United States
Environmental Protection
Agency
    Office of Air Quality
    Planning and Standards
    Research Triangle Park, NC 27711
April 2000
AIR
   &EPA

   Final Report

   Manual Testing and Continuous
   Emissions Monitoring
   Vertical Lime Kiln
   Baghouse Inlet and Outlet
   Chemical Lime Company
   Marble Falls, Texas
                   '«&
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           Clean
                       U.S. Environmental Protection Agency
                       Region 5, Library (PL-12J)

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                       FINAL REPORT

MANUAL TESTING AND CONTINUOUS EMISSIONS MONITORING
    VERTICAL LIME KILN BAGHOUSE INLET AND OUTLET
                 CHEMICAL LIME COMPANY
                   MARBLE FALLS, TEXAS
                  EPA Contract No. 68-D98-004
                   Work Assignment No. 3-03


                         Prepared for:

                  Mr. Michael L. Toney (MD-19)
                   Work Assignment Manager
                     SMTG, EMC, OAQPS
               U.S. Environmental Protection Agency
                 Research Triangle Park, NC 27711
                          April 2000
           P:\S523\FINRPTS\TEXAS\MARBFALL\REPORTVCL_MF.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

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                                  DISCLAIMER

      This document was prepared by Pacific Environmental Services, Inc. (PES) under EPA
Contract No. 68-D98-004, 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
1.0   INTRODUCTION	1-1

2.0   SUMMARY OF RESULTS	2-1

     2.1   PCDDs/PCDFs MEASUREMENTS 	2-1
     2.2   CEM MEASUREMENTS 	2-3

3.0   PROCESS DESCRIPTION	3-1

4.0   SAMPLING LOCATIONS 	4-1

     4.1   VERTICAL KILN BAGHOUSE INLET SAMPLING LOCATION  ... 4-1
     4.2   VERTICAL KILN BAGHOUSE OUTLET SAMPLING
          LOCATIONS	4-2

5.0   SAMPLING AND ANALYTICAL PROCEDURES 	5-1

     5.1   LOCATION OF MEASUREMENT SITES AND
          SAMPLE/VELOCITY TRAVERSE POINTS 	5-1
     5.2   DETERMINATION OF EXHAUST GAS VOLUMETRIC
          FLOW RATE	5-1
     5.3   DETERMINATION OF EXHAUST GAS MOISTURE CONTENT ... 5-1
     5.4   DETERMINATION OF PCDDs/PCDFs 	5-4
     5.5   DETERMINATION OF HYDROGEN CHLORIDE  	5-4
     5.6   DETERMINATION OF CARBON DIOXIDE, OXYGEN, AND
          TOTAL HYDROCARBONS	5-7
     5.7   CEMs DATA ACQUISITION AND HANDLING	5-9

6.0   QUALITY ASSURANCE/QUALITY CONTROL (QA/QC) PROCEDURES
     AND RESULTS 	6-1

     6.1   CALIBRATION AND PREPARATION OF APPARATUS	6-1
     6.2   REAGENTS AND GLASSWARE PREPARATION	6-3
     6.3   ON-SITE SAMPLING	6-5
     6.4   LABORATORY ANALYTICAL QA/QC PROCEDURES 	6-9
                              m

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                  TABLE OF CONTENTS (Concluded)
APPENDICES
     APPENDIX A - RAW FIELD DATA
     APPENDIX B - METHOD 23 LABORATORY ANALYTICAL DATA
     APPENDIX C - CALCULATIONS & COMPUTER SUMMARY
     APPENDIX D - EXAMPLE EQUATIONS
     APPENDIX E - QA/QCDATA
     APPENDIX F - PROCESS DATA
     APPENDIX G - SAMPLING & ANALYSIS METHODS
     APPENDIX H - PROJECT PARTICIPANTS
                             IV

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                                 LIST OF TABLES
                                                                            Page

Table 2.1     Emissions Test Log, Chemical Lime Company - Marble Falls, Texas  	2-2
Table 2.2     PCDDs/PCDFs Sampling and Exhaust Gas Parameters, Vertical Kiln
             Baghouse Inlet and Stack, Chemical Lime Company -
             Marble Falls, Texas  	2-4
Table 2.3     PCDDs/PCDFs Concentrations and Emission Rates, Vertical Kiln
             Baghouse Inlet and Stack, Chemical Lime Company -
             Marble Falls, Texas  	2-5
Table 2.4     PCDDs/PCDFs Concentrations and 2378-TCDD Toxic Equivalent
             Concentrations Adjusted to 7 Percent Oxygen, Vertical Kiln Baghouse
             Inlet and Stack, Chemical Lime Company - Marble Falls, Texas	2-6
Table 2.5     HC1 and THC Concentrations and Emission Rates, Vertical Kiln Baghouse
             Inlet and Stack, Chemical Lime Company - Marble Falls, Texas	2-7

Table 5.1     Summary of Sampling and Analysis Methods, Chemical Lime Company -
             Marble Falls, Texas  	5-2
Table 5.2     Summary of Sampling Locations, Test Parameters, Sampling Methods,
             and Number and Duration of Tests, Chemical Lime Company -
             Marble Falls, Texas  	5-3

Table 6.1     Summary of Temperature Sensor Calibration Data	6-2
Table 6.2     Summary of Pitot Tube Dimensional Data 	6-4
Table 6.3     Summary of Dry Gas Meter and Orifice Calibration Data	6-4
Table 6.4     Summary of EPA Methods 23 Field Sampling QA/QC Data	6-7
Table 6.5     Summary of Calibration Gas Cylinders	6-7
Table 6.6     Summary of Method 322 HC1 In Situ Spiking Data	6-8
Table 6.7     Summary of EPA Method 23 Blanks and Sample Catches	6-10
Table 6.8     Summary of EPA Method 23 Standards Recovery Efficiencies	6-11

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                                LIST OF FIGURES
                                                                             Page

Figure 1.1    Project Organization - US EPA Texas Lime Kiln Screening, Chemical
             Lime Company - Marble Falls, Texas	1-3

Figure 4.1    Vertical Kiln Process Exhaust Gas Schematic, Chemical Lime
             Company - Marble Falls, Texas	4-3
Figure 4.2    Vertical Kiln Baghouse Inlet Sample Port and Sample Point Locations,
             Chemical Lime Company - Marble Falls, Texas	4-4
Figure 4.3    Vertical Kiln Baghouse Outlet Sample Ports and Sample Point Locations
             For Isokinetic Testing, Chemical Lime Company - Marble Falls, Texas ....  4-5

Figure 5.1    Sampling Train Schematic for EPA Method 23   	5-5
Figure 5.2    Sampling Train Schematic for Proposed EPA Method 322  	5-6
Figure 5.3    Sampling Train Schematic for EPA Methods 3A and 25A  	5-8
                                        VI

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                               1.0  INTRODUCTION
       The U.S. Environmental Protection Agency (EPA) Office of Air Quality Planning and
Standards (OAQPS) 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 OAQPS 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. Initial planning, pre-test site survey, and preparation
activities were conducted under EPA Contract No. 68-D7-0002, Work Assignment No. 0/005.
Remaining preparation and field mobilization were conducted under EPA Contract No.
68-D7-0002, Work Assignment No. 1/007.  The draft final report was completed under EPA
Contract No. 68-D98-004, Work Assignment No. 2-04.  Generation of the Final Report,
incorporating EPA's comments on the Draft Final Report, was completed under EPA Contract
No. 68-D98-004, Work Assignment No. 3-03.

       The primary objective was to characterize the uncontrolled and controlled emissions of
selected HAPs from a vertical kiln located at Chemical Lime Company's Marble Falls, Texas
facility.  The "screening" tests were conducted to quantify the air emissions of hydrogen
chloride (HC1), total hydrocarbons (THC), and polychlorinated dibenzo-p-dioxins and
polychlorinated dibenzofurans (PCDDs/PCDFs).  The basic test methods that were employed
were US EPA Test Methods 1 (sample point location), 2 (effluent gas velocity), 3 A (oxygen
and carbon dioxide content), 4 (moisture content), 23 (PCDDs/PCDFs content) with proposed
revisions, 25A (total hydrocarbon content), and Proposed Method 322 (HC1 content). Testing
at the facility was conducted on June 25, 1998. One 3-hour test, comprised of the sampling
methods mentioned previously, was conducted at the baghouse inlet and baghouse outlet; inlet
and outlet sampling were performed simultaneously. During testing, Research Triangle
Institute (RTI), an ESD contractor, monitored and recorded process and emission control
system operating parameters.

       PES used three subcontractors for this effort: Air Pollution Characterization and
Control Inc. (APCC), Paradigm Analytical Laboratories, Inc. (PAL), and Atlantic Technical
Services, Inc. (ATS).  APCC provided field testing support for measurement of oxygen (O2),
carbon dioxide (CO2), total hydrocarbon (THC) and hydrogen chloride (HC1) concentrations
using Continuous Emission Monitors (CEMs); PAL prepared the XAD®-2 sorbent resin traps
and performed the  analysis of the Method 23 sample fractions to determine catch weights of
PCDD/PCDF congeners;  and ATS provided support during preparation of the Quality
Assurance Project Plan (QAPP), Site Specific Test Plan (SSTP), field testing and field data
reduction, reduction of laboratory analytical data,  and preparation of the Draft Final Report.
                                         1-1

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       The PES test crew consisted of Michael D. Maret (who served as the Task Manager
and Field Team Leader), Troy Abernathy, Gary Gay, Dennis D. Holzschuh, and Paul Siegel.
APCC was represented by John Powell, Eric Dithrich, and Peter Day, and ATS was
represented by Emil Stewart. Also present during the testing was Michael L. Toney, the EPA
Work Assignment Manager, Joseph P. Wood, EPA, OAQPS, BSD, and Cybele M. Brockmann
of RTI.  Chemical Lime Company was represented by Rick L. Hohman, Plant Manager, and
David R Christiansen, Environmental, Health and Safety Manager.

       Figure 1.1  presents the project organization and major lines of communication.
Section 2.0 presents the results of the testing; Section 3.0 is reserved for a process description
and operational data; Section 4.0 presents descriptions of the sampling locations; Section 5.0
presents descriptions of the sampling and analysis procedures; and Section 6.0 presents the
Quality Assurance/Quality Control procedures that were employed during the testing program,
and the results of calibrations and analytical QA data.  Copies of all field data generated during
the testing, the subcontracting laboratory analytical report, computer calculations and example
calculations, calibration data and compressed gas certifications of analysis, reprints of the EPA
Test Methods, and project participants are presented in the appendices to this document.
Appendix F is reserved for process and operational data.
                                         1-2

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                                               Chemical Lime Company
                                         Environmental, Health & Safety Manager
                                                David R. Christiansen
                                                   (817)732-8164
                                                 I
                                             EPA/EMC
                                       Work Assignment Manager
                                          Michael L. Toney
                                           (919) 541-5247
                                                                                          PES
                                                                                     Program Manager
                                                                                     John T. Chehaske
                                                                                      (919) 941-0333
                                                                            PES
                                                                    Corporate QA/QC Officer
                                                                      Jeffrey L. Van Atten
                                                                        (703)471-8383
 i
U)
                                                                                          PES
                                                                                      Project Manager
                                                                                     Franklin Meadows
                                                                                      (919) 941-0333
                                                                                          PES
                                                                                       Task Manager
                                                                                     Michael D.Maret
                                                                                      (919) 941-0333
                                                     EPA/ESD

                                                  Joseph P. Wood
                                                  (919) 541-5446
                                                                           Research Triangle Institute
                                                                               BSD Contractor
                                                                            Cybele M Brockmarm
                                                                               (919)990-8654
                     Pretest
                   Site Survey

                      PES
Quality Assurance
  Project Plan

     PES
Site Specific
 Test Plan

   PES
                                             Subcontractor

                                           Atlantic Technical
                                             Services, Inc.
 Field
Testing

 PES
                            Subcontractor

                          Atlantic Technical
                            Services, Inc.
 Sample
Analysis

  PES
                               Subcontractor

                         Air Pollution Characterization
                             and Control, Ltd.
                                                                                                      Subcontractor

                                                                                                    Atlantic Technical
                                                                                                      Services, Inc.
Draft Final
 Report

   PES
                             Subcontractor

                          Paradigm Analytical
                           Laboratories, Inc.
                         Subcontractor

                       Atlantic Technical
                         Services Inc.
               Figure  1.1  Project Organization - US EPA Texas Lime Kiln Screening, Chemical Lime Company - Marble Falls, Texas

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                           2.0  SUMMARY OF RESULTS
       This section summarizes the results of the testing that was conducted on the vertical
kiln at Chemical Lime Company's facility at Marble Falls, Texas.  Testing was conducted at the
inlet to the baghouse and at the main stack.  Table 2.1 presents the Emissions Test Log, which
summarizes the sample ran designators, test dates and times, target pollutants, and downtimes
for port changes and other stoppages. Flue gas parameters, pollutant concentrations, and
pollutant mass emission rates are summarized in Tables 2.2 through 2.5.
2.1    PCDDs/PCDFs MEASUREMENTS

       Table 2.2 presents the Method 23 sampling parameters and parameters of the baghouse
inlet and outlet airstreams. One Method 23 sampling run was performed at the baghouse inlet
location, and one Method 23 sampling run was performed at the outlet location.  Both runs
were conducted simultaneously, and both sample runs were within the isokinetic sampling ratio
criterion of 100 ± 10 percent(%); the isokinetic sampling ratio for the inlet ran (M23-I-1) was
102.2% and the isokinetic sampling ratio for the outlet ran (M23-O-1) was 101.6%.  For
purposes of the calculation of the volumetric flow rates, O2 and CO2 data were determined
from the Method 3 A CEM data, and moisture content was determined using the mass of
condensate collected in the impinger trains during the runs.

       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 fifteen percent.  If the mass ratio of
chlorine isotopes does not agree with the natural chlorine isotope ratio then the peak is flagged
as an Estimated Maximum Possible Concentration, or "EMPC".

       In-stack concentrations and associated mass emission rates of the PCDDs/PCDFs
congeners are presented  in Table 2.3 for the inlet and outlet sampling runs. The values
presented as "Total PCDDs" are the sum of the "12346789 OCDD" polychlorinated dibenzo-
p-dioxin and all of the dioxins labeled "Total"; "Total PCDFs" values are the sum of the
"12346789 OCDF" polychlorinated 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
                                         2-1

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                             TABLE 2.1

                       EMISSIONS TEST LOG
        CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS
Run No.
Date
Vertical Kiln Baehouse Inlet

M23-I-1
M3A-I-1
M25A-I-1
M322-I-1

06/25/98
06/25/98
06/25/98
06/25/98
Vertical Kiln Baehouse Stack

M23-O-1
M3A-O-1
M25A-O-1
M322-O-1

06/25/98
06/25/98
06/25/98
06/25/98
Pollutant
Run Time
Downtime,
Minutes *

PCDDs/PCDFs
C02 / 02
THC
HC1
1520-1857
1543-1826
1543-1826
1543-1826
37
87
87
87

PCDDs/PCDFs
C02 / 02
THC
HC1
1518-1855
1519-1850
1519-1850
1519-1850
37
116
116
116
The CEMs sample acquisition system operated on a time-shared basis, switching between
the baghouse inlet and stack locations. This applies to Methods 3A, 25A,  and 322.
                                2-2

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       Table 2.4 presents two PCDDs/PCDFs concentration-based measurements for both the
inlet and the outlet sampling locations.  In the second and third columns of the table, the
in-stack concentrations of the 2378-PCDDs/PCDFs congeners as well as the homologues (i.e.,
PCDDs and PCDFs groups that have the same degree of chlorination) are presented adjusted
to 7% O2. The fourth and fifth columns of the table present the 2378 tetra-chloro dibenzo-
dioxin (TCDD) toxic equivalent values for those congeners chlorinated at the 2, 3, 7, and 8
positions.  These columns represent the in-stack concentrations of the 2378  congeners after
being adjusted for toxicity relative to 2378-TCDDs. PCDDs/PCDFs congeners that are not
chlorinated at the 2,3,7, and 8 positions have a relative toxicity of zero and therefore the total
homologues (e.g., Total TCDD) are not presented in the Toxic Equivalency columns.
2.2    CEM MEASUREMENTS

       Measurements were conducted at the baghouse inlet and the outlet to determine the
concentrations of O2, CO2, THC, and HC1. These measurements were conducted using CEMs.
The CEMs were housed in a trailer supplied by APCC. Table 2.5 presents the average THC
and HC1 concentrations and mass emission rates.

       O2 and CO2 concentrations have been corrected for observed calibration and bias errors
using Equation 6C-1, as required in Method 3 A, and HC1 concentrations have been corrected
using Equation 1 in Proposed Method 322.  THC concentrations are presented uncorrected, as
required in Method 25 A; the uncorrected O2, CO2, and HC1 concentrations are given in
Appendix A. 3.  Refer to Appendix D for example equations.

       The CEMs collected data from the inlet and the outlet locations on a time-sharing basis.
The system was switched from inlet to outlet and back again every twenty-four minutes. The
first five minutes of data from each 24-minute period were excluded from the calculation of
average responses to allow for the time necessary to purge the CEMs system of the stack gases
from the previous sampling location and for the responses to stabilize.
                                        2-3

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                            TABLE 2.2

    PCDDs/PCDFs SAMPLING AND EXHAUST GAS PARAMETERS
          VERTICAL KILN BAGHOUSE INLET AND STACK
       CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS
Run No.
Date
Time
Total Sampling Time, minutes
Average Sampling Rate, dscfm "
Sample Volume:
dscfb
dscm"
Average Exhaust Gas Temperature, °F
O2 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfmd
dscfin"
dscmme
Isokinetic Sampling Ratio, %
M23-I-1
06/25/98
1520-1857
180
0.710

127.849
3.620
254
9.8
24.6
10.0

50,900
33,300
943
102.2
M23-O-1
06/25/98
1518-1855
180
0.740

133.265
3.774
231
13.6
15.7
9.9

52,400
35,400
1,000
101.6
* 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.
                                   2-4

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                                 TABLE 2.3

          PCDDs/PCDFs CONCENTRATIONS AND EMISSION RATES
              VERTICAL KILN BAGHOUSE INLET AND STACK
           CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS

CONGENER

DIOXINS:
2378 TCDD
Total TCDD
12378PeCDD
Total PeCDD
123478HxCDD
123678 HxCDD
123789HxCDD
Total HxCDD
1 234678 HpCDD
Total HpCDD
1 2346789 OCDD
Total PCDDs
FURANS:
2378 TCDF
Total TCDF
12378 PeCDF
23478 PeCDF
Total PeCDF
1 23478 HxCDF
1 23678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1 234678 HpCDF
1 234789 HpCDF
Total HpCDF
12346789 OCDF
Total PCDFs
Total PCDDs + PCDFs
CONCENTRATION *
(ng/dscm, as measured)
M23-I-1

{0.00472}
0.375
{0.00594}
0.152
{0.00348}
{0.00576}
0.00696
0.145
0.0141
0.0266
0.0156
0.715

0.0520
2.85
0.0356
0.0436
0.749
0.0446
0.0169
0.0126
0.00351
0.157
0.0189
{0.00199}
0.0238
{0.00267}
{3.78}
{4.50}
M23-0-1

0.00318
0.292
0.00238
0.0700
0.000795
0.00132
0.00106
0.0307
0.00185
0.00344
0.00636
0.403

0.0424
2.42
0.0231
0.0228
0.421
0.0125
0.00450
0.00291
0.00106
0.0440
0.00450
0.000530
0.00609
0.00265
2.89
3.29
EMISSION RATE *
(Hg/hr)
M23-I-1

{0.267}
21.2
{0.336}
8.62
{0.197}
{0.326}
0.394
8.23
0.795
1.51
0.881
40.4

2.94
161
2.01
2.47
42.4
2.52
0.956
0.714
0.198
8.87
1.07
{0.113}
1.34
{0.151}
{214}
{254}
M23-0-1

0.192
17.6
0.144
4.21
0.0479
0.0798
0.0638
1.85
0.112
0.207
0.383
24.2

2.55
146
1.39
1.37
25.4
0.750
0.271
0.176
0.064
2.65
0.271
0.0319
0.367
0.160
174
198
 1 Nanograms per dry standard cubic meter at 20°C and 1 atm.
 b Micrograms per hour.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
                                       2-5

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                                          TABLE 2.4

   PCDDs/PCDFs CONCENTRATIONS AND 2378-TCDD TOXIC EQUIVALENT CONCENTRATIONS
                             ADJUSTED TO 7 PERCENT OXYGEN
                       VERTICAL KILN BAGHOUSE INLET AND STACK
                    CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS

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
12378 PeCDF
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 O2)
M23-I-1

{0.00591}
0.469
{0.00744}
0.191
{0.00436}
{0.00722}
0.00872
0.182
0.0176
0.0333
0.0195
0.895

0.0652
3.57
0.0446
0.0547
0.938
0.0558
0.0212
0.0158
0.00439
0.196
0.0237
{0.00250}
0.0297
{0.00335}
{4.74}
{5.63}
M23-O-1

0.00605
0.556
0.00454
0.133
0.00151
0.00252
0.00202
0.0585
0.00353
0.00656
0.0121
0.766

0.0807
4.60
0.0439
0.0434
0.802
0.0237
0.00858
0.00555
0.00202
0.0838
0.00858
0.00101
0.0116
0.00505
5.50
6.27
2378-TCDD "
Toricity
Equivalency
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 percent Oj)
M23-I-1

{0.00591}

{0.00372}

{0.000436}
{0.000722}
0.000872

0.000176

0.0000195
{0.0119}

0.00652

0.00223
0.0273

0.00558
0.00212
0.00158
0.000439

0.000237
{0.0000250}

{0.00000335}
{0.0461}
{0.0579}
M23-0-1

0.00605

0.00227

0.000151
0.000252
0.000202

0.0000353

0.0000121
0.00898

0.00807

0.00219
0.0217

0.00237
0.000858
0.000555
0.000202

0.0000858
0.0000101

0.00000505
0.0361
0.0450
 " Nanograms per dry Stanford cubic meter at 20°C and 1 atm and corrected to 7 percent oxygen.
 b North Atlantic Treaty Organization, Committee on the Challenges of Modern Society. Pilot study on Information
  Exchange on Dioxins and Related Compounds: International Toxicity Equivalency Factor (I-TEF) Methods of Risk
  Assessment for Complex Mixtures of Dioxins and Related Compounds. Report No. 176, August 1988.
{ } Estimated Maximum Possible Concentration. EMPC values are included in totals.
                                               2-6

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                          TABLE 2.5

    HCL AND THC CONCENTRATIONS AND EMISSION RATES
        VERTICAL KILN BAGHOUSE INLET AND STACK
      CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS
Run No.
Date
Sampling Location
Total Sampling Time, minutes
O2 Concentration, % by Volume
Moisture, % by Volume
Volumetric Flow Rate, dscfin "
HC1:
Formula Weight, Ib/lb-mole
Concentration, ppmvw b
Concentration, ppmvd °
Concentration, ppmvd @ 7%O2 d
Emission Rate, Ib/hr e
THC (as propane):
Formula Weight, Ib/lb-mole
Concentration, ppmvw b
Concentration, ppmvd c
Concentration, ppmvd @ 7%O2 d
Emission Rate, Ib/hr e
M322-I-1
06/25/98
Inlet
76
9.8
10.0
33,300

36.47
22.7
25.2
31.6
4.77

44.11
17.8
19.8
24.8
4.52
M322-O-1
06/25/98
Stack
95
13.6
9.9
35,400

36.47
15.8
17.5
33.4
3.53

44.11
10.2
11.3
21.6
2.76
Dry standard cubic feet per minute at 68° F (20° C) and 1 atm.
Parts per million by volume wet basis.
Parts per million by volume dry basis.
Parts per million by volume dry basis corrected to 7% oxygen.
Pounds per hour.
                              2-7

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                            3.0 PROCESS DESCRIPTION
       The process description is considered confidential business information (CBI) and is not
discussed in this report. During the testing, however, an ESD contractor, Research Triangle
Institute, monitored and recorded process operational data which will be supplied to EPA EMC
under a separate EPA contract.
                                          3-1

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                             4.0  SAMPLING LOCATIONS
       As stated previously, source sampling was conducted to determine uncontrolled and
controlled emissions of HCI, PCDDs/PCDFs, and THC from the vertical kiln located at Chemical
Lime Company's Marble Falls, Texas facility. Testing was conducted at the inlet of the baghouse
and at two locations on the baghouse outlet. Figure 4.1 presents a simplified process flow
schematic depicting the sampling locations. Descriptions of the sampling locations are presented
in the following text; additional figures showing details of the sampling locations are also
presented.
4.1    VERTICAL KILN BAGHOUSE INLET SAMPLING LOCATION

       The baghouse inlet was a 47.5-inch inside diameter (ID) round duct which leads from the
kiln to baghouse. Due to geometric constraints, only one portion of the duct was accessible for
isokinetic sampling.  The location used was previously occupied by an auxiliary air preheater
which was retired from service prior to the testing program.  The air preheater interface was a
14-inch square duct which was joined to the baghouse inlet duct. A square plate with a 3-inch
sample port was fabricated  and attached to the preheater duct; it was through this port that the
PCDDs/PCDFs sampling was conducted.  Two additional ports were installed on the baghouse
inlet duct approximately fifteen inches downstream of the PCDDs/PCDFs sampling port, and it
was through these ports that CEM samples were extracted.

       A schematic diagram of the inlet sampling location is presented in Figure  4.2. The nearest
upstream disturbance was a bend 1080 inches (22.7 equivalent duct diameters) from the sample
port.  The nearest downstream disturbance was an elbow 128 inches (2.7 equivalent duct
diameters) downstream of the sample port. Method 1  specifies a 12 point sample matrix for this
test location.  Due to space constraints at the sampling location, only one traverse axis was
available  for isokinetic sampling.  Therefore, with approval of the WAM, PES conducted
isokinetic testing for PCDDs/PCDFs using one sample port and a six point traverse on a single
traverse line.  Figure 4.2 also shows the sample points within the duct that were used for
isokinetic testing.

       A check for the presence of non-parallel or cyclonic flow, as outlined in Section 2.4 of
EPA Method 1, was performed prior to testing. The results of the  cyclonic flow test indicated an
average yaw angle (a), of 6.8°.  Since the average yaw angle was less than 20°, which is the
maximum allowed by Method 1, the location was considered suitable for isokinetic sampling and
required no adjustment to the alignment of the nozzle direction.
                                          4-1

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4.2    VERTICAL KILN BAGHOUSE OUTLET SAMPLING LOCATIONS

       Sampling at the vertical kiln outlet was conducted at two locations.  Isokinetic sampling
was conducted using existing sample ports located close to the stack exhaust. In order to
decrease the amount of heated sample line required for the CEMs testing, additional sample ports
were installed approximately 34 feet upstream of the PCDDs/PCDFs sampling ports.

4.2.1   PCDDS/PCDFS Sampling Location

       The baghouse stack at the top of the kiln is a 47.84-inch average ID round stack (47.1875
inches on the A axis and 48.5 inches on the B axis) which exhausts emissions to the atmosphere.
An induced draft fan located at ground level pulls kiln exhaust gases through the baghouse; the
gases are transported through approximately 200 feet of ductwork prior to release. A sampling
platform located at the top of the kiln provided access to the sample ports.  A schematic diagram
of the sample ports and sample point locations is presented in Figure 4.3. The nearest
downstream disturbance was the opening to the atmosphere which was 209 inches (4.4 equivalent
duct diameters) from the sample ports.  The nearest upstream disturbance was a 45° bend located
128 inches (2.7 equivalent duct diameters) upstream of the sample ports. PES conducted
isokinetic testing for PCDDs/PCDFs using a 24 point traverse matrix consisting of 12 traverse
points on each of two perpendicular traverse lines.

       A check for the presence of non-parallel or cyclonic flow, as outlined in Section 2.4 of
EPA Method 1, was performed prior to testing.  The results of the cyclonic flow test indicated an
average yaw angle (a), of 7.3°.  Since the average yaw angle was less than 20°, which is the
maximum allowed by Method 1, the location was considered suitable for isokinetic sampling and
required no adjustment to the alignment of the nozzle direction.

4.2.2   CEM Sampling Location

       The CEM sampling location was located approximately 34 feet upstream of the outlet
isokinetic sampling ports. Two ports were installed at this location to facilitate the extraction of
samples for analysis of O2, CO2, THC, and HC1 using CEMs. The nearest disturbances were
bends in the duct, located approximately 8 feet downstream and 25 feet upstream from the
location of the ports.
                                          4-2

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Combustion Air
     Fan
Combustion Air
     Fan
Combustion Air
    Fan
Combustion Air
     Fan
Combustion Air
     Fan
                            Atmosphere
                                 t
                               Stack
                                Fan
                             Baghouse
                                                   Baghouse Stack
                                                  Sampling Location
Double Shaft Vertical Kiln
     t
t
                                                      Baghouse Inlet
                                                    Sampling Location
                                                       Cooling Air Fan
                                                       Cooling Air Fan
                                                       Cooling Air Fan
 Figure 4.1 Vertical Kiln Process Exhaust Gas Schematic, Chemical Lime
          Company - Marble Falls, Texas
                              4-3

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                                                         Cross Sectional View
From Vertical
    Kiln   ~
                          1080"
                          128"
                                            =0
                                                                47.5 "
                                                               Traverse Points
                                                          (Distance from Inside Wall, in.)
                                                              1
                                                              2
                                                              3
                                                              4
                                                              5
                                                              6
2 1/8
67/8
14
33 1/2
40 5/8
45 3/8
                                               To Baghouse
           Figure 4.2 Vertical Kiln Baghouse Inlet Sample Port and Sample Point Locations,
                     Chemical Lime Company - Marble Falls, Texas
                                           4-4

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            Cross Sectional View
                        48.5"
      47.1875"
P  PortB
                       Port A
                Traverse Points
           (Distance from Inside Wall, in.)

1
2
3
4
5
6
7
8
9
10
11
12
PORT A
1
3 1/8
5 5/8
8 3/8
11 3/4
163/4
303/8
353/8
387/8
41 5/8
44
46 1/4
PORTB
1
3 1/4
5 3/4
8 5/8
121/8
171/4
31 1/4
36 3/8
397/8
42 3/4
45 1/4
47 1/2
                                      209"
                                                                        128"
                                                     From
                                                      Fan

Figure 4.3 Vertical Kiln Baghouse Outlet Sample Ports and Sample Point Locations for
          Isokinetic Testing, Chemical Lime Company - Marble Falls, Texas
                                      4-5

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                  5.0 SAMPLING AND ANALYSIS PROCEDURES
       Source sampling was performed at the baghouse inlet and baghouse stack to determine the
concentrations and mass emission rates of PCDDs/PCDFs, THC, and HC1. One test run was
performed at each location, with each run having a net sampling time of three hours. The
sampling and analytical methods that were used are summarized in Table 5.1. In Table 5.2, the
parameters measured, the sampling method, the number of tests performed, and the duration of
each test are summarized.  Brief descriptions of the sampling and analysis procedures used are
presented below. Copies of all the methods that were used are presented in Appendix G.
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. The process ductwork and the locations of
measurement sites and traverse points, are discussed in Section 4.0 of this document.
5.2    DETERMINATION OF EXHAUST GAS VOLUMETRIC FLOW RATE

       EPA Method 2, "Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S
Pitot Tube)," was used in conjunction with EPA Method 23 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.  The pitot tube was inserted into the
duct and the velocity pressure (Ap) was recorded at each traverse point. The effluent gas
temperature was also recorded at each traverse point using a Type K thermocouple.  The average
exhaust gas velocity was calculated from the average square roots of the velocity pressure,
average exhaust gas temperature, exhaust gas molecular weight, and absolute stack pressure. The
volumetric flow rate is the product of velocity and the stack cross-sectional area of the duct at the
sampling location.
5.3    DETERMINATION OF EXHAUST GAS MOISTURE CONTENT

       EPA Method 4, "Determination of Moisture Content in Stack Gases," was used to
determine the exhaust gas moisture content. EPA Method 4 was performed in conjunction with
each EPA Method 23 test run. Integrated, multi-point, isokinetic sampling was performed.
Condensed moisture was determined by recording pre-test and post-test weights of the impingers,
XAD® sorbent module, and silica gel.

                                         5-1

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                               TABLE 5.1

           SUMMARY OF SAMPLING AND ANALYSIS METHODS,
          CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS
    Sampling Method
   Parameter or Target
  Measurement Principle
EPA Method 1

EPA Method 2


EPA Method 3 A


EPA Method 4


EPA Method 23 (Proposed
Revisions)


EPA Method 25A


EPA Proposed Method 322
Traverse Point Locations
Velocity and Flow Rate
CO, and O, Content
Moisture Content
PCDDs/PCDFs
THC
HC1
Linear Measurement

Differential Pressure,
Thermocouple

Micro-Fuel Cell, FINOR


Gravimetric


Gas Chromatography / Mass
Spectrometry (GC/MS)


Flame lonization Detector


Gas Filter Correlation /
Infrared (GFC/IR)
                                    5-2

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                     TABLE 5.2
  SUMMARY OF SAMPLING LOCATIONS, TEST PARAMETERS,
SAMPLING METHODS, AND NUMBER AND DURATION OF TESTS,
    CHEMICAL LIME COMPANY - MARBLE FALLS, TEXAS
Sampling
Location
Baghouse
Inlet




Baghouse
Stack




Test Parameter
Exhaust Gas Flow Rate
CO2 & O2 Content
Moisture Content
PCDDs/PCDFs
THC
HC1
Exhaust Gas Flow Rate
CO2 & O2 Content
Moisture Content
PCDDs/PCDFs
THC
HC1
Sampling Methods
EPA Method 2
EPA Method 3 A
EPA Method 4
EPA Method 23 (Proposed
Revisions)
EPA Method 25A
EPA Proposed Method 322
EPA Method 2
EPA Method 3 A
EPA Method 4
EPA Method 23 (Proposed
Revisions)
EPA Method 25 A
EPA Proposed Method 322
Number
of Tests
1
1
1
1
1
1
1
1
1
1
1
1
Duration,
(minutes)
180
76
180
180
76
76
180
95
180
180
95
95
                        5-3

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5.4    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 employed. These proposed rules correct
existing errors in the method, eliminate the methylene chloride rinse, and clarify the quality
assurance requirements of the method.  A multi-point integrated sample was extracted
isokinetically from the six (at the baghouse inlet) or 24 (at the baghouse stack) traverse points
shown in Section 4.0. At each traverse point, sampling was performed for 15 (at the baghouse
inlet, with each point traversed twice), or 7.5 (at the baghouse stack) minutes for a total run time
of 180 minutes per test.  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 a sorbent trap containing approximately 40 g of XAD®-2 sorbent resin. The EPA Method 23
sampling train is shown in Figure 5.1.

       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.  For the inlet sample analysis, an additional separate "loose" particulate fraction
was also Soxhlet extracted and analyzed; results of the two inlet analyses were added to get a
single inlet catch weight.  Refer to Appendix B for a tabulation of the inlet sample catches.
Analysis was performed on a high resolution Gas Chromatograph with a high resolution Mass
Spectrometer (GC/MS) detector.
5.5    DETERMINATION OF HYDROGEN CHLORIDE

       EPA Proposed Method 322, "Measurement of Hydrogen Chloride Emissions from
Portland Cement Kilns by GFGTR," was used to monitor HC1 emissions at each location.  Stack
gas samples were extracted from each duct or stack and transported through a heated sample
probe, sample conditioning system, heated sample line, and a heated sample pump into the
analyzer containing the gas filter correlation infrared spectrometer (GFC/IR). 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.

       HC1 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 5.2.
                                          5-4

-------
                           Temperature
                                                    Condenser
 Button Hook
   Nozzle
Gas
Exit
                Stack
                Wall
                                                                                   Temperature
                                                                                      Sensor
                                                            Adsorbent Resin Trap
                                                   Empty 100 ml HPLC Water  Empty  Silica Gel
Vacuum
 Line
            Inclined
           Manometer
                                                      Vacuum
                                                       Pump
                   Figure 5.1 Sampling Train Schematic for EPA Method 23

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  Heated Probe                 Three-way
   (mln. 37«*F)  Heated Fitter Box      I
PM-10
Cyclon
                                        Sample UM   HMtad 8ampl«/C«Ubr«tlon  Urn
                      In-SHu MUttta
            ThrM-way   Spiking  Nm
              v«lv«
                                                    P»rkln-Elm«r
                                                Uleroproe*«tor
                                              DDDD DDDDD
                                              GM Filter Correlation
                                               Infrared Analyzer
                                              Infrared
                                              Detector
      Figure 5.2  Sampling Train Schematic for Proposed EPA Method 322
                                       5-6

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5.6   DETERMINATION OF CARBON DIOXIDE, OXYGEN, AND
      TOTAL HYDROCARBONS

      Continuous emission monitoring (CEM) was performed at the baghouse inlet and stack.
All CEM data was recorded using a Tracor/Westronics 3000 automatic digital data logger. The
CEMs were housed in the APCC Envkonmental Monitoring Laboratory positioned at the base of
the stack. Stack gas was drawn from the stack through a heated Teflon® sample line which is
maintained at a temperature of approximately 375°F. A portion of the extracted sample was
conditioned to remove moisture and directed to the O2 and CO2 analyzers to determine diluent
concentrations on a dry basis.  The remaining portion of the stack gas sample was directed to the
THC analyzer. Figure 5.3 shows a schematic of the sampling system.

5.6.1  Carbon Dioxide and Oxygen

      EPA Method 3 A, "Determination of Oxygen and Carbon Dioxide Concentrations in
Emissions from Stationary Sources," was used to determine the O2 and CO2 concentrations at the
inlet and outlet test locations.

      A Westinghouse/Maihak FINOR CO2 analyzer was used to monitor CO2 concentrations.
The measurement principle for CO2 is IR absorption. Radiation absorbed by CO2 in the sample
cell produces a capacitance change in the detector which is proportional to the CO2 concentration.

      A Teledyne Analytical Instruments Model 326 O2 analyzer was utilized to measure the
percentage concentration of 02 in the gas stream. The analyzer utilizes a unique micro-fuel cell to
measure the concentration of O2.  The output signal is linear over the specified ranges of analysis.

5.6.2  Total Hydrocarbons

      EPA Method 25 A, "Determination of Total Gaseous Organic Concentration using a Flame
lonization Analyzer," was used to determine the THC concentrations at both test locations.  A
VIG Industries THC analyzer (or equivalent), which utilizes a flame ionization detector (FED) to
measure THC, was calibrated with propane. Approximately 5.0 liters per minute (1pm) of sample
gas is drawn from the source through a heated Teflon® sample line.  The sample gas is drawn
through a heated filter and valves by a heated pump. The sample gas is introduced into the FID
chamber and THCs in the sample are ionized by a hydrogen flame. The flame is positioned
between two charged plates, and the associated electric field induces the migration of the ions
towards the charged plates.  The ion migration results in the generation of a current, which is
directly proportional to the amount of THCs present in the sample.
                                         5-7

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                                       Stack
                                       Wall
                                                  Heated Filter
                                                                                            Sample By-Pass
                                                                                                Vent
oo
By-Pass Flow
Control Valve
                                          Figure 5.3 Sampling Train Schematic for EPA Methods 3A and 25A

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5.7    CEMs DATA ACQUISITION AND HANDLING

       Analyzer responses were recorded by a Tracor/Westronics 3000 digital data logger which
recorded the O2, C02, HC1 and THC concentrations using its integral color printer.  Trends were
monitored using the strip chart mode with averages printed digitally at 19 minute intervals and at
the conclusion of the test period. Analyzer responses were  recorded by the data logger at 5
second intervals.
                                        5-9

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             6.0  QUALITY ASSURANCE/QUALITY CONTROL (QA/QC)
                           PROCEDURES AND RESULTS
      For any environmental measurement, a degree of uncertainty exists in the data generated
due to the inherent limitations of the measurement system employed.  The goals of a QA/QC
program are to ensure, to the highest degree possible, the accuracy of the data collected. This
section summarizes the QA/QC procedures that were employed by PES in the performance of this
test program.  The procedures contained in the reference test methods and in the "Quality
Assurance Handbook for Air Pollution Measurement Systems, Volume III, Stationary Source
Specific Methods," EPA/600/R-94/038c, served as the basis for performance for all testing and
related work activities in this project.
6.1    CALIBRATION AND PREPARATION 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 are presented below.
The results of equipment and sensor calibrations may be found in Appendix E. Detailed
procedures as presented in the EPA test methods are presented in Appendix G.

6.1.1   Barometers

       PES used aneroid barometers which were calibrated against a barometric pressure value
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 2e 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

       PES used Type S pitot tubes constructed according to EPA Method 2 specifications.
Each pitot tube was inspected for conformance to the geometric specifications by the application
of Calibration Procedure 2 of EPA/600/R-94/038c.  Pitot tubes that meet these
                                         6-1

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                   TABLE 6.1
SUMMARY OF TEMPERATURE SENSOR CALIBRATION DATA
Temp.
Sensor
I.D.
T5A



T6F



MB-10






RMB-15






Usage
Stack Gas



Stack Gas



Meter Box
Inlet


Outlet


Meter Box
Inlet


Outlet


Temperature, °R
Reference
532
504
664
860
534
494
632
809

493
536
666
492
536
666

493
534
668
493
534
668
Sensor
532
504
664
860
534
493
632
810

494
536
665
494
537
665

495
534
670
493
535
668
Temperature
Difference
0.0%
0.0%
0.0%
0.0%
0.0%
-0.20%
0.0%
0.12%

0.20%
0.0%
-0.15%
0.40%
0.19%
-0.15%

0.40%
0.0%
0.30%
0.00%
0.19%
0.00%
Tolerances
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%

<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%

<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
<±1.5%
                       6-2

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requirements are assigned a pitot coefficient, Cp, of 0.84. The dimensional criteria and results for
each pitot tube used are presented in Table 6.2.

 6.1.4  Differential Pressure Gauges

       PES used Dwyer inclined/vertical manometers to measure differential pressures.  The
differential pressure 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  EPA Method 23 Pry Gas Meters and Orifices

       The EPA Method 23 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 and
annually thereafter, the metering system is calibrated over the entire range of operation as
specified in EPA Method 5. Acceptable tolerances for the individual dry gas meter correction
factor (y) and orifice calibration factor (AH@) during initial or annual calibrations are ± 0.02 and
± 0.20 from the average, respectively. After field use, a calibration check of the metering system
was performed at a single intermediate setting based on the previous field test. The post-test
calibration check of the dry gas meter correction factor must agree within 5% of the correction
factor generated during the initial or annual calibration. The results for the gas meters and orifices
used in this test program are summarized in Table 6.3.
6.2    REAGENTS AND GLASSWARE PREPARATION

       Sample reagents consisted of pesticide (or better) grade acetone and toluene for glassware
preparation and sample recoveries, and pesticide (or better) grade hexane for glassware
preparation.  Sample filters and the XAD®-2 sorbent resin traps were prepared by PAL according
to the procedures outlined in Method 23.  Water used in the impinger trains was HPLC-grade
reagent water.

       After preparation of the XAD®-2 sorbent resin traps by PAL, each trap was spiked with a
mixture of PCDDs/PCDFs surrogates, and capped with glass balls and sockets until used in the
field.

       Prior to the field testing portion of the program, all sampling train components and sample
recovery apparatus were prepared according to the following procedure.

       1.     Wash in hot soapy water (Alconox®).
       2.     Rinse three times with tap water.
       3.     Rinse three times with distilled/deionized water.
                                           6-3

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                     TABLE 6.2
       SUMMARY OF PITOT TUBE DIMENSIONAL DATA
Measurement
«,
02
Pi
P2
Y
e
A
z
w
Dt
(A/2)/Dt
Criteria
<10°
<10°
<5°
<5°
-
-
-
< 0.125"
< 0.0313"
0.1875" £ Dts
0.375"
1.05 < (A/2)/D,s
1.50
Acceptable
Assigned Coefficient
Results
Pitot Tube Identification
5H
0.7
1.6
4
3.3
0.6
0.4
0.956
0.010
0.0067
0.375
1.27
Yes
0.84
6A
1
0.2
0.2
0.8
2.2
1.1
1.006
0.039
0.019
0.375
1.34
Yes
0.84
                      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
1.020
0.995
% Diff.
-0.2
-0.5
EPA Criteria
±5%
±5%
Orifice Coefficient, AH@
Average
1.92
1.90
Range
1.73 - 2.44
1.86 - 1.92
EPA Criteria
1.72-2.12
1.70-2.10
                         6-4

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       4.     Rinse with pesticide-grade acetone.
       5.     Rinse with pesticide-grade-toluene.
       6.     Rinse with pesticide-grade hexane.
       7.     Allow to air dry.
       8.     Cap all openings with hexane-rinsed aluminum foil.
6.3    ON-SITE SAMPLING

       The on-site QA/QC activities included:

6.3.1   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
through both traverse axes to confirm uniformity of the stack/duct inside diameter. The baghouse
outlet stack was found to be out-of-round; therefore, two sets of sample traverse points were
calculated.  The inside stack/duct dimensions, wall thickness, and sample port depths were
measured to the nearest 1/16 inch.

6.3.2   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.

6.3.3   Moisture

       The Method 23 trains were used to determine stack gas moisture.  During sampling, the
exit gas of the last impinger was maintained below 68°F to ensure adequate condensation of the
exhaust gas water vapor. The total moisture was determined on-site gravimetrically using an
electronic platform balance with 0.1 gram sensitivity.  The amount of moisture collected by the
XAD® trap was also measured.

6.3.4   EPA Method 23

       The field sampling QA/QC for EPA Method 23 began in the sample recovery area. The
sample trains were set up and leak-checked to verify sample train integrity before transport to the
sampling sites. At the sampling sites, the sample trains were leak checked a second time.  Leaks
found in excess of 0.02 cubic feet per minute (cfin) were corrected prior to beginning the test
runs.  Leak checks were also conducted before and after any sample train component changes,
between sample ports, and upon completion of the test runs. Sampling was conducted within the
isokinetic sampling criteria of 100 ± 10%.  Table 6.4 summarizes the EPA Method 23 field
sampling QA/QC  measurements and EPA's acceptability criteria.
                                           6-5

-------
       In addition to the inlet and outlet samples, one field blank sample was collected.  A
Method 23 sampling train was assembled and transported to the outlet sampling location, and
leak-checked twice.  The sample train was then recovered using the same procedures employed
during the recovery of the sample trains used during actual sample runs. The collected fractions
were transferred to labeled, pre-cleaned sample bottles, transported to the subcontract laboratory,
and analyzed in the same manner as the collected samples.

       PES  also collected samples of the reagents that were used during the program as blanks.
Samples were collected of the acetone and toluene; an unused filter and XAD*-2 sorbent module
were also collected.  These reagent blank samples were transported to the subcontract laboratory
and analyzed for PCDDs/PCDFs using the same procedures as during the analysis of the collected
samples.

6.3.5   Continuous Emission Monitors

       CEMs were used to quantify the in-stack concentrations of O2, CO2, THC, and HC1 using
EPA Methods 3 A, 25A and Proposed Method 322, respectively. QA/QC checks performed
included direct calibrations, bias checks, and drift checks; matrix spikes were also performed on
the Method  322 HC1 CEMs sampling system.  Table 6.5 summarizes the compressed gas
standards that  were used during the test program.

6.3.5.1  EPA Method 3A

       Prior to the start of each day of testing, the 02 and CO2 analyzers were calibrated with a
zero gas standard and two upscale standards corresponding to approximately 55 and 85% of the
instrument measurement ranges. The calibration error of the analyzers on direct calibration was
less than or  equal to 2% of span.  The sampling line bias was then checked with the zero gas and
one upscale gas for each analyzer.  The sampling line bias was less than or equal to 5% of the
response of the analyzer to the calibration standard when injected directly into the analyzer. At
the conclusion of the sampling run, the sampling system was again checked by introducing the
zero and upscale standard into the system at the probe end.  The sampling system drift was less
than 3% of the instrument span for both the zero and upscale calibration gases. The true
concentration of the gases measured was then calculated from the  average instrument response
and the results of the calibration responses using Equation 6C-1 as found in Method 6C, which is
the procedure specified in Method 3 A. The gases used for calibrations were certified by the
manufacturer, and prepared according to the procedures in "EPA Traceability Protocol for Assay
and Certification of Gaseous Calibration Standards (September 1993)." Results of the above
mentioned QC checks are tabulated in Appendix E.
 6.3.5.2 EPA Method 25A

        Prior to the start of each day of testing, the THC sampling system was calibrated with a
 zero gas standard and three upscale propane standards corresponding to approximately 25, 50,
 and 85% of the instrument measurement range.  The calibration errors of the THC system
                                           6-6

-------
                     TABLE 6.4
SUMMARY OF EPA METHOD 23 FIELD SAMPLING QA/QC DATA
Run No.
Site
Date
Pre-Test Leak Rate, acfin
Post-Test Leak Rate, acfin
EPA Criteria, acftn
Percent Isokinetic
EPA Criteria
M23-I-1
Vertical Kiln
Baghouse Inlet
06/25/98
0.001 @ 15" Hg
0.001 @ 15" Hg
0.02
102.2
90-110%
M23-O-1
Vertical Kiln
Baghouse Stack
06/25/98
0.004 @ 15" Hg
0.004 @10"Hg
0.02
101.6
90-110%
                     TABLE 6.5
       SUMMARY OF CALIBRATION GAS CYLINDERS
Cylinder Number
CC88470
1836637Y
AAL-13302
SG9128557BAL
SG9128479BAL
CC84329
CC84329
CC86922
CC86922
Contents
46.0 ppm HC1 in nitrogen
303.0 ppm HC1 in nitrogen
30.0 ppm C3Hg in air
58.3 ppm C3Hg in air
92.4 ppm C3Hg in air
11.03%CO2inN2/02/C02
11.04%O2inN2/O2/CO2
19.01 %CO2 in N2/O2/CO2
19.17%O2inN2/O2/CO2
Expiration Date
Certified on 6/1 2/98
Certified on 6/12/98
5/01/01
9/27/99
2/18/01
3/02/01
3/02/01
3/02/01
3/02/01
                        6-7

-------
were less than 5% of the instrument operating range.  At the conclusion of the sampling run, the
sampling system was again checked by introducing the zero and one upscale standard into the
system at the probe. The sampling system drift was less than 3% of the instrument span for both
the zero and upscale calibration gases. The THC results are reported as the average of the
instrument responses over the period of the sampling run.  The gases used for calibration were
certified by the manufacturer, and prepared according to the procedures in "EPA Traceability
Protocol for Assay and Certification of Gaseous Calibration Standards (September 1993)."
Results of the above mentioned QC checks are tabulated in Appendix E.

6.3.5.3 Proposed Method 322

       Prior to the start of each day of testing, the HC1 analyzer was  calibrated with a zero gas
standard and two upscale standards corresponding to approximately 25 and 85% of the
instrument measurement ranges.  The calibration error of the analyzers on direct calibration was
less than or equal to 5% of span or 1 ppm, whichever was greater.  The sampling line bias was
then checked with the zero gas and one upscale gas. The sampling line bias was less than or equal
to 7.5% (or 1.5 ppm, whichever was greater) of the response of the analyzer to the calibration
standard when injected directly into the analyzer.  Results of the above mentioned QC checks are
tabulated in Appendix E.

       Following the direct calibration and bias checks, a matrix spike for HC1 was conducted so
that the integrity of the  sampling and  analysis system for HC1 could be ascertained. The flue gas
was sampled to determine the baseline concentration of the HC1, and after the baseline
concentration was established, a known quantity of HC1 was injected into the sampling system.
The analyzer response must report the concentration of the HC1 in the effluent stream plus the
contribution of the HC1 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 Chemical Lime Company, the matrix spikes were within the ± 30% tolerance.
The results of the matrix spikes are presented in Table 6.6 and Appendix E.
                                       TABLE 6.6
              SUMMARY OF METHOD 322 HC1IN-SITU SPIKING DATA
Test
Location
Inlet
Stack
HC1 Spike Recovery Efficiencies, %
Pre-test
109
106
Post-test
122
106
Average
116
106
EPA
Criteria
70-130
70-130
                                           6-8

-------
6.4    LABORATORY ANALYTICAL QA/QC PROCEDURES

6.4.1   Analysis of Blank Samples

       The Method 23 blank samples were analyzed following the procedures of EPA
Method 23. Field blanks (FB), reagent blanks (RB), and laboratory blanks were used to evaluate
the effectiveness of the sample train clean-up procedures and to check for contamination of the
reagent materials.  In addition, the subcontract laboratory conducted the Laboratory Method
Blank (LMB) to evaluate the presence of contamination of the samples during analysis.  The
results of these blank analyses and the actual run sample catches are presented in Table 6.7.

6.4.2   Standards Recovery Efficiencies

       Prior to shipment of the XAD®-2 sorbent modules by PAL, each module was spiked with
a mixture of surrogate (sampling) standards. The modules were then sent to Marble Falls, Texas,
via Federal Express for use in the sampling program.  Upon analysis, the recoveries of the
surrogate standards provide a measure of the capture and holding efficiency of the XAD®-2
sorbent traps for the sampled PCDDs/PCDFs.  A low recovery efficiency may indicate the loss of
PCDDs/PCDFs congeners from the XAD®-2 sorbent module after its recovery from the sampling
train.  A special "cleanup" standard was added to the separate particulate sample fraction of the
inlet Method 23 sample train sample (recovered separately due to the excessively large amount of
the particulate). The recovery efficiency of these standards are presented in lieu of the non-
existent surrogate standard recoveries. Table 6.8 presents the results of the surrogate and
"cleanup" standards recoveries.

       Four of the five M23-I-1 sampling standards were below 70%; the laboratory case
narrative states "No simple explanation can be offered for this observation." The sampling
standards are an indication of the efficiency of the sample recovery effort. When the sampling
standards are less than 100%, the sample catches may be under-reported.  Since the samples in
question are from the inlet location, the removal efficiency of the baghouse would be biased high.
The inlet concentration may be biassed low by 25 to 67%; note that Method 23  accepts a low bias
of 30%.

       Upon receipt of the XAD®-2 sorbent modules by the laboratory after sampling, the
XAD®-2 sorbent resin modules are spiked with a mixture of internal (extraction) standards.  The
purpose of these standards is to evaluate the efficiency of the extraction of the PCDDs/PCDFs
congeners from the sample fractions. The results of these recoveries are presented in Table 6.8.
                                          6-9

-------
                              TABLE 6.7
SUMMARY OF EPA METHOD 23 BLANKS AND SAMPLE CATCHES



PAL Lab Report Page
Numbers in Appendix B
Analvte
2378-TCDD
12378-PeCDD
123478-HxCDD
123678-HxCDD
123789-HxCDD
1234678-HpCDD
OCDD
2378-TCDF b
12378-PeCDF
23478-PeCDF
123478-HxCDF
123678-HxCDF
234678-HxCDF
123789-HxCDF
1234678-HpCDF
1234789-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
Total PCDD/Fs c
Catch, ng Per Sample
PAL
LMB
003 / 025


{0.00094}
{0.00052}
(0.0007)
(0.0006)
(0.0006)
0.0032
0.0093
{0.00104}
(0.0004)
(0.0004)
{0.00112}
0.0006
(0.0003)
(0.0004)
0.0027
(0.0007)
0.0021
{0.0009}
{0.0004}
{0.0016}
0.0032
0.0012
(0.0004)
0.0004
0.0028
0.019
M23-
RB-1
003/112


0.0011
(0.0004)
(0.0006)
{0.00096}
0.0014
0.0031
0.0096
(0.0006)
(0.0004)
(0.0004)
0.0008
(0.0003)
(0.0003)
(0.0004)
0.0030
(0.0006)
0.0028
0.0011
(0.0004)
0.0024
0.0032
(0.0006)
(0.0004)
0.0008
0.0032
0.023
M23-
FB-1
003 / 093


{0.00095}
(0.0003)
(0.0005)
{0.00092}
{0.00088}
0.0045
0.0162
0.0030
(0.0005)
(0.0004)
0.0014
{0.00044}
(0.0002)
(0.0003)
0.0071
(0.0008)
0.0059
0.0016
0.0016
0.0040
0.0080
0.0108
{0.0016}
0.0024
0.0072
0.058
M23-I-
1 + FH"
0 / 043 /
129

{0.0171}
{0.0215}
{0.0126}
{0.0209}
0.0252
0.0509
0.0564
0.1884
0.1288
0.158
0.1613
0.0612
0.0457
0.0127
0.0684
{0.00722}
{0.00968}
1.3562
0.5514
0.5264
0.0964
10.3236
2.7118
0.5676
0.0860
16.3
M23-
O-l
068


0.0124
0.0087
0.0027
0.0049
0.0043
0.0073
0.0243
0.160
0.0874
0.0864
0.0474
0.0171
0.0114
0.0037
0.0170
0.0016
0.0103
1.102
0.264
0.116
0.0132
9.12
1.59
0.166
0.0228
12.4
 a Result obtained by summing the two inlet sample fractions analyzed.
 b Result obtained from the DB-225 analysis.
 0 Total PCDD/Fs represent the sum of all polychlorinated dibenzo-p-dioxins & dibenzofurans.
() Denotes a non-detect value using the detection limit.
{ } Denotes an EMPC value.
                                  6-10

-------
                                  TABLE 6.8

  SUMMARY OF EPA METHOD 23 STANDARDS RECOVERY EFFICIENCIES



FULL SCREEN ANALYSIS
PAL Lab Report Page Number
Internal (Extraction) Standards
2378-TCDD
12378-PeCDD
123678-HxCDD
1234678-HpCDD
OCDD
2378-TCDF
12378-PeCDF
123678-HxCDF
1234678-HpCDF
Surrogate (Sampling) Standards
2378-TCDD
23478-PeCDF
123478-HxCDD
123478-HxCDF
1234789-HpCDF
Percent Recoven
PAL
LMB

026

94.6
101.9
96.3
91.8
86.2
91.4
88.1
100.8
74.5

104.4
109.4
103.0
95.8
97.7
M23-
1-1

044

94.8
108.8
88.6
93.7
84.0
95.4
95.9
80.6
78.8

69.2
61.0
75.3
56.2
33.2
M23-
I-1FH

130

74.4
83.9
76.8
78.3
66.5
69.2
63.3
61.2
53.5

100.2 a
107.0 a
110.73
103.7 a
109.1 a
M23-
O-l

069

97.4
113.1
93.8
102.1
92.4
98.6
101.2
94.2
82.9

95.3
98.5
109.6
96.3
92.0

M23-
FB-1

094

87.4
100.9
94.6
95.6
87.1
88.2
87.1
94.8
75.2

94.4
97.8
90.2
79.6
77.8
M23-
RB-1

113

86.4
94.1
87.4
92.3
83.6
87.7
81.5
91.8
73.7

96.4
98.2
110.1
88.2
81.6

QC
Limits



40-130%
40-130%
40-130%
40-130%
40-130%
40-130%
25-130%
25-130%
25-130%

70-130%
70-130%
70-130%
70-130%
70-130%
The "Surrogate" recoveries presented for Sample "M23-I-1 FH" are actually recoveries for the "cleanup"
standards which were added to the separate paniculate phase of the inlet sample only.
                                      6-11

-------
  APPENDIX A




RAW FIELD DATA

-------
      Appendix A. 1




      Raw Field Data




Vertical Kiln Baghouse Inlet


-------
        TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS-^
Plant.
Date:
Sampling Location:.
                                   1*1 el
Inside of Far Wall to Outside of Nipple:    * ? Vlf
Inside of Near Wall to Outside of Nipple (Nipple Length):.
Stack I.D.:
Dbtance Downstream from Flow Disturbance (Dbtance B):
                        inches / Stack I.D. -
           c
Dbtance Upstream from Ftew Disturbance (Distance A):
                 12?   inches / Stack I.D. « _£
Calculated By:_
                                              dd
                                                             Schematic of
                                                           Sampling Location
Traverse
Point
Number
/
2
3
4
5"
fr






Fraction
of
Length
O.PW
0.1W
O.llb
fi^oi
o.zsi
0.1M






Length
Onches)
H7,5











Product of
Columns 2&3
(To nearest 1/8")
2.01
£.?35
(1.'(,
*3.vy
4^ 5^^
•if.il

**
b7'*
'•/
33 >t
^•^
v*il






Nipple
Length
(inches)
10.1$



\
}






Traverse Point
Location
(Sum of Col. 4 & 5)
/a.^ 'Z-^
/7.^5 /7-fg
^y.^/ ^i34
4*/,/^ 4f tytt
j/.s/5 s-/ H
Zt.lt, S6, Vo







-------
   Duct Diameters Upstream From Row Disturbance* (Distance A)
 0.5           1.0           1.5           2.0           2.5
50
40
30
20
 10
         I
I
T
r
T
             24
                 16
                           20
          I
J_
 I
                 16
      Velocity (Non-Particulate)   [  12[
 I
 _L
I
I
                                12
                                   8     ~"
 I
 I
   2      3      4      56      7      8      9     10
   Duct Diameters Downstream From Flow Disturbance* (Distance B)
   • Rom Pbhrtof Any Typ« el DMutbwtM (Band, Expmton. Contracted. *to)
           LOCATION OF TRAVERSE POINTS IN CIRCULAR DUCTS
          (Fraction 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

Number of Traverse Points on a Diameter

4
0.067
0.250
0.750
0.933

•>






6
0.044
0.146
0.296
0.704
0.854
0.956


*



8
0.032
0.105
0.194
0.323
0.677
0.806
0.895
0.966




10
0.026
0.082
0.146
0.226
0.342
0.658
0.774
0.854
0.918
0.974


12
0.021
0.067
0.118^
0.177
0.250
0.356
0.644
0.750
0.823
0.882
0.933
0.979

-------
             GAS VELOCITY .CYCLONIC, AND VOLUMETRIC FLOW RATE
Plant:
Sample Location: &a"*iyO'J*
Run No.: C».t.Wu. *\
Pbar, in. Hg: eS^ , ^
Moist, %: 3 q •*
Stack Dimension, in. Dia. 1 :
Wet Bulb. °F:
,0. Xfv\<£\ Clock Time: /«3C*P
JMI-X ^-«U»tcVC. Operators: ^S^Y^
Static Pressure, in. H2O: ~«^O
r.O <2.*A Pilot Tube, Cp: . gj*f
y?*Zt " Dia- 2: " — '
	 Dry Bulb. °F: 	
Traverse
Point
Number
ft 1
^
3
4
5
^



















Velocity
Head, in.
H,O
. "*»cr>
/.GO
^t>fc>
->
-------
        Plant!
                       GAS VELOCITY AND VOLUMETRIC FLOW RATE
                                                   Date:
Sampling Location:.
                                                           Clock Time:
        Barometric Pressure.Tn. Hg:   JS.^Q       Static Pressure, in. H^O:
        Moisture, %:_^_s_2o_ Molecular wt, Dry^.T'
        Stack Dimension, in.  Diameter or Side 1:     ^ ~? £
        Wet Buib.o*    -             Dry Bulb,°F:_iIZ
                                                   PitotTube,Cp:.
                                                   Side 2:.
A-Wx,
           T
            Point
           Numbw
          / O '. O I
          /o : o 3
               . DC*
           /o /-?
                     /. .2
                      /••id
           ^SF-
                         Stock
                         Twnp.
T«-
               Md - (OaxXCOj) -I- (OJ2X%0^) + (O^axXNj)

               Md-(044x    ) + (OJ2X   )4-(02BX

               Md-                       CD
                                                       100
                                                         too
                                            TS
                                             V»-65.48 X(
                                             w-
                                             Q«-V«xA«xeo«/m
                                             QB-
                                                             lxt
                                                           xeo
                                                   p.     %H.O
                                     Qi ..-Qtx 17*47x	x(1	-A-)
                                       •»           Tt       100
                                             ^rti-
                                                X 17.647 X-
                                          •X(1-
                                                                             100

-------
GAS VELOCITY AND VOLUMETRIC FLOW RATE
Plant ^ov---"-^ u.x»^e- ^luie^v^ J Date: Ce-^av-*?s?
Sampling Lo
Barometric F
Moisture, %:
Stack Dimer
Wet Bulb, °F
TfWWM
Point
NUTMMT
yC5/S?
/<^ f «V
//*\ i ^i * I ^>
;o iVio
i^K.-qS
to 
ICJO • &
iru^- *^
/o^v
10 J- -L
IO J-^>















cafion: ^r^=.Vs«L3*^ ii^v=.«r. ~^ Clock Time: c^ -5S - ia>~
;^vv^~ -fV^v-SVorV. Onerators: "NCSXS. f^c^*^
'ressure.lh. 1
3-$
Ha: ^CT.^O Static Pressure, in. I-UO: -^C5
Molecular wt.Drv! ?^.o^ PitotTube. CD: . S*^
ision, in. Diameter or Sid
r. 	 rjjv

Hud
1 . t£ O
/ . ^zo
. -go
.-Q,.
.C.,-5
. -?f^
. -a,^
-5^0
1 . .i
1 ^
1. Ji














£F-
Stack
Twnp.
°F
^S9"^
•5.0CN
^&>0
J?^}^
J)^J
-3JiO
ji^^
^ O "7
:> /e>
A/G
^ i~>














T«-

9 1 : Ll~? ^ Side 2: —
Buibt°F:
Md - (QA4xXCOy) -I- (OJSZK%02) + 
-------
Ptant  dU&uLic^l
Sampling Ijocation
Run Number:
FIELD DATA SHEET
               Operator:
                                         Sample Type:
                                         Pbar:
Pretest Uak Rate:
Pretest Uak Check: i
cfmi
•'
                            is" In. Hg.
                         Orsaf:
Probe Length/Type: 5'
Stack Diameter:
Pilot *:
Nozzle ID: sm - .Ji"7Thermocouple
Assumed Bws: ~]   Filter #: _
Meter Box #: mfo ID Y: l.tO\
Post-Test Uak Rate:  .aen cfm
Post-Test Uak Check: Pilot:
                                                                  in. Hg.

-------
                        SAMPLE RECOVERY DATA
PLANT

DATE
                        Sample Box No.
                                              Run No. tAl3~  1 ~

                                         -$*   Job No.   ^^ • OO3
SAMPLE LOCATION
                                              Filter No.
TRAIN PREPARER    C-C-/  1> H
SAMPLE RECOVERY PERSON
COMMENTS

FRONT HALF
Acetone
Container No.

Filter
Container No.

Description of Filter
                            Liquid
                            Level Marked
                                               Sealed
                                               Sealed
Samples Stored and Locked

BACK HALF/MOISTURE
Container No.        	
 Liquid Level Marked
                                               Sealed
    IMP. NO.
               CONTENTS
                           INITIAL VOL
                              (ml)
                                                  WEIGHT (grams)
                                        INITIAL
                                                     FINAL
                                                                  NET
                            \0 -0
                                                   725,1
                 PT f
                                          M. 1
                                                    522.9
                5/6-
                                       325-^
          TOTAL
 Description of Impinger Catch:

-------
       Appendix A. 2




      Raw Field Data




Vertical Kiln Baghouse Outlet

-------
Plant:.
Date:
        TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
                        Co
Sampling Location:	^
Inside of Far Wall to Outside of Nipple:.
Inside of Near Wall to Outside of Nipple (Nipple Length):,
Stack I.D.:	«9* V      (
                                             rtm"t?
Distance Downstream
                        w Disturbance (Distance B):  -
                         inches/StackI.D.-  ^»l dd
Distance Upstream from Flow Disturbance (Distance A):   ^  -*,
               "^  >^*   inches / Stack I.D. - &a&1 dd
Calculated By:_
                                                              &
3
                                                              Schematic of
                                                            Sampling Location
Traverse
Point
Number
i
3
s
^i
5
\c
7
^
1
10
n
U
Fraction
of
Length
, Cu I
. (h/^*7
, //S
» /•>*»
• JSC5
S5^
. f/2/
• 75O
.«^S
.W
.^55
.^7^1
Length
(inches)
-^^^
^ «-5
^'^
1^
4*^
'/?^
*l8b
^^
«rt5
^^
^^
^^
Product of
Columns 2 & 3
(To nearest 1/8")
/•o^ i"
3,-J-S 3^'
S . 73 5%
g.S'g 2%
O. / "5 /j-^
/7. P-7 ,7^
3 ; • P 3 3i^
3fo.3^ y^
39. ^^ J?^
-/2^¥^
^5^^ ^
-«/7.-f PV7-
Nipple
Length
(inches)
L









\









/
V
V
i
Traverse Point
Location
(Sum of Col. 4 & 5)
*/"
fa-h
s%
//•%
/5^
^o^t
3*1 ^ '
17 ^^g
33~^
4€ ^?
tz^
50^"

-------
        TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
Plant.
Date:
                              Co
                               .,r e
Sampling Location:  /fi I ^   BA C ,
Inside of Far Wall to Outside of Nipple:.
Inside of Near Wall to Outside of Nipple (Nipple Length):
Stack I.D.:
Dbtance Downstream from Flow Disturbance (Distance B):
                        Inches / Stack 1.0. -  f-3/ dd
Dbtance Upstream from Flow Disturbance (Distance /^:
                 l>^   Inches / Stack I.D. - 7.fef dd
Calculated By: _
                                                             Schematic of
                                                           Sampling Location
Traverse
Point
Number
I
•a,
3
4-
/
C
7
?

• #s t
, ^33
\ °ll°i
Length
(inches)
4- "7 Vfc











Product of
Columns 2 & 3
(To nearest 1/8^
/
3 *'»
s fy
% >4
n 3Ai
\y3^
10%
3S%
2£7/&
*ll*b
W
uyn
Nipple
Length
(inches)
Z.











Traverse Point
Location
(Sum of Col. 4 & 5)
3
5'/£
7f%
/***
13 ^
l&3*+
zzty
37**
w ^
wty
^
Hb*\

-------
             GAS VELOCITY .CYCLONIC. AND VOLUMETRIC FLOW RATE
Plant:
Sample Location:
Run No.:
Pbar, in. Hg:
Moist, %:
Stack Dimension, in. Dia. 1:
Wet Bulb. °F:
Date:
Clock Time:
Operators:
Static Pressure, in. HjO:
Pilot Tube, Cp:   	
Dia 2:          	•
Dry Bulb. °F:        -
Traverse
Point
Number
fi ,
J
3
«
Jfo
/C^
3,
^
~J
o
o
<^5
r~5
-6s
-o?
o
o
3>
r^>
<*^
n
~«o
r"^
"Co
%3o
-3o
•^JX

Directon
of Angle

























          sq.rt. dp   Stack Temp    Angle,'
Average |
                                                                Md - (0.44 x %C02) + (0.32 X %02) -t- (0.28 X %^)

                                                                Md - (0.44X      ) •»• (0.32X     ) + (0.28X      )

                                                                Md-
                                                                             % H,0        % H20
                                                                             _._, + 18(-j55-)
                                                                          13.6
                                                                 Pa .            in. Hg
                                                                                              13.6
             Vs - 85.49 x i
                                                                 Vt - 85.49 X (
                                                                       .49 x Cp x <]& x U	pj1
                                       Pax Ms
                                                                 Q«-VtxAax00a/m
                                                                 Qt-
                                                                 Qi-
                                                                                              xOO
                               aefm
                                 Pa
                                                                                    p,      %H,0
                                                                                       x1.-
                             Xl7.e47x-

                               oacffn
                                                                                                             too

-------
             GAS VELOCITY AND VOLUMETRIC FLOW RATE
Plant
»
Sampling Lo
Barometric F
Moisture, %:
Stack Dimen
Wet Bulb, °F
TrawtM
Point
Numb*
/^\ »
j
•$
^,
5
C,
7
^
Cj
/to
/ i
t*
/V |
iT^ 1
j
3
V
s
r«
7
2
^
/t?
/ i
U
^MMMH^HMHM^MM
cation: P^c.W^<^ r>. iv v j^ s-^c^t Clock Time: OQ y<^
\.-.^v.^.^0 -f\^,.^>L.., A^V? Oneraters: ^^x\\ ^lJL^-^
'ressure, in. 1
Hen^ JIA ,-s ° static Pressure, in. K^O: - . ?»«^
y_ Molecular wt. Drv: 3^.o-> PftotTube.CD: .**,
sion, in. Diameter or Sid
'- Dry

HMd
1.4^
/ /.r
/ ^
/.•So
/.^^
/ ^O
/./<^
/. J?O
/^^
.^0
•_^
^^-
1 * / ^-v
/.^r-»
(. -^r-s
/ . .3.O
;.Jir-.
/. IO
>.Jo
/.JJO
J.^o
/. 20
i>2o
/. <5O

^SF-
Stack
Twnp.
°F
*AO
^s\
1 \*1
UlF
;M->
J /&
«=? 1?
<5>J\
^5)
PJ?<


^0^
=2 / J
^J^
32V
224
££S

^<20

T«-
e1: ^/7.2^ Side 2: 	 —
BuIb.°F:
Md-(O44x ) • LM vM. 1+HI/ 1
.., 100 100
'Co
*^ 100 100
5 Ms-
-^ oo
o - _. IP.
o ' «- . « .
o P«- In-Hg
^ fip-
" ~ ~ / T«f*R)
^ y— ^^*V p-«-i
C^ ^^^^"^^"*
^ ( V
0 Vb- ft*
o
o *•• *
o
..^ 0»« x xeo
"do Q»» «dm
-30 p. %K.O
-ov> Q"— " Q»X17*47X 	 x(1 	 -*- )
ef& ««B TB 100
•to too

-------
GAS VELOCITY AND VOLUMETRIC FLOW RATE
Plant* i_K«?"» ."tr.v v VVJL>^«- £,,., *x£>e>-*. <. /HtrLu /•**& Date: ( a ~*3 *-/ "^y
Sampling Lo
Run#: f^i.
Barometric F
Moisture, %:
Stack Dimen
Wet Bulb, °F
TnvtfM
Point
Numb*
fl ^
























O
cation: R^-W^-^ f^rr*-^ :5-fe^t_ Clock Time: /fS<> -j
.^.~. r. iiti«r;K. £V, «.^.. Onerstors! r^>fc>Vk fctO":^
•ressure, in. i
to: Ip^.,300 Static Pressure, in. HUO: --So
Molecular wL. Drv: 3p . o ^ pftot TubeTCo: - &/
sion, in. Diameter or Sid
•i r^nf
e1: 
jx ; 7
-3> 7
J>/~?
J i \.
^ 1 1
J M
bl ll
^ 1 1
J 1 0
J.II
4 /4
J/^
J/L
, J^0
J)6!
*J / "7
y^
Tt- ^,^
Md-(044x )-f(O32X ) + (0i8x )
Md-
%H.jO %H2O
kto-
^_ o o» o 	 ^
PB • kv MQ
»
£F-
— / T«^fl)
V* - «s.40xCpx JSF x y — ptxut
Vs»65.48x( )X( )Xll
A*- ft2
Ot» x xeo
Q»» aefen
no 100

-------
                                              FIELD DATA SHEET
Plant  C V^
                            Coi»if*»-<
Sampling Location Bt\k
Run NumtwPoA      Date
                            GUI Ml
                            Sample Type:
                            Pbar: >0\ ^
                            CO2:
                                     Operator:  C^/f 3     Nozzle ID:
                                                    ><•
                                 Ps:	~ .
                                 O2:
                                                                                                Thermocouple #: ~T
                                                                                Assumed Bws:  £  Filter #:   — — - >JQ
                                                                                Meter Box #: £oig/S Y: (,QO AH@:   t.f
Pretest Leak Rate:
          cftn @ \5 in. Hg.
Pretest Leak Check: Pitot:  y/ Orsa|L  W
                 Probe Length/Type:  (,
                 Slack Diameter:
                                                                   Pilot #: 6
                                                                As:
                                                                                Post-Test Leak Rate: ,QQ<|^ cfm @ J_Q_ in. Hg.
                                                                                Post-Test Leak Check: Pitot:   \/ Orsat:
Traverse
 Point
Number
     Samplng
      Tim.
      (mln)
            CkxJdlnw
             (24-hour
           Gas Meter
            Reading
            (Vm)ft3
              Velocity
             Head (Ap)
              inH2O
Orifice Pressure Differential
    (AH) in H2O
                                               Desired
                                                         Actual
Stack
Temp.
 (Ts)
Temperature
   °F
                           Probe
      Filter
knpinger
 Temp.
  °F
Dry Gas Meter Temp.
  Inlet
(Tmln0F)
  Outlet
(Tmout°F:)
 Pump
Vacuum
(in.Hg)
        0
                                  y////////////////////////// //'/////////////////////////////
       15
                        1
                                                                                         cy
                                                                                                          10
                                                                                                    7
       IS
                           .0
                                                          \A
                                                                                  4-7-
                                                                                                     7
              •v,
                                                                                                         f /
                                                                                                               -Z
                                                                                                                 7
      37
                                     \ A
                                                                         osc.
                                                                                                         •17.
                                                                                                    3-
                                      \±:
                                                _2L
                                                           I.-1!
                        JL
 '0
              VVfc
 :JL_
                                                    - 3
                                                          2 J
                                                                                          £7.
                                                         ITT
                                                  2-1
                                                                                                                       ^"3
                                                                                                                       ss
                                                                                                                         7
                                                          -H-
      io.
                            ji_
                                                                                                         13
ULL
°\o\.\
                                      l.i-
                                                                                        (fO
      14-a.s
                                                         ^4-
     \So o
                                                i-
                                                                          >S
       ts
                                                                                                   *\\
                                                                                                                 D
                                                                                                                      J"
                                                                                                   e\\
                 AVm»\MAVV
                                                                                               Tm=

-------
                       SAMPLE RECOVERY DATA
PLANT

DATE
                              Run No.
                                                          - Q - \
                       Sample Box No.
                        <0    Job No.
                                                           . QO5
SAMPLE LOCATION
TRAIN PREPARER
      Oint
                            VO
                                  -16*1.1
                                      3m
           TOTAL
 Description of Impinger Catch:

-------
                          FIELD DATA SHEET
Plant: t,^« w\xC»^ Vv^
Sampling Location ^^
Run Number: "C ^>— \
Pretest Leak Rate : r^ o ^
Pretest Leak Check: PHot:
«_ t rt*P*-'A r\Mfc^
\X«i^ -^.<\\
cfm @ \S in- Hg.
\MYN Orsat: .IN A
^v Sample Type: Wi-"1}
Pbar: VvVO Ps:
CO2: rJ (\ O2:
Probe LengbYType: ^' C
Stack Diameter:
Operator: v
— .T»t>
fVn,
Lvw, P'tot *
As:
tS^b.

':U
                                                                           Thermocouple #: T 4
Assumed Bws: \o  Filter #:  K>0
Meter Box *:t»«n.S  Y:
Post-Test Leak Rate:
cfm
                                                                                          in. Hg.
                                                            Post-Test Leak Check: Pilot: ^ Orsat:
Point
Number

























Samplng
Time
(mln)

























CtockTime
(24-hour
dock)

























Gas Meter
Reading
(Vm)ft3
°\ V4 . TO 0
























Velocity
Head (Ap)
inH20
Orifice Pressure Differential
(AH) in H2O
Desired
Actual
Stack
Temp.
(Ts)
Temperature
°F
Probe
//////////////////////////// '//'///.








































































...
1










































Filter
'//////
















#
)
r





knpinger
Temp.
Y////
























Dry Gas Meter Temp.
Inlet
(Tmbi°F)
Y/////
























Outlet
(Tmout°F)
t J S J f S
Y/////
























Pump
Vacuum
On.Hg)

























                                                                                                       ,*»
AVm=
                               AH=
                                                                          Tm=

-------
                       SAMPLE RECOVERY DATA
PLANT

DATE
                                             Run No.   M3.3-
SAMPLE LOCATION
TRAIN PREPARER
   Sample Box No.

       a/> K
                                             Job No.  RO)2
                                             Filter No.
T.
                                J
SAMPLE RECOVERY PERSON  T,

COMMENTS
FRONT HALF
Acetone
Container No.

Filter
Container No.

