-sJ

^ ^

-

S ^

^ s

01

70

90

^C^A /<=tUNITED STATES ENVIRONMENTAL PROTECTION AGENCY

REGION VI^"^W^^f "»».«Mr» TI

*'-. «<,,«'•' HOUSTON •RANCH•«0a HORNWOOO DRIVEHOUSTON. TEXAS 77074

Ref. Case So. 6ft<> -3 33' t^ P

Site Name /^C//?<1 ^

Date: / ^ - / y ' ^ ^0

Subject: CLF Data Review F—y€^Fron: lucKael L. Daggett, Chief, Organic Lab Section, 6E-HL Q

To: Hank Thompson, 6E-SH

A review of the laboratory raw data for the reference site has beencompleted by aeabers of the Laboratory Section. Samples were:

INORGANIC;

ORGANIC; ^^V/ /' JJ / ^ J J

The data was found:

( ) Acceptable

(y) Provisional; use of data requires caution. Problems are noted In Review Sui

( ) Unacceptable; data should not be used. Problems are noted In Review Summar

Questions regarding the review can be addressed co me.

Attachments

cc: David Stockton, 6E-HLDuane Geuder, WH-548A

recycled paper ••"''•W l-1 <••"'"••"•""••"

ORGANIC QA CHECKLIST

Site VERTAC____________ Contract No. SAS#- 3354F

Case (to. SAS#- 3354F______ Contractor Chemwest Anal Labs

Reviewed By Melvin Ritter Matrix Duck Tissue (Dioxins)

Date 12/11/87 Acgt. f 8TFAJN57 3? TFAU04 (M0-'0

Sample No. Batch 01 of duck samples; SAS 3354F-01-A1 through r—

3354F-20-B2 0

OVERALL COMMENTS (-TO Be Completed By EPA PERSONNEL) •7\i,sJ 01 C

fii^^/f^WA B/H A Fest Other /

1. Holding Tines _____ ____ _____ ____ r\

2. Tuning/Performance _____ ____ ^___ _ _ _ _ A

3. Calibrations _____ ____ ____ ____ A

4. Blanks _____ _____ _____ • fif

5. Surrogates ' ____ ____ ____ /V

6. Matrix Spike/Dup _____ ____ ____ ____ ft,

7. Compound Identity _____ ____ _____ ____ P\

8. Case Assessment _____ ____ ____ ____ /~T

COMMENTS OR CLARIFICATIONS (See Attached)

A - Acceptable - All items delivered? all criteria met.__________________

P - Provisional - Data usable; some non-essential review items missing or criteria

were not met._____________________________________________

U - Unacceptable - Data unusable; essential review items missing or criteria not met.

recycled paper ••c•>l°8'' "1<1 «•-""•"""•"

^COMMENTS/CLARIFICATIONSREGION VI CLP QA REVIEW

CASE SAS# 3354F SITE VERTAC____________ ^g Chemwest

The following is a summary of sample qualifiers used by Region VI inreporting this CLP Case data:

No. Acceptable Provisional UnacceptableVOA _________ ________ __________ ftBNA _________ ________ ___________ ^PEST _________ ________ ___________ °OTHER pjWfH 2.0 Q ____Q._____ T-

0COMMENTS:Data package for Batch 01 of duck tissue dioxins is acceptable. Thisbatch comprises 20 samples of the total of nearly 80 samples analyzedfor total tetra-octa chlorodibenzodioxins/furans. Resubmissions havebeen requested from the lab for several deliverables such as Forms I & IV,but these resubmittals are only to make the data presentation consistentand do not affect the case results. The narrative presented by thelab relate some of the changes and/or modifications to the technicalaspects of the work based on the fact that the samples were tissueand no specific guidelines or protocols were available. Also notethat the narrative contains a typo error in that page 005, thirdparagraph from the bottom, relates the samples that were re-extracted;one sample mentioned was -07-A3 (Y0015) but this should be -06-A2.Evaluation:

1. Holding Times-Acceptable. Duck samples collected and shipped to lab.2. Tunine/Performance-Acceptable. No special problems noted by lab that

would effect performance. Lab did note that some samples were redoneafter a contaminated blank. Analytical sequence and mass assignmentwas without problems.______________________________________

3. Calibrations-Acceptable. Initial and continuing calibrations met requiremenWindow mix and mass monitors were done to check for overlap of isomers.Initial five-point cal ibration had less than 157.RSD and all continuingcal. checks had +/- 30% QC criteria fulfilled._________________

4. Blanks-Acceptable. Due to acontaninated blank early in the runs,___re-analysis was required. No problems with the data were found dueto blanks.

recycled paper ecology and enrironmeni

ORGANIC CLP/QA REVIEWCONTINUATION PAGE

CASE NO. SAS# 3354F________ SITE VERTAC

COMMENTS:

