with Method 205 of appendix M to
part 51 of this chapter, "Verification of Gas Dilution Systems
for Field Instrument Calibrations." If this option is used, the
tester shall also introduce an undiluted calibration gas
approximating the effluent HC1 concentration during the initial
calibration error test of the measurement system as a quality
assurance check.
8.0 Test System Performance Specifications
8.1 Analyzer Calibration Error. This error shall be less
than ±5 percent of the emission standard concentration or ±1
ppm,(whichever is greater) for zero, mid-, and high-range gases.
. 8.2 Sampling System Bias. This bias shall be less than
±7.5 percent of the emission standard concentration or ±1.5 ppm
(whichever is greater) for zero and mid-range gases.
8.3 Analyte Spike Recovery. This recovery shall be between
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70 to 130 percent of the expected concentration of spiked samples
calculated with the average of the before and after run spikes.
9.0 Sample Collection, Preservation, and Storage
9.1 Pretest. Perform the procedures of sections 9.1.1.
through 9.1.3.3 of this method before measurement of emissions
(procedures in section 9.2 of this method). It is important to
note that after a regulator is placed on an HC1 gas cylinder
valve, the regulator should be purged with dry N2 or dry
compressed air for approximately 10 minutes before initiating any
HC1 gas flow through the system. This purge is necessary to
remove any ambient water vapor from within the regulator and
calibration gas transport lines; the HC1 in the calibration gas
may react with this water vapor and increase system response
time. A purge of the system should also be performed at the
conclusion of a test day prior to removing the regulator from the
gas cylinder. Although the regulator wetted parts are corrosion
resistant, this will reduce the possibility of corrosion
developing within the regulator and extend the life of the
equipment.
9.1.1 Measurement System Preparation. Assemble the
measurement system by following the manufacturer's written
instructions for preparing and preconditioning the gas analyzer
and, as applicable, the other system components. Introduce the
calibration gases in any sequence, and make all necessary
adjustments to calibrate the analyzer and the data recorder. If
necessary, adjust the instrument for the specific moisture
content of the samples. Adjust system components to achieve
correct sampling rates.
9.1.2 Analyzer Calibration Error. Conduct the analyzer
calibration error check in the field by introducing calibration
gases to the measurement system at any point upstream of the gas
analyzer in accordance with sections 9.1.2.1 and 9.1.2.2 of this
method.
9.1.2.1 After the measurement system has been prepared for
use, introduce the zero, mid-range, and -high-range gases to the
analyzer. During this check, make no adjustments to the system
except those necessary to achieve the correct calibration gas
flow rate at the analyzer. Record the analyzer responses to each
calibration gas. Note: A calibration curve established prior to
the analyzer calibration error check may be used to convert the
analyzer response to the equivalent gas concentration introduced
to the analyzer. However, the same correction procedure shall be
used for all effluent and calibration measurements obtained
during the test.
9.1.2.2 The analyzer calibration error check shall be
considered invalid if the difference in gas concentration
displayed by the analyzer and the concentration of the
calibration gas exceed? ±5 percent of the emission standard
concentration or ±1 ppm, (whichever is greater) for the zero,
mid-, or high-range calibration gases. If an invalid calibration
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is exhibited, cross-check or recertify the calibration gases/
take corrective action, and repeat the analyzer calibration error
check until acceptable performance is achieved.
9.1.3 Sampling System Bias Check. For nondilution
extractive systems, perform the sampling system bias check by
introducing calibration gases either at the probe inlet or at a
calibration valve installed at the outlet of the sampling probe.
For dilution systems, calibration gases for both the analyzer
calibration error check and the sampling system bias check must
be introduced prior to the point of sample dilution. For
dilution and nondilution systems, a zero gas and either a mid-
range or high-range gas (whichever more closely approximates the
effluent concentration) shall be used for the sampling system
bias check.