Description of Filter
        Liquid
        Level Marked
                                              Sealed
                          Sealed
Samples Stored and Locked

BACK HALF/MOISTURE
Container No.        	
                                              Sealed

IMP. NO.
t
2
3
4
S

TZ^/.I,
•6/7//
73^^?
~3^/

NET
(9
^>
0
0
O
O
O
Description of Impinger Catch:

-------
        Appendix A.3




       Raw Field Data




CEMs Summaries & Strip Charts

-------
 HCI Correction Worksheet
         Marble Falls
       Chemical Lime
         25-June-98

          OUTLET
|| Actual value
zero
siid
; tJtgr*




0
46
303
3 Point Cal
1.1
47.4
300.8
slope (m) 0.988
Y-lntercept (b) 1.49
Avgconc: 15.5
Actual Cone: 15.8
Pre Bias
1.1

300.8
0.989
1.10


Post Bias
2.1

308.4
1.011
2.10


            INLET
Actual value   3 Point Cal   Pre Bias    Post Bias
zero
sift
r»gfc
0
46
303
1.9
44
299.4
slope (m) 0.986
Y-lntercept (b) 0.41
Avg cone: 20.9
Actual Cone: 22.7
1.9

299.4
0.982
1.90


3

296.9
0.970
3.00



-------
HCI Emission Measurements from a Vertical Kiln
       Chemical LimeMarble Falls Plant
             Marble Falls, Texas
                  6/25/98
Time

Date

Inlet/Outlet

HCI
ppm
THC
ppm
02
%
CO2
%

15:19-15:38
16:07-16:26
16:55-17:14
17:43-18:02
18:31-18:50
6/25/98




Outlet




Average
16.1
13.8
18.8
14.9
14.0
15.5
10.0
10.1
10.7
10.5
9.8
10.2
13.6
13.9
13.7
13.5
14.0
13.7
15.8
15.1
15.7
15.8
15.0
15.5

15:43-16:02
16:31-16:50
17:19-17:38
18:07-18:26
6/25/98



Inlet



Average
20.5
7.0
16.6
39.3
20.9
18.6
17.4
17.9
17.4
17.8
9.8
9.8
9.8
9.8
9.8
24.0
24.0
23.9
23.8
23.9

-------
c
f
»•» fEET flVEWCE U IS 61 >- 11. 1 -^n
'•» fElT AWWE :: u .Ji .2 17 1 FCT
/ _, ,, ,,;Uo 4
I J . , - * ,-•
*»« RESET RVEKflGE 12-12 8^ 24 - 1 RFII
1 *** RE?T AVERflGE 12 12.86 22 17 9 PCT
| - - - ' 1 1
1 , «** RESET AVERAGE 12 11.45 24-4 PWt
Ii , • ( ,...« i .--•"•
' ! F j ' «** RESET AVERAGE 12.11j8» 21 O Pljfl
. ! | «*» RESET AVERAGE 12 18:li 22 23 7 PtfT
! j ' m RESET fiVWflDE 12-18 84 23 -59|5 PCI
1 , *** RESET AVERAGE 12 18:84 21-8.5 PW-
«** RESET AVEROGE 12 «9.44 21-1 PW1
, , *** RESqr flVERflGE 12:87 83 24-3119.8 PP*
! ' ' ' •*» RESET AVERAGE 12 97:85 22-3119.8 PCT.
'
**•»» SVSTEM RESTRRT<32>
!
CO >T-ij «•
rc.-. M ir. r. ^o. o i:.. ^ :c; "• -" . • •
co avii »*«
oznvp *•» ; «
! '
C0fl« **»
; NKCIjVfi • • ! *«f ' i r
	 n- 	 ,),-----! ~~T~™ 	 " ' " Ui"1 ' T ri 4 ' -
	 . , i . . , 	 i . i . i . . , ,.,.•.,, 	 	 	 ,.,,F,]~ t~-£- ?J*^--.
1 i)2 flVC ***
' ' ' i • i
NOXIJVG **f i ' ' . '•
	 ' ' ' '! ' ' •' li •!? i? *5 2
NOXffVG **» , : !
! : ' j 12 87 i4 a I
; '• , ' ! U «? « 22 1
CO flVS **« : i
02 (WG **» ' i i
	 	 •••-;-- -.-...--. - - li « 24 02 4
12:06:20 JUN 25/98 *** . /
! ' ' 12 •>» :» at 2
12*00 02      '
.us     ~eJ e
                                 25. e
                                                                                     i-5.. e
                                                                                                              175.. O
200. o
                                                                                                                                        225. 8
                                                                                                                                                         en
                                                                                                                                                           9  PFM
                                                                                                                                                          .1
                                              «« RESET ftVERfCE 12.46 88   24 I B8E+:8 Frit
                                               «« RESET ilVOftl 12 4* X  22 L 88E+38 PCT
                                                                                                                                                           : 11 54 *•» >W :
                                                                                                  COflVO
                                                                                                  02 flVC
                                                          •»-»•»  SYSTEM  RESTflRT<32>    12:45:25  JU^4 25/98

-------
                                                                                                                      -L U
-air
 IB
««* RES£T flffRffi^ 12.;« 82j  24  18(5   PF*
 *»* RESET fWRMfc 12 36:4  23 6.6    PPM
»*. RES^T (WERflCE 12:36 82)  22  14J8   PCT
 **« REjIBVERftGE 12 16:9?  21 14.2   KT
                                                                              THC,fMI
                                                                             CKffJG
                                                                              02 R
                                                                  25.
                                              !/:•::
                                               i .'•'   i
                                         : «« RESET fWRflCg 12:24.8t
                                                     12:24.91
                                         • m REST flVTOtt 12 24:9^ 21 11.2   P>:T
                                    38. j 0    I
                                                                                         '--f
35., i
                                                                                                  i   -4Q.I0
                              Yi     !
                  24 8.1
                                                                    PPM
                                                                    ret
                                                                                       i  •   I
                                                 ***;
                                                  *»»
                                                                       45. i
             *** LOO ORP 1  ***  UNIT  81
            «.. «. jnL^-J-i. .......
                                                 *** STRUTS flT  12:23:13 *** ENDS flT 12 : 23 : 14 JUN 25,99
                                                                                                                                *  mm
                                   50. 0   PPM
                                                                 -
                                                Hgy     ;PT MTB  UN^S__ST	_JJI*__


-------
 B
13 88 87  —
            34
             I.  *
 • • -t.i  M.cN.i i. :: i?  _.  ', i    t»\
• H i^ET rtilix/S. L ;i -J.   ^  : 3    Pi'T
•«« ?£."£' rtVEFWE II i: 02  a  I.1 -"   FCT
                                                                          _"t.. y
                                                                                       .n. Aj
                                                                                      V£. IWG
                                                                                       02 flVD
IM

 Kt

• • , •• — — — 	 . 	 ~,
_ — - • • • •*•* *
r7 	 -•;, / 	
'I
, \
1 i
l
tl
ej
'f
it

i*
PT
*
il
i. e
1
*-
EL
i.-ii
* itr""i~.— ~- .*-^~" '
" ' — •"*& . V~
; «*« RESET fiVERflCE: 13:08 831 24 5 ? PFU
«*« UESET RVEPftt 13 98 -8J 23 1^5 PFtt
! *** KSET RVERflGFJ 13.89.631 22 U.4 PCI
i • «* RESET ftVEBtt 13 98:8^ 21 1< 4 PCT
l :-. 5 Pt o 7pt~~~-1 — u^^rigr1 12i "H"
\8BR 8Z-C, , : !
•P ~ 	 	 -----?. : • , >•'
/ ' : • \ : y
' "• •- , t=t — '
	 h 	 	 *™:u 1':K-' 	 J— 	
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i
: i
»=*= LOI3 GRP 1 *** UNIT 01 *** STRRTS RT 12; 48
OfiTR UNITS ST LEGENJ PT CflTFl UNITS ST LEGEW .PT
21 5: ;: oa 92 2 PCT coz [83
1 25. 0 70. 0 IttSi 0 " ' 140. 0 175. 0
*** RESET RVERFCE 12.48. 8S 24 5.3 PF1
«** RESET RVERflCE 12 48:82 23 43 5 PPM
«« K£ET RVEffiGE U'.48.82J 22 5 8 KT
»» RESET HVEKflGE 12.48. 9Z ^. 19 3 FtjT

»•* LOG ORP 1 *** UNIT 01 *** 5TRRTS RT 12:46
OflTR 'JNITS n LEGEND PI DWfl WITS 5T LEGOIi PT

»* LOG ORP 1 *•»* UNIT 01 *•»••»= STRPTS RT 12.44;
VTM UNITS ;T UljEMQ FT ^Tfl UNITS JT UCflff >r Ff
M ,'"••'' ",t>'' " i " • -n" ' 'i A ^-
'•— - — .-- 	 s ;
HCLfflfc ' «**i i
THCA'G • «** , .
C02flVC *«| ' i
i32 RVC *^ ; i
" •- iL5. 0 17. 5 2Oj O 22. 5 25J 8 PCT
J . , • : l
t f .1
, 	 ., , , L, '
i : ''• i
;4-2 *** ENDS RT '12:48:48 !JUN 25,98 *** ,
WTft UNITS SJ LEGEM) PT MT8 UNITS 5T , UKBSl
3Z? PPh THC ' 84 2.9 PPN *L
210; 0 245. 0 280] 0 ^ 215.' 0 350; 0 PPM
naw ***
THC ftVG •*» , ,
C02 RVG *<*
02 RVG >*»
•^ , ',
. 42 *** ENDS RT 12 : 46 : 42 JUN £5, 98! ***
CflTfl '.HITS ST LEGE* F'T WT» UNIT? ST LEGEND
9 PF'H THC 94 3 2 Ff« HCL

-------
«i. LUIJ • '!-("• L «•' uriir yL »••••> irnFis HI" i-^^X"*!
•fl* j^r _,.,,, ,WIt, -[ LOTS fi t+iTrt _ WIT: JT LEGEND ...QjT MT*
4* >A .1 . •; 02:; £ - f'-f -^ \^ja
;/
'/ .... 	 	 - - -
,jf- 	 	 —"
*** LOG "3RP 1 •»•** UNIT 01 *** STRRTS flT 13 : 44 38
^ PT DflTft UNITS ST LflGENO PT DflTfi UNITS ST LEGEHP . .FT WTft
.*& ^^ ri unin UHIIJ -M _„, _ ,™Sssfls.rl.— .-- — — . — >• - - — — *- — — 	 	 • 	 * — ,
v ^P V : ;: "" W, 83-
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r ;
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1
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25 51 & T, 5 10i 0 , 12. 5
, '
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i 1 *

i • ' ! «*RB^T flVKflGE 13.36. B8J 24 91 ' Pff •
! , *«* RESET flVERflGE 13.36:8f 23 S,2 PPM
tw RO6T HVERflGEi 13:34.81' 22 6 PCT .
! *** RESET flVERflct 13:3S:8* 21 ^4 PCT
! : ' i
m M

'i
!l
r
ri
|
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• ' X.
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-------
            APPENDIX B




METHOD 23 LABORATORY ANALYTICAL DATA

-------

-------
                           LabData

             Summary of Method 23 Analytical Results
                  Air Emissions Screening Test
           Chemical Lime Company - Marble Falls, Texas
             US EPA Test Method 23 - PCDDs / PCDFs
            Vertical Kiln Baghouse Inlet - Run M23-1-1
Congeners

DIOXINS:
2378 TCDD
Total TCDD
12378 PeCDD
Total PeCDD
123478 HxCDD
123678 HxCDD
123789 HxCDD
Total HxCDD
1234678 HpCDD
Total HpCDD
12346789 OCDD
OCDD+Totals PCDDs

Back Half

0.0146
1.247
0.0181
0.477
{0.0098}
0.0155
0.018
0.388
0.0301
0.0588
0.0364
2.2072
Catches, ng/sample
Front Half

{0.0025}
0.1092
{0.0034}
0.0744
0.0028
{0.00536}
0.0072
0.1384
0.0208
0.0376
0.02
0.3796
Total

{0.0171}
1.3562
{0.0215}
0.5514
{0.0126}
{0.0209}
0.0252
0.5264
0.0509
0.0964
0.0564
2.5868

FURANS:
2378 TCDF
Total TCDF
12378 PeCDF
23478 PeCDF
Total PeCDF
123478 HxCDF
123678 HxCDF
234678 HxCDF
123789 HxCDF
Total HxCDF
1234678 HpCDF
1 234789 HpCDF
Total HpCDF
12346789 OCDF
OCDF+Totals PCDFs
Total of Totals
0.17
9.696
0.109
0.134
2.391
0.129
0.048
0.0343
0.0096
0.460
0.0469
{0.0049}
0.0616
0.0066
12.6152
14.8224
0.0184
0.6276
0.0198
0.024
0.3208
0.0323
0.0132
0.0114
0.0031
0.1076
0.0215
{0.00232}
0.0244
{0.00308}
{1.0835}
{1.4631}

0.1884
10.3236
0.1288
0.158
2.7118
0.1613
0.0612
0.0457
0.0127
0.5676
0.0684
{0.00722}
0.0860
{0.00968}
{13.6987}
{16.2855}
{ } Estimated Maximum Possible Concentration.  EMPC values are included in totals.
                                                                      ooo

-------
                 PARADIGM ANALYTICAL LABORATORIES, INC.
                             2627 Northchase Parkway S.E.
                          Wilmington, North Carolina  28405
                                     (910) 350-1903
                                   Fax (910) 350-1557
24 July 1998
Michael Maret
Pacific Environmental Services, Inc.
5001 S. Miami Blvd
Research Triangle Park, NC 27709-2077

Contract-          68D70002
Sub-Contract:      R012-002
Work Assignment:   1-007

Subject: Polychlorinated Dibenzo-p-Dioxins & Dibenzofurans Measurements (PAL Project No. L-1070'i

Dear Mike;

        Enclosed are the final results for the flue gas samples under your Project R012.003 Texas Lime
Kiln.  As you requested, we divided up the set of 17 samples into three separate projects (L-1070, L-1071,
and L-1072). This report covers the first set under PAL L-1070. The analytical procedures conformed or
exceeded the ones described in Method 23 using isotope-dilution high-resolution gas chromatography
combined  with high-resolution mass spectrometry. The Level n reporting format is described on the next
page. A general summary of the analytical results is presented in Table 1. Tables 2 and 3 summarize the
results for the front-halve of the four inlet samples, expressed in absolute amount "ng" per sample,
and in relative concentrations "part-per-trillion" based on the weight of dust collected. Figures land
2 show the TEQs and total homologues corresponding to Table 1 data.

        No. of  Samples Received:         4
        No. of Samples Analyzed:         5
        No. of Lab. Method Blanks:      1

        Your Project Number:          R012.003 Texas Lime Kiln
        PAL Project No.:               L-1070

        Remarks:
                •   Data  meet QA/QC requirements with the exception of sample M23-I-1 for which the sampling
                    standards recoveries for four out of five standards are lower than the 70 percent limit. No simple
                    explanation can be offered here for this observation.
                •   The FH of sample M23-I-1 contained 15.6 g of dust, and was processed as a separate sample. The
                    results are reported in two ways:
                        a) Absolute amount in "ng" per sample,
                        b) Relative concentration in parts-per-trillion (ppt) based on the weight of dust.
                •   No analytical difficulties to be reported.	


        We wanted to thank you for the opportunity to serve you. Please, feel free to contact us if you
 have questions or should you need additional technical support.

 Sincerely,
 Yves Tondeur, Ph.D.
                                                                                           TOO    O
                       North Carolina Wastewater Certification #481

-------
           Project No. R012.003; Project Name: US EPA Lime Kiln Screening, Texas Lime;
                               Sample and Project Identifications.
        PES Sample ID
       PAL Sample ED
       PAL Project No.
M23-I-1
M23-O-1
M23-FB-1
M23-RB
1070-1
1070-2
1070-3
1070-4
M23-I-1-FH (DUST & FILTER)   1070-5

M23-I-2                         1071-1
M23-O-2                        1071-2
M23-FB-2                       1071-3
M23-I-2-FH (DUST & FILTER)   1071-4

M23-I-3                         1072-1
M23-0-3                        1072-2
M23-FB-3                       1072-3
M23-I-3-FH (DUST & FILTER)   1072-7
M23-I-4                         1072-4
M23-O-4                        1072-5
M23-FB-4                       1072-6
M23-I-4-FH (DUST & FILTER)   1072-8
L-1070
L-1070
L-1070
L-1070
T-1070

L-1071
L-1071
L-1071
1-1071

L-1072
L-1072
L-1072
L-1072
L-1072
L-1072
L-1072
L-1072
                                           Level II Report
        Section 1: Cover Letter, contains a brief description of the project, the client and PAL Project
                  Numbers, the number and type of samples, the methodology used to process the
                  samples, QC remarks where any analytical difficulties are discussed and the impact on
                  the quality of the data presented, a summary table with the analyte concentrations,
                  detection limits, the client sample identification numbers, units to report the
                  concentrations, and a graphical representation of the TEQs and totals.

        Section 2: Project Synopsis, contains the Sample Tracking & Management Forms,
                  Communications Form, any correspondence, chain-of-custody and the last page is
                  always a copy of the sample injection log(s). This section is designed to help the
                  laboratory and the data reviewer with an overall view of the entire analytical
                  procedure, the initials and dates of who did what when on which sample. Spiking
                  solution IDs are recorded along with the batch numbers of the supplies and reagents
                  used.

        Section 3: Analytical Results, contains the sample results topsheets (one set of two per sample),
                  the raw data (i.e., the selected ion current profiles, the areas, heights, ion abundance
                  ratios, signal-to-noise ratios, and retention times of the GC peaks).

        Section 4: System Performance, contains the documentation on the GC/MS system performance.
                  In particular, the mass resolution checks, GC column performance checks, initial and
                  continuing calibration summary tables and, when applicable, associated raw data for
                  both column types.
                                                                                         f'    002

-------
Table 1: Analyte Concentrations in "ng" per Sampling Train
               (FH of the inlet sample shown in Tables 2 and 3).
•*^#^ '^"^^^^^^^^^pjl^^B
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF"
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
Total PCDD/Fsb
TEQ (ND=0)C
TEQ (ND=l/2)d
TEQ EMPC(ND=0)e
TEQ EMPC (ND=l/2)

[0.00094]
[0.00052]
(0.001)
(0.001)
(0.001)
0.003
0.009
[0.00104]
(0.000)
(0.000)
[0.00112]
0.001
(0.000)
(0.000)
0.003
(0.001)
0.002
[0.0009]
[0.0004]
[0.0016]
0.003
0.001
(0.000)
0.000
0.003
0.019
0.000
0.001
0.002
0.002
•1
0.015
0.018
[0.00976]
0.016
0.018
0.030
0.036
0.170
0.109
0.134
0.129
0.048
0.034
0.010
0.047
[0.00492]
0.007
1.247
0.477
0.388
0.059
9.696
2.391
0.460
0.062
14.822
0.139
0.139
0.140
0.140
|if|||9Hj
BB
0.012
0.009
0.003
0.005
0.004
0.007
0.024
0.160
0.087
0.086
0.047
0.017
0.011
0.004
0.017
0.002
0.010
1.102
0.264
0.116
0.013
9.120
1.590
0.166
0.023
12.428
0.090
0.090
0.090
0.090
H
[0.00095]
(0.000)
(0.001)
[0.00092]
[0.00088]
0.004
0.016
0.003
(0.000)
(0.000)
0.001
[0.00044]
(0.000)
(0.000)
0.007
(0.001)
0.006
0.002
0.002
0.004
0.008
0.011
[0.0016]
0.002
0.007
0.058
0.001
0.001
0.002
0.002
M^^^^^^BIwH
0.001
(0.000)
(0.001)
[0.00096]
0.001
0.003
0.010
(0.001)
(0.000)
(0.000)
0.001
(0.000)
(0.000)
(0.000)
0.003
(0.001)
0.003
0.001
(0.000)
0.002
0.003
(0.001)
(0.000)
0.001
0.003
0.023
0.001
0.002
0.002
0.002
 a) Result obtained from the DB-225 analysis.
 b) Total PCDD/Fs represent the sum of all polychlorinated dibenzo-p-dioxins & dibenzofurans.
 c) TEQ computed using ITEF and setting non detected analytes with a "Zero" concentration.
 d) TEQ computed using ITEF and setting non detected analytes with a concentration half the
   calculated detection limit.
 e) TEQ computed using ITEF and setting the concentration of EMPC analytes to the EMPC value.
 NOTE:
        ( ) = ND using DL value.
        [ ] = EMPC value.
                                        06 AUG 98 Revision

-------
 Table 2: Analyte Concentrations in "ng" per Front-Half Sampling Train (i.e., filter and dust) for aJl runs.

2,3,-7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF"
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
Total PCDD/Fs"
TEQ (ND=0)C
TEQ (ND=l/2)d
TEQ EMPC(ND=0)'
TEQ EMPC (ND=l/2)
mmmimmam
E9HBnn|HKg5SH
^3sR9flH|H^HBEiH^^H
Bp^B^HKgM^^^^^BBB^^^^^B
[0.0025]
[0.0034]
0.0028
[0.00536]
0.0072
0.0208
0.0200
0.0184
0.0198
0.0240
0.0323
0.0132
0.0114
0.0031
0.0215
[0.00232]
[0.00308]
0.1092
0.0744
0.1384
0.0376
0.6276
0.3208
0.1076
0.0244
1.4600
0.0220
0.0230
0.0270
0.0270

[0.00156]
(0.0003)
(0.0007)
0.0010
0.0016
0.0028
0.0060
0.0180
0.0184
0.0124
0.0102
0.0066
[0.00376]
(0.0008)
0.0061
[0.00176]
(0.0008)
0.0348
0.0060
0.0024
0.0028
0.3548
0.1644
0.0348
0.0092
0.6152
0.0110
0.0110
0.0130
0.0130
••
[0.00099]
(0.0003)
(0.0005)
(0.0004)
[0.00088]
[0.00168]
0.0051
[0.00124]
(0.0004)
[0.00064]
[0.0008]
[0.00032]
(0.0003)
(0.0003)
0.0006
(0.0006)
(0.0006)
[0.003]
(0.0003)
0.0016
0.0008
[0.001]
[0.001]
[0.001]
0.0008
0.0083
0.0000
0.0010
0.0020
0.0020
••••••BBjraHBBHI
[0.00108]
(0.0004)
(0.0007)
(0.0005)
[0.00108]
0.0018
0.0046
0.0126
[0.0044]
0.0052
0.0024
[0.00084]
(0.0004)
(0.0004)
0.0012
(0.0006)
(0.0008)
0.0012
[0.002]
0.0056
0.0016
0.0948
0.0280
0.0040
0.0012
0.1410
0.0040
0.0050
0.0060
0.0060
a) Result obtained from the DB-225 analysis.
b) Total PCDD/Fs represent the sum of all polychlorinated dibenzo-p-dioxins & dibenzofurans.
c) TEQ computed using ITEF and setting non detected analytes with a "Zero" concentration.
d) TEQ computed using ITEF and setting non detected analytes with a concentration half the
   calculated detection limit
e) TEQ computed using ITEF and setting the concentration of EMPC analytes to the EMPC value.
NOTE;
        () = ND using DL value.
        [ ] = EMPC value.
                                       06 AUG 98 Revision

-------
  Table 3: Analyte Concentrations in "parts-per-trillion" for the Front-Half Sampling Trains (i.e., filter and
                                            dust).


2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF*
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
Total PCDD/Fs"
TEQ (ND=0)C
TEQ (ND=l/2)d
TEQ EMPC(ND=0)e
TEQ EMPC (ND=l/2)
jswtmsMiam^^m
mntSnmwmtotNlfm
gflHE&HMaMjaiBSflj^^^R
[0.16055]
[0.21809]
0.180
[0.34381]
0.464
1.332
1.280
1.178
1.270
1.539
2.073
0.849
0.731
0.198
1.380
[0.14881]
[0.19756]
7.004
4.772
8.877
2.412
40.257
20.577
6.902
1.565
93.647
1.429
1.457
1.735
1.735
BBBi
IBi
[0.04808]
(0.009)
(0.021)
0.030
0.049
0.085
0.186
0.553
0.568
0.382
0.314
0.204
[0.11576]
(0.024)
0.187
[0.05419]
(0.026)
1.071
0.185
0.074
0.086
10.924
5.062
1.071
0.283
18.942
0.337
0.352
0.397
0.402
mu^mat
IBR
[0.07707]
(0.026)
(0.038)
(0.027)
[0.06843]
[0.13064]
0.395
[0.09642]
(0.031)
[0.04977]
[0.06221]
[0.02488]
(0.021)
(0.025)
0.050
(0.049)
(0.045)
[0.249]
(0.026)
0.124
0.062
[0.093]
[0.062]
[0.093]
0.062
0.644
0.001
0.042
0.129
0.142
«__-|
BB
PBBB8BBI
[0.03639]
(0.014)
(0.023)
(0.016)
[0.03645]
0.059
0.154
0.424
[0.1485]
0.176
0.080
[0.02835]
(0.013)
(0.015)
0.042
(0.020)
(0.025)
0.041
[0.054]
0.189
0.054
3.199
0.945
0.135
0.041
4.757
0.139
0.156
0.190
0.197
a) Result obtained from the DB-225 analysis.
b) Total PCDD/Fs represent the sum of all polychlorinated dibenzo-p-dioxins & dibenzofurans.
c) TEQ computed using ITEF and setting non detected analytes with a "Zero" concentration.
d) TEQ computed using ITEF and setting non detected analytes with a concentration half the
   calculated detection limit.
e) TEQ computed using ITEF and setting the concentration of EMPC analytes to the EMPC value.
NOTE:
        () = ND using DL value.
        [ ] = EMPC value.
                                           06 AUG 98 Revision

-------
                                       TEQ Summary Results
                 0.140 -f
                 0.120 -'
                 0.100 -'
                 0.080 -'
Amount in ng per train
                 0.060 -'
                 0.040 -'
                 0.020 -'
                 0.000
                         LMB1      M23-I-1     M23-O-1    M23-FB-1    M23-RB-1
                        R023-002   R023-002    R023-002    R023-002    R023-002
                                             Sample
                              Figure 1: Graphical representation of the TEQs
OTEQ (ND=0)C
HTEQ (ND=1/2)d
0TEQ EMPC(ND=0)e
BTEQ EMPC (ND=1/2)
                                                                                            OCG

-------
                                           Total PCDD/Fs Summary
                   16.000 -r
Amount in ng per train  8.000 -
                    6.000 -
                    2.000 -
                    0.000
                                LMB1
                              R023-002
 M23-I-1
R023-002
M23-O-1
R023-002
 Sample
M23-FB-1
R023-002
M23-RB-1
R023-002
                  Figure 2: Graphical representation of the totals (terra- through octachlorinated congeners)
                                                                                                  r     ccv

-------
                 PAL Project No.: L-1070
                                            12. -
                     Section 2

                 Project Overview


                        &

     Sample Tracking & Communication Forms
o
o
00

-------
     Project Overview for the Analysis of Polychlorinated Dibenzo-/i-Dioxins & Dibenzofurans
    No. of Field Samples:    H_
    No. of Billable Samples:  _Y -/* /
PAL Project No.:   L-1070
                                                                          Date Received:   08 JUL 98
                                                                          Due Date:        29 JUL 98
                                                                          Client Project ID: R012.003 TX
                                                                          LIME KILN
o
o
                                                        «fv #   '*?T   • . >yf
                                                   .^j&o*X\  >*
               Concentration  sopsp-N-02
             Spike Profile
         ES:  23
         SS:  23
         JS:  23
          4 ng (1-2)
          4 ng (1-1)
          2ng(l)/x
                                                                    tethM23
                                                                                         XAD
                                                                         Sampling Modules Prep. Project No.:^~
   Add M23-ES-^^fTSOt- H
  Vol.: 40 n L;   Cone.: 0.1 ng/ n L
                                                                            SOPSP-S-OJ
Tridecane batch No.:
Thimbles batch No.:
Toluene batch No.:
Pre-Soxhlet:
Others:
                                         Soxhlet 16 H Toluene
                                                                        SOPSP-E-01
Concentration & Solvent Exchange
                                                                             SOPSP-N-01
                                                     Split Extract
                                                          I
                                                            SOPSP-D-01
                                              Hexane batch No.:
                                              CH2C12 batch No.:

                                              Silica batch No.:
                                              Alumina batch No.:
                                              PCU-F batch No.:
                                              NajSO4 batch No.:
                                                                                                      /J
                                                                                                     96
                                SOPSP-D-01
       Special Instructions:

fatd   £6
                                                                                       Fractionation  SOPSP-U-OS
                                                                              Concentration
                                                                                   J
                                                                                                 $t> 7-
                                    Add M23-JS-W7fc$Qr-_
                                   Vol.: 20 \i L;  Cone.; 0.1 ng/ |i L
                                                                                                      SOPSP-N-01
                                                                                                          SOPSP-S-01
                                                                                      HRGC - HRMS  I sQPSP-A-Ol

-------
    Project Overview for the Analysis of Polychlorinated Dibenzo-/>-Dioxins & Dibenzofurans
   No. of Field Samples:     _
   No. of Billable Samples:
o
p
O
      Special Instructions:
^f^v  \0'±o-$-l
                                  PAL Project No.:  L-1070
                                                     tod 23

                                                 SOPSP-A-01
Date Received:   08 JUL 98
Due Date:       29 JUL 98
Client Project ID: R012.003 TX
LIME KILN
           "••"»!"""
           dtfi£ t*
              Method
                                              Sample Extract
                                             Fortified with JSJ
                                                                        Reporting Level;  I ( H) III  11+  III+
                                                   T
                                                         SOPRP-G-01
                                              Data Package
                                                Assembly
                                                      SOPSH-A-01
                                     Archive Data
                                      SOPRP-A-01
                                                      SOPSH-D-01

1


i
8A.
r
ro
la
k
M.

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^



r PH *•
Calibration




^



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LJ



1 L-l fc
laukj ^



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oalllplcS ~
J



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i^oncai

81

.
.

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ro
Li5
•
     Instrument ID:   HlU'^')!
     HP-5MS batch No.:
     DB225 batch No.:
     ICal:
     ConCal:
                                                                                -,
                                                                                t?

-------
 Sample Tracking for the Analysis of Polychlorinated Dibenzo-/i-Dioxins & Dibenzofurans

No. of Field Samples:
PAL Project No.:  L-1070
Date Received:   08 JUL 98
Due Date:       29 JUL 98
Client Project ID: R012.003 TX
LIME KILN

-------
o
               Communication Exchanges Form for the Analysis of PCDD/PCDFs
   No. of Field Samples:
   Page _/_ of _/_
PAL Project No.: L-1070
                                         .1$  t**.~MAttUn>*i »•«* ^
Date Received:   08 JUL 98
Due Date:       29 JUL 98
Client Project ID: R012.003 TX
LIME KILN
                  id
                         *1,. ft
                                .^^      ^
                                   l»^^^

-------
Contract No.:           68D70002
Subcontract No.:        R012-002
Work Assignment:       1-007

08 July 1998

Michael Maret
Pacific Environmental Services, Inc.
5001 S. Miami Blvd
P.O. Box 12077
Research Triangle Park, NC 27709-2077

Reference:  Project No. R012.003; Project Name: US EPA Lime Kiln Screening, Texas Lime

Subject: Inlet Samples Heavy Particulate Load

Dear Mike:

        The thirteen Method 23 samples were received in good condition and no discrepancies were noted
between the sample labels and the chain-of-custody. As we discussed, we organized the samples into three
separate projects, each assigned a specific PAL Project No. Table 1 summarizes the sample identification
and their associated PAL Project Nos.

        The object of this letter is to bring to your attention the following concerns. Following a
description of the issues, possible solutions are discussed for your consideration.

        The  issue pertains to the "inlet" samples.  Each of the four inlet samples shows relatively high
levels of dust (particulates). Depending on the sample, we estimated the amount of solids to range from
10 g to 35 g.

        The first concern is a practical one. Indeed, the capacity of a normal Soxhlet extraction set up is
exceeded if we want to combine the front- and back-halves of the sampling train (FH & BH).  Two separate
extractions would be required for each of the inlet samples. This leads to the following two options:

         1.   Combine the two extracts and process the FH and BH as a single sample.
             >   The question remains as to where the Method 23 internal standards are added.

         2.   Treat the FH and BH as two separate samples.
             >   Each sample receives a normal dose of Method 23 internal standards before the extraction.
             >   This option resembles Method 0023A's and results in four additional samples.

         The second concern is related to generating "meaningful" results for your client's study.
 Reporting PCDD/F results in "ng /dscm" in the flue gas in such circumstances — where particulate levels
 are so high - may be of no value to your client.  We recommend Option 2 above and  propose to report the
 analytical results for the inlet samples in two ways: a) absolute amount (e.g., ng per FH) of the PCDD/Fs
 and, b) relative concentrations of PCDD/Fs expressed in parts-per-trillion (ppt) or picogram per gram of
 "dust" recovered in the inlet sample. Note that this approach can only be achieved if Option 2 is selected,
 which amounts to treating the inlet FH as a solid sample rather than as a flue gas sample.

         Please, let us know if you have questions and we are waiting for a decision on how you would like
 us to handle  these particular inlet samples.  I can be reached at 910-350-2839.

 Sincerely,


  t?
  fvesTondeur, Ph.D.

-------
Table 1: Project No. R012.003; Project Name: US EPA Lime Kiln Screening, Texas Lime;
                       Sample and Project Identification.
       PES Sample ID
       PAL Sample ID
                                                           PAL Project No.
M23-I-1
M23-0-1
M23-FB-1
M23-RB
1070-1
' 1070-2
1070-3
' 1070^4
L-1070
L-1070
M23-I-2
M23-O-2
M23-FB-2

M23-I-3
M23-0-3
M23-FB-3

M23-I-4
M23-O-4
M23-FB-4
1071-1
1071-2
1071-3

1072-1
1072-2
1072-3

1072-4
1072-5
1072-6
                                                    L-1071
                                                    L-1071
                                                    L-1071

                                                    L-1072
                                                    L-1072
                                                    L-1072
                                                    L-1072
                                                    L-1072
                                                    L-1072
                                                    L-1072
                                                                                    014

-------
 PACIF1C 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
                                                 Chain of Custody Record
    7/7/98
Uk
                                                                                                             Page 1 of 3 Pages

-------
             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
                                                          Chain of Custody Record
Project Num          project Name
          R012.003
                           US EPA Lime Kiln Screening - Texas Lime
Samplers:
          Abemathy, Gay, Maret, O.D Holzschuh, Siegal, Stewart
   Date
Time
                                                    Sample Description
                                                                             Analysis Requested
                                                                                                                 Remarks
   6/25/98
   6/28/98
   6/28/98
   6/28/98
   6/28/98
   6/30/98
   6/30/98
   6/30/98
  6/30/98
    7/1/98
    7/1/98
    7/1/98
    7/1/98
  6/25/98
  1518
  1414
  1414
  1414
  1414
M23-O-4-1
M23-O-4-2
M23-O-4-3
M23-O-4-4
       M23-FB-1-1
                    Container No. 4 - XAD Sorbent Resin
                             ntainer No. 1 - Filter
                           Container No. 2 - Train Acetone Rinse
                            ontainer No. 3 - Train Toluene Rinse
                           Container No. 4 - XAD Sorbent Resin
                            ontainer No. 1 - Filter	
                            ontainer No. 2 - Train Acetone Rinse
                           Container No. 3 - Train Toluene Rinse
                             mtainer 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
                                                                                                                            - 2.
                                                                           FIELD BLANK 1
  6/25/98
       M23-FB-1-2
                    Container No. 2 - Train Acetone Rinse
FIELD BLANK 1
                                                                                                   - J
  6/25/98
       M23-FB-1-3
                    Container No. 3 - Train Toluene Rinse
                                                                           FIELD BLANK 1
  6/25/98
  6/27/98
  6/27/98
       M23-FB-1-4
                    Container No. 4 - XAD Sorbent Resin
                             mtainer No. 1 - Filter
                                liner No. 2 - Train Acetone Rinse
                                                                           FIELD BLANK 1    //?»,?- 3
                                                                                               FIELD BLANK 2
                                                                                               FIELD BLANK 2
       7/7/98
                                                                                                                             Page 2 of 3 Pages

-------
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
                                                Chain of Custody Record
'reject Num
R012.003
Project Name
US EPA Lime Kiln Screening - Texas Lime
Samplers:
Abemathy, Gay, Maret, D.D Holzschuh, Siegal, Stewart
Date
6/27/98
6/27/98
6/30/98
6/30/98
6/30/98
6/30/98
7/1/98
7/1/98
7/1/98
7/1/98
7/7/98
7/7/98
7/7/98
7/7/98
Time
Field Sample ID
Sample Description
Analysis Requested


^•••••••••MLContainer No. 3 - Train Toluene Rinse •• L *
^^^L^^^^^^Hn Container No. 4 - XAD Sorbent Resin I ^^B •

mam^
Container No. 1 - Filter
•
«
•
•JL^HBL^L^L^HPrContainer No. 2 - Train Acetone Rinse {^•V '
^^•^•^•^•^•BContainer No. 3 - Train Toluene Rinse Utt •









aamm
M23-FB-4-2
M23-FB-4-3
M23-FB-4^
M23-RB-1
M23-RB-2
M23-RB-3
M23-RB-4
Relinquished by: (Signature)
/)
RSDrbufsfwa by: ffinnature)
*~-^yJ*-y /up wMer

Date/Time
Date/Time
| \&^
bontainer No. 4 - XAD Sorbent Resin 4flE *
Container No. 1 - Filter

•
Container No. 2 - Train Acetone Rinse lAH
•
I * '
Container No. 3 - Train Toluene Rinse ^^Epj *
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)
Received tor lab by: (Signature)
^ 	 ""
=^^Tro^z»ew»#- otMi-W
•
•
•
•
EH •

•
-
•













































Relinquished by: (Signature)






























Date/Time
Remarks
FIELD BLANK 2 /^ ?/-3
FIELD BLANK 2 /0J/' 2
FIELD BLANK 3 i&Z -_?
FIELD BLANK 3 /^2-J
FIELD BLANK 3 /^2-J
FIELD BLANK 3 f^Z^3,
FIELD BLANK 4 //?7/^"
FIELD BLANK 4 /0fef
FIELD BLANK 4 fO?2'6*
FIELD BLANK 4 /O^Z ^T
REAGENT BLANK fafr-tj
REAGENT BLANK /^ --/
REAGENT BLANK /^>^ ^
Received by: (Signature)
REMARKS
   7/7/98
                                                                                                            Page 3 of 3 Pages

-------
 •5
P
GO
                 Preparation of the XAD-2 Resin for Method 23 Sampling Session
   No. Sampling Modules: 15
   No. Filters:            25
                                  PAL Project No.:   L-1043
                                                PES.
Order Received:  04 JUN 98
Due Date:       22 JUN 98
Client Project ID: T\ Lime Kilns
P.O. No.:
Ph.:       (512)-693-5122
   to ensure proper handling of the samples, please return this form with the field samples to:
                                        Paradigm Analytical Labs
                                       2627 Northchase Pkwy S.E.
                                        Wilmington, NC 28405
                   Thank you for your cooperation. Our phone number is 910-350-2839. (Fax: 910-350-1557)
f a.
                 ,
        ethod2$ Sampling


Mailing Address:
Special Instructions:
Best western
Attn.: Mike Maret
1403 Hiway 281 N
Marble Falls, TX 78654-4505
Ph.: (512)693-5122
Note: An amount of resin equal to one module was fortified as 	 	
described above, retained by the laboratory and kept at 4°C. ^ — •
Upon return of the field samples, this aliquot will be^ '
used to process the Laboratory Method Blanjs^-''"*'^

	
                                                                    Filters

                                                                    Batch No.:
                                                                    Size:
                                                                           83 mm diameter
                                                                    Type:     CGlassFibej) Quartz

                                                                    XAD-2 Resin Modules
                                                                                     3-7
             QC sample.
                                                                Batch No.:	
                                                                Type: Ball/Socket (6-Ring Ball/Socket^ Screw Cap

                                                                Add  M23-SS-M*M-SOz.- K
                                                                Vol.: 40 n L ;  Cone.: 0.1 ng/ n L
                                                                Preparation Date:
                                                                [Two-week holding time]

                                                                Analyst:

-------
                                        Paradigm
                              Sample Receipt Checklist
                     1027
Client:

Client Project ID:  R012.003
Lab Project: L1070
No
1
/
2 V
3
n
4 (
5
£
i
8 /
i
9

Check
YES/JJpX
'-^ESjp'NO
oXES-Y^no— v
YES (/NOx
YES A NOx
YEijxy NU
A-"c
; YES^ / Nu
YES / NO
YES / NO
^^
/ YE?^/ Nn
YES /NO ^x

Description
Shipped
Hand Delivered
COC Present on Receipt
Additional Transmittal Form
COC Tape on Shipping Container
Samples Intact
Temperature
umcien~ Jdiujjj.t; dUDmirteci
Nc3__ELreservative Noted
/^N/A J^ione recommeded)
Rpceiv^d within Holding time
N/A
1
^Discrepancies between COC & Label
N/A (no COC Received)
Notes









   Note : Use this form to record, comment and report any damages, observations  (be specific) of
   signficance or potentially important for the resolution of downstream problems.


    Additional  Comments:
       Inspected & Logged in by
                 Date:
                 Time:
                                                                                    019

-------
          Paradigm Analytical Ub»
             Login  Report (h*01)
                 Jut. 08, 1998
                   10:01 AM
   Login Number: L1070
Account:         1027         Pacific Environmental Services,
 Project:       R012.003       Texas Lime Kiln               Page: 1 of  1
Laboratory
Sample Number
L1 070-1
StackAir -fr M0010

L1 070-2
L1 070-3
L1 070-4
Client
Sample
M23-I-1
0270>AS j^
M23-O-1
M23-FB-1
M23-RB-1
Collect
Number Date
25-JUN-98
^jHold: 09-JUL-98
25-JUN-98
25-JUN-98
25-JUN-98
Receive
Date
08-JUL-98
08-JUL-98
08-JUL-98
08-JUL-98
Due
PR Date
29-JUL-98
29-JUL-98
29-JUL-98
29-JUL-98
Comments
^ f~tf*
1
1 XT
\y otoot f f
                              Date :
— CZQ

-------
                                           Paradigm Analytical Labs
                                              Login Report (In01)
                                                  Jul. 13, 1998
                                                     11:42 AM
                                  Login Number: L1070
                               Account:          1027
                                Project:
                             R012.003
                           Pacific Environmental Services, It
                           Texas Lime Kiln                  Page:  1 of  1
Laboratory
Sample Number
Client             Collect       Receive
Sample Number  Date         Date
                           PR
                  Due
                  Date
              Comments
L1070-1
M23-I-1
25-JUN-98
08-JUL-98
 StackAir    P 23-TO
 StackAir    C 8290-TO-FT
 StackAir    C 8290-TO-SL
             Hold:
             Hold: 02-JUL-98     4 oz. Glass
             Hold: 02-JUL-98     4 oz. Glass
  29-JUL-98


1 Bottles
1 Bottles
L1070-2
M23-O-1
25-JUN-98
08-JUL-98
 StackAir    P 23-TO
 StackAir    C 8290-TO-FT
 StackAir    C 8290-TO-SL
             Hold:
             Hold: 02-JUL-98     4 oz. Glass
             Hold: 02-JUL-98     4 oz. Glass
  29-JUL-98


1 Bottles
1 Bottles
L1070-3
M23-FB-1
25-JUN-98
08-JUL-98
 StackAir    P 23-TO
 StackAir    C 8290-TO-FT
 StackAir    C 8290-TO-SL
             Hold:
             Hold: 02-JUL-98     4 oz. Glass
             Hold: 02-JUL-98     4 oz. Glass
   29-JUL-98


1  Bottles
1  Bottles
L1070-4
M23-RB-1
25-JUN-98
08-JUL-98
 StackAir    P 23-TO
 StackAir    C 8290-TO-FT
 StackAir    C 8290-TO-SL
             Hold:
             Hold: 02-JUL-98     4 oz. Glass
             Hold: 02-JUL-98     4 oz. Glass
   29-JUL-98


1  Bottles
1  Bottles
                                                            Signature:   vU4  iVxJL
                                                                 Date:
                                                                                           JC21

-------
OPUSquan 20-JUL-1998 Paqe 1
Paradigm Sample Log
Data File S Sample ID .
\/
a!7ju!98b 1 DB-5 Retchk ' I
al7ju!98b 2 FE CS3 • 	 v
a!7ju!98b 3 098-M23 xl/2
a!7ju!98b 4 598-M23 xl/2
al7ju!98b 5 SB
a!7ju!98b 6 fHUKfiSiSf •
a!7ju!98b 7 1072-0 xl/2
al7ju!98b 8 1072-2 xl/2
a!7ju!98b 9 1072-3 xl/2
al7jul98b 14
a!7ju!98b 15 " BE CS3 * — •V^/
Page 1 of 1
Acq. Date Time
17-JUL-98 16:45:56^£r^-
17-J0L-98 17:31:00 ^^
17-JUL-98 18:16:05
17-JUL-98 19:01:10
17-JUL-98 19:46:16
17-JUL-98 20:31:20
17-JUL-98 21:16:26
17-JUL-98 22:01:31
17-JUL-98 22:46:36
17-JUL-98 23:31:42
18-JUL-98 00:16:48
18-JUL-98 01:01:55
18-JUL-98 01:47:01
18-JUL-98 02:32:07
18-JUL-98 03:17:11'^

-------
 'V
OPUSquan 22-JUL-1998
Paradigm Sample
Data File
A21JUL98A
A21JUL98B
A21JUL98C
A21JUL98C
A21JUL98C
A21JUL98D
A21JUL98E
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A210UL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
A21JUL98F
' A21JUL98F

Log
S
1
1
1
2
3
1
1
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
Page 1

Sample ID
Sand QC
B-225 Retchk
B-225 Retchk
CS3
sb
B-225 Retchk
B-225 Retchk
B-225 Retchk
CS3
sb
mmnHRHff —
T^^SBSRwiPBpis^

1072-2 xl/2
1068-1 xl/2
1069-1 xl/2
1069-2 xl/2
1069-3 xl/2
1072-1 xl/2
1071-2 xl/2
1072-4 xl/2
1072-5 xl/2
1072-8 xl/2
CS3


Acq. Date
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
21-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98
22-JUL-98

Page 1 of 1
Time
11:08:47
16:44:01
17:52:30
18:29:30
19:06:30
19:59:35
20:01:06
20:06:58 <==~
20:43:56 4r"
21:20:54
21:57:56
22:34:59
23:12:05
23:49:03
00:26:13
01:03:12
01:40:19
02:17:20
02:54:34
03:31:35
04:08:35
04:46:12
05:23:13
06:01:17 £-
CO

-------
                         Section 3
                    Analytical Results
                 Documentation for the Analysis
                             of
        Polychlorinated Dibenzo-/;-Dioxins & Dibenzofurans
"»
'•\

-------
                                                                        Paradigm Analytical Labs
Analytical Data Summary Sheet
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total IfctCDFs
Total HpCDFs
TEQ(ND=0)
TEQ (ND=l/2)
Concentration
- .9&'--V%
EMPC
EMPC
ND
ND
ND
0.0032
0.0093
EMPC
ND
NDr£;.?A
EMPC
0.0006
ND
'ND ;\,
0.0027
ND
0.0021
ND
ND
ND
0.0032
0.0012
ND
0.0004
0.0028
0.0001
0.0007

0.0004
0.0007
0.0006
0.0006
0.0003
0.0008
0.0006
0.0004
0.0004
0.0003
0.0003
0.0003
Q.oqo4
0.0006
0.0007
0.0007
0.0004
0.0003
0.0006
0.0003
0.0006
0.0004
0.0003
0.0006


•pratfc .-•
:;;-}.-«OT;^
0.0009





0.0010

0.0011



0.0009
0.0004
0.0016
0.0056
0.0024

0.0020

0.0015
0.0018
'•& ;JHC._ -\
28:28
i-r-3S3?F-|
34:42
34:45
34:59
37:10
40:03
27:29

.''•-,32:^
34:11
34:15
34:38
36:22

40:10








* ",-

;;-.»SI : =
1.25
"ill
;5J^3
2.76
1.14
0.86
1.06

f-;;3.69
1.63
; 1.3
0.95
1.00

0.84










Qualifier
,-*



















ITEF
ITEF
Client Information
Project Name:
Sample ID:
Laboratory Information
Project ID:
Sample ID:
tf"*V^]1 A/*£^nn T^O^A.
v/ouecuon uaie.
,Re«!JptJ>^te:,._; , '; ,,,^:
Extraction Date:
Analysis Date: , *
Texas Lime Kiln
LMB
L1070
1070-0
, ^S'A1' ' "-'' : ~ ~ .
f *%<' .'--W" ^ ' ^ At.'
•--„.. • ,ll^,i);t;4r^;y.>,-4«i£;v?p-'';
-..^•-•'tjSfc^^H.-": ft.-p-
Sample Information
Matrix:
Weight /Volume:
Moisture / Lipids:
Filename:
„ -n - f_Llii1_'
- Kfiten86;s,
^•(&5gwi^SM:^ . -
•;;; EMCoii^r '
Air
- ' 1
0.0 °,
al7jul98b-6
« 1 o * snoL i
8l7jul98b-l
Al7jul98b-2
al7ju!98b-15
' ;jn8290-s23j0';
                                          1/2
                                                                                                 C2

-------
                                      Method 23
                                                                 Paradigm Analytical Labs
                            Analytical Data Summary Sheet
Labeled
Standard s:^r%r
Extraction Standards
13C12-2,3,7,8-TCDD
13Cl2-U,3,7,8-PeCDD
*C12-1, 2,3,6,1, S-HxCDD
13Cl2-l,2,3,4,6,7,8-HpCDD
13C12-OCDD
13C12-2,3J,8-TCDF
I3C,2-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
I3Cu-l,2,3,4,6,7,8-HpCDF
Sampling Standards
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
"Cirl,2,3,4,7,8-HxCDD
13C12-l,2,3,4,7,8-HxCDF
13C12-1,2,3,4,7,8,9-HPCDF
Injection Standards
13C12-1,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
•

4
4
4
4
8
4
4
4
4

4 '
4
4
4
4



Measured

3.79
-;;'}4:d8'rCl
3.85
3.67
6.90
3.65
3.53
4.03
2.98

4,17
4.38
4.12
3.83
3.91



percent °
^Recovery;
{*/.)

94.6
101:9;
96.3
91.8
86.2
91.4
88.1
100.8
74.5

104.4
109.4
103.0
95.8
97.7



tlg|:|

28:27
32:37
34:45
37:10
40:01
27:25
31:56
34:15
36:21

28:28
32:24
34:42
34:10
37:31

28:09
34:58
>;'Ratio ,

0.78
1.56
1.26
1.05
0.88
0.78
1.57
0.52
0.44


1.57
1.25
0.52
0.44

0.78
1.24
Qualifier



















Client Information
Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:

Collection Date:
Receipt Date:
Extraction Date:
Analysis Date:
Texas Lime Kiln
LMB • •?•;*./• \



Lld70 9 ,';•'•-' '.' '';*l?-
IQJQ-Q ""•„' - .;,-i
-••."> . '• "'" ;•''•.&
, , NA. . - - -i>if_ •.,
'"' •'• '-NJi":" " - '; "----''
10-JaI-98
17-Ju|-S8 , k
Sample Information

Matrix:,,
;; Wei^i^VoIurae:
Mo&ttoB/14nds:
•;';", -. -.-^^A^:'_ _.. .
:y^;\;\,'";;^'V' '
/-%' -Fiileaante:,., ••
Recite
-'..'' •" "'.'Bei^p^tM:
BndpoaCal:
'-; , \r3n^®&.:


Air
1
0.0


al7ju!98b-6
al7ju!98b-l
al7jul98b-2
al7ju!98b-15
',*#>&&&
Reviewed by:
                                                                              %
                                                             Date Reviewed:
                                      2/2
                                                                                r
                                                                                      026

-------
O
OPUSquan 20-JUL-1998
Filename al7ju!98b
Sample 6
Acquired 17-JUL-98 20
Processed 20-JUL-98 09
Sample ID 1070-0 xl/2
Page 1


:31:20
:03:15









































Cal Table m8290-23-071798
Results Table M8290-23-071798B
Comments
Typ
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS
SS
SS
SS
SS
SS
Name;
2,3,7,8-TCDD; 3
1,2,3,7,8-PeCDD; 4
1,2,3,4,7,8-HxCDD; 4
1,2,3,6,7,8-HxCDD; 8
1,2,3,7,8,9-HxCDD; 6
1,2,3,4,6,7,8-HpCDD; 1
OCDD; 4
2,3,7,8-TCDF; 1
1, 2,3,7, 8-PeCDF;
2,3,4,7,8-PeCDF; 8
1,2,3,4,7,8-HxCDF; 1
1,2,3,6,7,8-HxCDF; 7
2,3,4, 6,7, 8-HxCDF; 1
1,2,3,7,8,9-HxCDF;
1,2,3,4,6,7,8-HpCDF; 1
1,2,3,4,7,8,9-HpCDF;
OCDF; 1
13C-2,3,7,8-TCDD; 4
13C-l,2,3,7,8-PeCDD; 3
13C-1,2,3, 6,7,8-HxCDD; 3
13C-l,2,3,4,6,7,8-HpCDD; 2
13C-OCDD; 3
13C-2,3,7,8-TCDF; 5
13C-l,2,3,7,8-PeCDF; 4
13C-l,2,3,6,7,8-HxCDF; 4
13C-l,2,3,4,6,7,8-HpCDF; 1
13C-1,2,3,4-TCDD; 4
13C-l,2,3,7,8,9-HxCDD; 3
37Cl-2,3,7,8-TCDD; 4
13C-2,3,4,7,8-PeCDF; 4
13C-l,2,3,4,7,8-HxCDD; 2
13C-l,2,3,4,7,8-HxCDF; 3
13C-1,2,3,4,7,8, 9-HpCDF; 1
37Cl-2,3,7,8-TCDD; 4
13C-2,3,4,7,8-PeCDF; 4
13C-l,2,3,4,7,8-HxCDD; 2
13C-l,2,3,4,7,8-HxCDF; 3
13C-1,2, 3,4,7,8,9-HpCDF; 1


Resp;
.64e+05;
.85e+04;
.63e+04;
.08e+04;
.156+04;
.83e+05;
.55e+05;
.336+05;
* .
.21e+04;
.07e+05;
.03e+04;
.94e+04;
* .
.70e+05;
* .
.09e+05;
.43e+08;
.33e+08;
.65e+08;
.58e+08;
.90e+08;
.37e+08;
.516+08;
.41e+08;
.98e+08;
.27e+08;
.53e+08;
.24e+08;
.826+08;
.53e+08;
.32e+08;
. 51e+08;
.24e+08;
.82e+08;
.53e+08;
.326+08;
.51e+08;

Ion 1;
5.69e+04;
2.56e+04;
3.41e+04;
4.46e+04;
4.516+04;
9.756+04;
2.116+05;
6.856+04;
* .
5.98e+04;
6.626+04;
3.97e+04;
9.41e+03;
* .
8.546+04;
* .
5.006+04;
1.94e+08;
2.03e+08;
2.03e+08;
1.32e+08;
1.83e+08;
2.36e+08;
2.756+08;
1. 51e+08 ;
6.08e+07;
1.886+08;
1.96e+08;
4.246+08;
2.946+08;
1.41e+08;
1.13e+08;
4.606+07;
4.24e+08;
2.94e+08;
1.416+08;
1.13e+08;
4.606+07;

Ion 2;
3.07e+05;
2.29e+04;
1.22e+04;
3.626+04;
1.63e+04;
8.536+04;
2.446+05;
6.466+04;
* .
2.236+04;
4.066+04;
3.066+04;
9.96e+03;
* .
8.516+04;
* .
5.916+04;
2.506+08;
1.30e+08;
1.61e+08;
1.26e+08;
2.07e+08;
3.01e+08;
1.76e+08;
2.90e+08;
1.37e+08;
2.396+08;
1.57e+08;
-;
1.886+08;
1.13e+08;
2.19e+08;
1. 056+08; ;

1.886+08;
1.136+08;
2.19e+08;
1.05e+08;

RA; ?;
0.18;n;
1.12;n;
2.81;n;
1.23,-y;
2.76;n;
1.14,-y;
0.86;y;
1.06;n;
*;n;
2.69;n;
1.63;n;
1.30;y;
0.95;n;
*;n;
1.00;y;
*;n;
0.84;y;
0.78;y;
1.56,-y;
1.26;y;
1.05;y;
0.88;y;
0.78;y;
1.57;y;
0.52;y;
0.44;y;
0.78;y;
1.24;y;
- ; - ;
1.57;y;
1.25,-y;
0.52;y;
0.44;y;

1.57,-y;
1.25;y;
0.52,-y;
0.44;y;

RT;
28:28;
32:37;
34:42;
34:46;
34:59;
37:10;
40:03;
27:29;
NotFnd;
32:24;
34:11;
34:15;
34:38;
NotFnd;
36:22;
NotFnd;
40:10;
28:27;
32:37;
34:45;
37:10;
40:01;
27:25;
31:56;
34:15;
36:21;
28:09;
34:58;
28:28;
32:24;
34:42;
34:10;
37:31;
28:28;
32:24;
34:42;
34:10;
37:31;

Cone ;
0.084;
0.013;
0.019;
0.026;
0.020;
0.079;
0.233;
0.026;
* .
0.020;
0.028;
0.015;
0.005;
* .
0.068;
* .
0.052;
94.630;
101.898;
96.241;
91.828;
172.398;
91.338;
88.116;
100.761;
74.472;
88.482;
89.034;
98.685;
96.355;
99.268;
97.332;
72.753;
104.344;
109.389;
103.011;
95.831;
97.728;

DL;
0.0098;
0.0069;
0.0180;
0.0142;
0.0140;
0.0085;
0.0204;
0.0137;
0.0100;
0.0097;
0.0082;
0.0065;
0.0076;
0.0087;
0.0140;
0.0170;
0.0163;
0.0335;
0.0317;
0.0417;
0.0319;
0.0143;
0.0215;
0.0082;
0.2929;
0.1413;
-;
- ;
0.0239;
0.0084;
0.0619;
0.3759;
0.1805;
0.0259;
0.0059;
0.0577;
0.3311;
0.2918;

S/N1;?;
10;y;
5;y;
4;y;
6;y;
6;y;
35;y;
25, -y;
8;y;
*;n;
22;y;
8;y;
5,-y;
2;n;
*;n;
11; y;
*;n;
10;y;
5479,-y;
14436;y;
7530;y;
6744;y;
17487; ;y;
12736;y;
88252, -y;
1214;y;
2809, -y;
5439 ;y;
6617 ; y;
12073 ;y;
98823, -y;
6521;y;
1069 ;y;
1869;y;
12073 ;y;
98823;y;
6521;y;
1069;y;
1869;y;

S/N2;?
39 ;y
7;y
l;n
3;n
2;n
26;y
63, -y
3;y
*;n
3;n
9;y
6;y
3;n
*;n
22 ;y
*;n
10, -y
13615;y
19123;y
7892, -y
6370 ;y
34203;y
12195;y
31811;y
1122, -y
1065;y
13386;y
6801;y
-; -
35003 ;y
6558;y
1008 ;y
720, -y
_ . _
35003, -y
6558;y
1008;y
720, -y
mod?
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
                                                                                                                                                     Page  11

-------
OPUSquan   20-JUL-1998
                   Page 1
                                                                    Page  1  of  8

 Ent: 39 Name: Total Tetra-Furans  F:l  Mass:  303.902 305.899  Mod?  no  #Hom:3

 Run: 11 File: al7ju!98b    S:6  Acq:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-0 xl/2
   Amount: 0.05
     Cone: 0.05
   Tox #1: -
Name
of which 0.03
of which 0.03
     Tox #2:  -

#     RT Respnse
named and 0.03
named and 0.03
      Tox #3: -
                                        RA
2,3,7,8-TCDF
1  24:51 1.66+04  0.45 n
         1.6e+04

2  25:46 1.3e+05  0.80 y
         1.3e+05

3  27:29 1.3e+05  1.06 n
         1.3e+05
                                              Cone

                                               0.00
                                                   4
                                                   1
                                               0.03
                                                   C

                                               0.03
unnamed
unnamed
                                                      Area  Height
                                  S/N  Mod?
               4.8e+03 1.4e+03 l.le+00 n  n
               l.le+04 2.8e+03 8.1e-01 n  n
              3
               5.7e+04 1.2e+04 9.2e+00 y  n
               7.1e+04 1.6e+04 4.6e+00 y  n
              3
               6.9e+04 l.le+04 8.4e+00 y  n
               6.5e+04 l.le+04 3.4e+00 y  n
                                                                    Page 2 of 8

 Ent: 40 Name: Total Tetra-Dioxins F:l  Mass: 319.897 321.894 Mod? no   #Hom:2

 Run: 11 File: al7ju!98b    S:6  Acq:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-0 xl/2
   Amount: 0.09
     Cone: 0.09
   Tox  #1: -
Name
 2,3,7,8-TCDD
of which 0.08
of which 0.08
     Tox #2: -

#     RT Respnse
named and 0.01
named and 0.01
      Tox #3: -
                                        RA
1  25:16 3.6e+04  1.29 n
         3.6e+04

2  28:28 3.6e+05  0.18 n
         3.6e+05
                                              Cone

                                               0.01

                                                   ]
                                               0.08
unnamed
unnamed
                  Area  Height    S/N  Mod?
               2.0e+04 3.8e+03 3.1e+00 y  n
               1.6e+04 3.7e+03 2.3e+00 n  n

               5.7e+04 1.2e+04 9.6e+00 y  n
               3.1e+05 6.5e+04 3.9e+01 y  n
                                                                    Page 3 of 8

  Ent:  41 Name: Total Penta-Furans  F:2  Mass: 339.860 341.857 Mod? no   #Hom:l

  Run:  11 File: a!7ju!98b    S:6  Acq:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
  Tables: Run: al7jul98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
  Version: V3.5 17-APR-1997 11:14:34   Sample text: 1070-0 xl/2
   Amount:  0.02
      Cone:  0.02
   Tox  #1:  -

Name

2,3,4,7,8-PeCDF
of which 0.02
of which 0.02
     Tox #2: -

#     RT Respnse
named and *
named and *
      Tox #3: -
    RA
1  32:24 8.2e+04  2.69 n
         8.2e+04
          Cone

           0.02
unnamed
unnamed
Area   Height
                                  S/N  Mod?
                                                   6.0e+04 2.0e+04 2.2e+01 y  n
                                                   2.2e+04 8.8e+03 2.6e+00 n  n
                                                                    Page  4 of  8

  Ent:  42 Name: Total  Penta-Dioxins F:2  Mass:  355.855 357.852 Mod? no   #Hom:5

  Run:  11 File: a!7ju!98b     S:6  Acq:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
                                                                                                       f   028

-------
OPUSguan   20-JUL-1998
                   Page  2
 Tables: Run: a!7ju!98b  Analyte:  m8290-23-»  Cal: m8290-23-»Results:
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-0 xl/2
                                                                     M8290-23»
   Amount: 0.05
     Cone: 0.05
   Tox #1: -
Name
1,2,3,7,8-PeCDD
of which 0.01
of which 0.01
     Tox #2:  -

#     RT Respnse
named and 0.03
named and 0.03
      Tox #3:  -
                                        RA
1  31:30 2.1e+04  0.79  n
         2.1e+04

2  31:57 6.4e+04  10.28n
         6.4e+04

3  32:04 1.3e+04  0.81  n
         1.3e+04

4  32:37 4.8e+04  1.12  n
         4.8e+04

5  32:55 2.46+04  2.71  n
         2.4e+04
          Cone

           0.01
               S
               ]
           0.02
               c
               c
           0.00
               c
               1
           0.01


           0.01
    unnamed
    unnamed
    Area  Height
 9.1e+03  3.8e+03  2.
 1.2e+04  4.4e+03  4.

 5.8e+04  1.6e+04  8.
 5.7e+03  1.6e+03  1.
D
 5.9e+03  2.5e+03  1.
 7.3e+03  3.0e+03  2.
I
 2.6e+04  9.2e+03  4.
 2.36+04  7.5e+03  7.
L
 1.8e+04  6.06+03  3,
 6.6e+03  2.26+03  2,
                                                                      S/N  Mod?
,Oe+00 n  n
,3e+00 y  n

,4e+00 y  n
,6e+00 n  n

.3e+00 n  n
.9e+00 n  n

.9e+00 y  n
.3e+00 y  n

 2e+00 y  n
 2e+00 n  n
                                                                                                         029

-------
OPUSguan   20-JUL-1998
                                      Page 3
 Ent: 43 Name: Total Hexa-Furans
                                                 Page  5  of  8

                F:3  Mass:  373.821 375.818  Mod?  no   #Hom:9
 Run: 11 File: al7ju!98b    S:6  Acg:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results:  M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-0 xl/2
   Amount: 0.08
     Cone: 0.08
   Tox #1: -
of which 0.05
of which 0.05
     Tox #2:  -
named and 0.03
named and 0.03
      Tox #3: -
Name
                         RT Respnse
                                        RA
                      33:31 2.1e+04  1.85 n
                            2.1e+04
                   2  33:38 5.2e+04  1.58 n
                            5.26+04

1,2,3,4,7,8-HxCDF  3  34:11 l.le+05  1.63 n
                            l.le+05

1,2,3,6,7,8-HxCDF  4  34:15 7.0e+04  1.30 y
                            7.0e+04

2,3,4,6,7,8-HxCDF  5  34:38 1.9e+04  0.95 n
                            1.9e+04

                   6  34:44 l.le+04  0.42 n
                            l.le+04

                   7  34:46 2.1e+04  1.68 n
                            2.1e+04

                   8  34:56 2.6e+03  1.41 y
                            2.6e+03

                   9  34:59 l.Oe+04  2.12 n
                            l.Oe+04
                           Cone

                            0.01
                                3

                            0.01


                            0.03
                                e
                                4
                            0.01
                                4

                            0.00
                                c
                                ]
                            0.00


                            0.01
                                3

                            0.00
                                1
                                1
                            0.00
                                   unnamed
                                   unnamed
                  Area  Height    S/N  Mod?
               1.4e+04 5.4e+03 2.1e+00 n  n
               7.46+03 3.0e+03 2.0e+00 n  n
              I
               3.2e+04 9.6e+03 3.8e+00 y  n
               2.06+04 6.5e+03 4.3e+00 y  n
              3
               6.6e+04 2.1e+04 8.3e+00 y  n
               4.1e+04 1.4e+04 8.9e+00 y  n

               4.0e+04 1.4e+04 5.5e+00 y  n
               3.1e+04 9.0e+03 5.9e+00 y  n
              3
               9.4e+03 4.2e+03 1.6e+00 n  n
               l.Oe+04 4.1e+03 2.7e+00 n  n

               3.3e+03 1.3e+03 5.2e-01 n  n
               7.8e+03 1.7e+03 l.le+00 n  n

               1.3e+04 2.9e+03 l.le+00 n  n
               7.8e+03 1.7e+03 l.le+00 n  n
              3
               l.Se+03 8.9e+02 3.5e-01 n  n
               l.le+03 5.1e+02 3.4e-01 n  n
              3
               7.1e+03 2.2e+03 8.8e-01 n  n
               3.3e+03 1.36+03 8.7e-01 n  n
                                                                    Page 6 of 8

 Ent: 44 Name: Total Hexa-Dioxins  F:3  Mass: 389.816 391.813 Mod? no   ttHom:10

 Run: 11 File: al7ju!98b    S:6  Acq:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results:  M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-0 xl/2
   Amount: 0.19
     Cone: 0.19
   Tox #1: -
Name
of which 0.06
of which 0.06
     Tox #2:  -

#     RT Respnse
                 named and 0.12
                 named and 0.12
                       Tox #3:  -
                                        RA
                   1  33:52 3.0e+04  1.27 y
                            3.0e+04

                   2  33:56 3.8e+03  0.47 n
                            3.8e+03

                   3  34:03 1.3e+04  1.02 n
                            1.3e+04

                   4  34:10 1.2e+05  2.49 n
                            1.2e+05

                   5  34:15 9.8e+04  3.07 n
                            9.8e+04
                           Cone

                            0.01
                                1
                                1
                            0.00
                                1

                            0.00
                                e
                                e
                            0.04
                                £

                            0.03
                  unnamed
                  unnamed
                                                      Area  Height    S/N  Mod?
               1.7e+04 7.4e+03 3.4e+00 y  n
               1.3e+04 4.9e+03 1.4e+00 n  n
              3
               1.2e+03 6.0e+02 2.8e-01 n  n
               2.6e+03 l.le+03 3.2e-01 n  n
              3
               6.3e+03 1.9e+03 8.8e-01 n  n
               6.2e+03 2.2e+03 6.3e-01 n  n
              \
               8.3e+04 2.6e+04 1.2e+01 y  n
               3.3e+04 1.2e+04 3.3e+00 y  n
              3
               7.4e+04 2.3e+04 l.le+01 y  n
                                                                                                         r\
                                                                                      339

-------
OPUSguan   20-JUL-1998
                   Page 4
                   6  34:20 8.1e+04  1.35 y    0.03
                            S.le+04

                   7  34:32 1.2e+04  2.22 n    0.00
                            1.2e+04

1,2,3,4,7,8-HxCDD  8  34:42 4.6e+04  2.81 n    0.02
                            4.6e+04

1,2,3,6,7,8-HxCDD  9  34:46 8.1e+04  1.23 y    0.03
                            8.1e+04

1,2,3,7,8,9-HxCDD  10 34:59 6.1e+04  2.76 n    0.02
                            6.1e+04
                                2.4e+04  7.6e+03  2.2e+00  n  n
                               3
                                4.6e+04  1.3e+04  6.0e+00  y  n
                                3.4e+04  9.5e+03  2.7e+00  n  n

                                S.le+03  2.1e+03  9.6e-01  n  n
                                3.6e+03  1.4e+03  4.1e-01  n  n
                               2
                                3.4e+04  9.6e+03  4.4e+00  y  n
                                1.2e+04  5.1e+03  l.Se+00  n  n
                               3
                                4.5e+04  1.4e+04  6.3e+00  y  n
                                3.6e+04  9.5e+03  2.7e+00  n  n

                                4.5e+04  1.4e+04  6.5e+00  y  n
                                1.6e+04  7.1e+03  2.0e+00  n  n
                                                                    Page 7 of 8

 Ent: 45 Name: Total Hepta-Furans  F:4  Mass: 407.782 409.779 Mod? no   #Hom:l

 Run: 11 File: al7ju!98b    S:6  Acg:17-JUL-98 20:31:20 Proc:20-JUL-98 09:03:15
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-0 xl/2
   Amount: 0.07
     Cone: 0.07
   Tox #1: -
of which 0.07    named and *       unnamed
of which 0.07    named and *       unnamed
     Tox #2:  -         Tox #3:  -
Name
                         RT Respnse
                                        RA
                           Cone    Area  Height    S/N  Mod?
1,2,3,4,6,7,8-HpCDFl  36:22 1.7e+05  l.OOy    0.07
                            1.7e+05                8.56+04 2.4e+04 l.le+01 y  n
                                                   8.5e+04 2.86+04 2.2e+01 y  n

-------
OFUSguan   20-JUL-1998                Page 5
                                                                   Page  8  of  8

 Ent: 46 Name:  Total Hepta-Dioxins F:4  Mass:  423.777  425.774 Mod? no   #Hom:3

 Run: 11 File:  a!7ju!98b    S:6  Acq:17-JUL-98 20:31:20  Proc:20-JUL-98  09:03:15
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-0 xl/2

   Amount: 0.14    of which 0.08    named and 0.06     unnamed
     Cone: 0.14    of which 0.08    named and 0.06     unnamed
   Tox #1: -            Tox #2: -         Tox #3:  -

Name               tt     RT Respnse     RA    Cone     Area   Height    S/N  Mod?

                   1  36:21 6.56+04  2.78 n    0.03
                            6.5e+04                4.8e+04  1.46+04 1.9e+01  y  n
                                                   1.7e+04  5.4e+03 5.5e+00  y  n
                   2  36:35 7.0e+04  1.28 n    0.03
                            7.0e+04                3.9e+04  1.3e+04 1.7e+01  y  n
                                                   3.1e+04  8.8e+03 9.06+00  y  n
1,2,3 4,6,7,8-HpCDD3  37:10 1.8e+05  1.14 y    0.08
                            1.8e+05                9.8e+04  2.6e+04 3.5e+01  y  n
                                                   8.5e+04  2.6e+04 2.6e+01  y  n
                                                                                                       Q3Z

-------
File: A17JUL98B Acq: 17-JUL-1999 20:31:20 Exp : EXP_M23
Sample #6 Text: 1070-0 xl/2
319.8965 S:6 SMO(1,3) BSUB(128
100%,
"
50 j
:
ol


A4.59E3
_x—s^v~-\-r\/X— ^^* — ^^Xv^v^-x/^-^/i 	 'V--
24 loo'
321.8936 S:6 SMO(1,3) BSUB(128
100%
50 j




	 24!oo'
331.9368 S:6 SMO(1,3) BSUB(128
100%,
50J
o"



	 24 loo'
333.9339 S:6 SMO(1,3) BSUB(128
100%
50 J
o:



24 loo'
327.8847 S:6 SMO(1,3) BSUB(128
lOOSj
50J
0 '



w— ' — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1—
24:00
316.9824 S:6 SMO(1,3) PKD(3,3,
1004 23:27 24:04 24
50 j
o:


	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00
ALS #6
,15, -3.0) PKD(3,3,3,0.10%,



A2.02E4 A5.41E3
^~^^-^_/\A/_^~x-^X\yx ^V_ ^_
25:00 	 26:00
,15, -3.0) PKD(3,3,3,0.10%,


A1.56E4
25 loo' ' ' ' 26 loo'
,15, -3.0) PKD(3,3,3,0.10%,



25 100 	 26 loo'
,15, -3.0) PKD(3,3,3,0.10%,



25 100 26100
,15, -3.0) PKD(3,3,3,0.10%,



— T 	 "I 1 "I" "I~VT ! 	 1 	 1 	 1 1 	
25100 26:00
3, 100. 00%, 0.0,1. 00%, F,F)
:44 25:14 25i49 26U


— r— ] 	 1 	 1 	 1 i i | i 	 1 —
25:00 26:00
_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm

1224. 0,1. 00%, F,F)
A7.76E4 ,_1.7E4
A A5.69E4
/ 1 A
/ \ A9.47E3/ \
~> — x-^y~A — ^\^~v/vyV^J^vA^^^^Sp~-~^i'Clt-^ — V/-^-^x~Vy\-^^^^yx ^^^-r^~^f^

_8.7E3

O.OEO
"""'" ' 27 loo' ' ' 28:00 	 29loO 	 3oloO Time
1644. 0,1. 00%, F,F)
A3.07E5
ft
Jv
6.8E4
L3.4E4

27 100 	 28 100 	 29 100 	 3oloO Time
7104. 0,1. 00%, F,F)
A1.94E8
A A
n
/ W V
3.9E7
_1.9E7
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27100 28100 29100 3oloO Time
3696. 0,1. 00%, F,F)
A2.50E8
A A
ft
/v
5.0E7
.2 . 5E7
O.OEO
27100 28100 29100 3oloO Time
7056. 0,1. 00%, F,F)
A4.24E8
A
f[

_8.5E7
_4.3E7
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27loO 28loO 29:00 30:00 Time

9 26:51 27:16 27:45 28:25 28:52 7.4R7
\T

_3.7E7
O.OEO
27 100 	 28 100 ' 29 100 ' 3oloO Time
o
CO
CO

-------
File: A17JUL98B Acq: 17-JUL-1998
Sample #6 Text: 1070-0 xl/2 ALS
355.8546 S:6 F:2 SMO(1,3) BSUB (128
100%,

50

0



\^_— ^-v ^/— V>~— -v—
20:31:20 Exp: EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
#6
,15, -3.0) PKD(3,3,3,0.10%,1888.0,1.00%,F,F)
c O-.T-,,, A4.67E4 2.0E4
A5.82E4 n
A 1
\\ \ A2.56E4
A9 10E3 \ A A1.79E4
_^_^^A__^J-te^J4_A^ vCLx^v-


1.0E4

n DRO
1 1 1 | 1 1 1 1 1 | 1 1 1 1 1 | 1 1 1 1 1 | 1 1 1 1 1 | 1 1 1 1 1 | 1 'I-T-I 1 1 1 1 1 1 1 1 	 I 1 1 1 1 1 1 	 1 1 1 1 1 1 1 1 1 1 1 1 1 	 V 1 Y- 	 1 | | l-l | 1 | ,' - ' 	
30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32ll2 32:24 32136 32U8 33:00 33:12 Time
357.8517 S:6 F:2 SMO(1,3) BSUB(128
100S

50J
-
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A3.71E3
f\^\
-—Ny^ 	 ^Vx~------~v/-l-X-x-/V^V-~-
30:12 30:24 30:36 30:48 31
367.8949 S:6 F:2 SMO(1,3) BSUB(128
100%
so:
0-



3b!i2 30124 3bl36 3ol48 31
369.8919 S:6 F:2 SMO(1,3) BSUB(128
100%.
50J
0"



30112 30124 3b:r36 3ol48 31
,15, -3.0) PKD(3,3,3,0.10%,1032.0,1.00%,F,F)
A2.29E4 7.8E3
A1.16E4 A
A A7.35E3 \ A6.6QE3
/ \ A. A A4..50E3I \ A
^x^--^^^-^"^^/^^^^^ W^XX/J^=:>^V^^ ^\^L_--^-A y^/vv\^^\y^

13.9E3
.
' O.OEO
:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 Time
,15, -3.0) PKD(3,3,3,0.10%,4788.0,1.00%,F,F)
A2.03E8
A
A
i\.
6.9E7
L3.5E7
" O.OEO
166 3ill2 31124 31136 31:48 32166 32112 32124 32136 32\48 33166 33112 Time
,15, -3.0) PKD(3,3,3,0.10%,2320.0,1.00%,F,F)
A1.30E8
A
f\
l\.
4.4E7
L2.2E7
' O.OEO
166 31:12 31124 3ll36 31:48 32166 32:12 32: 24 32:36 32148 33166 33ll2 Time
366.9792 S:6 F:2 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
lOOi 30:15 30:44

so:
0'
31:14 31:25 31:52 32:03 32:25 32:37 32:49 33:10 8. 3E7
V
3bll2 36124 3ol36 30:48 31

_4.2E7
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:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12 Time

-------
File: A17JUL98BAcq:  17-JUL-1998  20:31:20Exp:  EXP_M23_DB5_OVATION Voltage SIR EI+GC Autospec-UltimaEParadigm
Sample #6  Text: 1070-0  xl/2   ALS  #6
389.8156 S:6 F:3 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,2180.0,1.00%,F,F)
100$                                  A8.32E4                                                                     2.7E4
 so:

  0
A1.69E4
        A6.32E3
                                           J A4.62E4

                                              y  V9.53E3
                                                                A4.46E4  A4.51E4
                                                                          11.4E4


                                                                           O.OEO
      33:24    33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00    35:12    35:24   35:36    35:48  Time
391.8127 S:6 F:3 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,3516.0,1.00%,F,F)
                                       A3.35E4
                                             A3.43E4
                                       A3.62E4  A1.63E4
      33  24    33:36    33 48    34:00    34:12    34:24    34:36    34:48    35:00    35:12    35:24    35:36    35:48  Time
401.8559 S:6 F:3 BSUB(128,15,-3.0) PKD(3,5,2,0.10%,10300.0,1.00%,F,F)
100%                                                           A2.Q3E8
 50J
                                                                         A1.96E8
      33:24    33:36    33.:48    34:00   34:12    34:24    34:36   34:48    35:00
403.8530 S:6 F:3 BSUB(128,15,-3.0) PKD(3,5,2,0.10%,8084.0 ,1.00%,F,F)
lOOi                                                           A1.61E8
                                                          35:12    35:24
                                                                                                     35:36
 50J
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                                                                         A1.57E8
     '33:24'
                                34:00   34:12    34:24
380.9760 S:6 F:3 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100%            33jJ38    33:50          34:10    34:23    34:35
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                                                                              35^04   35:13   35:24   35:34
                                                                                        r_7.8E7
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                                                                      35:48  Time

                                                                          6.4E7


                                                                         .3.2E7
                                                                                        10.0EO
                                        T34UV  ' '35 loo' '  '35! 12' '  's'sbV  ' YshV '  '35:48  Time
                                                                                         1.8E8
r— i — | — r -T
 33:24
i — i — i — i — i
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                                                                                        L9.1E7
                                                                                                                 .O.OEO
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35:48  Time
 i — I — i — i
33:48
r~ T — I — i — i
 34:00
i — i — I — i — i
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                                                i — i — I — i — \
                                                 34:24
                                i — i — | — i — i — i — i — i — I — i — i
                                34:36    34:48
                                                                                                       i
                                                                           35:00    35:12    35:24    35:36

-------
File
Samp
423.
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: A17JUL98B Acq: 17-JUL-1998 20:31:
le #6 Text: 1070-0 xl/2 ALS #6
7767 S:6 F:4 SMO(1,3) BSUB (128 , 15 , -3
A4.79E4 A3.93E4
. - A. A..
36:00 36:12 36:24 36:36 36:48
7737 S:6 F:4 SMO(1,3) BSUB (128, 15, -3
A3.08E4
A1.72E4 A
^—^ r^^J\*~^^
36:00 36:12 36:24 36:36 36:48
8169 S:6 F:4 SMO(1,3) BSUB (128, 15, -3
1 1 1 1 1 1 1 1 1 1 1 | 1 1 1 1 1 I I I I I"T'T 1 I 1 1 1 | 1 1
36:00 36:12 36:24 36:36 36:48
8140 S:6 F:4 SMO(1,3) BSUB(128, 15, -3
36:00 36:12 36:24 36:36 36:48
9728 S:6 F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 .
35:57 36:14 36:27 36:41
f~
36:00 36:12 36:24 36:36 36:48
20 Exp: EXP_M23_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Parad
.0) PKD(3,3,3,0.10%,752.0,1.00%,F,F)
A9 . 7 5E4
/ 1 A3.45E4
/ V /\ A6.16E3
1 \ / \ 	 f~^^~~^/~\ 	 - f~\ r- 	 ^— .-•=»
37:00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:
.0) PKD(3,3,3,0.10%,972.0,1.00%,F,F)
A8 . 53E4
_/ \3^24E3 ^ 	 ^ ^^
37:00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:
.0) PKD(3,3,3,0.10%,5188.0,1.00%,F,F)
A1.32E8
' 37!6d 37I12 ' 37I24 ' 37I36 37I48 SsloO 38112 38I24 Ssls'e 38I48 39!
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A1.26E8
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2.6E4
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3.5E7
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37:00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:00 Time
00%, 0.0,1. 00%, F,F)
36:59 37:10 37:32 37:4337:52 38j_D838:17 38:29 38:45 rl.!E8

L5.7E7
"O.OEO
37:00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39 00 Time
o
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-------
File
Saim:
457.
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1001
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:: A17JUL98B Acq: 17-JUL-1998 20:31:20 Exp: EXP_M23 DBS OVATION Voltage SIR EH- GC Autospec-UltimaE Paradigm
)le #6 Text: 1070-0 xl/2 ALS #6
7377 S:6 F:5 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2084 . 0 , 1 . 00%, F, F)
A2.11E5 5.5E4
yy 	
39ll2 39124 39136 39148 4o!ob 4o!l2 ' 4ol24 ' ' ' 4o!36 ' ' ' 4ol48 41:
7348 S-.6 F:5 SMO(1,3) BSUB ( 128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 936 . 0, 1 . 00%, F, F)
A2.44E5
J\__
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
7780 S:6 F:5 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2372 . 0, 1 . 00%, F, F)
Al . 83E8
/V^
39ll2 39124 39136 39\48 4o!ob 4o!l2 4ol24 4o!36 4ol48 41 !
7750 S:6 F:5 SMO(1,3) BSUB(128 , 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1376 . 0, 1 . 00%, F, F)
A2.07E8
f\_
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
9728 S:6 F:5 SMO(1,3) PKD(3 , 3 , 3, 100 . 00%, 0 . 0, 1 . 00%, F, F)
39:05 39^21 39:42 39:52 40:03 40:13iQjJ9 40i42 40:48 40:55
1
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
_2.8E4
_O.OEO
00 Time
6.0E4
.3.0E4
.O.OEO
00 Time
4.2E7
'.2 . 1E7
.O.OEO
00 Time
_4.7E7
_2 . 4E7
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1.3E8
.6.4E7
O.OEO
DO Time
o
CO

-------
File: A17JUL98B Acq:
17-JUL-1998 20:31
20 Exp: EXP_M23_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm
Sample #6 Text: 1070-0 xl/2 ALS #6
303.9016 S:6 SMO(1,3)
100%

50 1
Q-

A1.26E4
-A-\ /v\
'~v"/V^s£jv^J-J--X-^-»'v/\_-'^
" 	 1 	 1 	 1 	 1 	 r 	 1 	 r
24:00
305.8987 S:6 SMO(1,3)
100%,
:
50 1
;
o:



-^vAswN-v^-^^Vx/V/VV
	 \ 	 1 	 1 	 1 	 1 	 1 	 r
24:00
315.9419 S:6 SMO(1,3)
100%
50 j
0 :



"-1 	 1 	 1 	 1 	 1 	 1 	 1 	 r
24:00
317.9389 S:6 SMO(1,3)
100%
50 j
0 '



"— ' 	 1 	 1 	 1 i 	 1 	 1 	 r
24:00
375.8364 S:6 SMO(1,3)
100%

-
C A •
50_
0 '



23:24
A /^3:47
U ' '!"' 	 "V--1 	 1 ' f "i
24:00
316.9824 S:6 SMO(1,3)
BSUB(128,15,-3.0)


A4.80E3
^_^/~-/\S^s-J^~^J**^
25 !00
BSUB(128,15,-3.0)



A1.08E4 r
^-^/vA^y^-^
25 loo'
BSUB(128,15,-3.0)



— i 	 1 	 1 	 1 	 1 	 1 	
25:00
BSUB(128,15,-3.0)



— i 	 1 	 \ 	 1 	 1 	 1 	
25:00
BSUB(128,15,-3.0)



_. _. 24:46 25:
24:24 A A
_^/V-^_~/ UA_A/W \
25 loo'
PKD(3,3,3,100.00%
100% 23:27 24:04 24:44 25:1
50 j
0 '
'

U-" 	 1 	 1 	 1 	 1 	 r—, 	 r
24:00


— i 	 > 	 1 	 1 	 1 	 1 	
25:00
PKD(3,3,3,0.10%,1292.0,1.00%,F,F)
A5.68E4 c 01o. 1.3E4
rt A6.91E4
/ 1 A
l\ A1.34E4 (\ ,-„. ,., T)^A A A1.99E4
/ \ A3 77E3A/\ AA7'05E3/ \ Al.b/E4 A±./^t.4l AA /-i
^V-^-^^-J-vJ1-/^ rJ V/^/-J--\\./X^/\/ WYV\ .-y/^A/ \/v^vV'S. /-y / \ ^ / V^'VV^'^v^v^

L6.7E3
: O.OEO
26:00 	 27 I 00 28:00 29loO 30:00 Time
PKD(3,3,3,0.10%,3424.0/1.00%,F,F)
A7.11E4 2.0E4
A A6.46E4
l\ A2.78E4 A
/ \ A /V\ L\ A A^\ AA
^\A^ N^yA^^^-^A^^A /^ X/\x-~^\V/A^^/^^^^^^~N^V^yv/ ^W ^^\AX VY

L1.0E4

1 O.OEO
26loO 27loO 28100 29loO 3oloO Time
PKD(3,3,3,0.10%,3712.0,1.00%,F(F)
A2.36E8
A
/v
_4.7E7
12.4E7
: O.OEO
26100 27100 28:00 29:00 30:00 Time
PKD(3,3,3,0.10%,5000.0,1.00%,F,F)
A3.01E8
A
/ V
6.1E7
_3.1E7
O.OEO
26loO 27100 28IOO 29:00 30:00 Time
PKD(3,3,3,100.00%,808.0,1.00%,F,F)
29:45 r!.3E4
?fl • 53 A
27:29 28:27 A L

^ 25^26^ ^34 ^^nJ\^^J\J\^\^J\ 2J\rA J \/u


_6.3E3
O.OEO
26100 27100 28100 29:00 30:00 Time
0.0,1.00%,F,F)
4 25:49 26:19 26:51 27:16 27:45 _ 28:25 28:52 ,_7.4E7
" ' V

L3.7E7
: O.OEO
26100 27100 28100 29loO 30:00 Time
O
CO
00

-------
     File:  A17JUL98BAcq: 17-JUL-1998 20:31:20Exp: EXP_M23_DB5_OVATION Voltage  SIR  EI+GC Autospec-UltimaE—Paradigm	
     Sample #6  Text: 1070-0 xl/2  ALS #6
     339.8597 S:6 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,944.0,1.00%,F,F)
     100%,                                                                            A5.98E4                            2.1E4
           Al.08E4
                                A2.25E3
                                             A4.70E4

                                                  I.66E3
                                                                     A2.86E4
                                                              A2.86E4   A   A1.97E4
                                                                                                    A8.76E3,
                                     11.0E4
                                                                                                                       .O.OEO
            I ' i  i i i I i i  i i i | i i  i i i | i i i  i i | i i"-l 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 fl~f r iT i  PIT i is T~? i i
          30:12   30:24   30:36   30:48   31:00  31:12  31:24  31:36  31:48   32:00   32:12  32:24  32:36  32:48  33:00  33:12    Time
     341.8568 S:6 F:2  SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,3456.0,1.00%,F,F)
     100%,                                                                            A2.23E4                            1.3E4
      50J
       0.
      3C)!i2 ' 30124 ' 36!36
                                                                                                                       _6.7E3
                                                                                                                       O.OEO
                                              ! 12 ' 3il24 ' 31\36 ' 31 Us '  32!6d ' 32!l2 ' 32124 ' 32136 ' 32U8 ' 33166 ' 33112    Time
    351.9000  S:6  F:2 SMO(1,3)  BSUB{128,15,-3.0) PKD(3,3,3,0.10%,1040.0,1.00%,F,F)
    100%                                                            A2.75E8         A2.94E8

      50J
       Oj
                                                                                                                   1.0E8

                                                                                                                  _5.1E7
                                                                                                                   O.OEO
         T'T'TT T 1  I I -r-r-r I  | | I I T I I  I' pT" 1 I I' T' I I T I—I—I—|~T—I—I I 1 I I T"T l—I j 1" I l—I"T"T I 1 "1"~T—1 [I I I 1  I I 1 1—I "I"*T 1 1 I*T""T' I^F"! I I " I "I 1  I I I I I I 1 " I I |"T'I I I
         30:12   30:24  30:36  30:48  31:00  31:12  31:24   31:36   31:48   32:00  32:12  32:24  32:36  32:48  33:00  33:12    Time
353.8970 S:6 F:2 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1860.0,1.00%,F,F)
100*.                                                            A1.76E8         A1.JJ8E8
      OJ
                                                                                                                       6.5E7

                                                                                                                      .3.3E7
                                                                                                                   O.OEO
         30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00  33:12    Time
409.7974 S:6 F:2 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,4384.0,1.00%,F,F)
                                                            31:48
               30:30                                    „,  „
 50 J
                                                                                             32:37
         30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00  33:12     Time
    366.9792 S:6 F:2 SMO(1,3)  PKD(3,3,3,100.00%,0.0,1. 00%, F, F)
    100%   30:15            30:44            31:14  31j25	
 50J

  ol
                                                               31:52  32:03
32:19  32:32
32:49
33:10
.8.3E7
                                                                                                                      _4.2E7

                                                                                                                       O.OEO
         "T i  I ' i i T—i—|—i i i—i—i—|  i i—i—i—i—|—i—i—i—i—i—|—i—i—r-T—i—i—i—i—i—i—i—I—i—i—i—i—i—i—i—i—i—i—i—I—i—i—ri—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—T
         30:12  30:24  30:36  30:48  31:00  31:12   31:24  31:36  31:48  32:00  32:12  32:24   32:36   32:48   33:00  33:12     Time
o
CO

-------
































"*1
"•*'
File: A17JUL98B Acq: 17-JUL-1998
Sample #6 Text: 1070-0 xl/2 ALS
373.8207 S: 6 F:3 SMO(1,3) BSUB(128
1003
50_
0

A3.21E4
A1.37E4A
/\7 V 	 A1.62E3
i i | I i i I i -| i T— r i t— p i i— T--I i
33:24 33:36 33:48 34:
375.8178 S:6 F:3 SMO(1,3) BSUB(128
1003
sol
-
o-

A2.03E4
— ^\/\~-^

33!24 33!36 33\48 34!
383.8639 S:6 F:3 BSUB (128, 15, -3 . 0)
lOOi
50.:
ol



33-124 33-136 33! 48 34-1
385.8610 S:6 F:3 BSUB(128, 15, -3 . 0)
100%
50J
o:



33!24 33!36 33!48 34?
445.7555 S:6 F:3 SMO(1,3) BSUB(128
lOOSi
50J
-
0"


33:3933:46
/"Xx1 	 y^-^-\>\/X^-^
'33:2'4' ' VsbV ' YsUV ' '34!
20:31:20 Exp: EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
#6
,15, -3.0) PKD(3,5,2,0.10%,2524.0
A6.62E4
/ \f\ A9.41E3

r i i i i | 1-1 i i 'T | i i ••! i r | i i i i
00 34:12 34:24 34:36
,15, -3.0) PKD{ 3, 5, 2, 0.10%, 1524.0
A4.06E4
/ VA A9.96E3
J 1 Y A6.69E3 ^C\ A7

00 34!l2 34?24 34!36

,1.00%,F,F)


^x__^_^ _x^_^^ /A — '^_ - __— -_^~^^_^-~ 	
2.2E4
L1.1E4
: O.OEO
34:48 35!oO 35:12 3S.-24 35:36 35 48 Time
,1.00%,F,F)


/75E3 A3.33E3 	 	 -^ ^
	 ~S| 	 .1 r *•• -v 	 -^ " 	 \ 	 . 	 ^_s 	 • 	 _S" 	 ^~^J
1.5E4
_7.4E3

O.OEO
34!48 35!oO 35!l2 35!24 3s!36 3s!48 Time
PKD(3,5,2,0.10%,48684.0,1.00%,F,F)
A1.51E8
A A
J ] ^^
00 34-1 12 34-124 34-136
PKD (3, 5, 2, 0.10%, 100276. 0,1. 00%,
A2.90E8
\ n
AA
/ Y v
00 34!l2 34!24 34!36
,15, -3.0) PKD(3,3,3,100.00%,1444
34-1!
7v

— ^ y^* ^ — '~\_/ \ /^~^
	 | i i r i i | , , i , . 1 . , , .
00 34:12 34:24 34:36



5 . 9E7
.3 . OE7
.O.OEO
34-148 35! 00 35-1 12 35-124 35-136 35-148 Time
F,F)



1.1E8
.5.6E7
_O.OEO
34!48 35!oO 35!l2 3s!24 3s!36 3s!48 Time
.0,1.00%,F,F)
;45 34:59

V~A / ^-^x 35-14 r~\

1.0E4
L5.2E3

LO.OEO
34! 48' ' '35! 00 35! 12' 35! 24 '35! 36' ' 3s!48 Time
380.9760 S:6 F:3 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
lOOSj 33^38 33:50
50 j
o"
y

33:24 33:36 33!48 34:
o
o
_34_il° 34:23 34:35


o'o' ' '34! 12' ' '34! 24' ' '34 be'


35^04 35:13 35:24 35:34 1 . 8E8


L9.1E7
: O.OEO
34:48 35:00 35:12 35:24 35:36 35:48 Time



-------
File: A17JUL98BAcq: 17-JUL-1998 20:31:20Exp: EXP_M23_DB5_OVATION Voltage SIR EI+GC Autospec-UltimaEParadigm
Sample #6  Text: 1070-0 xl/2  ALS #6
407.7818 S:6 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,2088.0,1.00%,F,F)
100%               A8.54E4                                       *                                                _2. 5E4
 50J

  OJ
                                                                                                                  1.3E4

                                                                                                                  .O.OEO
       36166 ' 36!i2 ' 36124 ' 36!36 ' 36U8  37:00  37:12  37:24  37:36  37:48  38:00  38:12  38:24  38:36  38:48  39:00
409.7788 S:6 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3 , 3 , 3,0.10%,1292.0,1. 00%, F, F)
100%               A8.51E4
                                                                                                                  2
       36:00  36:12  36:24  36:36  36:48  37:00  37:12  37:24  37:36   37:48  38:00  38:12  38:24  38:36  38:48  39:00
417.8253 S:6 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,6268 . 0,1. 00%, F, F)
100%,              A6.^8E7
                                                          A4.60E7
 50J                 M                                     A                                                  t-8
  o
       36:00  36:12  36i24
                                         37:00
419.8220 S:6 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,37392.0,1.00%,F,F)
100%,              A1.37E8
                                                          A1.05E8
                     I I
 50J

  OJ
                                                                               	  	  	
                                                       37I24 ' 37136 '  37:48  38:00  38:12  38:24  38:36  38:48  39:00
                                                                             T
       i i i  i i i i i I i  i < i i i n 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  36:12  36:24  36:36   36:48  37:00  37:12  37:24   37:36   37:48  38:00  38:12  38:24  38:36  38:48  39:00
479.7165 S:6 F:4 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,3672.0,1.00%,F,F)
100%               36:20                        37-10
               1C .
 50J
                                                                                                                     Time

                                                                                                                   .9E4

                                                                                                                   .5E4

                                                                                                                    OEO
                                                                                                                     Til

                                                                                                                   .8E7

                                                                                                                   .8E6

                                                                                                                   .OEO
                                                                                                                     Time

                                                                                                                   .OE7

                                                                                                                   .OE7

                                                                                                                   .OEO
                                                                                                                     Time
     T—I—I—I—I—I—I—I—I—I—1—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—f
       36:00  36:12  36:24   36:36   36:48  37iOO  37il2  37i24
430.9728 S:6 F:4 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100% 35:57     36:14  36:27    36:41	36:5_9  37:10  37:23
                                                                           38:00  38il2  38i24  38i36  38i48  39iOO
  OJ
                                                                 J37:4337:52    38-L_0838:17  38:29
                                                                                                     38:45
       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   36:12   36:24   36:36  36:48  37:00  37:12  37:24   37:36  37:48  38:00  38:12  38:24   38:36  38:48  39:00
                                                                                                                   .OEO
                                                                                                                    Time

                                                                                                                   .1E8

                                                                                                                   .7E7

                                                                                                                   .OEO
                                                                                                                    Time

-------
File: A17JUL98B
Sample #6 Text:
441.7427 S:6 F:5
100%
50 j
•
0 " "" — — 	 	 	 — -v^
39:12
443.7398 S:6 F:5
100%,
Acq: 17-JUL-1998 20:31:20 — ExpT~
1070-0 xl/2 ALS #6
SMO(1,3) BSUB(128,15,-3.0) PKD(3



^- — 	 	 — ~ 	 	 	 	
39!24 39!36 39548
SMO(1,3) BSUB(128,15,-3.0) PKD(3

EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
,3, 3, 0.10%, 1160.
A5
/
A5.12E3/

40:00
,3, 3, 0.10%, 1416.