5. Surrogates-Acceptable. Surrogate recoveries for 37CL-TCDD were goodand within the QC desired limit of 60-140%. but the recoveries for ^the two hepta surrogates, UC-HpCDD and 13C-HpCDF. generally were____Q_high due to the low recovery of the internal standard.13C-OCDD. from ^~———————KTEKB————————————————————————————————'————————^•—'——;:—which they^calculated. Because these samples were tissue and no precedentwas available for internal standard or surrogate recoveries from______tissue, the lab was directed to proceed with the analysis and that_____no reanalysis would be required due Co out of limit 13C-OCDD recovery.As explained in the narrative, the 13C-OCPD Identification and quantitatiormet all resonable criteria. Recoveries for 13C-TCDD and 13C-TCDF______internal standards, as measured against the recovery standard 13C-1,2,34-TCDD, met all Method 8280 criteria._______________________________

6. Matrix Spike/Duplicate-Acceptable. Sample F-12-A4 was used for spiking;here some confusion or inconsistency in the presentation of the resultsis seen in Form I and Form IV. The lab has been requested to resub_____these forms. The results for the sample F-12-A4 were presented as______ppb found or as calculated quantitation (MFC) limit; the results_______for the MS/MSD sample analysis were given as total nanograms of spikerecovered with corrections for amounts in sample (Form I ) and withoutcorrections for 2,3,7,8-TCDD/TCDF amounts (Form IV) . The recovery______percentage and relative per cent (RPD) differences between spike_______and duplicate met all criteria, except the recovery for 2,3,7,8-TCDD.Because of the amount found in the sample and the low amount of________spike specified, the recovery appears to be more variable than desired.The spike level should have been higher than that specified by the SAS.

7. Compound Identity/Results- Acceptable. Eight samples had positive______hits or to possibly contain native 2 ,3 ,7 ,8-TCDD in amounts of < 1 ppb.These were rerun as per IFB for specific 2 ,3 ,7 ,8-TCPD analysis (all____data acceptable) and five samples were confirmed; F-06-A2 ( 0.20 ppb)and F-12-A4 ( 0 . 2 5 ppb) had the highest 2 ,3 ,7 ,8-TCDD. The remaining____samples. F-03-A1. F-16-B1, and F-19-B2 all had 0.05 ppb or less 2,3 ,7 ,8-TCE

8. Case Assessment- Acceptable for Batch 01 data package for dioxins._____Minor resubmissions requested to clear up data presentation.

recyclod paper ecology and environmeru

••ANALYTICAL LABORATORIES, INC.

Date Reported:ChemWest Id's:Date Received;Case/SAS No:

11/28/87Y0010 thru Y008710/10/873354F

Mr. Richard ThackerHWI/Sample Management Office209 Madison Street, Suite 200Alexandria, VA 22314

inG-1.01~-

Dear Mr. Thacker: 0The technical staff at CHEMWEST is pleased to provide thefollowing summaries and documentation for SAS 3354F receivedOctober 10, 1967. The low concentration wood duck tissue sampleswere analyzed for 2,3,7,8-TCDD, and total tetra thru octa dioxinsand furans using EPA Method 8280. The cross correlation of ID'Sis shown below:

ChenWest ID EPA ID

Y0010Y0011Y0012Y0013Y0014Y0015Y0016Y0017Y0018Y0019YCC20Y0021Y0022Y0023Y0024Y0025Y0026Y0027Y0028Y0029Y0030Y0031Y0032Y0033Y0034Y0035Y0036Y0037

600W North Morket Boulevord • Socramento, CA 95834 •

A Subsidiary of CompuChem Corporation ^ li 1recycled paper

3354F-01-A13354F-02-A13354F-03-A13354F-04-A23354F-05-A23354F-06-A23354F-07-A33354F-08-A33354F-09-A33354F-10-A43354F-11-A43354F-12-A43354F-13-A53354F-14-A53354F-15-A53354F-16-B13354F-17-B13354F-13-B13354F-19-323354F-20-B23354F-21-S23354F-22-B33354F-23-B33354F-24-B33354F-25-C13354F-26-C13354P-27-C13354F-28-C2

Phone (916) 923-0840 • FAX (916) 923-1938

ecology and environment

Sample Management Office11/28/87Page 2

ChemWest IDY0038Y0039Y0040Y0041Y0042Y0043Y0044Y0045Y0046Y0047Y0048Y0049Y0050Y0051Y0052Y0053Y0054Y0055Y0056Y0057Y0058Y0059Y0060Y0061Y0062Y0063Y0064Y0065Y0066Y0067Y0068Y0069Y0070Y0071Y0072Y0073Y0074Y0075Y0076Y0077Y0078