9.1.3.1 Introduce the upscale calibration gas, and record
the gas concentration displayed by the analyzer. Then introduce
zero gas, and record the gas concentration displayed by the
analyzer. During the sampling system bias check, operate the
system at the normal sampling rate, and make no adjustments to
the measurement system other than those necessary to achieve
proper calibration gas flow rates at the analyzer. Alternately
introduce the zero and upscale gases until a stable response is
achieved. The tester shall determine the measurement system
response time by observing the times required to achieve a stable
response for both the zero and upscale gases. Note the longer of
the two times and note the time required for the measurement
system to reach 95 percent of the step change in the effluent
concentration as the response time.
9.1.3.2 For nondilution systems, where the analyzer
calibration error test is performed by introducing gases directly
to the analyzer, the sampling system bias check shall be
considered invalid if the difference between the gas
concentrations displayed by the measurement system for the
sampling system bias check and the known gas concentration
standard exceeds ±7.5 percent of the emission standard or ±1.5
ppm, (whichever is greater) for either the zero or the upscale
calibration gases. If an invalid calibration is exhibited, take
corrective action, and repeat the sampling system bias check
until acceptable performance is achieved. If adjustment to the
analyzer is required, first repeat the analyzer calibration error
check, then repeat the sampling system bias check.
9.1.3.3 For dilution systems (and nondilution systems where
all calibration gases are introduced at the probe), the
comparison of the analyzer calibration error results and sampling
system bias check results is not meaningful. For these systems,
the sampling system bias check shall be considered invalid if the
difference between the gas concentrations displayed by the
analyzer and the actual gas concentrations exceed ±7.5 percent of
the emission standard or ±1.5 ppm, (whichever is greater) for
either the zero or the upscale calibration gases. If an invalid
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calibration is exhibited, take corrective action, and repeat the
sampling system bias check until acceptable performance is
achieved. If adjustment to the analyzer is required, first
repeat the analyzer calibration error check.
9.2 Emission Test Procedures
9.2.1 Selection of Sampling Site and Sampling Points.
Select a measurement site and sampling points using the same
criteria that are applicable to Method 26 of appendix A to part
60 of this chapter.
9.2.2 Sample Collection. Position the sampling probe at
the first measurement point, and begin sampling at the same rate
as used during the sampling system bias check. Maintain constant
rate sampling (i.e., ±10 percent) during the entire run. Field
test experience has shown that conditioning of the sample system
is necessary for approximately 1-hour prior to conducting the
first sample run. This conditioning period should be repeated
after particulate filters are replaced and at the beginning of
each new day or following any period when the sampling system is
inoperative. Experience has also shown that prior to adequate
conditioning of the system, the response to analyte spikes and/or
the change from an upscale calibration-gas to a representative
effluent measurement may be delayed by more than twice the normal
measurement system response time. It is recommended that the
analyte spikes (see section 9.3 of this method) be performed to
determine if the system is adequately conditioned. The sampling
system is ready for use when the time required for the
measurement system to equilibrate after a change from a
representative effluent measurement to a representative spiked
sample measurement approximates the calibration gas response time
observed in section 9.1.3.1 of this method.
9.2.3 Sample Duration. After completing the sampling
system bias checks and analyte spikes prior to a test run,
constant rate sampling of the effluent should begin. For each
run, use only those measurements obtained after all residual
response to calibration standards or spikes are eliminated and
representative effluent measurements are displayed to determine
the average effluent concentration. At a minimum, this requires
that the response time of the measurement system has elapsed
before data are recorded for calculation of the average effluent
concentration. Sampling should be continuous for the duration of
the test run. The length of data collection should be at least
as long as required for sample collection by Method 26 of part 60
of this chapter. One hour sampling runs using this method have
provided reliable data for cement kilns.
9.2.4 Validation of Runs. Before and after each run, or if
adjustments are necessary for the measurement system during the
run, repeat the sampling system bias check procedure described in
section 9.1.3 of this method. (Make no adjustments to the
measurement system until after the drift checks are completed.)
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Record the analyzer's responses.