0,1.00%,F,F)
• &OE4 1.3E4
\\
\ _6.7E3
__3^~ ^
— " 	 ' 	 	 	 ^-^ 	 -— ^ 	 _^ — ^_^~ — . — n OTTO
— i — p"1 — ' — ' — ' — ' — i — ' — ' — ' — r— ' — i — ' — i — ' — i — ' — i — ' — i — i — i — i — r -uljU
40:12 40:24 40:36 40:48 41 00 Time
0, 1.00%,F,F)
A6.75E4 2.1E4
: A5.91E4 /\ r - -
50J
0:— — • 	 	 	
39:12
469.7780 S:6 F:5
100S
50.
o: 	
39ll2
471.7750 S:6 F:5
100%
501
0:
39:12
513.6775 S:6 F:5
100%
50J
: 39:09
n: (^^ ^-^
39!l2
454.9728 S:6 F:5
100%39:05
50j
o.: , 	
39:12

A5.12E3
39524 39536 39548
SMO(1,3) BSUB(128,15,-3.0) PKD(3



39524 39536 39548
SMO(1,3) BSUB(128,15,-3.0) PKD(3



39524 39536 39548
SMO(1,3) BSUB(128,15,-3.0) PKD(3



39:23 J-\ 39:39
39:24 39536 39548
SMO(1,3) PKD(3,3,3,100.00%,0.0,1
39:21 39:42 39:


39524 39536 39548

—^-——^L
40:00
,3, 3, 0.10%, 2372.
Al . 83E8
/\
J V___
4o5ob
,3, 3, 0.10%, 1376.
A2 . 07E8
/\
J V__
1 1 1 -1 1 1 1 1 1
40:00
,3, 3, 100. 00%, 88.
40:01
/ \
/ V
J \ 	
4o!ob
.00%,F,F)
52 40:03


' 1 'T '!• | 1 1 II'
40:00
f\/\ i-124
	 V \ _^ 	 ^A1.89E3 	 ^ /^ „ npn
— i — | — i — i — i — i — i — | — i — i — i — i — i 7^1 — i — i — , < — TTT i^< i 7 '
40:12 40:24 40:36 40:48 41 00 Time
0, 1.00%,F,F)
4.2E7
_2.1E7
n npn
40:12 40!24 ' 4ol36 ' ' ' 40:48 41 00 Time
0,1.00%,F,F)
4.7E7
L2.4E7
•
i | I i i 'i "i1--] — r i i i i | i — i — i — i — i i i — i — i — i — i — C-U . UEU
40:12 40:24 40:36 40:48 41 00 Time
0,1.00%,F,F)
8.5E3
_4.3E3

	 40^15 	 ^A7 _/~\_ 4/^\ n nc-n
i 1 i i i r r 	 T^-I — T \ i '< 1 — i — i * i ' i i 1 i i ' i — i — ^-C-U.lmU
40:12 40:24 40:36 40:48 41 00 Time

40:1340_:19 40:42 40:48 40:55 1.3E8
_6.4E7
0 OF.O
•i (•— i 	 T""i " i i | "t'-'T — i 	 r-r- i 	 1 	 1 	 1 	 1 	 1 	 1— — i 	 1 	 1 	 1 	 1 	 f— '•' • u'-'"
40:12 40:24 40:36 40:48 41:00 Time
O
^
to

-------
                                                                      Paradigm Analytical Labs
Analytical Data Summary Sheet
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD

OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ(ND=0)
TEQ (ND=l/2)
Concentration
0.0146
0.0181
EMPC
0.0155
0.0180

0.0364
•010CT"!''-'
0.109
' 0:i34 *.$#
0.129
0.0480 :::':
0.0343
0.0096
0.0469
EMPC
0.0066
1.25
0.477
0.388
0.0588
9.70 .
2.39
0.460,
0.0616
0.139
0.139
lillP
0.0005
0.0004
0.0016
O.OQJ2
0.0012

0.0006
' "'$&&&.. :
0.0018
i/Jpjta:;?
0.0013
"0.0011
0.0012
0.0014
0.0011
0.0013
0.0008
0.0005
0.0004
0.0012
0.0007
0.0018
0.0018
0.0011
0.0011


r?8&*j

'•':\
0.0098




"'•'• '--'^

A/-: -^





0.0049

1.26
0.499
0.406

9.73


0.0664
0.140
0.140
JIT
- ' i'*f?:<"vJ
28:28
32:37
34:43
34*46
J"?»"»V
34:59
37:11
40:03
27^9
31:57
•>, 32:24^;-
34:11
34:15
34:38
35:12
36:22
37:32
40:10










ffiHy
0.83
1.49
1 67
A ,\J 1
1 I1?
1*U
1 28
JL >^O
1.13
0.87
0.77
L63
1.55
1.23
1.24
1.31
1.26
1.02
1.24
0.95










Qualifier

























ITEF
ITEF
Client Information

Project Name:
Sample ID:

Laboratory Information

Project ID:
SamplelD:
CoBecHonCate:
                          Texas Lime Kiln
                          M23-I-1
                          L1070
Sample Information

Matrix:
Weight/Volume:
Moisture / Lipids:
          ite:
                                                                          Air
                                                                           1
                                                                          0.0    %
                    al7ju!98b-10
             •:  '    •**
             1-;--.''-^
                    al
         ^  > -,;?.;ip$29Q-23-071798
                                         1/2
                                                                                            043

-------
                                                                       Paradigm Analytical Labs
                              Analytical Data Summary Sheet
Labeled
Standard
Extraction Standards
13CI2-2,3,7,8-ircDD
13Cl2-U,3,7i8-PeCDD
13C12-l,2,3,6,7,8-HxCDD

13C12-OCDD
0Cir2,3,7,8-TCDF
13C,2-l,2,3,7,8-PeCDF
uC,2-l,2,3,6,7,8-HxCDF
13C12-l,2,3,4,6,7,8-HpCDF
Sampling Standards
37Cl4-2,3)7,8-TCDD
13C12-2,3,4,7,8-PeCDF
'3C12-l,2,3,4,7,8-HxCDD
13C12-l,2,3,4,7,8-HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
Injection Standards
BCu-lA3t4-TCDD
13C12-l,2,3,7,8,9-HxCDD
Expected 1 :
Amount i
(.«&)

4
..,4^.
4
"4,..*."r
8
•4..'::.^
4
4
4

4
4
4
4
4



Measured

3.79
••Jip;,
3.54
.•;. -.3,75"
6.72
'"'^te ••:••
3.84
3.22
3.15

2.77
2.44
3.01
2.25
1.33



"»;;^j •

94.8
108.8
88.6
93.7
84.0
'\. 95^ V
95.9
80.6
78.8

693
61.0
75.3
56.2
33.2



(mid.)

28:27
32:37
34:46
37: tO
40:02
,27:26
31:57
34:15
36:22

28:28
32:24
34:42
34:11
37:32

28:09
34:59


0.78
1.56
1.25
1.04
0.89
0.79
1.56
0.52
0.44


1.56
1.24
0.52
0.43

0.79
1.25
Qualifier



















Client Information
Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:

Collection Date:
Receipt Bate;
Extraction Date:
Analysis Date:
 ^ ->   7 ->* f ** \          *•

Reviewed by; *^>TI
                          Texas Lime Kiln
                          M23-I-1
                          L1070
                          1070-1
                             25-Jun-98
Sample Information

Matrix:
Weight/Volume:
Moisture / Lipids:
Filename:
Retchk:
Begin ConCal:
EndConCaL
                                                                           Air
                                                                            1
                                                                           0.0
al7ju!98b-10
al7jul98b-l
                                                                        al7ju!98b-15
                                                                   Date Reviewed: 2
                                         212

-------
o
^
en
OPUSquan 20-JUL-1998
Filename a!7ju!98b
Sample 10
Acquired 17-JUL-98
Processed 20-JUL-98
Sample ID 1070-1 xl/2
Page 1


23:31:42
09:06:13














-^








f
t\,»*
ft 4>

,ii
^v^\
w











Cal Table m8290-23-071798 Vjv
Results Table M8290-23-071798B
Comments
Typ
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS
SS
SS
SS
SS
SS
Name;
2,3,7,8-TCDD;
1, 2,3,7, 8-PeCDD;
1,2,3,4,7, 8-HxCDD;
1,2,3,6,7,8-HxCDD;
1,2,3,7,8,9-HxCDD;
1,2,3,4,6,7,8-HpCDD;
OCDD;
2,3,7,8-TCDF;
1, 2,3,7, 8-PeCDF;
2,3,4,7,8-PeCDF;
1,2,3,4,7,8-HxCDF;
1,2,3,6,7,8-HxCDF;
2,3,4,6,7,8-HxCDF;
1,2,3,7,8,9-HxCDF;
1,2,3,4,6,7, 8-HpCDF;
1,2,3,4,7,8,9-HpCDF;
OCDF;
13C-2,3,7,8-TCDD;
130-1, 2,3,7, 8-PeCDD;
130-1, 2, 3,6,7, 8-HxCDD;
13C-1 ,2,3,4,6,7, 8-HpCDD;
13C-OCDD;
130-2, 3,7, 8-TCDF;
130-1 ,2,3,7, 8-PeCDF;
13C-l,2,3,6,7,8-HxCDF;
13C-l,2,3,4,6,7,8-HpCDF;
130-1,2,3,4-TCDD;
13C-l,2,3,7,8,9-HxCDD;
37Cl-2,3,7,8-TCDD;
13C-2 ,3,4,7, 8-PeCDF;
130-1, 2, 3,4,7, 8-HxCDD;
130-1,2,3,4,7,8-HxCDF;
13C-l,2,3,4,7,8,9-HpCDF;
3701-2, 3,7, 8-TCDD;
130-2 ,3,4,7, 8-PeCDF;
130-1 , 2,3,4,7, 8-HxCDD;
13C-l,2,3,4,7,8-HxCDF;
13C-1,2,3,4, 7,8,9-HpCDF;


Resp;
1. 80e+06;
1.82e+06;
6.60e+05;
1.336+06;
1.56e+06;
2.126+06;
2.07e+06;
1.536+08;
1.196+07;
1. 51e+07, •
1. 18e+07 , •
5.51e+06;
3.386+06;
8.23e+05;
3.71e+06;
3.21e+05;
4.03e+05;
4.526+08;
3.616+08;
4.02e+08;
3.156+08;
4.55e+08;
5.71e+08;
4.99e+08;
4.22e+08;
2.51e+08;
4.34e+08;
4.23e+08;
2.86e+08;
2.986+08;
2.046+08;
1.86e+08;
6.52e+07;
2.86e+08;
2.986+08;
2.04e+08;
1.866+08;
6.52e+07;

Ion 1;
7.37e+05;
1.09e+06;
4.13e+05;
7.06e+05;
8.77e+05;
1.12e+06;
9.62e+05;
6.666+07;
7.35e+06;
9.17e+06;
6.496+06;
3.05e+06;
1.926+06;
4.596+05;
1.87e+06;
1.77e+05;
1.976+05;
1.986+08;
2.206+08;
2.246+08;
1.616+08;
2.14e+08;
2.52e+08;
3.04e+08;
1.456+08;
7.68e+07;
1.92e+08;
2.356+08;
2.86e+08;
1.81e+08;
1.13e+08;
6.346+07;
1.976+07;
2.866+08;
1.81e+08;
1.13e+08;
6.346+07;
1.976+07;

Ion 2;
1.06e+06;
7.336+05;
2.486+05;
6.246+05;
6.82e+05;
l.OOe+06;
l.lle+06-
8.656+07;
4.52e+06;
5.926+06;
5.266+06;
2.46e+06;
1.47e+06;
3.64e+05;
1.846+06;
1.436+05;
2.066+05;
2.546+08;
1.416+08;
1.786+08;
1.546+08;
2.406+08;
3.19e+08;
1.95e+08;
2.776+08;
1.74e+08;
2.43e+08;
1.886+08;
-;
1.16e+08;
9.12e+07;
1.23e+08;
4.556+07;
_ .
1.16e+08;
9.12e+07;
1.23e+08;
4.55e+07;

RA;?;
0.69;y;
1.49;y;
1.67;n;
1.13;y;
1.28;y;
1.13,-y;
0.87;y;
0.77;y;
1.63;y;
1.55;y;
1.23;y;
1.24;y;
1.31;y;
1.26;y;
1.02;y;
1.24;n;
0.95;y;
0.78;y;
1.56;y;
1.25;y;
1.04;y;
0.89;y;
0.79;y;
1.56,-y;
0.52;y;
0.44;y;
0.79;y;
1.25;y;
- ; - ;
1.56;y;
1.24;y;
0.52;y;
0.43;y;
_ . _ .
1.56;y;
1.24;y;
0.52;y;
0.43;y;

RT;
28:28;
32:37;
34:43;
34:46;
34:59;
37:11;
40:03;
27:29;
31:57;
32:24;
34:11;
34:15;
34:38;
35:12;
36:22;
37:32;
40:10;
28:27;
32:37;
34:46;
37:10;
40 : 02 ;
27:26;
31:57;
34:15;
36:22;
28:09;
34:59;
28:28;
32:24;
34:42;
34:11;
37:32;
28:28;
32:24;
34:42;
34:11;
37:32;

Cone;
0.405;
0.452;
0.244;
0.388;
0.451;
0.752;
0.909;

^ZTTZQ]
3.351;
3.233;
1.200;
0.858;
0.240;
1.173;
0.123;
0.166;
94.746;
108.756;
88.602;
93.683;
167.968;
95.373;
95.901;
80.565;
78.818;
90.053;
106.614;
65.473;
58.436;
66.782;
45.629;
26.175;
69.143;
60.955;
75.275;
56.187;
33.221;

DL;
0.0122;
0.0095;
0.0389;
0.0307;
0.0304;
0.0171;
0.0144;
0.0443;
0.0457;
0.0442;
0.0333;
0.0264;
0.0307;
0.0353;
0.0271;
0.0328;
0.0195;
0.0328;
0.0242;
0.0333;
0.0230;
0.0112;
0.0222;
0.0144;
0.0990;
0.0384;
-;
-;
0.0117;
0.0147;
0.0494;
0.1270;
0.0491;
0.0127;
0.0093;
0.0577;
0.1359;
0.0838;

S/N1;?;
89;y;
143;y;
23;y;
36, -y;
35;y;
207;y;
165;y;
1176;y;
216;y;
235;y;
210;y;
104;y;
52, -y;
13 ;y;
12 1 * v *
10;y;
33;y;
5611;y;
26720;y;
7648;y;
5707;y;
20398;y;
9170;y;
48034;y;
4022 ;y;
3554;y;
5603;y;
8240;y;
16203 ; ;y;
30676;y;
4987 ;y;
1736, -y, •
839;y;
16203 ;y;
30676;y;
4987 ;y;
173 6; y;
839;y;

S/N2;?
107 ;y
156;y
16;y
27;y
25;y
94 ;y
233;y
1732 ;y
239;y
258;y
188;y
94 ;y
48;y
12,-y
142, -y
11, -y
25;y
13814;y
18804;y
7795;y
17845;y
34679,-y
18445;y
22227;y
2424 ;y
5227 ;y
13533;y
8615;y
-; -
13931;y
5246;y
1050 ;y
1229;y
-; -
13931;y
5246;y
1050;y
1229;y
mod?
no
no
no
no
no
no
no
no /./.
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
                                                                                                                                                    Page 15

-------
OPUSquan   20-JUL-1998
                                      Page 1
                                                                    Page 1 of 8

 Ent: 39 Name: Total Tetra-Furans  F:l  Mass:  303.902 305.899 Mod?  no   #Hom:25

 Run: 15 File: a!7ju!98b    S:10 Acq:17-JUL-98 23:31:42 Proc:20-JUL-98  09:06:13
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*.
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 243.37  of which 28.16
     Cone: 243.37  of which 28.16
                        Tox #2:  -
   Tox #1: -

Name
named and 215.22  unnamed
named and 215.22  unnamed
      Tox #3: -
2,3,7,8-TCDF
                         RT Respnse
                                        RA
                   1  23:41 9.8e+07  0.76 y
                            9.8e+07

                   2  24:15 4.8e+07  0.76 y
                            4.8e+07

                   3  24:34 4.4e+07  0.77 y
                            4.4e+07

                   4  24:52 2.0e+08  0.76 y
                            2.0e+08

                   5  24:59 5.1e+07  0.76 y
                            5.1e+07

                   6  25:11 4.7e+07  0.76 y
                            4.7e+07

                   7  25:17 1.46+08  0.77 y
                            1.4e+08

                   8  25:41 4.2e+07  0.75 y
                            4.2e+07

                   9  25:45 7.3e+07  0.77 y
                            7.3e+07

                   10 26:01 3.7e+07  0.76 y
                            3.7e+07

                   11 26:09 5.8e+07  0.77 y
                            5.8e+07
                                              Cone

                                              18.08
                                                   <
                                                   C
                                               8.82


                                               8.12
                                                   ]

                                              36.88
                                                   £
                                                   1
                                               9.31


                                               8.58


                                              24.92
                                                   C

                                               7.79
                                                   ]

                                              13.47

                                                   t
                                               6.76
                                                   1
                                                   2
                                              10.76
                  Area  Height
                                                                      S/N  Mod?
                   12 26:26 l.le+08  0.76 y   19.64
                            l.le+08

                   13 26:34 9.2e+07  0.76 y   16.96
                            9.2e+07

                   14 26:51 5.3e+07  0.76 y    9.70
                            5.3e+07

                   15 27:04 2.9e+06  0.76 y    0.53
                            2.9e+06

                   16 27:11 2.5e+07  0.76 y    4.60
                            2.5e+07

                   17 27:29 1.5e+08  0.77 y   28.16
                            1.5e+08

                   18 28:03 3.0e+07  0.76 y    5.45
                            3.0e+07

                   19 28:20 1.7e+07  0.74 y    3.19
                            1.7e+07
                .3e+07 9.1e+06 l.le+03 y  n
               5.6e+07 1.2e+07 1.6e+03 y  n
              2
               2.1e+07 4.5e+06 5.2e+02 y  n
               2.7e+07 6.1e+06 8.0e+02 y  n

                .9e+07 4.2e+06 4.8e+02 y  n
               2.5e+07 5.4e+06 7.1e+02 y  n

               J.7e+07 1.7e+07 2.0e+03 y  n
               l.le+08 2.2e+07 2.9e+03 y  n
              1
               2.2e+07 3.3e+06 3.8e+02 y  n
               2.9e+07 4.36+06 5.7e+02 y  n
              3
               2.0e+07 4.5e+06 5.2e+02 y  n
               2.7e+07 5.8e+06 7.7e+02 y  n
              2
               5.96+07 7.96+06 9.1e+02 y  n
               7.7e+07 l.Oe+07 1.4e+03 y  n

                .8e+07 4.9e+06 5.6e+02 y  n
               2.4e+07 6.4e+06 8.4e+02 y  n
              7
               3.2e+07 6.36+06 7.3e+02 y  n
               4.1e+07 8.26+06 l.le+03 y  n

               1.6e+07 3.4e+06 4.0e+02 y  n
               2.1e+07 4.5e+06 5.9e+02 y  n
              5
               2.56+07 5.4e+06 6.3e+02 y  n
               3.36+07 7.0e+06 9.2e+02 y  n
              1
               4.6e+07 9.0e+06 l.Oe+03 y  n
               6.1e+07 1.2e+07 1.6e+03 y  n
              5
               4.0e+07 8.3e+06 9.6e+02 y  n
               5.2e+07 l.le+07 1.4e+03 y  n
              3
               2.3e+07 4.6e+06 5.3e+02 y  n
               3.0e+07 6.0e+06 7.8e+02 y  n
              3
               1.2e+06 3.3e+05 3.8e+01 y  n
               1.6e+06 4.1e+05 5.4e+01 y  n

               l.le+07 2.3e+06 2.6e+02 y  n
               1.4e+07 3.0e+06 3.9e+02 y  n

               6.7e+07 l.Oe+07 1.2e+03 y  n
               8.7e+07 1.36+07 1.7e+03 y  n

               1.3e+07 2.6e+06 3.0e+02 y  n
               1.7e+07 3.4e+06 4.4e+02 y  n
              ?
               7.4e+06 1.4e+06 1.7e+02 y  n
               l.Oe+07 1.9e+06 2.5e+02 y  n
                                                                                                   Of/  046

-------
3PUSquan   20-JUL-1998
Page 2
                   20  28:33  3.1e+06   0.75 y     0.58
                            3.1e+06

                   21  28:53  5.7e+05   1.04 n     0.11
                            5.7e+05

                   22  29:05  2.4e+05   0.74 y     0.04
                            2.4e+05

                   23  29:18  5.0e+05   0.82 y     0.09
                            5.0e+05

                   24  29:48  4.2e+06   1.19 n     0.77
                            4.2e+06

                   25  30:00  3.1e+05   1.12 n     0.06
                            3.1e+05
             1.4e+06 2.
             1.8e+06 3.
            L
             2.9e+05 5.
             2.86+05 5.
            1
             l.Oe+05 3.
             1.4e+05 4.
            9
             2.2e+05 6.
             2.7e+05 7.
            7
             2.3e+06 4.
             1.9e+06 3.

             1.7e+05 3,
             1.5e+05 3.
6e+05 3.0e+01 y  n
5e+05 4.6e+01 y  n

9e+04 6.86+00 y  n
7e+04 7.56+00 y  n

, Oe+04 3.5e+00 y  n
,le+04 5.3e+00 y  n

.Oe+04 6.9e+00 y  n
.Oe+04 9.26+00 y  n

.le+05 4.8e+01 y  n
.6e+05 4.7e+01 y  n

.8e+04 4.4e+00 y  n
8e+04 5.0e+00 y  n

-------
OPUSguan   20-JUL-1998
                                      Page 3
                                                                   Page  2  of  8

 Ent: 40 Name: Total Tetra-Dioxins F:l  Mass:  319.897  321.894 Mod? no   #Hom:15

 Run: 15 File: al7ju!98b    S:10 Acq:17-JUL-98 23:31:42  Proc:20-JUL-98 09:06:13
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3 . 5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 31.42
     Cone: 31.42
   Tox #1: -
Name
2,3,7,8-TCDD
of which 0.41
of which 0.41
     Tox #2:  -

#     RT Respnse
named and 31.01
named and 31.01
      Tox #3:  -
                                        RA
1  25:16 5.6e-t-07  0.77 y
         5.6e+07

2  25:41 2.8e+07  0.77 y
         2.86+07

3  26:04 4.9e+06  0.80 y
         4.9e+06

4  26:55 1.8e+07  0.78 y
         1.8e+07

5  27:08 3.5e+06  0.81 y
         3.5e+06

6  27:17 4.6e+06  0.79 y
         4.6e+06

7  27:24 9.1e+05  1.02 n
         9.1e+05

8  27:46 3.9e+06  0.81 y
         3.9e+06

9  28:11 4.8e+06  0.77 y
         4.8e+06

10 28:20 8.3e+06  0.77 y
         8.3e+06

11 28:28 1.8e+06  0.69 y
         1.8e+06

12 28:40 1.7e+06  0.79 y
         1.7e+06

13 28:58 1.8e+06  0.80 y
         1.8e+06

14 29:18 5.8e+05  0.77 y
         5.8e+05

15 29:54 4.7e+05  0.69 y
         4.7e+05
          Cone

          12.69
              2
              3
           6.40
              1
              1
           1.09
              2
              2
           3.95
              1
              S
           0.79
              3
              ]
           1.03


           0.21


           O.I


           1.09


           1.87

              4
           0.41
              1
              1
           0.37
              1
              9
           0.40
              £
              c
           0.13


           0.11
    unnamed
    unnamed
                                                     Area  Height
                                                  S/N  Mod?
 2.5e+07 5.3e+06  3.3e+03  y  n
 3.2e+07 6.8e+06  3.4e+03  y  n
3
 1.2e+07 2.6e+06  1.6e+03  y  n
 1.6e+07 3.4e+06  1.7e+03  y  n
3
 2.2e+06 4.5e+05  2.8e+02  y  n
 2.7e+06 5.7e+05  2.9e+02  y  n

 7.7e+06 1.4e+06  8.5e+02  y  n
 9.8e+06 1.8e+06  8.9e+02  y  n
9
 1.6e+06 2.4e+05  1.5e+02  y  n
 1.9e+06 3.1e+05  1.5e+02  y  n

 2.0e+06 4.0e+05  2.5e+02  y  n
 2.6e+06 5.1e+05  2.6e+02  y  n
1
 4.6e+05 l.Oe+05  6.4e+01  y  n
 4.5e+05 l.le+05  5.3e+01  y  n
3
 1.7e+06 3.6e+05  2.2e+02  y  n
 2.2e+06 4.5e+05  2.3e+02  y  n
3
 2.1e+06 4.3e+05  2.7e+02  y  n
 2.7e+06 5.4e+05  2.7e+02  y  n
7
 3.6e+06 6.9e+05  4.3e+02  y  n
  .7e+06 8.7e+05  4.4e+02  y  n

 7.4e+05 1.4e+05  8.9e+01  y  n
 l.le+06 2.1e+05  l.le+02  y  n
7
 7.3e+05 1.4e+05  8.9e+01  y  n
 9.3e+05 1.9e+05  9.3e+01  y  n
                                                   8.06+05  1.6e+05  9.9e+01 y n
                                                   9.9e+05  2.0e+05  l.Oe+02 y n
                                                  3
                                                   2.5e+05  5.5e+04  3.4e+01 y n
                                                   3.3e+05  6.7e+04  3.4e+01 y n
                                                  L
                                                   1.96+05  3.96+04  2.4e+01 y n
                                                   2.8e+05  5.9e+04  3.0e+01 y n
                                                                                                   frf048

-------
OPUSguan   20-JUL-1998
                   Page  4
                                                                    Page 3  of  8

 Ent: 41 Name: Total Penta-Furans  F:2  Mass:  339.860 341.857  Mod?  no   #Hom:16

 Run: 15 File: al7ju!98b    S:10 Acq:17-JUL-98 23:31:42 Proc:20-JUL-98 09:06:13
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results:  M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 59.75
     Cone: 59.75
   Tox #1: -
Name
 1,2,3,7,8-PeCDF
 2,3,4,7,8-PeCDF
of which 6.08
of which 6.08
     Tox #2:  -

#     RT Respnse
named and 53.67
named and 53.67
      Tox t3:  -
                                        RA
1  30:17 3.3e+07  1.52  y
         3.3e+07

2  31:16 1.8e+07  1.57  y
         1.8e+07

3  31:22 7.7e+07  1.53  y
         7.7e+07

4  31:30 1.26+07  1.53  y
         1.2e+07

5  31:36 1.7e+06  1.43  y
         1.7e+06

6  31:39 1.7e+06  1.77  y
         1.7e+06

7  31:45 3.7e+07  1.50  y
         3.7e+07

8  31:55 1.7e+07  1.47  y
         1.7e+07

9  31:57 1.2e+07  1.63  y
         1.26+07

10 32:04 6.9e+06  1.48  y
         6.9e+06
                    11  32:08 1.56+07
                            1.56+07
                  1.53 y
12 32:24 1.5e+07  1.55 y
         1.56+07

13 32:30 1.4e+07  1.46 y
         1.46+07

14 32:36 7.5e+05  1.47 y
         7.5e+05

15 32:39 1.7e+06  1.49 y
         1.7e+06

16 32:58 l.Oe+06  1.52 y
         l.Oe+06
          Cone

           7.40
               2
               1
           4.08
               1
               1
          17.38
               4
               3
           2.77
               1
               4
           0.38
               c
               e
           0.39
               1
               e
           8.33

               3
           3.94
               1
               1
           2.73

               <
           1.57
               4

           3.44
               c
               6
           3.35
               S
                C
           3.23
                £
                c
           0.17
                <

           0.38
                1
                e
           0.23
   unnamed
   unnamed
                                                      Area  Height
                                  S/N  Mod?
                                                   2.0e+07 3.8e+06 2.7e+02 y  n
                                                   1.3e+07 2.5e+06 3.0e+02 y  n
                                                  3
                                                   l.le+07 3.8e+06 2.7e+02 y  n
                                                   7.0e+06 2.4e+06 2.9e+02 y  n
                                                  3
                                                   4.6e+07 1.4e+07 1.Oe+03 y  n
                                                   3.0e+07 9.4e+06 l.le+03 y  n
                                                  7
                                                   7.4e+06 2.1e+06 1.5e+02 y  n
                                                   4.8e+06 1.4e+06 1.7e+02 y  n

                                                   9.8e+05 3.9e+05 2.8e+01 y  n
                                                   6.8e+05 2.66+05 3.1e+01 y  n
 l.le+06  3.86+05  2.7e+01  y  n
 6.3e+05  2.26+05  2.6e+01  y  n
}
 2.2e+07  7.1e+06  5.0e+02  y  n
 1.5e+07  4.8e+06  5.8e+02  y  n

 l.Oe+07  3.5e+06  2.5e+02  y  n
 7.1e+06  2.3e+06  2.86+02  y  n
J
 7.3e+06  3.16+06  2.2e+02  y  n
 4.5e+06  2.0e+06  2.4e+02  y  n
 4.1e+06 l.Se+06 l.le+02 y  n
 2.8e+06 l.Oe+06 1.2e+02 y  n
1
 9.2e+06 3.36+06 2.3e+02 y  n
 6.0e+06 2.2e+06 2.6e+02 y  n

 9.2e+06 3.3e+06 2.4e+02 y  n
 5.9e+06 2.26+06 2.6e+02 y  n

 8.56+06 2.9e+06 2.1e+02 y  n
 5.8e+06 2.06+06 2.3e+02 y  n

 4.5e+05 1.7e+05 1.2e+01 y  n
 3.0e+05 l.le+05 1.3e+01 y  n
                                                    l.Oe+06  3.5e+05  2.5e+01 y n
                                                    6.86+05  2.36+05  2.86+01 y n
                                                   5
                                                    6.0e+05  2.26+05  1.5e+01 y n
                                                    4.0e+05  l.Se+05  1.7e+01 y n
                                                                     Page 4 of 8

  Ent:  42 Name:  Total Penta-Dioxins F:2   Mass:  355.855  357.852  Mod?  no   #Hom:ll

  Run:  15 File:  al7ju!98b    S:10 Acq:17-JUL-98 23:31:42  Proc:20-JUL-98 09:06:13
  Tables: Run:  a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
  Version: V3.5  17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
                                                                                                 rr ' 049

-------
OPUSguan 20-JUL-1998
Amount: 12.48 of
Cone: 12.48 of
Tox #1: -
Name f
1


2


3


4


5


6


7


8


1,2,3,7,8-PeCDD 9


10


11



which 0 .
which 0 .
Tox #2

45
45
: -
RT Respnse
31:30 1.
1.

31:49 1.
1.

32:00 1.
1.

32:04 1.
1.

32:10 7.
7.

32:20 2.
2.

32:26 3.
3.

32:30 1.
1.

32:37 1.
1.

32:43 9.
9.

32:54 7.
7.

6e+07
6e+07

Oe+06
Oe+06

3e+07
3e+07

8e+06
8e+06

8e+06
8e+06

2e+06
2e+06

8e+06
8e+06

6e+06
6e+06

8e+06
8e+06

3e+05
3e+05

4e+05
4e+05

Page 5
named and
named and
Tox
RA
1.51 y


1.53 y


1.54 y


1.43 y


1.49 y


1.10 n


1.60 y


1.67 y


1.49 y


1.62 y


1.42 y



12
12
#3

.03
.03
: -
Cone
3


0


3


0


1


0


0


0


0


0


0


.88
9
6
.25
6
4
.21
7
5
.44
1
7
.95
4
3
.55
1
1
.94
2
1
.39
9
6
.45
1
7
.23
5
3
.18
4
3






unnamed
unnamed

Area

.4e+06
.2e+06

.le+05
.Oe+05

.9e+06
.le+06

.Oe+06
.3e+05

.7e+06
.2e+06

.2e+06
.le+06

.3e+06
.5e+06

.9e+05
.Oe+05

.le+06
.3e+05

.7e+05
.5e+05

.3e+05
.le+05

Height

3.1e+06
2.06+06

2.2e+05
l.Se+05

2.8e+06
1.8e+06

3.8e+05
2.6e+05

1.7e+06
1. le+06

3.66+05
2.3e+05

8.5e+05
5.4e+05

3.6e+05
2.2e+05

4.0e+05
2.7e+05

2. Oe+05
1.2e+05

1.6e+05
1. le+05



1
1

8
8

1
1

1
1

6
6

1
1

3
3

1
1

1
1

7
7

5
6

S/N

.16+03
.2e+03

.le+01
.6e+01

.Oe+03
.le+03

.4e+02
.5e+02

.le+02
.7e+02

.3e+02
.3e+02

.le+02
.2e+02

.3e+02
.3e+02

.4e+02
.6e+02

.2e+01
.Oe+01

.9e+01
.4e+01


Mod?

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n
050

-------
OPUSquan   20-JUL-1998
                                      Page 6
 Ent: 43 Name: Total Hexa-Furans
                                                 Page  5  of  8

                F:3   Mass:  373.821  375.818  Mod? no   #Hom:12
 Run: 15 File: a!7ju!98b    S:10 Acq:17-JUL-98 23:31:42 Proc:20-JUL-98  09:06:13
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 11.52
     Cone: 11.52
   Tox #1: -
Name
of which 5.53
of which 5.53
     Tox #2:  -

#     RT Respnse
named and 5.99
named and 5.99
      Tox #3:  -
                                        RA
                   1  33:32 5.5e+06  1.18 y
                            5.56+06

                   2  33:38 1.3e+07  1.24 y
                            1.3e+07

                   3  33:43 8.3e+05  1.32 y
                            8.36+05
                      33:49 9.8e+05
                            9.8e+05
                  1.33  y
                   5  33:55 5.3e+05  1.33 y
                            5.3e+05
                      34:03 2.36+04
                            2.36+04
                                     1.73 n
1,2,3,4,7,8-HxCDF  7  34:11 1.2e+07  1.23 y
                            1.2e+07

1,2,3,6,7,8-HxCDF  8  34:15 5.5e+06  1.24 y
                            5.5e+06

                   9  34:20 l.le+06  1.38 y
                            l.le+06

                   10 34:28 1.2e+06  1.39 y
                            1.2e+06

2,3,4,6,7.8-HxCDF  11 34:38 3.4e+06  1.31 y
                            3.4e+06

1,2,3,7,8,9-HxCDF  12 35:12 8.2e+05  1.26 y
                            8.2e+05
          Cone

           1.41


           3.37

               C
           0.21
               i

           0.25
               c
               4
           0.14


           0.01
               3
               £
           3.23
               e
               c
           1.20


           0.29
               f
               <
           0.31

               C
           0.86
               3
               :
           0.24
    unnamed
    unnamed
                                                      Area  Height
                                                   S/N  Mod?
 3.0e+06 l.le+06  l.le+02  y  n
 2.5e+06 9.2e+05  l.le+02  y  n
7
 7.3e+06 2.6e+06  2.7e+02  y  n
 5.9e+06 2.0e+06  2.4e+02  y  n
L
 4.7e+05 1.5e+05  1.5e+01  y  n
 3.6e+05 l.le+05  1.3e+01  y  n

 5.6e+05 1.9e+05  1.9e+01  y  n
 4.2e+05 1.4e+05  1.7e+01  y  n
1
 3.1e+05 l.Oe+05  l.le+01  y  n
 2.3e+05 8.7e+04  l.Oe+01  y  n
L
 1.5e+04 5.9e+03  6.2e-01  n  n
 8.5e+03 3.3e+03  3.8e-01  n  n

  .5e+06 2.0e+06  2.1e+02  y  n
 5.3e+06 1.6e+06  1.9e+02  y  n
D
 3.1e+06 l.Oe+06  l.Oe+02  y  n
 2.5e+06 8.1e+05  9.4e+01  y  n

  .56+05 2.1e+05  2-le+Ol  y  n
  .7e+05 1.6e+05  1.8e+01  y  n

 7.1e+05 1.7e+05  l.Se+01  y  n
 5.1e+05 1.2e+05  1.4e+01  y  n
                                1.96+06 4.9e+05 5.26+01 y  n
                                1.56+06 4.1e+05 4.86+01 y  n

                                4.6e+05 1.3e+05 1.3e+01 y  n
                                3.66+05 l.Oe+05 1.2e+01 y  n
                                                                    Page 6 of 8

 Ent: 44 Name: Total Hexa-Dioxins  F:3  Mass: 389.816 391.813 Mod? no   #Hom:10

 Run: 15 File: al7ju!98b    S:10 Acq:17-JUL-98 23:31:42 Proc:20-JUL-98 09:06:13
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-1 xl/2
   Amount:  10.16
     Cone:  10.16
   Tox #1:  -
Name
of which 1.08
of which 1.08
     Tox #2: -

#     RT Respnse
named and 9.08
named and 9.08
      Tox #3: -
                                        RA
                    1   33:52 2.0e+06  1.21 y
                            2.0e+06

                    2   34:11 2.3e+07  1.25 y
                            2.3e+07
                           Cone

                            0.63
                                ]
                                t
                            7.08
    unnamed
    unnamed
                                                      Area  Height
                                  S/N  Mod?
               l.le+06 3.9e+05 6.1e+01 y  n
               9.1e+05 3.2e+05 4.7e+01 y  n
               3
               1.3e+07 4.3e+06 6.7e+02 y  n
                                                                                                         '  os:

-------
OPUSquan   20-JUL-1998
                Page 1
                   3  34:20 3.7e+06
                            3.7e+06

                   4  34:26 6.7e+05
                            6.7e+05

1,2,3,4,7,8-HxCDD  5  34:43 6.66+05
                            6.66+05
1,2,3,6,7,8-HxCDD  6
1,2,3,7,8,9-HxCDD  7
34:46 1.3e+06
      1.3e+06

34:59 1.6e+06
      1.6e+06
                   8  35:06 3.8e+04
                            3.8e+04

                   9  35:12 6.56+03
                            6.5e+03

                   10 35:16 l.le+04
                            l.le+04
1.23 y


1.48 n


1.67 n


1.13 y


1.28 y


0.58 n


0.31 n


2.70 n
                                                   l.Oe+07 3.5e+06 5.1e+02 y  n
                         1.15
                         0.21
                         0.24
                                               0.39
                                               0.45
                                               0.01
 2.06+06
 1.6e+06
L
 4.0e+05
 2.7e+05
4
 4.1e+05
 2.56+05
3
 7.1e+05
 6.2e+05
5
 8.86+05
 6.86+05
L
 1.46+04
 2.46+04
                         0.00
                         0.00
 l.Se+03
 4.96+03
D
 7.96+03
 2.9e+03
6.5e+05 l.Oe+02 y  n
5.26+05 7.66+01 y  n

l.le+05 1.7e+01 y  n
8.4e+04 1.2e+01 y  n

1.5e+05 2.3e+01 y  n
l.le+05 1.6e+01 y  n

2.3e+05 3.6e+01 y  n
1.9e+05 2.7e+01 y  n

2.2e+05 3.5e+01 y  n
1.7e+05 2.5e+01 y  n

5.9e+03 9.2e-01 n  n
6.5e+03 9.66-01 n  n

S.le+02 1.36-01 n  n
1.86+03 2.76-01 n  n
                                                           2.2e+03 3.4e-01 n
                                                           1.66+03 2.46-01 n

-------
OPUSguan   20-JUL-1998
                                      Page 8
                                                                    Page  7  of  8

 Ent: 45 Name: Total Hepta-Furans  F:4  Mass:  407.782  409.779 Mod? no   #Hom:4

 Run: 15 File: a!7jul98b    S:10 Acq:17-JUL-98 23:31:42  Proc:20-JUL-98  09:06:13
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount:  1.67
     Cone:  1.67
   Tox #1:  -
Name
of which 1.30
of which 1.30
     Tox #2:  -

#     RT Respnse
                 named and 0.37
                 named and 0.37
                       Tox #3: -
                                        RA
1,2,3,4,6,7,8-HpCDFl  36:22 3.7e+06  1.02 y
                            3.7e+06

                   2  36:34 5.7e+05  0.97 y
                            5.7e+05

                   3  36:40 5.0e+05  1.08 y
                            5.0e+05

1,2,3,4,7,8,9-HpCDF4  37:32 3.2e+05  1.24 n
                            3.2e+05
                           Cone

                            1.17
                               ]
                               1
                            0.20


                            0.17


                            0.12
                  unnamed
                  unnamed
                                                      Area  Height
                                  S/N  Mod?
               1.9e+06 5.4e+05 1.2e+02  y  n
               l.Se+06 5.5e+05 1.4e+02  y  n
              D
               2.8e+05 8.0e+04 1.8e+01  y  n
               2.9e+05 8.3e+04 2.2e+01  y  n
              7
               2.6e+05 6.8e+04 1.5e+01  y  n
               2.4e+05 6.9e+04 1.8e+01  y  n
              2
               1.8e+05 4.5e+04 l.Oe+01  y  n
               1.4e+05 4.1e+04 l.le+01  y  n
                                                                    Page  8  of  8

 Ent: 46 Name: Total Hepta-Dioxins F:4  Mass:  423.777  425.774  Mod?  no   #Hom:4

 Run: 15 File: a!7ju!98b    S:10 Acq:17-JUL-98 23:31:42  Proc:20-JUL-98  09:06:13
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 1.51
     Cone: 1.51
   Tox #1: -
Name
of which 0.75
of which 0.75
     Tox #2:  -

#     RT Respnse
named and 0.76
named and 0.76
      Tox #3: -
                                        RA
                   1  36:22 7.7e+04  4.63 n
                            7.7e+04

                   2  36:35 2.0e+06  0.99 y
                            2.0e+06

                   3  36:49 2.9e+04  0.81 n
                            2.9e+04

l,2,3,4,6,7,8-HpCDD4  37:11 2.1e+06  1.13 y
                            2.1e+06
          Cone

           0.03
               e
               3
           0.72
               3
               3
           0.01
               ]
               ]
           0.75
                                   unnamed
                                   unnamed
                                                      Area  Height
                                                   S/N  Mod?
                                6.3e+04  1.9e+04  1.2e+01  y  n
                                1.4e+04  5.2e+03  1.8e+00  n  n
                               I
                                l.Oe+06  3.0e+05  2.0e+02  y  n
                                l.Oe+06  3.0e+05  l.Oe+02  y  n

                                 .3e+04  4.3e+03  2.8e+00  n  n
                                 .6e+04  4.0e+03  1.4e+00  n  n

                                l.le+06  3.1e+05  2.1e+02  y  n
                                l.Oe+06  2.7e+05  9.4e+01  y  n
                                                                                                       053

-------
File: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP M23
Sample #10 Text: 1070-1 xl/2 ALS #10
319.8965 S:10 SMO(1,3) BSUB ( 128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% ,
100% A2.45E7
n
50J M A1.24E7
0; ]\ J\A2.I6E6
24loO ' ' 25100
321.8936 S:10 SMO(1,3) BSUB (128, 15, -3
100% A3
50 1
o: 	
24:00 25:00
331.9368 S:10 SMO(1,3) BSUB (128, 15, -3
100%
sol
1 ' ' ' ' | 	 i '
24:00 25:00
333.9339 S:10 SMO(1,3) BSUB (128, 15 , -3
100%
50 j
0:
	 24 100 	 25 loo'
327.8847 S:10 SMO(1,3) BSUB(128, 15, -3
100%
50 j
26:00
.0) PKD(3,3,3,0.10%,
.19E7
11 A1.60E7
/ \ /\ A2.69E6
/ V J V ^x\
26:00
.0) PKD(3,3,3,0.10%,
26:00
.0) PKD(3,3,3,0.10%,
26 loo'
.0) PKD(3,3,3,0.10%,
24:00 25:00 26:00
316.9824 S:10 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00% , F, F)
100% 23:42 24:26 24:51 25:40 26:07 26
:/ — "
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-------
File: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
Sample #10 Text: 1070-1 xl/2 ALS #10
355.8546 S:10 F:2 SMO(1,3) BSUB (128 , 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 2768 . 0 , 1 . 00%, F, F)
100% A9.42E6 A7.86E6
" l\ l\ A4.69E6
50- A
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/ \ A6 10E5 MM A A1.09E6
0- / V Ab^bby \^J ^^^J \^ /^^ ^
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357.8517 S:10 F:2 SMO(1,3) BSUB(128 , 15, -3 . 0) PKD(3,
1004 A6.
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3bli2 30124 30136 sbUs 3ll66 3ill2 31124
367.8949 S:10 F:2 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3,
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369.8919 S:10 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3,
1004
so:
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366.9792 S:10 F:2 SMO(1,3) PKD (3 , 3 , 3 , 100 . 00%, 0 . 0, 1 .
1004 	 30:18 31:18
so:
^ 30:12 30:24 30:36 30:48 31:00 31:12 31:24
31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
3, 3, 0.10%, 1712. 0,1. 00%, F,F)
32E6 A5.09E6
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3, 3, 0.10%, 2868. 0,1. 00%, F,F)
A2 . 20E8
3ll36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
3, 3, 0.10%, 2632. 0,1. 00%, F,F)
A1.41E8
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00%,F,F)
31:36 31:52 32:04 	 32j23 32:33 32^53 33:J.2 7.4E7

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-------
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: A17JUL98B Acq: 17-.JUL-l99fi 23:31:42 Exp : EXP M23 DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
le #10 Text: 1070-1 xl/2 ALS #10
8156 S:10 F:3 SMO(1,3) BSUB ( 128 , 15, -3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 6412 . 0 , 1 . 00% , F, F)
Al . 2 6E7
A
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33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35
8127 S:10 F:3 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 6832 . 0, 1 . 00%, F, F)
A1.00E7
A
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33124 33136 33Us 34!oO 34ll2 34:24 34!36 34Us 35loO 3s!l2 3s!24 35I36 3s!
8559 S.-10 F:3 BSUB(128, 15, -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 11192 . 0 , 1 . 00%, F, F)
A2.24E8 A2.35E8
A A

33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:
8530 S:10 F:3 BSUB(128, 15 , -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 8556 . 0 , 1 . 00%, F, F)
A1.78E8 A1.88E8
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33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:
9760 S:10 F:3 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
33-27 33-40 33:55 31^0334:10 34^21 34^3534^42 35:00 35:16 35:29 35:37
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-------
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-: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP_M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE — Paradiom 	 ~~1
xle #10 Text: 1070-1 xl/2 ALS #10 y
7767 S:10 F:4 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 1508 . 0 , 1 . 00%, F, F)
A1.01E6 A1.12E6 3 . 1E5

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BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10%, 7732 . 0 , 1 . 00%, F,F)
A1.61E8
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36136 36148 37166 37112 37124 37136 37148 SsloO 38 1 12 ' 38 124 ' 38 lie ' 38 J48 ' 39
BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10%, 2368 . 0 , 1 . 00%, F, F)
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: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
le #10 Text: 1070-1 xl/2 ALS #10
7377 S:10 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10% , 1416 . 0 , 1 . 00%, F, F)
A9 . 62E5
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36 39:48 40:00 40:12 40:24 40:36 40:48 41
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36 39:48 40:00 40:12 40:24 40:36 40:48 41:
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A2.40E8
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41
9728 S:10 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
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-------
File: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP M23 DBS OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm
Sample #10 Text: 1070-1 xl/2 ALS #10
303.9016 S:10 SMO(1,3) BSUB (128 , 15, -3 . 0) PKD (3, 3 , 3 , 0 . 10%, 8648 . 0, 1 . 00%, F, F)
100% A8.67E7 1.7E7
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305.8987 S:10 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 7600
100% A1.14E8
50 1 A5.57E7 A A7.66E7 A6.08E7
A A2.73E7 M A « A3.30E7A /\A3
A A A /VW\ /i\ AA /Yv
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315.9419 S:10 SMO(1,3) BSUB (128, 15, -3 . 0)
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-------
  File: A17JUL98BAcq:  17-JUL-1998 23:31:42Exp:  EXP_M23_DB5_OVATION Voltage SIR EI+GC Autospec-UltimaEParadigm
  Sample #10  Text:  1070-1  xl/2   ALS #10                        I
  339.8597 S:10 F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,14124.0,1.00%,F,F)   ,
  100%,                                        A4.65E7            I     I                                              1.4E7
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       30:12  30:24  30:36  30:48  31:00  31:12   31:24   31:36  31.:48  32:00  32:12  32:24  32:36  32:48  33:00  33:12
                                  _7.2E6

                                   O.OEO
  341.8568 S:10 F:2 SMO(1,3)  BSUB (128,15 ,-3 . 0 )  PKD(3 , 3 , 3 , 0 .10% , ^344 . 0 ,'1. 00%, F, F)
  100*.                                        A3.Q4E7            |     r
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351.9000 S:10 F:2 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,2140.0,1.00%,F,F)
10°*.                      /•      (  ,-*  S*\  ^L U  n            A3.04E8
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  353.8970 S:10 F:2 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,2984.0,1.00%,F,F)
  100%.                   ^lJL(\i       ft. //2r-.~'x)               A1.25E8                                           ,-6
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       30:12  30:24  30:36  30:48  31:00   31:12   31:24  31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00  33:12
  409.7974  S:10 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,100.00%,2604.0,1.00%,F,F)
  100%
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       30:12  30:24  30:36-^315148  31:00u31:12   31:24  31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00  33:12
  366.9792 S:10 F:2 SMO(1,3) f>KD (3 ,3 , 3<, 100 . 00% , 0 . 0 ,1. 00%, F, F)
  100%,    30:18              I   „  1& vo*      31:18     31:36     31:52   32; 04	32:23  32:33	22^3	3J_O2_7
1     30:12  30:24  30:36  30:
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-------
File: A17JUL98B Acq: 17-JUL-199S 2J:J1:42 Exp
Sample #10 Text: 1070-1 xl/2 ALS #10
: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm

373.8207 S:10 F:3 SMO(1,3) BSUB (128 , 15, -3 . 0) PKD(3 , 5, 2 , 0 . 10% , 9596 . 0, 1 . 00%, F, F)
100% A7.28E6 1 r

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34:24 34!36 34Us 3s!oO 3s!l2 3sl24 3s!36 35:48 Time
375.8178 S:10 F:3 SMO(1,3) BSUB (128, 15, '-3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 8608 . 0 , 1 . 00%, F, F)
100% A5.87E6

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383.8639 S:10 F:3 BSUB(128, 15, -3 . 0) PKD(3,5,2,0
100%
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385.8610 S:10 F:3 BSUB(128, 15, -3 . 0) PKQ(3,5-,2,0
100%. 1 A2,-77E
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100% . 34^13
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-------
I
File: A17JUL98B
Sample #10
407.7818
100%
50 1
'_
o-


S


Text
:10 F:


Acq: 17-JUL-1998 23:31:42
Exp: EXP_M23_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm
: 1070-1 xI/2 ALS #10
4 SMO(1,3)
Al . 87E6
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PKD (3,3,3


/ \ A2.79E5

36
409.7788
100%
sol
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1
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00 36
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J X 	
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4 SMO(1,3)
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BSUB(128,15,-3.0)



66 37112
PKD (3,3,3


/ V A2.88E5
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36
417.8253
100%
50 j
.
o"




36
419.8220
100%
sol
:
0'




" ' 1 1 1 1
36
479.7165
100%
50 1




1
S




5
S




T
S



00 36
:10 F:




00 36
:10 F:




00 36
:10 F:


J X 	
Il2 36124
4 SMO(1,3)
A7.68E7
A
/ \
/ v
1 i i f i i | n-
:12 36:24
4 SMO(1,3)
Al -74E8
A
/ \
/ V_
•12 36:24
4 SMO(1,3)


35:57
36
430.9728
100%

50 j
0"
/


M 36
1
S




1
00 36
:10 F:
36:



00 36
:12 36:24
4 SMO(1,3)
11 36:22



| I . i i i | i r
:12 36:24
_/ ^+^mtS X^.
36\36 36 Us 37l
BSUB(128,15,-3.0)




36:36 36:48 37:
BSUB(128,15,-3.0)




36:36 36:48 37:
BSUB(128,15,-3.0)

37:
f
36:38 y
36:36 36:48 37:
PKD(3,3,3,100.00%
36_Li5_ 37:



i i i I 	 I ' ' ' ' ' I
36:36 36:48 37:

66 37:12
PKD(3,3,3




66 ' 37:12 '
PKD (3,3,3




66 37112'
PKD (3,3,3
37:10
00 / \
•v . 	 / \
x^ w
66 37! 12
,0.0,1.00%
00 37:1



66 ' 37! 12
,0.10%,


Al.

37! 24
,0.10%,


Al.

37124
,0.10%,


Al.
y
37124
,0.10%,


A4.
y
37124
4480. 0,1. 00%, F,F)


77E5
- — -^__
r5'
12.

" 0 .
37136 37148 38166 38112 38124 Sslie SsUs 39loO
3860. 0,1. 00%, F,F)


43E5

^5-
_2.

0 .
37: 36 37:48 3sl6o 3sll2 38l24 38\36 38:48 39loO
6348. 0,1. 00%, F,F)


97E7
"V^
2.
Li.

' 0 .
37 3' 6 37148 38166 38112 38124 38:36 38:48 39loO
9656. 0,1. 00%, F,F)


55E7
'V
5.
_2.

0.
37:36 37148 38166 38:12 38124 3s!36 SsUs 39loO
, 100. 00%, 5320. 0,1. 00%, F,F)


^N3Jjj2j5
37l24
,F,F)
6



37124



r
Ll.
•o
37136 37:48 38166 38:12 38124 bslie SsUs 39:00

37i_42 38:02 38:16 38:31 38:50 rl .




_5.
0.
37136 37148 38166 38112 38124 38l36 38: 48 39loO

5E5
7E5

OEO
Time

5E5
8E5

OEO
Time

3E7
1E7

OEO
Time

1E7
5E7

OEO
Time

3E5
1E5
OEO
Time

1E8

5E7
OEO
Time
   •N
 O

-------
File: A17JUL98B Acq: 17-JUL-1998 23:31:42 Exp: EXP M23 DBS OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm
Sample #10 Text: 1070-1 xl/2 ALS #10
441.7427 S:10 F:5 SMO(1,3) BSUB( 128, 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 1324 . 0, 1 . 00%, F, F)
lOOi A1.97E5 4.4E4
50 j
o:
443.
1002
50 j
o:
469.
100%
sol
o:
471.
100%
50 j
o;
513.
100%.
50J
o:
454.
100%
50 j
o-

39ll2
7398 S:10 F:

39ll2
7780 S:10 F:

39!l2
7750 S:10 F:

39ll2
6775 S:10 F:
39:
39:12
9728 S:10 F:
/
39!l2

39124
5 SMO(1,3)

39124
5 SMO(1,3)

39124
5 SMO(1,3)

39124
5 SMO(1,3)
15
^/ 	 v . r^
39124
5 SMO(1,3)
39:19

39124

39136
BSUB(128, 15

39!36
BSUB(128,15

39136
BSUB(128,15

39^36
BSUB(128,15
dy^Siai

39U8
,-3.0) PKD(3,3,3

39l48
,-3.0) PKD (3, 3, 3

s'gUs
,-3.0) PKD (3, 3, 3

39148
,-3.0) PKD (3, 3, 3
39:52
39136 39148
PKD (3 ,3, 3, 100. 00%, 0.0, 1.00%
39:42 39

39136

39 Us
/v..
4o!ob 4o!i2
, 0.10%, 2256. 0,1. 00%, F,
A2.06E5
6 44E3
4o!24 ' ' ' 4ol36 ' ' ' 4'oUs 41.
F)
/ \ A1.07E5
y v\
4oToO 4o!l2
,0. 10%, 2396. 0,1. 00%, F,
A2 J-4E8
J\_
4o!ob 4o!i2
,0. 10%, 1564. 0,1. 00%, F,
A2 . 40E8
y\_
4o!ob 4o!i2
,100. 00%, 1040. 0,1. 00%,
40:02
/ \ 40:1140:17
J WY/V
4o!ob 4o!i2
,F,F)

4o!ob 4o!i2
4ol24 •' ' ' 4ol36 ' ' ' 4o!48 41 !
F)

_2.2E4
_O.OEO
00 Time
5.8E4
L2.9E4
LO.OEO
00 Time
4.9E7
12.4E7
lO.OEO
40:24 40:36 40:48 41 00 Time
F)
5.4E7

L2.7E7
:O.OEO
40!24 4ol36 4o!48 41 00 Time
F,F)
8.1E3
40:25
L4.1E3
:O.OEO
40:24 40:36 40:48 41:00 Time
40:36 1.2E8

_5.8E7
.O.OEO
4ol24 4o!36 4ol48 4l!oO Time
 >
o

-------
       OPUSguan   22-JUL-1998
                                             Page 1
                Filename
                  Sample
                Acquired
               Processed
               Sample ID
               Cal Table
           Results Table
                Comments
        Typ
        Unk
        ES/RT
        Total
        DPE
        LMC
                                                                                                                                                      Page  9
        a21jul98f
        4
        21-JUL-98  21:57:
        22-JUL-98  08:31:
        1070-1 xl/2
        07feb-m23conf
        M8290-23-072198F
56
58
              Name;     Resp;
      2,3,7,8-TCDF; 5.65e+07;
  13C-2,3,7,8-TCDF; 1.40e+09;
      Tetra Furans; 2.82e+09;
            HxCDPE;        *;
QC CHK ION (Tetra);        * ;
        Ion 1;
     2.476+07;
     6.14e+08;
     l.OOe+08;
   Ion 2;
3.18e+07;
7.84e+08;
1.31e+08;
  RA; ?;
0.78;y;
0.78;y;
0.76;y;
 RT;
:56;
:53;
   Conc;       DL
  4.254;   0.0271
342.587;
212.616;   0.0271
                               ;NotFnd;
                               ;NotFnd;
S/N1;?;
 486;y;
3149;y;
3216;y;
   *;n
DivO;n
S/N2;?
 543 ;y
2895,-y
3579;y
mod?
  no
  no
  no
  no
  no
                                                                        -;-;  27:56
                                                                        -;-;  27:56
 >
o

-------
OPUSquan   22-JUL-1998
                                      Page 1
 Ent: 3  Name:  Tetra Furans
                                                                   Page  1 of 1

                                   F:l  Mass:  303.902  305.899 Mod? no   #Hom:30
 Run: 9  File:  a21jul98f    S:4  Acq:21-JUL-98  21:57:56  Proc:22-JUL-98  08:31:58
 Tables: Run: a21ju!98b  Analyte:  m23_conf   Cal:  07feb-m23»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-1 xl/2
   Amount: 212.62  of which 4.25
     Cone: 212.62  of which 4.25
                        Tox #2:  -
   Tox #1: -

Name
named and 208.36  unnamed
named and 208.36  unnamed
      Tox #3:  -
                         RT Respnse
                                        RA
                   1  18:12 2.36+08  0.76 y
                            2.3e+08

                   2  19:52 1.96+08  0.77 y
                            1.96+08

                   3  20:06 1.5e+08  0.77 y
                            1.5e+08

                   4  20:21 2.5e+08  0.76 y
                            2.56+08

                   5  20:40 l.Oe+08  0.76 y
                            l.Oe+08

                   6  21:13 1.5e+08  0.75 y
                            1.5e+08

                   7  21:32 1.76+08  0.73 y
                            1.7e+08

                   8  21:50 1.6e+07  0.48 n
                            1.6e+07

                   9  21:59 3.0e+07  0.55 n
                            3.06+07

                   10 22:10 1.5e+08  0.71 y
                            1.5e+08

                   11 22:35 7.56+07  0.73 y
                            7.5e+07

                   12 22:55 2.4e+05  1.26 n
                            2.46+05

                   13 23:17 2.76+08  0.76 y
                            2.7e+08

                   14 23:27 l.Se+08  0.77 y
                            1.5e+08

                   15 24:19 1.2e+08  0.76 y
                            1.26+08

                   16 24:32 9.2e+06  0.74 y
                            9.2e+06

                   17 25:01 1.4e+08  0.76 y
                            1.4e+08

                   18 25:27 7.4e+07  0.77 y
                            7.4e+07

                   19 25:59 7.4e+06  0.73 y
                            7.46+06
                                              Cone

                                              17.41
                                                  1
                                                  1
                                              14.65
                                                  £
                                                  ]
                                              11.58
                                                  e
                                                  £
                                              18.61
                                                  1
                                                  1
                                               7.85
                                                  4
                                                  C
                                              10.96
                                                  6
                                                  £
                                              12.83

                                                  c
                                               1.22
                                                  C
                                                  3
                                               2.29
                                                  1

                                              11.34
                                                  €
                                                  8
                                               5.66

                                                  4
                                               0.02
                                                   ]
                                                   ]
                                              20.06
                                                   1
                                                   ]
                                              11.58
                                                   6
                                                   £
                                               9.24
                                                   C

                                               0.69
                                                   3
                                                   C
                                              10.60
                                                   C
                                                   £
                                               5.59
                                                   i
                                                   4
                                               0.56
                  Area  Height
S/N  Mod?
               l.Oe+08 1.9e+07  3.2e+03  y  n
               1.3e+08 2.5e+07  3.6e+03  y  n

               8.5e+07 l.Se+07  2.5e+03  y  n
               l.le+08 2.06+07  2.8e+03  y  n

                .7e+07 l.le+07  1.7e+03  y  n
               8.7e+07 1.4e+07  2.0e+03  y  n
              1
               l.le+08 1.8e+07  3.Oe+03  y  n
               1.4e+08 2.3e+07  3.3e+03  y  n
              5
               4.5e+07 7.6e+06  1.3e+03  y  n
               5.9e+07 l.Oe+07  1.4e+03  y  n

                .2e+07 l.le+07  1.8e+03  y  n
               8.3e+07 1.4e+07  2.Oe+03  y  n
              3
               7.2e+07 9.8e+06  1.6e+03  y  n
               9.9e+07 1.3e+07  1.9e+03  y  n
              2
               5.36+06 1.66+06  2.6e+02  y  n
               l.le+07 2.7e+06  3.8e+02  y  n
              3
               l.le+07 2.8e+06  4.7e+02  y  n
               2.0e+07 4.5e+06  6.3e+02  y  n
               6.3e+07 l.le+07 1.9e+03 y  n
               8.8e+07 1.6e+07 2.2e+03 y  n
              5
               3.2e+07 5.7e+06 9.4e+02 y  n
               4.3e+07 7.6e+06 l.le+03 y  n
                .4e+05 6.1e+04 l.Oe+01 y  n
                .le+05 5.96+04 8.3e+00 y  n

               1.2e+08 1.5e+07 2.4e+03 y  n
               1.5e+08 1.9e+07 2.7e+03 y  n

               6.7e+07 9.5e+06 1.6e+03 y  n
               8.7e+07 1.3e+07 1.8e+03 y  n
               1
               5.3e+07 6.9e+06 l.le+03 y  n
               7.0e+07 9.1e+06 1.3e+03 y  n
               9
               3.9e+06 5.6e+05 9.2e+01 y  n
               5.3e+06 7.4e+05 l.Oe+02 y  n
               D
               6.1e+07 7.7e+06 1.3e+03 y  n
               8.0e+07 l.Oe+07 1.4e+03 y  n
               3
               3.2e+07 3.9e+06 6.4e+02 y  n
               4.2e+07 5.1e+06 7.3e+02 y  n
                                                   3.1e+06 4.3e+05 7.0e+01 y  n
                                                   4.3e+06 5.6e+05 7.9e+01 y  n
                                                                                                       065

-------
OPUSquan 22-JUL-1998 Page 2
20 26:32 l.le+08 0.76 y
l.le+08
21 27:35 l.le+08 0.77 y
l.le+08
2, 3, 7, 8-TCDF 22 27:56 5.7e+07 0.78 y
5.76+07
23 28:12 2.3e+06 0.90 n
2.3e+06
24 28:33 9.66+07 0.77 y
9.66+07
25 29:02 4.3e+05 0.29 n
4.36+05
26 29:18 5 . 5e+07 0.78 y
5.56+07
27 29:38 6.8e+07 0.77 y
6.8e+07
28 31:52 3.2e+07 0.78 y
3.2e+07
29 33:45 2.2e+06 0.20 n
2.2e+06
30 33:48 2.6e+06 0.45 n
2.6e+06
8.24
4.76+07
6.2e+07
7.92
4.6e+07
5.9e+07
4.25
2.56+07
3.26+07
0.17
1. le+06
1.2e+06
7.21
4.2e+07
5.46+07
0.03
9.7e+04
3.3e+05
4.16
2.46+07
3.16+07
5.14
3.06+07
3.9e+07
2.38
1.4e+07
l.Se+07
0.16
3.7e+05
1.8e+06
0.20
S.le+05
1.8e+06
5.
7.
5.
6.
2.
3.
1.
2.
4.
6.
3.
7.
2.
3.
3
4
1
1
1
2
1
2
7e+06
4e+06
2e+06
7e+06
9e+06
8e+06
8e+05
2e+05
7e+06
le+06
le+04
6e+04
6e+06
4e+06
le+06
le+06
3e+06
7e+06
2e+05
Oe+05
5e+05
Oe+05
9.
1.
8.
9.
4.
5.
2.
3.
7.
8.
5.
1.
4.
4
5
5
2
2
2
2
2
2
3e+02
le+03
7e+02
6e+02
9e+02
4e+02
9e+01
le+01
8e+02
7e+02
Oe+00
le+01
4e+02
8e+02
2e+02
8e+02
2e+02
4e+02
Oe+01
9e+01
4e+01
9e+01
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
r r
066

-------
File: A2UUL98F Acq: 21-JUL-199B 21:b7:56 Exp:
M23_DB225 Voltage SIR
~^TT
GC Autospec-UltimaE
Paradigm

Sample #4 Text: 1070-1 xl/2 ALS #4
303.9016 S:4
100%
-
50 j

SMO (1,3)
Al.
BSUB(128,15,-3.0) PKD(3,3,3
,0.10%,
6048. 0,1. 00%, F
,F)

OOE8 A1.07E8

1
1 . II A1.15E8


i i | i
16:00
305.8987 S:4
100%
-
50 j
o:



ieSob
315.9419 S:4
100%
50 j
o:


'I 1 ' T" T I'
is!

A
1 Ml
iA6.23E7 . f
K . n t
A LL
00 20:00 22:00
SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3
Al.



~I 	 1 ' 1 I 	 T1
18:
SMO (1,3)
A
ft A
24:00
,0.10%,

5.08E7 A4-74E7
AA T A
26:00
7044. 0,1. 00%, F



A4.17E7
AA A AA A1.JL8E7
'28S
,F)
00 30:00 32:

11E8 A1.40E8
.

ft
Ml

_9
0
00 34:00

_2
A1.51E8
A8.33E7 , /
A A A
AJA /
00 20:00 22:00
BSUB(128,15,-3.0) PKD(3,3,3
kA8 - OOE7 . , 	
,,A.
24:00
,0.10%,
AAb.^lli/
A A
26:00
21256.0,1.00%,
A5.41E7
.A/) A A A A1'X8E7
' 28!
F,F)
00 30:00 32:


_1
0
00 34:00

A6.14E8
A


— ' — ' — 1 — 1~
16:00
317.9389 S:4
100%
50 J
o:


-i — i — i — i — r
18:
SMO (1,3)




-"T "T 1 1 '"T" 'I 1 1 	 ! 	 1 	 1 	 [ 	 ' 	 ' 	 ' 	 \
00 20:00 22:00
BSUB(128,15,-3.0) PKD(3,3,3


24SOO
,0.10%,


' 26!ob
29544.0,1.00%,
l\

2s!
F,F)


ob s'oSob 32!



6
13
• o
00 34!ob

A7 . 84E8
A


— ' — ' — 1 — "~
ie!oo
375.8364 S:4
1002
50-
0-


\16:03

316.9824 S:4
100%15:30
50 J
o:


ieSob


T — i — i — i — r
SMO (1,3)






— i — i — i — i — i — i — i — i — i — i — i — i — i i i i
00 20:00 22:00
BSUB(128,15,-3.0) PKD(3,3,3
20
/
/
17:2518:25 l?jJ52
1 ' ' is!
SMO (1,3)
i23
V
\^]^20___23j
— I 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 r— t
00 20:00 22:00
PKD (3, 3, 3, 100. 00%, 0.0, 1.00%
17:03 18; 17 19_i_47




21:16 22:43


-I 	 1 	 1 	 1 	 1 	 1— 1 	 1 	 1 	 1 	 1 	 1 	 1 	 r — 1 	 1 	 1 	 1 	 1 	 1 	 r
18:00 20:00 22:00


24SOO


2'eSob


281
,100. 00%, 161372. 0,1. 00%, F


19 ^j
24!ob
,F,F)


^_26J27_
26:00

24jJL5_ 25:30 27 1


24!ob


i 	 1 	 r — i 	 1 	 1 i i
26:00


-_— •-v.
'28S

12


28!


00 30 Sob 32S
F)




8
U
:o
ob 34!ob



6 28:49 	 3 0^5 1^32^04 34:17
ob 30 Sob 32!

_5
12
- o
00 34!ob

29:05 30:2731:2532:2433:26 _7


ob 3o!ob 32!


_3
'o
ob 34!ob

.9E7

.7E6
.OEO
Time

.5E7

.3E7
.OEO
Time

.7E7
.4E7
.OEO
Time

.6E7
.3E7
.OEO
Time

.1E5
.5E5
.OEO
Time

.7E7
.9E7
.OEO
Time

-------
             Method 23
             M23=O-1
                                          Paradigm Analytical Labs
Analytical Data Summary Sheet
^^Anali^ .•;,;> -.
2,3,7,8-TCDD
1237 8-PeODO
9999" !S\JsM*A , ^. _ .
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
TotafPeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ(ND=0)
TEQ (ND=l/2)
Concentration
0.0124
' ' IVflftJtl?^"'^*
•f „,-£? ~'f'^$$j&, ; rl^' *'"' :7$
0.0027
0.0049
0.0043
0:0073
0.0243
0.160
0.0874
0.0864
0.0474
0.0171
0.0114
0-0037
0.0170

0.0103
4.10
0.264
0.116
0.0132
9.12
1.59
0.166
0.0228
0.0897
0.0897

0.0007


0.0006

0.0005
0.0004
0.0013
0.0010
0.0022
0.0021
0.0006
0.0005
0.0005
r 0.0006
0.0005
0$PM
0.0007
?.. 0^0007^*
0.0005
0.0005
0.0004
0.0010
0.0021
0.0005
0.0005




^-^\;^. >-° '-ff>
^^"^J^' ' ' '*^

- i--;|,,l;.










f


i'-'i'n-,^.
"

0.0144
9.15

0.170

0.0897
0.0897

28:27
'••/*" v^t$'$3i*7 "
\C0^^lp^^K ^
34:42
34:46
34:58
37:10
40:02
27:29
31:57
32:24
34-10
J~ • 1 V
34-15
—IT. L^f
34-37
«J^.»/ /
36-22
J \Jt4t4f
37:32
40:10
> .










0.74
; - ^ ;£^f
, -, ,;<« 'ir»3sl
1 "31
1 ,J 1
• i M-
Jl*Ar«'
1.20
1.12
0.84
0S?7
1.58
1.51
1 24
A >^*T
1 I1?
1 . 1 .J
1 00
1 •V/v
0.9,1
0.78










Qualifier


-l^*>"i ^























ITEF
ITEF
Client Information

Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:  -?-

Collection Date:
Receipt Date:
Extraction Date:
Analysis Date:
Texas Lime Kiln
                      Samle Information
                                              Air
25-lun-98
oMii^g
10-Jul-98
18-Jul-98
                                          al7ju!98b-ll
                        initial Ca!:
             1/2
                                                             068

-------
                                                                    Paradigm Analytical Labs
                             Analytical Data Summary Sheet
Labeled
-Standard
Extraction Standards
13C12-2,3,7,8-TCDD
13Cu-U,3,7,8-PeCDD
13C12-l,2,3,6,7,8-HxCDD
"CirlA3,4,6,7,8-I^>CI>D
13C12-OCDD
13C12-2,3,7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF


Sampling Standards
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
t3CI2- 1 ,2,3,4,7,8-HxCDD
13Cirl,2,3,4,7)8-HxCDF
13C,rl,2,3,4,7&9-HpCDF
Injection Standards
13C12-1,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
Am«BK*||
<**» '

4
4 - "';•;
4
4
8
4
4
4
4


;' 4? * ;g
4
•-'-41-!.— -
4
4



Measured

3.89
"'f452'
3.75
4.09
7.40
3.94
4.05
3.77
3.32
-..v n.