EPA ID3354F-29-C23354F-30-C23354F-31-C33354F-32-C33354F-33-C33354F-34-C43354F-35-C43354F-36-C43354F-37-C53354F-38-C53354F-39-C53354F-40-C63354F-41-C63354F-42-C63354F-43-D13354F-44-D13354F-45-DI3354F-46-E13354F-47-E13354F-48-E13354F-49-E23354F-50-E23354F-51-E23354F-52-E33354F-53-E33354F-54-E33354F-55-E43354F-56-E43354F-57-E43354F-58-E53354F-59-E53354F-60-E53354F-61-F13354F-62-F13354F-63-F13354F-64-F23354F-65-F23354F-66-F23354F-67-F33354F-68-P33354F-69-F3

recycled paperCHEMWEST ANALYTICAL LABORATORIES, INC. ecology and environment

Sample Management Office11/28/87Page 3

Y0079Y0080Y0081Y0082Y0083Y0084Y0085Y0086Y0087

3354F-70-F43354F-71-F43354F-72-F43354F-73-F53354F-74-F53354F-75-F53354F-76-ABCD3354F-77-E3354F-78-F

r'-o--o[—

0

During the course of the analysis of the samples for this SASChemWest had three telephone conversations with Mel Ritter ofRegion 6 . Several issues were discussed and for the purposes ofdocumentation they are addressed below.During the first conversation instrumental calibration procedureand acceptance criteria for tetra thru octa dioxin and furananalysis were mutually agreed upon. These are:

1. Run Brehm mix (window defining mixture ofisomers) once during the case.2. Run a 5 point calibration curve not a 15 pointcurve.3. 15% RSD for the initial calibration isacceptable.4. A continuing calibration must be run at the

end of each 12 hour period. The measuredrelative response factors of the analytes,surrogates and internal standards must bewithin +/- 30% of the mean values establishedduring initial calibration. If the endingstandard fails any criteria the positivesamples must be re-injected.5. A set of 4 groups of ions are used to monitorany overlapping elution between tetra andpenta, penta and hexa, hexa and hepta, andhepta and octa isomers.

In the second conversation GPC, disk deliverables, form formatsfor the pesticides, and a problem with one of the spikingcompounds for the dioxins were discussed.

recycled paperCHEMWEST ANALYTICAL LABORATORIES, INC.

ecology and environment

Sample Management Office11/28/87Page 4

1. ChemWest is using a nonautomated GPC systemwhich elutes from top to bottom but yieldscomparable results to the automated systemdescribed in the IFB-J001. As long as theIFB criteria for the calibration are met thissystem is acceptable.

CO0''

2. Chemwest has CompuChem's software for the HP- o1000 which automatically generates most of the i—required forms for the pesticide deliverables. _.However, these forms are slightly different in —format than those in the IFB-J001. Since MelHitter was familiar with CompuChem's forms, itwas agreed that these would be acceptable.3. When the matrix spike and matrix spikeduplicate for one set of samples was examinedit was discovered that all target analyteswere acceptably recovered and met RPD criteriaaccept the TCDD's. Because the originalsample was positive approximately 6 ppb andthe sample was spiked with only 1 ppb the RPDcriteria for the tetra spike recovery (aftersubtraction) was not met. However if onecompared the total amount of TCDD in thespike and spike duplicate the RPD criteria wasmet. This approach was agreed to bereasonable and re-extractions for thesesamples are not required.

The third conversation dealt with a problem encountered withseveral of the dioxin and furan samples. The absolute recoveryfor the 13C-OCDD internal standard was less than 40% in severalsamples while all other internal and surrogate recoveries were inexcess of 70%. This OCDD recovery was outside the criteriastated in Method 8280 - May 1986 (40 - 120%) for soil samples.These samples however were duck samples and a hard and fastcriteria has never been set. The 'SC-OCDD peaks in these caseswere well shaped, met chlorine cluster ratio criteria and hadsignal to noise ratios of greater than 10 to 1. But since thetwo hepta surrogates were quantitated using the HC-OCDD whichwere not recovered well and the two surrogates themselves wererecovered well (greater than 70%) the calculated surrogatespercent accuracies were skewed on the high side, i . e . greaterthan 140% (acceptable range 60-140%). Since all criteria for anacceptable sample were not met technically a re-extraction wasrequired. Mel Ritter, however, felt that if the samples wereflagged and the above explanation was given the re-extraction was

0&4recycled paper CHEMWEST ANALYTICAL LABORATORIES, INC. ecology and en

Sample Management Office11/28/87Page 5

not necessary.It was agreed that all of these items would be included in thecover letter accompanying the case. 0-