9.2.4.1 If the post-run sampling system bias for either the
zero or upscale calibration gas exceeds the sampling system bias
specification, then the run is considered invalid. Take
corrective action, and repeat both the analyzer calibration error
check procedure (section 9.1.2 of this method) and the sampling
system bias check procedure (section 9.1.3 of this method) before
repeating the run.
9.2.4.2 If the post-run sampling system bias for both the
zero and upscale calibration gas are within the sampling system
bias specification, then construct two 2-point straight lines,
one using the pre-run zero and upscale check values and the other
using the post-run zero and upscale check values. Use the slopes
and y-intercepts of the two lines to calculate the gas
concentration for the run in accordance with equation 1 of this
method.
9.3 Analyte Spiking—Self-Validating Procedure. Use analyte
spiking to verify the effectiveness of the sampling system for
the target compounds in the actual kiln gas matrix. Quality
assurance (QA) spiking should be performed before and after each
sample run. The spikes may be performed following the sampling
system bias checks (zero and mid-range system calibrations)
before each run in a series and also after the last run. The HC1
spike recovery should be within ±30 percent as calculated using
equations 1 and 2 of this method. Two general approaches are
applicable for the use of analyte spiking to validate a GFC HC1
measurement system: (I) two independent measurement systems can
be operated concurrently with analyte spikes introduced to one of
the systems, or (2) a single measurement system can be used to
analyze consecutively, spiked and unspiked samples in an
alternating fashion. The two-system approach is similar to
Method 301 of this appendix and the measurement bias is
determined from the difference in the paired concurrent
measurements relative to the amount of HC1 spike added to the
spiked system. The two-system approach must employ identical
sampling systems and analyzers and both measurement systems
should be calibrated using the same mid- and high-range
calibration standards. The two-system approach should be largely
unaffected by temporal variations in the effluent concentrations
if both measurement systems achieve the same calibration
responses and both systems have the same response times. (See
Method 301 of this appendix for appropriate calculation
procedures.) The single measurement system approach is
applicable when the concentration of HC1 in the source does not
vary substantially during the period of the test. Since the
approach depends on the comparison of consecutive spiked and
unspiked samples, temporal variations in the effluent HC1
concentrations will introduce errors in determining the expected
concentration of the spiked samples. If the effluent HC1
concentrations vary by more than ±10 percent (or ±5 ppm,
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whichever is greater) during the time required to obtain and
equilibrate a new sample (system response time), it may be
necessary to: (1) use a dual sampling system approach,
(2) postpone testing until stable emission concentrations are
achieved, (3) switch to the two-system approach [if possible] or,
(4) rely on alternative QA/QC procedures. The dual-sampling
system alternative uses two sampling lines to convey sample to
the gas distribution manifold. One of the sample lines is used
to continuously extract unspiked kiln gas from the source. The
other sample line serves as the analyte spike line. One GFC
analyzer can be used to alternately measure the HC1 concentration
from the two sampling systems with the need to purge only the
components between the common manifold and the analyzer. This
minimizes the time required to acquire an equilibrated sample of
spiked or unspiked kiln gas. If the source varies by more than
±10 percent or ±5 ppm, (whichever is greater) during the time it
takes to switch from the unspiked sample line to the spiked
sample line, then the dual-sampling system alternative approach
is not applicable. As a last option, (where no other
alternatives can be used) a humidified nitrogen stream may be
generated in the field which approximates the moisture content of
the kiln gas. Analyte spiking into this humidified stream can be
employed to assure that the sampling system is adequate for
transporting the HC1 to the GFC analyzer and that the analyzer's
water interference rejection is adequate.
9.3.1 Spike Gas Concentration and Spike Ratio. The volume
of HC1 spike gas should not exceed 10 percent of the total sample
volume (i.e., spike to total sample ratio of 1:10) to ensure that
the sample matrix is relatively unaffected. An ideal spike
concentration should approximate the native effluent
concentration, thus the spiked sample concentrations would
represent approximately twice the native effluent concentrations.