3.94
.„;•, ^-^jp-w-.
3.85
3.68





97.4
113.1
93.8
102.1
92.4
98.6
101.2
94.2
82.9


$jj$3'-:
98.5
'""TOOf"
96.3
92,0



(fflta^ "1

28:27
32:37
34:45
37:09
40:01
27:25
31:56
34:14
36:21


28:27
32:24
34:41
34:10
37:31

28:09
34:58
Ratio

0.77
1.55
1.27
1.03
0.88
0.78
1.57
0.52
0.45



1.58
. 1.26
0.52
0.45

0.79
1.26
Qualifier




















Client Information
Project Name:
Sample ID:

Laboratory Information

Project n>:
Sample ID:

Collection Date:
Receipt Date:
Extraction Date:
Analysis Date:

Reviewed by:  y.T-
Texas Lime Kiln
M23-O-1
Sample Information
Ma:
.W«j^^r<^ijpae:;
           ,  ,.,
    ->^-'X^-- /' >'.*$• • ? C '•::
-------
O

-------
OPUSquan   20-JUL-1998
                   Page  1
                                                                    Page  1  of  8

 Ent: 39 Name: Total Tetra-Furans  F:l  Mass:  303.902  305.899 Mod? no   #Hom:21

 Run: 16 File: a!7ju!98b    S:ll Acq:18-JUL-98 00:16:48 Proc:20-JUL-98  09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-2 xl/2
   Amount: 228.67  of which 25.77
     Cone: 228.67  of which 25.77
                        Tox #2: -
   Tox #1: -

Name
 2,3,7,8-TCDF
                 named and 202.89   unnamed
                 named and 202.89   unnamed
                       Tox #3:  -
                         RT Respnse
                                        RA
1  23:39 8.46+07  0.77 y
         8.4e+07

2  24:14 4.06+07  0.77 y
         4.0e+07

3  24:34 3.7e+07  0.76 y
         3.7e+07

4  24:51 1.8e+08  0.77 y
         1.8e+08

5  24:59 4.5e+07  0.79 y
         4.56+07

6  25:10 3.9e+07  0.72 y
         3.96+07

7  25:16 1.26+08  0.77 y
         1.2et-08

8  25:40 4.1e+07  0.75 y
         4.1e+07

9  25:44 5.6e+07  0.78 y
         5.66+07

10 26:01 3.26+07  0.79 y
         3.26+07

11 26:09 5.0e+07  0.75 y
         S.Oe+07

12 26:26 8.56+07  0.76 y
         8.5e+07

 13 26:34  8.1e+07  0.77 y
          8.1e+07

 14 26:51  4.26+07  0.76 y
          4.26+07

 15 27:03  2.76+06  0.77  y
          2.7e+06

 16  27:11  2.0e+07  0.77  y
          2.0e+07

 17  27:29  1.3e+08  0.77  y
          1.3e+08

 18  28:03  2.3e+07   0.79 y
          2.3e+07

 19  28:20 1.2e+07   0.79 y
          1.2e+07
                           Cone

                           17.18
   Area  Height    S/N  Mod?
                                               7.63
                                              36.11
 3.7e+07  8.0e+06  l.Se+03 y  n
 4.8e+07  l.le+07  3.1e+03 y  n
J
 1.7e+07  3.9e+06  7.3e+02 y  n
 2.3e+07  S.le+06  1.5e+03 y  n
5
 1.6e+07  3.56+06  6.6e+02 y  n
 2.1e+07  4.6e+06  1.3e+03 y  n
I
 7.7e+07  l.Se+07  2.8e+03 y  n
 l.Oe+08  1.9e+07  5.6e+03 y  n
                                               9.14
                                               7.91
                                              24.45
 2.06+07 2.9e+06  5.4e+02  y  n
 2.5e+07 3.7e+06  l.le+03  y  n
L
 1.6e+07 3.9e+06  7.36+-02  y  n
 2.3e+07 5.2e+06  1.5e+03  y  n

 5.2e+07 6.8e+06  1.3e+03  y  n
 6.8e+07 9.0e+06  2.6e+03  y  n
                                               8.29
                                                   1.7e+07 4.2e+06 7.96+02 y  n
                                                   2.3e+07 5.5e+06 1.6e+03 y  n
                                               11.49
                                                6.54
                                               10.28
 2.5e+07 5.2e+06 9.8e+02 y  n
 3.2e+07 6.8e+06 2.0e+03 y  n
1
 1.4e+07 3.0e+06 5.6e+02 y  n
 1.8e+07 3.9e+06 l.le+03 y  n
3
 2.2e+07 4.6e+06 8.6e+02 y  n
 2.9e+07 5.9e+06 1.7e+03 y  n
                                               17.40
                                                    3.7e+07  7.5e+06  1.4e+03  y  n
                                                    4.8e+07  9.6e+06  2.8e+03  y  n
                                               16.53
                                                8.65
                                                0.56
  3.5e+07 7.0e+06 1.36+03 y  n
  4.6e+07 9.1e+06 2.7e+03 y  n

  1.8e+07 3.6e+06 6.8e+02 y  n
  2.4e+07 4.8e+06 1.4e+03 y  n

  1.2e+06 2.7e+05 5.1e+01 y  n
  1.5e+06 3.4e+05 l.Oe+02 y  n
                                                4.17
                                               25.77
                                                4.77
                                                2.52
  8.9e+06  1.8e+06  3.4e+02  y  n
  1.2e+07  2.4e+06  6.9e+02  y  n
 7
  5.5e+07  8.5e+06  1.6e+03  y  n
  7.16+07  l.le+07  3.2e+03  y  n
 7
  l.Oe+07  2.1e+06  4.0e+02  y  n
  1.3e+07  2.7e+06  7.7e+02  y  n
 2
  5.4e+06  l.le+06  2.0e+02  y  n
  6.9e+06  1.4e+06  4.0e+02  y  n
                                                                                                       071

-------
OPUSquan   20-JUL-1998               Page 2
                  20 28:33 2.le+06  0.81 y   0.42
                          2.1e+06               9.3e+05  2.2e+05 4.2e+01 y n
                                                1.le+06  2.6e+05 7.5e+01 y n
                  21 29:47 3.3e+06  1.25 n   0.67
                          3.3e+06               1.8e+06  3.3e+05 6.1e+01 y n
                                                1.5e+06  2.8e+05 8.1e+01 y n
                                                                                             £'' 072

-------
OPUSquan   20-OUL-1998
                                      Page 3
                                                                   Page 2 of 8

 Ent: 40 Name: Total Tetra-Dioxins F:l  Mass:  319.897  321.894 Mod? no   #Hom:15

 Run: 16 File: a!7ju!98b    S:ll Acq:18-JUL-98 00:16:48  Proc:20-JUL-98  09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-2 xl/2
   Amount: 27.85
     Cone: 27.85
   Tox #1: -
Name
2,3,7,8-TCDD
of which 0.36
of which 0.36
     Tox #2: -

#     RT Respnse
named and 27.49
named and 27.49
      Tox #3:  -
                                        RA
1  25:15 4.7e+07  0.78 y
         4.7e+07

2  25:41 2.2e+07  0.77 y
         2.26+07

3  26:03 3.8e+06  0.78 y
         3.8e+06

4  26:54 1.4e+07  0.78 y
         1.4e+07

5  27:07 2.7e+06  0.77 y
         2.76+06

6  27:17 3.46+06  0.79 y
         3.4e+06

7  27:23 7.3e+05  0.98 n
         7.3e+05

8  27:45 2.7e+06  0.77 y
         2.7e+06

9  28:10 4.26+06  0.78 y
         4.2e+06

10 28:19 5.8e+06  0.78 y
         5.86+06

11 28:27 l.Se+06  0.56 n
         1.5e+06

12 28:40 l.le+06  0.77 y
         l.le+06

13 28:57 1.3e+06  0.80 y
         1.36+06

14 29:18 4.6e+05  0.80 y
         4.66+05

15 29:54 2.4e+05  0.94 n
         2.46+05
          Cone

          11.90


           5.59
              c
              ]
           0.95
              ]

           3.41
              «

           0.67
              ]
              ]
           0.84
              ]
              ]
           0.18

              T
           0.67
              ]
              :
           1.05
              ]

           1.45


           0.36
              c
              C
           0.28
              4
              6
           0.31
              C
              1
           0.12


           0.06
    unnamed
    unnamed
                                                     Area  Height
                                                  S/N  Mod?
 2.1e+07  4.5e+06  1.6e+03  y  n
 2.7e+07  5.8e+06  3.0e+03  y  n
3
 9.7e+06  2.1e+06  7.5e+02  y  n
 1.3e+07  2.6e+06  1.4e+03  y  n

 1.7e+06  3.46+05  1.2e+02  y  n
 2.1e+06  4.6e+05  2.4e+02  y  n

  .0e+06  l.le+06  4.0e+02  y  n
 7.6e+06  1.4e+06  7.5e+02  y  n

  .2e+06  1.7e+05  6.1e+01  y  n
  .5e+06  2.3e+05  1.2e+02  y  n

  .5e+06  3.0e+05  l.le+02  y  n
  .9e+06  3.86+05  2.0e+02  y  n

 3.6e+05  7.6e+04  2.8e+01  y  n
 3.7e+05  8.2e+04  4.3e+01  y  n

  .2e+06  2.46+05  8.76+01  y  n
  .5e+06  3.26+05  1.7e+02  y  n

 1.8e+06  3.86+05  1.46+02  y  n
 2.4e+06  4.8e+05  2.5e+02  y  n

 2.5e+06  4.8e+05  1.7e+02  y  n
 3.2e+06  6.1e+05  3.2e+02  y  n

 5.2e+05  l.le+05  4.0e+01  y  n
 9.3e+05  1.9e+05  l.Oe+02  y  n
                                                   4.8e+05  l.Oe+05  3.6e+01 y  n
                                                   6.2e+05  1.2e+05  6.5e+01 y  n
                                                  L
                                                   5.66+05  1.26+05  4.2e+01 y  n
                                                   7.0e+05  1.4e+05  7.5e+01 y  n
                                                  2
                                                   2.06+05  4.26+04  1.5e+01 y  n
                                                   2.5e+05  6.0e+04  3.1e+01 y  n

                                                   l.le+05  2.4e+04  8.6e+00 y  n
                                                   1.2e+05  2.96+04  1.5e+01 y  n
                                                                                                  C <    072

-------
OPUSquan   20-JUL-1998
                   Page  4
                                                                    Page 3  of  8

 Ent: 41 Name: Total Penta-Furans  F:2  Mass:  339.860 341.857 Mod?  no   #Hom:15

 Run: 16 File: al7ju!98b    S:ll Acq:18-JUL-98 00:16:48 Proc:20-JUL-98 09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-2 xl/2
   Amount: 39.73
     Cone: 39.73
   Tox #1: -
Name
 1,2,3,7,8-PeCDF
 2,3,4,7,8-PeCDF
of which 4.35
of which 4.35
     Tox #2:  -

#     RT Respnse
named and 35.39
named and 35.39
      Tox #3:  -
                                        RA
1  30:16 2.1e+07  1.52 y
         2.1e+07

2  31:15 1.2e+07  1.60 y
         1.26+07

3  31:21 4.4e+07  1.51 y
         4.4e+07

4  31:29 7.9e+06  1.56 y
         7.9e+06

5  31:36 2.2e+06  1.51 y
         2.2e+06

6  31:45 2.4e+07  1.51 y
         2.46+07

7  31:54 9.9e+06  1.44 y
         9.9e+06

8  31:57 8.7e+06  1.58 y
         8.7e+06

9  32:04 4.4e+06  1.46 y
         4.46+06

10 32:08 9.36+06  1.43 y
         9.36+06
 11 32:24 9.06+06
         9.0e+06
  1.51 y
                    12 32:29  6.7e+06   1.53 y
                             6.7e+06

                    13 32:35  4.6e+05   1.47 y
                             4.66+05

                    14 32:39  1.2e+06   1.55 y
                             1.26+06
                    15 32:57 6.16+05
                             6.16+05
                  1.74 y
                                              Cone

                                               5.17
        unnamed
        unnamed
                  Area  Height
                                                                      S/N  Mod?
     1.36+07 2.6e+06 1.7e+02 y  n
     8.4e+06 1.7e+06 1.6e+02 y  n
 3.04
     7.6e+06 2.5e+06 1.7e+02 y  n
     4.8e+06 1.7e+06 1.6e+02 y  n
10.90
     2.7e+07 7.26+06 4.7e+02 y  n
     1.8e+07 4.8e+06 4.6e+02 y  n
 1.94
     4.8e+06 1.4e+06 9.1e+01 y  n
     3.1e+06 8.96+05 8.5e+01 y  n
 0.55
     1.3e+06 2.8e+05 1.8e+01 y  n
     8.9e+05 1.96+05 1.8e+01 y  n
 5.82
     1.4e+07 4.8e+06 3.2e+02 y  n
     9.5e+06 3.1e+06 3.0e+02 y  n
 2.43
     5.8e+06 2.3e+06 1.5e+02 y  n
     4.1e+06 1.5e+06 1.5e+02 y  n
 2.19
     5.4e+06 1.9e+06 1.3e+02 y  n
     3.4e+06 1.2e+06 1.2e+02 y  n
 1.08
     2.6e+06 9.3e+05 6.1e+01 y  n
     1.8e+06 6.0e+05 5.7e+01 y  n
 2.27
     5.5e+06 2.1e+06 1.4e+02 y  n
     3.8e+06 1.4e+06 1.4e+02 y  n
 2.16
     5.4e+06 1.9e+06 1.3e+02 y  n
     3.6e+06 1.36+06 1.2e+02 y  n
 1.64
     4.0e+06 1.46+06 9.2e+01 y  n
     2.6e+06 9.4e+05 9.0e+01 y  n
 0.11
     2.8e+05 l.Oe+05 6.8e+00 y  n
     1.9e+05 7.3e+04 7.0e+00 y  n
 0.29
     '7.2e+05 2.6e+05 1.7e+01 y  n
     4.6e+05 1.7e+05 1.6e+01 y  n
 0.15
     3.9e+05 1.4e+05 9.2e+00 y  n
     2.2e+05 8.8e+04 8.4e+00 y  n
                                                                     Page 4  of  8

  Ent:  42 Name:  Total Penta-Dioxins F:2  Mass:  355.855  357.852  Mod?  no   #Hom:12

  Run:  16 File:  al7ju!98b    S:ll Acq:18-JUL-98 00:16:48  Proc:20-JUL-98 09:06:58
  Tables: Run:  a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
  Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-2 xl/2
    Amount:  6.59
      Cone:  6.59
 of  which 0.22
 of  which 0.22
 named and 6.37
 named and 6.37
         unnamed
         unnamed
                                                                                                          074

-------
OPUSquan 20-JUL-1998 Page 5
Tox #1: - Tox #2: - Tox
Name # RT Respnse RA
1 31:29 8.06+06 1.54 y
S.Oe+06

2 31:49 3.66+05 1.49 y
3.66+05

3 31:59 6.5e+06 1.56 y
6.5e+06

4 32:04 8.8e+05 1.59 y
8.8e+05

5 32:10 3.56+06 1.57 y
3.56+06

6 32:16 3.8e+05 1.43 y
3.8e+05

7 32:20 7.4e+05 1.64 y
7.4e+05

8 32:26 1.8e+06 1.62 y
1.8e+06

9 32:30 5.9e+05 1.46 y
5.9e+05

1, 2,3,7, 8-PeCDD 10 32:37 8.0e+05 1.56 y
8.0e+05

11 32:42 4.0e+05 1.47 y
4.0e+05

12 32:54 2.56+05 1.37 y
2.5e+05

#3: -
Cone
2.19
4
3
0.10
2
1
1.77
3
2
0.24
5
3
0.95
2
1
0.10
2
1
0.20
4
2
0.49
1
6
0.16
3
2
0.22
4
3
0.11
2
1
0.07
1
1
Area

.8e+06
.2e+06

.le+05
.4e+05

.9e+06
. 5e+06

.4e+05
.4e+05

.le+06
.3e+06

.2e+05
.6e+05

. 6e+05
.8e+05

.le+06
. 9e+05

.5e+05
.4e+05

.9e+05
.le+05

.4e+05
.6e+05

.4e+05
.le+05
Height

1
1

8
5

1
9

1
1

7
5

9
6

1
8

4
2

1
9

1
1

7
5

5
3

.6e+06
.Oe+06

.Oe+04
.3e+04

.4e+06
.4e+05

. 9e+05
.2e+05

.7e+05
.Oe+05

.4e+04
. 8e+04

.5e+05
. 6e+04

.Oe+05
.5e+05

.3e+05
.3e+04

.8e+05
.2e+05

.6e+04
.7e+04

.2e+04
.8e+04

4
5

2
2

4
4

5
6

2
2

2
3

4
4

1
1

3
4

5
6

2
2

1
1
S/N

.3e+02
.2e+02

.2e+01
.7e+01

.Oe+02
.7e+02

.3e+01
.Oe+01

. le+02
.5e+02

.6e+01
.4e+01

. le+01
.3e+01

.le+02
.2e+02

.6e+01
.7e+01

.le+01
.Oe+01

.le+01
.9e+01

.4e+01
.9e+01
Mod?

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

y
y

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n

n
n
Of < 071

-------
OPUSquan   20-JUL-1998
                                      Page 6
 Ent: 43 Name:  Total Hexa-Furans
                                                 Page  5  of  8

                F:3  Mass:  373.821  375.818  Mod?  no   #Hom:17
 Run: 16 File: a!7jul98b    S:ll Acq:18-JUL-98 00:16:48  Proc:20-JUL-98  09:06:58
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34   Sample text:  1070-2 xl/2
   Amount: 4.28
     Cone: 4.28
   Tox #1: -
Name
of which 1.99
of which 1.99
     Tox #2:  -

#     RT Respnse
named and 2.30
named and 2.30
      Tox #3: -
                                        RA
                   1  33:31 2.1e+06  1.21 y
                            2.1e+06

                   2  33:37 4.5e+06  1.15 y
                            4.5e+06

                   3  33:43 3.1e+05  1.20 y
                            3.16+05

                   4  33:48 4.1e+05  1.16 y
                            4.1e+05

                   5  33:55 1.8e+05  1.09 y
                            1.8e+05
                      34:01 1.46+04
                            1.4e+04
                                     0.39 n
1,2,3,4,7,8-HxCDF  7  34:10 4.1e+06  1.24 y
                            4.1e+06

1,2,3,6,7,8-HxCDF  8  34:15 1.9e+06  1.28 y
                            1.9e+06

                   9  34:19 4.36+05  1.00 n
                            4.3e+05

                   10 34:27 5.2e+05  1.13 y
                            5.26+05

2,3,4, 6,7,8-HxCDF  11 34:37 l.le+06  1.13 y
                            l.le+06

1,2,3,7,8,9-HxCDF  12 35:12 3.0e+05  1.32 y
                            3.06+05
                   13 35:23 3.8e+03
                            3.86+03
                                     0.71 n
                   14 35:27 4.0e+03  0.15 n
                            4.06+03

                   15 35:31 1.76+04  0.29 n
                            1.7e+04

                   16 35:39 l.le+04  0.67 n
                            l.le+04

                   17 35:46 6.9e+03  0.46 n
                            6.9e+03
          Cone

           0.56
               ]
               c
           1.22


           0.08
               1
               1
           0.11

               1
           0.05
               s
               E
           0.00

               ]
           1.18

               1
           0.43
               ]
               I
           0.12


           0.14


           0.28
               C
               C
           0.09
               ]
               ]
           0.00
               :

           o.oo
unnamed
unnamed
                                                      Area  Height     S/N  Mod?
                                l.le+06 4.2e+05  9.8e+01  y  n
                                9.4e+05 3.6e+05  l.le+02  y  n
                               2
                                2.4e+06 8.6e+05  2.0e+02  y  n
                                2.1e+06 7.4e+05  2.4e+02  y  n
                               3
                                1.7e+05 5.8e+04  1.4e+01  y  n
                                1.4e+05 4.9e+04  1.5e+01  y  n
                               I
                                2.2e+05 7.2e+04  1.7e+01  y  n
                                1.9e+05 6.4e+04  2.0e+01  y  n

                                9.2e+04 3.5e+04  8.3e+00  y  n
                                8.5e+04 2.8e+04  9.0e+00  y  n
                               D
                                3.9e+03 2.1e+03  4.9e-01  n  n
                                l.Oe+04 3.4e+03  l.le+00  n  n

                                2.3e+06 6.7e+05  1.6e+02  y  n
                                1.8e+06 5.3e+05  1.7e+02  y  n

                                l.Oe+06 3.7e+05  8.7e+01  y  n
                                8.2e+05 3.0e+05  9.7e+01  y  n
                               2
                                2.2e+05 8.1e+04  1.9e+01  y  n
                                2.1e+05 7.0e+04  2.2e+01  y  n
                               1
                                2.7e+05 7.06+04  1.7e+01  y  n
                                2.4e+05 5.6e+04  1.8e+01  y  n
                               3
                                5.7e+05 1.6e+05  3.7e+01  y  n
                                5.0e+05 1.3e+05  4.0e+01  y  n

                                 .7e+05 4.7e+04  l.le+01  y  n
                                 .3e+05 3.6e+04  1.2e+01  y  n
                                                   1.6e+03 7.26+02 1.7e-01 n  n
                                                   2.2e+03 l.le+03 3.5e-01 n  n
                            0.00
                            0.00
                            0.00
               5.1e+02 4.36+02 l.Oe-01 n  n
               3.5e+03 1.4e+03 4.66-01 n  n
               D
               3.7e+03 1.9e+03 4.56-01 n  n
               1.3e+04 3.46+03 l.le+00 n  n
               3
               4.6e+03 2.2e+03 5.1e-01 n  n
               6.9e+03 2.7e+03 8.6e-01 n  n
               }
               2.2e+03 6.66+02 1.6e-01 n  n
               4.7e+03 1.9e+03 6.0e-01 n  n
                                                                    Page 6 of 8

 Ent: 44 Name: Total Hexa-Dioxins  F:3  Mass: 389.816 391.813 Mod? no   #Hom:12
                                                                                                    C((  076

-------
OPUSquan   20-JUL-1998
                                      Page 7
 Run: 16 File: al7ju!98b    S:ll Acq:18-JUL-98 00:16:48 Proc:20-JUL-98  09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-2 xl/2
   Amount: 2.92
     Cone: 2.92
   Tox #1: -
Name
of which 0.30
of which 0.30
     Tox #2:  -

#     RT Respnse
named and 2. 62
named and 2.62
      Tox #3:  -
                                        RA
                   1  33:52 5.26+05  1.20 y
                            5.2e+05

                   2  34:11 5.5e+06  1.28 y
                            5.5e+06

                   3  34:20 9.3e+05  1.38 y
                            9.36+05

                   4  34:26 1.5e+05  1.34 y
                            1.5e+05

                   5  34:36 6.8e+03  0.39 n
                            6.8e+03
1,2,3,4,7,8-HxCDD  6
                      34:42 1.6e+05  1.31 y
                            1.66+05
1,2,3,6,7,8-HxCDD  7  34:46 3.6e+05  1.22 y
                            3.6e+05

1,2,3,7,8,9-HxCDD  8  34:58 3.2e+05  1.20 y
                            3.26+05

                   9  35:04 2.66+04  1.01 n
                            2.66+04

                   10 35:12 5.86+03  1.19 y
                            5.8e+03

                   11 35:17 8.4e+03  1.40 y
                            8.46+03

                   12 35:23 l.le+04  4.00 n
                            l.le+04
                           Cone

                            0.19


                            2.02


                            0.34
                               C

                            0.05
                               £
                               6
                            0.00
                               3
                               4
                            0.07
                               c
                               (.
                            0.12

                               3
                            0.11
                               1
                               ]
                            0.01
                               ]
                               1
                            0.00


                            0.00
                               4

                            0.00
unnamed
unnamed
                                                      Area  Height    S/N  Mod?
               2.9e+05 l.le+05 3.5e+01 y  n
               2.4e+05 8.4e+04 4.6e+01 y  n
              2
               3.16+06 l.Oe+06 3.4e+02 y  n
               2.4e+06 8.2e+05 4.5e+02 y  n
              1
               5.4e+05 1.76+05 5.5e+01 y  n
               3.9e+05 1.26+05 6.7e+01 y  n

               8.6e+04 2.5e+04 8.2e+00 y  n
               6.5e+04 1.8e+04 9.9e+00 y  n
              3
               1.9e+03 8.5e+02 2.8e-01 n  n
               4.9e+03 2.0e+03 l.le+00 n  n
              7
               9.0e+04 3.4e+04 l.le+01 y  n
                .9e+04 2.7e+04 1.5e+01 y  n

               2.0e+05 6.0e+04 2.0e+01 y  n
               1.6e+05 5.3e+04 2.9e+01 y  n
              1
               1.7e+05 4.1e+04 1.46+01 y  n
               1.4e+05 3.86+04 2.1e+01 y  n

               1.3e+04 2.7e+03 9-Oe-Ol n  n
               1.3e+04 4.6e+03 2.56+00 n  n
              D
               3.1e+03 1.46+03 4.7e-01 n  n
               2.6e+03 8.6e+02 4.7e-01 n  n

               4.9e+03 1.46+03 4.6e-01 n  n
               3.5e+03 1.3e+03 7.0e-01 n  n
              3
               9.0e+03 2.96+03 9.5e-01 n  n
               2.2e+03 1.26+03 6.5e-01 n  n
                                                                                                    rr
                                                                                        07

-------
OPUSquan   20-JUL-1998
                   Page 8
                                                                    Page  7  of  8

 Ent: 45 Name: Total Hepta-Furans  F:4  Mass:  407.782  409.779  Mod?  no   #Hom:4

 Run: 16 File: al7ju!98b    S:ll Acq:18-JUL-98 00:16:48  Proc:20-JUL-98  09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-2 xl/2
   Amount: 0.57
     Cone: 0.57
   Tox #1: -
Name
of which 0.46
of which 0.46
     Tox #2:  -

#     RT Respnse
named and 0.11
named and 0.11
      Tox #3: -
                                        RA
1,2,3,4,6,7,8-HpCDFl  36:22 l.le+06  1.00 y
                            l.le+06

                   2  36:34 1.3e+05  0.92 y
                            1.36+05

                   3  36:40 1.4e+05  1.02 y
                            1.4e+05

l,2,3,4,7,8,9-HpCDF4  37:32 8.8e+04  0.91 y
                            8.8e+04
          Cone

           0.42
               c
               c
           0.05
               e
               (.
           0.06


           0.04
unnamed
unnamed
Area  Height    S/N  Mod?
                                5.7e+05 1.8e+05  9.5e+01  y  n
                                5.7e+05 1.7e+05  1.3e+02  y  n

                                6.2e+04 2.2e+04  1.2e+01  y  n
                                i.7e+04 2.1e+04  1.6e+01  y  n

                                7.1e+04 2.1e+04  l.le+01  y  n
                                7.0e+04 2.1e+04  1.6e+01  y  n
                               1
                                4.2e+04 l.le+04  5.9e+00  y  n
                                4.6e+04 1.3e+04  l.Oe+01  y  n
                                                                    Page 8 of 8

 Ent: 46 Name: Total Hepta-Dioxins F:4  Mass: 423.777 425.774 Mod? no   #Hom:4

 Run: 16 File: al7ju!98b    S:ll Acq:18-JUL-98 00:16:48 Proc:20-JUL-98 09:06:58
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-2 xl/2
   Amount: 0.38
     Cone: 0.38
   TOX #1: -
Name
of which 0.18
of which 0.18
     Tox #2:  -

#     RT Respnse
named and 0.19
named and 0.19
      Tox #3: -
                                        RA
                   1  36:21 7.0e+04  3.06 n
                            7.Oe+04

                   2  36:35 3.7e+05  1.04 y
                            3.7e+05

1,2,3,4,6,7,8-HpCDD3  37:10 4.6e+05  1.12 y
                            4.6e+05

                   4  37:31 4.5e+04  3.93 n
                            4.5e+04
          Cone

           0.03
               C
               1
           0.15
               1
               1
           0.18


           0.02
unnamed
unnamed
                                                      Area  Height    S/N  Mod?
                                5.3e+04 1.8e+04 1.5e+01 y  n
                                1.7e+04 5.8e+03 6.4e+00 y  n

                                1.9e+05 5.4e+04 4.5e+01 y  n
                                1.8e+05 5.56+04 6-Oe+Ol y  n
                               3
                                2.4e+05 6.5e+04 5.3e+01 y  n
                                2.2e+05 5.96+04 6.4e+01 y  n
                               I
                                3.6e+04 9.16+03 7.5e+00 y  n
                                9.2e+03 2.46+03 2.6e+00 n  n
                                                                                                     J  078

-------
File: A17JUL98B Acq: 18-JUL-1999
Sample #11 Text: 1070-2 xl/2 ALS
319.8965 S:ll SMO(1,3) BSUB(128,15
100%
50 j
•
0 '




— \ 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
321.8936 S:ll SMO(1,3) BSUB(128,15
100%
50J
-
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— • 	 1 	 i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
331.9368 S:ll SMO(1,3) BSUB(128,15
100%
50 1
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333.9339 S:ll SMO(1,3) BSUB(128,15
100%
50 j
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w— ' — i 	 1 	 1 i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
327.8847 S:ll SMO(1,3) BSUB(128,15
100%
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u— ' — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
00:
16:48 Exp: EXP_M23
_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
#11
,-3
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316.9824 S:ll SMO(1,3) PKD(3 , 3 , 3 , 100 .
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27:00 28:00 29:00 30:00 Time
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i: A17JUL98B Acg: 18-JUL-1998 00:16:48 Exp: EXP M23 DBS OVATION Voltage SIR EI + GC Autospec-UltimaE Parad
)le #11 Text: 1070-2 xl/2 ALS #11
8546 S:ll F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 3608 . 0 , 1 . 00% , F, F)
A4.84E6 A3.94E6
M / 1 A2.11E6
/ \ MA A1.11E6
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3b!l2 3b!24 36136 30:48 Sllod 3i!i2 3il24 3ll36 31 -48' 32:
8517 S:ll F:2 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1988 . 0 , 1
A3.15E6 2 5
A t\£j • ^J
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36!i2 36I24 3o!36 30:48 3l!6d 3i!i2 3l!24 3ll36 31\48 32\
8949 S:ll F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 5140 . 0, 1
3b!i2 30124 3b!36 3()!48 Sllod 31112 3l!24 3ll36 sil-Js'1^!
8919 S:ll F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3660 . 0 , 1
3bli2 36!24 30136 30:48 3lS6d 31 ! 12 ' 31 124 ' 31 ! 36 ' 31 \48 ' 32 !
366.9792 S:ll F:2 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
100*30:1030:20 30:50 31:07 31:19 31:35 31:55
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-------
File: A17JUL98B Acq: 1«-JUL-1998 00:16:48 Exp: EXP_M23_
Sample #11 Text: 1070-2 xl/2 ALS #11
389.8156 S:ll F:3 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3,5,2,0.
100%
50J
-
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A3.11E6
A

A2.86E5 / \ A5^9E5

33!24 33136 33!48 34!oO 34! 12 34!24
391.8127 S:ll F:3 SMO(1,3) BSUB{128 , 15 , -3 . 0) PKD(3,5,2,0.
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33-24 33!36 33:48 34:00 34:12 34:24
401.8559 S:ll F:3 BSUB(128, 15 , -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 10960
100%
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" ' i i — 1 — i — r— i — i — i 1 i — i — i— i — i — 1 — r— T— T — r i i i i i i i i i i i i i i i > i
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" ' 1 1 	 1 	 1 	 1 	 1— 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 I—I — ' T1 T" 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
33!24 33!36 33:48 34:00 34:12 34:24
380.9760 S:ll F:3 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F,
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DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm

10%, 3040. 0,1. 00%, F,F)


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34!36 34148 3s!oO 3s!l2 3s!24 35:36 35 48 Time
10%, 1840. 0,1. 00%, F,F)


A1.62E5

8.2E5
L4.1E5

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34:36 34:48 35:00 35:12 35:24 35:36 35 48 Time
.0,1.00%,F,F)
A1'?3E8 A1.92E8
A A
M A
j]\^ j\^
8.4E7
_4.2E7
' O.OEO
34!36 34!48 35!oO 3s!l2 3s!24 3s!36 3s!48 Time
0,1.00%,F,F)
Al'f3E8 A1.52E8
A A
M A
n^]^
6.6E7
L3.3E7
' O.OEO
34! 36 34!48 35.!00 3s!l2 35^24 3s!36 35:48 Time
F)
34:36 34:48 34:58 35jJL6 35:29 1 . 6E8


_7.8E7
"O.OEO
34\36' ' 's^U's' 35!oO 3s!l2 3s!24 3s!36 3s!48 Time
O
00

-------
File
Saim:
423.
1003
50_
0
425.
100S
50J
0'
435.
100%
50J
0'
437.
100%
so:
0"
430.
100%
so:
0"
->'
>: A17JUL98B Acq: 18-JUL-1998 00:16:48
)le #11 Text: 1070-2 xl/2 ALS #11
7767 S:ll F:4 SMO(1,3) BSUB(128, 15, -3 . 0 )
A1.89E5
A
A5.29E4 / \
/Y J v_
36166 36112 ' 36124 ' 36136 ' 36! 48' ' 37:
7737 S:ll F:4 SMO(1,3) BSUB(128, 15, -3 . 0 )
A1.82E5
n
A
A1.73E4 / \
s^\ y » —
36166 36ll2 36124 36136 36148 37l
8169 S:ll F:4 SMO(1,3) BSUB (128, 15, -3 . 0)

36166 36112 36124 36:36 36! 48 37 1
8140 S:ll F:4 SMO(1,3) BSUB(128, 15, -3 . 0)

36:00 36:12 36:24 36:36 36:48 37:
9728 S:ll F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%
36:19 36:31 36:47
Exp: EXP_M23_DB5
PKD(3,3,3,0.10%
A2.41E5
A
/V,
66 37ll2 37124
PKD(3,3,3,0.10%
A2.16E5
A
A
/i_
66 37li2' 37124
PKD(3,3,3,0.10%
Al . 42E8
/I
66 37li2 37124
PKD(3,3,3,0.10%
A1.37E8
j\^
00 37:12 37:24
,0.0,1.00%,F,F)
37:05
_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
,1208.0,1.00%,F,F)
.60E4
/X_ 	 	 ^
37136' 37148 38166 38:12 38124 Sslie SsUs 39
,912.0,1.00%,F,F)


37136 37148 38166 3s!l2 38124 Sslie 38!48 39!
,5764.0,1.00%,F,F)

37!36 37148 38166 38112 38124 38136 SsUs 39!
,2924.0,1.00%,F,F)

igm
L3.3E4
LO.OEO
0 0 Time
6.0E4
L3.0E4
LO.OEO
00 Time
3.8E7
L1.9E7
' O.OEO
00 Time
3.7E7
.1.8E7
O.OEO
37:36 37:48 38:00 38:12 38:24 38:36 38:48 39 00 Time
37:38 37:57 38:12 38i24 38:52 1 . OE8

36166 36112 36124 36136 36l48 37 1
00 37:12 37:24
15.1E7
10.0EO
37:36 37:48 38:00 38:12 38:24 38:36 38:48 39 00 Time
o
00

-------
File
Samp
457.
1003
50J
0'

459.
100S
501
OJ

469.
100%
50J
0'

471.
1002
50J
0"

454.
1004
501
0'
O1
O
00
: A17JUL98B Acq: 18-JUL-1998 00:16:48 Exp : EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
le #11 Text: 1070-2 xl/2 ALS #11
7377 S:ll F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3376 . 0, 1 . 00%, F, F)
A5 -65E5
A
j \^
39ll2 39i24 39136 39148 4o!ob 4o!l2 40-124 4ol36 4oU8 41:
7348 S:ll F:5 SMO(1,3) BSUB (128 , 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1668 . 0 , 1 . 00%, F, F)
A6 - 76E5
A
/ V 	
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
7780 S:ll F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2452 . 0, 1 . 00%, F, F)
Al . 91E8
A
J V 	
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
7750 S:ll F:5 SMO(1,3) BSUB(128 , 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2040 . 0, 1 . 00%, F, F)
A2 .16E8
A
J V 	
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
9728 S:ll F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00% , 0 . 0 , 1 . 00%, F, F)
39:06 39il9 3_9j30 39:37 39:50 39:59 40:13 40:24 40:34 40:4640:51
7

39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:


igm


1.4E5
.7.1E4

00 Time

1.6E5
_8.0E4
.O.OEO
00 Time

4.4E7
12.2E7
' O.OEO
00 Time

_4 . 9E7
12 . 5E7
_O.OEO
00 Time

1.1E8
.5.5E7
.O.OEO
00 Time



-------
File: A17JUL98B Acq: 18-JUL-1998 00:16:48 Exp: EXP M23 DB5
Sample #11 Text: 1070-2 xl/2 ALS #11
303.9016 S:ll SMO(1,3) BSUB(128 , 15, -3 . 0 ) PKD(3 , 3 , 3 , 0 . 10%, 5320
100% A7.70E7
50j A3.66E7 M A5.20E7 A3.69E7
	 24 100
305.8987 S:ll SMO(1,3) BSUB(128
100% Al
5Q: A4.76E7
: A A2.27E7
0: A /\ A
24 100
315.9419 S:ll SMO(1,3) BSUB(128
100%
o:
24:00
317.9389 S:ll SMO{1,3) BSUB(128
100%
sol
24:00
375.8364 S:ll SMO(1,3) BSUB(128
100%
50 1
24:00
316.9824 S.-ll SMO(1,3) PKD(3,3,
100% 23_i35 24:06 24:33
50 j
|Q] 24:00
25 loo' ' ' ' 26 loo'
,15, -3.0) PKD(3, 3,3, 0.10%, 3436
. OOE8
l\ A6.78E7 A4.84E7
\ J\ ~A A2-S9E7AAA2
/ VVT \ /i\ AA /YV
25 loo' ' 26 loo'
,15, -3.0) PKD(3,3,3,0.10%,5408
25:00 26:00
,15, -3.0) PKD(3,3,3,0.10%,2728
25:00 26:00
,15, -3.0) PKD(3,3,3,100.00%,76
25:00 26:00
3,100.00%,0.0,1.00%,F,F)
_25jLOO 25:47 26:19

25:00 26100
OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
.0,1.00%,F,F)
A5.50E7
27 loo 	 28 loo' ' ' ' 29 loo' ' ' ' 30 !(
.0,1.00%,F,F)
y\
•AOE7 / \ A1.27E7
/ v ^\ / v rx ^-^
igm
1.5E7
L7.5E6
)0 Time
1.9E7
1.9. 7E6
: O.OEO
27 loo' ' ' ' 28 loo' ' ' ' 29 100 	 30:00 Time
.0,1.00%,F,F)
A2.26E8
27:00 28:00 29:00 30:(
.0,1.00%,F,F)
A2.89E8
27 loo' ' ' 28 Too 29 100 30 !(
.0,1.00%,F,F)
27:37
/! 27:58
27:11 /I A 28:27 29:35
_ _ _ _ ^— ^^ S*-S \ ^/ ^^^ _/X_ — 	 	 S-S-^^^r" 	 S^s. J ^V/V ^— N^
4.7E7
1.2. 4E7
i-O.OEO
)0 Time
6.0E7
_3.0E7
_O.OEO
JO Time
5.4E4
_2.7E4
O.OEO
27:00 28:00 29:00 30:00 Time
26:5427:1627:36 28:07 28:32 28:58 29 :28 29 : 51 6 . 4E7

_3.2E7
-O.OEO
27 loo' ' ' 28 100 29 100 '30:00 Time

-------
O
00
en
    File:  A17JUL98BAcq: 18-JUL-1998 00:16:48Exp:  EXP_M23_DB5_OVATION Voltage SIR EI +GC Autospec-UltimaE—Paradigm
    Sample #11  Text: 1070-2 xl/2  ALS #11
    339.8597 S:ll F:2 SMO(1,3) BSUB (128,15,-3 . 0)  PKD(3 , 3 , 3 , 0 .10%, 1|5232 . 0,1. 00%, F, F)
    1004
A2 . 67E7
A A]
A1.27E7 / \
/\ A / 44.81E6
y v / \/ y\ , 	 ,
Tn.io in . o^ i n . -jc in ! /i o 11 . nn -31.10 1 1 . o* 11 ! i c


A5.46E6
/ V /TV^X/V
•511^0 i^.rtn "» o . 1 o


A5.39E6
/Vx
i i *i i r i i i* i i V I i i i i i i i i i i i i i i i i i 1 1
7.2E6

_3.6E6
_0 . OEO

         30:12  30:24  30:36   30:48  31:00  31:12  31:24   31:36  31 48  32:00  32:12  32:24  32:36  32:48  33:00  33:12    Time
    341.8568 S:ll F:2 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,10444.0,1.00%,F,F)
    1004
A1.77E7
A A9.46E6
"'A'6 A/\3.09E6 AA4'^
/ \ J\J V\1 	 ,/V/l\
•jnlio "Jnlo^ inl-jc in ! /i o Tilnn 1 1 ! i o 11 ! o ji 1 1 ! or -n!/io T>!


A3.81E6
^J\^
nn '-> •-> ' 1' ->


A3.56E6
y\x\
i 1 1 I iyi i T i I *n i i i i i i i i "i i i i i i i j i i1
4.8E6

_2.4E6
" 0 OEO

    351.9000  S:ll  F:2 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1080.0,1.00%,F,F)
    1004
                                                                                                               33:12    Time
A2.81E8 A2.71E8
A A
/I A

o n . 1 o "3r».o>i •^n.'^^' *5A.>io "51. nn 11.10 i-i.n^ -ii_-i/- oi.jin •» *^ : /% n -»^io •* ^ ^ A o^'-ix- t n ' j n -i -^ ' « « ——',.—
1.0E8
L5.0E7
-O.OEO
         30:12   30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00  32:12   32:24  32:36  32:48  33:00  33:12    Time
   353.8970  S:ll  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1676.0,1.00%,F,F)
   1004                                                           A1.79E8        A1.72E8                            6. 4E7


                                                                                                                    _3.2E7

                                                                                                                    _O.OEO
                                                                                                                        Time
   409.7974  S:ll  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,5556.0,1.00%,F,F)
   1004                                                       31^47    |                                            _1.5E6


A A

      O
                                                                     31^58
                                                          31:39
                                                                                   32:24
_7.3E5

 O.OEO
         30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00   32:12  32:24  32:36  32:48 ' 33166 ' 33112     Time
366.
1004
50 j
o:
9792 S:ll F:2
^0:10 30:20


SMO(1,3) PKD(3,3,3,100.00%,0.0,1
30:50 31:07 31:19


00%,F,F)
31:35 31:5532:0532:1532:24 32:41 33:003J:09 7.2E7

L3.6E7
" O.OEO

                                                                                                                       Time

-------


































rv
^-N

File: A17JUL98B
Sample #11 Text:
373.8207 S:ll F:3
100% A2.
-
50 1
_
o-

A1.14E9
A 1
]
/
' i i — iii"i — i — r— r
33:24 33:
375.8178 S:ll F:3
100%, A2 .
.
50^
0 '
/
A9.43E9
A/
33:24 33:
383.8639 S:ll F:3
100%
50 j
o"
Acer:
18-JUL-1998 00:16:
48 Exp: EXP_M23 DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
1070-2 xl/2 ALS #11
SMO(1,3) BSUB(128, 15,-
43E6
A
\
\
V_-
— i — rn-
36

A2

A2.18E5 /

33:48 34:00
3.0)

.27E6
A
' V
1
34:12
SMO(1,3) BSUB(128,15,-3.0)
11E6
A
\
\
36

Al

A1.87E5 J
33:48 34:00

.82E6
A
/v
1 1 'l
34:12
BSUB(128,15,-3.0) PKD (3, 5, 2
PKD ( 3 ,



2v.l5E5
T~~^
34
PKD ( 3 ,



X-14E5
34
,0.10%
5, 2, 0.10%, 4220. 0,1. 00%, F,F)



A5.£
	 /•

!24' ' '34!;
5,2,0.10%,



A4.9
:2^~ 34!:
,37080.0,1
8.


^5 Al^UES


14.

U •
6 ' 's^UV ' '35 loo 35!l2 35124 3s!36 35 48
3152. 0,1. 00%, F,F)
7.


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13.
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6 34:48 35:00 35:12 35:24 35:36 35:48
.00%,F,F)
A1.38E8
]\


"— '—i — i — i — i — i i i i i
33:24 33:
385.8610 S:ll F:3
100%
50 j
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"-1— i — i — i — i — i — r— i — r— T
33:24 33:
445.7555 S:ll F:3
100%
-
~
0 "


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36

>
1 1 | 1 1 1 1 1 | 1 1 1 •*!
33:48 34:00
A/1

34 1 12
BSUB(128,15,-3.0) PKD(3,5,2


34
,0.10%




_5.
13.
^0.
:2'4' ' '34136 ' 34!48 35^00 3s!l2 35I24 35136 35 48
,64524.0,1
.00%,F,F)
A2.63E8
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33:48 34:00
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SMO(1,3) BSUB(128,15,-3.0)



V
34
PKD ( 3 ,




1.
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0.
!24' 34136 34148 35!oO 35ll2 35I24 35I36 35 48
7E5

3E5

Time

5E5

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Time

9E7
OE7
OEO
Time

1E8
7E7
OEO
Time
3, 3, 100. 00%, 4240. 0,1. 00%, F,F)
34:12
A
34:06 \
s\ 1 \


u ' i i | i r i-r-i-T
33:24 33:
380.9760 S:ll F:3
100% 33:23

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33:24 33:
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00


36
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33:48 34 00
SMO(1,3) PKD(3,3,3,100





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36


34




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33:48 34:00


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:0934




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34X3834-45
34^3^7
\_/X/— ^_i>
-------




































•">
— s
File: A17JUL98B Acq: 18-JUL-1998 00:16:48
Exp : EXP_M2 3 _DB 5
JDVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #11 Text: 1070-2 xl/2 ALS #11
407.7818 Sill F:4 SMO(1,3)
1008
50_


A5.73E5
A
A
BSUB(128,15,-3.0)


/ \ A6.15E4
/ \ -s~^- -"••-

36166 36112 36T24
409.7788 S:ll F:4 SMO(1,3)
lOOi
50 J
".
0
A5.73E5
A
A
/ \»6
J ^ 	
36 T66 36ll2r ' 36T24 "
417.8253 S:ll F:4 SMO(1,3)
100S
-
50^
OJ
A6.66E7
A
A
A
/ v_
36166 36112 36124
419.8220 S:ll F:4 SMO(1,3)
100%
•
50 J
o:
A1.48E8
A
A
\
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36166 36112 36124
479.7165 S:ll F:4 SMO(1,3)
100%
50 j
-
0.-

35:57
/\_ 36 :08 36
~— — -' s — ^"N, — . .-•'* ' 	 . _.- 	

36.:00 36:12 36^24
430.9728 S:ll F:4 SMO(1,3)
100%^ 36:19 36:
:
50J
o:
/


j--|--T — r— j — | — [ -T — (- — i — -| — j — i — | — j — i — j — | — [—
36:00 36:12 36:24
o
00
•si

36l:36 36 Us 37
BSUB(128,15,-3.0)


.71E4
f^^^l f^^^
36:36 36:48 37:
BSUB (128, 15, -3.0)




36\36 36! 48 37!
BSUB(128,15,-3.0)




36:36 36:48 37l
BSUB(128,15,-3.0)

37:
/
•z^j^i^^y

1 > i ' ' ' ' ' i ' ' ' ' ' i
36:36 36:48 37:
PKD(3,3,3,100.00%
31 36:47



i' i — i — i i ' i 'i 'i ' i i T i r i r~
36:36 36:48 37:



PKD(3,3,3,0.10%


A4

66 37ll2 37124'
PKD(3,3,3,0.10%


A4.

66 37! 12 ' 37124
PKD(3,3,3,0.10%

A4.
y
J
66 37li2' 37124
PKD(3,3,3,0.10%

Al.
1
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66 37112 37124
,1884. 0,1. 00%, F,F)


.19E4

1.8E5
19.1E4

• n r>Rfi
37:36 37:48 38:00 38:12 38124 38136 38148 39:00 Time
,1336.0,1.00%,F,F)


63E4

1.8E5
_8.8E4

n DRD
37:36 37:48 38:00 38:12 38:24 38:36 38:48 39 00 Time
,12880. 0,1. 00%, F,F)
r2.0E7
76E7
^\
V

_1.0E7
O.OEO
37136' 37148' 3s!66 38112 38124 Sslie SsUs 39 00 Time
6908. 0,1. 00%, F,F)
4.5E7
07E8
\
v

.2.2E7
O.OEO
37136 37148 38166 38112 38124 38l36 38:48 39 00 Time
PKD(3,3,3,100.00%,4704.0,1.00%,F,F)
37:09
00 / \
V-/ V_^37:21
\ j^~\.
\^^ 	
	 1 i i ? i i 1 i i
00 37:12 37:24
, 0.0,1. 00%, F,F)


31^9 37:56 38:11 38:22 38:41 38:53
— -^~V_^^ X- — • — — 	 ^s~—*s s 	 	 , — • 	 	 	 s 	 	 	 	 	 — ***^_ 	 • 	 • 	 •« 	

_5.8E4
12 . 9E4

O.OEO
37:36 37:48 38:00 38:12 38:24 38:36 38148 39:00 Time

37:05 37:33 37:47 37:57 38:12 38:24 38:52 1 . OEfi



1 1 1 1 1 I | — | — | — | — I — I — I — i — i
00 37:12 37:24






1 i i i i i i > | ' ' ' i ' | i i ' ' i | 	 | 	 | i i i 'i i | i i i i i |'

.5.1E7
O.OEO
37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:00 Time




-------
File: A17JUL98B
Sample #11 Text
441.7427 S:ll F:
100%
sol



39:12
443.7398 S:ll F:
100%
50J




39:12
469.7780 S:ll F:
100%
50 j
0 '


39:12
471.7750 S:ll F:
100%
50J:
o •


39:12
513.6775 S:ll F:
100%
50J
o •

^ 39:09
"-1 — i' i -r — e— i — i —
39:12
454.9728 S:ll F:
100% 39:06
50 j
o"
/

39:12
Acer: 18-JUL-1998 00:16
: 10'70-2 xl/2 ALS #11
5 SMO(1,3) BSUB(128,15,



39:24 39:36
5 SMO(1,3) BSUB(128,15,



39:24 39:36
5 SMO(1,3) BSUB(128,15,



T 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 r
39:24 39:36
5 SMO(1,3) BSUB(128,15,



T 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 < 	 r
39:24 39:36
5 SMO(1,3) BSUB(128,15,


:48 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec UltimaE Paradigm

-3.0) PKD(3,



s'gUs
-3.0) PKD(3,



39:48
-3.0) PKD(3,



39U8
-3.0) PKD(3,



39148
-3.0) PKD(3,

*» f\ r* r\
/-\ 3jL^° 3?j-42 ^^\
39124 ' ' ' 39\36
s'gUs
5 SMO(1,3) PKD{3,3,3,100.00%,0.0,1.
39:19 39:30 39:37 39:50


T 	 1 	 1 	 1 	 1 	 1 	 p 	 1 	 1 	 1 	 1 	 1 r
39:24 39:36


39:48

3, 3, 0.10%, 1028. 0,1. 00%, F,F)
A2 -46E5
/\

_b .bE4
12.8E4
: O.OEO
40:00 40:12 40:24 40:36 40:48 41:00 Time
3, 3, 0.10%, 2008. 0,1. 00%, F,F)
A3 J-4E5
A
y A4.22E4
_7 .8E4
L3.9E4
- O.OEO
40:00 40:12 40:24 40:36 40:48 41:00 Time
3, 3, 0.10%, 2452. 0,1. 00%, F,F)
Al . 91E8
/\
y v_
..4.4E/
_2.2E7
-O.OEO
4o!ob 4o!l2 40^24 4ol36 4oUs 41:00 Time
3, 3, 0.10%, 2040. 0,1. 00%, F,F)
A2 . 16E8
/\
y V 	
_4 . yE i
_2 . 5E7
" O.OEO
40:00 40:12 40:24 40:36 40:48 41:00 Time
3, 3, 100. 00%, 48. 0,1. 00%, F,F)
40:02
/ \ 40:10
^-J V^-^^^V^AH-^ 	 	 40^_44_^ ^ f~^
/ . /JiJ
_3.8E3
O.OEO
4o!ob 40:12 40:24 40:36 40:48 41:00 Time
00%,F,F)
39:59 40:13 40:27 40:34 40:4640:51 1 . 1E8


.5.5E7
O.OEO
40:00 40:12 40:24 40:36 40:48 4l!oO Time
O
00
00

-------
















0
o
OPUSquan 22-JUL-1998 Page 1
Filename
Sample
Acquired
Processed
Sample ID
Cal Table
Results Table
Comments
Typ
Unk 2
ES/RT 13C-2
a21ju!98f
5
21-JUL-98 22:34:59
22-JUL-98 08:32:14
1070-2 xl/2
07feb-m23conf
M8290-23-072198F

Name; Resp; Ion 1; Ion 2; RA;?; RT; Cone; DL; S/N1;?; S/N2;? mod?
,3,7,8-TCDF; 5.42e+07; 2.36e+07; 3.06e+07; 0.77;y; 27:55; 3.995; 0.0156; 711;y; 877;y no
,3,7,8-TCDF; 1.43e+09; 6.27e+08; 8.01e+08; 0.78;y; 27:53; 350.023; -; 3005;y; 4676;y no
Total Tetra Furans; 2.81e+09; 1.02e+08; 1.33e+08; 0.77;y; 18:12; 206.789; 0.0156; 5256;y; 6445;y no
DPE
LMC QC CHK



00
CO
HxCDPE; *; * ;NotFnd; *; -; *;n no
ION (Tetra); *; * ;NotFnd; *; -; DivO;n no
-;-; 27:55
-;-; 27:55 ; -; -; no



Page 1

-------
OPUSquan   22-JUL-1998
                                      Page 1
 Ent:  3  Name:  Tetra Furans
                                                                    Page 1  of 1

                                   F:l  Mass:  303.902  305.899  Mod?  no   #Hom:30
 Run: 10 File: a21ju!98f    S:5  Acq:21-JUL-98 22:34:59  Proc:22-JUL-98  08:32:14
 Tables: Run: a21ju!98b  Analyte: m23_conf    Cal:  07feb-m23»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-2 xl/2
   Amount: 206.79  of which 3.99
     Cone: 206.79  of which 3.99
                        Tox #2:  -
   Tox #1: -

Name
named and 202.79  unnamed
named and 202.79  unnamed
      Tox #3:  -
                         RT Respnse
                                        RA
                   1  18:12 2.4e+08  0.77 y
                            '2.4e+08

                   2  19:52 2.0e+08  0.77 y
                            2.0e+08

                   3  20:06 l.Se+08  0.77 y
                            l.Se+08

                   4  20:22 2.5e+08  0.77 y
                            2.5e+08

                   5  20:40 l.le+08  0.77 y
                            l.le+08

                   6  21:13 l.Se+08  0.76 y
                            1.5e+08

                   7  21:33 1.7e+08  0.76 y
                            1.7e+08

                   8  21:50 2.0e+07  0.71 y
                            2.0e+07

                   9  21:59 3.76+07  0.74 y
                            3.7e+07

                   10 22:10 1.5e+08  0.75 y
                            l.Se+08

                   11 22:35 7.7e+07  0.75 y
                            7.7e+07

                   12 22:56 1.4e+05  0.80 y
                            1.4e+05

                   13 23:18 2.7e+08  0.76 y
                            2.7e+08

                   14 23:28 1.5e+08  0.77 y
                            l.Se+08

                   15 24:19 1.26+08  0.77 y
                            1.2e+08

                   16 24:33 8.9e+06  0.75 y
                            8.9e+06

                   17 25:01 1.4e+08  0.76 y
                            1.4e+08

                   18 25:27 7.3e+07  0.77 y
                            7.3e+07

                   19 26:00 7.5e+06  0.76 y
                            7.5e+06
                                              Cone

                                              17.32
                                                   ]
                                                   ]
                                              14.40
                                                   £
                                                   1
                                              11.39
                                                   6
                                                   8
                                              18.40
                                                   1
                                                   1
                                               7.90
                                                   4
                                                   e
                                              10.87
                                                   e
                                                   £
                                              12.60

                                                   c
                                               1.47
                                                   £
                                                   ]
                                               2.72
                                                   ]

                                              11.22
                                                   €
                                                   £
                                               5.64
                                                   i
                                                   4
                                               0.01
                                                   e

                                              19.55
                                                   ]
                                                   ]
                                              11.13
                                                   e
                                                   £
                                               8.83
                  Area  Height    S/N  Mod?
                .Oe+08 2.1e+07 5.3e+03 y  n
                .3e+08 2.7e+07 6.4e+03 y  n

               8.56+07 1.5e+07 3.7e+03 y  n
               l.le+08 1.9e+07 4.5e+03 y  n
              3
               6.7e+07 l.le+07 2.7e+03 y  n
               8.7e+07 1.4e+07 3.3e+03 y  n
              3
               l.le+08 1.8e+07 4.6e+03 y  n
               1.4e+08 2.4e+07 5.6e+03 y  n

                .7e+07 7.8e+06 2.0e+03 y  n
               6.1e+07 l.Oe+07 2.4e+03 y  n
              7
               6.4e+07 l.le+07 2.8e+03 y  n
               8.4e+07 1.4e+07 3.4e+03 y  n
              D
               7.46+07 9.8e+06 2.5e+03 y  n
               9.7e+07 1.3e+07 3.0e+03 y  n

                .3e+06 2.0e+06 5.0e+02 y  n
                .2e+07 2.7e+06 6.5e+02 y  n

                .66+07 3.56+06 8.9e+02 y  n
               2.1e+07 4.7e+06 l.le+03 y  n
              I
               6.56+07 1.2e+07 3.0e+03 y  n
               8.7e+07 1.6e+07 3.7e+03 y  n

               3.3e+07 5.8e+06 1.5e+03 y  n
               4.4e+07 7.76+06 1.8e+03 y  n

               6.36+04 3.96+04 9.8e+00 y  n
               7.8e+04 4.86+04 l.le+01 y  n
               l.le+08 1.4e+07 3.6e+03 y  n
               l.Se+08 1.9e+07 4.5e+03 y  n

               6.66+07 9.2e+06 2.3e+03 y  n
               8.56+07 1.26+07 2.96+03 y  n
                                               0.66
                                              10.04
                                               5.35
                                               0.55
               5.2e+07 6.9e+06 1.8e+03 y  n
               6.8e+07 9.2e+06 2.26+03 y  n
              S
               3.8e+06 5.4e+05 1.4e+02 y  n
               S.le+06 7.2e+05 1.7e+02 y  n
              1
               5.9e+07 7.8e+06 2.0e+03 y  n
               7.7e+07 l.Oe+07 2.4e+03 y  n

               3.1e+07 3.8e+06 9.7e+02 y  n
               4.1e+07 5.0e+06 1.26+03 y  n

               3.2e+06 4.4e+05 l.le+02 y  n
               4.2e+06 5.7e+05 1.3e+02 y  n
                                                                                                r
                                                                                                       090

-------
OPUSquan   22-JUL-1998                Page 2
                   20 26:33  l.Oe+08   0.76 y    7.43
                            l.Oe+08                4.4e+07 5.4e+06 1.4e+03 y  n
                                                  5.7e+07 7.1e+06 1.7e+03 y  n
                   21 27:34  l.Oe+08   0.78 y    7.50
                            l.Oe+08                4.4e+07 5.2e+06 1.3e+03 y  n
                                                  5.7e+07 6.8e+06 1.6e+03 y  n
2,3,7,8-TCDF       22 27:55  5.4e+07   0.77 y    3.99
                            5.4e+07                2.4e+07 2.8e+06 7.1e+02 y  n
                                                  3.16+07 3.7e+06 8.8e+02 y'n
                   23 28:13  2.5e+06   1.57 n   .0.18
                            2.5e+06                l.Se+06 2.3e+05 5.8e+01 y  n
                                                  9.7e+05 2.86+05 6.7e+01 y  n
                   24 28:32  9.3e+07   0.76 y    6.87
                            9.3e+07                4.0e+07 4.5e+06 l.le+03 y  n
                                                  5.3e+07 5.9e+06 1.4e+03 y  n
                   25 29:03  l.Oe+06   0.39 n    0.08
                            l.Oe+06                2.9e+05 6.7e+04 1.7e+01 y  n
                                                  7.4e+05 1.7e+05 4.1e+01 y  n
                   26 29:18  5.3e+07   0.70 y    3.91
                            5.3e+07                2.2e+07 2.5e+06 6.4e+02 y  n
                                                  3.1e+07 3.46+06 8.1e+02 y  n
                   27 29:37  6.3e+07   0.75 y    4.63
                            6.3e+07                2.7e+07 2.9e+06 7.2e+02 y  n
                                                  3.6e+07 3.8e+06 8.9e+02 y  n
                   28 31:51  2.7e+07   0.80 y    2.01
                            2.7e+07                1.2e+07 1.2e+06 3.Oe+02 y  n
                                                  1.5e+07 1.5e+06 3.5e+02 y  n
                   29 33:46  7.6e+05   0.95 n    0.06
                            7.6e+05                3.7e+05 l.Oe+05 2.5e+01 y  n
                                                  3.9e+05 1.26+05 3.0e+01 y  n
                   30 33:48  1.2e+06   0.80 y    0.09
                            1.2e+06                5.2e+05 l.le+05 2.7e+01 y  n
                                                  6.5e+05 1.4e+05 3.2e+01 y  n
                                                                                                     091

-------
File: A21JUL98F  Acq:  21-JUL-1998  22:34:59   Exp:  M23_DB225  Voltage SIR EI+  GC Autospec-UltimaE  Paradigm
Sample #5  Text: 1070-2 xl/2  ALS  #5
303.9016 S:5 SMO(1,3)  BSUB (128 , 15 , -3 . 0)  PKD(3 , 3 , 3 , 0 . 10%, 3956 . 0 , 1 . 00% , F, F)
100%              A1.Q2E8     M.08E8
                                              A1.15E8
                                   A6.36E7
  O
                                                                                                                  2.1E7

                                                                                                                 _1.0E7
                                                      AA       '
                                                      A.  A A    A
                                                               T >' '—'—>r '" r
                                                             26:00      28:00
                                                                                   /\
                                                                                                                   .O.OEO
                                                                                                                      Time
                                                     I
 50_

  OJ
       16:00      18iOO      20iOO      22iOO      24iOO
305.8987 S:5 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,4208.0,1.00%,F,F)
100%              A1.33E8     A1.41E8
                                              A1.51E8
                                   A8.40E7  .
                                                       A7'74E7 A5.72E7    A5.24E7

                    -r'-'r—i—i—i—i' ) vr"i' i' V 'i IT|" 'i ' I—i ' i1 'i—| ' .'"i 'i' I 'i—T / >—i—J \f\—/H—r^r^
       16:00      18:00      20:00      22:00      24:00     26:00     28:00
315.9419 S:5 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3 , 3,3,0.10%,24212.0,1.00%,F,F)
100%                                                                  A6.27E8

 50J

  OJ
                                                                                   30:00 '  '  ' 32:00   '  '
                                                                                                                  2.7E7

                                                                                                                 L1.4E7
                                                                                            A1.51E7
                                                                                             —r-T—i—i—c—i  i i—i—i—r
                                                                                              32:00      34:00
                                                                                                                 LO.OEO
                                                                                                                     Time
                                                                                                                   7.3E7

                                                                                                                  _3.6E7
                                                                                                                  .O.OEO
                                                                                                                      Time

                                                                                                                  .9.3E7

                                                                                                                  .4.7E7

                                                                                                                  .O.OEO
                                                                                                                      Time
       16:00      18:00      20:00      22:00      24:00       26:00      28:00
317.9389 S:5 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3 , 3,3,0.10%,19864.0,1. 00%, F, F)
100%                                                                   A8.01E8
 50

  0
                                                                                   soo
                                                                                              32o
                                                                                                         34-o
        T
                              T
                                         T
                                                    T
                                                      -l	1—I	r
                                                             -i—|—i—r
                                                             26:00
                                                                          r—i—i—i-
                                                                        28:00
       16:00      18iOO      20.;00      22.:00      24^00
375.8364 S:5 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,15960.0,1.00%,F,F)
100%                     19.; 10
                                                     24:28
 50J
                                                                                   —\—i—i—i	1—i—i—i—r—i—r
                                                                                   30:00      32:00
                       I  i	r—r	r
                      34:00
                                                                       27:53   29:14   30:50    32:28   33:48
                                                             26iOO
                                                                        28:00
                                                                                   30:00
                                                                                              32:00
      16:00      18iOO      20iOO      22100       24iOO
16.9824 S:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
         16:35     18:20   ^20:04    21:39.     23;30 __ 25:11     27; 00 28 :Q1 29: 02  30^20     32:04
50_
 o
                                                                                                         33:57
                 18:00
.O.OEO
   Time

.7.3E7

.3.7E7

.O.OEO
   Time
                            20! ob
                                                  24 lob
                                                             26 lob
                                                                        28:00
3o!ob
32? 00
•• r —-1	1	1	r	r~
    34:00

-------
                                                                     Paradigm Analytical Labs
Analytical Data Summary Sheet
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ(ND=0)
TEQ (ND=l/2)
Concentration
Wft..
EMPC
ND
ND
EMPC
EMPC
0.0162
0.0030
ND
"tax-'' ' ••
0.0014
EMPC
ND
ND
0.0071
ND
0.0059
0.0016
0.0016
0.0040
0.0080
0.0108
ND
0.0024
0.0072
0.0006
0.0011
BJ,
tt*J
0.0005
0.0003
0.0005
^.0004
0.0004
0.060*
0.0010
&OOQ5
0.0005
,r 0,0004 -».
0.0003
OJ0002
0.0002
0.0003
0.0007
0.0008
0.0008
0,0005
"0.0003
0.0004
0.0004
.0.0005
0.0004
0;0002
0.0007

JWUQ&
^.•.4W-'^
0.0010
0.0069
0.0009
0.0004
0.0034
0.0024
0.0080
0.0092
0.0132
0.0016
0.0032
0.0080
0.0017
0.0020
:.-? »T -. •
_:*j^yia4,..^
28:29
34:43
34:47
35:00
37:11
40:03
27:28
34:11
34:16
34:38
35:10
36:23
40:11



Ratio
1.40
0.29
0,98
0.87
1.1
0.90
0.7
1.39
1.85
1.67
0.78
1.04
1.01



Qualifier



ITEF
ITEF
Client Information

Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:
Texas Lime Kiln
M23-FB-1
L1070
Sample Information

Matrix:
Weight /Volume:
Moisture / Lipids:
Analysis Date:
                                                Air
                                                 I
                                                0,0
                                                                      al7jul98b-12
                                                                      al7jul98b-l
                                         1/2
                                                                                      QLf. 093

-------
                                                                     Paradigm Analytical Labs
                             Analytical Data Summary Sheet
Labeled
Standard
Extraction Standards
13C,2-2,3,7,8-TCDD
13Cl2-l,2,3,7,8-PeCDD
13C12-l,2,3,6,7,8-HxCDD
13C12-1 ,2,3,4,6,7,8-HpCDD
13C12-OCDD
13Ci2-2,3,7,8-TCDF
I3C12-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13Ci2-l,2,3,4,6,7,8-HpCDF
Sampling Standards
37Cl4-2,3,7,8-TCDD
'3C12-2,3,4,7,8-PeCDF
"Cu-l,2,3,4,7,8-HxCDD
13C12-l,2,3,4,7,8-HxCDF
13C12-l)2,3,4,7,8,9-HpCDF
Injection Standards
uCu-lA3,4-TC3)D
l3C12-l,2,3,7,8,9-HxCDD
Expected
Amount" • •
(»B)

4
4
4
4
8
4
4
4
4

4
4
4
4
4



Measured
Amount
(ng)

3.50
4.04
3.78
3.82
6.97
3,53
3.48
3.79
3.01

3.78
3.91
3.61
3.19
3.11



Percent
Recovery
(%)

87.4
100.9
94.6
95.6
87.1
88.2
87.1
94.8
75.2

94.4
97.8
90.2
79.6
77.8



RT
(min.)

28:27
32:37
34:46
37:10
40:02
27:25
31:57
34:15
36:22

28:29
32:25
34:42
34:11
37:32

28:10
34:59
Ratio

0.77
1.56
1.26
1.05
0.89
0.78
1.55
0.52
0.44


1.56
1.24
0.52
0.44

0.79
1.26
Qualifier



















Client Information
Project Name:
Sample ID:

Laboratory Information
Texas Lime Kiln
M23-FB-1
Sample Information

Matrix:
Weight /Volume:
Moisture /Lipids:
Project ID:
Sample ID:
Collection Date:
Receipt Date:
Extraction Date:
Analysis Date: .
, " • ,,*. >v
Reviewed by: j
L1070
1070-3
25-Jun-98
08-JW-98
10-Jal-98
;. ;,. 1H$M?8-
\ .17 '' • - '' '^: .->?.$';;
Filename:
Retchk:
Begin ConCal;
EndConCal:
.,,;,,%,-irr. -'- 'Nti4Cal:
.%-&"Wji?:t:. '.^,-° ' .-
                                                Air
                                                 1
                                                0.0
                                                                      a!7juI98b-12
                                                                      al7juB8b-l
                                                                      al7ju!98b-2
                                                                      a!7jul98b-15
                                                                      m829fl-23-071798
                                                                 Date Reviewed:
                                        2/2
                                                                                          094

-------
o
C£
C/7
OPUSquan 20-JUL-1998 Page 1
Filename al7ju!98b
Sample 12
Acquired 18-JUL-98 01:01:55
Processed 20-JUL-98 09:07:42
Sample ID 1070-3 xl/2
Cal Table m8290-23-071798
Results Table M8290-23-071798B
Comments
Typ
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS
SS
SS
SS
SS
SS
Name; Resp; Ion 1; Ion 2; RA;?; RT;
2,3,7,8-TCDD; 2.94e+05; 5.23e+04; 2.41e+05; 0.22;n; 28:29;
1,2,3,7,8-PeCDD; *; *; * ; *;n;NotFnd;
1,2,3,4,7,8-HxCDD; 1.76e+04; 3.94e+03; 1.36e+04; 0.29;n; 34:43;
1,2,3,6,7,8-HxCDD; 6.966+04; 3.44e+04; 3.52e+04; 0.98;n; 34:47;
1,2,3,7,8,9-HxCDD; 6.67e+04; 3.10e+04; 3.57e+04; 0.87;n; 35:00;
1,2,3,4,6,7,8-HpCDD; 2.61e+05; 1.37e+05; 1.24e+05; 1.10;y; 37:11;
OCDD; 7.766+05; 3.67e+05; 4.08e+05; 0.90;y; 40:03;
2,3,7,8-TCDF; 3.466+05; 1.42e+05; 2.04e+05; 0.70;y; 27:28;
1,2,3,7,8-PeCDF; * ; * ; *; *;n,-NotFnd;
2,3,4,7,8-PeCDF; * ; * ; *; *;n;NotFnd;
1,2,3,4,7,8-HxCDF; 1.18e+05; 6.83e+04; 4.936+04; 1.39,-y; 34:11;
1,2,3,6,7,8-HxCDF; 4.65e+04; 3.02e+04; 1.636+04; 1.85;n; 34:16;
2,3,4, 6,7, 8-HxCDF; 2.31e+04; 1.45e+04; 8.66e+03; 1.67,-n; 34:38;
1,2,3,7,8,9-HxCDF; 1.06e+04; 4.62e+03; 5.94e+03; 0.78;n; 35:10;
1,2,3,4, 6,7, 8-HpCDF; 4.37e+05; 2.22e+05; 2.14e+05; 1.04;y; 36:23;
1,2,3,4,7,8,9-HpCDF; *; * ; *; *;n;NotFnd;
OCDF; 3.03e+05; 1.526+05; 1.51e+05; 1.01,-y; 40:11;
13C-2,3,7,8-TCDD; 3.82e+08; 1.67e+08; 2.15e+08; 0.77;y; 28:27;
13C-l,2,3,7,8-PeCDD; 3.07e+08; 1.87e+08; 1.20e+08; 1.56;y; 32:37;
13C-l,2,3,6,7,8-HxCDD; 3.48e+08; 1.94e+08; 1.54e+08; 1.26;y; 34:46;
13C-l,2,3,4,6,7,8-HpCDD; 2.61e+08; 1.34e+08; 1.27e+08; 1.05;y; 37:10;
13C-OCDD; 3.82e+08; 1.80e+08; 2.02e+08; 0.89;y; 40:02;
13C-2,3,7,8-TCDF; 4.83e+08; 2.12e+08; 2.71e+08; 0.78;y; 27:25;
13C-l,2,3,7,8-PeCDF; 4,15e+08; 2.53e+08; 1.63e+08; 1.55;y; 31:57;
13C-l,2,3,6,7,8-HxCDF; 4.03e+08; 1.37e+08; 2.66e+08; 0.52;y; 34:15;
13C-l,2,3,4,6,7,8-HpCDF; 1.94e+08; 5.97e+07; 1.35e+08; 0.44;y; 36:22;
13C-1,2,3,4-TCDD; 3.98e+08; 1.756+08; 2.22e+08; 0.79;y; 28:10;
13C-l,2,3,7,8,9-HxCDD; 3.43e+08; 1.91e+08; 1.52e+08; 1.26;y; 34:59;
37Cl-2,3,7,8-TCDD; 3.306+08; 3.306+08; -; -;-; 28:29;
13C-2,3,4,7,8-PeCDF; 3.97e+08; 2.42e+08; 1.55e+08; 1.56;y; 32:25;
13C-l,2,3,4,7,8-HxCDD; 2.126+08; 1.176+08; 9.47e+07; 1.24;y; 34:42;
13C-l,2,3,4,7,8-HxCDF; 2.52e+08; 8.586+07; 1.66e+08; 0.52;y; 34:11;
13C-1,2,3,4, 7,8,9-HpCDF; 1.186+08; 3.606+07; 8.226+07; 0 44;y; 37:32;
37Cl-2,3,7,8-TCDD; 3.30e+08; 3.30e+08; -; -,--; 28:29;
13C-2,3,4,7,8-PeCDF; 3.97e+08; 2.426+08; 1.55e+08; 1.56,-y; 32:25;
13C-1.2, 3 , 4, 7, 8-HxCDD; 2.12e+08; 1.17e+08; 9.47e+07- 1 24-y 34-42-
13C-l,2,3,4,7,8-HxCDF; 2.52e+08; 8.58e+07; 1.66e+08; 0.52,-y; 34:11;
13C-l,2,3,4,7,8,9-HpCDF; 1.18e+08; 3.60e+07; 8.22e+07; 0.44;y; 37:32;








Cone ;
0.078;
* .
0.008;
0.023;
0.022;
0.112;
0.404;
0.075;
* .
* .
0.034;
0.011;
0.006;
0.003;
0.178;
it .
0.148;
87.423;
100.876;
94.602;
95.601;
174.250;
88.212;
87.104;
94.834;
75.219;
82.464;
86.455;
82.479;
85.112;
85.426;
76.121;
58.518;
94.398;
97.746;
90.183;
79.631;
77.826;








DL;
0.0122;
0.0080;
0.0125;
0.0099;
0.0098;
0.0105;
0.0240;
0.0122;
0.0115;
0.0111;
0.0064;
0.0051;
0.0059;
0.0068;
0.0169;
0.0204;
0.0200;
0.0457;
0.0268;
0.0316;
0.0291;
0.2296;
0.0225;
0.0111;
0.1568;
0.0536;

-;
0.0219;
0.0113;
0.0469;
0.2012;
0.0685;
0.0261;
0.0077;
0.0490;
0.1787;
0.1170;








S/N1;?;
7,-y;
*;n;
l;n;
7;y;
6;y;
29;y;
36;y;
12; y;
*;n;
*;n;
10;y;
5;y;
2;n;
l;n;
26;y;
*;n;
45;y;
3515;y;
17251;y;
8162 ;y ;
6834;y;
637;y;
11770;y;
46692 ;y;
1653;y;
2222;y;
3867;y;
7930;y;
11127;y;
47310;y;
6286;y;
1118;y;
1187;y;
11127 ;y;
47310;y;
6286;y;
1118;y;
1187;y;
-







S/N2;?
39, -y
*,-n
2;n
5-v
-* ' Jr
4;y
40 ;y
105 ;y
15 ;y
*;n
*;n
H;y
•*• ^ / jr
5;y
2;n
2;n
46;y
^ V 1 Jf
*;n
17, -y
9897,-y
22604;y
10571;y
7219 ;y
30364;y
11292;y
32634;y
2517;y
4153;y
1057 5, -y
10371;y
-< -
33089 ;y
8406;y
1681;y
2232;y
~ 7 ~"
33089;y
8406;y
1681,-y
2232;y
mod?
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
                                                                                                                                                      Page 17

-------
OPUSquan   20-JUL-1998
                   Page 1
                                                                    Page  1  of  8

 Ent  39 Name: Total Tetra-Furans  F:l  Mass:  303.902  305.899  Mod?  no   #Hom:17

 Run: 17 File: a!7ju!98b    S:12 Acq:18-JUL-98 01:01:55 Proc:20-JUL-98  09:07:42
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-3 xl/2
   Amount:  0.36
     Cone:  0.36
   Tox #1:  -
Name
 2,3,7,8-TCDF
of which 0.08
of which 0.08
     Tox #2:  -
named and 0.28
named and 0.28
      Tox #3: -
                   tt     RT Respnse     RA

                   1  23:41 8.3e+04  0.92 n
                            8.3e+04

                   2  24:34 9.6e+04  0.44 n
                            9.6e+04

                   3  24:53 1.5e+05  0.69 y
                            1.5e+05

                   4  25:00 l.le+04  0.60 n
                            l.le+04
                      25:03 1.7e+04
                            1.7e+04

                      25:09 2.6e+04
                            2.6e+04
                                     1.60 n
                  0.38 n
                   7  25:20 1.le+05  0.74 y
                            l.le+05

                   8  25:42 8.2e+04  0.75 y
                            8.2e+04
                      25:46 8.36+04
                            8.3e+04
                                     0.95 n
10 26:00 2.7e+04  0.46 n
         2.7e+04

11 26:09 1.46+05  0.75 y
         1.4e+05

12 26:27 1.4e+05  0.66 y
         1.4e+05

13 26:35 9.8e+04  0.88 y
         9.8e+04

14 26:52 1.8e+05  0.73 y
         1.86+05

15 27:28 3.5e+05  0.70 y
         3.5e+05

16 28:03 4.2e+04  0.41 n
         4.2e+04
                    17  29:49 2.1e+04
                            2.1e+04
                                      0.56 n
          Cone

           0.02
               4
               t
           0.02

               {
           0.03
               e
               6
           0.00
               4
               6
           0.00
               1
               e
           0.01

               ]
           0.02
               4
               (
           0.02

               4
           0.02
               4
               $
           0.01
               E
               1
           0.03
               c
               £
           0.03
               C
               J
           0.02
               4
                C
           0.04

                ]
           0.08
                1

           0.01
                1
                i
           0.00
   unnamed
   unnamed
                                   Area  Height
                                                                      S/N  Mod?
 4.0e+04  9.5e+03 5.1e+00 y  n
 4.3e+04  l.Oe+04 5.4e+00 y  n

 2.9e+04  6.9e+03 3.8e+00 y  n
 6.7e+04  1.4e+04 7.1e+00 y  n

 6.1e+04  1.6e+04 8.5e+00 y  n
 8.8e+04  1.9e+04 9.9e+00 y  n

 4.0e+03  2.1e+03 1.2e+00 n  n
 6.6e+03  1.9e+03 l.Oe+00 n  n
3
 l.le+04  2.5e+03 1.3e+00 n  n
 6.6e+03  1.9e+03 l.Oe+00 n  n
I
 7.3e+03  3.1e+03 1.76+00 n  n
 1.9e+04  4.8e+03 2.4e+00 n  n

  .5e+04  9.2e+03 S.Oe+00 y  n
  .1e+04  9.0e+03 4.6e+00 y  n

 3.5e+04  7.6e+03 4.1e+00 y  n
 4.7e+04  l.Oe+04 5.3e+00 y  n
                                                   4.0e+04 9.3e+03 5.0e+00 y  n
                                                   4.3e+04 l.Oe+04 5.3e+00 y  n
 8.66+03 2.5e+03  1.3e+00 n  n
 1.96+04 5.0e+03  2.6e+00 n  n
3
 5.96+04 1.2e+04  6.3e+00 y  n
 8.0e+04 1.9e+04  9.6e+00 y  n
3
 5.4e+04 l.Oe+04  5.5e+00 y  n
 8.2e+04 1.26+04  6.2e+00 y  n

 4.6e+04 9.0e+03  4.9e+00 y  n
 5.2e+04 1.2e+04  6.2e+00 y  n
4
 7.6e+04 1.4e+04  7.5e+00 y  n
 l.Oe+05 2.1e+04  l.le+01 y  n

 1.4e+05 2.36+04  1.2e+01 y  n
 2.06+05 2.9e+04  1.5e+01 y  n
L
 1.2e+04 4.0e+03  2.2e+00 n  n
 3.0e+04 6.1e+03  3.1e+00 y  n
                                                   7.6e+03 1.7e+03 9.1e-01 n  n
                                                   1.3e+04 5.0e+03 2.6e+00 n  n
                                                                    Page 2 of 8

  Ent:  40 Name: Total Tetra-Dioxins F:l  Mass:  319.897  321.894 Mod? no   #Hom:4
                                                                                                      096

-------
OPUSquan   20-JUL-1998
                   Page 2
 Run: 17 File:  al?jul98b    S:12 Acq:18-JUL-98  01:01:55 Proc:20-JUL-98 09:07:42
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-3 xl/2
   Amount:  0.14
     Cone:  0.14
   Tox #1:  -
Name
of which 0.08
of which 0.08
     Tox #2:  -

#     RT Respnse
named and 0.06
named and 0.06
      Tox #3:  -
                                        RA
2,3,7,8-TCDD
1  25:16 1.46+05  0.83 y
         1.4e+05

2  25:41 5.8e+04  0.56 n
         5.8e+04

3  28:11 2.56+04  1.30 n
         2.5e+04

4  28:29 2.9e+05  0.22 n
         2.9e+05
                                              Cone

                                               0.04
                                                  e

                                               0.02


                                               0.01
                                                  1
                                                  1
                                               0.08
unnamed
unnamed
                  Area  Height
                                                                     S/N  Mod?
               6.1e+04 1.4e+04  8.16+00 y  n
               7.4e+04 1.6e+04  1.2e+01 y  n
              2
               2.1e+04 5.8e+03  3.56+00 y  n
               3.7e+04 7.2e+03  5.3e+00 y  n
              L
               1.4e+04 3.5e+03  2.16+00 n  n
               l.le+04 3.3e+03  2.46+00 n  n
              3
               5.2e+04 l.le+04  6.6e+00 y  n
               2.4e+05 5.3e+04  3.9e+01 y  n
                                                                    Page  3  of  8

 Ent: 41 Name: Total Penta-Furans  F:2  Mass:  339.860 341.857  Mod?  no   #Hom:3

 Run: 17 File: a!7ju!98b    S:12 Acq:18-JUL-98 01:01:55  Proc:20-JUL-98  09:07:42
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-3 xl/2
   Amount: 0.06
     Cone: 0.06
   Tox #1: -
Name
of which *
of which *
     Tox #2: -

#     RT Respnse
named and 0.06
named and 0.06
      Tox #3: -
                                        RA
                   1  31:22 1.66+05  1.86 n
                            1.6e+05

                   2  31:46 4.7e+04  2.68 n
                            4.7e+04

                   3  32:30 2.9e+04  0.78 n
                            2.96+04
          Cone

           0.04
               ]
               C
           0.01

               ]
           0.01
unnamed
unnamed
                                                      Area  Height
                                                                      S/N  Mod?
                                l.Oe+05 2.8e+04 2.56+01 y  n
                                5.4e+04 1.6e+04 4.3e+00 y  n
                               L
                                3.4e+04 l.Oe+04 9.2e+00 y  n
                                1.3e+04 4.9e+03 1.3e+00 n  n

                                1.3e+04 4.6e+03 4.1e+00 y  n
                                1.6e+04 5.0e+03 1.3e+00 n  n
                                                                                                r c
                                                                                 ' 097

-------
OPUSquan
           20-JUL-1998
                   Page  3
                                                                    Page 4  of  8

 Ent: 42 Name: Total Penta-Dioxins F:2  Mass:  355.855  357.852  Mod?  no   #Hom:5

 Run: 17 File: a!7ju!98b    S:12 Acq:18-JUL-98 01:01:55 Proc:20-JUL-98  09:07:42
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-3 xl/2
   Amount:  0.07
     Cone:  0.07
   Tox #1:  -
Name
of which *
of which *
     Tox #2:  -

#     RT Respnse
named and 0.07
named and 0.07
      Tox #3:  -
                                        RA
                   1  31:30 1.2e+05  1.64 y
                            1.2e+05

                   2  32:05 2.2e+04  0.76 n
                            2.2e+04

                   3  32:12 2.56+04  1.15 n
                            2.5e+04

                   4  32:20 2.4e+04  0.76 n
                            2.4e+04

                   5  32:25 5.2e+04  2.69 n
                            5.2e+04
          Cone

           0.04
               -
               4
           0.01
               c
               ]
           0.01
               1
               1
           0.01
               ]
               ]
           0.02
       unnamed
       unnamed
       Area  Height
                                                                      S/N  Mod?
                                7.5e+04  2.6e+04  1.3e+01 y  n
                                4.6e+04  1.7e+04  1.4e+01 y  n
                               L
                                9.3e+03  4.1e+03  2.1e+00 n  n
                                1.2e+04  4.5e+03  3.7e+00 y  n

                                1.3e+04  4.9e+03  2.5e+00 n  n
                                1.2e+04  4.0e+03  3.3e+00 y  n

                                 .le+04  4.4e+03  2.2e+00 n  n
                                 .4e+04  4.3e+03  3.5e+00 y  n

                                3.8e+04  1.3e+04  6.8e+00 y  n
                                1.4e+04  3.9e+03  3.2e+00 y  n
  Ent:  43 Name: Total Hexa-Furans
                                                                    Page 5 of 8

                                   F:3  Mass: 373.821 375.818 Mod? no   #Hom:15
  Run:  17  File: a!7ju!98b    S:12 Acq:18-JUL-98 01:01:55 Proc:20-JUL-98 09:07:42
  Tables:  Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results:  M8290-23»
  Version: V3.5 17-APR-1997  11:14:34  Sample text: 1070-3 xl/2
    Amount:  0.12
      Cone:  0.12
    Tox #1:  -
 Name
of which 0.05
of which 0.05
     Tox #2: -

#     RT Respnse
named and 0.07
named and 0.07
      Tox #3: -
                                        RA
                    1   33:32  4.56+04   0.97 n
                             4.56+04

                    2   33:38  l.le+05   1.30 y
                             l.le+05

                    3   33:55  2.4e+04   2.83 n
                             2.46+04
 1,2,3,4,7,8-HxCDF
    34:11  1.26+05
          1.26+05
  1.39 y
 1,2,3,6,7,8-HxCDF  5
    34:16  4.66+04   1.85 n
          4.6e+04

    34:21  5.56+03   4.41 n
          5.56+03
                    7  34:36 1.9e+04  1.25  y
                             1.9e+04

 2,3,4,6,7,8-HxCDF  8  34:38 2.36+04  1.67  n
                             2.3e+04

                    9  34:44 9.7e+03  5.13  n
                             9.7e+03
Cone

 0.01


 0.03
     (
     <
 0.01
     ]
     e
 0.03
     £
     4
 0.01

     ]
 0.00
     4
     ]
 0.01
     ]
     £
 0.01
     1
     6
 0.00
        unnamed
        unnamed
                                                      Area  Height
                                                                      S/N  Mod?
                                2.2e+04 8.6e+03 4.5e+00 y  n
                                2.3e+04 9.0e+03 6.1e+00 y  n
 j.le+04 2.1e+04  l.le+01 y  n
 l.7e+04 1.8e+04  1.2e+01 y  n

 1.7e+04 6.3e+03  3.3e+00 y  n
 6.16+03 2.46+03  1.66+00 n  n

 j.8e+04 2.0e+04  l.Oe+01 y  n
 1.96+04 1.6e+04  l.le+01 y  n

 3.06+04 9.6e+03  S.Oe+00 y  n
 1.6e+04 6.9e+03  4.6e+00 y  n

 l.5e+03 1.8e+03  9.2e-01 n  n
 L.Oe+03 7.3e+02  4.9e-01 n  n

 l.le+04 3.0e+03  1.6e+00 n  n
 8.7e+03 3.3e+03  2.3e+00 n  n
L
 1.46+04 4.4e+03  2.3e+00 n  n
 8.7e+03 3.36+03  2.3e+00 n  n

 8.1e+03 2.26+03  1.2e+00 n  n
                                                                                                      098

-------
OPUSquan   20-JUL-1998
                                     Page 4
                                                  1.6e+03 5.3e+02 3.6e-01  n n
                   10 34:47  9.56+03  1.48 n    0.00
                            9.5e+03

                   11 35:01  1.2e+04  2.17 n    0.00
                            1.2e+04

                   12 35:06  7.8e+03  0.73 n    0.00
                            7.8e+03

1,2,3,7,8,9-HxCDF  13 35:10  l.le+04  0.78 n    0.00
                            l.le+04

                   14 35:13  l.Se+04  1.65 n    0.00
                            1.6e+04

                   15 35:22  7.0e+03  0.65 n    0.00
                            7.0e+03
 5.7e+03
 3.8e+03
3
 8.36+03
 3.8e+03
D
 3.36+03
 4.56+03
3
 4.6e+03
 5.96+03
3
 9.86+03
 5.96+03
3
 2.8e+03
 4.26+03
2.16+03
7.56+02

1.56+03
l.Oe+03

1.3e+03
l.Se+03

2.06+03
2.36+03

3.2e+03
2.3e+03

1.2e+03
l.le+03
l.le+00 n  n
S.le-01 n  n

7.76-01 n  n
6.9e-01 n  n

7.0e-01 n  n
9.9e-01 n  n

l.Oe+00 n  n
1.6e+00 n  n

1.7e+00 n  n
1.6e+00 n  n

6-le-Ol n  n
7.3e-01 n  n
                                                                                               C<    099

-------
OPUSquan   20-JUL-1998
                   Page  5
                                                                    Page 6  of  8

 Ent: 44 Name: Total Hexa-Dioxins  F:3  Mass:  389.816 391.813 Mod? no   #Hom:ll

 Run: 17 File: al7ju!98b    S:12 Acg:18-JUL-98 01:01:55 Proc:20-JUL-98 09:07:42
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-3 xl/2
   Amount: 0.24
     Cone: 0.24
   Tox #1: -
Name
of which 0.05
of which 0.05
     Tox #2:  -

#     RT Respnse
named and 0.18
named and 0.18
      Tox #3: -
                                        RA
                   1  33:53 1.5e+05  1.39 y
                            1.5e+05
                    2  34:04 4.9e+03
                            4.9e+03
                                     0.52 n
                    3   34:11 1.6e+05  1.50 n
                            1.6e+05
                       34:20 1.5e+05
                            1.5e+05
                  1.33 y
                    5   34:26 2.2e+04  0.77 n
                            2.2e+04
                       34:30  6.1e+03
                             6.1e+03
                                     0.59 n
                    7   34:33  8.5e+03   1.20 y
                             8.5e+03

 1,2,3,4,7,8-HxCDD  8   34:43  1.8e+04   0.29 n
                             1.8e+04
 1,2,3,6,7,8-HxCDD  9
    34:47 7.0e+04  0.98 n
         7.0e+04
 1,2,3,7,8,9-HxCDD  10 35:00 6.7e+04   0.87  n
                             6.7e+04

                    11 35:07 4.2e+03   0.59  n
                             4.2e+03
          Cone

           0.05
               6
               C
           0.00
               3

           0.06
               c
               £
           0.05
               £
               e
           0.01
               c
               3
           0.00

               T
           0.00
               t

           0.01
                1
                3
           0.02


           0.02


           0.00
    unnamed
    unnamed
                                                      Area  Height
                                  S/N  Mod?
 8.8e+04  3.0e+04  1.9e+01 y  n
 6.3e+04  2.4e+04  l.le+01 y  n
3
 1.7e+03  6.4e+02  4.1e-01 n  n
 3.2e+03  1.2e+03  5.4e-01 n  n

 9.3e+04  3.1e+04  2.0e+01 y  n
 6.2e+04  1.5e+04  6.6e+00 y  n

 8.6e+04  2.7e+04  1.7e+01 y  n
 6.5e+04  2.0e+04  8.8e+00 y  n
                                9.5e+03 3.3e+03 2.1e-t-00 n  n
                                1.2e+04 3.4e+03 1.5e+00 n  n
                               D
                                2.3e+03 8.7e+02 5.5e-01 n  n
                                3.8e+03 2.0e+03 9.1e-01 n  n
 4.6e+03 1.5e+03 9.4e-01 n  n
 3.8e+03 2.0e+03 9.1e-01 n  n
L
 3.9e+03 1.9e+03 1.2e+00 n  n
 1.4e+04 4.0e+03 1.8e+00 n  n
2
 3.4e+04 1.2e+04 7.4e+00 y  n
 3.5e+04 l.Oe+04 4.6e+00 y  n
2
 3.1e+04 9.0e+03 5.7e+00 y  n
 3.6e+04 9.9e+03 4.4e+00 y  n
                                1.6e+03 7.0e+02 4.4e-01 n  n
                                2.7e+03 l.le+03 4.7e-01 n  n
                                                                     Page 7  of  8

  Ent: 45 Name: Total Hepta-Furans  F:4  Mass:  407.782 409.779 Mod? no   #Hom:3

  Run: 17 File: a!7ju!98b    S:12 Acq:18-JUL-98 01:01:55 Proc:20-JUL-98 09:07:42
  Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
  Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-3 xl/2
    Amount: 0.21
      Cone: 0.21
    Tox #1: -
 Name
 of which 0.18
 of which 0.18
      Tox #2:  -

 #     RT Respnse
 named and 0.03
 named and 0.03
       Tox #3: -
                                         RA
 1,2,3,4,6,7,8-HpCDFl  36:23 4.4e+05  1.04 y
                             4.4e+05

                    2  36:34 1.8e+04  2.78 n
                             1.8e+04

                    3  36:41 4.4e+04  2.59 n
                             4.4e+04
           Cone

            0.18


            0.01
                3
                4
            0.02
     unnamed
     unnamed
                                                       Area  Height
                                   S/N  Mod?
                                 2.2e+05 7.0e+04 2.6e+01 y  n
                                 2.1e+05 6.7e+04 4.6e+01 y  n
                                L
                                 1.3e+04 5.0e+03 1.9e+00 n  n
                                 4.7e+03 1.8e+03 1.3e+00 n  n

                                 3.2e+04 8.9e+03 3.3e+00 y  n
                                                                                                  <~ff  100

-------
OPUSquan   20-JUL-1998                Page  6
                                                   1.2e+04 4.7e+03 3.3e+00 y  n


                                                                   Page 8 of 8

 Ent: 46 Name: Total Hepta-Dioxins F:4  Mass:  423.777  425.774 Mod? no   fHom:3

 Run: 17 File: al7ju!98b    S:12 Acq:18-JUL-98 01:01:55  Proc:20-JUL-98 09:07:42
 Tables: Run: al7ju!98b  Analyte: m8290-23-»   Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-3 xl/2

   Amount: 0.23    of which 0.11    named and 0.12     unnamed
     Cone: 0.23    of which 0.11    named and 0.12     unnamed
   Tox #1: -            Tox #2:  -         Tox #3:  -

Name               #     RT Respnse     RA    Cone     Area   Height    S/N  Mod?