cr-This report applies to samples 3354F-01-A1 through 3354F-20-B2<r>ChemWest ID'S (Y0010 thru Y0029). ^Sample 3354F-12-A4, (Y0021) was analyzed as a sample, matrix"spike and matrix spike duplicate. 0The matrix spike sample and matrix spike duplicate were spikedwith one native 2 , 3 , 7 , 8 isomer representing each dioxin and furancongener group. Recoveries of Internal Standard and nativecompounds all fell within acceptable ranges, 40-120% for InternalStandard absolute recoveries, 60-140% for native 2,3.7,8-TCDD and2,3,7,8-TCDF, and 40-160% for all other native spike compounds,except the native 2,3,7,8-TCDD. As explained above the spikinglevel was too low for the amount of native found in the originalsample so the RPD was calculated on the total 2,3,7,8-TCDD foundin the MS and MSD.Eight of the samples were found to possibly contain native2,3,7,8-TCDD in the CL4-CL8 analysis. These samples wereanalyzed according to Dioxin IFB WA86-K357 and five wereconfirmed. Three others 3354F-10-A4 (Y0019). -15-A5 (Y0024) and-18-B1 (Y0027) could not be confirmed and are reported with MFCvalues. (Please see 2,3,7,8-TCDD Form-Bl)Several of the samples required re-extraction: Samples 3354F-01-A1 (Y0010), -02-A1 (Y0011), -03-A1 (Y0012), -04-A2 (Y0013), -05-A2 (Y0014), and -07-A3 (Y0015) were re-extracted because theywere associated with a contaminated method blank. Samples 3354F-08-A3 (Y0017). -09-A3 (Y0018), -10-A4 (Y0019), -11-A4 (Y0020),-16-B1 (Y0025), and -17-B1 (Y0026) were re-extracted due to lowinternal standard recoveries. The data from the first extractanalysis is provided in the rejected data section.Other than the aforementioned method blank, all others associatedwith this data package were free of contamination.Several of the samples had low is-OCDD recovery which skewed thetwo hepta surrogate percent accuracies to the high side. Pleasesee above comments. Hone of these samples were re-extracted per

5 Mel Ritter of Region 6 .

005

recycled paper CHEMWEST ANALYTICAL LABORATORIES. INC. |,gy , envlronm.-ni

Sample Management Office11/28/87Page 6

Routine calibration consisted of running a 0.15 sensitivitystandard and a shift standard where the measured RRF's for allanalytes were within +/- 30% of the mean values establishedduring initial calibration.In addition to the analysis of the GC window defining mixture a?the beginning of the project the ions in the descriptors were-combined such that any region of congener overlap (i.er?-tetradioxin/pentafuran) was simultaneously monitored for both-congener groups.Before any samples were analyzed, standards were run at fivedifferent concentrations (200, 500. 1000, 2000, 5000 pg/ul) andmean response factors were obtained. A relative standarddeviation of less than 15% was obtained. All sample calculationsare based on an average multipoint response factor. Thefollowing table provides a reference for compounds and theirappropriate Internal Standard.

INTERNALSTANDARD

"C-2,3,7,8-TCDD

SURROGATE

13C-2,3.^,B-TCDF

13C-OCDD

COMPOUND/SURROGATE

ALL NATIVE TETRADIOXIN ISOMERSALL NATIVE PENTADIOXIN ISOMERSALL NATIVE HEXADIOXIN ISOMERS

^Cl-^TS-TCDD

ALL NATIVE TETRAFURAN ISOMERSALL NATIVE PENTAFURAN ISOMERSALL NATIVE HEXATURAN ISOMERSALL NATIVE HEPTADIOXIN/FURAN ISOMERSALL NATIVE OCTADIOXIN/FURAN ISOMERS^C-HpCDD and ^C-HpCDF SURROGATES

Interferences were noted from the "C-2,3,7,8-TCDF in thetetradioxin regions of the chromatograms as the 13C carbonlabeled material contains the same ion present in the nativedioxin. These interferences were noted on all chromatograms andwere not counted as true interferences for use in detection limitcalculations.Extraction procedures were those outlined in the EPA 8280 soilmethod and the methods provided with the SAS.

CHEMWEST ANALYTICAL LABORATORIES. INC.recycled paper ecology and environmeni

OGG

SECTION 2

FORM-(n) SUMMARY REPORTS

Page

FORM 1 - OUANTITATION REPORT DATE: 11/20/87

LABORATORY: CHEWIEST

CASE: SAS 3354F

CLIENTID. CW

Method Blank YOOIOMERXDetection Limit

SAS3354F-01-A1 Y0010RXDetection Limit

SAS3354F-02-A1 YOOHRXDetection Limit

SAS3354F-03-A1 Y0012RXDetection Limit

SAS3354F-04-A2 Y0013RXDetection Limit

SAS3354F-05-A2 Y0014RXDetection Limit

SAS3354F-06-A2 Y0015RXDetection Limit

Method Blank Y0016MBRIDetection Limit

6: Maximum possible concentration.

00CO

DATE

11/19 /87

11/20/87

11/20/87

11/20/87

11/20/87

11/20/87

11/20/87

11/16/87

TIME

15:10

10 :17

10:52

1 1 : 2 9

13:22

13:57

14:32

14:58

INST.10.