The ideal spike concentration may not be achieved because the
native HC1 concentration cannot be accurately predicted prior to
the field test, and limited calibration -gas standards will be
available during the field test. Some flexibility is available
by varying the spike ratio over the range from 1:10 to 1:20.
Practical constraints must be applied to allow the tester to
spike at an anticipated concentration. Thus, the tester may use
a 100 ppm calibration gas and a spike ratio of 1:10 as default
values where information regarding the expected HC1 effluent
concentration is not available prior to the tests.
Alternatively, the tester may select another calibration gas
standard and/or lower spike ratio (e.g., 1:20) to more closely
approximate the effluent HC1 concentration.
9.3.2 Spike Procedure. Introduce the HC1 spike gas mixture
at a constant flow rate (±2 percent) at less than 10 percent of
the total sample flow rate. (For example, introduce the HC1
spike gas at 1 L/min (±20 cc/min) into a total sample flow rate
of 10 L/min). The spike gas must be preheated before
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introduction into the sample matrix to prevent a localized
condensation of the gas stream at the spike introduction point.
A heated sample transport line(s) containing multiple transport
tubes within the heated bundle may be used to spike gas up
through the sampling system to the spike introduction point. Use
a calibrated flow device (e.g., mass flow meter/controller) to
monitor the spike flow rate. Use a calibrated flow device (e.g.,
rotameter, mass flow meter, orifice meter, or other method) to
monitor the total sample flow-rate. Calculate the spike ratio
from the measurements of spike flow and total flow. (See
equation 2 and 3 in section 10.2 of this method.)
9.3.3 Analyte Spiking. Determine the approximate effluent
HC1 concentrations by examination of preliminary samples. For
single-system approaches, determine whether the HC1 concentration
varies significantly with time by comparing consecutive samples
for the period of time corresponding to at least twice the system
response time. (For analyzers without sample averaging, estimate
average values for two to five minute periods by observing the
instrument display or data recorder output.) If the concentration
of the individual samples varies by more than ±10 percent
relative to the mean value or ±5 ppm, (whichever is greater), an
alternate approach may be needed.
9.3.3.1 Adjust the spike flow rate to the appropriate level
relative to the total flow by metering spike gas through a
calibrated mass flow meter or controller. Allow spike flow to
equilibrate within the sampling system for at least the
measurement system response time and a steady response to the
spike gas is observed before recording response to the spiked gas
sample. Next, terminate the spike gas flow and allow the
measurement system to sample only the effluent. After the
measurement system response time has elapsed and representative
effluent measurements are obtained, record the effluent unspiked
concentration. Immediately calculate the spike recovery.
9.3.3.2 If the spike recovery is not within acceptable
limits and a change in the effluent concentration is suspected as
the cause for exceeding the recovery limit, repeat the analyte
spike procedure without making any adjustments to the analyzer or
sampling system. If the second spike recovery falls within the
recovery limits, disregard the first attempt and record the
results of the second spike.
9.3:3.3 Analyte spikes must be performed before and after
each test run. Sampling system bias checks must also be
performed before and after each test run. Depending on the
particular sampling strategy and other constraints, it may be
necessary to compare effluent data either immediately before or
immediately after the spike sample to determine the spike
recovery. Either method is acceptable provided a consistent
approach is used for the test program. The average spike
recovery for the pre- and post-run spikes shall be used to
determine if spike recovery is between 70 and 130 percent.
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10.0 Data Analysis and Emission Calculations
The average gas effluent concentration is determined from
the average gas concentration displayed by the gas analyzer and
is adjusted for the zero and upscale sampling system bias checks,
as determined in accordance with section 9.2.3 of this method.
The average gas concentration displayed by the analyzer may be
determined by integration of the area under the curve for chart
recorders, or by averaging all of the effluent measurements.
Alternatively, the average may be calculated from measurements
recorded at equally spaced intervals over the entire duration of
the run. For sampling run durations of less than 1-hour, average
measurements at 2-minute intervals or less, shall be used. For
sampling run durations greater than 1-hour, measurements at 2-
minute intervals or a minimum of 96 measurements, whichever is
less restrictive, shall be used. Calculate the effluent gas
concentration using equation 1.