                   1  36:22 6.5e+04  3.80 n    0.03
                            6.5e+04                5.1e+04  1.6e+04 1.26+01 y  n
                                                   1.4e+04  4.3e+03 5.0e+00 y  n
                   2  36:36 2.1e+05  1.02 y    0.09
                            2.1e+05                l.le+05  3.le+04 2.3e+01 y  n
                                                   l.Oe+05  3.0e+04 3.5e+01 y  n
l,2,3,4,6,7,8-HpCDD3  37:112.6e+05  l.lOy    0.11
                            2.6e+05                1.4e+05  4.0e+04 2.9e+01 y  n
                                                   1.2e+05  3.5e+04 4.0e+01 y  n
                                                                                                       101

-------
o
10
File: A17JUL98B Acq:
18-JUL-1998 01:01:55 Exp : EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #12 Text: 1070-3 xl/2 ALS #12
319.8965 S:12 SMO(1,3)
100S
50J
o:


^v_~^_~_ ^^-~J\
i IT -• ~i 	 1 	 1 	 r
24:00
321.8936 S:12 SMO(1.3)
1001
50 j
.
-
o •




*-
1111(11
24:00
331.9368 S:12 SMO(1,3)
100%
50J
o:



	 24 loo'
333.9339 S:12 SMO(1,3)
100%
50^
o:



24:00
327.8847 S:12 SMO(1,3)
100%
50 1
o:



24 loo'
316.9824 S: 12 SMO(1,3)
100% 23:44 24
50J
0_i


	 1 	 1 	 1 " i • i 	 1 	 r
24:00
BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10% , 1676 . 0 , 1 . 00%, F, F)
A6.13E4 A6.04E4 ,,- ,-,„,
M i .M.J . Z, O £jfz
j\ A2.09E4 A A
/ 1 A / \ A1.43E4/ 1
,^-^'X-~--x^~VNyvJ_X^^A^
1.5E4
.7.5E3
' O.OEO
'25-00' 26 loo' ' ' 27 100 ' ' 28 loo' ' ' ' 29! 00 	 3o!oO Time
BSUB(128, 15, -3 .0) PKD (3, 3, 3, 0.10%,1360.0,1.00%,F,F)
A2.41E5
A

A7.40E4 / \
yy A3^72E4 ^ A1.10E4 A1.10E^_\

5.5E4
_2.7E4


O.OEO
1 1 I I | J 1 r i i I i I i I t J i i 1 i i | i i i i 1 V i , i i T i
25:00 26:00 27:00 28:00 29:00 30:00 Time
BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10%, 9432 . 0 , 1 . 00%, F, F)
A1.75E8
A A
A A
A/V
3.7E7
.1.8E7
O.OEO
25100 26100 27100 28loO 29loO 3oloO Time
BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10%, 4344 . 0 , 1 . 00%, F, F)
A2.22E8
A A
AA

4 . 6E7
.2.3E7
O.OEO
25:00 26:00 27:00 28:00 29:00 30:00 Time
BSUB(128,15,-3.0) PKD (3 , 3 , 3 , 0 . 10%, 6064 . 0, 1 . 00%,F,F)
A3.30E8
A
A
A
6.8E7
L3.4E7
: O.OEO
25:00' ' 26loO 27loO 2sloO 29loO 3oloO Time
PKD(3,3,3,100.00%,0.0,1.00%,F,F)
:1324:34 25:03 25^37 26:10 26:3827:0227^23 27:52 28:26 29:14 29:40 6.3E7



.3 . 1E7
O.OEO
25:00 26:00 27:00 28:00 29:00 30:00 Time

-------





!;
o
co
File: A17JUL98B Acq: 18-JUL-1998 01:01:55 Exp : EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #12 Text: 1070-3 xl/2 ALS #12
355.8546 S:12 F:2 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD{3 , 3 , 3 , 0 . 10%, 1960 . 0, 1 . 00% , F, F)
100% A7.52E4 r_2.8E4
50:
oj
357.
1002
so:
0-
367.
100%
so:
o:
369.
100%
so:
OJ
366.
100%
so:
0'
AA6.92E4 A3.82E4
A A
A8.80E3/ \ -^y V A1.17E4 A1.24E4
361l2 36124 Solie 36148 3ll66 3lll2 31124 31\36 31\48 32166 32112 32124 32136 32l48 33166 33:12
8517 S:12 F:2 SMO(1,3) BSUB(128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1208 . 0 , 1 . 00% , F, F)
A4.58E4
/ \ A2.47E4
/ \ A A1.38E4
36112 36124 36136 36148 3ll66 3ill2 3ll24 31\36 SlUs 32166 32112 32124 32136 32148 33166 33112
8949 S:12 F:2 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3792 . 0, 1 . 00%, F, F)
A1.87E8
f[
36112 36124 36136 36148 3ll66 31112 3ll24 3ll36 31 Us 32166 32ll2 32124 32136 32148 33166 33112
8919 S:12 F:2 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1840 . 0 , 1 . 00%, F, F)
A1.20E8
j[
i i i I i i i i i I i i i i i 1 i i i i i I i i i i -i— i— r- 1 • 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 1 i i i i i 1 i i i i i I i i i i r I i i i~ni 1 I I I I i I i i i i I I i i
3oll2 30124 30136 3oUs 31:00 3lll2 31:24 3ll36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
9792 S:12 F:2 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
30-27 30:47 31:03 31:24 31:37 31:51 32:04 32j25 32:42 32:59

30ll2 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
L1.4E4
O.OEO
Time
1.8E4
19.0E3
O.OEO
Time
6.5E7
L3.3E7
' 0 . OEO
Time
12.1E7
' O.OEO
Time
7.0E7
_3.5E7
O.OEO
Time


-------
File: A17JUL98B Acq: 18-JUL-1998 01:01:bb
Sample #12 Text: 1070-3 xl/2 ALS #12
Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm

389.8156 S:12 F:3 SMO(1,3) BSUB (128 , 15 , -3 . 0 ) PKD(3 , 5, 2 , 0 . 10%, 1572 . 0, 1 . 00%, F,F)
100% A8.79E4 A9.31E4 r_3.2E4

50J


A A
A
/ L /
/ ^ 	 V J
A8.62E4
A A
A A
\ / \ . 4l4Hit4t -* -3 1 OT^A
\ / \ y-\ f\J . J.UIL'i
V \ /\ /\


_1.6E4

O.OEO
33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:48 Time
391.8127 S:12 F:3 SMO(1,3) BSUB (128 , 15 , -3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 2244 . 0 , 1 . 00% , F, F)
100%, A6.31E4


502


2.6E4
A6.50E4
A6.20E4 A
A
^ 	 /
/ \ A3.52E4 A3.57E4
/ \ /\ f\



_1.3E4
O.OEO
33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:48 Time
401.8559 S:12 F:3 BSUB(128, 15 , -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 9328 . 0 , 1 . 00%, F, F)
100%
50J
0 "



33:24 33:36 33:48 34:00 34:
403.8530 S:12 F:3 BSUB(128, 15, -3 . 0) PKD(3,5
100%
so:
0 '



A1.94E8 A1.91E8
A A
M A
I\V / v_
7.6E7
.3.8E7
'O.OEO
L2' ' '34! 24' 34136 34148 3s!oO 3s!l2 35124 35^36 35148 Time
2, 0.10%, 5660. 0,1. 00%, F,F)
f3 A1.52E8
A
A
/ v.
6.0E7
_3.0E7
O.OEO
'33S 24' ' VaSaV ' VsUV ' 's^Sdo' 34ll2 34124 34136 34U'8 35100 35!l2 35J24 35^36 35:48 Time
380.9760 S:12 F:3 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
100% 33:26 33:51 34:10
so:
0"
r

34-29 34j54_ 35:16 35:24 35_ii7 1 . 5E8
•

_7.3E7
O.OEO
'33! 24' ' '33:36' ' ' 33:48' ' '34:0'o' ' '34ll2 ' 34:24' 34136 34:48 35:00 35^12 35:24 35:36 35:48 Time

-------
File: A17JUL98B Acq: 18-JUL-1998 01:01:55
Sample #12 Text: 1070-3 xl/2 ALS #12
423.7767 S:12 F:4 SMO(1,3) BSUB(128, 15, -3 . 0)
lOOi
: A1.05E5
50^ A5.15E4 A
• /v ;V
36166 36112 36124 36136 SeUs 37!
425.7737 S:12 F:4 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
A1.03E5
A
A1.35E4 / \
n- ] ^V 7 V_
36166 36112 36124 36136 36 Us 37!
435.8169 S:12 F:4 SMO(1,3) BSUB(128, 15 , -3 . 0)
100%
so:
0"
36166 36112 36124 36136 36 Us 37 1
437.8140 S:12 F:4 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
so:
0" 	 t
36166 36112 36124 36136 36148 37!
430.9728 S:12 F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%
100% 36:03 36:29 36:56
;/
so:
Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
PKD(3,3,3,0.10%,1372.0,1.00%,F,F)
A1.37E5
/ \ A2.50E4
	 /-A^^^^/x^ , 	 	 	
00 37:12 37:24 37:36 37:48 38:00 3s!l2 38124 38136 3sl48 39!
PKD(3,3,3,0.10%,872.0,1.00%,F,F)
A1.24E5
00 37:12 37:24 37:36 37:48 38100 3s!l2 3sl24 3sl36 3s!48 39
PKD(3,3,3,0.10%,5352.0,1.00%,F,F)
A1.34E8
i i f i i I i iT1^ i 1 l l i i i | i i i i i 1 i i i i i 1 i i i i i 1 i i i i i 1" r~r- 1 i i 1 i i i i i 1 i i i i i '
00 37:12 37:24 37:36 37:48 38:00 38ll2 38124 38136 38148 39
PKD(3,3,3,0.10%,4872.0,1.00%,F,F)
A1.27E8
igm
4.2E4
L2.1E4
00 Time
3 . 6E4
_1.8E4
00 Time
3.7E7
.1.8E7
0 OEO
00 Time
3.5E7
11.8E7
' O.OEO
66 37112 37124 37\36 31^8 38:66 38112 Ss!^ 38136 38!48 39loO Time
,0.0,1. 00%, F,F)
37:18 37:36 37:52 38:22 38:39 38:51 9.7F7

_4.9E7
0 . OF.O
36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24 37136 37:48 38:00 38:12 38:24 38:36 38148 39loO Time
o
C/1

-------
10!
p,
O
File: A17JUL98B Acg: 18-JUL-1998 01:01:55 Exp : EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
Sample #12 Text: 1070-3 xl/2 ALS #12
457.7377 S:12 F:5 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2524 . 0 , 1 . 00%, F, F)
100% A3 . 67E5
so:
o:
459.
100%
50J
o:
469.
100%
so:
0'
471.
100%,
50J
OJ
454.
100%^
so:
OJ

39ll2 39
7348 S:12 F:5 SMO(1,

39:12 39:
7780 S:12 F:5 SMO(1,

39ll2 ' ' ' 39:
7750 S:12 F:5 SMO(1,

39:12 39:
9728 S:12 F:5 SMO(1,
39:07 39:16
'
39:12 39:
JV
24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
3) BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 912 . 0 , 1 . 00%, F, F)
A4.08E5
y\
24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41
3) BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 63476 . 0, 1 . 00%, F, F)
Al . 80E8
f\^
24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
3) BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 1492 . 0 , 1 . 00%, F, F)
A2 . 02E8
f\_
— i — i — i — i — i — 1 — i — i — i — r- • i • i i i i i *i i i i i i i 1 1 i 1 I I I i i i I r | i i i i i | i '•• '
24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
39:27 39:54 40:02 40:13 40:24 40:47

24 39:36 ' ' 39:48 ' 40:00 ' 40:12 40:24 40s36 40:48 41:
igm
9.3E4
L4.7E4
LO.OEO
00 Time
9.8E4
_4.9E4
O.OEO
00 Time
4 . OE7
_2.0E7
_O.OEO
00 Time
4.5E7
.2.3E7
O.OEO
00 Time
.1.1E8
_5.4E7
O.OEO
00 Time

-------
File: A17JUL98B Acq:
18-JUL-1998 01:01:
55 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #12 Text: 1070-3 xl/2 ALS #12
303.9016 S:12 SMO(1,3)
100%,
•
-
50j

I
o-


A4.00E4
*
A
/\
	 f^/^^^~^-J^^-^r 	 J*-^ f-s* — —
24100
305.8987 S:12 SMO(1,3)
1004
-
50 j
'.
o:

A4.33E4
A A2
^— ~^s^-t\^s^^^
	 24!oo'
315.9419 S:12 SMO(1,3)
1004
50J
OJ



24:00
317.9389 S:12 SMO(1,3)
1004
50 1
o"




	 24 loo'
375.8364 S:12 SMO(1,3)
1003i
I
o"

23:24 23:48
oAnA/W^V^V^
	 24 loo'
316.9824 S:12 SMo'(l,3)
100% 23:44 24
50J
o:
r

	 24 loo'
BSUB(128,15,-3.0)

A6.10E4
A
PKD(3,3,3,0.10%,1840.0,1.00%,F,F)
A1.42E5 2.5E4
A
AC Q/IU/I A7.56E4 / \
A2 91E4l\ A4.52E4 ""'A"* A /\
t\£t • -7 JLiJT± It _ „ / \ /\ / \ f\ •. * ri ii n *
* I \ r
y\ A /JW^ATT
/\_^A-\Cv_y--Aa:^a-L
25:00
BSUB(128,15,-3.0)

A8.80E4
A
A6.68E4 A
.75E4A \ ^
^---L~/-Lk, / V^^^^ — ^ — A — ^^^^~^^^__v>^^^r^^_^L^x~^


L1.3E4


: O.ORO
26:00 27:00 2s!oO 29loO 	 3oloO Time
PKD(3,3,3,0.10%,1952.0,1.00%,F,F)
A2.04E5 2.9E4
A7.96E4 A1.03E5 A
A4 65E4 A A8.19E4 /\ / \
'm /\ /^Y\ \ / \ A3'01E4 A1.34E4
\^ 	 ^LA\^_J^L\^J ] \ ^.X-X^^xOky \_ /"^V^^^VVV^^^^^^^^V^^^-N^V^V^^X/

L1.5E4

• n ORO
26 100 27:00 28loO ' 29: 00 ' 30:00 Time
PKD(3,3,3,0.10%,3640.0,1.00%,F,F)
A2.12E8
j[

4.3E7
.2 . 1E7
O.OEO
26:00 27:00 28:00 29:00 30:00 Time
PKD(3,3,3,0.10%,4892.0,1.00%,F,F)
A2.71E8
A
/v
r5.5E7
12.8E7
- O.OEO
I I I | I I i I P | i i i > i | i i i i I | i i i i r i
26:00 27:00 28:00 29:00 30:00 Time
PKD(3,3,3,100.00%,72.0,1.00%,F,F)
28:09 7.0E3
A ^28:37
25:50 26:34 27,J04 27:26 11 /\fl 29:02

_3 .5E3
O.OEO
26 loo 27 loo 28 loo 29! 00 ' ' 30:00 Time
, 0.0,1. 00%, F,F)
25j_37 26:10 26jJ8 27i02 27_L23 27;52 28:26 29_:14 29:40 6.3E7


.3.1E7
O.OEO
26 100 	 27 100 	 28 loo' ' ' ' 29loo' ' ' ' 3oloO Time

-------
    File: A17JUL98BAcq:  18-JUL-1998  01:01:55Exp: EXP_M23_DB5_OVATION Voltage  SIR  EI+GC  Autospec-UltimaEParadigm
    Sample f!2  Text:  1070-3  xl/2  ALS #12
    339.8597 S:12  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1132.0,1.00%,F,F)
                                                                                                                     _3.0E4
UU3
50 j
OJ
rt_L . y_LE.D
A5.36E4 / \ A4.09E4
Z\ _ J \7A8EL, /V//Y_y\
A2.73E4
/V/\ A4.55E3
i.1. 5E4
LO.OEO
          30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00  32:12   32:24  32:36  32:48  33:00  33:12
    341.8568 S:12  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,3732.0,1.00%,F,F)
    100%                                        A5.43E4

      50 J

       OJ
          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 i i i |  i i i i i | i  i
          30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36  31:48  32:00   32:12   32:24  32:36  32:48  33:00  33:12
    351.9000 S:12  F:2  SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,1896.0,1.00%,F,F)
    100%                                                            A2.53E8        A2.42E8

     50 j
  Time

 .1E4

 .1E4

 .OEO
  Time

 OE7

 .5E7

 .OEO
  Time

 .8E7

 .9E7

 .OEO
  Time

 .OE4

 .2E3

 .OEO
  Time

'.OE7

 .5E7

i. OEO
  Time
      0.
                                                                                                                 9.
        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 TT~| I I I I i I  I I I I I I  I I f I I I 'I I  I I I I I I I  I 1 I I 1*1 I  I | I I I I I  | I I I I I |  I I I I I | I  I
          30:12  30:24  30:36  30:48  31:00   31:12  31:24  31:36  31:48  32:00   32:12   32:24  32:36  32:48  33:00  33:12
    353.8970 S:12  F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,1744.0,1.00%,F,F)
    100%,                                                            A1.63E8        A1.55E8
50J
      OJ
                                                                      A
                                                                               T
                                                                                             T
                                                                                                           T
                                                                                                                  T
         3b!i2 ' 3b!24 ' 30 !36 ' 30 Us' ' 31166 ' 3i!i2 ' n!24 ' 31 lie ' 31 Us  32 loo  32ll2   32124  32i36  32i48  33iOO  33112
    409.7974 S:12 F:2 SMO(1,3)  BSUB(128,15,-3.0) PKD(3,3,3,100.00%,3668.0,1.00%,F,F)
    100%,                                                        31^48                       „.„
     50J
                   30:29
           3b!24 '
                                    ' 3l!6d


                                              3l24  3l36  3l48  32o   3
366.9792 S:12 F:2 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
100%          30:27       30:47    31:03 _ 31:24 _ 31:51   32:04
32124 ' 32136 ' 32I48 '  33166 ' 33il2
     50J
                                                                               32:25
                                                                                               32:42     32_L59
         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 | •  .
         30:12  30:24  30:36  30:48  31:00   31:12  31:24  31:36  31:48  32:00   32:12   32:24  32:36  32:48  33:00  33:12
O
00

-------
'Pile: A17JUL98B—Acq:  18-JUL-1998 01:01:55  Exp: EXP_M23_DB5_OVATION Voltage SIR EI+   GC Autospec-UltimaE—Paradigm
Sample #12  Text:  1070-3 xl/2  ALS #12
373.8207 S:12  F:3  SMO(1,3)  BSUB(128,15,-3.0) PKD(3,5,2,0.10%,1912.0,1.00%,F,F)
1004           A6.14E4                 A6.83E4
 50J

  OJ
                                                                                                                   2.2E4
           A2.21E
                            A1.74E4
                        A7.32E
      33:24    33^36    33148    34iOO    34il2    34i24    34i36    34i48    35iOO
375.8178 S:12  F:3  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,1480.0,1.00%,F,F)
100%,           A4.72E4                 A4.93E4

 50J       ^.28E/\
                                                          A8.66E3
                                                             /^xi coin   A4 t
  f\ J        /  \ i   »—.     -	    / \        /_   i •*i-Bv ^"-"-•~'        s<^nj. . JOCiJ   n.1* . •
                                                                                                                    O.OEO
                                                                                                                      Time
                                                                                                                   1.9E4

                                                                                                                   _9.6E3
                                                                                                     A2.33E3
                                                                                                                   .O.OEO
       T
                T


                                                          34! 36  '  '34 Us'
      33:24    33:36    33:48    34:00    34:12    34:24
383.8639 S.-12  F:3 BSUB(128,15,-3 .0)  PKD(3 , 5 , 2 , 0 .10%, 37812 . 0 ,1. 00%, F, F)
100%                                      A1.37E8
 50J

  ol
     I  I I I  I
       T
                 i  r I  i"*i  i i 'i-i i "i i* i*1 TT 1*1 i  f* ijiPiii|
                  35:00   35:12    35:24    35:36    35:48  Time
                                                                                                                   6.3E7

                                                                                                                  _3.1E7
                                                    i i -i i—r—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i
                                         34112    34:24    34:36    34:48    35:00
                                                                                                                   .O.OEO
                         -i—i—i—i—i—i—i—i—i—i—i—i—i—.  i	,
                          35:12    35:24    35:36    35:48  Time

                                                         1.2E8

                                                        _6.1E7
                         T
                                  T
      33:24   33:36    33:48    34:00
385.8610 S:12 F:3 BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,48108.0,1.00%,F,F)
100%                                     A2.66E8
 50
                                                                                                                   0. OEO
                                                                                     35:12    35:24    35:36    35:48  Time
      33:24   33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00
445.7555 S:12 F:3 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,1392.0,1.00%,F,F)
100%                                                              34;46
 50J
       _	!	,	,	,	,	1	,	,	,, . r—,	.
      33:24    33:36    33:48
                                34:00    34:12   34:24
380.9760 S:12 F:3 SMO(1,3)  PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100%,   33_i26__	 _  _ 33:51	34:10	34:29
  I	1	1	T~T	1	1	1	1	1	TT	p
34:36    34:48    35:00
  OJ
                                                                       34:54
                               O.OEO
35!12'  ' '35!24'  ' '35!36'   '35148  Time

   35:16 35:24    35:37        1 . 5E8
     r "r" i—i—r—i—i—i—i—i—r~i—r—T—i—r—i—i—r—i—j—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—r—r—i—i—i—i—i—i—i—r—r—i—i
     33:24    33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00
                                                                                                                  _7.3E7
                                                                                                                  .O.OEO
                                                                                    35:12    35:24    35:36    35:48  Time

-------
     File: A17JUL98BAcq:  18-JUL-1998  01:01:5bExp: EXP_M23_DB5_OVATION Voltage  SIR  EI +GC Autospec-UltimaEParadigm
     Sample #12  Text:  1070-3 xl/2  ALS #12
     407.7818 S:12 F:4  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3 , 3 , 3 , 0 .10% , 2700.0 , 1.00%,F,F)
     1004               A2.22E5
       50J
        0.
                                                                                               7.3E4

                                                                                               _3.7E4
                                   A3.17E4
          r~T i ' i "i i i "l*i i 'i i' i ii i I  i i~T I i 1 I  i i I i I i r~i i i I i- r i" i  i I i i i i i [  (T\ i i I  i i i r- i ji i i i "i I IT*
            36:00  36:12  36:24  36:36  36:48   37:00  37:12  37:24  37:36  37:48  38:00
     409.7788 S:12 F:4 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1444.0,1. 00%, F, F)
     100%               A2.J.4E5
                                                                                                                       O.OEO
       50J
       Oj
                                                                38:12  38:24   38:36  38:48  39:00  Time
                                                                                               6.8E4

                                                                                              _3.4E4
                                   A1.22E4
                                                                A8.20E3
                                                                                               O.OEO
            36!6o ' 36:12 ' 36124 ' 36136  36:48   37:00  37:12  37:24  37:36  37:48  38:00
     417.8253 S:12 F:4 SMO(1,3)  BSUB(128,15,-3.0) PKD(3,3,3,0.10%,8096 . 0,1. 00% , F, F)
     1004               A5.97E7
      50J
       OJ
                                                               A3.60E7
                                                                38:12  38:24  38:36  38:48  39:00  Time

                                                                                               1.8E7

                                                                                              _9.0E6
            i i  i i i i i i i  i i f i i i n i i i i i  i i i i i i i i  i i i i i i i i  i	i  i T i i i | ~ i  i i i i | i  i i i i | T i
            36:00  36:12  36:24  36:36  36:48   37:00  37:12  37:24  37:36  37:48  38:00
     419.8220 S:12 F:4  SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,9748.0,1. 00%, F, F)
     1004               A1.35E8
      50J
       OJ
                                                               A8.22E7
                                                                38:12  38:24  38:36   38:48  39:00  Time

                                                                                               4.1E7

                                                                                               _2 . OE7
          I I l l I  l l l l l I  I I f I l I T~T I I I I I I  l l l I 	 I i i i i i  i i I i I I I  I T I I I I  I I I I I I I  I I I I I I I
            36:00  36:12  36:24  36:36   36:48  37:00  37:12  37:24  37:36  37:48  38:00
     479.7165 S:12 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD{3,3,3,100.00%,4556.0,1.00%,F,F)
     1004                                           37:11                  37;49
                                     36:43
      50 J
36:20 36:31
            36:00  36:12  36:24  36:36  36:48  37:00  37:12  37:24  37:36  37:48  38:00
38:12 ' 38:24  38:36  38:48 '  39:00  Time

                               1.0E4

                               L5.2E3

                              F0.OEO
38:12  38:24  38:36  38:48   39:00  Time
     430.9728 S:12 F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00% , 0 . 0 , 1 . 00%, F, F)
     1004     36:03      ___3fil5 _ 36:48         37:13   37:2737:36    37:52
      50:
                                                                      38:22
                38:39  38:51
            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  36:12  36:24  36:36  36:48  37:00  37:12  37:24  37:36  37:48  38:00
.9.7E7
                                                                                                                      L4.9E7
                                                                                                                       .O.OEO
                                                                38112  ' 38124 '  38136 ' 38I48 ' 39iOO  Time
O

-------
101
File: A17JUL98B AcqrTS"-"JUL-"T998 01. -01
Sample #12 Text: 1070-3 xl/2 ALS #12
441.7427 S:12 F:5 SMO(1,3) BSUB(128,15,
100%
50J
n: ,
39ll2 39i24 39136
443.7398 S:12 F:5 SMO(1,3) BSUB(128,15,
100%
sol
0: 	 	 	
39!l2 39124 39136
469.7780 S:12 F:5 SMO(1,3) BSUB(128,15,
100%
50J
0:
39ll2 39124 39136
471.7750 S.-12 F:5 SMO(1,3) BSUB(128,15,
100%
50 j
0:
39.1 12 39.1 24 39! 36
513.6775 S:12 F:5 SMO(1,3) BSUB(128,15,
100%
sol
\ 39-06 39:16 39:27 39:33
:55 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-ttttimaE Parad
-3.0) PKD(3,3,3,0.10%,804.0,1.00%,F,F)
Al -52 E 5
/ VA1.28E4
39:48 40:00 40:12 40:24 40:36 40:48 41
-3.0) PKD(3,3,3,0.10%,2248.0,1.00%,F,F)
Al . 51E5
39:48 40:00 40:12 40:24 40:36 40:48 41:
-3.0) PKD(3,3,3,0.10%,63476.0,1.00%,F,F)
Al . 80E8
i i i | i i i i *i | r i i l " l | " 1 1 -T ' 1 T~1 1~~ T— -riMi '1 — | 	 p 	 1 i — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	
39:48 40:00 40:12 40:24 40:36 40:48 41
-3.0) PKD(3,3,3,0.10%,1492.0,1.00%,F,F)
A2 .02E8
39U8 40.-00 40.-12 40:24 40:36 40.-48 41
-3.0) PKD(3,3,3,100.00%,84.0,1.00%,F,F)
40:01
39:53 / \
A / \
^ /\V V ^ ^^^T^^^ J^A7 40^l_^46 ^£t
igm
3.7E4
Ll.9E4
00 Time
4.2E4
L2.1E4
00 Time
4.0E7
~^$ uEO
00 Time
4.5E7
L2.3E7
: O.OEO
00 Time
_7.0E3
_3 . 5E3
n nwn
T^T""! P | 1 i i r P | 1 i f>—i i p I 1 • i i i i i i i i i i i i i i r | i I r i I 1 i i I' I l— T-'i — i 	 1 	 1 	 1 — T— T 	 1 	 1 — T* I 	 • 	 ' •""
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41 00 Time
454.9728 S:12 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
100% 39:07 39:16 39:27 39:54 40:02 40:13 40:24 40:47 1 1R«
50J
o:
39.' 12 39124 ' ' 39!36

.5.4E7
n DT?n
1 1 1 | 1 l i i 1 1 1 1 P t 1 | 1 1 1 1 1 1 •!' 1 T— T1"! 	 1 	 1 	 1 	 T 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 f—~ • - — -
39:48 40:00 40:12 40:24 40:36 40:48 41:00 Time

-------
                                                                      Paradigm Analytical Labs
                                        M23-HB-1
                                            PBS
Analytical Data Summary Sheet
. ,/- \ :, Analyte .,,,>,-.« ,
2,3,7,8-TCDD
1,2,3,7,8-PeODD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1A3,4,7»8,9-%CDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ (ND=0)
TEQ (ND=l/2)

0.001 1
;; .._._.:
ND
EMFC
0.0014
0.0031
0.0096
ND
ND
ND
0.0008
ND
ND
ND
0.0030
- , M> ; : - -
0.0028
0.0011
ND
0.0024
0.0032
ND
ND
0.0008
0.0032
0.0014
0.0018
jJlJI$&^tt
0.0005
6.0006
0.0005
0.0005
"6.0605
0.0014
0.0006
0.0004
0.0004
0.0004
0.0003
0.0003
0.0004
0.0005
0.0006
0.0008
o:oo05
0.0004
0.0005
0.0005
0.0006
0.0004
0.0003
0.0005



O.Q048
0.0048

0.0015
0.0018
• , RT -tl
-,'-- (mln.) 'i2
28:28
»~ "32*38,
34:43
"34:4? ";
35:00
37:11
40:03
27:27
34:11
34:15
36:23
40:10

,~

^.-..^i^ftv •
*&••"•••• • ~
0.78
1.41
3.28
"tfcgS;:,
1.11
1.05
0.93
1.08
1.15
1.32
1.00
0.91



Qualifier



ITEF
ITEF
Client Information

Project Name:
Sample ID;

Laboratory Information

Project ID:
Sample ID:

CollectiefcDate;
Receipt Date:
Extraction Date:
Analysis Date:
Texas Lime Kiln
'M23-RB4???:-
                         Sample Information
                                                Air
                                                 1
L1070/^> "''",' -''.,: ^l^'f'^'''.'^-^^.
   Pfe;^':V'§v^%%^'. '"f'/i

   07^98   '   .:'     .
   10-M-98
   18-M-98
                                             al7ju!98b-13
                         Initial Cal:
m829-23-071798
                                         1/2
                                                                                           112

-------
                                            Paradigm Analytical Labs
               Method 23
             M23-RB-1
    Analytical Data Summary Sheet
^"^^y Labeled ^
•«-'?^ii.^W^" -
Extraction Standards
13Ci2-2,3,7,8-TCDD
I3C,2-l,2,3,7,8-PeCDD
13Cl2-l,2,3,6,7,8-HxCDD
13Ci2- 1,2,3,4,6,7,8-HpCDD
13C,2-OCDD
l3C,2-2,3,7,8-TCDF
l3C,2-l,2,3,7,8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
I3C12-l,2,3,4,6,7,8-HpCDF
Sampling Standards
3W2^7,8^CDD
13C12-2,3,4,7,8-PeCDF
SC/rl;24A7,8-HxCDD
13C12-l,2,3,4,7,8-HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
Injection Standards
13Ci2-l,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD

(ng)

4
^? -.$:,. B';.;4
4
4
8
4
4
4
4
-': *'-'4 :;
4
. --^--.w j
4
4



^Jtfeasiired:*
/ 198b-15


                                         Date Reviewed:
               2/2

-------
OPUSquan 20-JUL-1998 Page
Filename al7ju!98b
Sample 13
Acquired 18-JUL-98 01:47:01
Processed 20-JUL-98 09:08:26
Sample ID 1070-4 xl/2
Cal Table m8290-23-071798
Results Table M8290-23-071798B
Comments
TVD Name: Resp;
A j f
Unk
Onk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
cs
cs
cs
cs
cs
ss
ss
ss
ss
ss
2,3,7,8-TCDD; 2.83e+05;
1,2,3,7,8-PeCDD; 1.92e+04;
1,2,3,4,7,8-HxCDD; 2.77e+04;
1,2,3, 6,7, 8-HxCDD; 5.81e+04;
1,2,3,7,8,9-HxCDD; 8.43e+04;
1,2,3,4, 6,7, 8-HpCDD; 1.53e+05;
OCDD; 3.906+05;
2,3,7,8-TCDF; 6.34e+04;
1,2,3,7,8-PeCDF; * ;
2,3,4,7,8-PeCDF; * ;
1,2,3,4,7,8-HxCDF; 6.12e+04;
1,2,3,6,7,8-HxCDF; 3.75e+04;
2,3,4,6,7,8-HxCDF; *;
1,2,3,7,8,9-HxCDF; *;
1,2,3,4,6,7,8-HpCDF; 1.61e+05;
1,2,3,4,7,8,9-HpCDF; *;
OCDF; 1.20e+05;
13C-2,3,7,8-TCDD; 3.44e+08;
13C-1,2,3,7, 8-PeCDD; 2.61e+08;
13C-1 , 2,3,6,7, 8-HxCDD; 2 . 83e+08 ;
13C-l,2,3,4,6,7,8-HpCDD; 2.22e+08;
13C-OCDD; 3.23e+08;
13C-2,3,7,8-TCDF; 4.38e+08;
13C-l,2,3,7,8-PeCDF; 3.54e+08;
13C-l,2,3,6,7,8-HxCDF; 3.43e+08;
13C-1 , 2,3,4,6,7, 8-HpCDF; 1 . 67e+08 ;
13C-1,2,3,4-TCDD; 3.63e+08;
13C-l,2,3,7,8,9-HxCDD; 3.02e+08;
37Cl-2,3,7,8-TCDD; 3.04e+08;
13C-2,3,4,7,8-PeCDF; 3.40e+08;
13C-1 , 2,3,4,7, 8-HxCDD; 2 . 10e+08 ;
13C-1 , 2,3,4,7, 8-HxCDF; 2 . 38e+08 ;
13C-1, 2,3,4,7,8, 9-HpCDF; 1 . 07e+08 ;
37Cl-2,3,7,8-TCDD; 3.04e+08;
13C-2,3,4,7,8-PeCDF; 3.40e+08;
13C-1 , 2,3,4,7, 8-HxCDD; 2 . 10e+08 ;
13C-l,2,3,4,7,8-HxCDF; 2.38e+08;
13C-l,2,3,4,7,8,9-HpCDF; 1.07e+08;
1









4.
1.
2.
3.
4.
7.
1.
3.


3.
2.


8.

5.
1.
1.
1.
1.
1.
1.
2.
1.
5.
1.
1.
3.
2.
1.
8.
3.
3.
2.
1.
8.
3.









Ion 1;
15e+04;
12e+04;
13e+04;
62e+04;
44e+04;
85e+04;
87e+05;
30e+04;
+ .
* .
27e+04;
14e+04;
* .
* .
Ole+04;
* .
69e+04;
51e+08;
59e+08;
58e+08;
14e+08;
51e+08;
92e+08;
16e+08;
18e+08;
13e+07;
60e+08;
68e+08;
04e+08;
08e+08;
16e+08;
10e+07;
26e+07;
04e+08;
08e+08;
16e+08;
10e+07;
266+07;










2.
7
6.
2
3
7
2
3


2
1


8

6
1
1
1
1
1
2
1
2
1
2
1

1
9
1
7

1
9
1
7









Ion 2;
41e+05;
97e+03;
48e+03;
19e+04;
99e+04;
44e+04;
02e+05;
04e+04;
* .
* .
85e+04;
61e+04;
* .
it .
05e+04;
* .
28e+04;
93e+08;
02e+08;
25e+08;
08e+08;
72e+08;
46e+08;
386+08;
25e+08;
16e+08;
03e+08;
34e+08;

33e+08;
41e+07;
57e+08;
43e+07;

33e+08;
416+07;
57e+08;
43e+07;









RA;?; RT;
0.17,-n; 28:28;
1.41;y; 32:38;
3.28;n; 34:43;
1.65;n; 34:47;
l.ll;y; 35:00;
1.05;y; 37:11;
0.93;y; 40:03;
1.08;n; 27:27;
* ;n;NotFnd;
*;n;NotFnd;
1.15;y; 34:11;
1.32;y; 34:15;
*;n;NotFnd;
*,-n;NotFnd;
1.00;y; 36:23;
*;n;NotFnd;
0.91;y; 40:10;
0.78;y; 28:27;
1.56;y; 32:37;
1.26;y; 34:46;
1.06;y; 37:10;
0.88,-y; 40:02;
0.78;y; 27:26;
1.56;y; 31:57;
0.52;y; 34:15;
0.44;y; 36:22;
0.79;y; 28:10;
1.25;y; 34:59;
-;-; 28:28;
1.57,-y; 32:24;
1.23;y; 34:42;
0.52;y; 34:11;
0.44,-y; 37:32;
-,--; 28:28;
1.57,-y; 32:24;
1.23;y; 34:42;
0.52;y; 34:11;
0.44;y; 37:32;









Cone ;
0.084;
0.007;
0.015;
0.024;
0.035;
0.077;
0.241;
0.015;
* .
* .
0.021;
0.010;
* .
* .
0.076;
* .
0.069;
86.342;
94.107;
87.419;
92.327;
167.134;
87.672;
81.511;
91.739;
73.664;
75.191;
76.109;
83.199;
79.976;
96.382;
81.509;
60.110;
96.414;
98.151;
110.111;
88.145;
81.631;









DL;
0.0114;
0.0105;
0.0156;
0.0123;
0.0122;
0.0112;
0.0351;
0.0152;
0.0091;
0.0088;
0.0089;
0.0070;
0.0082;
0.0094;
0.0126;
0.0152;
0.0190;
0.0487;
0.0273;
0.0430;
0.0276;
0.0208;
0.0241;
0.0144;
0.1787;
0.0977;
-;
~ /
0.0202;
0.0148;
0.0639;
0.2293;
0.1249;
0.0238;
0.0105;
0.0670;
0.2151;
0.2158;









S/N1;?;
6;y;
2;n;
3;n;
5;y;
5;y;
19;y;
14, -y;
5;y;
*;n;
*;n;
4;y;
4;y;
*;n;
*;n;
15;y;
*;n;
15, -y, •
3589;y;
17216;y;
6066;y;
5293;y;
13121;y;
8853;y;
43021;y;
1389;y;
3242;y;
3900;y;
5940;y;
12478;y;
42528;y;
4471;y;
1039;y;
1790;y;
12478;y;
42528;y;
4471;y;
1039;y;
1790;y;









S/N2 ; ?
34, -y
3;n
2;n
4;y
6;y
28;y
46 ;y
3;n
*;n
*;n
7;y
3;n
*;n
*;n
27,-y
*;n
10 ;y
8202 ;y
19494;y
7523 ;y
10514 ;y
15246;y
13263;y
19577;y
2083 ;y
1476;y
8653;y
7373 ;y
-; -
19472 ;y
5760;y
1526;y
827, -y
-; -
19472,-y
5760;y
1526 ;y
827, -y
mod?
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
Page 18

-------
OPUSquan   20-JUL-1998                Page 1
                                                                   Page  1 of  8

 Ent: 39 Name: Total Tetra-Furans  F:l  Mass:  303.902  305.899  Mod? no   #Hom:l

 Run: 18 File: al7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98 09:08:26
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2

   Amount: 0.02    of which 0.02    named and *       unnamed
     Cone: 0.02    of which 0.02    named and *       unnamed
   Tox #1: -            Tox #2:  -         Tox #3:  -

Name               #     RT Respnse     RA    Cone     Area  Height    S/N Mod?

2,3,7,8-TCDF       1  27:27 6.36+04  1.08 n    0.02
                            6.36+04                3.36+04 7.7e+03 4.7e+00 y   n
                                                   3.0e+04 7.7e+03 2.9e+00 n   n


                                                                   Page  2 of  8

 Ent: 40 Name: Total Tetra-Dioxins F:l  Mass:  319.897  321.894  Mod? no   #Hom:2

 Run: 18 File: a!7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98 09:08:26
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2

   Amount: 0.09    of which 0.08    named and 0.01     unnamed
     Cone: 0.09    of which 0.08    named and 0.01     unnamed
   Tox #1: -            Tox #2:  -         Tox #3:  -

Name               #     RT Respnse     RA    Cone     Area  Height    S/N Mod?

                   1  25:16 2.4e+04  1.67 n    0.01
                            2.4e+04                1.5e+04 3.3e+03 2.6e+00 n   n
                                                   8.8e+03 2.7e+03 2.0e+00 n   n
2,3,7,8-TCDD       2  28:28 2.8e+05  0.17 n    0.08
                            2.8e+05                4.1e+04 6.9e+03 5.6e+00 y   n
                                                   2.4e+05 4.5e+04 3.4e+01 y   n


                                                                   Page  3 of  8

 Ent: 41 Name: Total Penta-Furans  F:2  Mass:  339.860  341.857  Mod? no   #Hom:4

 Run: 18 File: a!7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98 09:08:26
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2

   Amount: 0.02    of which *       named and 0.02     unnamed
     Cone: 0.02    of which *       named and 0.02     unnamed
   Tox #1: -            Tox t2:  -         Tox #3:  -

Name               #     RT Respnse     RA    Cone    Area  Height     S/N Mod?

                   1  31:23 2.2e+04  1.35 y    0.01
                            2.2e+04                1.3e+04 3.6e+03 3.7e+00 y   n
                                                   9.4e+03 2.8e+03 1.2e+00 n   n
                   2  32:31 1.7e+04  1.13 n    0.01
                            1.7e+04                9.06+03 2.9e+03 3.0e+00 n   n
                                                   7.9e+03 2.06+03 8.56-01 n   n
                   3  32:57 1.3e+04  0.27 n    0.00
                            1.3e+04                2.8e+03 1.2e+03 1.2e+00 n   n
                                                   l.Oe+04 4.3e+03 1.9e+00 n   n
                   4  33:01 1.3e+04  0.28 n    0.00
                            1.3e+04                2.96+03 l.le+03 l.le+00 n   n
                                                   l.Oe+04 4.36+03 1.9e+00 n   n
                                                                    Page 4 of 8
                                                                                                        us

-------
OPUSguan   20-JUL-1998
                                      Page 2
 Ent: 42 Name: Total Penta-Dioxins F:2  Mass:  355.855  357.852 Mod? no   #Hom:3

 Run: 18 File: al7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98 09:08:26
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2
   Amount: 0.03
     Cone: 0.03
   Tox #1: -
Name
1,2,3,7,8-PeCDD
of which 0.01
of which 0.01
     Tox #2:  -
named and 0.03
named and 0.03
      Tox #3: -
                         RT Respnse
                                        RA
                      31:57 3.8e+04  3.76 n
                            3.8e+04

                      32:24 4.1e+04  7.00 n
                            4.le+04
3  32:38 1.9e+04  1.41 y
         1.9e+04
          Cone

           0.01

               £
           0.01

               c
           0.01
    unnamed
    unnamed
                                   Area   Height     S/N  Mod?
 3.0e+04  9.3e+03  4.0e+00  y  n
 8.16+03  3.5e+03  2.7e+00  n  n
L
 3.6e+04  1.2e+04  5.3e+00  y  n
 5.1e+03  2.0e+03  1.5e+00  n  n
1
 1.le+04  3.7e+03  1.6e+00  n  n
 8.0e+03  3.8e+03  2.9e+00  n  n
 Ent: 43 Name: Total Hexa-Furans
                                                 Page  5  of  8

                F:3  Mass:  373.821  375.818 Mod? no   #Hom:3
 Run: 18 File: a!7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98  09:08:26
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2
   Amount:  0.04
     Cone:  0.04
   Tox #1:  -
of which 0.03
of which 0.03
     Tox #2:  -
named and 0.01
named and 0.01
      Tox #3: -
    unnamed
    unnamed
Name
                         RT Respnse
                                        RA
                   1  33:38 2.0e+04  1.23 y
                            2.0e+04

1,2,3,4,7,8-HxCDF  2  34:11 6.le+04  1.15 y
                            6.le+04

1,2,3, 6,7,8-HxCDF  3  34:15 3.8e+04  1.32 y
                            3.8e+04
                           Cone

                            0.01
                                ]
                                c
                            0.02


                            0.01
                  Area  Height
                    S/N  Mod?
               1.le+04 4.3e+03 1.8e+00 n  n
               9.1e+03 4.06+03 2.6e+00 n  n
              I
               3.3e+04 l.Oe+04 4.5e+00 y  n
               2.8e+04 l.Oe+04 6.6e+00 y  n
              1
               2.le+04 8.3e+03 3.6e+00 y  n
               1.66+04 4.4e+03 2.8e+00 n  n
                                                                                                 C<   116

-------
OPUSquan   20-JUL-1998
                                      Page 3
                                                                    Page 6 of 8

 Ent: 44 Name: Total Hexa-Dioxins  F:3  Mass: 389.816 391.813 Mod? no   #Hom:12

 Run: 18 File: al7ju!98b    3:13 Acq:18-JUL-98 01:47:01 Proc:20-JUL-98 09:08:26
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results:  M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-4 xl/2
   Amount: 0.21
     Cone: 0.21
   Tox #1: -
of which 0.07
of which 0.07
     Tox #2: -
named and 0.14
named and 0.14
      Tox #3: -
Name
                         RT Respnse     RA

                                     0.90 n
   33:53 3.6e+04
         3.6e+04
                   2  33:59 2.16+03
                            2.1e+03
                  0.40 n
                   3  34:06 6.1e+03  4.17 n
                            6.1e+03

                   4  34:11 9.4e+04  2.47 n
                            9.4e+04

                   5  34:15 6.8e+04  5.10 n
                            6.86+04

                   6  34:20 7.06+04  1.35 y
                            7.0e+04
                   7  34:24 9.1e+03
                            9.1e+03
                  0.81 n
                   8  34:28 l.le+04  1.03 n
                            l.le+04

                   9  34:31 l.le+04  1.07 y
                            l.le+04

1,2,3,4,7,8-HxCDD  10 34:43 2.86+04  3.28 n
                            2.8e+04

1,2,3,6,7,8-HxCDD  11 34:47 5.8e+04  1.65 n
                            5.86+04

1,2, 3,7,8,9-HxCDD  12 35:00 8.46+04  1.11 y
                            8.4e+04
          Cone

           0.02
               ]
               1
           0.00
               I
               1
           0.00
               c
               1
           0.04
               £

           0.03
               c
               ]
           0.03
               t,

           0.00
               4
               C
           0.00
               c
               c
           0.00
               c
               c
           0.01

               6
           0.02


           0.03
    unnamed
    unnamed
                                   Area  Height
                    S/N  Mod?
  .7e+04 6.6e+03 2.9e+00 n  n
  .9e+04 7.3e+03 4.0e+00 y  n

 6.16+02 3.6e+02 1.6e-01 n  n
 1.5e+03 6.2e+02 3.4e-01 n  n
 5.06+03 1.26+03 5.1e-01 n  n
 1.2e+03 7.2e+02 3.9e-01 n  n
1
 6.7e+04 2.36+04 9.8e+00 y  n
 2.7e+04 9.1e+03 5.0e+00 y  n
3
 5.7e+04 1.9e+04 8.4e+00 y  n
 l.le+04 4.0e+03 2.2e+00 n  n
3
 4.0e+04 1.26+04 5.4e+00 y  n
 3.0e+04 8.9e+03 4.9e+00 y  n

 4.1e+03 1.8e+03 8.0e-01 n  n
 S.Oe+03 1.6e+03 8.7e-01 n  n
D
 5.3e+03 2.0e+03 8.7e-01 n  n
 5.2e+03 1.7e+03 9.6e-01 n  n
D
 5.6e+03 1.9e+03 8.4e-01 n  n
 5.2e+03 1.76+03 9.6e-01 n  n
1
 2.1e+04 5.8e+03 2.5e+00 n  n
 6.5e+03 3.1e+03 1.7e+00 n  n
2
 3.6e+04 l.le+04 4.7e+00 y  n
 2.2e+04 7.0e+03 3.9e+00 y  n
3
 4.4e+04 l.le+04 4.7e+00 y  n
 4.0e+04 l.le+04 5.8e+00 y  n
                                                                    Page 7 of 8

 Ent: 45 Name: Total Hepta-Furans  F:4  Mass:  407.782 409.779 Mod? no   #Hom:l

 Run: 18 File: al7jul98b    S:13 Acq:18-JUL-98 01:47:01 Proc:20-JUL-98 09:08:26
 Tables: Run: al7ju!98b  Analyte: ro8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2
   Amount: 0.08
     Cone: 0.08
   Tox #1: -
Name
of which 0.08
of which 0.08
     Tox #2:  -

#     RT Respnse
named and *
named and *
      Tox #3:  -
                                        RA
1,2,3,4,6,7,8-HpCDFl  36:23 1.6e+05  1.00 y
                            1.6e+05
                           Cone

                            0.08
    unnamed
    unnamed
                                                      Area  Height    S/N  Mod?
                                                   8.0e+04 2.6e+04 1.5e+01 y  n
                                                   S.Oe+04 2.6e+04 2.7e+01 y  n
                                                                                                      117

-------
OPUSquan   20-JUL-1998
                   Page 4
                                                                   Page 8 of 8

 Ent: 46 Name: Total Hepta-Dioxins F:4  Mass:  423.777  425.774 Mod? no   #Hom:5

 Run: 18 File: a!7ju!98b    S:13 Acq:18-JUL-98 01:47:01  Proc:20-JUL-98 09:08:26
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3 . 5 17-APR-1997 11:14:34  Sample text:  1070-4 xl/2
   Amount: 0.15
     Cone: 0.15
   Tox #1: -
Name
of which 0.08
of which 0.08
     Tox #2:  -

#     RT Respnse
named and 0.07
named and 0.07
      Tox #3:  -
                                        RA
                   1  36:22 3.4e+04  6.09 n
                            3.4e+04

                   2  36:35 7.7e+04  1.21 n
                            7.7e+04

                   3  36:42 8.1e+03  0.74 n
                            8.1e+03

l,2,3,4,6,7,8-HpCDD4  37:11 1.5e+05  1.05 y
                            1.5e+05

                   5  37:32 3.0e+04  4.70 n
                            3.0e+04
          Cone

           0.02

               4
           0.04
               t,

           0.00

               4
           0.08


           0.02
unnamed
unnamed
                                                     Area  Height
                                                                     S/N  Mod?
                                2.9e+04  9.1e+03 7.7e+00 y  n
                                4.8e+03  1.8e+03 2.3e+00 n  n

                                4.2e+04  1.2e+04 l.Oe+01 y  n
                                3.5e+04  l.Oe+04 1.3e+01 y  n
                               3
                                3.4e+03  1.3e+03 l.le+00 n  n
                                4.7e+03  1.3e+03 1.6e+00 n  n
                               3
                                7.9e+04  2.3e+04 1.96+01 y  n
                                7.4e+04  2.2e+04 2.8e+01 y  n
                               2
                                2.5e+04  6.1e+03 5.1e+00 y  n
                                5.2e+03  2.1e+03 2.6e+00 n  n
                                                                                                        118

-------
File: A17JUL98B Acq: 18-JUL-199«
Sample #13 Text: 1070-4 xl/2 ALS
319.8965 S:13 SMO{1,3) BSUB(128,15
100%
50 J
-
o-



^^^^~s^^^^^~^^~^^v
"-1 — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 r— — i —
24:00 25
321.8936 S:13 SMO(1,3) BSUB(128,15
100%
50 1
'•
0




24:00 25
331.9368 S:13 SMO(1,3) BSUB(128,15
100S
50 1
o"



24:00 25
333.9339 S:13 SMO(1,3) BSUB(128,15
100%
50J
o •



"— ' — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
327.8847 S:13 SMO(1,3) BSUB(128,15
100%
50 j
0 '



u— ' — i 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 —
24:00 25
01:47:01 Exp: EXP M23
#13
,-3.0) PKD(3,3,3,0.10%


A1.47E4
A ^,.
100 26:00
,-3.0) PKD(3,3,3,0.10%


A8.80E3

loO ' 26:00
,-3.0) PKD(3,3,3,0.10%



loo' ' ' 2eloo
,-3.0) PKD(3,3,3,0.10%



1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 r—
:00 26:00
,-3.0) PKD(3,3,3,0.10%



100 26:00
_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm

,1248.0,1.00%,F,F)
A6.60E4
A
\ A4.15E4
/ \ r\
r^^-s^-s^xJ----^^^ ^-v^~~__^-~^~W~\~
1.5E4
_7.7E3

O.OEO
27loO 28loO 29100 3oloO Time
,1328.0,1.00%,F,F)
A2.41E5
A
A
/ \
	 	 , 	 _. - 	 	 ' V 	 	
4.6E4
_2.3E4

O.OEO
27loO 28loO 29loO 30:00 Time
,8376.0,1.00%,F,F)
A1.60E8
A A
A A
A A
3.3E7
11.6E7
•O.OEO
27:00 28:00 29:00 30:00 Time
,4732.0,1.00%,F,F)
A2.03E8
A A
A
A A
4.1E7
L2.1E7
VO.OEO
27loO 28100 29IOO 30:00 Time
,4996.0,1.00%,F,F)
A3.04E8
A
A
A
6.2E7
L3.1E7
O.OEO
27:00 28:00 29:00 30:00 Time
316.9824 S:13 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
100% 23:26 23:55 24:3724
50J
o-


	 24 !00 	 25
:5925:20 25:43


loo' ' ' ' 26 loo'
26:3626^56 27^27 27:51 28:2728^47 29_Lll 29:39 6 . 1E7


_3.0E7
O.OEO
27loO 28100 29:00 3oloO Time
CD

-------
File: A17JUL98B  Acq: 18-JUL-1998 01:47:01Exp:  EXP_M23_DB5_OVATION Voltage SIR EI+GC  Autospec-UltimaEParadigm
Sample  #13   Text: 1070-4 xl/2  ALS #13
355.8546  S:13 F:2 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,2324.0,1.00%,F,F)
100%                                                                            A3.5.5E4                            1.5E4
  so:
                                                                                                              7.4E3



                                     | 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 i1 " • UJ1U
30:12  30:24  30:36  30:48  31:00  31:12   31:24   31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00   33:12     Time
357.8517 S:13 F:2 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1280.0,1.00%,F,F)
100%.
                                                                  A1.38E4

 so:
                                                                                        A7 .97E3
                                                                                                              6.0E3
                                                                                                                  _3.0E3
                                                                                                                   O.OEO
     ~i—i—|—i—i—i—i—i—1—i—i—i—i—i—|—i—i—i—i—i—|—i—i—r—i—i—i—i—i—r—i—i—r—r—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—r—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—r~r~|—i—i—m—
      30:12   30:24   30:36  30:48  31:00  31:12  31:24   31:36   31:48   32:00  32:12  32:24  32:36  32:48  33:00  33:12    Time
367.8949 S:13  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,3272.0,1.00%,F,F)
100%
 50J
                                                                                        A1.59E8
                                                                                                             12.8E7
                                                                                                                   .O.OEO
     30:12  30:24  30:36  30:48  31:00  31:12  31:24  31:36   31:48  32:00  32:12  32:24  32:36 ' 32148 ' 33166 ' 33112    Time
369.8919 S:13  F:2  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1856.0,1.00%,F,F)
100%
 so:
  0.
                                                                                  Al.02E8
30:12  30:24  30:36  30:48  31:00   31:12  31:24
                                                                                                                  ,_3 . 6E7
                                                                                                             _1.8E7
                                                                                                            JLO.OEO
                                                                   32:    32!i2 ' 32!24 ' 32S361 ' 32:48  33:00  33:12    Time
366.9792 S:13 F:2 SMO(1,3)  PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100%,      30:20        30:42     31:00      31:19  31j32_U^J7___3!jL04	32_l25_
 so:
                                                                                                              6.6E7
                                                                                                             .3.3E7
                                                                                                                   .O.OEO
     ~i~t i—i—i—i—i—i—i—i—i—i—r "T • i—r r -1—i—i—i—i—i—i—i—i—i—i—i—r—i—i—|—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—r -T -i1 'i—i—i—r—i—r—i—i—i—i—i—i—i—i—(—i—i—i—i—i—r-i—i—i—r—i—i—i—i—i—i—t T i i i  i—r—T—i—i—r
     30:12  30:24  30:36  30:48  31:00   31:12   31:24   31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00   33:12     Time

-------
10
   File: A17JUL98BAcq: 18-JUL-1998 01:47:01Exp: EXP_M23_DB5_OVATION Voltage SIR EI +GC Autospec-UltimaEParadigm
   Sample #13  Text: 1070-4 xl/2  ALS #13
   389.8156 S:13 F:3 SMO(1,3) BSUB(128,15,-3.0) PKD(3,5,2,0.10%,2304.0,1.00%,F,F)
   100%,                                  A6.70E4
    so:
                                                                                                                  2.3E4


                                                                                                                 L1.2E4


                                                                                                                  O.OEO
      33:24   33:36    33:48    34:00    34il2    34i24    34:36    34i48    35:00    35:12    35:24    35:36    35:48  Time
391.8127 S:13 F:3 SMO(1,3)  BSUB(128,15,-3.0) PKD(3,5,2,0.10%,1824.0,1.00%,F,F)
   100%,
    so:
                                                                          A3.99E4
         33:24    33:36    33:48    34:00    34:12    34:24   34:36    34:48    35:00
                                                                                    35:12
   401.8559 S:13 F:3 BSUB(128,15,-3.0) PKD(3,5,2,0.10%,10884.0,1.00%,F,F)
   100%                                                           A1.58E8   A1.68E8
    50J
                                                1.1E4


                                               _5.7E3


                                                O.OEO
                          35124    35136    35i48  Time

                                              ,.6. 6E7
                                                                                                                 _3.3E7
        33:24    33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00
   403.8530 S:13 F:3 BSUB(128,15,-3.0) PKD(3,5,2,0.10%,6960.0,1.00%,F,F)
   lOOi                                                           A1.25E8   A1.34E8
    50J
                                                                                    35:12    35:24    35:36
      33:24    33:36    33:48    34:00   34:12    34:24   34:36
380.9760 S:13 F:3 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100% 33:23             33:47            	3j:19	34:38 34_:47
34:48    35:00
35:12    35:24    35:36
    so:
                                                                                                     35^2
                                                                                                                    .O.OEO
                                           35:48  Time

                                               5.2E7


                                               _2.6E7
                                                                                                                    O.OEO
                                                                                                                35:48  Time
     T	I	]	1—1	1—I	1	1	1	1	1	1	1	1	1	1	1	1	1	1™1	1	1	1	1	1	1	1	1	1	1	1	I	1	1	1	1	I	1	1	1	1	1	1	1	1	1	1	1	1	1	F
     33:24    33:36    33:48    34:00   34:12    34:24    34:36    34:48    35:00
                 '35! 12
                                                                                                                 _7.2E7
                                                                                                                    O.OEO
        i i  I i  i i  i i  I	I
         35:24    35:36    35:48  Time

-------
File: A17JUL98B
Sample #13 Text
423.7767 S:13 F:
100%
so:
o:
425.
100%:
so:
o:
435.
100%|
so:
o:
437.
so:
o:
430.
100%
50J
01


36:00 36
7737 S:13 F:


36:00 36
8169 S:13 F:

36:00 36
8140 S:13 F:

Aca: 18-JUL-1998 01:47:01 Exp : EXP M23 DBS
: 1070-4 xl/2 ALS #13
4 SMO(1,3) BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%
A7 . 85E4
A4.21E4
^L\_ y v_^ _
:12 36:24 36:36 36:48 37:
4 SMO(1,3) BSUB(128,15,-3.0)
A3.47E4
.65E3 _
..^^•^•N, / \ ^-—^^f
•12 36124 36:36 36:48 37:
4 SMO(1,3) BSUB(128,15,-3.0)

1 1 1 1 1 1 1 1 1 1 1 ' T \- 1 I I I 1 I 1 1 I 1 1 |
!l2 36124 36:36 36:48 37:
4 SMO(1,3) BSUB(128,15,-3.0)

1 l 1 l l 1 1 1 1 1 1 1 1 l l 1 l 1 1 1 l l *I~f l r I I I | I I i I I |
36lOD 36ll2 36:24 36:36 36:48 37:
9728 S:13 F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%
35:56 36:09 36:19 36:31 36:46 36:55
y 	

36166 ' 36


i i i i i i i i i i T-T i 	 l ' ' ' ' ' I
!l2 36124 36:36 36:48 37:
\ A2
/ W.15E3 .
00 37:12 37:24
PKD(3,3,3,0.10%
A7 . 44E4
A
/ V A5
00 37:12 37:24
PKD(3,3,3,0.10%
Al . 14E8
/I
i i i' i i 1 i i i i i 1 i i
00 37:12 37:24
PKD(3,3,3,0.10%
Al . 08E8
j[
00 37:12 37:24
, 0.0,1. 00%, F,F)
37:11 37


00 37112 37124
_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parada
, 1184.0, 1.00%,F,F)
.46E4
/ \^ ^ 	 ^ 	 	 	
37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:
,796.0,1.00%,F,F)

.24E3
' 37136 37148 38!6d 38112 38124 38:36 SsUs 391
,5712.0,1.00%,F,F)

37l36 37:48 Sslod 38112 38124 38\36 SsUs 39!
,2768.0,1.00%,F,F)

.gm
_2.4E4
_1.2E4
" O.OEO
00 Time
_2.3E4
_1.1E4
' O.OEO
00 Time
_3.0E7
_1.5E7
O.OEO
00 Time
2 . 9E7
_1.5E7
_O.OEO
37136 37:48 Sslod 38112 38124 38:36 38:48 39:00 Time
:29 37i40 37:50 38:02 38:13 38:26 38:47 p9.4E7



_4.7E7
.O.OEO
37136 37148 38l6d 38:12 38:24 38:36 38:48 39:00 Time
JO

-------
101
File
Samp
457.
1002
so:
0"
459.
100S
so:
469.
100%
so:
0"
471.
lOOi
so:
0"
454.
100%
so:
0'
>: A17JUL98B Acq: 18-JUL-1998 01:47:01 Exp: EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
>le #13 Text: 1070-4 xl/2 ALS #13
7377 S:13 F:5 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3224 . 0 , 1 . 00% , F, F)
A1.87E5
39ll2 39124 39136 39U8 4o!ob 4o!l2 4o!24 ' ' ' 4ol36 ' ' ' 4o!48 41
7348 S:13 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 1048 . 0, 1 . 00%, F, F)
A2 . 02E5
J \ 	 A5_.J9E3
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41
7780 S:13 F:5 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2608 . 0, 1 . 00%, F, F)
Al -51 E 8
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41
7750 S:13 F:5 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2528 . 0, 1 . 00%, F, F)
Al . 72E8
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
9728 S:13 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
39:09 39:18 39:24 39:33 39:44 40:0540:10 40:25 40:3540:41 40:49 40:56
r
5.0E4
_2.5E4
00 Time
4.9E4
_2.4E4
00 Time
3.4E7
_1.7E7
O.OEO
00 Time
_3.9E7
_1.9E7
O.OEO
00 Time
_1.0E8
.5.2E7
-O.OEO
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:00 Time
 r.a

-------
    File: A17JUL98BAcq:  18-JUL-1998  01:47:01Exp:  EXP_M23_DB5_OVATION Voltage  SIR  EI+GC  Autospec-UltimaE  Paradigm
    Sample  #13   Text:  1070-4 xl/2   ALS #13
    303.9016  S:13  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1628.0,1.00%,F,F)
    100%                                                                 A3.30E4                                      9.5E3
                     24:00           25:00           26:00          27:00
    305.8987  S:13  SMO(1,3)  BSUB(128,15,-3.0 )  PKD(3,3,3,0.10%,2644.0,1.00%,F,F)
    100%                                                                 A3.04E4
                 24:00           25:00          26:00           27:00
315.9419 S:13 SMO(1,3)  BSUB(128,15,-3 . 0) PKD(3,3,3,0.10%,4384.0,1.00%,F, F)
100%                                                                A1.92E8
                                     28:00
                                                                                                  29:00
       O
                                                     30:00  Time

                                                          3.9E7

                                                         L1.9E7

                                                         .O.OEO
                     24:00          25:00           26:00          27:00           28:00
    317.9389 S:13 SMO(1,3)  BSUB(128 . 15 ,-3 . 0) PKD(3,3,3,0.10%,3748.0,1.00%,F,F)
    100%                                                                 A2.46E8
     50_
                                                                                              29:00
      Oj
                                                                    30:00   Time

                                                                        5.0E7

                                                                       L2.5E7

                                                                         I. OEO
                     24:00          25:00           26:00          27:00           28:00           29:00
    375.8364 S:13 SMO(1,3)  BSUB(128,15,-3.0) PKD(3,3,3,100.00%,44.0,1.00%,F,F)
    100%,                                                                                  28;27
                                                                                     28:10
     50J
      OJ
           2323
                    23:58
                                25:00

                                   Wn.
                                                   25:55
AA
26:35       27:20   27:
       1:55
       *h
                                                     29:03
                                                  28:501
                                                                                                             29:43
30:00  Time

     7.4E3

    L3.7E3

     O.OEO
                     24:00          25:00           26:00           27:00           28:00           29:00           30:00   Time
    316.9824 S:13 SMO(1,3)  PKD(3,3,3,100.00%, 0.0,1.00%,F,F)
    100%    23:26   23:55     24:3724:5925:2025:43    _    26:3626^56_  27:27 27i51    28:2728j,47 29_;_11 _ 29:39    _6.1E7
10'
• X^v

p,

24:00 25:00 26:00 27:00 28:00 29:00 30:C
_3.0E7
O.OEO
)0 Time

-------
File: A17JUL98B — Acq: 18-JUL-1998  01:47:01  Exp: EXP_M23_DB5_OVATION Voltage SIR EI+  GC Autospec-UltimaE
Sample #13  Text: 1070-4 xl/2  ALS #13
339.8597 S:13 F:2 SMO(1,3) BSUB(128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 976 . 0 , 1 . 00%, F, F)
                                                                                                            Paradigm
100%

 50 j
                                                                                A2.20E4
  Oj
                                            A1.26E4
A1.10E4
                                                                           5.24E3
                                                                                                                  9.6E3

                                                                                                                 _4.8E3
                                                                                                  A2.80E3
                                                                                                                  .O.OEO
                                                                                                                     Time



     30il2  30i24  30i36  30148  31100  31:12  31:24  31:36
341.8568 S:13 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,2320.0,1.00%,F,F)
100%
                                            A9.39E3
 50J
                                                                   32166  32112  32124  32136  32148  33166
                                                                                                   A1.03E4
                                 3l!o6 ' 3l!l2  3l!24  31:36
     30ll2  30124  30136  30l48  31:00  31-12  31i24  31i36  31148  32:00   32:12  32:24  32:36  32:48  33:00
351.9000 S:13 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,1768.0,1.00%,F,F)
100%                                                            A2.16E8        A2.08E8

 50J
                                                  O.OEO
                                           33!12    Time

                                                  7 . 6E7

                                                 L3.8E7
                                                            31:48  32166  32!i2 ' 32:24  32:36  32:48  33:66
                                           ,     .PP. OEO
                                           33:12    Time
     3b!i2 ' 3b!24 ' 3b!36 ' 3o!48 ' 3llo6 ' 3lll2  3ll24
353.8970 S:13 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,2480.0,1.00%,F,F)
10Q%                                                            A1.38E8         A1.3.3E8

 50J
  0.
                                                                                                                  4 . 9E7

                                                                                                                 .2.4E7
                                                 -O.OEO
                                           33:12    Time
    ' 3b!i2 ' 30l24 ' 36136

                                              3ll24 ' 3l!36
                                 31100  31112  31124  31:36  31:48  32:00  32:12  32:24  32:36  32:48  33:00
409.7974 S:13 F:2 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,100.00%,3692.0,1.00%,F,F)
                                                                                         3 £* \ 4 U
                                                                                                      33:01
                                        31.,3 31:23    31:40           32:07        32:28
                                 30:59   J-1---1--3   A-
100S

 50J
                         30:47
                    30:38
                                                                                                            33:12
                                                                                                                 _1.2E4
                                                                                                                 L5.9E3
                                                 O.OEO
                                           33:12    Time
    ' 30112 ' 3b!24 ' 30136
                                 3l!66 ' 3l!l2 ' 3ll24
366.9792 S:13 F:2 SMO(1,3)  PKD( 3 , 3 , 3,100.00%,0.0,1.00%,F,F)
100%      30:20       J0:42	3_iiP_0	31L19__H:32_.  31:47
 50j
  OJ
                                                                    !:00  32:12  32:24  32:36

                                                                     31^04	32^15	
                                                                                                                 _6.6E7
                                                                                                                 L3.3E7
                                                                                                                 .O.OEO
                                                                                                            33:12     Time
     30ll2  30S24  30136  30148  3l!6o  3lSl2  3ll24  3l!36  3lUs  32IOO  32^12  32124  32-136  32i48  33iOO

-------
File: A17JUL98BAcq:  18-JUL-1998 01:47:01Exp: EXP_M23_DB5_OVATION Voltage  SIR EI+GC  Autospec-UltimaE
Sample #13  Text: 1070-4 xl/2  ALS  #13
373.8207 S:13 F:3 SMO(1,3) BSUB(128,15,-3.0) PKD(3,5,2,0.10%,2336.0,1.00%,F,F)
100%,                                   A3.27E4

              A1.12E4
   O
                                                                                                            Paradigm
                                                                                                                   1.3E4

                                                                                                                  L6.3E3
                                                                                                                  .O.OEO
      33:24    33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00    35:12    35:24    35:36
375.8178 S:13  F:3  SMO(1,3)  BSUB(128,15,-3.0) PKD(3,5,2,0.10%,1532.0,1.00%,F,F)
100%                                   A2.I
  50J

   ol
                                           5E4
               A9.13E3
                                                                   .90E3
                                                                                    A3.01E3
               A2.15E3
     i—l—i—r—T—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—i—r—i—i—i—i—r—i—i—i—i—i—i—i—i—r—r—i—i—i—i—i—i—i—i—i—|—i—i—i—i—r—[—i—i—i—i—i—|—l—i—i—i—i—i—i—r
      33:24    33:36   33:48    34:00    34:12    34:24    34:36    34:48    35:00    35:12    35:24    35:36
383.8639  S:13 F:3 BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,37376.0,1.00%,F,F)
100%                                      A1.18E8
  O
                           35:48  Time

                               1.1E4

                              _5.6E3
                                                                                                              35:48

                                                                                                                  5

                                                                                                                 12

                                                                                                              	10
 Time

,2E7

. 6E7

, OEO
 Time

,OE8

,OE7

.OEO
 Time

.1E3

,1E3

.OEO
 Time

 4E8

 2E7

 OEO
 Time:
      33:24    33:36    33:48    34:00    34:12    34:24    34:36    34:48
385.8610 S:13  F:3 BSUB(128,15,-3.0)  PKD(3,5,2,0.10%,48152.0,1.00%,F,F)
100%                                      A2.25E8
                                                                           35:00    35:12    35:24    35:36
     T—i—|—i—i i  I i—I • I  i i—i—i—|—i—i—i—i—i—|—i—i—i—f—i—r-*n—i—i~i I  I l  l I—l—l—I—l—i—i—l—i—|—i—i—i—i—i—|—i—r
      33:24   33:36    33:48    34:00    34:12    34:24    34:36    34:48    35:00
445.7555  S:13 F:3 SMO(1,3) BSUB{128,15,-3.0) PKD(3,3,3,100.00%,1852.0,1.00%,F,F)
1004           33;37                                             34:46    34:59
 50.:
'35! 12 '
                                                                                             35 124'  ' '35
                                                                                                   35:32
                           35:48

                               1

                              L5

                             JLo
 35:48

     8

    L4

    •O
  OJ
     l—l—I—l—i—r—i—i—r—T—i—i—p—i—i—i—i—i—i—i—i—i—i—i—i—i—|—i—i—i—i—r—T—i—r—i—i—i—i—i—i—i—l—i—I—i—i—i—i—i—l—i—r—i—i—i—i—i—i—i—i—i—i—I—i—I—i—I—|—i—r
      33124   33:36    33:48    34:00   34:12    34:24    34:36    34:48   35:00    35:12    35:24    35:36
 35:48

	1
380.9760 S:13 F:3 SMO(1,3)  PKD(3 , 3,3,100.00%,0.0,1.00%,F,F)
100%. 33:23             33:47 	    34:19	34:38  34j_47
 50J
                                                                             35:03	35:16
               35:32
                                                                                                  \7
     i—i—i—i—i—i—i—i—i—r—T—r—I—i—l—i—i—i—i—i—I—i—i—i—r—i—i—i—i—p—i—i—i—i—i—i—i—i—i—i—i—r—i—i—|—i—i—i—i—i—I—i  i i  i i I  i—l—l—i—i I—i—l—i—r—i—I—r—T
     33:24    33:36    33:48    34:00   34:12    34:24    34:36    34:48   35:00    35:12    35:24    35:36
                                                                                                                 L7

                                                                                                                 LO
                                                                                                              75:48

-------
     File:  A17JUL98B—Acq: 18-JUL-1998 01:47:01Exp: EXP_M23_DB5_OVATION Voltage SIR EI+GC Autospec-UltimaEParadigm
     Sample #13  Text: 1070-4 xl/2  ALS #13
     407.7818 S:13 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,1688.0,1.00%,F,F)
     100%               A8.Q1E4
       OJ
                                                                                                           2.8E4

                                                                                                          _1.4E4
                                                                                                          .O.OEO
            I I I I I  I I I | I I  I I I I	I—	Ill i i"TI  I I I I I I	I I I  I I I |	| I I I I I  | I I I 1 I |  I I
            36:00   36:12   36:24  36:36  36:48  37:00  37:12  37:24   37:36   37:48  38:00  38:12
     409.7788 S:13 F:4 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,980.0,1. 00%, F, F)
     100%              A8.Q5E4
      50J
       Oj
                                                                                  38:24  38:36  38:48  39:00  Time
                                                                                                           2.7E4

                                                                                                          _1.4E4
                                  A6.05E3
                                                                                                           O.OEO
            iT'i i I  i I i I i I  i 'i i i i i i  ill i i i " |-|iT r i" iji i i'l i | i i  i I i~| r ii i i | i i i  I I | i I ill | TT i TTip-i—r-
            36:00   36:12   36:24   36:36  36:48  37:00  37:12   37:24   37:36   37:48  38:00  38:12
     417.8253 S:13 F:4 SMO(1,3)  BSUB(128,15,-3.0) PKD(3,3,3,0.10%,4796.0,1.00%,F,F)
     100%              A5.13E7
       OJ
                                                               A3.26E7
                                                                                  38:24  38:36  38:48  39:00  Time

                                                                                                           1.6E7

                                                                                                          L7.8E6
                                                                            |
                                                                                                          .O.OEO
                                                                                  38124 ' 38136 ' 38.-48 ' 39loO  Time
                                                                                                           3 . 5E7

                                                                                                          .1.7E7
           i i i i i i  i i i i i i r i i i i t \  i i i i i i i  i i
            36:00   36:12   36:24   36:36  36:48  37:00  37:12  37:24   37:36  37:48  38:00  38:12
     419.8220 S:13 F:4 SMO(1,3)  BSUB(128, 15, -3 . 0)  PKD(3 , 3 , 3 , 0 . 10% , 23640 . 0 , 1 . 00%, F, F)
     100%              A1.16E8
      50J
       OJ
                                                               A7.43E7
            i i i i i  i i i i i i K i i i T~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 T i  i i i i i i i  i | i i i i i  |	|  ' •
            36:00   36112   36:24   36:36  36:48  37:00  37:12   37:24  37:36  37:48  38:00  38:12
     479.7165 S:13 F:4 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,2348.0,1.00%,F,F)
     100%,                                           37^10  37-21
                 36.09       36:30           36:58
      50J
                                                                                  38124 ' 38!36 ' SsUs ' 39!oO  Time
                                                                                  38:25
                                                                                             38:43
36166 ' 36!l2 ' 36124 ' 36I36 '  36! 48 ' 37!
                                                            37I24 '  37136  37148  38\00  38!l2
                                            7.7E3

                                           L3.9E3

                                           LO.OEO
     430.9728 S:13 F:4 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00% , F,F)
     100% 35:56   36:09 36j_19 36:31 36:41    36:55    37:11	37:34
      50J
       OJ
                   38:24  38:36  38:48  39:00  Time

37:50  38:02 38:13  38^26	38:47      ,_9. 4E7
              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   36:12  36:24  36:36  36:48  37:00  37:12   37:24   37:36  37:48  38:00  38:12
                                                                                                                      _4.7E7
                                                                                                                      O.OEO
                                                                                  38124 ' 38136 ' 38!48 '  39100  Time
10

-------
File: A17JUL98B
Sample #13 Text:
441.7427 3:13 F:5
100S
50_
0


A2 . 09E3
39ll2
443.7398 S:13 F:5
1002
50_
o:


^-^_— 	 ^— - 	
39ll2
469.7780 S:13 F:5
100%
50 J
OJ



39ll2
471.7750 S:13 F:5
100%
50 j
o:



39ll2
513.6775 S:13 F:5
100%
50 :
o:


3
39ll2
454.9728 S:13 F:5
Acq: 18-JUL-1998 01:4
1070-4 xl/2 ALS #13
SMO(1,3) BSUB(128,15



39:24 39:36
SMO(1,3) BSUB(128,15


"""^ 	 -^^^^ 	 — 	 -_ 	 _^. 	 • 	
39:24 39:36
SMO(1,3) BSUB(128,15



39124 39136
SMO(1,3) BSUB(128,15



39124 39136
SMO(1,3) BSUB(128,15


9 = 19 39:25 39:33
A ^\ /^
39124 39136
7:01 Exp: EXP M23 DB5 OVATION Voltage SIR EI+ . GC Autospec-UltimaE Paradigm

,-3.0) PKD( 3, 3, 3, 0.10%, 800. 0,1. 00%,
A5.69E4
/ \
— _-^__ ~_— _-— - *^—~±
39:48 40:00 40:12
,-3.0) PKD(3, 3, 3, 0.10%, 1660. 0,1. 00%
A6 . 28E4
/\
/ \^,
i i i i i i i "r'-T— i — i — i 	 1 — i — i — i — i — i — r —
39:48 40:00 40:12
,-3.0) PKD( 3, 3, 3, 0.10%, 2608. 0,1. 00%
Al . 51E8
f\
J \^_
igUs 4o!ob 4o!i2
,-3.0) PKD( 3, 3, 3, 0.10%, 2528. 0,1. 00%
Al . 72E8
f\
J \^__
39148 4o!ob 4o!l2
,-3.0) PKD (3, 3, 3, 100. 00%, 88. 0,1. 00%
40:02
/ \
39:42 39:53 / \,
39:48 40:00 40:12
'
F,F)


A329.79 A2.86E3
1.3E4
_6.7E3
n mm
' ' ' i 	 | i i r i r— T ^i -"TV^,' 	 -
40:24 40:36 40:48 41 00 Time
,F,F)


^___^^_ 	 _^_^^-^ 	 - -. 	 ,
1.9E4
L9.5E3
• n own
T 	 r — i 	 1 	 1 	 1 	 1 	 1 	 r — ] 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 — ._-•- — -
40:24 40:36 40:48 41 00 Time
,F,F)



3.4E7
_1.7E7
O.OEO
40!24 40!36 4'oUs 4l!oO Time
,F,F)



3.9E7
.1.9E7
.O.OEO
4o!24 ' ' ' 4ol36 ' ' ' 4o!48 ' ' ' 4l!oO Time
,F,F)


4U:zU /m.Tc
/\ ^32/^i__ «Jii*8
5.5E3
:2.8E3
_O.OEO
4ol24 40!36 4o!48 4l!oO Time
SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100% 39:09 39:18 39:24 39^33
50J
Oj
/

39!l2


39124 39136
39:44 40:0540:10


39148 4o!ob 4o!l2
40:25 40:3540:41 40:49 40:56 1 . OE8


_5.2E7
O.OEO
40124 4o!36 4ol48 41 00 Time
JO
00

-------
                                                                     Paradigm Analytical Labs
                             Analytical Data Summary Sheet
Analyte
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6.,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDI
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF .
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ(ND=0)
TEQ (ND=l/2)

EMPC
EMPC
0.0028
EMPC
0.0072

0.0200
' olol^P
0.0198
0.02403?«P
0.0323
0.0132^
0.0114
0.0031 V.*!
0.0215
EMPC
EMPC
0.109
0.0744
0.138
0.0376
0.628
0.321
0.108 .
0.0244
Q.0223 „.
0.0227

0.0006
0.000f ; ^
0.0007
0.0006
0.0006
;p.OQ08 ,
0.0008
©ioofe^
0.0006
**^^)J6 '.
"oboos"
E 0,0004
0.0004

0.0009
0;OQ10
0.0010
« 0^006
0.0004
0,0006
0.0008
0.0009
0.0006
; 0.0004
0.0009
f\" -£'-» \-.".


0.0025
^'0,01J1J>S::

0.0054





'•' •"^'2*-V

" 1^5;

• ; '-,-*" Ji,^

0.0023
0.0031
1 £r 0.123;--
0.0*840
0.147

0.714
0.326
0.109
0.0300
0.027^0
0.0270
^JKE.;
28:27
•• 3^r3f>,:
34:42
34:46
34:58
37:10
40:02
27:29
31:57
32:25
34:10
34:15
34:37
~ 35:12
36:22
37:32
40:11










Ratio
0.62
, \4.*».
1.34
1.55
1.39
0.98
0.95
0.78
1.59
1.52
1.25
1.22:
1.28
1.26
0.95
1.47
0.67










Qualifier

























FIEF
ITEF
Client Information

Project Name:              Texas lam
Sample ID:                M23-I4IW

Laboratory Information

Project ID:                L1070
Sample ID:                 1070-5

Collection Date:
Receipt Date:
                                                  Sample Information
                                                                         Atf
                                                                                Grams
                                                                         HA
                                                  Filename:
al7ju!98b-14
al7ji098b-l
Analysis pi|e
al7jul9Sb-15
mg290-23-071798
                                         1/2
                                                                                      c'r" 129

-------
                                                                 Paradigm Analytical Labs
                            Analytical Data Summary Sheet
Labeled
Standard
Extraction Standards
13C,2-2,3,7,8-TCDD
13Ci2-l,2,3,7,8-PeCDD
13C12-U,3,6,7,8-HxCDD
13Ci2-l,2,3,4,6,7,8-HpCDD
13C12-OCDD
13Ci2-2,3,7,8-TCDF
13C12-l,2,3,7,8-PeCDF
13Cu-l 2367 8-HxCDF
l3C12-l,2,3,4,6,7,8-HpCDF
Cleanup Standards
"CU-W.g-TCDD
13C12-2,3,4,7,8-PeCDF
I3C12-l,2,3,4,7,8-HxCDD
13Cirl,2,3,4,7,8-HxCDF
13Cirl,2,3,4,7,8,9-HpCDF
Injection Standards
13c12-i,2,3,4-TCDD
13C12-l,2,3,7,8,9-HxCDD
Expected ^
Amount :
(ng)

4
4
4
4
8
4
4
4
4

4
4
4
4
4



Measured
'Amount
tig)

2.98
3.36
3.07
3.13
5.32
2.77
2.53
2.45
2.14

4.01
4.28
4.43
4.15
4.37



Pe«*Bt
Recovery

74.4
83.9
76.8
78.3
66.5
69.2
63.3
61.2
53.5

100.2
107.0
110.7
103.7
109.1



RT ;
(nun.)

28:27
32:37
34:45
37:09
40:01
27:25
31:56
"- 34:14
36:21

28:27
32:24
34:42
34:10
37:31

28:09
34:58
.Ratio


0.78
1.57
1.25
1.05
0.88
0.79
1.55
052
V«***»
0.45


1.57
1.25
0.52
0.44

0.79
1.25
Qualifier




















Client Information
Project Name:
Sample ID:
Laboratory Information
Project ID:
Sample ID:
Collection Date:
Receipt Date:
Extraction Date:
Analysis Date:
I?A\)'UKCk^0'/i*hfcf* "'* "*~lt * *
rvCV-lwlfirUU^U'lr-* i"'""^ ~^s •
Texas Lime Kiln
M23-I-1FH
L1070
1070-5
25-Jun-98
08-Jul-98
10-Jul-98
^-•ff^-r '-'lit' ' ' -^ "'-
-. -—^ >>»%-" ' • '"'•"? • " "
£••'-;'?-<&> . *$-' : >' ^.,"
Sample Information
Matrix:
Weight 7 Volume:
Moisture / Lipids:
Original pH :
Filename:
Retchk:
Begin ConCal:
EndConCal:
•"" . "*'\ "%<*K '
Air
1 Grams
0.0 %
NA
al7ju!98b-14
a!7jul98b-l
al7juI98b-2
a!7jul98b-15
m8290-23-071798
Date Reviewed: 2Z^
                                      2/2
                                                                                    ' 13C

-------
                                                                     Paradigm Analytical Labs
                             Analytical Data Summary Sheet
Analyte

2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD

OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
O "^J A. *7 fi ¥j^**1»|"\?5^- ,
j^ j .*r- / sO**jtr^3x>JL/" " - .'
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-flxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDDs
Total PeCDDs
Total HxCDDs
Total HpCDDs
Total TCDFs
Total PeCDFs
Total HxCDFs
Total HpCDFs
TEQ(ND*=0)
TEQ (ND=l/2)
•
^,
. >. .