CN-1

CH-1

CW-1

CK-1

CB-1

CH-1

CW-1

CW-1

2,3,7,8TCOO

N00.0057

ND0.0090

N00.061

« N00.060

ND0.025

ND0.027

(0.27

ND0.0050

TCDD

ND0.0056

N00.0069

ND0.040

* N00.032

N00.0098

N00.025

0.34

N00.0068

PeCDO

N00.0070

ND0.0072

ND0.046

N00.0075

ND0.012

N00.032

' , N0-ti',006)

N00.0059

H>CDO

N00.0074

ND0.0059

ND0.053

ND0.0064

N00.0)1

ND0.027

ND0.0062

N00.0053

TOTAL AI

HpCDO

ND0.0088

NO0.018

ND0.15

NO0.018

NO0.025

ND0 . 1 1

ND0.0059

NO0.0091

NALYTE 01

OCOO

« NO0.010

NO0.017

« ND0.42

« ND0.037

NO0.025

« ND0.091

NO0.0069

ND0.010

JANTITr F2,3,7,8,

TCDF

NO0.0042

NO0.0046

NO0.057

^0.033

NO0.0085

NO0.016

(A^

NO0.0053

0

01MD (ppl

TCOF

NO0.0037

NO0.0033

NO0.022

0.066

NO0.0046

NO0.016

0.21

NO0.0047

1 7 1

b)

PeCDF

NO0.0041

NO0.0034

NO0.027

; 1 W0.016

N00.0053

ND0.015

0.79

N00.0041

02

HiCOF

N00.0037

N00.0031

N00.027

ND0.0034

N00.0056

ND0.016

v ND0.0032

ND0.0035

HpCDF

N00.0058

N00.0097

ND0.090

N00.0)3

N00.013

ND0.060

ND0,0042

N00.0062

OCDF

N00.0089

N00.013

N00.15

N00.019

N00.025

N00.081

N00.0057

N00.0081

Page 2SURROGATE AND INTERNAL STANDARD RECOVERIES WTE: 11/20/

LABORATORY: CHEMUST

CASE: SAS 33S1F

CLIENTID. CM* DATE TIME

INST.ID.

<Bof

•C-TCDO

SOLUTE f RHINTERNAL ST<

•C-TCDF

;OVERY(NMRDS

•C-OCDO

AE

«IX;I-TCOO

SOLUTE f RECOVERYof SURROGATE

*)3C-HpCOO *13C-HpCDF

Method Blank YOOIOMERX 11 /19 /87 1 5 : 1 0 CW-1Detection Limit

132 101 98

SASM54F-01-A1 YOOIORX 11/20/B7 1 0 : 1 7 CW-1Detection Limit

91 92 55 130 154 152 c

SASH54F-02-A1 Y0011RX 11/20/87 10:52 CW-1Detection Lliult

93 131 151 1 4 1

SAS3354F-03-A1 Y0012RX 11/20/87 11:29 CW-1Detection L i m i t

132 145 141 c

SAS3354F-04-A2 Y0013RX 11/20/87 13:22 CW-1Detection L i m i t

98 132 163 163 e

SAS3354F-05-A2 Y0014RX 11/20/87 13:57 CW-1Detection Limit

96 97 46 128 164 161 *'

SAS5354F-06-A2 Y0015RX 11/20/B7 14:32 CW-1Detection L i m i t

91 93 50 130 151 146 «'

Method Hank Y0016MBRI 11/16/87 14:58 CW-1Detection L i m i t

93 93 132 107 «'

Carbon 13 labeled 2,3,7,8-tetrachlorodlbenzodloxlnCarbon 13 labeled 2,3,7,8-tetrachlorodlbenzofuranCarbon 13 labeled 1,2,3,4,6,7,8-neptachlorodlbanzodloxlnCarbon 13 labeled 1,2,3,4,6,7,8-heptnchlorodIbenzofurBnCarbon 13 labeled oc+achlorodIbenzodloxin37CI labeled 2,3,7,8-tetrachlorodlbenzodloxln

•C-TCOO:"C-1CDF:»13C-H[]CDO:*13C-*1[CDF:*C-OCOO:•37CI-TCDO:

B High hepta surrogates due to lo» 13C-OCDO Internal standard reco»ery.0 1 7 1 0 3

Page 1

CLIENTID. W

SAS3354F-07-A3 Y0016RIDetection Limit

SAS3354F-08-A3 Y0017RXOet&ctlon Limit

SAS3354F-09-A3 Y0018RXDetection Limit

Method Blank Y00601WIDetection Limit

SAS3354F-10-A4 Y0019RXDetection Limit

SAS3354F-11-A4 Y0020RXDetection Limit

Method Blank Y0021HBDetection Limit

SAS3354F-12-A4 Y0021Detection Limit

1: Maximini possible concanti

» OuantIfated using 556 Ion

0(-*1-'

0 1 7

DATE

11/16 /87

11 /16 /87

11/20/87

11/16/87

11/16/87

11/ZO/B7

11 /10 /87

11 /10 /B7

ration.

due to

TIME

16:09

16:45

15:06

14:22

10:01

1 5 : 4 1

17:04

20:07

nterfer

FORM I -

INST. 2,5,7,8ID. TCDD

CW-1 ND0.0083

CW-1 ND0.097

CW-1 ND0.010

CW-1 ND0.0046

CW-1 ND0.0079

CW-1 ND0.035

CW-1 MD0.0055

/-'"''CW-1 ( 0.32

encas •Ith the 356 Ion.