/U .U N
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QT = Total sample flow rate (effluent sample flow plus
spike flow).
S0 = Native concentration of HC1 in unspiked effluent
samples.
Acceptable recoveries for analyte spiking are ±30 percent.
11.0 Pollution Prevention
Gas extracted from the source and analyzed or vented from
the system manifold shall be either scrubbed, exhausted back into
the stack, or discharged into the atmosphere where suitable
dilution can occur to prevent harm to personnel health and
welfare or plant or personal property.
12.0 Waste Management
Gas standards of HC1 are handled as according to the
instructions enclosed with the materials safety data sheets.
13.0 References
1. Peeler, J.W., Summary Letter Report to Ann Dougherty,
Portland Cement Association, June 20, 1996.
2. Test Protocol, Determination of Hydrogen Chloride
Emissions from Cement Kilns (Instrumental Analyzer Procedure)
Revision 4; June 20, 1996.
3. Westlin, Peter R. and John W. Brown. Methods for
Collecting and Analyzing Gas Cylinder Samples. Source Evaluation
Society Newsletter. 3_(3):5-15. September 1978.
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1. REPORT NO.
EPA-454/R-00-015
4. TITLE AND SUBTITLE
Final Report
Manual Testing and Continuous Emissior
Lime Kiln No. 4 Baghouse Inlet and Stac
Dravo Lime Company
Saginaw, Alabama
TECHNICAL REPORT DATA
Please read instructions on the reverse before completing
2.
s Monitoring
k
7. AUTHOR(S)
Michael D. Maret
Franklin Meadows
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Pacific Environmental Services, Inc.
Post Office Box 12077
Research Triangle Park, North Carolina 27709-2077
12. SPONSORING AGENCY NAME AND ADDRESS
U.S Environmental Protection Agency
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Research Triangle Park, North Carolina 277 11
3. RECIPIENT'S ACCESSION NO.
5. REPORT DATE
April 2000
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D-98004
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
EPA/200/04
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The United States Environmental Protection Agency (EPA) Emission Standards Division (ESD) is investigating the lime manufacturing industry to
identify and quantify hazardous air pollutants (HAPs) emitted from lime kilns. ESD requested that EPA's Emissions, Monitoring and Analysis Division
(EMAD) conduct the required testing. EMAD issued a work assignment to Pacific Environmental Services, Inc. (PES) to conduct a screening test to
collect air emissions data as specified in the ESD test request. The primary objective of the testing program was to characterize HAP emissions from one
lime kiln at the Dravo Lime Company's facility located in Saginaw, Alabama. Based on the pollutant concentrations and emission rates calculated
from the results of the screening tests, the kiln may be selected by EPA for further testing.
The tests were conducted to quantify the uncontrolled and controlled air emissions of hydrogen chloride (HC1), total hydorcarbons (THC), and
polychlorinated dibenzo-p-dioxins and polyclorinated dibenzofurans (PCDDs/PCDFs). Emissions from the kiln were controlled by a baghouse. Testing
was conducted at the baghouse inlet and at the stack. Inlet and stack runs were conducted simultaneously. Oxygen (OJ and carbon dioxide (CO2) were
also monitored at each location.
During the testing program another EPA contractor monitored and recorded process and emission control system operating parameters, and prepared
Section 3.0 of this report.
17.
a. DESCRIPTIONS
Baghouse
Dioxins/Furans
Hazardous Air Pollutants
Hydrogen Chloride
Total Hydrocarbons
18. DISTRIBUTION STATEMENT
Unlimited
KEY WORDS AND DOCUMENT ANALYSIS
b. IDENTIFIERS/OPEN ENDED TERMS
!*"- ' '
19. SECURITY CLASS (This Report)
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. COAST1 Field/Group
• •
21. NO. OF PAGES
540
22. PRICE
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE
F:\U\FMeadows\TRD.Frni\WP 6.1
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