^0,149
Oil 98
7.90
5.36
9.42

45.8
20.9
6.98
1.92
1.73
1.73
'*&$$$.: *
f^gii^p,', ~
28:27
. .''32^7?,"
34:42

34:58
37:10
40:02
-'' 27:2? , •
31:57
ii-pii's-'
~ 34:10
" 34:15
34:37
35:12 , :
36:22
37:32
40:11










;. JB&JJ& ...
•c-.g.; !-i«^ter;
0.62
-- J*|?i -
1.34
1.55
1.39
0.98
0.95
0.78
1.59
1-52
1.25
1,22
1.28
. 1.26
0.95
1.47
0.67










Qualifier


























ITEF
ITEF
Client Information

Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:

Collection Date:
Texas Lime Kiln
M23-MFJa
L1070
1070-5
Sample Information
                                                       Grams
ExtractoojLDate:
Aaalysisl
                                   r: r''   *i$5P!|g$
                                         1/2
                                                                                     r r

-------
                                                                     Paradigm Analytical Labs
                              Analytical Data Summary Sheet
Labeled
Standard
Extraction Standards
13C12-2,3,7,8-TCDD
13Ci2-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
13C,2-2,3,7,8-TCDF
13C,rl,2,3,7,8-PeCDF
13Ci2-l,2,3,6,7,8-HxCDF
l3CI2-l,2,3,4,6,7,8-HpCDF
Cleanup Standards
37Cl4-2,3,7,8-TCDD
'3C12-2,3,4,7,8-PeCDF
I3C12-l,2,3,4,7,8-HxCDD
13CI2-l,2,3,4,7,8-HxCDF
13C12-l,2,3,4,7,8,9-HpCDF
Injection Standards
13C12-1,2,3,4-TCDD
I3Cirl,2,3,7,8,9-HxCDD
Expected
Amount
(ng)

4
4
4
4
8
4
4
4
4

4
4
4
4
4



Measured
(ngJ

2.98
3.36
3.07
3.13
5.32
2.77
2.53
2.45
2.14

4.01
4.28
4.43
4.15
4.37



; • . o«i^

74.4
83.9
76.8
78.3
66.5
69.2
63.3
61.2
53.5

100.2
107.0
110.7
103.7
109.1



RT :
? Until.)

28:27
32:37
34:45
37:09
40:01
27:25
31:56
; 34:14
36:21

28:27
32:24
34:42
34:10
37:31

28:09
34:58
Ratio

0.78
1.57
1.25
1 05
Jl »W*/
0.88
0.79
1.55
0.52
0.45


1.57
1.25
0.52
0.44

0.79
1.25
Qualifier



















Client Information
Project Name:
Sample ID:

Laboratory Information

Project ID:
Sample ID:

Collection Date:
Receipt Date:
Extraction Date:
Analysis Date:
Texas Lime Kiln
M23-I-1FH



L1070
1070-5

25-Jun-98
08-M-98
10-Jal-98
If-Jul-tS
Sample Information

Matrix:
Weight /Volume:
Moisture / Lipids:
Original pH:

Filename:
Retook:
Begin ConCal:
EndConCal:
;IniiiaJjCal:


Air
15.59 Grams
0.0 %
NA

a!7jul98b-14
a!7jul98b-l
a!7jul98b-2
al7ju!9Sb-15
m8290-23-071798
                                        2/2

-------
CO
CO
OPUSguan 20-JUL-1998 Page 1
Filename al7ju!98b
Sample 14
Acquired 18-JUL-98 02:32:07
Processed 20-JUL-98 09:09:09
Sample ID 1070-5 xl/2
Cal Table m8290-23-071798
Results Table M8290-23-071798B
Comments
Typ
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS
SS
S3
SS
SS
SS
Name; Resp; Ion 1; Ion 2; RA;?; RT;
2,3,7,8-TCDD; 4.16e+05; 7.15e+04; 3.44e+05; 0.21;n; 28:27;
1,2,3,7,8-PeCDD; 2.24e+05; 1.44e+05; 8.01e+04; 1.79,-n; 32:37;
1,2,3,4,7,8-HxCDD; 1.24e+05; 7.09e+04; 5.28e+04; 1.34;y; 34:42;
1,2,3,6,7,8-HxCDD; 3.02e+05; 1.83e+05; 1.18e+05; 1.55;n; 34:46;
1,2,3,7,8,9-HxCDD; 4.10e+05; 2.38e+05; 1.72e+05; 1.39;y; 34:58;
1,2,3,4,6,7,8-HpCDD; 9.28e+05; 4.59e+05; 4.70e+05; 0.98;y; 37:10;
OCDD; 6.83e+05; 3.34e+05; 3.50e+05; 0.95;y; 40:02;
2,3,7,8-TCDF; 8.75e+06; 3.84e+06; 4.91e+06; 0.78;y; 27:29;
1,2,3,7,8-PeCDF; 1.21e+06; 7.39e+05; 4.66e+05; 1.59;y; 31:57;
2,3,4,7,8-PeCDF; 1.51e+06; 9.12e+05; 6.00e+05; 1.52;y; 32:25;
1,2,3,4,7,8-HxCDF; 1.69e+06; 9.38e+05; 7.51e+05; 1.25;y; 34:10;
1,2,3,6,7,8-HxCDF; 8.73e+05; 4.80e+05; 3.93e+05; 1.22;y; 34:15;
2,3,4,6,7,8-HxCDF; 6.46e+05; 3.62e+05; 2.84e+05; 1.28;y; 34:37;
1,2,3,7,8,9-HxCDF; 1.51e+05; 8.43e+04; 6.68e+04; 1.26;y; 35:12;
1,2,3,4,6,7,8-HpCDF; 8.74e+05; 4.26e+05; 4.48e+05; 0.95;y; 36:22;
1,2,3,4,7,8,9-HpCDF; 7.79e+04; 4.64e+04; 3.15e+04; 1.47;n; 37:32;
OCDF; 1.12e+05; 4.48e+04; 6.70e+04; 0.67;n; 40:11;
13C-2,3,7,8-TCDD; 3.01e+08; 1.31e+08; 1.70e+08; 0.78;y; 28:27;
13C-l,2,3,7,8-PeCDD; 2.37e+08; 1.45e+08; 9.20e+07; 1.57;y; 32:37;
13C-l,2,3,6,7,8-HxCDD; 2.64e+08; 1.47e+08; 1.17e+08; 1.25;y; 34:45;
13C-l,2,3,4,6,7,8-HpCDD; 1.99e+08; 1.02e+08; 9.75e+07; 1.05;y; 37:09;
13C-OCDD; 2.73e+08; 1.28e+08; 1.45e+08; 0.88;y; 40:01;
13C-2,3,7,8-TCDF; 3.51e+08; 1.55e+08; 1.97e+08; 0.79;y; 27:25;
13C-l,2,3.7,8-PeCDF; 2.80e+08; 1.70e+08; 1.10e+08; 1.55;y; 31:56;
13C-l,2,3,6,7,8-HxCDF; 2.43e+08; 8.35e+07; 1.59e+08; 0.52;y; 34:14;
13C-l,2,3,4,6,7,8-HpCDF; 1.29e+08; 4.01e+07; 8.88e+07; 0.45,-y; 36:21;
13C-1,2,3,4-TCDD; 3.69e+08; 1.62e+08; 2.06e+08; 0.79;y; 28:09;
13C-l,2,3,7,8,9-HxCDD; 3.20e+08; 1.78e+08; 1.42e+08; 1.25;y; 34:58;
3701-2,3, 7, 8-TCDD; 3.72e+08; 3.72e+08; -; -;-; 28:27;
13C-2,3,4,7,8-PeCDF; 4.63e+08; 2.83e+08; 1.80e+08; 1.57;y; 32:24;
13C-l,2,3,4,7,8-HxCDD; 2.57e+08; 1.43e+08; 1.14e+08; 1.25;y; 34:42;
13C-l,2,3,4,7,8-HxCDF; 3.21e+08; 1.09e+08; 2.11e+08; 0.52;y; 34:10;
13C-l,2,3,4,7,8,9-HpCDF; 2.06e+08; 6.28e+07; 1.43e+08; 0.44,-y; 37:31;
37Cl-2,3,7,8-TCDD; 3.72e+08; 3.72e+08; -; -;-; 28:27;
13C-2,3,4,7,8-PeCDF; 4.63e+08; 2.83et08; 1.80e+08; 1.57;y; 32:24;
13C-l,2,3,4,7,8-HxCDD; 2.57e+08; 1.43e+08; 1.14e+08; 1.25,-y; 34:42;
13C-l,2,3,4,7,8-HxCDF; 3.21e+08; 1.09e+08; 2.11e+08; 0 52;y; 34-10;
13C-l,2,3,4,7,8,9-HpCDF; 2.06e+08; 6.28e+07; 1.43e+08; 0.44,-y; 37:31;


*** ^
<&'




Cone ;
0.140;
0.085;
0.070;
0.134;
0.181;
0.519;
0.499;
2.613;
0.495;
0.600;
0.808;
0.331;
0.285;
0.077;
0.538;
0.058;
0.077;
74.379;
83.935;
76.811;
78.297;
133.080;
69.167;
63.264;
61.146;
53.443;
76.468;
80.780;
100.214;
107.006;
110.726;
103.709;
109.124;
134.810;
169.200;
143.966;
168.265;
204.264;

uO
V\ \J





DL;
0.0147;
0.0105;
0.0182;
0.0144;
0.0142;
0.0193;
0.0207;
0.0225;
0.0159;
0.0154;
0.0120;
0.0095;
0.0111;
0.0127;
0.0213;
0.0258;
0.0248;
0.0426;
0.0205;
0.0339;
0.0124;
0.0155;
0.0215;
0.0099;
0.1718;
0.1030;
-;
_ .
0.0153;
0.0101;
0.0504;
0.2204;
0.1317;
0.0215;
0.0095;
0.0623;
0.3181;
0.3148;








S/N1;?;
10;y;
25;y;
ll;y;
22;y;
26;y;
55;y;
88;y;
315,-y;
115;y;
142;y;
144;y;
72;y;
53, -y;
11 ;y;
66 ;y;
8;y;
ll;y;
3338;y;
23082 ;y;
9483 ;y;
10663 ;y;
11857 ,-y;
8595;y;
34158;y;
1381,-y;
1537,-y;
4328;y;
10837,-y;
19251, -y;
58412 , -y;
9289;y;
2048;y;
2152, -y;
19251;y;
584 12 ,-y;
9289;y;
2048;y;
2152;y;








S/N2 ; ?
56 ;y
24 ;y
ll;y
21;y
25;y
163, -y
63, -y
243, -y
75;y
96 ;y
133 ;y
68, -y
45;y
10 ;y
89, -y
6;y
10;y
8191,-y
17838;y
5440,-y
17074, -y
19215;y
10041;y
30128;y
1132 ;y
1118;y
10379;y
6346;y

51435, -y
5383;y
1644;y
1580;y
-; -
51435;y
5383;y
1644 ;y
1580;y
mod?
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
no
                                                                                                                                                 Page 1!

-------
OPUSguan   20-JUL-1998
                                      Page 1
                                                                   Page 1 of 8

 Ent: 39 Name: Total Tetra-Furans  F:l  Mass:  303.902  305.899 Mod? no   #Hom:22

 Run: 19 File: al7ju!98b    S:14 Acq:18-JUL-98 02:32:07  Proc:20-JUL-98 09:09:09
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-5 xl/2
   Amount:  17.84
     Cone:  17.84
   Tox #1:  -
Name
2,3,7,8-TCDF
of which 2.61
of which 2.61
     Tox #2:  -

#     RT Respnse
named and 15.23
named and 15.23
      Tox #3:  -
                                        RA
                   1  23:39 3.4e+06  0.77  y
                            3.4e+06

                   2  24:14 1.9e+06  0.75  y
                            1.9e+06

                   3  24:34 2.2e+06  0.76  y
                            2.2e+06

                   4  24:52 7.8e+06  0.80  y
                            7.86+06

                   5  24:58 1.8e+06  0.38  n
                            1.8e+06

                   6  25:10 1.8e+06  0.74  y
                            1.8e+06

                   7  25:17 5.4e+06  0.75  y
                            5.46+06

                   8  25:40 1.9e+06  0.63  n
                            1.96+06
                   9  25:44 3.1e+06
                            3.1e+06
                                     0.92  n
10 26:01 1.5e+06  0.78  y
         l.Se+06

11 26:09 3.1e+06  0.78  y
         3.1e+06

12 26:26 5.5e+06  0.81  y
         5.5e+06

13 26:34 4.1e+06  0.74  y
         4.1e+06

14 26:50 2.5e+06  0.83  y
         2.5e+06

15 27:03 1.3e+05  2.14  n
         1.3e+05

16 27:11 1.2e+06  0.78  y
         1.2e+06

17 27:29 8.8e+06  0.78  y
         8.8e+06

18 27:41 1.3e+04  0.52  n
         1.3e+04

19 28:03 1.9e+06  0.81  y
         1.9e+06
          Cone

           1.03
               ]
               }
           0.58
               £
               1
           0.65
               c
               1
           2.34

               4
           0.53
               4
               a
           0.54
               "
               3
           1.63


           0.57

               ]
           0.92
               :
               i
           0.46
               e
               £
           0.92
               ]
               1
           1.64


           1.22
               3

           0.75
               3
               ]
           0.04
               6
               4
           0.36
               C
               6
           2.61

               t
           0.00
               <
               £
           0.56
    unnamed
    unnamed
                                                      Area  Height
                                  S/N  Mod?
  .5e+06  3.2e+05  1.6e+02 y  n
  .9e+06  4.2e+05  1.3e+02 y  n

 8.3e+05  1.8e+05  9.4e+01 y  n
 l.le+06  2.4e+05  7.8e+01 y  n

 9.4e+05  1.9e+05  9.9e+01 y  n
 1.2e+06  2.6e+05  8.3e+01 y  n
1
 3.5e+06  6.76+05  3.4e+02 y  n
  .4e+06  8.4e+05  2.7e+02 y  n

  .9e+05  1.5e+05  7.7e+01 y  n
 1.3e+06  1.9e+05  6.1e+01 y  n
9
 7.7e+05  l.Se+05  9.1e+01 y  n
 l.Oe+06  2.3e+05  7.4e+01 y  n

 2.3e+06  3.06+05  1.6e+02 y  n
 3.1e+06  4.16+05  1.3e+02 y  n
7
 7.4e+05  2.16+05  l.le+02 y  n
  .2e+06  2.7e+05  8.6e+01 y  n

  .5e+06  2.76+05  1.4e+02 y  n
  .6e+06  3.46+05  l.le+02 y  n

 6.7e+05  l.Se+OS  7.5e+01 y  n
 8.6e+05  l.Se+05  5.7e+01 y  n

 1.3e+06  2.86+05  1.4e+02 y  n
 1.7e+06  3.56+05  l.le+02 y  n
1
 2.5e+06  4.76+05  2 . 4e-t-02 y  n
 3.0e+06  5.96+05  1.96+02 y  n
2
 1.7e+06  3.66+05  1.9e+02 y  n
 2.3e+06  4.76+05  1.5e+02 y  n

 l.le+06  2.3e+05  1.2e+02 y  n
  .4e+06  2.9e+05  9.1e+01 y  n

 8.6e+04  1.7e+04  8.5e+00 y  n
 4.0e+04  l.Se+04  4.7e+00 y  n

 5.3e+05  l.le+05  5.5e+01 y  n
 6.8e+05  1.3e+05  4.'3e+01 y  n
1
 3.8e+06  6.16+05  3.1e-i-02 y  n
 4.9e+06  7.66+05  2.4e+02 y  n

 4.5e+03  1.96+03  9.8e-01 n  n
 8.7e+03  2.06+03  6.4e-01 n  n

 8.3e+05  1.7e+05  8.6e+01 y  n
 l.Oe+06  2.1e+05  6.7e+01 y  n
                                                                                                 5C'  134

-------
OPUSquan   20-JUL-1998                Page  2
                   20 28:19 1.3e+06  0.83  y    0.40
                           1.3e+06               6.le+05 1.le+05  5.8e+01 y  n
                                                 7.3e+05 1.4e+05  4.6e+01 y  n
                   21 28:33 1.3e+05  1.35  n    0.04
                           1.3e+05               7.7e+04 1.4e+04  7.0e+00 y  n
                                                 5.7e+04 1.3e+04  4.0e+00 y  n
                   22 29:46 2.5e+05  1.60  n    0.07
                           2.5e+05               l.Se+05 2.6e+04  1.3e+01 y  n
                                                 9.5e+04 1.9e+04  6.0e+00 y  n
                                                                                              Of'  135

-------
OPUSquan   20-JUL-1998
                                      Page 3
                                                                    Page  2  of  8

 Ent: 40 Name: Total Tetra-Dioxins F:l  Mass:  319.897  321.894  Mod? no   fHorn:15

 Run: 19 File: a!7ju!98b    S:14 Acq:18-JUL-98 02:32:07  Proc:20-JUL-98  09:09:09
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3 .5 17-APR-1997 11:14:34  Sample text:  1070-5 xl/2
   Amount: 3.10
     Cone: 3.10
   Tox #1: -
Name
2,3,7,8-TCDD
of which 0.14
of which 0.14
     Tox #2:  -

#     RT Respnse
named and 2.96
named and 2.96
      Tox #3:  -
                                        RA
                   1  25:15 3.5e+06  0.79 y
                            3.5e+06

                   2  25:41 2.0e+06  0.73 y
                            2.0e+06

                   3  26:04 3.1e+05  0.86 y
                            3.1e+05

                   4  26:54 9.5e+05  0.78 y
                            9.5e+05

                   5  27:08 2.1e+05  0.85 y
                            2.1e+05

                   6  27:17 2.9e+05  0.87 y
                            2.9e+05
                      27:25 l.le+05
                            l.le+05
                                     1.84 n
8  27:45 2.8e+05  0.72 y
         2.8e+05

9  28:10 3.4e+05  0.67 y
         3.4e+05

10 28:20 4.9e+05  0.94 n
         4.9e+05

11 28:27 4.2e+05  0.21 n
         4.2e+05

12 28:40 l.Oe+05  0.67 y
         l.Oe+05

13 28:57 1.2e+05  0.82 y
         1.2e+05

14 29:18 4.2e+04  1.69 n
         4.2e+04

15 29:54 4.8e+04  0.48 n
         4.86+04
          Cone

           1.19
               1
               2
           0.66
               £
               1
           0.10
               1
               1
           0.32
               A
               C
           0.07
               c
               1
           0.10
               ]
               ]
           0.04


           0.09
               ]
               ]
           0.12
               ]

           0.17


           0.14


           0.04
               <
               f
           0.04
               C
               (.
           0.01

               ]
           0.02
    unnamed
    unnamed
                                                      Area  Height
                                  S/N  Mod?
 1.6e+06  3.4e+05  2.1e+02 y   n
 2.0e+06  4.26+05  3.4e+02 y   n

 8.3e+05  1.7e+05  l.Oe+02 y   n
 l.le+06  2.3e+05  1.9e+02 y   n
)
 1.4e+05  2.9e+04  1.8e+01 y   n
 1.76+05  3.1e+04  2.5e+01 y   n

 4.1e+05  7.7e+04  4.6e+01 y   n
 5.3e+05  9.8e+04  7.8e+01 y   n
7
 9.5e+04  l.Se+04  9.0e+00 y   n
 l.le+05  1.8e+04  1.4e+01 y   n

  .3e+05  2.4e+04  1.5e+01 y   n
  .5e+05  3.0e+04  2.4e+01 y   n

 7.36+04  1.6e+04  9.76+00 y   n
 3.9e+04  8.8e+03  7.0e+00 y   n

  .2e+05  2.66+04  1.5e+01 y   n
  .6e+05  3.3e+04  2.6e+01 y   n

 1.4e+05  2.8e+04  1.7e+01 y   n
 2.06+05  4.2e+04  3.3e+01 y   n
7
 2.4e+05  4.8e+04  2.9e+01 y   n
 2.6e+05  5.2e+04  4.1e+01 y   n
4
 7.2e+04  1.6e+04  9.5e+00 y   n
 3.4e+05  6.9e+04  5.6e+01 y   n

  .2e+04  l.Oe+04  6.3e+00 y   n
 6.2e+04  1.4e+04  l.le+01 y   n
1
 5.3e+04  1.3e+04  7.9e+00 y   n
 6.5e+04  1.5e+04  1.2e+01 y   n

 2.7e+04  6.0e+03  3.7e+00 y   n
 1.6e+04  5.26+03  4.1e+00 y   n

 1.6e+04  4.86+03  2.9e+00 n   n
 3.3e+04  5.9e+03  4.7e+00 y   n
                                                                                                      136

-------
OPUSquan   20-JUL-1998
                   Page 4
                                                                    Page  3  of  8

 Ent: 41 Name: Total Penta-Furans  F:2  Mass:  339.860 341.857 Mod?  no   #Hom:15

 Run: 19 File: a!7ju!98b    S:14 Acq:18-JUL-98 02:32:07 Proc:20-JUL-98  09:09:09
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal:  m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-5 xl/2
   Amount: 8.16
     Cone: 8.16
   Tox #1: -
Name
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
of which 1.09
of which 1.09
     Tox #2:  -
named and 7.07
named and 7.07
      Tox #3:  -
#     RT Respnse     RA    Cone

1  30:15 2.3e+06  1.54  y    0.93
         2.3e+06

2  31:15 1.2e+06  1.56  y    0.47
         1.2e+06

3  31:21 5.0e+06  1.57  y    2.03
         5.0e+06

4  31:29 8.9e+05  1.39  y    0.36
         8.9e+05

5  31:36 2.5e+05  1.43  y    0.10
         2.5e+05

6  31:45 3.1e+06  1.51  y    1.24
         3.1e+06

7  31:54 1.2e+06  1.49  y    0.47
         1.2e+06

8  31:57 1.2e+06  1.59  y    0.49
         1.2e+06

9  32:04 5.6e+05  1.69  y    0.22
         5.6e+05

10 32:08 1.3e+06  1.54  y    0.52
         1.3e+06

11 32:25 l.Se+06  1.52  y    0.60
         1.5e+06

12 32:29 1.5e+06  1.56  y    0.59
         1.5e+06
unnamed
unnamed
                                                      Area  Height
                                                  S/N  Mod?
                                                   1.4e+06 2.9e+05  1.3e+02  y  n
                                                   9.1e+05 1.9e+05  8.4e+01  y  n
                                                  7
                                                   7.1e+05 2.4e+05  l.Oe+02  y  n
                                                   4.5e+05 l.Se+05  6.7e+01  y  n
                                                  3
                                                   3.16+06 8.1e+05  3.6e+02  y  n
                                                   2.0e+06 5.4e+05  2.4e+02  y  n
                                                  5
                                                   5.2e+05 1.6e+05  7.0e+01  y  n
                                                   3.7e+05 l.le+05  4.96+01  y  n
                    13 32:35 6.0e+04  2.37 n    0.02
                            6.06+04

                    14 32:38 1.6e+05  1.22 n    0.06
                            1.6e+05

                    15 32:57 1.3e+05  1.25 n    0.05
                            1.3e+05
               l.Se+05 2.7e+04 1.2e+01 y  n
               l.Oe+05 1.9e+04 8.2e+00 y  n
              J
               l.Se+06 6.16+05 2.7e+02 y  n
               1.2e+06 4.0e+05 1.7e+02 y  n
              7
               6.9e+05 2.6e+05 l.le+02 y  n
               4.66+05 1.7e+05 7.3e+01 y  n
              3
               7.46+05 2.6e+05 l.le+02 y  n
               4.7e+05 1.7e+05 7.5e+01 y  n
              2
               3.5e+05 1.2e+05 5.2e+01 y  n
               2.1e+05 7.06+04 3.16+01 y  n
              2
               7.86+05 2.86+05 1.26+02 y  n
               S.le+05 1.86+05 7.86+01 y  n
              D
               9.1e+05 3.3e+05 1.4e+02 y  n
               6.06+05 2.2e+05 9.6e+01 y  n
              3
               9.06+05 3.16+05 1.46+02 y  n
               5.76+05 2.0e+05 9.06+01 y  n
              2
               4.2e+04 1.66+04 6.8e+00 y  n
               1.8e+04 9.1e+03 4.0e+00 y  n
                                8.86+04 2.96+04 1.3e+01 y  n
                                7.2e+04 2.0e+04 8.6e+00 y  n
                               5
                                7.2e+04 2.7e+04 1.2e+01 y  n
                                5.8e+04 1.8e+04 7.9e+00 y  n
                                                                    Page 4 of 8

  Ent:  42  Name: Total  Penta-Dioxins F:2  Mass: 355.855 357.852 Mod? no   #Hom:ll

  Run:  19  File: a!7ju!98b    S:14 Acq:18-JUL-98 02:32:07 Proc:20-JUL-98 09:09:09
  Tables:  Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
  Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-5 xl/2
   Amount:  2.10
      Cone:  2.10
of which 0.08
of which 0.08
named and 2.01
named and 2.01
 unnamed
 unnamed
                                                                                                         137

-------
OPUSguan   20-JUL-1998
                                      Page 5
   Tox #1: -

Name
1,2,3,7,8-PeCDD
     Tox #2:  -

#     RT Respnse

1  31:29 1.7e+06
         1.7e+06

2  31:59 1.4e+06
         1.4e+06

3  32:04 1.5e+05
         l.Se+05

4  32:10 l.le+06
         l.le+06

5  32:16 9.4e+04
         9.4e+04

6  32:20 1.8e+05
         l.Se+05

7  32:26 4.0e+05
         4.0e+05

8  32:30 1.4e+05
         1.4e+05

9  32:37 2.2e+05
         2.2e+05

10 32:43 9.6e+04
         9.6e+04

11 32:54 1.2e+05
         1.26+05
     Tox #3:  -

   RA    Cone

1.57 y    0.65
              ]
              £
1.59 y    0.51
              £
              C
1.68 y    0.06
              c
              c
1.51 y    0.40
              £
              4
2.03 n    0.04
              6

1.79 n    0.07
              ]
              6
1.62 y    0.15
              2
              1
1.68 y    0.05
              E
              C
1.79 n    0.08
              1
              £
1.39 y    0.04
              C
              4
2.18 n    0.04
                                                      Area  Height
                 S/N  Mod?
                                                   3.
,le+06  3.36+05  1.66+02 y  n
,7e+05  2.2e+05  1.8e+02 y  n

 4e+05  3.06+05  1.5e+02 y  n
 2e+05  2.0e+05  1.7e+02 y  n

,6e+04  3.16+04  1.56+01 y  n
,7e+04  2.0e+04  1.7e+01 y  n

.46+05  2.36+05  l.le+02 y  n
,2e+05  1.56+05  1.3e+02 y  n

,3e+04  2.9e+04  1.4e+01 y  n
 le+04  1.2e+04  l.Oe+01 y  n

,2e+05  3.3e+04  1.6e+01 y  n
,5e+04  2.2e+04  1.8e+01 y  n

.5e+05  7.56+04  3.6e+01 y  n
.5e+05  5.5e+04  4.6e+01 y  n

.9e+04  3.2e+04  1.6e+01 y  n
.3e+04  2.1e+04  1.8e+01 y  n

.4e+05  5.le+04  2.5e+01 y  n
.Oe+04  2.9e+04  2.4e+01 y  n

.6e+04  1.7e+04  8.1e+00 y  n
.Oe+04  1.3e+04  l.le+01 y  n

.Oe+04  2.5e+04  1.26+01 y  n
.7e+04  1.2e+04  l.Oe+01 y  n
                                                                                                        < 138

-------
OPUSquan   20-JUL-1998
                   Page 6
 Ent: 43 Name: Total Hexa-Furans
                                                 Page 5 of 8

                F:3  Mass:  373.821 375.818 Mod?  no   #Hom:12
 Run: 19 File: al7ju!98b    S:14 Acq:18-JUL-98 02:32:07 Proc:20-JUL-98 09:09:09
 Tables: Run: al7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results:  M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-5 xl/2
   Amount: 2.73
     Cone: 2.73
   Tox #1: -
Name
of which 1.50
of which 1.50
     Tox #2:  -

#     RT Respnse
named and 1.23
named and 1.23
      Tox #3:  -
                                        RA
                   1  33:31 6.7e+05  1.32 y
                            6.7e+05
                      33:37 1.6e+06
                            1.66+06
                  1.25 y
                   3  33:43 8.9e+04  1.21 y
                            8.9e+04

                   4  33:49 1.26+05  1.36 y
                            1.2e+05
                   5  33:55 7.7e+04
                            7.7e+04
                                     0.98 n
1,2,3,4,7,8-HxCDF  6  34:10 1.7e+06  1.25 y
                            1.7e+06
1,2,3,6,7,8-HxCDF  7
2,3,4,6,7,8-HxCDF  9
   34:15 8.7e+05  1.22 y
         8.7e+05

   34:27 1.7e+05  1.23 y
         1.7e+05

   34:37 6.5e+05  1.28 y
         6.5e+05
                   10 34:47 2.6e+04
                            2.66+04
                                     1.02 n
1,2,3,7,8,9-HxCDF  11 35:12 l.Se+05  1.26 y
                            1.56+05
                    12 35:19 6.0e+03
                            6.0e+03
                  1.14 y
          Cone

           0.30
               •a

           0.71
               £

           0.04
               4
               4
           0.06

               C
           0.03


           0.81
               c

           0.33
               4

           0.08
               c

           0.28


           0.01
               3
               :
           0.08
               £
               e
           0.00
    unnamed
    unnamed
                                                      Area  Height
                                  S/N  Mod?
 3.86+05  1.4e+05  7.06+01  y  n
 2.9e+05  l.le+05  6.5e+01  y  n
I
 8.9e+05  3.26+05  1.6e+02  y  n
 7.1e+05  2.5e+05  1.5e+02  y  n

  .9e+04  1.5e+04  7.7e+00  y  n
 4.0e+04  1.3e+04  7.8e+00  y  n
S
 7.2e+04  2.36+04  1.2e+01  y  n
 5.36+04  1.8e+04  l.Oe+01  y  n
3
 3.8e+04  1.3e+04  6.8e+00  y  n
 3.9e+04  1.2e+04  7.le+00  y  n
 9.46+05 2.8e+05 1.4e+02 y  n
 7.5e+05 2.2e+05 1.3e+02 y  n
3
 4.8e+05 1.4e+05 7.2e+01 y  n
 3.9e+05 1.2e+05 6.8e+01 y  n
3
 9.5e+04 2.4e+04 1.2e+01 y  n
 7.76+04 l.Se+04 l.le+01 y  n
3
 3.6e+05 l.Oe+05 5.3e+01 y  n
 2.8e+05 7.6e+04 4.5e+01 y  n
L
 1.36+04 3.96+03 2.06+00 n  n
 1.36+04 3.3e+03 2.06+00 n  n

 8.46+04 2.1e+04 l.le+01 y  n
 6.7e+04 1.6e+04 9.5e+00 y  n
                                                   3.2e+03 9.9e+02 5.1e-01 n  n
                                                   2.8e+03 1.5e+03 8.86-01 n  n
                                                                    Page  6  of  8

  Ent:  44 Name: Total  Hexa-Dioxins   F:3  Mass:  389.816  391.813 Mod? no   #Hom:10

  Run:  19 File: a!7ju!98b     S:14 Acq:18-JUL-98 02:32:07  Proc:20-JUL-98  09:09:09
  Tables: Run: a!7ju!98b  Analyte: m8290-23-»   Cal: m8290-23-»Results: M8290-23»
  Version: V3.5 17-APR-1997  11:14:34  Sample text:  1070-5 xl/2
    Amount:  3.69
      Cone:  3.69
    Tox #1:  -
 Name
 of which 0.38
 of which 0.38
     Tox #2: -

 #     RT Respnse
 named and 3.30
 named and 3.30
       Tox #3: -
                                         RA
                    1   33:52  3.7e+05   1.19  y
                             3.7e+05

                    2   34:11  5.6e+06   1.28  y
                             5.6e+06
           Cone

            0.18

                ]
            2.68
    unnamed
    unnamed
                                                       Area  Height
                                   S/N  Mod?
                                 2.0e+05  7.5e+04  2.9e+01  y  n
                                 1.7e+05  5.9e+04  3.2e+01  y  n

                                 3.2e+06  l.le+06  4.2e+02  y  n

-------
















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-------
OPUSquan   20-JUL-1998
                   Page 8
                                                                    Page 7 of 8

 Ent: 45 Name: Total Hepta-Furans  F:4  Mass: 407.782 409.779 Mod? no   #Hom:4

 Run: 19 File: a!7ju!98b    S:14 Acq:18-JUL-98 02:32:07 Proc:20-JUL-98 09:09:09
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-5 xl/2
   Amount: 0.75
     Cone: 0.75
   Tox #1: -
Name
of which 0.60
of which 0.60
     Tox #2:  -

#     RT Respnse
named and 0.15
named and 0.15
      Tox #3: -
                                        RA
1,2,3,4,6,7,8-HpCDFl  36:22 8.7e+05  0.95y
                            8.7e+05

                   2  36:34 l.le+05  1.00 y
                            l.le+05

                   3  36:40 1.2e+05  1.42 n
                            1.26+05

l,2,3,4,7,8,9-HpCDF4  37:32 7.8e+04  1.47 n
                            7.8e+04
          Cone

           0.54
               4
               4
           0.07
               C
               c
           0.08
               e
               4
           0.06
unnamed
unnamed
                                                      Area  Height
                                  S/N  Mod?
                                 .3e+05 1.3e+05 6.6e+01 y  n
                                 .5e+05 1.4e+05 8.9e+01 y  n

                                5.56+04 1.4e+04 7.26+00 y  n
                                5.5e+04 1.6e+04 l.le+01 y  n
                               3
                                6.9e+04 1.9e+04 9.8e+00 y  n
                                4.8e+04 1.5e+04 9.9e+00 y  n

                                4.6e+04 l.Se+04 7.8e+00 y  n
                                3.16+04 8.6e+03 5.6e+00 y  n
                                                                    Page 8 of 8

 Ent: 46 Name: Total Hepta-Dioxins F:4  Mass: 423.777 425.774 Mod? no   #Hom:3

 Run: 19 File: a!7ju!98b    S:14 Acq:18-JUL-98 02:32:07 Proc:20-JUL-98 09:09:09
 Tables: Run: a!7ju!98b  Analyte: m8290-23-»  Cal: m8290-23-»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text: 1070-5 xl/2
   Amount: 0.96
     Cone: 0.96
   Tox #1: -
Name
of which 0.52
of which 0.52
     Tox #2: -

#     RT Respnse
named and 0.44
named and 0.44
      Tox #3: -
                                        RA
                    1   36:21 3.7e+04  3.10 n
                            3.7e+04

                    2   36:35 7.56+05  0.98 y
                            7.56+05

 l,2,3,4,6,7,8-HpCDD3   37:109.3e+05  0.98y
                            9.3e+05
          Cone

           0.02

               c
           0.42


           0.52
unnamed
unnamed
                                                      Area  Height
                                  S/N  Mod?
                                2.8e+04 9.16+03 4.0e+00 y  n
                                9.1e+03 2.0e+03 2.6e+00 n  n
                               2
                                3.76+05 l.le+05 4.8e+01 y  n
                                3.86+05 l.le+05 1.5e+02 y  n
                               2
                                4.6e+05 1.3e+05 5.5e+01 y  n
                                4.7e+05 1.3e+05 1.6e+02 y  n
                                                                                                  r

-------
File: A17JUL98B Acq: 18-JUL-1998 02:32:07 Exp : EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #14 Text: 1070-5 xl/2 ALS #14
319.8965 S:14 SMO(1,3)
1008
50_
0



24100
321.8936 S:14 SMO(1,3)
100S
50J
0-





24100
331.9368 S:14 SMO(1,3)
100%,
-
50J
0:



24 : 00
333.9339 S:14 SMO(1,3)
100%

50J
o:



24:00
327.8847 S:14 SMO(1,3)
100%
50 1
o:



T 1 1 1 | | |
24:00
316.9824 S:14 SMO(1,3)
100% 23^2123:42
50 j
o:


i i < i i i i ~
24:00
BSUB (128, 15, -3
Al


2s!oo
BSUB (128, 15, -3
Al



25:00
BSUB (128, 15, -3




25IOO
BSUB (128, 15, -3




25:00
BSUB(128,15,-3



i i i i | i
25:00
.0) PKD (3, 3, 3, 0.10%, 1652. 0,1. 00%, F,F)
.56E6
A
/ A8.29E5
A
/I A«
26
.0) PKD (3, 3, 3
.98E6
A
\ A1.13E6
A
I /W
' V / V
26:
.0) PKD (3, 3, 3




' ' ' 26!
. 0) PKD (3, 3, 3




26:
.0) PKD (3, 3, 3



1 I T 1 1
26:
PKD (3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%
3.

43E5 A4.14E5 A2.39E5
Ll.
- n
^•*~i 	 1 	 1 	 1 	 ' r — f * i"""^!""1 \ 	 r*^ 	 1 — <~TV|^ \*~f T" i ^> ' i -*i 	 1 	 1 	 1— i ' - •
00 27:00 28:00 29:00 30:00
, 0.10%, 1248. 0,1. 00%, F,F)
4.

66E5 A5-33E5 A3 . 44E5

_2.

n
°~i i 	 1 	 r "1 	 ] "i"^ 1 — i 	 r*— =*i 	 1 * i Y i^ — r — f 	 1 — «=i 	 1 	 1 i 	 1 	 1 i •
00 27:00 28:00 29:00 30:00
, 0.10%, 7832. 0,1. 00%, F,F)
A1.62E8 3.
A A1.31E8
A
/I /v

_1.
0.
00 27:00 28:00 29:0o' ' ' 30:00
, 0.10%, 4152. 0,1. 00%, F,F)
A2.06E8 4.
AA1.70E8
/ 1 n
A
l\ A

:2.
'• o.
00 27:00 28:00 29:00 30:00
,0.10%,3952.0,1.00%,F,F)
A3.72E8
A
A
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_3.
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i f P i r i i i i i i | i i i i i i i i i i i i
00 27:00 28:00 29:00 30:00
,F,F)
24:26 25jQ3 25:3225:54 26:42 27:11 27:40 28:04 28:27 29:03 29:51 5.


' '! 1 1 1 t""~~'""~"T"
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00 	 27 loO 	 28 100 	 29! 00 	 3o!oO
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Time

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Time

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Time

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8E7
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Time

7E7
9E7
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Time

-------
File: A17JUL98B Acq: 18-JUL-1998 02:32:07 Exp : EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #14 Text: 1070-5 xl/2 ALS #14
355.8546 S:14 F:2 SMO(1,3) BSUB (128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2060 . 0 , 1 . 00%, F, F)
1002
-
so:
-
0'
A1'95E6 A8.35E5
\ A A6.35E5
A
I A
1 V _ J w7 U
3bli2 30124 3ol36 3ol48 3ll6d 31:12 31\24 3ll36 33.1 48 32l6d 32112
357.8517 S:14 F:2 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 1200 . 0 , 1 . 00%, F, F)
1002
-
so:
"
~
0
A6.69E5 A5.25E5
A .
/\ A A4.20E5
A
/ /\ ,
y \ — ^ y \^j vj-

' 3bll2 ' 30124 ' sbls'e ' SoUs" " Sllod ' 3l! 12 ' 33.124 ' 3l] 3 6 ' 31 Us "32l6d " 32Tl2~
367.8949 S:14 F:2 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2212 . 0, 1 . 00%, F, F)
100*
50J
0"



30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12
369.8919 S:14 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1820 . 0 , 1 . 00%, F, F)
100*
50J
OJ



3bli2 30124 30136 3o!48 3i!6o 3i!l2 3l!24 3l!36 3l!48 32:00 32^12
366.9792 S:14 F:2 SMO(1,3) PKD (3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
lOOi 30:27 30:49 31:04 31:30 31:56
so:
0'


30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12





A2.47E5
T— vyv~v_/\__^^ A8 .04^E4
3.3E5
-
11.7E5

' O.OEO
32124 32136 32U8 33l6d 33ll2 Time

r2.2E5


A1.52E5
.jl6E4/\^A8^0lE4 A3 ^ 68E4


_1.1E5


O.OEO
32124 32i36 32148 33l6d 33112 Time

A1.45E8
A
/ v_
5.1E7
L2 . 6E7
' O.OEO
32:24 32:36 32:48 33:00 33:12 Time

A9.20E7
A
ft
/ L
_3.2E7
11.6E7
"O.OEO
32124 32136 32148 33l6d 33112 Time

32^24 33:10 6.4E7


_3.2E7
.O.OEO
32124 32136 32148 33l6d 33112 Time
CO

-------
File
Samp
389.
1003
50_
0
391.
1002
50J
0"
401.
1002;
so:
0"
403.
100%,
so:
0'
380.
100%;
so:
o:

>: A17JUL98B Acq: 18-JUL-1998 02:32:07 Exp : EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
)le #14 Text: 1070-5 xl/2 ALS #14
8156 S:14 F:3 SMO(1,3) BSUB (128, 15 , -3 . 0) PKD(3 , 5, 2 , 0 . 10% , 2580 . 0 , 1 . 00% , F, F)
A3.16E6
A
/I...,.
33:24 33:36 33:48 34:00 34:12 34:24 34:36 34 48 35:00 35:12 35:24 35:36 35:
8127 S:14 F:3 SMO(1,3) BSUB (128 , 15, -3 . 0 ) PKD (3 , 5, 2 , 0 . 10%, 1804 . 0 , 1 . 00%, F, F)
A2.47E6
A
/ \
ai imy^. / \ A3 . 06E5
f\J. m 1 \J Cl J / \ ^~^
33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35
8559 S:14 F:3 BSUB(128, 15, -3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 6340 . 0 , 1 . 00%, F, F)
A1.47E8 'I E
A A A

33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35
8530 S:14 F:3 BSUB(128, 15, -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 8728 . 0 , 1 . 00%, F, F)
A1.42E8
A1.17E8 A
AV IV
33J24 33136 33!48 34loO 34!l2 34!24 34136 34148 35!oO 3s!l2 35!24 3s!36 35!
9760 S:14 F:3 SMO(1,3) PKD (3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
33:33 33:54 34^LD 34:18 34:36 35:00 35U6 35:24 35:33

33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:
igm
1.1E6
L5.4E5
" 0 OEO
48 Time
8.3E5
_4.1E5
O.OEO
48 Time
6.9E7
L3.4E7
" 0 . OEO
48 Time
5.5E7
12 . 8E7
O.OEO
48 Time
1.3E8
16.7E7
O.OEO
48 Time

-------
File: A17JUL98B Acq: 18-JUL-1998 02:32:07
Sample #14 Text: 1070-5 xl/2 ALS #14
423.7767 S:14 F:4 SMO(1,3) BSUB (128, 15, -3 . 0 )
10°^ A3.71E5
/I
' A2.83E4 / V
36:00 36:12 36!24 36!36 36:48 37:
425.7737 S:14 F:4 SMO(1,3) BSUB (128, 15 , -3 . 0)
100^ A3.77E5
/I
°" i / ^
36!6d 36!l2 36!24 36!36 SeUs 37!
435.8169 S.-14 F:4 SMO(1,3) BSUB(128, 15, -3 . 0)
100S
so:
36:00 36:12 36:24 36:36 36:48 37:
437.8140 S:14 F:4 SMO(1,3) BSUB (128, 15, -3 . 0)
100%
so:
0" 	 r
Exp: EXP_M23_DB5_OVATION Voltage SIR EH- GC Autospec-UltimaE Parad
PKD (3, 3, 3, 0.10%, 2292. 0,1. 00%, F,F)
A4 . 59E5
/ y A3.26E4
00 37:12 37:24 37:36 37:48 38:00 38:12 3s!24 3s!36 38!48 39
PKD (3, 3, 3, 0.10%, 780. 0,1. 00%, F,F)
A4.70E5
66 37!i2 37!24 37!36 37!48 38!66 38!l2 38!24 38!36 38!48 39!
PKD(3,3,3,0.10%,2544.0,1.00%,F,F)
Al . 02 E8
00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39
PKD (3, 3, 3, 0.10%, 1524. 0,1. 00%, F,F)
A9 . 7 5E7
igm
1.3E5
L6.5E4
00 Time
1.3E5
_6.4E4
_O.OEO
00 Time
2.7E7
-1.4E7
0 OEO
00 Time
_2.6E7
_1.3E7
O-OFO
" ' i i i i i i i i i i i i i i i i i i i i iri 7 i i i i i -r i i i-i i i i r- 1 i i -I- 1 i i i -T i i i v i i | ri— rT-v'i i i- i i— i -T i i -i r t i -r-t i i i— TTT i i i i r i i i i i i i i i i i 	 -
36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:00 Time
430.9728 S:14 F:4 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
lOOi 36:1236:22 36:46 37:03 37:21 37:3337:43 38:07 38:22 38:39 38:53 R . 9F.7
so;
36!6d 36!i2 36!24 36 ! 36 ' 36 ! 48 ' 37 !

_4.4E7
^O.OEO
00 37:12 37:24 37:36 37:48 38:00 38:12 38:24 38:36 38:48 39:00 Time
en

-------
File
Samj
457
1003
50.
0
459.
100S
50:
0'
469.
iooa
so:
0"
471.
1002
so:
0
454.
100%
so:
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?: A17.JUL98B Acq: 18-JUL-1998 02:32:07 Exp : EXP M23 DB5 OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
3le #14 Text: 1070-5 xl/2 ALS #14
7377 S:14 F:5 SMO(1,3) BSUB(128, 15, -3 . 0 ) PKD(3 , 3 , 3 , 0 . 10% , 872 . 0 , 1 . 00% , F, F)
\ A3 . 34E5 7 . 8E4
J\_
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41
7348 S:14 F:5 SMO(1,3) BSUB(128 , 15, -3 . 0 ) PKD(3 , 3 , 3 , 0 . 10%, 1248 . 0 , 1 . 00%, F, F)
A3 . 50E5
/V_
39!l2 ' 39!24 ' ' ' 39136 ' ' 39^8 ' ' ' 4o!ob ' ' ' 4o!l2 ' ' ' 40^24 ' ' ' 4ol36 ' ' ' 4'oUs 41
7780 S:14 F:5 SMO(1,3) BSUB(128 , 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2420 . 0 , 1 . 00%, F, F)
A1.28E8
J\_
39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 4ol48 41
7750 S:14 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1688 . 0 , 1 . 00%, F, F)
Al . 45E8
J\_
39\12 39124 39136 39!48 4o!ob 4o!l2 4o!24 4o!36 4o!48 4l!
9728 S:14 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
39:08 39:16 39^23 39^40 39:48 40:04 40:33 40:54
/
39!l2 39124 39136 39.-48 4o!ob ' 4o!l2 4ol24 ' 4o!36 ' ' ' 4ol48 41
_3.9E4
_O.OEO
00 Time
8 . OE4
_4.0E4
_O.OEO
00 Time
2 . 9E7
11.4E7
•Q.OEO
00 Time
_3.2E7
11.6E7
"O.OEO
00 Time
9.8E7
_4 . 9E7
O.OEO
00 Time

-------
File: A17JUL98B Acq: 18-JUL-199« 02:32:07 Exp: EXP M23
Sample #14 Text: 1070-5 xl/2 ALS #14
303.9016 S.-14 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%
100% A3.47E6
: A A2-
^ Ai-r6 A9.36E5 A2A4E6 ^ Ai-/n
0: A /\ A / WT V /r\ A/V 1
24100 25:00 26loO
305.8987 S:14 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%
100% A4.36E6
' A A3-
50" A1.94E6 A3.11E6 A1 7opfi
A A1.23E6/ f\ ~ A1-'^bl
„; A A A /VvA /f\ AA /
24:00 25:00 26:00
315.9419 S:14 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%
1001
50J
o;
24:00 25:00 26:00
317.9389 S:14 SMO(1,3) BSUB(128 , 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%
100%
0:
_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
,1948.0,1.00%,F,F)
A3.84E6
47E6 A
(W.UE^ A A8.35E5
27:00 28:00 29:00 30
,3132. 0,1. 00%, F,F)
A4.91E6
Cl 37- A
TV A|6-AOE5/ I A1A3E
-------
File: A17JUL98B Acer: 18-JUL-1998 02:32:07 Exp : EXP M23 DB5 OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #14 Text: 1070-5 xl/2 ALS #14
339.8597 S:14 F:2 SMO(1,3) BSUB(128 , 15 , -3 . 0) PKD ( 3 , 3 , 3 , 0 . 10%,
1002

50J
0_
A3.07E6
A A1.8
A1.39E6 / \ A
y^ /V tA8E5 /
3oli2 36124 36136 36148 31.166 33.112 31.124 3ll36 31
341.8568 S:14 F:2 SMO(1,3) BSUB(128 , 15 , -3 . 0 ) PKD(3 , 3 , 3 , 0 . 10%,
1002

50J
o:
A1.96E6
A A1.2
A9.07E5 / \ A
S\ A/ t^E5 / }

30il2 30124 30i36 30:48 31iOO 31:12 31:24 31:36 31,
351.9000 S:14 F:2 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%,
100%
~
50J
OJ




36112 36124 3Q\36 SoUs 33.166 33.112 31.24 33.136 31
353.8970 S:14 F:2 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% ,
100%
50J
o"



301l2 30:24 30136 30:48 31:00 31:12 31:24 31:36 31
409.7974 S:14 F:2 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 100 . 00
100%
-
50J
-
o •
31
/

31:39 /
S\ J
"'i 1 i | i i i 1 1 1 1 1 i i 1 1 1 i 1 1 1 1 1 i 1 1 i 1 -r 1 1 I-T'T-I I 11-r-r I1 i i T-T— r t i I i T
30:12 30:24 30136 30:48 31:00 31:12 31:24 31:36 33
366.9792 S:14 F:2 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
100%
50 j
o"
30:27 30:49 31:04 31:30


292.0,

E6

^ /r
Us 3
1276.0,

!E6
v /T

:48 3
.756.0,

Al .7
A
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284.0,

Al.li
A
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Us 3:
,3932.
47
1 31

V /-/
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:48 3:

31:5


30:12 30:24 30:36 30:48 ,31:00 31:12 31:24 31:36 31 48 31
1.00%,F,F)


A7.80E5 A9.12E5
vVv A/V ^
8.2E5

L4.1E5
: O.OEO
2166 32:12 32124 32l36 32l48 33166 33ll2 Time
1.00%,F,F)


AC n OT^C Ao . 0 OE5
v ™ AA _

5.4E5

_2.7E5
_O.OEO
2:00 32:12 32:24 32:36 32:48 33:00 33:12 Time
1.00%,F,F)
A2.83E8
A
3E8 /I

v / I
1.0E8

_5.1E7
O.OEO
2166 32li2 32124 32136 32148 33166 33112 Time
1.00%,F,F)
Al . 80E8
3E8 /\
^ / V
6.6E7
_3.3E7
- O.OEO
1:66 ' 32112 ' 32124 ' 32136 ' 32148 33166 33112 Time
0,1.00%,F,F)

58
\
\ 32-29

1.8E5
;
_9.2E4

O.OEO
!-loO 32:12 32:24 32:36 32:48 33:00 33:12 Time

6 ^12-L24 33:10


6.4E7
L3.2E7
-O.OEO
166 32112 32124 32: 36 32 Us ' 33 1 66 ' 33 1 12 Time
on

-------
File: A17JUL98B Acq: 18-JUL-1998 02:32:07
Sample #14 Text: 1070-5 xl/2 ALS tt!4
373.8207 S:14 F:3 SMO(1,3) BSUB(128 , 15 , -3 . C
lOOi A8.89E5 A9 3g
A ' f\
50.
o:
375.
1002
50_
0
383.
lOOi
50J
o:
385.
100*
50 j
o:
445.
100%
o:
380.
100%
50J
o:
A3.82E3 \
A / \

33:24 33:36 33:48 ' 34:00
8178 S:14 F:3 SMO(1,3) BSUB(128,15
A7.14E5
A2.90E3 \
J\J \V___A5.27E4
33!24 33136 33Us 34loO
8639 S:14 F:3 BSUB(128, 15, -3 . 0) PK

33:24 33:36 33:48 34:00
8610 S:14 F:3 BSUB (128, 15 , -3 . 0) PK

33! 24 33:36 3s! 48 34^00
7555 S:14 F:3 SMO(1,3) BSUB (128, 15
34
y
33.1 24 33136 33 .-48 34. -00
9760 S:14 F:3 SMO(1,3) PKD(3,3,3,1
33:33 33:54
/
/
34
-3.(
7.51
i\
A
/
34!
(3 c
1.09
A
A
34
2f
A
34
-3.(
34
\J
Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
) PKD (3, 5 ,2, 0.10%, 1956. 0,1. 00%, F,F)
C5 3.2E5
A A3'

12 34:24 34:
} PKD (3, 5, 2, 0.10%
55
A A2-
f \ 	 A7.70E4 /
— r 	 1 r —
12 34i24 34!
,2, 0.10%, 25996.0,:
E8
/V ,
12 34:24 34:
,2,0.10%,62072.0,:
/v
12' ' '34 124' ' '34!
) PKD(3,3,3,100.0(
12
v_ /
34 12 34:24 34 !
52E5
\_ A8.43E4
' — r-T" r-T— T- i T — i — r 	 i — i — i — i — i- i T f~*l — i — i — i — i — i — r— r — i — i — i — i — i — r— 1 — i — l —
36 34:48 35:00 35:12 35:24 35:36 35
1692. 0,1. 00%, F,F)
)4E5
\ Ao . oc?E4
r i 1 I 1 I l l i i '1 1 l l 1 1 i i i 1 i ' i -T-'l — i i l l i i i — i i i i
36 34:48 35:00 35:12 35:24 35:36 35
.00%,F,F)

36 34:48 35:00 35:12 35:24 35:36 35
.00%,F,F)

^6 34148 3s!oO 35!l2 3s!24 35:36 35
%,2460.0,1.00%,F,F)
-^7 34:45 34:57
^-^^/^ 	 J^iL- 	 35-40
L1.6E5
i.O.OEO
48 Time
2.5E5
_1.3E5
.O.OEO
48 Time
5.3E7
-2.7E7
O.OEO
48 Time
1.0E8
-5.1E7
O.OEO
48 Time
_9.3E4
_4.6E4
O.OEO
6 34:48 35:00 35:12 35:24 35:36 35:48 Time
0.00%,0.0,1.00%,F,F)
34J.O 34:18 34:36 35:00 35:16 35:24 35:33
/^

33:24 33:36 33:48 34:00 34 12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35:'
1.3E8
-6.7E7
O.OEO
J8 Time

-------
    'File:  A17JUL98BAcq:  18-JUL-1998 02:32:07Exp:  EXP_M23_DB5_OVATION Voltage SIR EI +GC Autospec-UltimaEParadigm
    Sample #14   Text:  1070-5 xl/2  ALS #14
    407.7818  S:14  F:4 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3 , 0.10%, 1964.0 ,1.00%,F,F)
    100%,              A4.26E5                                                                                        1.3E5
  50J

   OJ
                                  A6.89E4
                                                               A4.64E4
            36:00  36:12  36:24  36:36  36:48  37:00  37:12   37:24  37:36  37:48  38:00  38:12  38:24  38:36
     409.7788  S:14 F:4  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1532.0,1.00%,F,F)
     100%              A4.48E5
               _6.5E4

                O.OEO
  50J

   OJ
            39:00

                1

               _6
                                .48E4
                                                               A3.15E4
           36:00  36:12  36:24  36:36  36:48  37:00  37:12  37:24  37:36  37:48  38:00  38:12  38:24  38136 ' 38 Us '  3gloO
    417.8253  S:14  F:4  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,7868.0,1.00%,F,F)
    100%                                                      A6.28E7
        -               A4.01E7
      501

       OJ_
                                                                                                                  1.

                                                                                                                 _8.

                                                                                                                  0,
           36:00  36:12  36:24  36:36  36:48  37:00   37:12  37:24  37:36  37:48  38:00  38:12  38:24  38:36   38:48  39:00
419.8220 S:14 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,24240.0,1. 00%, F, F)
100%,                                                      A1.43E8
                  A8.88E7
      Oj
                                                                                                                      3 .
                                                                                                                      .1
         i i i i  I i i i i i I  i i f 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 r i i i i ii I I i I I i  i i i i I	iii—i i i I i i  i i i | i i i  i i I i i i  i i I
           36:00  36ll2  36124  36:36  36:48   37:00   37:12  37:24  37:36  37:48  38:00  38:12  38:24   38:36   38:48   39:00
    479.7165 S:14 F:4 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,100.00%,2940.0,1.00%,F,F)
    100%                                           37;10
     50
      o
          35:58
                                3643
                                                         3720
                1

               16,

               Lo.
           36166 ' 36 lid ' 36124 ' 36136 ' 36:48   37:00  37:12  37:24  37:36  37:48  38:00  38:12  38:24   38:36  38:48  39:00
  Time

.4E5

. 9E4

.OEO
  Time

.7E7

,5E6

,OEO
  Time

,8E7

,9E7

,OEO
  Time

,2E5

 OE4

 OEO
  Time
430.9728 S:14 F:4 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100%, 	36_LJ.2 36:22	3_6j_46     37:03	37:2JL_37:33 37:43	38:01
     50J
      o
                                                                                             38:22
18:39   38:53   8.9E7

               _4.4E7
       36:00  36:12  36:24  36:36   36:48  37:00  37:12  37:24  37:36  37:48  38:00
                                                                                              38124  38136  38 Us  39loO
                  OEO
                   Time
c/r
O

-------
File: A17JUL98B Acq: 18-JUL-1998 02:J2:0
Sample #14 Text: 1070-5 xl/2 ALS #14
441.7427 S:14 F:5 SMO(1,3) BSUB (128, 15 , -3
100%
50 J
0 '


^^^ 	
— I 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 I 	 1 	 r — r
39:12 39:24 39:36
443.7398 S:14 F:5 SMO(1,3) BSUB (128, 15 , -3
100%
50 j
o'


	 • — — 	 	 	 • — 	 	 	 	 — -~ — - -
39:12 39:24 39:36
469.7780 S:14 F:5 SMO(1,3) BSUB(128, 15, -3
100%
50 j
0 '



39:12 39:24 39:36
471.7750 S:14 F:5 SMO(1,3) BSUB(128, 15, -3
100%
50 j
n •


" ' i — i — i T i i 	 r— i — i — i — | 	 1 — i — i — T " i | i i i
39:12 39:24 39:36
513.6775 S:14 F:5 SMO(1,3) BSUB (128, 15, -3
100%,
-
50 j
0 '


3^_ /^^39:34 3/^
u-j — i — i — i — i — i — i — i — i — i — i—i • i i i i i | i i i
39:12 39:24 39:36
7 Exp: EXP_M23_DB5_OVATION Voltage

SIR EI+ GC Autospec-UltimaE Paradigm

.0) PKD(3,3,3,0.10%,960.0,1.00%,F,F)
A4.48E4
/ \
/ \4_,J55E3
•r-r [-T-^r^T^rT | 1 1 I I 1 | 1 1 1 i
39:48 40:00 40:12
.0) PKD (3, 3, 3, 0.10%, 1744. 0,1. 00%, F,
A6 . 70E4
/\
_ _ 	 / ^^/^
39:48 4o!ob 4o!l2
.0) PKD (3, 3 ,3, 0.10%, 2420. 0,1. 00%, F,
Al . 28E8
/\
J \^__
39:48 40:00 40:12
.0) PKD (3, 3, 3, 0.10%, 1688. 0,1. 00%, F,
Al . 4 5E8
/\

39 Us 40!00 40ll2
.0) PKD (3, 3, 3, 100. 00%, 1016. 0,1. 00%,
40:16
40:01 40:08 A
_/^vV\y

39:48 40:00 40:12
454.9728 S:14 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
1004 TO-no TQ.tfi TQ.9T 39:40 39:48 40:04
50J
n -
r

U— ' 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 T' - I | 1 1 I | 1 1 1
39:12 39:24 39:36


39U8 4o!ob 4o!l2


	 	 _^____^--^_
1.3E4
i_6.3E3
: O.OEO
40:24 40:36 40:48 41 00 Time
F)


• — - — - — s s^ 	 	 — ^ — ••• — _^ — . 	 . 	 v
1.8E4
_9.0E3
O.OEO
40:24 40:36 40:48 41 00 Time
F)



2.9E7
_1.4E7
.O.OEO
40:24 40:36 40:48 41 00 Time
F)



3.2E7
L1.6E7
: 0 . OEO
40:24 40:36 40:48 41:00 Time
F,F)
40 • 39
A

\2^\^J ^^-^^-^^r^
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L3.2E3
_O.OEO
40:24 40:36 40:48 41:00 Time
40:33 40:54 _9.8E7


L4.9E7
: O.OEO
40:24 40:36 40:48 41:00 Time

-------
cn
        OPUSquan   22-JUL-1998
                          Page 1
                                                                                                                                                     Page 11
                 Filename
                   Sample
                 Acquired
                Processed
                Sample ID
                Cal Table
            Results Table
                 Comments
         Typ
         Unk
         ES/RT
        a21ju!98f
        6
        21-JUL-98  23:12:05
        22-JUL-98  08:32:29
        1070-5 xl/2
        07feb-m23conf
        M8290-23-072198F
         Total
         DPE
         LMC
      2,3,7
  13C-2,3,7
      Tetra
            HxCDPE;
QC CHK ION (Tetra);
   Name;
,8-TCDF;
,8-TCDF;
 Furans;
    Resp;
3.73e+06;
8.56e+08;
1.306+08;
   Ion 1;
1.67e+06;
3.75e+08;
3.54e+06;
   Ion 2;
2.06e+06;
4.81e+08;
4.59e+06;
  RA;?;
0.81;y;
0.78;y;
0.77;y;
   RT;
27:56;
27:53;
18:11;
   Cone;       DL;
  0.459;   0.0259;
209.890;
 15.967;   0.0259;
                                             ;NotFnd;
                                             ;NotFnd;
S/N1;?;
  94,-y ;
1215,-y;
 315;y;
   *;n
DivO;n
S/N2;?
  45,-y
1959,-y
 165;y
mod?
  no
  no
  no
  no
  no
                                                                         -;-;  27:56
                                                                         -;-;  27:56

-------
OPUSquan   22-JUL-1998
                                      Page 1
 Ent: 3  Name: Tetra Furans
                                                 Page  1  of  1

                F:l  Mass:  303.902  305.899 Mod? no   #Hom:28
 Run: 11 File: a21ju!98f    S:6  Acq:21-JUL-98 23:12:05  Proc:22-JUL-98  08:32:29
 Tables: Run: a21ju!98b  Analyte: m23_conf    Cal:  07feb-m23»Results: M8290-23»
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  1070-5 xl/2
   Amount: 15.97
     Cone: 15.97
   Tox #1: -
Name
of which 0.46
of which 0.46
     Tox #2:  -

#     RT Respnse
named and 15.51
named and 15.51
      Tox §3:  -
                                        RA
                   1  18:11 S.le+06  0.77 y
                            S.le+06

                   2  18:20 1.9e+04  1.95 n
                            1.9e+04

                   3  19:51 7.6e+06  0.78 y
                            7.6e+06

                   4  20:06 5.9e+06  0.81 y
                            5.9e+06

                   5  20:21 l.Oe+07  0.79 y
                            l.Oe+07

                   6  20:39 4.5e+06  0.84 y
                            4.5e+06

                   7  21:12 5.4e+06  0.79 y
                            5.4e+06

                   8  21:32 6.8e+06  0.78 y
                            6.8e+06

                   9  21:49 5.0e+05  0.70 y
                            5.0e+05

                   10 21:58 9.3e+05  0.84 y
                            9.3e+05

                   11 22:09 6.0e+06  0.79 y
                            6.0e+06

                   12 22:34 3.8e+06  0.77 y
                            3.8e+06

                   13 23:17 1.2e+07  0.76 y
                            1.2e+07

                   14 23:27 6.6e+06  0.82 y
                            6.6e+06

                   15 24:19 6.2e+06  0.78 y
                            6.2e+06

                   16 24:31 4.2e+05  0.47 n
                            4.2e+05

                   17 25:00 7.4e+06  0.77 y
                            7.4e+06

                   18 25:27 3.7e+06  0.81 y
                            3.7e+06

                   19 26:33 4.9e+06  1.54 n
                            4.9e+06
                           Cone

                            1.00
                               T
                               4
                            0.00
                               ]
                               e
                            0.94

                               4
                            0.72


                            1.22
                               4
                               C
                            0.55


                            0.67


                            0.83


                            0.06


                            0.11
                               <
                               C
                            0.74


                            0.47
                               ]

                            1.47
                               C
                               (
                            0.81


                            0.76
                               2
                                3
                            0.05
unnamed
unnamed
                                                      Area   Height
                                  S/N  Mod?
               3.5e+06 7.0e+05 3.1e+02 y  n
                .6e+06 9.2e+05 1.6e+02 y  n

               1.3e+04 5.8e+03 2.6e+00 n  n
               6.6e+03 3.8e+03 6.9e-01 n  n
              1
               3.3e+06 5.8e+05 2.6e+02 y  n
               4.3e+06 7.4e+05 1.3e+02 y  n

               2.6e+06 4.2e+05 1.9e+02 y  n
               3.2e+06 5.5e+05 9.8e+01 y  n

               4.4e+06 7.4e+05 3.4e+02 y  n
               5.6e+06 9.7e+05 1.7e+02 y  n

               2.0e+06 3.2e+05 1.4e+02 y  n
               2.4e+06 3.9e+05 7.0e+01 y  n
              7
               2.4e+06 4.2e+05 1.9e+02 y  n
               3.06+06 5.46+05 9.6e+01 y  n
               3.06+06 4.16+05 1.8e+02 y  n
               3.8e+06 5.2e+05 9.3e+01 y  n
              5
               2.0e+05 6.4e+04 2.9e+01 y  n
               2.9e+05 9.0e+04 1.6e+01 y  n

               4.2e+05 l.le+05 5.0e+01 y  n
               5.1e+05 1.3e+05 2.3e+01 y  n
              1
               2.6e+06 4.8e+05 2.2e+02 y  n
               3.3e+06 6.16+05 l.le+02 y  n

               1.7e+06 2.8e+05 1.3e+02 y  n
               2.2e+06 3.96+05 6.9e+01 y  n
              7
               5.2e+06 6.7e+05 3.Oe+02 y  n
               6.86+06 8.76+05 1.6e+02 y  n

               3.0e+06 4.2e+05 1.96+02 y  n
               3.6e+06 5.4e+05 9.6e+01 y  n
               2.76+06 3.7e+05 1.7e+02 y  n
               3.56+06 4.66+05 8.3e+01 y  n
                                1.3e+05 3.2e+04 1.5e+01 y  n
                                2.96+05 4.46+04 7.8e+00 y  n
                            0.91
                                3.26+06 4.1e+05 1.9e+02 y  n
                               •4.2e+06 5.4e+05 9.7e+01 y  n
                            0.46
                                1.7e+06 2.16+05 9.46+01 y  n
                                2.1e+06 2.6e+05 4.7e+01 y  n
                            0.60
                                2.9e+06 3.6e+05 1.6e+02 y  n
                                1.96+06 4.5e+05 B.le+Ol y  n

-------
OPUSquan   22-JUL-1998
                                      Page  2
                   20 27:33  6.2e+06   0.78 y    0.76
                            6.26+06

2,3,7,8-TCDF       21 27:56  3.7e+06   0.81 y    0.46
                            3.7e+06

                   22 28:14  5.2e+04   2.15 n    0.01
                            5.26+04

                   23 28:32  5.3e+06   0.81 y    0.65
                            5.3e+06

                   24 29:17  3.8e+06   0.87 y    0.47
                            3.8e+06

                   25 29:36  3.5e+06   0.40 n    0.43
                            3.56+06

                   26 29:38  3.4e+06   0.35 n    0.41
                            3.4e+06                8

                   27 31:24  4.4e+04   7.94 n    0.01
                            4.4e+04

                   28 31:51  3.2e+06   1.15 n    0.39
                            3.26+06
,7e+06 3.2e+05 1.
,5e+06 3.9e+05 7.

.7e+06 2.1e+05 9.
.le+06 2.5e+05 4.

.5e+04 1.3e+04 6,
,7e+04 9.1e+03 1,

,4e+06 2.7e+05 1.
,9e+06 3.3e+05 5.

,8e+06 1.9e+05 8.
.Oe+06 2.3e+05 4,

,9e+05 2.0e+05 9,
,5e+06 2.7e+05 4,

,7e+05 1.9e+05 8,
 5e+06 2.7e+05 4,

.9e+04 l.le+04 5,
,9e+03 4.7e+03 8,

.7e+06 1.66+05 7
,5e+06 1.6e+05 2
5e+02 y  n
Oe+01 y  n

4e+01 y  n
5e+01 y  n

Oe+00 y  n
6e+00 n  n

2e+02 y  n
9e+01 y  n

5e+01 y  n
2e+01 y  n

2e+01 y  n
9e+01 y  n

6e+01 y  n
9e+01 y  n

le+00 y  n
4e-01 n  n

le+01 y  n
8e+01 y  n
                                                                                                   i<  154

-------
File: A21JUL98F Acq: 21-JUL-1998
Sample #6 Text: 1070-5 xl/2 ALS
303.9016
100S
50 1
o:



16
305.8987
100S
50 j

o:





16
315.9419
100%
50J
oj



16
317.9389
100%
50J
o:



16
375.8364
1002

50 j
o:

JkJ .
r/fffV

16
316.9824
S:6



lob
S:6





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16

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loo
S:6
SMO(1,3) BSUB{128,15
A3.54E6
i

11
isloo
A4.4
y
P
20:00
SMO(1,3) BSUB(128,15
A4.59E6




18:00
A5.5
ii
1 A


20:00
SMO(1,3) BSUB(128,15



islob



2olob
23:
#6
,-3.
1E6
A2.
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—3
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A3.
*
A


-3.




SMO(1,3) BSUB(128,15,-3.



' islob



2olob




SMO(1,3) BSUB(128,15,-3.
:38
ll 18:15
v i A, i\ J «k,


18:00
SMO(1,3) PKD(3
100% 16:17 18:34
50 j
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18:00


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0) PKD(3,3



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22:24
ii flL 111 1 L.
jyH^AvHWV^

22:00
: M23_DB225 Voltage SIR EI+ GC Autospec-UltimaE Paradigm

,3,0.10%,
.17E6
i



2212. 0,1. 00%, FrF)

A3.23E6 A2.95E6
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III A™
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t
AA T A
26-00
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: o
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.5E5
.7E5
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Time
5592. 0,1. 00%, F,F)

A4.17E6 A1.91E6
y\ A
'Ii ,A-

24lob
,3,0.10%,



24lob
,3,0.10%,



24lob
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26:00
34324.0,1.00%,



26100
27188.0,1.00%,



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9

. A2 . 94E6
A A A A A A1.48E6
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28:00 30:00 32:00 34:00
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, 3, 100. 00%, 11560. 0,1. 00%, F,F)

24:03
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26:00
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27k,5, 28:56 29:59 31:41 f 33.58
1 1 IT .1 L. *• J i A kl fill 1 1 ulh 1 IJillAl ii u. UnllLhJ t > lJ.1 J ui
\w WV^WVMW
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, 3, 3, 100. 00%, 0.0,1. 00%, F,F)
19:46


T 1 1 I—
20:00
21:3.0 22:4923:47






— i i i i r— r
22:00


r i i 	 1 	 1
24:00
25:09 26:18_


• 	 1 	 1 	 1 	 ] 	 1 	 1 	 1 	
26:00
27:49 29:05 30:1631^.13 32:4933:48 6


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0

28:00 30:00 32:00 34:00
.9E7
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Time
tn
c/i

-------
                           Section 4
                        Svstein PerfoKmanc
                           Section 4-1
         Mass Spectrometer Performance Check
                       Mass Resolution
                  Documentation for the Analysis
                              of
         Polychlorinated Dibenzo-/i-Dioxins & Dibenzofurans
cn

-------
                   Peak Locate Examination:17-JUL-1998:16:42  File:A17JUL98B
                  Experiment:EXP_M23_DB5_OVATION Function:! Reference:PFK317
PPM
200
 Volts
2.3390
292.95315  292.98245  293.01175
 Volts
1.1178
        304.95195  304.98245  305.01295
 Volts
0.7482
        316.95075  316.98245  317.01415
                         Volts
                        2.9977
330.94615  330.97925  331.01235
                         Volts
                        0.9412
366^.94255  366.97925  367.01595
                                Volts
                                2.6891
        342.94495  342.97925  343.01355
                                Volts
                                2.1965
        380.93795  380.97604  381.01414
                                 Volts
                                1.3903
        354.94375  354.97925  355.01475
  C/l

-------
                   Peak Locate Examination:18-JUL-1998:04:00 File:A17JUL98B
                  Experiment:EXP_M23_DB5_OVATION Function:! Reference:PFK317
292.95315  292.98245 293.01175
                         Volts
                        2.3195
330.94615  330.97925 331.01235
                                                         Volts
                                                        0.8423
304.95195  304.98245  305.01295
                         Volts
                        1.9680
342.94495  342.97925  343.01355
                                                         Volts
                                                        0.5709
316.95075  316.98245  317.01415
                         Volts
                        1.0102
354.94375  354.97925  355.01475
                         Volts
                        0.6985
                         Volts
                        1.6313
366.94255  366.97925  367.01595
380.93795  380.97604  381.01414
    C/l

-------
                   Peak Locate Examination:21-JUL-1998:20:06 File:A21JUL98F
                       Experiment:M23_DB225  Function:! Reference:PFK317
PPM
200
 Volts
4.2302
292.95315  292.98245  293.01175
 Volts
1.8577
        304.95195  304.98245  305.01295
 Volts
1.1518
        316.95075  316.98245  317.01*415
                         Volts
                        5.6745
330.94615  330.97925  331.01235
                                Volts
                                4.8040
        342.94495  342.97925 343.01355
                                 Volts
                                2.4566
        354.94375  354.97925  355.01475
PPM
200
 Volts
1.5610
366.94255  366.97925  367.01595
 Volts
4.6436
        380.93795  380.97604 381.01414
    tn

-------
                   Peak Locate Examination:22-JUL-1998:08:11 File:A21JUL98S
                       Experiment:M23_DB225 Function:! Reference:PFK317
                         Volts
                         0.8568
292.95315  292.98245 293.01175
                         Volts
                        0.4258
304.95195 304.98245  305.01295
PPM
200
 Volts
0.2889
316.95075  316.98245  317.01415
                         Volts
                        1.0522
                         Volts
                        0.9891
                         Volts
                        0.6053
330.94615  330.97925 331.01235
342.94495  342.97925  343.01355
354.94375  354.97925  355.01475
                         Volts
                        0.3802
                         Volts
                        0.9007
366.94255  366.97925  367.01595
- =»: -
380.93795 380.97604  381.01414
    m

-------
                    Section 4
                 System Perfor<
                    Section 4-2
Gas Chromatography Performance Check
•— — ^— — — — — — — — — — •— — — — <^ "~ ~ jp11""— •• ^ •" ^™ •" "^ ~ "^— " " ~ ~^ — ^ — — i— — ^ ^_^^__^__
    Isomer Specificity 4& Retention Time Windows

           Documentation for the Analysis
                       of
  Polychlorinated Dibenzo-/;-Dioxins & Dibenzofurans

-------
File: A17JUL98B Acq: 17-JUL-1998 16:45:56 Exp: EXP_M23 DB5 OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #1 Text: DB-5 Retchk ALS #1
303.9016,319.8965 -*£-
100% _ k ' 27
80J:
60 j
40 j
20 j
0;
r
23:39
n
A
/
A 1




V 7
24:00 25:00 26:00 27:00
F:2 339.8597,355.8546 ^_-
100% r
80 J
60J
40 j
20J
n •
30:14 / A
A
A
\ \
/ \^ / ^
U T| 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 t 1 1 1 1 1 1 1 1 1 ' 1 	 | 1 1 1 1 1 1 1 1 1 T 1 | 1 1
30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00
F:3 373.8207,389.8156
100% 33i32n » F~
80J
60 j
40J
20J
0:
A '


\ \
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33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48
F:4 407.7818,423.7767 f^ "& .
100% 36j22l t ' < — - L-
80 j
60 J
40 j
20J
OJ
A A 37:32
A A A
\ \ /\ A
/ V / V r^ / V
j \ — / x — j ^ — / x —
36:00 36:12 36:24 36:36 36 48 37:00 37:12 37:24 37:36 37
319.8965,331.9368
100% 25 14
80 J
60J
40 j
20J
o;




j




^
24:00 25:00 26:00 27:00


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A A /I
m-i
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/U IV
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28:00






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:39
A


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29:00


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_
-
-


30:00 Time
7 { 	
i A
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y i
r~~^~~«
'-
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'-
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33166 33:12 Time







r
-
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36 ijsUe 39
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_
29:53
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-
-
-
:.

30:00 Time

-------
File: A17JUL98BAcq: 17-JUL-1998 16:45:56Exp:  EXP_M23_DB5_OVATION Voltage  SIR  EI+GC Autospec-UltimaE
Sample #1  Text: DB-5 Retchk  ALS #1
319.8965
                                                               28:39
                                                                                                             Paradigm
10
. .-I i  i i i i I i i  i i i I i i i  i i I i i i  i r\	I i i i i i I  i i i i i 1	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'|
27:48  27:54   28:00   28:06   28:12  28:18  28:24  28:30  28:36   28:42   28:48  28:54  29:00  29:06  29:12
                                                                                                              29:18
                                                                                                                    Time

-------
10
£
   File: A21JULy8F  Acq:  21-JUL-1998 20:06:58Exp: M23_DB225 Voltage SIR EI+—GC Autospec-UltimaE—Paradigm
   _Qamr\1 o Jt 1  Td-vi- - r\n_OOt;  n,-»*-,-ii-»v  TIT o -1*1
   Sample #1  Text:  DB-225 Retchk  ALS il
   303.9016
   100%
                                                                           I  ' '  '  ' '  I  '  ' '  '  ' _ I
          27:00     27:12      27:24     27:36      27:48      28:00     28:12      28:24     28:36      28:48
29:00  Time
          27:00     27:12      27:24     27:36     27:48      28:00     28:12      28:24     28:36      28  48
     O.OEO

29:00  Time

-------
                    Section 4
                System Perfonmanc
                    Section 4-3

            Initial Calibrations
              (HP-5MS & DB-225 Columns)
          Documentation for the Analysis
                       of
Polychlorinated Dibenzo-/;-Dio\ins & Dibenzofurans

-------
OPUSquan   20-JUL-1998
Page 1
   Run: 0716crv    Analyte: m8290-23-» Cal: m8290-23-» Results:
                                                                      Page 1 of

                                     Version:  V3.5 17 APR-1997 11:14:34
                                                                                                                      '7/
                        Name Mean RRF
                                         S. D.
                                                   %RSD
                                                          17jul98a S3 17jul98a S4 17jul98a S5 17jul98a S6 17jul98a S7
                                                           RRFttl   SD  RRF#2   SD  RRF#3   SD  RRF#4   SD  RRF#5   SD
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7, 8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
13C-2,3,7,8-TCDD
13C-l,2,3,7,8-PeCDD
13C-1 , 2,3,6,7, 8-HxCDD
13C-l,2,3,4,6,7,8-HpCDD
13C-OCDD
13C-2,3,7,8-TCDF
13C-l,2,3,7,8-PeCDF
13C-1 , 2 , 3 , 6 , 7 , 8-HxCDF
13C-1 , 2 , 3 , 4 , 6 , 7 , 8-HpCDF
1301,2, 3, 4-TCDD
1301,2,3,7,8,9-HxCDD
37Cl-2,3,7,8-TCDD
1302,3,4,7,8-PeCDF
13C-1, 2 ,3,4,7, 8-HxCDD
13C-1, 2 ,3,4,7, 8-HxCDF
13C-l,2,3,4,7,8,9-HpCDF
3701-2,3, 7, 8-TCDD
13C-2,3,4,7,8-PeCDF
13C-1 , 2 , 3 , 4 , 7 , 8-HxCDD
13C-1 ,2,3,4,7, 8-HxCDF
13C-l,2,3,4,7,8,9-HpCDF
Total Tetra-Furans
Total Tetra-Dioxins
Total Penta-Furans
0.
1.
0.
0.
0.
0.
1.
0.
0.
0.
0.
1.
0.
0.
1.
1.
1.
1.
0.
1.
0.
0.
1.
1.
1.
0.


1.
1.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
9843
1157
6718
8518
8597
8965
0033
9531
8711
9020
8611
0877
9347
8123
2600
0402
0684
0970
7648
0729
7951
6399
3772
1987
2388
7529
-
-
0062
1724
7230
9654
5892
9166
9777
6747
7855
7823
9531
9843
8866
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.


0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
Oil
016
023
119
115
Oil
004
008
009
023
047
183
129
082
040
103
040
024
056
161
020
032
039
086
206
010
-
-
058
095
114
104
084
035
025
056
054
109
008
Oil
012
1
1
3
13
13
1
0
0
1
2
5
16
13
10
3
9
3
2
7
14
2
5
2
7
16
1


5
8
15
10
14
3
2
8
6
13
0
1
1
.14
.46
.35
.96
.32
.21
.40
.86
.04
.50
.49
.79
.85
.14
.1$
.89
.72
.18
.28
.99
.49 !
.03
.82
.14
.62
.36


.74
.13
.80
.79
.34
.84
.55
.32
.85
.97 s
.86 <
.14 1
.31 '
fc 1.
i 1.
* 0.
i 	 0.
4 •— 0.
i 0.
fc 1.
fc 0.
t 0.
* 0.
fc 0.
*>" 1.
I/ 1.
i ' 0.
i 1.
k 0.
k 1.
i 1.
k y 0.
\r o.
t 0.
k 0.
k 1.
k / 1.
* ' 1.
k 0.
*
t
k 0.
k 1.
* 0.
fc 0.
fc 0.
k 0.
fc 1.
i 0.
fc 0.
k 0.
fc 0.
I 1.
k 0.
00
14
67
96
95
89
00
96
87
88
87
25
03
87
23
93
03
07
71
95
78
63
36
13
08
76
-
-
92
13
64
90
53
86
01
67
83
69
96
00
87
1.
1.
-0.
0.
0.
-0.
0.
1.
-0.
-0.
0.
0.
0.
0.
-0.
-1.
-0.
-1.
-1.
-0.
-0.
-0.
-0.
-0.
-0.
0.


-1.
-0.
-0.
-0.
-0.
-1.
1.
0.
0.
-0.
1.
1.
-1.
1
2
1
9
8
1
1
4
3
9
1
9
7
8
9
1
8
2
0
8
6
4
5
8
8
6
-
-
5
4
7
6
8
7
2
0
8
8
4
1
0
0
1
0
0
0
0
1
0
0
0
0
1
1
0
1
0
1
1
0
0
0
0
1
1
1
0


0
1
0
0
0
0
0
0
0
0
0
0
0
.97
.11
.68
.94
.95
.88
.00
.95
.87
.87
.89
.20
.04
.88
.22
.96
.02
.08
.73
.95
.78
.61
.34
.14
.07
.74
-
-
.99
.08
.58
.84
.49
.91
.95
.62
.79
.66
.95
.97
.87
-1.
-0.
0.
0.
0.
-1.
-1.
-0.
0.
-1.
0.
0.
0.
0.
-1.
-0.
-1.
-0.
-0.
-0.
-0.
-0.
-1.
-0.
-0.
-1.


-0.
-0.
-1.
-1.
-1.
-0.
-1.
_ T
0.
-1.
-0.
-1.
-1.
2
2
3
7
8
6
0
9
3
2
6
6
8
8
0
7
2
6
6
8
9
9
1
6
8
0
-
-
3
9
2
2
1
2
3
1
0
1
9
2
0
0.
1.
0.
0.
0.
0.
1.
0.
0.
0.
0.
1.
1.
0.
1.
1.
1.
1.
0.
0.
0.
0.
1.
1.
1.
0.