OUANT11

-TCDD

NO0.0083

NO0.097

ND0.004

NO0.0045

ND0.0064

NO0.056

NO0.0060

0.46

FATION RE

PeCOD

* NO0.0093

* MO0.068

NO0.0060

ND0.0054

ND0.0087

ND0.063

NO0.0072

; NO0.0091

PORT

HtCDO

NO0.0081

NO0.078

ND0.0064

ND0.0043

ND0.0056

NO0.051

NO0.0056

NO0.0070

TOTAL A

HpCDO

ND0.027

ND0.3)

ND0.017

ND0.010

ND0.016

ND0.18

ND0.012

NO0.015

NALYTE W

OCOD

NO0.031

ND0.45

NO0.048

ND0.0078

« NO0.089

ND0.20

ND0.0082

/ 0.081

UANTITY2,3,7,8

TCOF

ND0.0078

ND0.065

NO0.012

ND0.0028

NO0.0041

NO0.024

ND0.0042

0.14

LABOF

FOUND (pp

1CDF

NO0.0064

NO0.059

NO0.0031

NO0.0028

ND0.0041

NO0.030

ND0.0041

0.37

DATE

RATORY:

CASE

b)

PeCDF

NO0.0064

NO0.053

NO0.0029

ND0.0033

NO0.0040

NO0.02A

NO0.0049

0.10

1 0

: 11/20/B

CHEMWES

: SAS 33

HiCDF

ND0.0057

NO0.058

ND0.0036

NO0.0026

NO0.0039

ND0.027

NO0.0039

: ND0.0043

4

7

T

54F

HpCDF

NO0.021

NO0.25

NO0.010

NO0.0057

NO0.0)1

ND0.10

NO0.0062

NO0.011

OCDF

NO0.028

NO0.23

NO0.021

NO0.0063

NO0.017

ND0.14

NO0.0083

NO0.014

Page 2SURROGATE AND INTERNAL STANDARD RECOVERIES D»TE: 11/20/87

LABORATORY; CHEMWEST

CASE: SAS 3354F

CL IENTID. W DATE TIME

INST.ID.

ABof

•C-TCOO

SOLUTE f RE(INTERNAL ST;

•C-TCDF

:0»ERYI WARDS

•C-OCDO

AB

«37CI-TCOO

SOLUTE % RECOVERYof SURROGATE

«13C-HpCOD "13C-HpCDF

SAS3354F-07-A3 Y0016RI 11/16/87 16:09 CW-1Detection Limit

SAS3354F-08-A3 Y0017RX 11/16/87 16:45 CW-1Detection L i m i t

89 32 126 140 147 «'

SAS3554F-09-A3 YOOIflRX 11/20/87 15:06 CW-1Detection Limit

y> 131 135 127

Method Bank Y0060MERI 11/16/87 14:22 CW-1Detection Limit

96 101 89 129 104 112

SAS3354F-10-A4 Y0019RX 11/16/87 10:01 CW-1Detection Limit

101 74 132 123 118

SAS3354F-11-A4 Y0020RX 11/20/B7 15 :41 CW-1Detection Limit

93 49 127 156 162 c

Method Blank Y0021MB 11/10/87 17:04 CW-tDetection Limit

93 90 98 123 102

SAS3354F-12-A4 Y0021 11/10/B7 20:07 CW-1Detection L imi t

87 65 125 125 113

•C-TCDO: Carbon 13 labeled 2,3,7,8-tetrachlorodlbenMdloxln•C-1CDF: Carbon 13 labeled 2,3,7,8-tatrachlorodlbenzoturan"ISC-HpCDO: Carbon 13 labeled 1,2,3,4,6,7,8-heptachlorodlbenzodloxln"13C-HpCOF: Carbon 13 labeled 1,2,3,4,6,7,8-heptachlorodllrnzofuran

^•fC-CCW: Carbon 13 labeled octachlorodlbenzodloxin^.J37CI-1COD: 37CI labeled 2,3,7,8-tetrachlorodlbenzodloxlnM

< Htgh hepta surrogates due to low 15C-OCDO Internal standard recovery.

0 1 7 1 0 5

Page 1

CLIENT10.

^ SAS3354F-12-A471s Detection Limit

,. SAS3354F-12-A4tSF Detection Limit

SAS3354F-13-A5Detection Limit

SAS1354F-14-A5Detection Limit

SAS3354F-15-A5Detection Limit

SAS3354F-16-B1Detection Limit

SAS3354F-17-B1Detection Limit

CM

Y0021MS

Y0021MSD

Y0022

Y0023

Y0024

Y0025RX

Y0026RX

DATE

H/10/87

11/10/87

I1/05/87

11/05/87

11/05/B7

11/20/87

11/20/87

TIME

19:35

20:10

1 1 : 1 1

1 1 : 4 6

1 3 : 1 0

1 6 : 1 6

16:51

INST.10.

CW-1

CW-1

CW-1

CW-1

CW-1

CW-1

cw-i

FORM I -

2,3,7,81CDD

2.30

0.91

N00.0041

N00.0089

« N00.0089

N00.022

N00.046

• QUANTIT

TCDO

2.30

0.91

ND0.0015

ND0.0097

N00.0017

ND0.0092

ND0.040

•AT ION RE

PeCOO

4.08

3.97

NO0.0062

• ND0.016

ND0.0089

NO0.015

NO0.039

PORT

HiCDO

4.22

3.80

NO0.0036

NO0.022

ND0.0045

N00.014

N00.035

TOTAL AI

HpCDO

5.15

5.77

ND0.0089

ND0.058

ND0.010

ND0.032

N00.084

»LYTE 0

OCDO

-W-t6Id-

9.36

/0.036

ND0.069

« ND0.057

N00.042

ND0.098

IIWITY F2,1,7,8,

1C OF

1.542.

1.00

ND'''0.0017

ND0.0075

ND0.0040

ND0.0091

ND0.018

LABO

OUND (pp-TCDF

1.54

1.00

N00.0010

ND0.0060

ND0.0012

ND0.0082

ND0.018

DATE:

RATORY:

CASE:

M

PBCDF

4.17

3.89

NO0.00)4

ND0.0083

ND0.0016

ND0.0075

ND0.022

11/20/8

CHEWES

SAS 33

HxCDF

3.74

3.76

ND0.0023

ND0.012

ND0,0024

NO0.0082

NO0.025

7

T

,54F

H(CDF

4.13

3.98

ND0.0016

NO0.043

ND0.0071

ND0.027

NO0.058

OCDF

9.'!

10.3

(0.028

ND0.053

NDO.OOB7

ND0.0 ')

N00.079

SAS3354F-18-BI Y0027Detection Limit

11/05/87 15:02 CW-1 0.15 ND ND ND0.0049 0.0057 0.0090

• ND ^.065 0.098 0.0320.021 -' -

« ND NO NO0.0032 0.0060 0.0079

t: Maximim possible concentration.

*': Used 358 Ion for quant I tat Ion.

^ I YoCTap AS TOTALAMC^I^T -—— ^V\ (_^

A/G- FCAJLW C^JfZ^L-r^O /-^AS. S^MI^CF0 1 7 1 0 6

(.F-?4/

Page 2SURROGATE AND INTERNAL STANDARD RECOVERIES DATE; 11/20/87

LABORATORY: CHEMWEST

CASE: SAS 3354FABSOLUTE 1, RECOVERY ABSOLUTE f RECOVERY

of INTERNAL STANDARDS of SURROGATECLIENT INST.ID. W DATE TIME ID. *C-TCDO -C-TCDF •C-OCDO *37CI-TCDO *13C-HpGDO ") 3C-HpCDF

SAS3354F-12-A4 Y0021MS 11/10/B7 19:35 CW-1 86 88 62 131 130 127Detection L i m i t

SAS3354F-12-A4 Y0021MSO 11/10/87 20:10 CW-1 88 88 54 127 134 122Detection L imi t

SAS3354F-13-A5 Y0022 11/05/87 11:11 CW-1 86 88 58 127 133 130Detection L i m i t

SAS3354F-14-A5 Y0023 H/05/87 11:46 CW-1 87 88 48 128 134 126Detection L i m i t

SAS3354F-15-A5 Y0024 11/05/87 13:10 CW-1 86 88 56 126 133 134Detection L i m i t

SAS3354F-16-B1 Y0025RX 11/20/B7 16:16 CW-1Detection L i m i t

SAS3354F-17-B1 Y0026RX 11/20/87 16:51 CW-1Detection Limit

SAS3354F-18-BI Y0027 )1/05/87 15:02 CW-1Detection Limit

96

98

90

69

84

126

128

125

142

137

110

143 »

128

106

•C-TCDO:"C-1COF:"13C-HICDO:»)3C-«|COF:•C-OCDO;"37CI-TCDD:

Carbon 13 labeled 2,3,7,8-tetrachlorodlbenzodloxlnCarbon 13 labeled 2,3,7,8-tetrachlorodlbeniofuranCarbon 13 labeled 1,2,3,4,6,7,8-haptachlorodlbenzodloxtnCarbon 13 labeled 1,2,3,4,6,7,8-heptachlorodIbenzofuranCarbon 13 labeled oc+achlorodlbenzodloxin37CI labeled 2,3,7,8-te+rachlorodlbenzodloxln

0 1 7 1 0 7c High hepta surrogates due to low 13C-OCDO Internal standard recovery.