1.
1.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
97
13
70
91
93
90
00
95
88
91
92
20
02
86
25
01
08
09
74
98
78
61
36
14
11
75
-
-
01
10
73
95
58
93
96
75
85
77
95
97
90
-0
0
1
0
0
0
-1
-0
1
0
1
0
0
0
-0
-0
0
-0
-0
-0
-0
-0
-0
-0
-0
-0


0
-0
0
-0
-0
0
-0
1
1
-0
-0
-0
0
.9
.6
.4
.5
.6
.2
.0
.5
.1
.3
.2
.6
.7
.6
.2
.3
.2
.4
.5
.6
.6
.8
.6
.7
.6
.4
-
-
.1
.8
.1
.2
.1
.4
.7
.4
.2
.1
.5
.9
.7
0
1
0
0
0
0
1
0
0
0
0
0
0
0
1
1
1
1
0
1
0
0
1
1
1
0


1
1
0
1
0
0
1
0
0
0
0
0
0
.99
.11
.64
.71
.72
.90
.01
.96
.87
.93
.83
.90
.80
.73
.28
.12
.10
.12
.81
.27
.82
.68
.42
.26
.45
.77
-
-
.06
.26
.80
.06
.67
.94
.00
.63
.73
.87
.96
.99
.90
0
-0
-1
-1
-1
0
1
0
0
1
-0
-1
-1
-1
0
0
0
0
0
1
1
1
1
0
1
1


0
0
0
0
1
0
0
-0
-1
0
0
0
1
.6
.2
.4
.2
.2
.7
.0
.7
.4
.0
.8
.0
.0
.0
.6
.8
.8
.9
.9
.2
.0
.2
.1
.8
.0
.4
-
-
.8
.9
.6
.9
.0
.7
.7
.8
.0
.8
.7
.6
.2
0
1
0
0
0
0
1
0
0
0
0
0
0
0
1
1
1
1
0
1
0
0
1
1
1
0


1
1
0
1
0
0
0
0
0
0
0
0
0
.99
.09
.67
.74
.75
.91
.01
.95
.86
.92
.80
.88
.78
.72
.32
.17
.11
.12
.83
.23
.82
.67
.42
.32
.48
.75
-
-
.06
.29
.86
.09
.68
.94
.98
.70
.73
.91
.95
.99
.89
0.3
-1.4
-0.2
-1.0
-1.0
0.9
0.9
-0.7
-1.5
0.8
-1.2
-1.2
-1.2
-1.1
1.4
1.3
1.1
1.2
1.3
1.0
1.2
1.0
1.1
1.4
1.2
-0.7
-
-
0.9
1.2
1.2
1.2
1.1
0.7
0.1
0.5
-1.0
1.2
-0.7
0.3
0.2

-------
OPUSguan   ll-FEB-1998                Page 1
                                                                                                            Page 1 of 1

   Run: 07FEB98    Analyte: M23_CONF   Cal: 225-07feb  Results:             Version:  V3.5 17-APR-1997 11:14:34

                                                          07feb98d S4 07feb98d S5 07feb98d S6 07feb98d S7 07feb98d S8
                        Name Mean RRF    S. D.     %RSD    RRF#1   SD  RRF#2   SD  RRF#3   SD  RRF#4   SD  RRF#5   SD

                2,3,7,8-TCDF   0.9472    0.033   3.49 %     1.00  1.5   0.91 -1.3   0.94 -0.4   0.95  0.0   0.95  0.1
            13C-2,3,7,8-TCDF        -        -      -%        _-      .    -      _    -      -_      _    _
                      HxCDPE        -        -      -%        --      --      --      --      --
          QC CHK ION (Tetra)        -        -      - %        -    -      --      --      -    -      -    -

-------
                              Section 4
                          Sstem Perfor<
                             Section 4-4
                   Documentation for the Analysis
                                 of
         Polychlorinated Dibenzo-p-Dioxins & Dibenzofurans
00

-------
         OPUSquan   20-JUL-1998
Page 1
                                                                                                                     Page 1 of 2
CT5
            Run #6    Filename al7ju!98b        S:  2   1:1  Acquired:  17-JUL-98  17:31:00 Processed:  20-JUL-98 08:49:43
            Run:  a!7ju!98b  Analyte:  m8290-23-» Cal:  m8290-23-» Results:  m8290-23-»    Quan :  V3.5 17-APR-1997 11:14:34
            Sample  text:  FE CS3                     Comments:  ^t-\n4l.    ,          OPUS :  A3.6/8X 18-MAR-1998 16:12:42
                 Typ
                                           Name
            Resp
                                                                     RA
                                                                                RT
                                                                                         Cone
                                                                                                 Dev'n
                                                                                                                     Mod?
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS

SS
SS
SS
SS
SS
DPE
DPE
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3, 6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
13C-2,3,7,8-TCDD
13C-1 ,2,3,7, 8-PeCDD
13C-1,2,3,6,7, 8-HxCDD
13C-1,2,3,4, 6,7,8-HpCDD
13C-OCDD
13C-2,3,7,8-TCDF
13C-1 , 2,3,7, 8-PeCDF
13C-l,2,3,6,7,8-HxCDF
13C-l,2,3,4,6,7,8-HpCDF
13C-1,2,3,4-TCDD
13C-l,2,3,7,8,9-HxCDD
37Cl-2,3,7,8-TCDD
13C-2 ,3,4,7, 8-PeCDF
13C-l,2,3,4,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
13C-l,2,3,4,7,8,9-HpCDF

37Cl-2,3,7,8-TCDD
13C-2,3,4,7,8-PeCDF
13C-l,2,3,4,7,8-HxCDD
13C-1 , 2,3,4,7,8 -HxCDF
13C-1,2,3, 4,7,8, 9-HpCDF
HxCDPE
HpCDPE
2
8
5
7
7
5
1
2
1
1
8
1
9
8
7
6
1
4
3
3
2
3
6
4
3
2
4
3
2
1
5
7
4

2
1
5
7
4


.4e+07
.6e+07
.9e+07
.3e+07
.7e+07
,8e+07
.Oe+08
.9e+07
.le+08
.le+08
.2e+07
.2e+08
.6e+07
.le+07
.7e+07
.2e+07
.le+08
.8e+08
.Oe+08
.3e+08
. 6e+08
.9e+08
.Oe+08
. 8e+08
.8e+08
.5e+08
.5e+08
. 4e+08
.2e+07
.le+08
.le+07
.2e+07
.8e+07

.2e+07
.le+08
.le+07
.2e+07
8e+07
*
*
0
1
1
1.
1.
1.
0.
0.
1.
1.
1.
1.
1.
1.
1.
1.
0.
0.
1.
1.
1.
0.
0.
1.
0.
0.
0.
1.
1.
1.
0.
0.

1.
1.
0.
0.




77
54
26
24
23
06
90
77
52
52
38
14
23
24
01
02
90
77
54
26
04
89
78
57
52
44
79
26
57
24
52
45

57
24
52
45




y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y

y
y
y
y




28:27
32:37
34:42
34:46
34:59
37:11
40:02
27:26
31:57
32:24
34:11
34:15
34:37
35:08
36:22
37:32
40:10
28:26
32:36
34:45
37:10
40:01
27:25
31:56
34:14
36:21
28:09
34:58
28:27
32:24
34:42
34:10
37:31

28:27
32:24
34:42
34:10
37:31
NotFnd
NotFnd
5.00
25.5
26.0
25.6
26.6
25.0
51.2
5.07
25.8
24.8
24.7
27.6
26.8
26.1
24.6
24.1
51.5
98.2
88.9
92.7
96.3
182
97.6
89.1
92.0
98.1
92.6
84.9
4.91
21.8
20.8
22.0
24.3

5.01
24.5
22.5
23.7
24.8
*
*
0
2
4
2
6
-0
2
1
3
-0
-1
10
7
4
-1
-3
3
-1
-11
-7
-3
-9
-2
-10
-8
-1


-1
-12
-16
-12
-2

0
-2
-10
-5
-0


.0
.1
.1
.6
.5 .
.1 //}
.3 /A,
.3 j
.3 1
.7
.2
.5
.2
.6
.6
.8
.0
.8
.1
.3
.7
.0
.4
.9
.0
.9
_
-
.7
7
.6
0
9

1
0
2
0
9

-
n
n
y? itA-Tii^vit0^'
S — Jj * -* (t\I
f n
./I n
"y n

n
n
n
n
n
_
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n
n

n
n
n
n
n
n
n

-------
•Y
File: A17JUL98B Acq: 17-JUL-1998 17:31:00 Exp: EXP M23 DBS OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm
Sample #2 Text: FE CS3 ALS #2
319.8965 S:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 1564 . 0 , 1 . 00%, F, F)
100% A1.03E7 2.0E6
50 j
o:
321.
100%
50 j
o:
331.
100%
50J
o:
333.
100%
50 J
OJ
327.
100%
50J
o:
316.
100*
50^
o:

_1.0E6
O.OEO
24:00 25:00 26:00 27:00 28:00 29:00 30:00 Time
8936 S:2 SMO ( 1 , 3 ) BSUB(128, 15 , -3 . 0 ) PKD(3 , 3 , 3 , 0 . 10%, 1824 . 0 , 1 . 00%, F, F)
A1.33E7 2.7E6
A F
A
_1.3E6
O.OEO
24100 25100 26:00 27loO 2sloO 29loO 30:00 Time
9368"S:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 11164 . 0 , 1 . 00%, F, F)
A2.10E8 4.1E7
AA
i.2 . 1E7
LO.OEO
24 loo 	 25 100 	 26:00 27loO 28:00 29:00 30:00 Time
9339 S:2 SMO(1,3) BSUB(128, 15, -3 .0) PKD(3 , 3 , 3 , 0 . 10%, 3908 . 0 , 1 .00%,F,F)
A2.71E8 ,_5.3E7
A A F

24:00 25100 26loO 27:00 28:00 29:00 30:(
8847 S:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 7592 .0, 1 .00%,F,F)
A2.21E7
A
_2.7E7
:O.OEO
10 Time
4.4E6
_2.2E6
LO.OEO
24100 25100 26:00 27:00 28:00 29:00 30:00 Time
9824 S:2 SMO(1,3) PKD(3 , 3 , 3 , 100 .00%, 0 . 0, 1 . 00%, F, F)
23:30 24:17 24:4625;08 25:43 26^07 26:48 27:19 28:02 28^44 29:1029:32 7.8E7

L3.9B7
LO.OEO
24,00 25100 26:00 27;00 28:00 29:00 30:00 Time

-------
File: A17JDL98B Acq: 17-JUL-1998 17:31:00 Exp: EXP_M23_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Parad:
Sample #2 Text: FE CS3 ALS #2
355.8546 S:2 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2136 . 0 , 1 . 00%, F, F)
100% A5.24E7
so:
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357.
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100%
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30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
8517 S:2 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD (3 , 3 , 3 , 0 . 10%, 692 . 0, 1 . 00%, F, F)
A3.41E7
A

3b!l2 ' 30:24 ' 30l36 ' 3bl48 ' 31:66 ' 3iSl2 3il24 31\36 3i!48 32166 32112 32-124 32136 32J48 33166 33li2
8949 S:2 F:2 SMO(1,3) BSUBU28, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 4016 . 0 , 1 . 00%, F, F)
A1.84E8
1L
' 3bli2" 30124" 30l36" 30148" 3ll66 ' 3lll2 3ll24 3ll36 3ll48 32l6o 32ll2 32:24 32:36 32148 33loO 33ll2
8919 S:2 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2840 . 0, 1 . 00%, F, F)
A1.20E8
IL
"30112" 36124" 36136" 30148" 3llo6 ' 3lll2 3ll24 3ll36 3ll48 32166 32! 12 32124 32136 32:48 33:00 33:12
9792 S:2 F:2 SMO(1,3) PKD(3 , 3 . 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
30-14 30:47 31:05 31:22 31:39 31=57 32:11 32:36 3ii33 	


' 361l2" 36124" 36136" 36148" 3ll6o '3lll2 3ll24 3lS36 3ll48 32100 32ll2 32?24 32136 32J48 33:00 33:12
Lgm
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_8.8E6
O.OEO
Time
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O.OEO
Time
6.5E7
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0 . OEO
Time
4.3E7
_2 . 1E7
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Time
8.7E7
_4.3E7
O.OEO
Time

-------
File
Samp
389.
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391.
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401.
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:: A17JUL98B Acq: 17-JUL-19W
>le #2 Text: FE CS3 ALS #2
8156 S:2 F:3 SMO(1,3) BSUB(128
33J24 33136 33 Us 34:
8127 S:2 F:3 SMO(1,3) BSUB(128
33124 33136 33:48 34!
8559 S:2 F:3 BSUB(128, 15, -3 . 0)
33124 33136 33:48 34!
8530 S:2 F:3 BSUB(128, 15, -3 . 0)
17:31:00 Exp : EXP_M23_DB5_OVATION Voltage SIR EI + GC Autospec-UltimaE Paradigm
,15, -3.0) PKD(3,5,2,0.10%,1860.0.1.00%.F.F)
A4
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00 34!l2 34!24 34:36
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PKD(3,5/2,0.10%,11648.0,1.00%,F
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34:48 35:00 35:12 35!24 3s!36 35
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6.8E7
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5.5E7
_2.7E7
.O.OEO
33?24 33!36 33!48 34^00 34!l2 34!24 34!36 34!48 35!oO 35!l2 3s!24 3s!36 35 48 Time
9760 5:2 F:3 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0, 1 . 00%, F, F)
33:42 33:56 34:08 34:18 34:31 34:43 34:53 35:14 35:43 1 . 8E8
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i i i i i | i i i i i i i i r i i i i i i i
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34:48 35:00 35:12 35:24 35:36 35:48 Time

-------
File
Samp
423.
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i: A17JUL98B Acq: 17-JUL-1998 17:31:00 Exp: EXP M23 DBS OVATI6N Voltage SIR EI+ GC Autospec -UlfimaE Paradigm '
>le #2 Text: FE CS3 ALS #2
7767 S:2 F:4 SMO ( 1 , 3 ) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1392 . 0, 1 . 00%, F, F)
A2.96E7 7.1E6
/\
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36566 36512' 36-24 36536 36548 37566 37! 12 37! 24 37! 36 37548 38566 38512 38524 38 536 ' 38548 ' 39
7737 S:2 F:4 SMO(1,3) BSUB{128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3648 . 0, 1 . 00%,F,F)
A2 . 81 E7
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36:00 36:12 36:24 36:36 36:48 37:00 37:12 37:24 37:36 37:48 38:00 3s!l2 38524 38536 3s!48 39
8169 S:2 F:4 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2028 . 0, 1 . 00%, F, F)
A1.31E8
j[_
36566 36512 '36:24 36:36 36{48 37566 37!i2 37524' 37536 37548 38566 385l2 38524 38536 38548 39?
8140 S:2 F:4 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 860 . 0, 1 . 00%, F, F)
A1.27E8
j[_
36566 36512 36:24 36536 36548 37566 375l2 37!24 37536 37548 38566 385l2 38524 38:36 38548 39!
9728 S:2 F:4 SMO(1,3) PKD(3,3,3, 100 .00%, 0 .0,1 . 00%,F,F)
35^5936:10 36j22 36:33 36:47 37:1137:21 37:45 38:10 38:33 3R;45
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36566 36:12 36:24 36536 36548 37566 37 5 12 ' 37 524 ' 37 536 ' 37 548 ' 38 5 66 38 5 12 ' 38 524 ' 38 5 36 38 5 48 ' 39 5
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-------
File
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: A17JUL98B Acq: 17-JUL-1998 17:31:00 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC AutOSpec-UltimaE Parad
le #2 Text: FE CS3 ALS #2
7377 S:2 F:5 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2336 . 0, 1 . 00%, F, F)
A4.77E7
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39:12 39:24 39:36 39:48 40:00 40:12 4o!24 40:36 40:48 41:
7348 S:2 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 332 . 0 , 1 . 00% , F, F)
A5.30E7
J\__
39:12 39:24 39:36 39:48 40:00 40:12 4o!24 40:36 40:48 41:
7780 S:2 F:5 SMO(1,3) BSUB(128, 15, -3 .0) PKD(3 , 3 , 3 , 0 . 10%, 3976 . 0 , 1 . 00%, F, F)
A1.84E8
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39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
7750 S:2 F:5 SMO(1,3) BSUB(128, 15, -3 .0) PKD(3 , 3 , 3 , 0 . 10%, 1228 . 0 , 1 . 00%, F, F)
A2 . Q8E8
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39:12 39:24 39:36 39:48 40:00 40:12 4o!24 40:36 40:48 41:
9728 S:2 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
39JJJ. 39:2939:35 39:49 40:01 40:08 40:24 40:34 40:54
/
39! 12 39:24 39:36 39148 40:00 40:12 4o!24 40:36 40:48 41
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00 Time
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L6.8E7
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00 Time

-------
File: A17JUL98B Acq:
17-JDL-1998 17:31:
00 Exp: EXP_M23_DB5_OVATION Voltage SIR El-t- GC Autospec-UltimaE Paradigm
Sample #2 Text: FE CS3 ALS #2
303.9016 S:2 SMO(1,3)
100%
50 j
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305.8987 S:2 SMO{1,3)
100%
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i i ii i | i
24:00
315.9419 S:2 SMO{1,3)
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24:00
317.9389 S:2 SMO(1,3)
100%
50 1
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24:00
375.8364 S:2 SMO(1,3)
100%

50_
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23:36 24
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24:00
316.9824 5:2 SMO(1,3)
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25 loo'
BSUB{128,15,-3.0)



25:00
BSUB(128,15,-3.0)



25:00
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25:00
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PKD(3,3,3,0.10%,1660.0,



26 loo'
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1.



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1.



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27:19 28;02 28:44 29:1029:32 7 . 8E7


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-------
File: A17JUL98B
Sample #2
339.8597 S:
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' 36112
341.ftSfift S:
100%
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Acq: 17-JUL-1998 1
FE CS3
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30:36
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i i i 1 i i i
30:36
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i i i I i i i
30:36
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30:36
SMO (1,3)

ALS #2
BSUB(128,



36148 ' 3ll
BSUB(128,



i ' I ' ' ' ' ' 1
30:48 31:
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30:48 31:
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30:48 31:
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30:55


i i i i i i i i i
30:48 31:
7:31:00 Exp:

15, -3.0) PKD (3



00 31:12 31:
15, -3.0) PKD (3



00 31:12 31:
15, -3.0) PKD(3




00 31:12 31:
15, -3.0) PKD(3




00 31:12 31:
15, -3.0) PKD(3

EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm

,3,3,0.10%



24 31:36
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24 31:36
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24 31:36
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-------
-**>
File: AI7JUL98B Acq: 17-
Sample #2 Text: FE CS3
373.8207
100%
50

OJ




33 1
375.8178
100%
50 j
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S:2 F:3 SMO(1,3)




24 33136 33
S:2 F:3 SMO(1,3)
JUL-1998 17:31:
ALS #2
BSUB(128,15,-3



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Exp: EXP_M23_DB5_6VATION
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100%
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24 33:36 33
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24 33:36 33
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24 33:36 33
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34:43

/ \ 35:09 oc oo TR-T7
v / ^N S^\^/^ AT 35:29 \AT 35:45
^" 	 -^ \-S ^^^ \ 	 / \^ — s^^-^ \—^_f~~^-^'
r1'
5.

0.
48 35loO 35ll2 35?24 35136 35Us

34:53 35:14 35:43 1.
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24 33:36 33
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34!
12 34:24 34:
36 34:
.9.
0.
48 35:00 35:12 35:24 3sl36 35Us


8E7

2E6
npn
Time
5E7
5E6
OEO
Time

9E7
5E7

OEO
Time

6E7
8E7

OEO
Time

OE4
2E3

OEO
Time

8E8
1E7
OEO
Time

-------
iFile: A17JULyHB  Acq:  17-JUL-1998  17:31:00   Exp:  EXP_M23_DB5_OVATION Voltage SIR EH-  GC Autospec-UltimaE—Paradigm
Sample #2  Text: FE  CS3   ALS  #2
407.7818 S:2 F:4 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,9768.0,1.00%,F, F)
100%               A3.88E7
 50J

   OJ
                                                           A3.14E7
                                                                                                                  1.1E7

                                                                                                                  L5.5E6
       i  i | i—i"i"i i  I i i f i mi"YiMr i i i—t11!1 i  I "T"T i I i i  i i i i—i i i—t—i—i—i—i—i—i—T-J—i f i i i  I i i "I I i r"m™i 'i i i i  i i i i i—i—r-
       36:00   36:12  36:24  36:36  36:48   37:00   37:12  37:24  37:36  37:48  38:00  38:12
409.7788  S:2 F:4  SMO(1,3)  BSUB(128,15,-3.0) PKD(3 , 3 , 3,0.10%,7452.0,1.00%, F, F)
100%               A3.83E7
                                                                                          i i i i i i  i i i i i i  i i i i i i i  i i'   • UE.U
                                                                                          38:24   38:36   38:48  39:00  Time
 50-
                                                           A3.08E7
      I I ' I  I I ' I I I  I I f 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 T I i i  [ I I1 I I I I I  I I I I I I I  I I I I i i
       36:00  36:12  36:24  36:36  36:48   37:00  37:12  37:24  37:36  37:48  38:00   38:12
417.8253 S:2 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3 , 3 , 3,0.10%,14644.0,1.00%, F,F)
100%.              A7.60E7
                                                                                                                  L5.4E6
                                                                                                                  .O.OEO
                                                                                                          I
 50J
  O
        38:24  38:36  38:48  39:00  Time

                                 2.1E7

                                Ll.OE7
                                                          A1.50E7
       36:00  36:12  36:24  36:36  36:48  37:00  37:12  37:24  37:36  37|48  38100  38ll2
419.8220 5:2 F:4 SMO{1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,10404.0,1.00%,F,F)
100%              A1.73E8
                                                                                                                  LO.OEO
 50J
                                                                                          38:24   38:36   38J48  39:00  Time
                                                                                                                  4.7E7

                                                                                                                  -2.4E7
                                                          A3.32E7
                                                                                                                  O.OEO
       36^00  36112  36:24  36:36  36:48  37:00  37:12  37:24  37:36  37:48  38:00  38:12
479.7165 S:2 F:4 SMO(1,3) BSUBU28,15, -3 . 0) PKD(3 , 3 , 3 ,100 . 00%, 2976.0,1.00%, F, F)
100%                                           37jlO
    :  35:58
 50J

  ol
                                                                                          38:24   38:36   38:48  39lOO  Time
                                                                                                                  9.6E3

                                                                                                                  L4.8E3
                                                                                                                 LO.OEO
       36:00  36:12  36:2436:36  36:48   37:00  37:12  37:24  37:36  37:48  38:00  38:12
430.9728 S:2 F.-4 SMO(1,3) PKD(3,3,3,100. 00%, 0. 0,1. 00%,F,F)
100%   35:5936:10   36:22  36:33   36:47	37:11 37^21
                                                                   37:45
38:10
 38:24   38:36  38:48  39:00  Time

	38:33  38:45	1. 2E8
                                                                                                                  L6.1E7

                                                                                                                  lO.OEO
       36!6d ' 36:12 ' 36:24 ' 36:36  36:48  37:00  37:12  37:24  37:36  37:48  38:00  38:12
                                                                                          38:24  38:36  38i48  39:00  Time

-------
File: A17JUL98B
Sample #2 Text:
441.7427 S:2 F-.5
100%
°: .,,,,,
39:12
443.7398 S:2 F:5
100%
50J
o: 	
39:12
469.7780 S:2 F:5
100%
50J
o:
39:12
471.7750 S:2 F:5
100%
50J
0:
39ll2
513.6775 S:2 F:5
100%
50 1
': 39:10
0 .j_/-\-X>^"S^;
1 11 1 1 1
39:12
454.9728 S:2 F:5
100% 39:11
;/
50J
0: 	
39:12
Acq: 17-JUL-1998 17:31:00
FE CS3 ALS #2
SMO(1,3) BSUB(128,15,-3.0)

39!24 39136
SMO(1,3) BSUB(128,15,-3.0)

39124 39.'36
SMO(1,3) BSUB (128, 15, -3.0)

39124 39536
SMO(1,3) BSUB (128, 15, -3.0)

39:24 39136
SMO(1,3) BSUB(128,15,-3.0)
3^19 39:31 39:40
/\ ^/V^-vYA ^
iiiiiiiiiiiiii
39:24 39:36
SMO(1,3) PKD(3,3,3,100.00%
39:2939:35 39:

39:24 39136
Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec -Ul timaE Paradigm
PKD(3,3,3,0.10%,772.0,1.00%,F,F)
A5.10E7 1.1E7
T
V 	
• I i i i i i 1 i i r i i | i i i i i | i i i < i r—r -i — i — i — , — i — | — i — | — , — , — | — .
39:48 40:00 40:12 40:24 40:36 40:48 41
PKD(3,3,3,0.10%,1372.0,1.00%,F,F)
A5 -£9E7
7"
39 .Us 40 lob 40 1
PKD(3,3,3,0.10%,3976.0,1
A1.84E8
J\^__
39148 40 lob 401
PKD(3,3,3,0.10%,1228.0,1
A2.Q8E8
J\_
39148 4olob 401
PKD(3,3,3,100.00%,1228.0
40:02
39:52 / \
- — ^^^ / —

39:48 ' ' 40:00 ' ' 401
,0.0,1.00%,F,F)
44 40:01 40:08

39:48 4olob ' ' 4o!
v_
1 1 1 1 1 | 1 1 1 -T—l 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 , 	 1 	 1 	 r
12 40:24 40:36 4ol48 41
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=-l" 1 i i i — p-i — i — i — i — i — r — r— r — i — i — i — i — , — , — , — i — , — j
12 40:24 40:36 40:48 41
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12 40:24 40:36 4ol48 4l!
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40:27 40:39 40:53
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12 40:24 4ol36 40:48 4ll
40:24 40:34 40:54

i i i i i | i i i i i | i i i i i • | T— r — i 	 1 	 1 	 11-
12 40:24 40:36 4ol48 4ll
_5.3E6
LO.OEO
00 Time
1.2E7
_6.0E6
LO.OEO
00 Time
3.9E7
L1.9E7
_O.OEO
00 Time
4.3E7
_2.2E7
_O.OEO
00 Time
_8.2E3
_4.1E3
_O.OEO
00 Time
1.4E8
_6.8E7
O.OEO
00 Time

-------
       OPUSquan   20-JUL-1998
Page 1
                                                                                                                   Page 2 of 2
          Run #7   Filename ai7jui98b        S: 15  1:1  Acquired: 18-JUL-98 03:17;11 Processed: 20-JUL 98 08:49:48
          Run: 0716crv    Analyte: m8290-23-» Cal:  m8290-23-» Results:              Quan :  V3.5 17-APR-1997 11:14:34
          Sample text: BE CS3                     Comments:   C             /       OPUS :  A3-6/8x 18-MAR-1998 16:12:42
00
o
               Typ
                                         Name
            Resp
                                                                   RA
                                                                              RT
                                                                                       Cone
                                                                                               Dev'n
                                                                                                                   Mod?
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
Unk
ES/RT
ES
ES
ES
ES
ES/RT
ES
ES
ES
JS
JS
CS
CS
CS
CS
CS

ss
ss
ss
ss
ss
DPE
DPE
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
13C-2,3,7,8-TCDD
13C-l,2,3,7,8-PeCDD
13C-l,2,3,6,7,8-HxCDD
13C-l,2,3,4,6,7,8-HpCDD
13C-OCDD
13C-2,3,7,8-TCDF
13C-l,2,3,7,8-PeCDF
13C-l,2,3,6,7,8-HxCDF
13C-1 , 2,3,4,6,7, 8-HpCDF
13C-1,2,3,4-TCDD
13C-l,2,3,7,8,9-HxCDD
37Cl-2,3,7,8-TCDD
13C-2,3,4,7,8-PeCDF
13C-l,2,3,4,7,8-HxCDD
13C-l,2,3,4,7,8-HxCDF
13C-l,2,3,4,7,8,9-HpCDF

37Cl-2,3,7,8-TCDD
13C-2,3,4,7,8-PeCDF
13C-1 , 2,3,4,7, 8-HxCDD
13C- 1,2,3,4,7, 8-HxCDF
13C-l,2,3,4,7,8,9-HpCDF
HxCDPE
HpCDPE
3
1
7
1
1
8
1
4
1
1
1
1
1
1
1
9
1
6
4
4
3
5
8
6
5
3
6
4
3
1
8
1
7

3
1
8
1
7


.26+07
.2e+08
.8e+07
.le+08
.le+08
.46+07
.5e+08
.Oe+07
.5e+08
.5e+08
.2e+08
.5e+08
.3e+08
.2e+08
.16+08
.5e+07
. 6e+08
.5e+08
.4e+08
.6e+08
. 8e+08
.8e+08
.3e+08
.8e+08
.2e+08
. 6e+08
.2e+08
.7e+08
.le+07
. 6e+08
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.le+08
. 4e+07

.le+07
. 6e+08
. 3e+07
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.4e+07
*
*
0.
1.
1.
1.
1.
1.
0.
0.
1.
1.
1.
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1.
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78
55
22
27
25
01
88
78
53
53
21
23
21
22
02
03
89
78
56
26
04
89
79
56
52
45
79
26
56
23
52
45

56
23
52
45




y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y
y

y
y
y
y




28:27
32:37
34:42
34:46
34:59
37:10
40:02
27:26
31:57
32:24
34:11
34:15
34:37
35:08
36:22
37:31
40:10
28:26
32:36
34:45
37:09
40:01
27:25
31:56
34:14
36:21
28:09
34:58
28:27
32:24
34:41
34:10
37:31

28:27
32:24
34:41
34:10
37:31
NotFnd
NotFnd
5.04
24.6
25.0
28.2
26.6
24.9
50.3
5.03
26.0
25.1
25.7
27.2
25.8
27.4
25.1
25.3
51.7
96.9
94.4
92.1
101
194
97.9
91.6
89.1
102
128
119
5.01
22.5
24.3
24.3
26.5

5.18
24.6
26.3
27.0
25.9
*
*
0
-1
0
12
6
-0
0
0
4
0
2
8
3
9
0
1
3
-3
-5
-7
0
-2
-2
-8
-10
2


0
-10
-2
-3
6

3
-1
5
8
3


"7 /
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n
n
n
n
n
n
n
n
n
n
n
n
n

n
n
n
n
n
n
n

-------
File: A17JUL98S Acq: 18-JUL-1998 03: IV:
Sample #15 Text: BE CS3 ALS #2
319.8965 S:15 SMO(1,3) BSUB(128 , 15, -3 . 0)
100%
50:
o:



	 24:00 25:00
321.8936 S:15 SMO{1,3) BSUB(128, 15, -3 .0)
100%
50:
o:

24:00 25:00
331.9368 S:15 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50:
o:



" ' i l i l i l l T — r— i i | i i
24:00 25:00
333.9339 S:15 SMO(1,3) BSUB(128, 15, -3 .0)
100%
50:
0



v ' i 	 r" i 	 1 	 1 	 1 	 1 	 1 — r i i i i i
24:00 25:00
327.8847 S:15 SMOU.3) BSUB(128, 15, -3 . 0)
100%
50.
0 "



"-* 	 1 	 1 	 1 	 1 	 1 	 1 	 1 	 r 	 1 	 i "i | i i
24:00 25:00
316.9824 S:15 SMO{1,3) PKD(3, 3, 3, 100. 00%
11 Exp: EXP_M23_DB5_OVATION Voltage SIR El-t- GC Autospec-UltimaE Paradigm

PKD(3,3,3,0.10%,1568.0,1.00%,F,F)
A1.42E7
A
|\

2.9E6
_1.4E6
•O.OEO
26:00 27:00 28:00 29:00 30:00 Time
PKD(3,3,3,0.10%,1024.0,1.00%,F,F)
A1.82E7
3.7E6
_1.9E6
LO.OEO
26!oO 	 27 [OO 	 28 loo 	 29! 00 	 3o!oO Time
PKD(3,3,3,0.10%,8452.0,1.00%,F,F)
A2.72E8n
A A
n
i\i\
5.7E7
_2.8E7
.O.OEO
26\00 27:00 28\00 29\00 3o!oO Time
PKD(3,3,3,0.10%,3540.0,1.00%,F,F)
A3.69E8
A A
A
i\ 	
7.3E7
.3.7E7
.O.OEO
26!oO 27!00 28!00 29:00 30:00 Time
PKD(3,3,3,0.10%,5376.0,1.00%,F,F)
A3.11E7
A
A
i\
6.4E6
.3.2E6
-O.OEO
26!00 27100 28100 29!00 30IOO Time
, 0.0,1. 00%, F,F)
100% 2^-4« ™:1fi 3A:4fi 3S;1A 25;4526:Q7 26:32 26:59 27:26 28il4 28:58 29:38 ..5.5E7
-
50^
o-
1


V 	 , 	 , 	 , 	 , 	 , 	 1 -T ,_.,,,., | , ,
24:00 25:00




.2 . 8E7
' 0 . OEO
26!00 	 27! 00 28!oO 29 5 00 3o!oO Time
00

-------
File
Samp
355.
100%^
so:
0"
357.
100%^
so:
0"
367.
100%
so:
OJ
369.
100%
50:
o:
366.
100%
50:
0'
: A17JUL98B Acq: 18-JUL-1998 03:17:11 Exp: EXP_M2 3_DB5_OVATlON Voltage SIR EI+ GC Autospec-UltimaE Parad:
le #15 Text: BE CS3 ALS #2
8546 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1636 . 0 , 1 . 00%, F, F)
A7.42E7
A
l\
30:12 30:24 30:36 30:48 31:00 31:12 31:24 31:36 31:48 32:00 32:12 32:24 32:36 32:48 33:00 33:12
8517 S:15 F:2 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 1152 . 0 , 1 . 00% , F, F)
A4.78E7
A
n
365l2 36524 30:36 30548 31566 3l5i2 31524 31536 31548 32566 325l2 32524 32536 32548 3356o 335l2
8949 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 3688 . 0, 1 . 00%, F,F)
A2.71E8
A
t
' 3o!i2 ' 3o!24 ' 30I361 ' 3o!«8 ' nloO ' 3i!l2 ' 3i!24 ' 3i\36 ' nUs ' 32566 ' 325l2 ' 32!24 ' 325^6 ' 32548 ' 33566 ' 335l2
8919 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 2720 . 0 , 1 . 00%, F, F)
A1.74E8
IL
rt-i^r t n A o *a i rt n 0110 O1O/1 "311C T1./1Q TO«nn T5 • 1 O "%*} • 0 A "^ ^ • "\(\ "^?«4R 1 ^ • fl fl ^"^'15
9792 S:15 F:2 SMO(1,3) PKD (3 , 3 , 3 , 100 . 00%, 0 . 0 , 1 . 00%, F, F)
30-26 30-4230-52 31-0831:18 31:4331:53 32:08 32:20 32i37 33^:00 33:12

' 30:12 ' 36S24 ' 30:36 ' 30S48 ' 3iS66 3l5i2 31524 31536 31548 32566 32512 32524 32536 32548 33566 33ll2
igm
_2.7E7
_1.3E7
O.OEO
Time
_1.7E7
18.4E6
" O.OEO
Time
1.0E8
L5.0E7
0 . OEO
Time
6.4E7
.3.2E7
O.OEO
Time
6.2E7
_3.1E7
O.OEO
Time
00

-------
File
Samp
389.
100%
so:
391.
100%
so:
0'
401.
100%
so:
0"
403.
100%
so:
0
380.
100%
so:
0'
: A17JUL98B Acq: 18-JUL-1998 03:17:11 Exp: EXP M23 DB5 OVATION Voltage SIR EI + GC Autospec-Ul timaE "•paradigm" '
le #15 Text: BE CS3 ALS #2
8156 S:15 F:3 SMO(1,3) BSUB(128, 15 , -3 . 0) PKD(3 , 5 , 2 , 0 . 10%, 1552 . 0, 1 . 00%, F, F)
A6.24E7 A5.90E7 1.8E7
A A A F
/i\A
1 1 I 1 1 1 1 1 1 l 1 1 l 1 1 1 1 1 l 1 1 l l 1 l 1 1 l l 1 1 l 1 1 l l i l 1 l ' l l l 1 1 l l T l l i l i l i 1 "f" 1 1 1 1 1 I I — i— 1 — i — l — l — 1 — I — I — I — I —
33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35124 35J36 35
8127 S:15 F:3 SMO(1,3) BSUB (128, 15, -3 . 0) PKD(3 , 5, 2 , 0 . 10%, 2248 . 0 , 1 . 00%, F, F)
A4.93E7 A4.73E7
n V /V
33:24 33:36 33148 34loO 34!l2 34124 34136 34Us 3s!oO 3s!l2 3sl24 35J36 3s!
8559 S:15 F:3 BSUB(128, 15, -3 . 0) PKD(3 , 5, 2, 0 . 10%, 12588.0, 1 . 00%, F, F)
J3 A2.62E8
A
/I
33:24 33:36 33.!48 34.-00 34.-12 34!24 34be 34.U8 35.-00 35.!12 35$24 35.!36 35
8530 S:15 F:3 BSUB(128, 15, -3 .0) PKD(3 , 5, 2 , 0 . 10%, 10808 . 0, 1 .00%,F,F)
A2.J36E8 A2.08E8
A /i
L9.2E6
.O.OEO
48 Time
1.5E7
.7.3E6
.O.OEO
48 Time
1.1E8
.5.5E7
.O.OEO
48 Time
8.7E7
_4.4E7
.O.OEO
33l24 33S36 33Us 34!oO 34^12 34!24 34136 34!48 3s!oO 35:12 35124 35^36 35J48 Time
9760 S:15 F:3 SMO(1,3) PKD{3 , 3 , 3 , 100 . 00%, 0 .0, 1 . 00%, F, F)
33:22 33:30 34:15 34:47 34:58 35:08 35:20 35:32 1.3RB

33:24 33:36 33:48 34:00 34:12 34:24 34:36 34:48 35:00 35:12 35:24 35:36 35
16.4E7
' O.OEO
48 Time
00
CO

-------
   File:  A17JUL98B  Acq: 18-JUL-1998 03:17:11  Exp: EXP_M23_DB5_OVATION Voltage SIR EI +  GC Autospec-UltimaE—Paradigm
   Sample #15  Text: BE CS3  ALS #2
   423.7767 S:15 F:4 SMO(1,3) BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,1484.0,1.00%,F, F)
   1004                                          A4.24E7
    50J
     OJ
                                                                                                                    _1.2E7
                                                                                                                    ,,5.8E6
                                                                                                                     O.OEO
          36100  36112  36124  36:36   36148  37166  37!l2  37!24 ' 37136 ' 37148 ' 38166 '  38112 ' 38:24 ' 38^36 ' 38-48 ' S^OO
   425.7737 S:15 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3 , 0.10%, 884.0,1.00%,F,F)
                                                 A4.17E7                                                             1-1E7
    so:
          36!66  36!l2  36I24  31136  36148  37166  37:12  3?S24  37.!36  37148  38166  38S12 ' 38124 ' 38136
   435.8169 S:15 F:4 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,0.10%,6540.0,1.00%,F,F)
   1004                                         A1.92E8
    50J
                                                                                                                    _5.7E6
                                                                                                                     O.OEO
                               39:00  Time

                                  ,-5.
                                                                                                                    _2.5E7
                                                                                                                     O.OEO
        i i I i I I I  i i I I i i  i i i I i i  r l*T"p 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   36:12   36:24   36:36  36:48  37:00  37:12  37:24  37:36   37:48   38:00   38:12  38:24  38:36  38:48  39:00  Time
   437.8140 S:15 F:4 SMOU.3)  BSUBU28,15, -3 .0) PKD(3 , 3 , 3 , 0.10%, 3636 .0,1. 00%, F, F)
   100%                                         A1.54E8                                                            _4.9E7
    50J
     OJ
                                  ^2.4E7
                                   O.OEO
        i I i i i i  i i i i i I i  I i i i I i  i I*T"T 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  36:12   36:24   36:36  36:48  37:00  37:12  37:24  37:36  37:48   38:00   38:12  38:24  38:36  38:48  39:00  Time
   430.9728 S:15 F:4 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
   100% 	     36j09	36:36_    36:53  _ 37:07 37il8	3?j_41
    50.,
38:06 38:17    38:33   38=45
.8.5E7
                                  _4.2E7
     ^ ' i  i i i i i i i  i i i r 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 -r I i '' r" 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*1 • ^*i"
          36:00   36:12   36:24   36:36  36:48  37:00  37:12  37:24   37:36   37:48   38:00   38:12  38:24  38:36  38:48  39:00  Time
00

-------
File
Samp
457.
iooa
so:
0"
459.
100%
50J
0'
469.
100%
so:
0'
471.
100%
so:
0.'
454.
100%
so:
0'
>: A17JUL98B Acq: 1B-JUL-1998 03:17:11 Exp: EXP_M23_DB5_6vATl6N Voltage SIR EI+ GC Autospec-ultimaE — Paradigm 	 1
>le #15 Text: BE CS3 ALS #2
7377 S:15 F:5 SMO(1,3) BSUBU28, 15, -3 .0) PKD(3 , 3, 3 , 0 . 10%, 1824 . 0, 1 . 00%, F,F)
A6.91E7 1.6E7
/v
39ll2 39124 39136 39U8 4o!ob 4o!l2 4o!24 4ol36' ' '4'oUs' " '41
7348 S:15 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 756 . 0, 1 . 00%, F, F)
A7 . 84E7
/v
39ll2 39!24 39!36 39:48 4o!ob 4o!l2 4o!24 4o!36 ' ' 4o!48 ' ' 41
7780 S:15 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10% , 2176 . 0 , 1 . 00%, F, F)
A2 . 76E8
/Y^
39!l2 39124 39136 39148 4o!ob 4o!l2 40l24 4o!36 ' ' ' 40:48 '''41!
7750 S:15 F:5 SMO(1,3) BSUB(128, 15, -3 .0) PKD(3 , 3 , 3 , 0 . 10% , 1480 . 0 , 1 . 00%, F, F)
A3 . 08E8
J\_
39ll2 39:24 39136 39:48 40:00 4o!l2 4ol24 4o!36 40:48 4l!
9728 S:15 F:5 SMO{1,3) PKD(3,3,3, 100.00%, 0.0, 1.00%,F,F)
39:0739:12 39:18 39:25 39:36 39:49 39:58 40:08 40:14 40:22 40:32 40:44 40:52

39:12 39:24 39:36 39:48 40:00 40:12 40:24 40:36 40:48 41:
,8.0E6
LO.OEO
00 Time
1.8E7
_9.0E6
.O.OEO
00 Time
6.4E7
_3.2E7
_O.OEO
00 Time
_7 . 1E7
_3.6E7
_O.OEO
00 Time
9.4E7
_4.7E7
O.OEO
00 Time
00

-------
File: A17JUL98B Acq: 18-JUL-1998 03:17:
Sample #15 Text: BE CS3 ALS #2
303.9016 S:15 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50 j
24!00 25!oO
305.8987 S:15 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50 J
°" r-
24SOO 25!oO
315.9419 S:15 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50 J
o •
" ' i 	 1 i i i 	 1 	 1 	 r— T 	 i i i i i
24:00 25:00
317.9389 S:15 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50J
n -
" ' i 	 1 	 1 i i 	 1 i i 	 1 	 r— i 	 r • i i
24:00 25:00
375.8364 S:15 SMO(1,3) BSUB(128, 15, -3 .0)
100%
50j 23 :12
'' Jl 23A44 A. 24:26 25:02 25
0 - /* U^ ^ /V\ An vsA _j\ r~ (43-^j-^
11 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Parad
PKD(3,3,3,0.10%,1572.0,1.00%,F,F)
A1.75E7
26!oO '27:00' 28!oO 29! 00 30 :(
PKD(3,3,3,0.10%,2200.0,1.00%,F,F)
A2.23E7
26!oO 27:00' 2s!oO 29:00 30:(
PKD(3,3,3,0.10%,4528.0,1.00%,F,F)
A3.66E8
26:00' ' 27!00 2s!oO 29!oO 3o!(
PKD(3,3,3,0.10%,5308.0,1.00%,F,F)
A4.64E8
/i
2e!oo 27!oo 2s!oo 29loo soli
PKD(3,3,3,100.00%,48.0,1.00%,F,F)
AT
:24 25:58 26;22 A fL A ^7 = 34 27:5B \ / I /. 29:00
igm
_3.6E6
_1.8E6
LO.OEO
)0 Time
4.7E6
_2.3E6
O.OEO
)0 Time
7 . 6E7
.3.8E7
lO.OEO
)0 Time
9.6E7
.4 . 8E7
.O.OEO
30 Time
9.3E3
_4.7E3
.O.OEO
	 24! 00 	 25! 00 	 26!oO 27! 00 28!00 29!00 30 lOO Time
316.9824 S:15 SMO(1,3) PKD{3, 3, 3 , 100 . 00%, 0 . 0, 1 .00%,F,F)
100% 23:48 24:16 24:48 25:14 25:4526:07 26:32 26i59 27:26 2BU4 28:58 29:1S ,_5.5E7
50J
o-
" ' 1 1 1 — 'T 	 1 " 1 " 1 1 i'.— T.-. -| 1 |
24:00 25:00

L2.8E7
lO.OEO
26:00 27:00 28:00 29!oO 30:00 Time
00
Oi

-------
File: A17JUL98B Acq: 18-JUL-1998 03:17:11
Sample #15 Text: BE CS3 ALS #2
339.8597 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 .0)
100%
50:
30li2 30124 30136 SoUs 31:66 3ill2
341.8568 S:15 F:2 SMO(1,3) BSUB (128 , 15 , -3 . 0)
100%
50:
3bll2 30124 30136 3ol48 SlloO 3ill2
351.9000 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50J
30:12 30 1 24 ' 30 136 3ol48 31:66 ' 31 -12
353.8970 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
50.
30:12 30124 30:36 30:48 31:00 31:12
409.7974 S:15 F:2 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
_. ' in . ">Q
50: ,A Vf 30:44 31
ni/ U^^K^Wxxk/v^v^
3bll2 30124 30136 30148 3ll66 31112
366.9792 S:15 F:2 SMO(1,3) PKD(3, 3 , 3, 100 .00%
100% 30:26 30:4230:52 31:04 31
50J
o-
30:12 30:24 30:36 30:48 31:00 31:12
Exp: EXP_M23_DB5_OVATlON Voltage SIR EI+
PKD(3,3,3,0.10%,984.0,1.00%,F,F)
A9.27E7 A9.26E7
A A
3il24 3ll36 biUs 32lo6 32ll2 32124
PKD(3,3,3,0.10%,2800.0,1.00%,F,F)
A6.04E7 A6.06E7
A A
3il24 31\36 3i.!48 32166 32112 32l24
PKD(3,3,3,0.10%,608.0,1.00%,F,F)
A4.12E8
/ \ A9.90E7
31:24 31:36 31:48 32:00 32:12 32:24
PKD(3,3,3,0.10%,1788.0,1.00%,F,F)
A2.64E8
/ \ A6.33E7
31:24 31:36 31:48 32:00 32:12 32:24
PKD(3,3,3,100.00%,3904.0,1.00%,F,F)
.,- 32:12
1^31j26 31:45 31:56 ^/Vv^ 32:26.
31124 31136 blUs 32166 32li2 '32:24
0.0,1.00%,F,F)
:18 31:43 31:53 32:08 32:20

31:24 31:36 3ll48 32:00 32!l2 32?24
3C Autospec-UltimaE Paradigm
3.4E7
.1.7E7
n ORO
' "i | i i i i i i i i i i i i i i i i i i i i1 " • "•E|"
32:36 32:48 33:00 33:12 Time
2 . 2E7
L1.1E7
32:36 32:48 33.;00 33ll2 Time
1.4E8
.7.2E7
32:36 32:48 33100 33:12 Time
9.3E7
.4.6E7
32:36 32:48 33:00 33:12 Time
32:36 1.5E4
/\ 33:07 -7'7E3
V-^^-^Xy«n.«
32136 32148 33166 33ll2 Time
32:37 33:00 33: IP. fi . 2R1
.3.1E7
32:36 32148 33:00 33:12 Time

-------
?ile: A17JUL98B
Sample #15
373.8207
100%
I
50 J
0'



'33!
375.8178
100%
"
sol
0 '



•33!
383.8639
100%
50J

0"




'33!
385.8610
100%
50 J
•
o •




•33!
445.7555
100%
I
50^
o •


33:
'33i
380.9760
S:




24
S:




24
S:




24
S:




24
S:


24
24
S
100% 33 •?.•>.
50 J
o •
y

Vs!


24
Text
Acq:
18-JUL-1998 03: IV
: BE CS3
15 F:3




33




T
15 F:3




33




T
15 F:3




i— i — i i
33
15 F:




33
15 F:






T
3




7
3


33:33
' ' '33!
15 F:
33 :30


r~i — r— r*
33
3



T
SMO (1,3)




36




'33:
SMO (1,3)




i i i
36




'33!
ALS #2
BSUB(128,15,




48 34:00
BSUB(128,15,




48' ' '34:00'
:11 Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm


-3.0) PKD(3,5,2,0.10%,53560.0,1.00%,F,F)
§7



34:12 34
-3.0) PKD(3,
A6.87E7
A l\
Y \
J 1 V_
34:12 34
BSUB(128,15,-3.0) PKD(3 , 5 , 2 , 0 . 10%




— T — r— r
36




'33!




i i i — i — i i i — r—r
48 34:00
A1.77E8.
f\
A
^ \ \
/v V
'34: 12 34
BSUB(128,15,-3.0) PKD(3 , 5, 2 , 0 . 10%




— i — i — r
36




'33!
SMO(1,3)


33
36


:43
^x^_
Vs!
SMO (1,3)



— 1 	 IT
36



—r— i — i
331




48 34:00
BSUB(128,15,


33:52
48 34:00
A3.42E8
f\
A
yv / I
/V V.
34^12 34
-3.0) PKD(3,


34:11
34ll2 34
PKD(3, 3,3, 100. 00%, 0.0,1.



48' ' '34:00
34:15


34:12 34
A6 .85E7
A A6.35E7
A A
J V. J ^-
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.1.
0.
1 1 1 1 1 'f 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 ' ' I ' ' 1 	 1 1 ' r~l ' I
:24 34:36 34:48 35:00 35:12 35:24 35:36 35:48
5, 2, 0.10%, 42572. 0,1. 00%, F,F)
A5.67E7
A A5.22E7
A A
1 V_ 1 V.
72'

_1.
0.
•241 ' '34136 34148 35100 35ll2 3s!24 35I36 35 48
,40516. 0,1. 00%, F,F)


A3.69E7
^"\_
_7
_3

0
124 34!36 34148 3s!oO 3s!l2 3s!24 35I36 35 48
,49724. 0,1. 00%, F,F)


A6.78E7

1
-7
•
:o
!24 34136 34U8 35:00 35:12 35:24 35:36 35:48
3, 3, 100. 00%, 1832. 0,1. 00%, F,F)
34:45 34:58
1 \ f\
rJ \ 1 V 35:08 , 35-32 35:43
i
_6
0
124 34136 34:48 35:00 35:12 35:24 35:36 35:48
00%,F,F)
34^42 34:58 35_dlfl 35:20 35:32 rl


Le
0
•24 34:36 34:48 35:00 35:12 35:24 35:36 35:48


7E7

3E7
OEO
Time

2E7

1E7
OEO
Time

9E7
9E7

OEO
Time

5E8
.7E7

.OEO
Time

. 4E4
. 9E3
.OEO
Time

. 3E8
.4E7
.OEO
Time
00
00

-------
File: A17JUL98B Acq: 18-JUL-1998 OJ
Sample #15
407.7818 S:l
100%
-
50^
o:
Text: BE CS3
5 F:4 SMO(1,3)
A5.79E7
ALS #2
:17:11

BSUB(128,15,-3.0)


Exp: EXP_M23_DB5_OVATION Voltage SIR EI+ GC Autospec-UltimaE Paradigm

PKD(3,


3,3,0.


10%,


2896.0


,1.00%,F,F)
r-1-
/\ A4.83E7


beloo'
409.7788 S:l
100%
"
50J
OJ

/ v..
3 6! 12 36! 24
5 F:4 SMO(1,3)
A5.68E7


36136 36


148" 37 1
BSUB(128,15,-3.0)




66 37!
PKD ( 3 ,



12 37
3,3,0.

I
, J
•24
10%,

(\
v
37:36
4068.0



•
L8.
"o.
37:48 38:00 38:12 38:24 38:36 38:48 39:00
,1.00%,F,F)
r-1-
/\ A4.71E7


36:66
417.8253 S:l
100%
50J
.
0




"' i i i i 1 i i
36:00
419.8220 S:l
100%
50 1
'.
0 '




"' i i i i 1 i i
36:00
479.7165 S:l
100%
•
50J
o"

rf\
' I — y
" L i i i i i i i
36:00
430.9728 S:l
100%

50J
0 '
/


36166

/ V,
ijelii 36:24
5 F:4 SMO(1,3)
A1.13E8
A
A
/ \
y v^
-T-l 1 | TT V-T-I l"T
36:12 36:24
5 F:4 SMO(1,3)
A2.50E8
A
A
/ \
J v_
i i i | T i *i-r i | i-r
36:12 36:24
5 F:4 SMO(1,3)


36136 36


148 37!
BSUB(128,15,-3.0)




36136 36




1 i i i i i 1
Us 37!
BSUB(128,15,-3.0)




•T 1 1 I 1 1 1 1 1
36:36 36




Us 37!
BSUB(128,15,-3.0)


66 37:
PKD ( 3 ,




66 37!
PKD ( 3 ,




66 37!
PKD ( 3 ,


12 37
3,3,0.




12 37
3,3,0.




12 37
1
J
124
10%,


A2.

124
10%,


A5.

124
/\
v
37:36
6436.0


28E7

37:36
14988.


08E7

37 -.36
3, 3, 100. 00%, 2332
37 A09
36:19
36:11 A
A 1 HA
Aj W ^ V
i i i i ' ' '' ' T ' i
36:12 36:24
5 F:4 SMO(1,3)
36:09



1 1 1 ]-!• I-I-T 1 | 1 1
36:12 36:24



_8.
0
37148 38166 38112 38124 38136 bsUs 39 00
,1.00%,F,F)




3.
.1.

0.
37148 38:66 38112 38124 38136 38:48 39:00
0,1.00%,F,F)




7.
13.
•
0.
37148 38166 38112 38124 38:36 38:48 39.00
.0,1.00%,F,F)
1.
36:58 /\ ^fl-ifi
36:40
-S^J*^
' 36136 ' 36
PKD(3,3,3
36:36



i i ' I — i— i—i— i i
36:36 36
36:5lA
s\ / \
\/\J v
Us 37!
,100.00%
36:53



•48 ' 37!
/ \ ^37:22
/ ^AA A
-^J
66 37:
,0.0,1.
37:07



66 37!

12 37
00%, F,
.izoa-



12 37
^-y
124
F)




124
VA/^-
37136

37



37136
i*, A*r, f\ f~\ l\ r\ 38:45 A
v/v x^y \i i/ v^ v/^-xx^Vyv/
|
.5.
•o.
37148 38166 38112 38124 38136 38:48 39:00

41 38:06 38:17 38:33 38:45 8.




_4.
0.
37148 38166 38!i2 38124 38136 38148 39 00


8E7

8E6
OEO
Time

7E7

5E6
OEO
Time

5E7
7E7

OEO
Time

7E7
8E7

OEO
Time

1E4

5E3
OEO
Time

5E7

2E7
OEO
Time
00

-------
File: A17JUL98B Acq: 18-JUL-1998 03:17:11 Exp: EXP M23 DB5 OVATION Voltage SIR EH- GC Autospec-UltimaE Parad
Sample #15 Text: BE CS3 ALS #2
441.7427 S:15 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD( 3 , 3 , 3 , 0 . 10%, 540 . 0, 1 . 00%, F, F)
100%. A7.59E7
:l f\^
39ll2 ' ' ' 39124 ' ' ' 39!36 ' ' ' s'gUs
443.7398 S:15 F:5 SMO(1,3) BSUB( 128, 15, -3 . 0) PKD(3
100%
50J
n:
39ll2 ' ' 39!24 ' 39136 ' ' 39U8
469.7780 S:15 F:5 SMO(1,3) BSUB<128 , 15, -3 . 0) PKD(3
100%
50 j
n:
39:12 39:24 39!36 39148
471.7750 S:15 F:5 SMO(1,3) BSUB(128 , 15, -3 . 0) PKD(3
100%
50 j
0:
39!l2 39124 39136 39l48
513.6775 S:15 F:5 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3
100%
50J
: 39:11 39:21 ^\I 39:47
39!l2 39!24 39!36 39148
454.9728 S:15 F:5 SMO(1,3) PKD(3 , 3 , 3 , 100 .00%, 0 . 0, 1
100% 39:0739:12 39:18 39:25 39:36 39:49
50 J
o:
39:12 39:24 39136 39U8
40:00 40:12 40:24 40:36 40:48 41
, 3, 3, 0.10%, 1976. 0,1. 00%, F,F)
A8 J?6E7
i i I- 1 v i "i1 i -T i — i I—T r"l 1— "1 I i — i i 1 i — i — i — i — i — 1 — i — i— i — i — i —
40:00 40:12 40:24 40:36 40:48 41
, 3, 3, 0.10%, 2176. 0,1. 00%, F,F)
A2 . 76E8
4o!ob 4o!l2 4o!24 4o!36 4'oUs 4l!
,3,3,0. 10%, 1480 . 0 , 1 . 00% , F, F)
A3 . 08E8
4o!ob 4o!l2 4o!24 4o!36 4o!48 4l!
, 3, 3, 100. 00%, 84. 0,1. 00%, F,F)
40:01
^~J ^^——T\^ 40^22^ 4Jhv294°-\f_ 40^43 40j_51_
igm
1.7E7
L8.5E6
_O.OEO
00 Time
1.9E7
.9.4E6
00 Time
6.4E7
L3.2E7
.O.OEO
00 Time
7 . 1E7
.3 . 6E7
: O.OEO
00 Time
1.3.E4
_6.5E3
_O.OEO
4o!ob 4o!l2 4o!24 4o!36 4o!48 4l!oO Time
.00%,F,F)
39:58 40:08 40:14 40:22 40:32 40:44 40:52 9.4E7

_4.7E7
.O.OEO
4o!ob 40:12 40?24 4o!36 40:48 41:00 Time

-------
OPUSquan   22-JUL-1998
                   Page 1
                                                                                                            Page 2 of 2
   Run #7   Filename a21ju!98f
   Run: a07feb98f  Analyte:
   Sample text: CS3
                  S: 2   I: 1  Acquired: 21-JUL-98 20:43:56 Processed: 22-JUL-98 08:22:02
                   Cal: 07feb-m23» Results:              Quan : V3.5 17-APR-1997 11:14:34
                       Comments:                         OPUS : V3.5X 17-APR-1997 11:31:23
        Typ

        Unk
        ES/RT
        Total
        DPE
        LMC
                                  Name
      2,3,7,8-TCDF
  130-2,3,7,8-TCDF
      Tetra Furans
            HxCDPE
QC CHK ION  {Tetra)
   Resp

4.0e+07
8.4e+08
4.7e+07
  RA

0.77
0.78
1.74
/    RT

  27:53
  27:51
  19:51
 NotFnd
 NotFnd
Cone

5.04
 205
5.96
Dev'n

  0.8

  0.8
Mod?

n
n
n
n
n

-------
File: A21JUL.98F Acq: 21-JUL-199« 20:43
Sample #2 Text: CS3 ALS #2
303.9016 S:2 SMO(1,3) BSUB(128 , 15 , -3 . 0)
100%
50 j
o:
' ielob
305.8987 S:2
100%
50 j
0:
ielob
315.9419 S:2
100*
50 j
0:
ielob
317.9389 S:2
1001
50J
0:


islob 2olob
SMO(1,3) BSUB(128,15,-3.0)


islob 2olob
SMO(1,3) BSUB(128,15,-3.0)

islob 2olob
SMO(1,3) BSUB(128,15,-3.0)

16100 18:00 20:00
375.8364 S:2 SMO(1,3) BSUB(128, 15, -3 . 0)
100%
1 16:53 19:57 21:03
5jMrt^^
"''— T 'I- -) 	 1 	 1
16100
316.9824 S:2
100% 16:12
50J
0:
ielob
18:00 20:00
SMO(1,3) PKD(3,3,3,100.00%
17:4818:47 20i2_t

18:00 20:00
:56 Exp: M23_DB225 Voltage SIR EI+ GC Autospec-UltimaE Paradigm
PKD (3, 3, 3 ,0.10%, 3488. 0,1. 00%, F,F)
A1.74E7 2.0E6
A F


22:00 24:00 26:00 2
PKD (3, 3, 3, 0.10%, 5344. 0,1. 00%, F,F)
A2.

J

\ Al .J19E6
alob s'olob 32lob 34lob
26E7

\ A7 .J30E5
2T2lob 24100 26lob 28lob 3olob 32lob 34lob
PKD(3,3,3,0.10%,18656.0,1.00%,F,F)
A3 . 67E8
A
	 )
22:00 24:00 26:00 2
PKD(3,3,3,0.10%,22144.0,1.00%,F,F
A4.


, , ,
3:00 30:00 32:00 34:00
)
68E8
i
1 I 1 1 1 1 1 1 '1 1 1 1 1 1 ' 1 1 "T" 1 1 	 1 ' ' ' ' ' 1 	 1 ' ' '
22 100 24 !00 26 100 28:00 30:00 32:00 34:00
PKD (3 ,3, 3, 100. 00%, 11180. 0,1. 00%, F,F)
21:59 27:51
1 22:5823:59 26:34 1 29:1930,2031:2932:30 34:16
m^^^
22lob ' ' ' 24100 ' ' 26lob 28lob 3olob 32lob 34lob
,0.0,1.00%,F,F)
22^0623:0324:01 25:34 27:5129:0029:5730:5932:1033:0934:13


22lob ' ' ' 24100 ' ' ' 26100 ' ' ' 2s!ob 30:00 32lob 34:00
L1.0E6
" O.OEO
Time
r2.5E6
_1.3E6
O.OEO
Time
_4 . 1E7
_2.1E7
O.OEO
Time
_5.2E7
_2 . 6E7
O.OEO
Time
2.9E4
' o .OEO
Time
9.4E7
L4.7E7
O.OEO
Time
CO
w

-------
        OPUSquan   22-JUL-1998
                  Page 1
                                                                                                                   Page 3 of 3
           Run #8    Filename a21ju!98f
           Run:  a07feb98f  Analyte:
           Sample  text:  CS3
                  S: 17  I: 1  Acquired:  22-JUL-98 06:01:17 Processed:  22-JUL-98  08:24:11
                   Cal: 07£eb-m23» Results:               Quan :  V3.5  17-APR-1997  11:14:34
                       Comments:                          OPUS :  V3.5X 17-APR-1997 11:31:23
                Typ

                Unk
                ES/RT
                Total
                DPE
                LHC
              Name
      2,3,7,8-TCDF
  13C-2,3,7,8-TCDF
      Tetra Furans
            HxCDPE
QC CHK ION (Tetra)
   Resp

3.0e+07
6.6e+08
3.5e+07
  RA

0.78
0.78
1.11
/   RT

 27:53
 27:51
 17:59
NotFnd
NotFnd
Cone

4.85
 161
5.55
'Dev'n

  -3.0 '

  -3.0
Mod?

n
n
n
n
n
(D

-------
File: A21JUL98F Acq: 22-JUL-1998 06:01:17 	 Exp: M23 DB225 Voltage
Sample #17 Text: CS3 ALS #2
303.9016 S:17 SMO(1,3) BSUB(128 , 15, -3 .0) PKD(3 , 3 , 3 , 0 . 10% , 3076 . 0, 1 .
100%
50_
0
305.
1003
50_
o-
315.
100%
50_
o:
317.
100%
50J
o:
375.
100%
50 j
oJ
316.
100%
50.
> OJ


ielob
8987 S:17


ielob
9419 S:17

ielob
9389 S:17

ielob
8364 S:17



islob
SMO (1,3)


ielob
SMO (1,3)

' islob
SMO(1,3)

islob
SMO (1,3)

16:3117:30
r «' i i — JL^O<"
16:00
9824 S:17
16:20

16:00


2olob 22lob 24-100 26:00
BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 3112 . 0, 1 .


20100 22100 24100 26lob
BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 21212 . 0 , 1

20:00 22:00 24:00 26:00
BSUB(128,15,-3.0) PKD(3 , 3 , 3 , 0 . 10%, 33252 . 0, 1

SIR EI+ GC Autospec-UltimaE Paradigm
00%,F,F)
A1.32E7 ,_1.5E6
fl
1
A A7.^03E5
i i i i | i i r ' — T • i — r -i — i i i — i i i — i — i  i — i — r— r
28:00 30:00 32:00 34:00
00%,F,F)
A1.69E7
A
1
/I A9 -1.2E5
I i I i' |X r I i i 'i | i i i •! i — f — i — i — i — i ^ i — i — i — i-l
28:00 30:00 32loO 34loO
.00%,F,F)
A2.87E8
A

28:00 30:00 32:00 34:00
.00%,F,F)
A3.68E8
A
1
20:00 22:00 24:00 26:00 28:00 30:00 32:00 34:00
BSUB(128-15,-3.0) PKD(3 , 3, 3 , 100 . 00%, 6884 . 0, 1 . 00%, F, F)
19:08
JV
/ \ -M^i^lB^^-^^^^^iiJ.L^-^Eiii
islob iolob 22lob 24lob 26lob
SMO (1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
18:23 21:02 22:09 .23 ai_.._. 24j 53. 26

islob

20:00 22:00 24lob 26:00

!L~~^2j2^~~~~^~~~^- 30J^i*^_-^-Jli?° 34:23
28:00 3oloO 32lob 34loO
;3827;34 28;57 30:01 31:08 32:22 33:32

28:00 3olob 32:00 34lob
L7.5E5
LO.OEO
Time
1.9E6
L9.4E5
_O.OEO
Time
3.3E7
i.l.7E7
O.OEO
Time
_4.2E7
.2 . 1E7
O.OEO
Time
_1.9E5
_9.4E4
_O.OEO
Time
3 . 8E7
_1.9E7
O.OEO
Time

-------
file": A21JOL98B—Acq: 21-JUL-1998 16:44:01Exp: M23_DB225 Voltage SIR EI+ GC Autospec-UltimaEParadigm
Sample II  Text: DB-225 Retchk  ALS #1
TIC (+RP)
100%

 95J

 90J

 85J

 80 J

 75J

 70J

 65 J

 60J

 55J

 50 J

 45 J

 40J

 35:

 30J

 25J

 20J

 15 J

 10 j
                                                          28:51
                           28:27
28:02 28:07
 4.7E8

_4.5E8

_4.3E8

-4.0E8

_3.8E8

.3.5E8

L3.3E8

L3.1E8

L2.8E8

12.6E8

.2.4E8

_2.1E8

.1.9E8

L1.7E8

.1.4E8

.1.2E8

L9.5E7

:7.1E7

L4.7E7

_2.4E7
   28J66 ' 28-06''28:i2'28li8'28:24'28536'28S36'28S42'28S48'28S54'29S66'29S66'29 1J2'29SJ^
                                                                                                            O.OEO
                                                                                                               Time

-------
OPUSquan   22-JUL-1998
                                      Page 1
         Filename
           Sample
         Acquired
        Processed
        Sample ID
        Cal Table
    Results Table
         Comments
 Typ
 Unk
 ES/RT
 Total
 DPE
 LMC
        a21ju!98f
        3
        21-JUL-98
        22-JUL-98
        sb
        07feb-m23conf
        M8290-23-072198F
                 21:20:54
                 08:31:41
              Name;
        3,7,8-TCDF;
            8-TCDF;
            Furans;
            HxCDPE;
QC CHK ION  (Tetra);
                      Resp;
                  2.23e+05;
   Ion 1;
1.10e+05;
   Ion 2;
1.12e+05;  0
13C-2,3,7,
    Tetra
                  2.67e+06;  2.62e+05;  6.62e+04;  3
RA;?;
98; n;
 *;n;
95,-n;
    RT;
 27:53;
NotFnd;
 17:56;
NotFnd;
NotFnd;
                                                                                                                                              Page
Cone ;
                                                                                 DL
                  S/N1;?;
                     6;y;
                     *;n;
                    14,-y;
                     *;n
                  DivO;n
S/N2;?
   9,-y
   *;n
   7;y
mod?
  no
  no
  no
  no
  no
                                                                 -;-;  27:53
                                                                 -;-;  27:53
                                                                                                                          no

-------
OPUSquan   22-JUL-1998
                  Page 1
 Ent: 3  Name: Tetra Furans
                                                                   Page  1 of  1

                                   F:l   Mass:  303.902  305.899 Mod? no   #Hom:8
 Run: 8  File: a21ju!98f    S:3   Acq:21-JUL-98  21:20:54  Proc:22-JUL-98  08:31:41
 Tables: Run: a21ju!98b  Analyte: m23_conf   Cal:  07feb-m23»Results: M8290-23*
 Version: V3.5 17-APR-1997 11:14:34  Sample text:  sb
   Amount:  *
     Cone:  *
   Tox #1:  -
Name
 2,3,7,8-TCDF
of which *
of which *
     Tox #2:  -

#     RT Respnse
named and *
named and *
      Tox #3: -
unnamed
unnamed
                                        RA
1  17:56 3.3e+05  3.95 n
         3.3e+05

2  18:01 5.9e+05  1.63 n
         5.9e+05

3  18:02 7.1e+05  2.16 n
         7.16+05

4  27:32 2.0e+05  0.76 y
         2.0e+05

5  27:35 2.46+05  1.08 n
         2.4e+05

6  27:53 2.2e+05  0.98 n
         2.2e+05

7  27:55 2.7e+05  0.47 n
         2.76+05

8  28:13 l.le+05  2.12 n
         l.le+05
          Cone    Area  Height    S/N  Mod?
               2.6e+05 6.3e+04 1.4e+01 y  n
               6.6e+04 2.8e+04 6.6e+00 y  n
              *
               3.6e+05 S.Oe+04 1.8e+01 y  n
               2.2e+05 5.56+04 1.3e+01 y  n
              *
               4.8e+05 7.36+04 1.76+01 y  n
               2.26+05 5.5e+04 1.3e+01 y  n
              *
               8.7e+04 2.5e+04 5.7e+00 y  n
               l.le+05 3.3e+04 7.8e+00 y  n
              *
               1.2e+05 2.7e+04 6.2e+00 y  n
               l.le+05 2.8e+04 6.6e+00 y  n
              *
               l.le+05 2.8e+04 6.4e+00 y  n
               l.le+05 3.8e+04 9.1e+00 y  n
              *
               8.7e+04 2.7e+04 6.1e+00 y  n
               1.8e+05 4.3e+04 l.Oe+01 y  n
              •*
               7.8e+04 1.6e+04 3.7e+00 y  n
               3.76+04 1.5e+04 3.56+00 y  n
                                                                                                197

-------
File: A21JUL98FAcq:  21-JUL-1998 21:20:54Exp:  M23_DB225 Voltage SIR EI+GC Autospec-UltimaEParadigm
Sample  #3   Text:  sb ALS #3
303.9016 S:3  SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,4352.0,1.00%,F,F)
100%             A3.65E5
       16:00      18:00      20:00      22:00      24:00      26:00      28:00
305.8987 S:3 SMO(1,3)  BSUB(128,15,-3.0)  PKD(3,3,3,0.10%,4188.0,1.00%,F, F)
100%             A2.24E5                                               A1.85E5
                                                                                   30:00
                                                                 32:00
                                                                 34:00
 50J

  OJ
                                                 A8.63E3
                                                        -/VpV^v^V^!^
                                                                  A9.25E3

                                                   .MA.  ^.J*v'***V<)ly*~VV*^^
                                                        — r
                                                      30:00
                                                                .O.OEO
                                                                   Time

                                                                .5. 6E4

                                                                .2. 8E4

                                                                .O.OEO
                                                                   Time

                                                                I —
       16o        so       20:00     22:00      24:00      26:00      28:00
315.9419 S:3 SMO(1,3) BSUB(128, 15, -3 . 0) PKD(3 , 3 , 3 , 0 . 10%, 19804 . 0, 1 . 00%, F, F)
1004              17-Sfi                                                 27; 53
                                                       24:
      .. _ __        M      u : j j.        _  _ _
 50J
                                                                                              32iOO
                                                                 34:00
       16IOO      18:00   '  '20:00      22iOO      24:00      26iOO      28iOO
317.9389 S:3 SMO(1,3)  BSUB(128,15,-3.0) PKD{3,3 , 3 , 0.10%, 23456.0,1.00%,F,F)
100%              17;58
 50J
                                                                                   30:00
                                                                 32:00
                                                                 34:00
                                                                .O.OEO
                                                                   Time
       16100      18)00      20:00     22iOO      24.:00      26:00      28)00
375.8364 S:3 SMO(1,3) BSUB(128,15,-3.0) PKD(3,3,3,100.00%,8900.0,1.00%,F,F)
100%                                                   24;56
 50.;

  0
                                                                                   30:00
                                                                 32:00
                                                                 34:00
.O.OEO
   Time

 7.2E5

 3.6E5

 O.OEO
   Time

 8. 5E7

 4.2E7

 O.OEO
   Time
                                                             26:00
                                                                        28:00
                                                      30:00
                                                      32:00
                                                       34:00
       16:00      18:00      20:00     22:00      24:00
316.9824 S:3 SMO(1,3) PKD(3,3,3,100.00%,0.0,1.00%,F,F)
100%19:22  20:42  21:57  23:1524:1525:1626:1427:14  28:28   30:0131:00   32:18   33:3734:34
 50_

  OJ
       ielob
                  islob
20:00
22! ob
24! ob
                                                             26:00
28:00
3o!ob
-i—i—|—i—i—i—i—i—|—i—
  32:00      34:00

-------
           APPENDIX C




CALCULATIONS & COMPUTER SUMMARIES

-------
Summary of Stack Gas Parameters and Test Results
            Air Emissions Screening Test
   Chemical Lime Company - Marble Falls, Texas
      US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Inlet
                      Page 1  of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                               M23-1-1
                                               6/25/98
                                              1520-1857
           MEASURED DATA
           Meter Box Correction Factor                  1.021
           Avg Meter Orifice Pressure, in. H20             2.12
           Barometric Pressure, inches Hg               29.40
           Sample Volume, ft3                       136.787
           Average Meter Temperature, °F               109.5
           Stack Static Pressure, inches H2O              0.00
           Average Stack Temperature, °F                254
           Condensate Collected, ml                    301.1
           Carbon Dioxide content, % by volume           24.6
           Oxygen content, % by volume                   9.8
           Nitrogen content, % by volume                 65.6
           Pilot Tube Coefficient                        0.84
           Average Square Rool Ap, (in. H2O)1/2          1.0831
           Sample Run Duration, minutes                 180
           Nozzle Diameter, inches                     0.217

           CALCULATED DATA
           Nozzle Area, ft2                          0.00026
           Standard Meter Volume, dscf               127.849
Vm(s,dimS     Standard Meter Volume, dscm                3.620
           Stack Pressure, inches Hg                   29.40
  BW,       Moisture, % by volume                       10.0
 Vwshj      Standard Water Vapor Volume, ft3            14.173
 1-6*8      Dry Mole Fraction                         0.9002
  Md       Molecular Weight (d.b.), Ib/lb-mole             32.33
  Ms       Molecular Weight (w.b.), lb/lb«mole            30.90
  V8       Stack Gas Velocity, ft/s                      68.94
  A       Stack Area, ft2                            12.306
  Qa       Stack Gas Volumetric flow, acfm             50,903
  Qs       Stack Gas Volumetric flow, dscfrn            33,297
Qs(onm)     Stack Gas Volumetric flow, dscmm             943
   I	Isokinetic Sampling Ratio, %	102.2
  Y
  AH
  Pbar
 "static

  V,c
 CO2
  02
  N2
  Cp
 AP1/2
  0
  An
 An(std)
 m(std)m3
  P,

-------
   Summary of Stack Gas Parameters and Test Results
      Chemical Lime Company - Marble Falls, Texas
         US  EPA Test Method 23 - PCDDs / PCDFs
               Vertical Kiln Baghouse Inlet
                        Page 2 of 6
             RUN NUMBER
             RUN DATE
             RUN TIME
 M23-I-1
 6/25/98
1520-1857
             EMISSIONS DATA

             DIOXINS:

             2378 TCDD
     ng      Catch, ng                              {0.0171}
   ng/dscm    Concentration, ng/dscm, as measured       {0.00472}
    ug/hr     Emission Rate, ug/hr                      {0.267}

             Total TCDD
     ng      Catch, ng                                1.356
   ng/dscm    Concentration, ng/dscm, as measured          0.375
    ug/hr     Emission Rate, ug/hr                        21.2

             12378 PeCDD
     ng      Catch, ng                              {0.0215}
   ng/dscm    Concentration, ng/dscm, as measured       {0.00594}
    ug/hr     Emission Rate, ug/hr                      {0.336}

             Total PeCDD
     ng      Catch, ng                               0.5514
   ng/dscm    Concentration, ng/dscm, as measured          0.152
    ug/hr     Emission Rate, ug/hr                        8.62

             123478 HxCDD
     ng      Catch, ng                              {0.0126}
   ng/dscm    Concentration, ng/dscm, as measured      {0.00348}
    ug/hr     Emission Rate, ug/hr                      {0.197}

              123678 HxCDD
     ng      Catch, ng                             {0.02086}
   ng/dscm   Concentration, ng/dscm. as measured      {0.00576}
    ug/hr      Emission Rate, ug/hr	{0.326}
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.

-------
    Summary of Stack Gas Parameters and Test Results
       Chemical Lime Company - Marble Falls, Texas
          US EPA Test Method 23 - PCDDs / PCDFs
                 Vertical Kiln Baghouse Inlet
                          Page 3 of 6
              RUN NUMBER
              RUN DATE
              RUN TIME
 M23-I-1
 6/25/98
1520-1857
              EMISSIONS DATA -Continued

              DIOXINS - Continued

              123789 HxCDD
      ng      Catch, ng                               0.0252
    ng/dscm    Concentration, ng/dscm, as measured       0.00696
     ug/hr     Emission Rate, ug/hr                       0.394

              Total HxCDD
      ng      Catch, ng                               0.5264
    ng/dscm    Concentration, ng/dscm, as measured          0.145
     ug/hr     Emission Rate, ug/hr                        8.23

              1234678 HpCDD
      ng      Catch, ng                               0.0509
    ng/dscm    Concentration, ng/dscm, as measured         0.0141
     Mg/hr     Emission Rate, ug/hr                       0.795

              Total HpCDD
      ng      Catch, ng                               0.0964
    ng/dscm    Concentration, ng/dscm, as measured         0.0266
     ug/hr     Emission Rate, pg/hr                        1.51

              OCDD
      ng      Catch, ng                               0.0564
    ng/dscm    Concentration, ng/dscm, as measured         0.0156
     ug/hr     Emission Rate, ug/hr                       0.881

              Total PCDD
      ng      Catch, ng       .                        2.587
    ng/dscm    Concentration, ng/dscm, as measured          0.715
     yg/hr     Emission Rate, ug/hr                        40.4
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.

-------
   Summary of Stack Gas Parameters and Test Results
      Chemical Lime Company - Marble Falls, Texas
         US EPA Test Method 23 - PCDDs / PCDFs
               Vertical Kiln Baghouse Inlet
                        Page 4 of 6
             RUN NUMBER
             RUN DATE
             RUN TIME
 M23-I-1
 6/25/98
1520-1857
             EMISSIONS DATA - Continued

             FURANS

             2378 TCDF
     ng      Catch, ng                               0.1884
   ng/dscm    Concentration, ng/dscm, as measured        0.0520
    ug/hr     Emission Rate, ug/hr                       2.94

             Total TCDF
     ng      Catch, ng                               10.324
   ng/dscm    Concentration, ng/dscm, as measured          2.85
    ug/hr     Emission Rate, ug/hr                        161

             12378 PeCDF
     ng      Catch, ng                                0.129
   ng/dscm    Concentration, ng/dscm, as measured        0.0356
    ug/hr     Emission Rate, pg/hr                       2.01

             23478 PeCDF
     ng      Catch, ng                                0.158
   ng/dscm    Concentration, ng/dscm, as measured         0.0436
    ug/hr     Emission Rate, ug/hr                        2.47

             Total PeCDF
     ng      Catch, ng                                2.712
   ng/dscm    Concentration, ng/dscm, as measured          0.749
    ug/hr     Emission Rate, ug/hr                        42.4

             123478 HxCDF
     ng      Catch, ng                               0.1613
   ng/dscm   Concentration, ng/dscm, as measured        0.0446
    ug/hr     Emission Rate, ug/hr        	2.52
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.

-------
   Summary of Stack Gas Parameters and Test Results
       Chemical Lime Company - Marble Falls, Texas
         US EPA Test Method 23 - PCDDs / PCDFs
                Vertical Kiln Baghouse Inlet
                         Page 5 of 6
              RUN NUMBER
              RUN DATE
              RUN TIME
 M23-I-1
 6/25/98
1520-1857
              EMISSIONS DATA - Continued

              Furans - Continued

              123678 HxCDF
      ng       Catch, ng                               0.0612
   ng/dscm    Concentration, ng/dscm, as measured        0.0169
     ug/hr     Emission Rate, ug/hr                       0.956

              234678 HxCDF
      ng       Catch, ng                               0.0457
   ng/dscm    Concentration, ng/dscm, as measured        0.0126
     ug/hr     Emission Rate, ug/hr                       0.714

              123789 HxCDF
      ng       Catch, ng                               0.0127
   ng/dscm    Concentration, ng/dscm, as measured       0.00351
     ug/hr     Emission Rate, ug/hr                       0.198

              Total HxCDF
      ng       Catch, ng                               0.5676
   ng/dscm    Concentration, ng/dscm, as measured         0.157
     ug/hr     Emission Rate, ug/hr                        8.87

              1234678 HDCDF
      ng       Catch, ng                               0.0684
   ng/dscm    Concentration, ng/dscm, as measured        0.0189
     pg/hr     Emission Rate, ug/hr                        1.07

              1234789 HoCDF
      ng       Catch, ng                             {0.00722}
   ng/dscm    Concentration, ng/dscm, as measured      {0.00199}
     Mg/hr     Emission Rate, ug/hr	{0.113}
{} Estimated Maximum Possible Concentration. EMPC values are included in totals.

-------
   Summary of Stack Gas Parameters and Test Results
       Chemical Lime Company - Marble Falls, Texas
         US EPA Test Method 23 - PCDDs / PCDFs
                Vertical Kiln Baghouse Inlet
                         Page 6 of 6
              RUN NUMBER
              RUN DATE
              RUN TIME
 M23-I-1
 6/25/98
1520-1857
             EMISSIONS DATA - Continued

             Furans - Continued

             Total HpCDF
     ng      Catch, ng                              0.0860
   ng/dscm   Concentration, ng/dscm, as measured        0.0238
    ug/hr     Emission Rate, ug/hr                        1.34

             OCDF
     ng      Catch, ng                            {0.00968}
   ng/dscm   Concentration, ng/dscm, as measured      {0.00267}
    ug/hr     Emission Rate, ug/hr                     {0.151}

             Total PCDF
     ng      Catch, ng                            {13.6987}
   ng/dscm   Concentration, ng/dscm, as measured         {3.78}
    ug/hr     Emission Rate, pg/hr                       {214}

             Total PCDD + PCDF
     ng      Catch, ng                            {16.2855}
   ng/dscm   Concentration, ng/dscm, as measured         {4.50}
    ug/hr	Emission Rate, ug/hr	{254}
{}  Estimated Maximum Possible Concentration. EMPC values are included in totals.

-------
 Summary of Stack Gas Parameters and Test Results
             Air Emissions Screening Test
    Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Stack
                       Page 1  of 6
   Y
  AH
  Pbar
  vm

 Pstatic
  T.
  Vte
  C02
  02
  N2
  CP
 Ap1*
   0
  An
Vm(std)m3
  PS
 1-Bw
  Md
  Ms
  V8
  A
          RUN NUMBER
          RUN DATE
          RUN TIME
                                   M23-O-1
                                    6/25/98
                                   1518-1855
MEASURED DATA

Meter Box Correction Factor                 1.000
Avg Meter Orifice Pressure, in. H20             2.10
Barometric Pressure, inches Hg               29.40
Sample Volume, ft3                       141.112
Average Meter Temperature, °F                92.0
Stack Static Pressure, inches H20             -0.30
Average Stack Temperature, °F                 231
Condensate Collected, ml                   310.9
Carbon Dioxide content, % by volume           15.7
Oxygen content, % by volume                 13.6
Nitrogen content, % by volume                70.7
Pitot Tube Coefficient                       0.84
Average Square Root Ap, (in. H20)1/2         1.0968
Sample Run Duration, minutes               180.0
Nozzle Diameter, inches                    0.217

CALCULATED DATA
Nozzle Area, ft2                          0.00026
Standard Meter Volume, dscf              133.265
Standard Meter Volume, dscm               3.774
Stack Pressure, inches Hg                  29.38
Moisture, % by volume                        9.9
Standard Water Vapor Volume, ft3           14.634
Dry Mole Fraction                        0.9011
Molecular Weight (d.b.), Ib/lb-mole            31.06
Molecular Weight (w.b.), Ib/lb-mole            29.76
Stack Gas Velocity, ft/s                       70.0
Stack Area, ft2                            12.48
Stack Gas Volumetric flow, acfm             52,443
Stack Gas Volumetric flow, dscfm            35,448
Stack Gas Volumetric flow, dscmm            1,004
Isokinetic Sampling Ratio. %	101.6
 Q,
Qs
s(cmm)
 I

-------
 Summary of Stack Gas Parameters and Test Results
    Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Stack
                      Page 2 of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                  M23-O-1
                                   6/25/98
                                  1518-1855
  ng
ng/dscm
 ug/hr
EMISSIONS DATA

DIOXINS:

2378 TCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
  0.012
0.00318
  0.192
          Total TCDD
  ng      Catch, ng
ng/dscm   Concentration, ng/dscm, as measured
 ug/hr     Emission Rate, ug/hr
                                       1.102
                                       0.292
                                        17.6
           12378 PeCDD
   ng       Catch, ng                               0.009
ng/dscm    Concentration, ng/dscm, as measured       0.00238
  ug/hr     Emission Rate, ug/hr                      0.144

           Total PeCDD
   ng       Catch, ng                               0.264
ng/dscm    Concentration, ng/dscm, as measured        0.0700
  ug/hr     Emission Rate, ug/hr                       4.21

           123478 HxCDD
   ng       Catch, ng                               0.003
ng/dscm    Concentration, ng/dscm, as measured      0.000795
  ug/hr     Emission Rate, ug/hr                     0.0479
           123678 HxCDD
   ng      Catch, ng                               0.005
ng/dscm    Concentration, ng/dscm, as measured      0.00132
  ug/hr     Emission Rate, ug/hr	0.0798

-------
 Summary of Stack Gas Parameters and Test Results
    Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Stack
                      Page 3 of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                  M23-O-1
                                   6/25/98
                                 1518-1855
  ng
ng/dscm
 pg/hr
EMISSIONS DATA-Continued

DIOXINS - Continued

123789 HxCDD
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
  0.004
0.00106
 0.0638
          Total HxCDD
  ng      Catch, ng                               0.116
ng/dscm   Concentration, ng/dscm, as measured        0.0307
 ug/hr     Emission Rate, ug/hr                       1.85

          1234678 HpCDD
  ng      Catch, ng                               0.007
ng/dscm   Concentration, ng/dscm, as measured       0.00185
 ug/hr     Emission Rate, ug/hr                      0.112

          Total HpCDD
  ng      Catch, ng                               0.013
ng/dscm   Concentration, ng/dscm, as measured       0.00344
 ug/hr     Emission Rate, ug/hr                      0.207

          OCDD
  ng      Catch, ng                               0.024
ng/dscm   Concentration, ng/dscm, as measured       0.00636
 Mg/hr     Emission Rate, ug/hr                      0.383
           Total PCDD
   ng      Catch, ng
ng/dscm    Concentration, ng/dscm, as measured
  pg/hr     Emission Rate, ug/hr	
                                       1.519
                                       0.403
                                        24.2

-------
 Summary of Stack Gas Parameters and Test Results
    Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical  Kiln Baghouse Stack
                      Page 4 of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                  M23-O-1
                                   6/25/98
                                  1518-1855
  ng
ng/dscm
 ug/hr
EMISSIONS DATA - Continued

FURANS

2378 TCDF
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
 0.160
0.0424
  2.55
          Total TCDF
  ng      Catch, ng
ng/dscm   Concentration, ng/dscm, as measured
  ug/hr    Emission Rate, ug/hr
                                       9.120
                                        2.42
                                        146
           12378 PeCDF
   ng       Catch, ng                               0.087
ng/dscm    Concentration, ng/dscm, as measured        0.0231
  ug/hr     Emission Rate, ug/hr                       1.39

           23478 PeCDF
   ng       Catch, ng                               0.086
ng/dscm    Concentration, ng/dscm, as measured        0.0228
  ug/hr     Emission Rate, ug/hr                       1.37
           Total PeCDF
   ng      Catch, ng
 ng/dscm    Concentration, ng/dscm, as measured
  ug/hr     Emission Rate, ug/hr
                                       1.590
                                       0.421
                                        25.4
   ng
 ng/dscm
  ug/hr
 123478 HxCDF
 Catch, ng                               0.047
 Concentration, ng/dscm, as measured       0.0125
 Emission Rate, ug/hr   	0.750

-------
 Summary of Stack Gas Parameters and Test Results
     Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Stack
                       Page 5 of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                  M23-O-1
                                   6/25/98
                                  1518-1855
  ng
ng/dscm
 ug/hr
EMISSIONS DATA - Continued

Furans - Continued

123678 HxCDF
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
  0.017
0.00450
  0.271
          234678 HxCDF
  ng      Catch, ng                               0.011
ng/dscm   Concentration, ng/dscm, as measured       0.00291
 ug/hr     Emission Rate, ug/hr                      0.176

          123789 HxCDF
  ng      Catch, ng                               0.004
ng/dscm   Concentration, ng/dscm, as measured       0.00106
 ug/hr     Emission Rate, ug/hr                      0.064

          Total HxCDF
  ng      Catch, ng                               0.166
ng/dscm   Concentration, ng/dscm, as measured        0.0440
 ug/hr     Emission Rate, ug/hr                       2.65

          1234678 HoCDF
  ng      Catch, ng                               0.017
ng/dscm   Concentration, ng/dscm, as measured       0.00450
 ug/hr     Emission Rate, ug/hr                      0.271
           1234789 HpCDF
  ng       Catch, ng                               0.002
ng/dscm    Concentration, ng/dscm, as measured      0.000530
  ug/hr     Emission Rate, ug/hr	0.0319

-------
 Summary of Stack Gas Parameters and Test Results
    Chemical Lime Company - Marble Falls, Texas
       US EPA Test Method 23 - PCDDs / PCDFs
             Vertical Kiln Baghouse Stack
                      Page 6 of 6
          RUN NUMBER
          RUN DATE
          RUN TIME
                                  M23-0-1
                                  6/25/98
                                 1518-1855
  ng
ng/dscm
 (jg/hr
EMISSIONS DATA- Continued

Furans - Continued

Total HoCDF
Catch, ng
Concentration, ng/dscm, as measured
Emission Rate, ug/hr
  0.023
0.00609
  0.367
          OCDF
  ng      Catch, ng                               0.010
ng/dscm    Concentration, ng/dscm, as measured       0.00265
 ug/hr     Emission Rate, ug/hr                      0.160

          Total PCDF
  ng      Catch, ng                              10.909
ng/dscm    Concentration, ng/dscm, as measured          2.89
 ug/hr     Emission Rate, ug/hr                       174
          Total PCDD + PCDF
   ng      Catch, ng                             12.428
ng/dscm   Concentration, ng/dscm, as measured         3.29
  ug/hr    Emission Rate, ug/hr	198

-------
    APPENDIX D




EXAMPLE EQUATIONS

-------

-------
                       Nomenclature
      Y
      AH
      Pbar
      ts
      Vic
     CO2
      02
      N2
      CP
     Api/2

      0
      Dn
      An
     Vm(Std)
     * m(std)m3
      PS
      Bws
     Vw(std)
     l-ljws
      Ma
      Ms
      Vs
      A
      Qa
     Qs(std)
     Qs(cmm)
       I
    ng/dscm
ng/dscm@7%O2
     ug/hr
     Ib/hr
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H2O
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
Pitot Tube Coefficient
Average Square Root Ap, (in. H2O)1/2
Sample Run Duration, minutes
Nozzle Diameter, inches
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, dry, lb/lb«mole
Molecular Weight, wet, lb/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, %
Concentration, ng/dscm
Concentration, ng/dscm adjusted to 7% oxygen
Emission Rate, ug/hr
Concentration, parts per million, dry
Concentration, parts per million, wet
Emission Rate, pounds per hour

-------
                                 Example Calculations
                      Chemical Lime Company - Marble Falls, Texas
                            US EPA Method 23-PCDD/PCDF
                             (Using Data from Run M23-I-1)

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     =  17
                           Vm(std)    ll-
                                                      AH
                                                      13.6
                                                460  + t.
                          = (17.64)(136.787)(1.021)
                                                    29.4 +
2.115
 13.6
                                                    460  + 109.52
                                 Vm(std)  =  127.849 dscf
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)
                                     = (127.849)(0.028317)
                                 Vm(std)m3 =  3.620 dscm
 3. Volume of water vapor at standard conditions, ft3.
                                  Vw(std)  = 0.04707V1C
                                Vw(std) = (0.04707)(301.1)
                                         =  14-173 scf

-------
4. Moisture content in stack gas.
                                        v         (ioo)
                                            v
                                     m(std)   v w(std)
                            BWS = _     _ (100)
                                   127.849+ 14.173
                                     Bws = 9.98
5. Dry molecular weight of stack gas, Ib/lb-mol.




                  Md  -  0.44(%CO2)  + 0.32(%O2)  +  0.28(%N2+%CO)



                     Md = 0.44(24.6)  + 0.32(9.8) + 0.28(65.6+0)



                                Md = 32.33 Ib/lb-mol
6. Molecular weight of stack gas, Ib/lb-mol.




                         Ms =Md(l-BJ100) + 18(Bws/100)




                       Ms = 32.33(1-9.98/100) +  18(9.98/100)




                          Ms = 32.33(0.9002) + 18(0.0998)




                               M. = 29.1035 + 1.7964
                                Ms = 30.90 Ib/lb-mol

-------
7.  Absolute stack gas pressure, in. Hg.
                                    P  = P.   +
                                     s     bar
                                                  static


                                                7i6~
                                       = 29.4 +
                                                 13.6
                                   P. = 29.4 inches Hg
8.  Stack velocity at stack conditions, fps.





                            v  = 85.49  C.
                                                    ^
                                                      ts+460



                                                       M. P.
                       v  = (85.49)(0.84)(1.0831)
                                                  ^
                                                    (253.7 +  460)


                                                     (30.90) (29.4)
                                      vs  = 68.94 fps
9. Isokinetic Variation.
                             T „
                                                    (17.32)
                                  (vs) (Dn2) (0) f s) (1 -BJ100)
                      I =
                                (127.849) (253.7^460) (17.32)


                          (68.94) (0.217)2 (180) (29.4) (1-9.98/100)
                                        I =  102.2

-------
10.     Stack gas volumetric flow rate at stack conditions, acfrn.


                                   Qa  =  (60)  (A) (vs)



                               Qa  = (60) (12.306) (68.94)



                                    Qa  = 50,903 acfm




11.     Dry stack gas volumetric flow rate at standard conditions, dscfin.




                               =  17 64 Q-
                  Q     = (17.64) (50,903)  	—	   (1-9.98/100)
                   s(std)   V                 253.7+460   V           ;
                                  Qs(std) = 33,297 dscfm
12.     Dry stack gas volumetric flow rate at standard conditions, dscmm.





                                       = Qs(std) 0-028317




                                     = C33'297) (0-028317)





                                         = 943

-------
13.     Pollutant (2378 TCDD) concentration, ng/dscm.
                                 ng/dscm  = 	—
                                             *m(std)m3
                                   ,,        [ 0.0171 ]
                                 ng/dscm =	-
                                              3.620
                                ng/dscm = [ 0.00472 ] 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, = ([0.00472]) 	—	
                             02               (20.9 - 9.8)



                     ng/dscm@7%O2 = [0.00591] ng/dscm@7%O2
15.     Pollutant (2378 TCDD) emission rate, ng/hr.


                                       (60) (ng) (Q5(5td))

                                         do3) (vm(std))
                             ^hr- (60) ([0.0171]) (33,297)

                                        (103) (127.849)
                                //g/hr = [0.267] //g/hr

-------
16.     CEM Pollutant (HC1) Concentration, ppmd

                             ppmd = ppmw / (1 -Bws/100)

                             ppmd = 22.7 / (1-9.98/100)

                                  ppmd  = 25.2  ppmd



17.     CEM Pollutant (HC1) Emission Rate, Ib/hr.

                           lb/hr = (60) (ppmd) (Fwt) (Qs(std))
                                         (106) (385.3)

                          lb/hr  =  (60) (25.2) (36.47) (33,300)
                                         (106)  (385.3)

                                  lb/hr  = 4.77  lb/hr


18.     Method 3A Calibration Error, %. Values are for the oxygen, high range.

       Cal Err % =(100) (Instrument Response-Calibration Gas Concentration)/Span
                          Cal Err % = (100) (19.0 - 19.2) / 25

                                 Cal Err % =  -0.8 %


19.     Method 3 A System Bias Check, %. Values are for the oxygen, final upscale check.

          Sys Bias %  =(100) (Instr. ResponseCALERR-Instr. ResponsesysCAL)/Span

                          Sys Bias % = (100) (19.0 - 19.3) / 25

                                  Sys Bias %  = -1.2 %

-------
20.    Method 3 A Drift, %. Values are for the oxygen, upscale check.

        Drift % = (100) (Instr. ResponseFINAL sys CAL - Instr. Response^^ SYS CAL ) / Span

                           Drift %  - (100)  (19.3 - 18.9) / 25

                                    Drift %  = 1.6 %
21.      Method 3 A Zero & Upscale Sampling System Check Adjustment.  Values are for
        oxygen, %.

                                                  C
                                r    =(c   -c ^    ma
                                \^	   \ ^-s „,,„  V^/-\ I
                                C   =(9.8-0.1)
                                                  19.2
                                                19.1-0.1
                                      Cgas =  9.8 %
   Where:
C
C
C,
^i
C
                      avg

                      O

                      ma
= Adjusted gas concentration, ppm or %
= Average unadjusted gas concentration from analyzer
= Average of zero gas initial & final system cal. bias check
= Actual concentration of the upscale calibration gas
= Average of upscale initial & final system cal. bias check

-------
22.     Method 322 Zero & Upscale System Bias Checks Adjustment To Analyzer HCI Average.

                                            (C   -b)
                                              avg   °
                                               m
                            C   = - -
                             gas                 ~
                           (0.989 + 1.011) [(2°-49  M9)] +(1.10+2.10)
                         = _	      0.988	
                      gas
                                          = 22'7
   Where:            bc      = Y-intercept of the calibration least-squares line.
                     bf      = Y-intercept of the final bias check 2-point line.
                     b;      = Y-intercept of the initial bias check 2-point line.
                     Cgas    = Effluent gas concentration, as measured, ppm.
                     Cavg    = Average gas concentration indicated by gas analyzer, as
                              measured, ppm.
                     mc     = Slope of the calibration least-squares line.
                     mf     = Slope of the final bias check 2-point line.
                     m,     = Slope of the initial bias check 2-point line.

-------
23.     Method 322 HCI Matrix Spike Recovery, Pretest

  In Situ HCI Expected (Predicted) Spike Concentration, ppm.

                        CE = (Cs) (Q./QJ +(Su)(l-(Qs/Qtot))

                      CE = (303) (1.5/14.0) + (7.4)(1-(1.5/14.0))

                                   CE  = 39.1 ppm
  Where:            CE    = Recovery efficiency of spiked HCI, %
                    Cs    = Concentration of HCI in spike gas, ppm
                    Qs    = Spike gas (dilution) flow rate, 1pm
                    Qt    = Sample gas (unspiked) flow rate, 1pm
                    Qtot    = (Qs+Qt)  Sum of the spike gas and the sample flow rates, 1pm
                    Sy    = Concentration of unspiked (native) sample gas
   In Situ HCI Spike Recovery Efficiency. %.

                                 %R  = (SM/CE)(100)

                                %R = (42.6/39.1)(100)

                                    %R = 109 %
   Where:           %R   =  Efficiency of recovery of spiked HCI, %
                    SM    =  Observed concentration of spiked + sample gas, ppm
                    CE    =  Expected or predicted concentration of HCI in spike gas, ppm

-------
APPENDIX E




QA/QC DATA

-------

-------
                                                                                                   10f2
                 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

£-,;..:.-: . ' •' ' *;^w3K«i^
Date:
Pb., in Hg

9/1/97
30.16

Calibrator Tom McDonald Meter Box No.:
Reference Meter Correction Factor
MB-10
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
(^
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
<°F)
74
77
80
Final, Inlet
CF)
78
80
81
Avg. Inlet
CF)
76
78.5
80.5
Initial, Outlet
CF)
73
75
77
inal, Outle
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. H2O)
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
^
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, Outle
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
T
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)
80
80
80
inal, Outle
CF)
80
80
80
Avg. Outlet
CF)
80
80
80

Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
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
10 09017.XLS
                                                                                           Printed: 6/11/98

-------
                                                                                                      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
(^
55.868
63.519
71.182
Final
(ft3)
63.519
71.182
78.845
Net
(ft3)
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
81
81
81
inal, 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
Y
1.021
1.025
1.024
Reference
Orifice Press
AH0
(in. H20)
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
(ft3)
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
693.395
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
T
1.023
1.021
1.025
Reference
Orifice Press
AH0
(in. H20)
2.44
2.45
2.43
    Calibration Results
| AH | y | AHe |
0.50
0.75
1.0
2.0
4.0
1.020
1.020
1.020
1.023
1.023
1.73
1.79
1.78
1.86
2.44
                                                 Dry Gas Meter MB-10 on 09/01/97
                                                 Meter Box Calibration Factor
                                                 Meter Box Reference Orifice Pressure
                            1.021
                             1.92
10 09017.XLS
                            Printed: 6/11/98

-------
    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:         7/9/98   P^, in Hg
  1.021
    17
 1.0077
29.95   Calibrator:
D. Holzschuh
Meter Box No.
MB-10
AH= 1.53
Trial
1
2
3
Duration
(min)
10
11
10
Dry Gas Meter
Initial
(ft3)
611.3
618.025
625.403
Final
(ft3)
618.025
625.403
632.111
Net
(ft3)
6.725
7.378
6.708
Initial, Inlet
(°F)
79
77
77
Final, Inle
(°F)
77
77
77
Avg. Inlet
(°F)
78
77
77
Initial, Outlet
(°F)
79
78
77
Final, Outlet
(°F)
78
77
77
Avg. Outlet
(°F)
78.5
77.5
77

Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
432.055
438.894
446.392
Final
(ft3)
438.894
446.392
453.2
Net
(ft3)
6.839
7.498
6.808
Meter Temperature
Initial
(°F)
77
79
77
Final
(°F)
79
77
77
Avg.
(°F)
78
78
77
Meter Box
Correction
Factor
y
1.021
1.019
1.019
Reference
Orifice Press
AH0
(in. H2O)
1.85
1.87
1.87
10 09017.XLS
                    PostTest07-09-98
                                                                   7/10/98

-------
                                                                                                        1of2
                                    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:
        10/13/97
Calibrator.   MMD
                                                                            Meter Box No.:   RMB-15
, in Hg   29.86
                                                           Reference Meter Correction Factor     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
CF)
72
74
76
inal, Outle
CF)
75
75
77
Avg. Outlet
CF)
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
y
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
T
0.996
0.997
0.995
Reference
Orifice Press
AH0
(in. H2O)
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
•IK 4MVT Yl
                                                                                                 Printed: 6/11/98

-------
                                                                                                               2 of 2
J
5 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
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
13.863
20.884
26.372
Final
(ft3)
20.884
26.372
31.871
Net
(ft3)
7.021
5.488
5.499
Meter Temperatures
Initial, Inlet
(eF)
87
90
90
Final, Inlet
CF)
91
92
93
Avg. Inlet
CF)
89
91
91.5
Initial, Outlet
CF)
83
84
84
inal, Outte
(°F)
83
84
84
Avg. Outlet
CF)
83
84
84

Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
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
(°F)
73
73
73
Final
(°F)
73
73
74
Avg.
(°F)
73
73
73.5
Meter Box
Correction
Factor
y
1.001
1.002
1.002
Reference
Orifice Press
AHC
(in. H20)
1.90
1.89
1.88
AH = 4.0
Trial
1
2
Trial
Duration
(min)
6.5
15.5
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
32.371
39.484
Final
^
39.484
56.484
Net
^
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. H2O)
1.92
1.92
          Calibration Results
AH
Y
AH0
                         0.50
                         0.75
                          1.0
                          2.0
                          4.0
            0.999
            0.996
            1.000
            1.002
            1.004
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
      15  10137.XLS
                                                                                  Printed: 6/11/98

-------
                                                           €
    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:            7/9/98 P**, in Hg
 1.000
   16
1.0077
 29.95 Calibrator
DDH
Meter Box No.
RMB-15
AH= 1.39
Trial
1
2
3
Duration
(min)
10
10
10
Dry Gas Meter
Initial
(ft3)
356.55
362.922
369.302
Final
(ft3)
362.922
369.302
375.662
Net
(ft3)
6.372
6.380
6.360
Initial, Inlet
(°F)
77
77
77
Final, Inle
(°F)
77
77
77
Avg. Inlet
(°F)
77
77
77
Initial, Outlet
(°F)
77
77
77
Final, Outlet
(°F)
77
77
77
Avg. Outlet
CF)
77
77
77

Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
455.45
461.749
468.028
Final
(ft3)
461.749
468.028
474.295
Net
(ft3)
6.299
6.279
6.267
Meter Temperature
Initial
(°F)
75
74
74
Final
CF)
74
74
74
Avg.
(°F)
74.5
74
74
Meter Box
Correction
Factor
Y
0.997
0.994
0.995
Reference
Orifice Press
AH0
(in. H20)
1.96
1.97
1.98
15 10137
                    PostTest07-9-98
                                                                  8/18/98

-------
                                                        REFERENCE  METER  CALIBRATION
                                                        ENGLISH REFERENCE METER UNITS
Barometric Pressure    29.82
Meter Yw             1.00000
K ( deg R/inches Hg)   17.64
                                                        DGN Serial
                                                        Date
                                                                          6841495
                                                                         10/5/97
                                               Temperature
                                                Initial    Final
                                   (cubic feet) (deg F)   (deg F)
                       Dry Gas Meter (DGM)
 Time  Pressure   Meter Readings      Volune
(win)  (in. H20)  Initial   Final                  .
20.50     -8.000  742.719  768.193      25.474      78.0     79.0
 5.00     -8.000  768.193  774.402       6.209      79.0     79.0
13.00     -8.000  774.402  790.575      16.173      79.0     79.0
 8.50     -5.400  790.575  798.821
27.50     -5.400  798.821  825.423
26.50     -5.400  825.423  850.983
14.00     -3.800  850.983  861.899
15.50     -3.800  861.899  873.960
12.50     -3.800  953.219  962.970
23.50     -2.400  962.970  976.611
17.50     -2.400  976.611  986.740
15.00     -2.400  986.740  995.413
32.00     -1.600  995.413 1008.596
3S.C'>     -1.600 1008.596 1022.986
15.00     -1.600 1022.986 1029.158
8.246
26.602
25.560
10.916
12.061
9.751
13.641
10.129
8.673
13.183
14.390
6.172
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
80.0
81.0
81.0
82.0
86.0
87.0
87.0
88.0
89.0
89.0
90.0
                             Filename:   F:\DATAFILE\CALIBRAT\CAL NENU.DSKXDGH REF.
                             Revised:    06/08/95
             Wet Test Meter (UTM)           DGM      Coefficient     Flow
Meter Readings      Volume      Temp    Coefficient   Variation     Rate
Initial   Final  (cubic feet)  (deg F)      Yds      Vds-(Avg.Yds)   (CFM)
671.890  697.180      25.290       77.0       1.016         0.002      1.208
697.180  703.325       6.145       77.0       1.013         0.000      1.204
703.325  719.309      15.984       77.0       1.012        -0.002      1.204
                     Max Yds - Min Yds -0.003626886 Must  be no  greater than 0.030
                           Average Yds -1.013636253 Nust  be between 0.95 to 1.05

                       8.176       77.0       1.009         0.001      0.942
                      26.324       77.0       1.008         0.000      0.938
                      25.216       77.0       1.006        -0.001      0.932
                     Nax Yds - Min Yds -0.002262496 Nust  be no  greater than 0.030
                           Average Yds -1.007525980 Nust  be between 0.95 to 1.05

                      10.795       77.0       1.006         0.001      0.755
                      11.920       77.0       1.006         0.001      0.753
                       9.554       78.0       1.004        -0.001      0.747
                     Max Yds - Min Yds -0.002245979 Must  be no  greater than 0.030
                           Average Yds -1.005164785 Nust  be between 0.95 to 1.05

                      13.394       78.0       1.003        -0.001      0.557
                       9.946       78.0       1.004         0.000      0.556
                       8.524       78.0       1.006         0.002      0.556
                     Nax Yds - Nln Yds -0.002785363 Nust  be no  greater than 0.030
                           Average Yds -1.004591811 Nust  be between 0.95 to 1.05

                      12.956       78.0       1.006        -0.002      0.396
                      14.150       78.0       1.007         0.000      0.395
                       6.080       78.0       1.010         0.002      0.396
                     Nax Yds - Nin Yds -0.004205886 Must  be no  greater than 0.030
                           Average Yds -1.007822494 Nust  be between 0.95 to 1.05

                   Overall Average Yds -1.007748265
                                                                 719.309  727.485
                                                                 727.485  753.809
                                                                 753.809  779.025
                                                                 779.025  789.820
                                                                 789.820  801.740
                                                                 879.651  889.205
                                                                 889.205  902.599
                                                                 902.599  912.545
                                                                 912.545  921.069
                                                                 921.069  934.025
                                                                 934.025  948.175
                                                                 948.175  954.255
                 I certify that the above Dry  Gas Meter was calibrated in accordance  with E.P.A. Method 5  , paragraph 7.1 :CFR 40 Part 60,
                 using the Precision Wet Test Meter * 11AE6, which in turn was calibrated using the American Bell Prover * 3785,
                 certificate * F107, whJcX is traceable to the National Bureau of  Standards (N.I.S.T.).
                                     /IS    u
                          Signature  /gL^ M
                                                                 Date
                                                                           SO-Sr-

-------
                                     REFERENCE METER  CALIBRATION
                                     ENGLISH  REFERENCE METER UNITS
Barometric Pressure    29.73
Meter Yw              1.00000
K ( deg R/inches Hg)   17.64
                                     OGM Serial  *
                                     Date
         6841495
        8/28/96
                                                                             Filename:  F:\OATAFILE\CALIBRAT\CAL MENU.OSKXDGM REF.
                                                                             Revised:   06/08/95
Time Pressure Meter Readings
(min) (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
15.30
13.50
35.30
-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 Meter (DGM)     Temperature
                    Volume    Initial    Final
                 (cubic feet) (deg F)   (deg F)
             Wet Test Meter (UTM)
Meter Readings      Volune
Initial   Final  (cubic feet)
                                                                                           DGM       Coefficient      Flow
                                                                                Temp    Coefficient   Variation      Rate
                                                                               (deg F)      Yds       Yds-(Avg.Yds)  (CFM)
                                                                       7.415       77.0       1.007         -0.004     1.207
                                                                      29.484       77.0       1.011          0.000     1.200
                                                                       9.808       77.0       1.015          0.004     1.197
                                                                     Max Yds - Hin Yds -0.007489914  Must be no greater than 0.030
                                                                           Average Yds >1.011058546  Must be 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       77.3       0.999         -0.006     0.927
                                                                     Max Yds - Nin Yds »0.014197179  Must be no greater than 0.030
                                                                           Average Yds '1.004786738 Must be 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 be no greater than 0.030
                                                                           Average Yds '1.000808891  Must be between 0.95 to 1.35

                                                                       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 be no greater  than 0.030
                                                                            Average Yds  '1.003302205  Must be between  0.95 to  1.35

                                                                        6.393        78.0      1.016         0.011     0.396
                                                                        5.406        78.0      0.994         -0.010    0.390
                                                                       14.115        78.0      1.003         -0.001     0.393
                                                                      Max 'a*  -  Hin fds *0.321724294  Must be no greater  than 0.030
                                                                            Average Yds »1.004344616  Must be between 0.95 to 1.35

                                                                    Overall Average Yds »1.004860199

!  certify that the above Ory  Gas Meter was calibrated in accordance  with s.P.A. Method 5 .  paragraoh 7.1  ,-CFR 40 Part 60,
      the Precision Wet rest Meter # 11AE6. which  in  :urn xas calibrated using the American  Sell Prover 4 3785,
7.450
29.523
9.809
9.442
33.472
15.845
9.706
10.896
45.469
9.176
23.504
37.397
6.052
5.493
14.209
73.0
74.0
76.0
76.0
77.0
77.0
78.0
78.0
78.0
79.0
80. 3
80.0
81.0
82.0
82.0
76.0 496.572 503.987
76.0 503.987 533.471
76.0 533.471 543.279
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
31.0 734.785 771.901
32.0 771.901 777.994
32.0 777.994 783.400
32.0 783.400 797.515
certificate 4 ?107. vdijfch is traceable to the National Sureau if Standards (N.i.S.r.;.
         Signature
 Date

-------
              TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No. l\Avb-

Ambient Temp. °F
                               Sensor Type
                                                     Length
                                                           **
                                    Barometric Pressure, "Hg
                                                             , c/
Reference Temp. Sensor:
Date
b-zo-<^















Test
Sensor
34-
7t
^>5-



,











Temp.
Diff. %

o
















Within
Limits
Y/N


















Calibrated
By


















% Temp. Diff =  (Ref' Temp * 4!0) " (  Tegt
     ^                    (Ref.  Temp. + 4
                                                    460)
                                         460}
                                                         x 100 * 1.5 *

-------
(C
TEMPERATURE SENSOR CALIBRATION FORM
       Temperature Sensor No.
       Ambient Temp. °F
       Reference Temp. Sensor:
rNo. K^-io
"1 <•
oisor:
Sensor Type |£-Tc. Length
Barometric Pressure. "Hg Z

i~*
,<*t&/

Date
VZ0-1Y
•*(
»/•















Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
,
triP-
ftoic-
K«-0















Temp. °F
Ref.
Sensor
3-z-
•7<*
-Z^«pc,















Test
Sensor
3f-
17
'^^"















Temp.
Diff. %
.^•oc,
./ ^Q,
O/S^















Within
Limits
Y/N
y
y
X















Calibrated
By
(1U^
a^
^















 C.
         % Temp. Diff =
         Temp + 460) -  ( Test Temp. * 460)  x 10Q
              (Ref. Temp. + 460)

-------
              TEMPERATURE SENSOR CALffiRATION FORM
                   £K3>~                  ^  -r             \(

Temperature Sensor No. DG.M - \ P     Sensor Type s -TC    Length  v


Ambient Temp. °F	T4	  Barometric Pressure, "Hg -*>o
Reference Temp. Sensor:
Date
^ifr-^lr
Cf
tf















Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
iVio
k~\ C-
^feV<-i















Temp. °F
Ref.
Sensor
33
7t
zov















Test
Sensor
^ o
""7 ^h*
tl O















Temp.
Diff . %
.4ot>
o
.*1T















Within
Limits
Y/N
N|
V
X















Calibrated
By
\(,J^
a^S
\i^















Tenip
   c
. Diff = (*ef '
                                   Te8t
                                                    46Q)
                            (Ref. Temp. + 460)
                                                         x 100 S 1.5

-------
              TEMPERATURE SENSOR CALIBRATION FORM
                                          .
Temperature Sensor No. PC .n-oof   Sensor Type K-T^     Length
Ambient Temp. °F	3^	   Barometric Pressure, "Eg •sa.'E.V
Reference Temp. Sensor:	
Date
,-l*V
'•
.1















Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
£1
£**
^0















Temp. °F
Ref.
Sensor
&
•7-t
^o'6















Test
Sensor
33
-7^
tcof




•










Temp.
Diff. %
0
.it!
Q
•














Within
Y/N
V
Y
Y
- -














Calibrated
By
f\i^>
7
-------
09/14/98   10:09    ©313  398 3342
                                       PES CINCINNATI   -»-»•» DURHAM
                              121010/012
                      PACIFIC ENVIRONMENTAL SERVICES.1NC.
                                                                   4700 Duke Drive,
                                                                         Suite-ISO
                                                                      Mason, Ohio
                                                               Phone: (513) 398-2556
                                                                 Fax:(513)3983342
                                                                     www.pes.com
                   TEMPERATURE SENSOR CALIBRATION DATA
                          FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
                                   T5A
                                             DATE:
                       12/22/97
BAROMETRIC PRES.(in.Hg):
  AMBIENT TEMP. °F:
                                   29.52
                                  72
 REFERENCE:
"Mercury-in-glass:

 Other:

"CALIBRATOR:
                                                                    ASTM-3F
                                                                      J.C.
Reference
point
number
1
2
3
4
Source*
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
72
44
204
400
Thermocouple
Potentiometer
Temperature,1^
72
44
204
400
Temperature
Difference,*
%
0.00
0.00
0.00
0.00
 "Type of calibration used.

 6fref. temp-'F+AeOWtest thermometer temp °F+46Q1
                                        X100
             ref temp,°F+460
  Comments:
                  100<1.5%
                        STACK THERMOCOUPLE CALIBRATION FORM      1998 Yearly Calibration

-------
09/14/98   10:09    C513 398 3342
      PES CINCINNATI   •»•»•» DURHAM
                                                                           10012/012:
                     PACIFIC ENVIRONMENTAL SERV1CES.INC.
                                 4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                             Phone: (513) 338-2556
                                Fax: (513)3983342
                                   www.pM.com
                   TEMPERATURE SENSOR CALIBRATION DATA
                          FOR STACK THERMOCOUPLES
 THERMOCOUPLE NUMBER:
T6F
 DATE:
12/23/97
 BAROMETRIC PRES-(ln.Hg):
 AMBIENT TEMP. °F:
29.52
 74
 REFERENCE:
'Mercury-in-glaaa:

 Other:

'CALIBRATOR:
                                                                   ASTM-3F
                                                                     G.Gay
Reference
point
number
1
2
3
4
Source"
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot OH
Reference
Thermometer
Temperature.'F
74
34
172
349
Thermocouple
Potentiometer
Temperatur»,eF
74
33
172
350
Temperature
Difference,"
%
0.00
0.20
0.00
0.12
  Type of calibration used.

  bfreL temp.°F+4eOWtest thermomete
             reftemp,°F+460
  Comments:
       X100
                  100<1.5%
                        STACK THERMOCOUPLE CALIBRATION FORM       1998 Yearly Calibration

-------
5H
PACIFIC ENVIRONMENTAL SERVICES, INC.
                       4700 Duke Drive.
                              Suite ISO
                      Mason, Ohio 45040
                    Phone: (513) 398*2526
                      Fax (513) 398-3342
                          www.pes.com
Pitot Tube Number: 5H Date:
Effective Length: 59" . Calibrated By:
Pitoc Tube Openings Damaged? YES | NO j
Pitot Tube Assembly Level? | YES j NO
a , = 0.7 '(< 10°) a 2 -
P , - 4 " « 5°) p , =
Y= 0.6 9 = 0.4 A =
z = A sin Y = 0.0100 cm (in.) 0.32 cm ( < 1/8 in.)
w » A sin 9 = 0.0067 cm (in.) 0.08 cm ( < 1/32 in.)
PA = 0.478 cm (in.)
12/22/97
S. Simon
1.6 °(< 10°)
3.3 °«5e)
0.956

                         Pfl =
                       0.478
cm (in.)
              i e
              1A
                         D,
         >\
                       0.375
                                           A
                              ...-g^^g.-.
cm (in.)
                                                                                       it»X>iiim!!i
           The types of face-opening mb alignment snawnaeovo wll not area tha D««»lna v>kJ«or CO(S) ao
           long as a, ana «JIB less tnon or equal to 10*. B, ana a, to !«• than or equal to S", i« las* than or
           •gualio O.32 cm (1/6 in.), and w » laaa than oraqual toO.OS on(1<»2 in.) (mforencel 1.O m
           grtftiCTrt -i B m	
                                     Pitot Tube Calibration Form
                                                                                     1998 Yearly Calibration

-------
6A
PACIFIC ENVIRONMENTAL SERVICES, INC.
                       4700 Duke Drive,
                              Suite ISO
                      Mason, Ohio 45040
                   Phone: (513) 398-2556
                      Fax (513) 398-3342
                          www.pes.com
Pitot Tube Number: 6A Date:
Effective Leneth: 75.5' Calibrated By:
Pitot Tube Openings Damaged? YES . | NO |
Pitot Tube Assembly Level? | YES | NO
a , - 1 c(< 10°) a , =
P , « 0.2 *(< 5*) pa -
Y= 2.2 6 = 1.1 A -
z = A sin Y = 0.039 cm (in.) 0.32 cm ( < 1/8 in.)
w = A sin 8 = 0.019 cm (in.) 0.08 cm (< 1/32 in.)
PA = 0.504 cm (in.)
12/23/97
S. Simon
0.2 *(< 10°)
0.8 °(<5°)
1.006

                                              0.505
                                            cm (in.)
                          Dt =
                              "vi,,.,



                       0.375
                                                     (•)
cm (in.)
                                                                          i a          rnowt V
                                                                          "		-~.»..j«MfatBg!H!l,.,.H..iti !•«»*>«.«.
                                                                               	."sl^,::
                                                                                   (c)
                                                                  (fl)
            T>* type* or face opening mBaignmenc mown above wil noc eftocx tn« &*««ln» vaiua of Qp(») so
            long a a ^anoOji* tees tnftnoroqukl to 1O". B,ona a. to le»*tr»n cr«qu«|to 6", *i« toes thud or
            oqu^ to 0.32 cm(i/fi in.), and w « toss than oraqutf toO.06 cm (1/32 In.) (rafaraneaii.o m
              rtin^ 1 A O
                                      Pitot Tube Calibration Form
                                                               1998 Yearly Calibration

-------
            NOZZLE CALIBRATION SHEET

Nozzle
Identification
Number

D 1 , in.

D2,in.

Dg, in.

AD, in.

Davg

Where:
   D1 2 3 = nozzle diameter measured on a different diameter, in.
          Tolerance = measure within 0.001 in.

   AD = maximum difference in any two measurements, in.
          Tolerance » 0.004 in.
   Davg= average of D1, D2,

-------
c
            NOZZLE CALIBRATION SHEET
DATE:
                                          CAUBRATION BY-
Nozzle
Identification
Number
c>urs3;£s;
Dvln.
0,~L\L
D2,in.
o,z^?
D3, in.

-------
            Po»t-K»Faxl*Dte .. • ;; 7671
                                                Airqas Specialty Gases
                                                                    325 McCaaUnd C«t
               •"  ,   |	     •*      	
Certificate of Analysis: E.K.A.  protocol vias Mixture
Red*
Cylinder No:
Cylinder Pressure:
Certification Date
   4149
CC84329
  I 2000
Reference Standard
                                     Purchase Order*
                                     Expiration Date:
                                     Laboratory:
                                      139680
3/2/01
                                     Cheshire, CT
        ation:
                   Component
     GMIS         Carbon Dioxide
     GMIS         Oxygen

Instrumentation:
     instrument/ModeUSerial No,
     RosemounVNGA20( I0/Rack*l
     S»rvomexA244/701 A188  •
Certified Concentrations
                                              Cvl. Number
                                              CC34977
                                              CC10014
                           Analytical Principle
                           NDIR
                           Parmagnetie
                                                  Concentration
                                                      14.08%
                                                      20.98%
     Analytical Methodoli >gy does not require correction for analytical Interferences.
Analytical Results:
      1st Component:
 Certification performed in
 procedures listed.
 Do not use cylinder below
                                                      11.033%
                                                                 Cone
                                                                 Cone
                                                                 Cone     11:627%
                                                                 AVG:     11484%
                                                                 Cone
                                                                 Cone
                                                                 Cone
                                                                 AVG:
                                                      114367%
                                                      it.040%
                                                      11.017%
                                                       11.040%
   Accordance with 'EPA Trsceabitity Pmiepot f.
   150pstg.
                                                                 using the assay
                                               Approve^ for Release

-------
Airgas
                                                                               Airgas Specialty Gas
                                                                                325 McCausland Court
                                                                                Cheshire. CT 06410
                                                                                FAX:  (203)250-6642
          Certificate of Analysis:  E.P.A. Protocol Gas Mixture
         Rec#
         Cylinder No:
         Cylinder Pressure:
         Certification Date
   4150
CC86922
   2000
  3/2/98
      Purchase Order*
      Expiration Date:
      Laboratory:
                13980
               3/2/01
             Cheshire. CT
         Reference Standard Information;
              Type          Component
              GMIS
              GMIS
Carbon Dioxide
Oxygen
         instrumentation:
              tnstmment/Model/Serial No.
              Rosemount/NGA2000/Rack#1
              Servomex/244/701/488
               Cvl. Number
               CC34977
               CC19914
                            Analytical Principle
                            NDIR
                            Parmagnetic
                          Concentration
                              14.08 %
                              20.98%
              Analytical Methodology does not require correction for analytical interferences.
         Certified Concentrations:
         Analytical Results:
               1st Component:
               2nd Component:
Cone
Cone
Cone
AVG:
19.066%
19.006 %
18.964%
19.012 %
               1st Analysis 0**:
               R       173.630
               S       156-970"
               Z         1.800
    3/298
    S
    Z
    R
156.890
  1.420
173.630
Z
R
S
                                  1.460
ITSTStO
157.030
Cone
Cone
Cone
AVG:
                                                        19.175 %
                                           19.165 %
                                           19.158 %
                                                                                    19.168 %
         Certification performed in accordance with "EPA Traceabfflty Protocol (Jan. 1998)" using ffie assay
         procedures listed.                                   ,
-------
     Scott Specialty Gases
    pped
 From:
1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
NC  27704
                                               Fax: 919-220-0808

             CERTIFICATE   OF   ANALYSIS
 PACIFIC ENVIRONMENTAL SER

 5001 SOUTH MIAMI
 3RD FLOOR,  SUITE #300
 RESEARCH TRIANGLE PA
               NC  27709-2077
                                    PROJECT #: 12-28662-001
                                    PO#: 104-98-0178
                                    ITEM #: 12023411   CAL
                                    DATE:  5/01/98
   CYLINDER #:  AAL13302
   FILL PRESSURE:   1400  PSIG
                       ANALYTICAL ACCURACY: +-1%
                       PRODUCT EXPIRATION:   5/01/2001
   BLEND TYPE :  RECERTIFICATION OF  CYLINDER
                                   REQUESTED GAS
COMPONENT                            CONC HOLES
                                           ANALYSIS
                                              (MOLES)
PROPANE
AIR
                         30.
           PPM
           BALANCE
30.0
PPM
BALANCE
 ANALYST:
           B.M. BECTON

-------
             Scott Specialty Gases
             1750 EAST CLUB BOULEVARD, DURHAM, NC 27704
                                                                  (919)2200803  FAX (919) 22DQBQB
             CERTIFICATE OF ANALYSIS: EPA PROTOCOL GAS
&
':>
Customer
Pacific Environmental Services
Attn: Mr. Frank Meadows
P.O. Box 12077              ;:
Research Triangle Park, NC 27709
                  .YTICAL INFORMATION
                                                 Assay Laboratory
                                                 Scott Specialty Gases, lac.
                                                 1750 East Club Boulevard
                                                 Durham, NC 27704 --
                                                                                    Pordiae Order 104-95-0121
                                                                                    Scott Project*  12-11271
                                                                                                   J$4, ' v.'^i;..
                       STATION
                    to exceed the minimum specifications of EPA Protocol Procedure #G1, issued September, 1993.   - •
                    Number   AAL-13302          Certification Date         04-18-95     Expiratkm Date
                    Pressure   2000  PSIG         Previous Certification      None
                                                 wkkfc* lent acted* reference
                                                  Cylinder Number
                                                  ALM-032005
                                                 Last Date Calibrated
                                                 03-23-95
                                                                                    Analvtica
                                                                                    +/- 1% NIST Directly Traceable
                                                                                    Balaace
                            Expiration Date
                            06-%
      73400/16804

      .YZER READINGS  &-Z*nG~ R-Refertac»C» T-TatC«.  i^ComfattoaCotflVfaat)
                                                                        Concentration
                                                                        95.5 PPM Balance in Air
                                                                                     Analytical Principle
                                                                                     Gas Chromatography
                           First Triad Analysis
                                                        Second Triad Analysis
                                                                                     Calibration Curve
                                M-1S-93   Ropowi Unto: Ana

                            STD-1397517   SPL-4M96I
                            SPL-437952    SPL-43M70
                            STD-1396973   STO-1395705
                                                         sn>-
                                                         SPL-
                                                         sn>-
                                                       SPL-
                                                       SPL-
                            Drte:
                            STD~
                            SPL-
                            SID-
                                       SPL-
                                       5PL-
                                            STD-
                                            SPL-
                                            SII^
SPL-
5PL-
5f&*
                                                                                      DMK
                             STD-     SPL-
                             SPL-     SPL-
                             STT>     STD-
                                                                  SPL-
                                                         SPL-     • SPL-
                                                         sn>-

-------
SPECIALTY GK.  DEPARTMENT
12722 S. WENTWORTH AVENUE
CHICAGO, IL  60628
                                         Certificate of Analysis - EPA Protocol Gas Standard                       page i of i
PERFORMED ACCORDING TO EPA TEACHABILITY PROTOCOL FOR ASSAY AND CERTIFICATION OP GASEOUS CALIBRATION STANDARDS (PROCEDURE *Q1)
Customer:Order Not314-053317-
  ROCHESTER  - APCI                                                                           Batch No:           861-34622
  77 DEEP ROCF.  RD.                   Notes i
  ROCHESTER            NY 14624-                                                             Cylinder Not        SG91S1288BI
                                                                                             Bar Code No:        DDJ496
                                                                                             Cylinder Pressure*: 2000 paig
  PO: GALSON   Rel:                                                                          Certification Date: 09/27/96
                                                                                             Expiration Date:    09/27/99
*** Certified Concentration **«  ********* Reference standards *********  ************* Analytical Instrumentation *********'
                    Certified                      Standard                Instrument      Serial     Last     Measurement
Component         Concentration    Cylinder /       Number   Concentration Make/Model      Number Calibration   Principal
PROPANE             58.3 t.28  PPM SG9128557BAL   GMIS            50.33  PPM Gow-Mac  750    594050    09/10/96 GC-FID

Balance Gas: AIR
Oxygen Concentration     19.9 %                                                      '


   * standard should not be used below 150 psig
Analyst: ^^/y     ^  J*?f~~~~^                      Approved By:

-------
For Technical Information Call
1-800-752-1597
                                                             PRODUCTS
 Air Produce* and Chemicals, Inc. • 12732 S. Hentworth Avenue, Chicago, IL 60628
                                                         ISO CERTIFICATION: 9002
  CERTIFICATE OF ANALYSIS:     EPA PROTOCOL GAS STANDARD
   PERFORMED ACCORDING TO EPA 1HACEABILITY PROTOCOL FOR ASSAY ANL CERTIFICATION OF GASEOUS CAUBRATION STANDARDS (PROCEDURE KG1)
Customers
 AIR PRODUCTS AND CHEMICALS, INC.
 4822 INDUSTRY LANE
 UDI BUSINESS PARK
 DURHAM            NC 27709
              Order No: 833-075875-01
              Batch No: 861-45269
              PO:
              Release:
Cylinder No:
Bar Code No:
                SG9170173BAL
                DDT476
Cylinder Pressure*: 2000 psig
Certification Date: 02/18/98
Expiration Date:   02/18/01
CERTIFIED CONCENTRATION
COBjMTB 0P t
PROPANE
Certified
Concentration
92.4t.C7 PPM
REFERENCE STANDARDS
Cylinder
Muabar
SG9128479BAL
Standard
TVP«
3MIS
Standard
Concentration
100.7 PPM
ANALYTICAL INSTRUMENTATION
XnatruMBt
Kaka/Model
Oow-Mac 750
Serial
Number
S940SU
La>t
Calibration
02/10/98
Maaauraaapt
rriaeipal
GC-PIO
 AIR
 Contaminant
 Oxygen Concentration
             Balance Ga*
21.0 %
 * STANDARD SHOULD NOT BE USED BELOW 150 PSIQ
                                                    Approved By;
                                                                             Jamet

-------
              SPECTRfl BH5ES
              277 Colt Street « Irvington. NJ 07111 USA  Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551

SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL (908) 454-7455
SHIPPED TO:
APCCLTD
60 Industrial Park Road West
Tolland.CT 06084
                                     CERTIFICATE
                                          OF
                                       ANALYSIS
861 ORDER*:        133817
TTERM:              3
CERTIFICATION DATE:  6/12/98
P.OJP:               3426
BLEND TYPE;	CERTIFIED
                                     CYLINDER f:CC88470
                                  CYLINDER PRES: 2000 psig
                                 CYLINDER VALVE: CGA330
                                               ANALYTICAL ACCURACY: + / - 6%
    COMPONENT
                 REQUESTED GAS
                      CONC
                                                                       ANALYSIS
Hydrogen Chloride


Nitrogen
                     42.0 ppm


                      Balance
46.0 ppm
 Balance
ANALYST:
-JL
                                           DATE:
 6/12/98
                 Ted Neeme
                          USA • United Kingdom • Germany • Japan
                                    tea  a a a a

-------
             SPECTRH ERSES
                                                           RECEIVED JUN  1  7
        ^^B 277 Cott Street • Irvington, NJ 07111 USA  Tel: (973) 372-2060 • (800) 929-2427 » Fax: (973) 372-8551

SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL (908) 454-7455
SHIPPED TO:
APCCLTD
60 Industrial Park Road West
Toiland,CT 06084
                                     CERTIFICATE
                                          OF
                                      ANALYSIS
SOI ORDER*:        133817
ITEM*:             4
CERTIFICATION DATE: 0/12/98
P.O.*:              3426
BLEND TYPE:        CERTIFIED
                                     CYLINDER *: 1836837Y
                                  CYLINDER PRES: 2000 psig
                                 CYLINDER VALVE: CGA330
                                              ANALYTICAL ACCURACY: + / - 8%
    COMPONENT
                 REQUESTED GAS
                      CONG
                                                                      ANALYSIS
Hydrogen Chloride
                     300 ppm
303 ppm
Nitrogen
                                                                        Balance
ANALYST:
                                           DATE:
                                                                         6/12/98
                Milp-iDoyle
                          USA • United Kingdom • Germany • Japan
                                    iso eooa

-------
        TABLE C-3.2
Chemical Lime Calibration Table
         25-June-98
           INLET
Marble FallsJX
THC

ZERO GAS
LOW RANGE
MID RANGE
HIGH RANGE
02

ZERO GAS
MID RANGE
HIGH RANGE
CO2

ZERO GAS
MID RANGE
HIGH RANGE
HCI

ZERO GAS
MID RANGE
HIGH RANGE
CALIBRATION ERROR TEST
Range 0 - 100ppm
ACTUAL CONG
0.0
30.0
58.3
92.4
Range 0 - 25%
ACTUAL CONC
0.0
11.04
19.2
Range 0 - 50%
ACTUAL CONC
0.0
11.03
19.0
RESPONSE
0.0
32.7
58.0
90.2

RESPONSE
0.1
11.2
19.0

RESPONSE
0.3
11.3
19.0
PREDICTED
-
29.3
56.9
90.2

DIFFERENCE
0.1
0.2
-0.2

DIFFERENCE
0.3
0.3
0.0
% CAL ERR
-
11.4%
1.9%
0.0%

% SPAN
0.4%
0.6%
-0.8%

% SPAN
0.6%
0.5%
0.0%
Range 0 - 350ppm
ACTUAL CONC
0.0
46.0
303.0
RESPONSE
1.9
44
299.4
DIFFERENCE
1.9
-2.0
-3.6
% SPAN
0.5%
•0.6%
-1.0%

-------
Project Number
Firm Name
Site Location
Test Number
Source
Date
                                             Continuous Emissions Monitoring Data Sheet
                                                          EPA Methods 3A, 25A, and 322
                          98042
       PES
    Marble Falls
	1	
 Inlet Chemical Lime
      6/25/98
 Testers
_ Ambient Temp
 Time
                                     100
15:43-18:26
     Analyzer
Hydrogen Chloride
Total Hydrocarbons
Oxygen
Carbon Dioxide
     Range
     0-350ppm
     0-lOOppm
                          D-25%
                          0-50%
                                     :ero
                                     upscale
                                                     Rack Cal.
                                     zero
                                     upscale
                                     upscale
                                     zero
                                     upscale
                                                         1.9
                                                        299.4
                                                        n/a
                                                        n/a
                                                         0.1
                                                        19.0
                                                         0.3
                                                        19.0
                               PreTest
                               Sys. Cal.
                                                                     1.9
                                                                    299.4
                                                                     0.0
                                                                     90.2
                                                                     0.2
                                                                     18.9
                                                                     18.5
                         Cal. Bias
                         % of Span
                                                                                 0.0%
                                                                                 0.0%
                                                                                  n/a
                                                                                  n/a
                                                                                 0.4%
                                                                                 -0.4%
                                                                                 0.0%
                                                                                 -1.0%
Post Test
Sys. Cal.
                                                                                               3.0
                                                                                              296.9
                                                                                               0.2
                                                                           90.3
                                                                           0.0
                                                                                              19.3
                                                                                               0.3
                                                                                              18.5
 Cal. Bias
% of Span
                                                                                 ±5%
                                                                                                           0.3%
                                                                                                          -0.7%
                                                                                                            n/a
                                                                        n/a
                                                                       -0.4%
                                                                                       1.2%
                                                                                       0.0%
                                                                                       -1.0%
                                                                                        ±5%
   Drift
% of Span
                                                                                                                       -0.3%
                                                                                                    0.7%
                                                                                                    -0.2%
                                                                  -0.1%
                                                                  0.8%
                                                                                    -1.6%
                                                                                    0.0%
                                                                                    0.0%
                                                                                    ±3%
Avg. Analyzer
Response
20.9
Actual Qas
Cone.
n/a

-------
                                INLET
                      HCIIn-SItu Matrix Spike
                       Recovery Efficiencies
Plant         Chem LimeMarble Falls, TX
Date         25-Jun-98
Project No.    98042
                              Cs-Spike Gas Cone, (ppm)     303
FesM
nitial
Rnal
Su-Native Concentration (ppm)
Qt-Analyzer Flow (Ipm)
Qs-DHution Rate (Ipm)
Sm-Observed Concentration (ppm)
Ce-Expected Concentration (ppm)
Spike Recovery (%)

Su-Native Concentration (ppm)
Qt-Analyzer Row (Ipm)
Qs-Dilution Rate (Ipm)
Sm-Observed Concentration (ppm)
Ce-Expected Concentration (ppm)
Spike Recovery (%)
 7.4
 12.5
 1.5
 42.6
 39.1
109%

 39.3
 11.7
 1.5
 84.3
 69.3
122%

-------
        TABLE C-3.1
Chemical Lime Calibration Table
         25-June-98
          OUTLET
Marble FallsJX

THC

ZERO GAS
LOW RANGE
MID RANGE
HIGH RANGE
02

ZERO GAS
MID RANGE
HIGH RANGE
CO2

ZERO GAS
MID RANGE
HIGH RANGE
HCI

ZERO GAS
MID RANGE
HIGH RANGE
CALIBRATION ERROR TEST




Range 0 - 100ppm
ACTUAL CONC
0.0
30.0
58.3
92.4
Range 0 - 25%
ACTUAL CONC
0.0
11.04
19.2
Range 0 - 50%
ACTUAL CONC
0.0
11.03
19.0
RESPONSE
0.0
32.7
58.0
90.7

RESPONSE
0.1
11.2
19.0

RESPONSE
0.3
11.3
19.0
PREDICTED
-
29.4
57.2
90.7

DIFFERENCE
0.1
0.2
-0.2

DIFFERENCE
0.3
0.3
0.0
% CAL ERR
-
10.8%
1.3%
0.0%

% SPAN
0.4%
0.6%
-0.8%

% SPAN
0.6%
0.5%
0.0%
Range 0 - 350ppm
ACTUAL CONC
0.0
46.0
303.0
RESPONSE
1.1
47.4
300.8
DIFFERENCE
1.1
1.4
-2.2
% SPAN
0.3%
0.4%
-0.6%

-------
Project Number
Firm Name
Site Location
Test Number
Source
Date
       98042
        PES
     Marble Falls
         1
                                               Continuous Emissions Monitoring Data Sheet
                                                             EPA Methods 3A, 25A, and 322
 Test era
_ Ambient Temp
 Time
 Outlet Chemical Lime
	6/25/98
                                       100
                                    15:19-18:50
      Analyzer
Hydrogen Chloride
Total Hydrocarbons
Oxygen
Carbon Dioxide
      Range
     0-350ppm
     0-100ppm
       0-25%
                           0-50%
                                       zero
                                       upscale
                  Rack Cal.
                                       zero
                                       upscale
                                       zero
                                       upscale
                                       zero
                                       upscale
                                       1.1
                                                          300.8
                                       n/a
                                                           n/a
                                                           0.1
                                                           19.0
                                       0.3
                                       19.0
Pre Test
Sys. Cal.
                                                    1.1
                                                                       300.8
                                                    0.0
                                                   90.7
                                                    0.1
                                                                         19
                                  0.3
                                  18.7
 Cal. Bias
% of Span
                                                                0.0%
                                                                                     0.0%
                                                                 n/a
                                                                 n/a
                                                                0.0%
                                                                                     0.0%
               0.0%
               -0.6%
               ±5%
Post Test
Sys. Cal.
                                                                              2.1
                                                                                                 308.4
                                                                              0.0
                                                                              92.8
                                                                              0.1
                                                                                                  19.5
                 0.3
                 18.8
 Cal. Bias
% of Span
                                                                                          0.3%
                                                                                                               2.2%
                                                                                           n/a
                                                                                                               n/a
                                                                                          0.0%
                                                                                                               2.0%
                0.0%
               -0.4%
                ±5%
   Drift
% of Span
                                                                                                       -0.3%
                                                                                                                           -2.2%
                                                                                                       0.0%
                                                                                                       •2.1%
                                                                                                       0.0%
                                                                                                                           -2.0%
                0.0%
                -0.2%
                ±3%
Avg. Analyzer
Response
15.5
Actual Gas
Cone.
n/a

-------
                                Outlet
                      HCI In-SItu Matrix Spike
                        Recovery Efficiencies
Plant          Cham LimeMarbte Falls, TX
Date          25-Jun-98
Project No.     98042	
                              Cs-Spike Gas Cone, (ppm)     303
Festl
nitial
Rnal
Su-Native Concentration (ppm)
Qt-Analyzer Row (Ipm)
OS-Dilution Rate (Ipm)
Sm-Observed Concentration (ppm)
Ce-Expected Concentration (ppm)
Spike Recovery (%)

Su-Native Concentration (ppm)
Qt-Analyzer Row Opm)
Qs-Dilution Rate (Ipm)
Sm-Observed Concentration (ppm)
Ce-Expected Concentration (ppm)
Spike Recovery (%)
 6.5
16.25
 1.5
33.3
31.5
106%

14.6
16.25
 1.5
41.2
39.0
106%

-------
                    APPENDIX?

                  PROCESS DATA
       Process data to be supplied to EPA EMC by
Research Triangle Institute under a separate work assignment.

-------

-------
                  APPENDIX G

         SAMPLING & ANALYSIS METHODS
(EPA Methods 1, 2, 3 A, 23 and proposed amendments, 25A, 322)

-------

-------
       Appendix G.I




Sampling & Analysis Methods




      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
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross section,  an equivalent diameter  (D.)  shall
be  calculated  from the  following  equation,   to  determine the
upstream and downstream  distances:
Prepared by Emission Measurement Branch              EMTIC TM-001
Technical Support Division, OAQPS, EPA

-------
        EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                        NSFS TEST METHOD
                           D.=
                                 2LW
                               (L + W)
                                                       Eq. 1-1
     Where
                    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
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.
 Prepared by Emission Measurement Branch
 Technical Support Division, OAQPS, EPA
EMTIC TM-001

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EMTIC TM-001          EMTIC NSPS TEST METHOD               Page 3


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.
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-

-------
EMTIC TM-001          EMTIC NSPS  TEST METHOD                Page 4


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-
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

-------
EMTIC TM-001          EMTIC NSPS  TEST METHOD               Page 5
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.
 (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

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EMTIC TM-001          EMTIC NSPS  TEST METHOD               Page 6


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.

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:

                R^^ = arc cosine [ (cosineYj)  (cosineP^ ]


                                                        Eq. 1-2

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EMTIC TM-001          EMTIC NSPS TEST METHOD               Page 7
Where:
          Ri   «    resultant angle at traverse point i, degree.
          Yi   =    yaw angle at traverse point i, degree.
          P4   m    pitch angle at traverse point i, degree.

2.5.4.2  Calculate the average resultant for the measurements:
                                                             Hj. 1-3
Where:
          Ravg  »    average resultant angle, degree.
          n    «    total number of traverse points.

2.5.4.3  Calculate the  standard deviations:
                                  (n-1)

                                                             Hj. 1-4
Where:
          Sd    =     standard deviation,  degree.

2.5.5   The  measurement location is acceptable if Ravg s 20° and S&
£  10°.

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.

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EMTIC TM-001          EMTIC NSPS TEST METHOD                Page 8


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
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

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EMTIC TM-001          EMTIC NSPS TEST METHOD                Page 9


     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
     1976.

6.   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.

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.

8.   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.

9.   Entropy Environmentalists,  Inc.   Traverse  Point Study.  EPA
     Contract No. 68-02-3172.  June 1977.  19 p.

10.  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.

11.  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.

12.  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.

13.  Smith,  W.S.  and D.J.   Grove.   A  Proposed  Extension of EPA
     Method 1 Criteria.   Pollution Engineering.   XV  (8):36-37.

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 10
     August 1983.

14.  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.

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
Page 11
               Table 1-1.   CROSS-SECTION LAYOUT FOR
                        RECTANGULAR STACKS
                      Number  of  traverse points
                          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
EMTIC NSPS TEST METHOD
Page 12
                            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 ....
.LA • • • •
13 ....
14 ....
Number of traverse points on a diameter
2
14
.6
85
.4












4
6.
7
25
.0
75
.0
93
.3










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
98.
2
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
91.
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
85
.4
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
79
.6
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
73.
8
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
67.
7

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 13
15 ....
16 ....
17 ....
18 ....
19 ....
20 ....
21 ....
22 ....
23 ....
24 ....






































































95.
1
98.
4








89
.1
92
.5
95
.6
98
.6






83
.5
87
.1
90
.3
93
.3
96
.1
98
.7




78.
2
82.
0
85.
4
88.
4
91.
3
94.
0
96.
5
98.
9


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
   EMTIC NSPS TEST METHOD
Page 14
              so
              40 -
              30 -
              20 -
              10 -
Duet Dtomotore Updraug tram Flow DMufbinco* (D

    1.0         1J
                                                 A)
1 1 1 1 1 1
•
10 MMkOk
1
1
V
I
\

:
i
\
i
?W»»tn»i
J,-.--
^Otrt»tiiiii
-
•MM>U1a(24M
11
•FimiP(M«fA«Typiof
OkkMkMic* (BMd. tUpvukw. Canine* «. «O
«HkDlMIMli
1 1 1 1 1 1
.„.•
< «OJO to OJIll (11-14 M
1 1
                      S     4     S      t     7     I

                      Dud Dtamttora Downstraim from Flow DMuibwic** (DManeo B)
                                                             10
         Figure  1-1. Minimum  number of  traverse points  for
         particulate traverses.

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 15
          so
             O.S
          40 -
          30 -
           20 -
           10 -
                     Duct Diameter* Upstream from Flow Dieturbance* (Dlatance A)

                          1.0           1.S            2.0
                                        2.5
1 1 1 1 1 1 1 1
a
Higher Number Is hr
Rectangular Stacks or Ducts




1* Stack Da

1


T5
T
B
i






^^Disturbance
UeaaiMMient
4

1
—

Disturbance
V - — 1



-






12
— • From Point of Any Type of
Disturbance (Bend. Expansion, Contraction, etc.)
aer.'
Stack Diameter - 0 JO to O.o t n (12-24 to.)
I I I I I I

I
                    3      4      5      6      7      B

                     Duct Diameters Downstream from Flow Disturbance* (Distance B)
                                                                   10
     Figure 1-2. Minimum number of  traverse  points for velocity
     (nonparticulate)  traverses.

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 16
        1      4A
        *      147
        *      2U
        4      7*J
        S      «U
    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
EMTZC NSPS TEST METHOD
Page 17
o
o
	
o
o
0
	
o
o
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.

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       Appendix G.2




Sampling & Analysis Methods




       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
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.
        j*
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  P» and  Ife ,  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. HjO 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.)  H,0.  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.)  H,0;  (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                            EMTZC M-002
 Technical Support Division, OAQPS,  EPA

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EMTIC TM-002                     HSPS TEST METHOD                       Page 3
                               + K
Where:

        Apt  -    Individual velocity head reading at a traverse point,  mn (in.)
                  H,0.

        n    »    Total number of traverse points.

        K    m    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.)
Kg.  The static tap  of a  standard type pitot  tube  or  one leg of a Type 8 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 TBST MBTROD                       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 8,  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  8 Pitot Tube.  Before its initial use, carefully examine the Type S
pi tot 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 P,,
Figure 2-2b) .   If Dt is between 0.48 and 0.95 cm (3/16  and 3/8 in.),  and if %
and P, are  equal  and between 1.05 and  1.50 £^, 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  De,  l)k, 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:

                                 D.  =    2LM
                                   *    (L  + W)


                                                                 Eq.  2-1
 Where:

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EMTIC TM-002                     NSPS TBST METHOD                       Page  7


        D.   •    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.

NOTB:  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/rain  (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 MRTHOD                        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 pi tot tube from the duct, and disconnect it
from the manometer.  Seal the standard  entry port.

4.1.3.5  Connect the Type S pi tot 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 Ap.,  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:
                              c    -c        AP>M
                               P(a)  ^ptstd)
                                             AP,


                                                                         Bq. 2-2
         Where:

         Cp(.)       -    Type S pitot tube coefficient.

         Cp(ltd)      »    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.

         Apltd      •    Velocity head measured by the standard  pitot tube,  cm
                        (in.) HjO.

         Ap.        -    Velocity head measured by the Type S pitot tube,  cm (in.)
                        H20.

 4.1.4.2  Calculate q, (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,.> from Cp (side A) ,  and the deviation of each B-side values of Cp,.,  from
Cp (side B) .  Use the  following equation:


                        Deviation  = C    -C  (A or B)
                                      p     p
                                                                  Eq.  2-3

4.1.4.4  Calculate o,  the  average deviation from the mean, for both the A and B
sides of the pi tot tube.  Use the following equation:
                  o(side A or B)  =
                                                                  Eg.  2-4

4.1.4.5  Use the Type S pitot tube only if the values of a  (side A) and  a (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.
2. 3
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.
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 XBTHOD
                                                                        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 nay 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,,, 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 f t/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,,,.
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 Tubes.  After each field use,  the pitot tube shall be

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EMTIC TM-002                     KSPS 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.  Qtherwise, 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
            NSPS TEST METHOD
                                                                      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)
                                                      1/2
                                     (°K)  (mmH-O)
for the metric system.
                   85.49
       ft
      sec
                                Ib/lb-mole) (in.Hg)
                                          (in.H,0)
                                                       1/2
for the English system.
          M.
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) .
                            = MH(1-BMJ +  18. OB
                                     ws
                                                ws
          '9


          P.
                                             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
                                                                 Eq.  2-6
                    Standard absolute pressure,  760 mm Hg (29.92  in. Hg) .

                    Dry volumetric stack gas  flow rate corrected to standard
                    conditions, dsmj/hr  (dscf/hr) .
          t.
Stack temperature, 8C (°F) .

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EMTIC TM-002
             NSPS TEST METHOD
Page 13
for metric.
                    Absolute stack temperature, °K (°R)
                                  = 273  + t.
                                                                  Eq.  2-7
                                  = 460  + t.
for English.

          T.td
          Ap    =

          3,600=

          18.0  =
                                                                  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. HaO) .

Conversion factor, sec/hr.

Molecular weight of water, g/g-mole  (Ib/lb-mole).
5.2  Average  Stack Gas Velocity.
— v r* /,/An I
KpCp (V^P)
T
1s(avg)
PsM»
                                                                  Eq. 2-9
5.3  Average  Stack Gaa Dry Volumetric Flow Rate.

                                               T
                    Qsd = 3,600(l-Bws)vsA
                                                std
                                               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.
                                              Eq. 2-10



                                          McGraw-Hill Book


                                          McGraw-Hill Book

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EMTIC TM-002                     NSPS TEST MBTHOD                      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. '  ASHRAB 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,  Bast
     Hartford, CT.   1975.

-------
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.

-------
EMTIC TM-002
                            NSPS TEST METHOD
                                                                               Page 16
   (Q.7S-1.0kq
    .La
           7J2cm(lki.)*
I  TwMc


V^
T*mp«nhin SMIMT
                         /     k
                               Typ*8PKDtTub*
               • 8ugg«iM Ontoitcnne* FtM)
               PNotlubWrtwrniocoupl* Spadng
Figure 2-1.   Type S pitot tube  manometer  assembly.

-------
EMTIC TM-002
NSPS  TEST METHOD
                                                                                              Page  17
                TubtAxto
         Ungtudlntl
         TutaAxh
                                            Fsra
                                           Opening
                                           PtaM
                                                 A-SktoPkuM
                                                                      Note:
                          M	s-
       	*_/L_.J 1*ll>|« P < 1.»ODt
                                                 B-SktoPlMM
                           _ —^|       fyi       \j- —3- — — — — -
                                             (e)
                                                                      (») tnt Htm; fce« •p»
                                                                        to kuwwiM nfc;
                                                                      (e) tM« vtow; bom tog* of •**! ktngth vid
                                   FIT-HTI nuifllrlinlTrtin ot
                             O.M m«y b* tulgiwd to plot Uwt eon.
                             MnietotfMiwir
Figure 2-2.    Properly constructed  Type S pi tot tube.

-------
EMTIC TM-002
NSPS TEST METHOD
Page 18
                                 2=37
           •-S
                     ~ in	    "V" 7y
 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 aj slO°, 31 and p* i5", z iO.32 cm  (1/8
 in.)  and w iO.OB cm (1/32 in.)  (citation 11 in Bibliography).

-------
EMTIC TM-002
NSPS TEST METHOD
Page 19
                                                     Cwndw
    Figure 2-4.   Standard pitot tube design specifications.

-------
EMTIC TM-002                     NSPS TEST MBTHOD                      Page 20

-------
EMTIC TM-002
                  NSPS TEST METHOD
                                 Page  21
PLANT
DATE _
RUN NO.
(in.)  __
.STACK DIA.  OR
DIMENSIONS, m  (in.)  	  BAROMETRIC PRESS., mm  Hg
 (in. Hg)      CROSS SECTIONAL AREA, m2 (ft*)	
OPERATORS 	
PITOT TOBE I.D. NO. 	
  AVG. COEFFICIENT, Cp -  	
  LAST DATE CALIBRATED,
                                 SCHEMATIC OF  STACK
                                   CROSS  SECTION
Traverse
Pt. No.













Vel. Hd., Ap
mm (in.) H2O













Stack Temperature
T.,
°C (°F)













Average
T.,
°K (°R)














*»
mm Hg
(in.Hg)














Up)1"














                      Figure 2-5.   Velocity traverse data.

-------
EMTIC TM-002
NSPS TKST MBTHOD
                                                                                Page 22
                                            !*•     t
                           A* Botton vbwi •nowinQ MMMMMH pMol
                            B. SldaVtnr. k>»nv«n1|>totlulwln>ffllMw1*ikl9wMgu
                             Dow «™»mSn« ippreichlng VM neijte. Vw Impact pn»ura
                             opwUnj pten* of *• plot Ink* Mwl t* *VM •*> of akev* ft*
                             nezzh •nby phiw.
  Figure  2-6.   Proper  pitot  tube-sampling  nozzle configuration  to prevent
  aerodynamic interference: button-hook type nozzle;  centers  of  nozzle  and
  pitot opening aligned; Dt between 0.48 and  0.95 cm  (3/16  and 3/8 in.).

-------
EMTIC TM-002
NSPS TEST MJCTHOD
Page 23
                              I  •
                    fa,  T>nirfc
                 |ot
                            ."»"•". I
                             • H  |
   Figure 2-7.   Proper thermocouple  placement to  prevent interference:  Dt

   between  0.48 and 0.95 cm (3/16 and 3/8 in.).

-------
KMTIC TM-002
NSPS TEST METHOD
Page 24
                                      TypcS Not Tufa*     ^
   Figure 2-8.    Minimum  pitot-sample  probe  separation  needed to  prevent
   interference;  Dt between  0.48  and  0.95 cm  (3/16 and  3/8 in.).

-------
EMTIC TM-002
NSPS TEST METHOD
         Page 25
PITOT TUBE IDENTIFICATION NUMBER:
         DATE:
.CALIBRATED BY:  _

RUN NO.
1
2
3
"A" SIDE CALIBRATION
AP.td
cm H2O
(in H2O)




AP(.>
cm HjO
(in H2O)



Cp.avg
(SIDE A)
Cp<»>





Deviation
Cp,., - Cp(A)





RUN NO.
1
2
3
"B" SIDE CALIBRATION
AP.td
cm H2O
(in H2O)




AP(.)
cm H2O
(in H,0)



Cp,,v5
(SIDE B)
Cpli)





Deviation
Cp,., - Cp(B)




   Average Deviation = a
                                 E
       Cp(s)   Cp(AorB)
                          (AorB)
                       •MustBesO.Ol
                   Cp(SideA) -Cp(SideB)hMustBes0.01

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EMTIC TM-002                  NSPS TEST MBTHOD                    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.

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       Appendix G.3




Sampling & Analysis Methods




      EPA Method 3A

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                  EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                                  NSPS TEST METHOD
        Method 3A -  Determination of Oxygen and Carbon Dioxide Concentrations
                        1n Emissions from Stationary Sources
                          (Instrumental Analyzer  Procedure)
1.  APPLICABILITY AND PRINCIPLE

1.1  Applicability.  This method is 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 CQ  concentration(s).    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 02
or C02 concentration.  The measurement system consists of the same major  subsystems as
defined in 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  System.   Any  measurement system  for 02 or  CQ  that  meets  the
specifications  of  this  method.   A schematic of an acceptable measurement  system 1s
shown in 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 Renoval  System.
Part1culate  Filter.  Sample Pump.  Sample Flow Rate Control.  Sample 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 02 or C02 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 C02 analyzers  shall  be C02  in N2 or
C02 in air.  Alternatively. C02/S02, 02/S02. or 02/C02/S02 gas mixtures in N2 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 in the field.  Thereafter, recheck the measurement system 1f

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EMTIC TM-003A                  NSPS TEST METHOD                               Page 3
changes are  made in 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 recommended  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 02 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 the2 0  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 02 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 QZ  analyzers that  use  a low-level  calibration gas in place  of a zero gas.
  Toil ate the effluent gas concentration using  Equation 3A-1.
                                     - C.) + C*                   Eq. 3A-1
                         c.-c0
Where:
       Cgw ~ Effluent gas concentration, dry basis, percent.
        C., - Actual concentration of the upscale  calibration  gas. percent.
        CM - 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.
         C - Average gas concentration indicated by the gas analyzer, dry basis.
        percent.
 10.   BIBLIOGRAPHY
 Same  as in Bibliography of Method 6C.

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       Appendix G.4




Sampling & Analysis Methods




      EPA Method 23

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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

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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.

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     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

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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

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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 Combust or s




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:

-------
itackwtl
X
IwMtd gtou «n«r

tampMM
MDU
I
h«»l
1
1
urn
tr
t
d

OwFtow
                 •8-Vp.
                  pltot
                            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 £l20°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 Nodule.  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 O-ring shall be used to make




the seal at the nozzle end of the probe.





                                12

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  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

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                T
                 3
                 to
                 o
   Flue
   Gas
   Flow
                 o
                 h.
       O
o
O
8
5
E
E
•o
* 20/15
                                        Sorbent Trap
                                              G)*M Sintered Dick
                                              XAD-2
                                                 Water Jacket
                                            Glass Wool Plug
             Condenser
                                              Cooling Coil
                                                 Water Jacket
                                               * 20/15
Figure 23.2  Condenser and Adsorbent Trap
                                 14

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15

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  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-tnL,  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

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  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

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  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

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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  MeCla 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 /il 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 /il of methylene chloride into 100 raL of toluene.   This




corresponds to 100 /KJ of methylene chloride per g of  adsorbent.




The maximum acceptable concentration is 1000 pig/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 jil




of the  surrogate standard solution  (Section  3.3.21) to each trap




for a sample that will be split prior to analysis or 20 fj.1 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 pil 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 Fractionation.




  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/Gelite™ 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

-------
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 /zl 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

-------
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

-------
  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

-------
  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

-------
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 /il 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

-------
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 /xl of




the surrogate standards in Table 2 for samples split for analysis




or 20 //I 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

-------
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.  Pill 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.




Aoij =   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.




AcSl =   Integrated ion current of the  two ions characteristic of





                                44

-------
        surrogate  compound i in the calibration standard.




 Ai =   Integrated ion current of the two ions characteristic of




        compound i in the sample.




 A\ =   Integrated ion current of the two ions characteristic of




        internal standard i in the sample.




 Aj-g =   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.




   Ci =  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.




DLgum  =   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

-------
  nirg =  Mass of recovery standard in the calibration standard



        injected into the analyzer, pg.



   tns =  Mass of surrogate compound  in the  sample  to be analyzed,



        pg.



  msi -  Mass of surrogate compound  i in the  calibration standard,



        pg.


 RRFi =  Relative response factor for compound i.



RRFrs =  Recovery standard response  factor.



 RRF8 -  Surrogate  compound  response factor.



vm(std)=    Metered  volume of sample  run, dscm.



 1000 =   pg per ng.



   9.2  Average Relative Response Factor.
                        A   10.

             RRF = -    C1J  Ci                           E<3- 23-1

                        A*  m
                         Clj  Ci
  9.3  Concentration of the PCDD's and PCDF'a,
                   A,* RRF. V
                     •*    •*  *".
                                                         Eq. 23-2
   9.4   Recovery Standard Response Factor.

-------
               RRF  =   ci ""                            Eq. 23-3
                  rs        *                              ^

                      Ars md
  9.5   Recovery of Internal Standards (R*)
                    i—££__xiOO%                         Eq. 23-4
                 *rs *Frs
  9.6  Surrogate Compound Response Factor.
                         .J m .
                                                        Eq. 23-5
                                                          ^
9.7  Recovery of Surrogate Compounds  (R.) .
            R  = 	Lf	xiQO%                          Eq.  23-6
             3     *                                       •*
  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 H .) 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 .) n^
            DL =	                         Eq. 23-8
                      *
Detection  limit using area of the noise.
                    2 . 5 Aai m,
               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.
         =  (13 DLICDD + 16 DLICDF + 12


         14 DL+ 7 "J     + 12
                                                           23 10
         + 2 DL    + 4 D£    + DL                            . 23-10
               BpCDD      BpCDF   OCDD

                      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.
                  C =   c.                             Eq. 23-11
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//*L)
                         Internal Standards
       13C12-2,3,7,8-TCDD
         100
       13C12-l,2,3,7,8-PeCDD
         100
       13
        C12-l,2,3,6,7,8-HxCDD
         100
       13C12-l,2,3,4,6,7,8-HpCDD
         100
       13Cn,-OCDD
        -12
         100
       13C12-2,3,7,8-TCDF
         100
       13C12-l,2,3,7,8-PeCDF
         100
       13
        C12-1, 2, 3 , 6 , 7 , 8 -HxCDF
         100
       13
        C12-1,2,3,4,6,7,8- HpCDF
         100
                        Surrogate  Standards
       37Cl4-2,3,7,8-TCDD
         100
       13C12-1,2,3,4,7,8 -HxCDD
         100
       13C12-2,3,4,7,8-PeCDF
         100
       13C12-l,2,3,4,7,8-HxCDF
         100
       13C12-l,2,3,4,7,8,9-HpCDF
         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//iD
1
2
3
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
4
5

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

-------
13C12-2/3,7,8-TCDF
13C12-1, 2 ,3,7, 8-PeCDF
13C12-l,2,3,6,7,8-HxCDF
13C12-l,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//xl)
1
2
3
4
5
SURROGATE STANDARDS
37Cl4-2,3,7,8-TCDD
13C12-2,3,4,7,8-PeCDF
13C12-l,2,3,4,7,8-HxCDD
13C12-l,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 (/zm)
Carrier Gas
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  (o 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
305.8987
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,Fu
CuH^C^O
C12H43SC13C137O
13C12H435C140
13C12H435C1337C10
C12H435C1402
C12H435C1337C102
C12H437C1402
C7F13
"C12H435C1402
"C12H43SC137C102
C12H335C1437C10
C12H335C1337C120
13C12H335C1437C10
13C12H335C1337C120
C12H335C1337C102
C12H335C1337C1202
13C12H335C1437C102
13C12H335C1337C1202
C12H43SC1537C10
C12H335C1637C10
C12H235C1537C1O
C12H235C1437C120
"C12H235C160
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

-------

401.8559
403.8529
445.7555
430.9729
M+2
M+4
M+4
QC
"C12H235C1537C102
13C12H235C1437C120
C12H23SC1637C120
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
C12H3SC1637C1O
C12H35C1S37C12O
13C12H3SC170
C12H235C1537C102
C12H235C1437C1202
C9F1S
13C12H23SC1537C102
"C12H235C1437C120
C12H235C1637C120
C9F17
C12H35C1637C1O
C12H35C1537C120
13C12H35C17O
13C12H35C1637C10
C12H35C1637C102
C12H35C1S37C1202
13C12H35C1637C102
13C12H35C1537C1202
C12H35C1737C120
C9F17
C1235C1737C10
C123SC1637C12O
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)
                                   57

-------

471.7750
513.6775
442.9728
M+4
M+4
QC
13C123SC1637C1202
C1235C1837C1202
^10^*17
OCDD(S)
DCDPE
PFK
                    35C1 = 34.968853
The following nuclidic masses were used:
H - 1.007825      O = 15.994914    C = 12.000000
"C = 13.003355   37C1  =  36.965903     F  =  18.9984
S = Labeled Standard
QC SB ion selected for monitoring instrument stability during  the
GC/MS analysis.
58

-------
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
                                  59

-------
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
13Ci2 - 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-l,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-l,2,3,6,7,8-HxCDF
13C12-1, 2 ,3,6,7, 8-HxCDF
13C12-1, 2 , 3 , 6 , 7 , 8-HxCDF
"C12 - 1 , 2 , 3 , 6 , 7 , 8 - HxCDF
13C12-l,2,3,6,7,8-HxCDF

1,2,3,4,6,7,8-HpCDF
"C12-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
"C12-l,2,3,4,6,7,8-HpCDF
                          61

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 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-l,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
13C12-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-l,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-l,2,3,6,7,8-HxCDD
13C12-l,2,3,6,7,8-HxCDF
13C12-l,2,3,4,6,7,8-HpCDF

-------
TABLE 23-10.  MINIMUM REQUIREMENTS FOR INITIAL AND DAILY CALIBRATION
                                  RESPONSE FACTORS
COMPOUND

RELATIVE RESPONSE FACTORS
INITIAL
CALIBRATION
(RSD)
DAILY
CALIBRATION
(% DIFFERENCE)
UNLABELED ANALYTES
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
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
25
25
25
25
25
25
25
25
25
25
25
25
25
25
30
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- 1 ,2,3,4,7,8, 9 -HpCDF
25




25




                                   63

-------
J\ Thermocouple

 U   Probe
              Filter Holder
                       Thermocouple Tlwrmocoapte

                                       f    Ch«ckV«lv«

                                           X
                                                                                     H
                                                                                     s
                                XAO-2Trap
                                                  Silica Qal
                                                 (300 grama)
  Manometer     ^
                                100ml HPLC W.,.,
           Implngar

Thermocouplee

      OHflca
                               By»Paaa
                                 Yalta
                                      MabiValva
                                                                  Vacuum Una
                               Air-Tight
                                Pump
        Figure 5-1. CDD/CDF Sampling Train Configuration

-------
                                 Condenser
Sorbent Trap
                                                  Flue GM Flow
                                                                    H-

                                                                   •§
                                                                    l-{
                                                                    tt>

                                                                    to
en

ui
         •20/16
                                   37cm-
                                  8 mm Glass Cooling Coll
 •To Suit-
                                                                       iiijj  jjj i liiiiijp
                                                                        I  HlXil    **•• ' ***!
                                                                                                   »
                                                                                                   /
                                                                                                 y
            \
                                                         7
                                                        •20/15
                      Water Jacket    Cooling Coll
Glass Wool Plug  Water Jacket   XAD - 2

                          (76 Grams)
         OleM Sintered Disk
                   FIGURE 2. CONDENSER AND SORBENT TRAP FOR COLLECTION OF GASEOUS PCDDs AND

                   PCDFe

-------
       Appendix G.5




Sampling & Analysis Methods




     EPA Method 25A

-------
               EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                               NSPS 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                           EMTIC TM-25A
Technical Support Division, OAQPS, EPA                           June  23,  1993

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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 (FIA) capable
of meeting or exceeding the  specifications in  this method.

3.2   Sample  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-stack 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 Gases.

      Gases used for calibrations,  fuel,   and  combustion air  (if  required) are

-------
EMTIC TM-25A                EMTIC 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 H2/60 percent  1% 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 Gas.  High purity air with less than 0.1 parts per  million by volume
 (ppmv)  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 Gas.  An organic calibration gas with a concentration
equivalent to  25 to 35 percent of the applicable span value.

4.4   Mid-level Calibration Gas.  An organic calibration gas with a concentration
equivalent to  45 to 55 percent of the applicable span value.

4.5   High-level  Calibration  Gas.    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.

-------
EMTIC 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 (>l.O 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 Time 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 test 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 the average organic concentration in terms of pprav 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 pprav as carbon, adjust measured concentrations
using Equation 25A-1.

                     Cc=KCmea9                                     Eq. 25A-1


  Where:
      Cc    *     Organic concentration as carbon, ppnrv.

      C,..,-       Organic concentration as measured, ppnrv.

      K     »     Carbon equivalent  correction  factor.

      K     «     2  for ethane.

      K     -     3  for propane.

      K     »     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 Gases
            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.  EMB  Report  No. 75-GAS-6.
            August  1975.

-------
EMTIC TM-25A
EMTIC NSPS TEST METHOD
Page 6
         Prob»
                                                                       Organic
                                                                      Analyzer
                                                                        and
                                                                      Racordwr
                           CaUbration
                             V«lv»
                                                     Pump
           Slack
    Figure  25A-1.   Organic Concentration Measurement System.

-------
       Appendix G.6




Sampling & Analysis Methods




 EPA Proposed Method 322

-------
(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 HCl 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., HCl in N2) .
     4.1.2  Analyte Spiking Checks.  For analyte spiking checks,
HCl 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 HCl 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 HCl 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 HCl 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, Hastalloy*", 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.   (Hats.:  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
specificati6ns 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  exceeds  ±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:  (1) 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:   (I) 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 HCl 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 HCl 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  HCl  concentration.
      9.3.2  Spike Procedure.  Introduce  the  HCl  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  HCl
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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(nij + nif )
gas
(Cavg - b
mc
2



Kb. -

-bf)

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.

                                                          (Eq.  1)

                                           where:
                                               bc    =  Y-
                                                     intercept of
                                                     the
                                                     calibration
                                                     least-
                                                     squares
                                                     line.
     bf   =   Y-intercept of the  final bias check 2-point    line.
     bt   =   Y-intercept of the  initial bias check 2-point
              line.
     Cgas  =   Effluent gas concentration, as measured, ppm.
     Cavg  =   Average gas concentration indicated by  gas
          analyzer, as measured, ppm.
     mc   =   Slope  of the calibration least-squares  line.
     mf   =   Slope  of the final bias check 2-point line.
     nti   .   Slope  of the initial bias check 2-point line.

The  following equations are used to  determine  the percent
recovery  (%R)  for  analyte spiking:
                  %R =  (SM/CB)  x  100                    (Eq. 2)
where:
      SM =  Mean concentration of duplicate analyte spiked
           samples  (observed).
      CE =  Expected concentration of analyte spiked  samples
            (theoretical).
            CE = CS(QS/QT)  + Sad-Qs/Qr)                 (Eq. 3)
where:
      Cs =  Concentration of HC1  spike gas  (cylinder  tag
           value).
      Qs =  Spike gas flow rate.

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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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     APPENDIX H
PROJECT PARTICIPANTS

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1. REPORT NO.
EPA-454/R-00-010
TECHNICAL REPORT DATA
Please read instructions on the reverse before completing
2.
4. TITLE AND SUBTITLE
Final Report
Manual Testing and Continuous Emissions Monitoring
Vertical Lime Kiln Baghouse Inlet and Outlet
Chemical Lime Company
Marble Falls, Texas
7. AUTHOR(S)
Franklin Meadows
Emil W. Stewart
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 2771 1
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 (BSD) 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 a
vertical lime kiln at the Chemical Lime Company's facility located in Marble Falls, Texas. 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 outlet. Inlet and outlet runs were conducted simultaneously. Oxygen (O2) 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. COASTI Field/Group

21. NO. OF PAGES
v 528 - --.'..-''
22. PRICE
EPA Form 2220-1 (Rev. 4-77)  PREVIOUS EDITION IS OBSOLETE
F:\U\FMeadows\TRD.Frm\WP 6.1

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                          PROJECT PARTICIPANTS
Affiliation
Name
Responsibility
USEPA
Joe Wood, ESD
                             Michael L. Toney, EMC
Environmental Engineer

Work Assignment Manager
Pacific Environmental Services,
Inc.
Franklin Meadows

Michael D. Maret

Dennis P  Holzschuh

Dennis D. Holzschuh

Gary Gay

Paul Siegel

Troy Abernathy
Project Manager

Task Manager
                                                     QA Coordinator
                                                     Site Leader/Console Operator

                                                     Site Leader/Console Operator

                                                     Sampling Technician

                                                     Sample Recovery
Atlantic Technical Services
(PES Subcontractor)
Emil Stewart
                             Alan F. Lowe
                             Marshall M. Cannon
Sampling Technician/Data
Reduction

Technical Support

Technical Support
APCC, Ltd.
(PES Subcontractor)
John Powell

Eric Dithrich

Peter Day
President
                                                     CEM Team Leader
                                                     CEM Sampling Technician
Research Triangle Institute
(EPA/ESD Contractor)
Cybele M. Brockmann
Process Coordinator

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