FORM I - OUAMTITATION REPORT MTE: 11/20/87Page I

LABORATORY: CHEMWEST

CASE! SAS 3354F

TOTAL ANALYTE QUANTITY FOUND (ppb)CLIENT INST. 2,3,7,8- 2,3,7,8,-ID. CM DATE TIME 10. TCDO TCOO PeCDO H)CCO HpCDO OCDO TCDF TCDF PsCOF HiCDf HpCDF OCOF

SAS3354F-19-B2 Y0028 H/05/87 19:35 CW-1 /'0.02S 0^28~ • c ND ND NO NO ( 0.014' NO NO NO NO NO "\Detection Limit - — — — — — - — — y^^ o^o65 0.012 0.013 '~-——-'0.0020 0.0027 0.0048 0.011 0.010 /

SAS33S4F-20-B2 Y0029 11/05/87 16:52 CW-1 ND NO 0 ND ND HO f 1C NO NO NO NO NO NDOa+ectlon Limit 0.033 0.019 0.034 0.038 0 .15 0.33 0.024 0.015 0.018 0.032 0.076 0.095

(: Maximum possible concentration.

c: Used 358 Ion For quantltatlon.

0

w 0 1 7 1 0 8

SURROGATE AND INTERNAL STANDARD RECOVERIES DATE; H/ZO/B7Page 2

LABORATORY: CHEMNEST

CASE: SAS 3354FABSOLUTE t RECOVERY ABSOLUTE f RECOVERY

of INTERNAL STANDARDS of SURROGATECL IENT INST.10. CM DATE TIME ID. *C-TCOO *C-TCDf "C-OCDO »3X;1-TCDD •ISC-HlCDD *13C-HpCDF

SAS3354F-19-B2 Y0028 11/05/87 19:35 CW-1 92 90 72 123 119 119 ^Detection L i m i t '

SAS3354F-20-B2 Y0029 11/05/87 16:52 CW-1 85 84 44 125 153 123Detection Limit

•C-TCOO; Carbon 13 labeled 2,3,7,8-tetrachlorodlbenzodlo)(ln•C-TCOF: Carbon (3 labeled 2,3,7,8-tetrachlorodlbanzoturan"13C-HpCCO: Carbon 13 labeled 1,2,3,4,6, 7,8-hep+achlorodlbenzod loxin•HC-HpGOF; Carbon 1 3 labeled 1,2,3,4,6,7,8-heptachlorodlbenzofuran•C-OCOO: Carbon 13 labeled octachlorodlbenzodloxin"37CI-1CDO: 37CI labaled 2,3,7,8-tetrachlorodlbenzodloxln 0 1 7 1 0 9

FORM 2 - MULTIPOINT CALIBRATION SUMMARY

TARGET COMPOUND INTERNAL STANDARD

INST. DATE

CN-1 11-04-87CK-1 11-04-87CW-1 11-04-87CK-1 11-04-87CW-1 11-04-87

MEAN RESPONSE FACTORS 0.80 0.63 0.42STANDARD DEVIATIONRSO

SO10

«C-TCDO«C-TCOF"C-HpCOO*C-H|)CDF"C-CCOO

SO 200SO 500SO 1000SD 2000

-^SO 5000

(-*•4

TIME

15:4815!l016:26)7!041 7 s 4 1

2,3,7,8-TCOO, 2,l,7.a-TCDF1,2,3,7,8-PaCDD, 1,2,3,7,8-PtCDF1,2,1

1,2,3,4,5,6,7,8-OCOD, 1,2.3,4.5,6,

RESTD. —————————————ID. TCOO PeCOO HMCDD

-/

200 0.79 0.60 0.41500 0.77 0.64 0.411000 0.83 • 0.65- 0.44 /2000 0.82-'' 0.65^ 0.45 i5000 0.79/ 0.62 •/ 0.41^

0.02 0.02 0.025 . 1 - 3.4' 4.6

STANWROS

*11C12-2,3,7,8-TCOO*l.iC12-2,3,7,8-TCDF

*13C12-t,2,3,4,6,7,8-H|)CDF•13C12-1,2.3,4,5,6,7,8-CCOO

SHIFT STANDARD COMPOUNDS *

4,7,B-HlCOD, 1,2,3,4,7,8-HlC

SPONSE FACTORS ' RESPONSE FACTORS

HpCOO

1.04't f1 . 1 1 -l.oa J1.07^

/ .a?+.88-0.032.5

DF-HllCDF7,8-OCOF

OCOO

/1 . 1 4^1.02 /1.04 •t1.0V

^0.054.9

TCDF PeCDF HiCW

•/ • i/0.91 0.75 0,530.92 0.75 0.561.00 0.80 0.580.99 -' 0.78 •J 0.590.96 0.75 / 0.55

0,96 0.77 0.560.04 0.02 0.024.2 3.0 4.2

CONCENTRATION

500500

1000

200500

100020005000

HpCOF OCDF •C-TCDD •C-TCDF «C-HpCDD •C-HpCOD •C-OCDO

L/'

l.Tp- 0.95^ ^-1.90 1 . 1 2

-' 1.79 ' 1.08''•' 1.80- 1 . 1 0 •

i-fl /.c.6-I.IJ" wr0.17 0.07 0.02 0.02 0.02 0.02 0.019.6 6.4

(pg/ul)

^.39.41.41.42 /

.44 y

.42 1.88 0.99 1.45 0.38

1.4

0 1

• \/ y ^.87 0.99 1.43 0.37.87 0.99 1.46 0.38.91 1.00 1.45 0.38.87-^ 0.961' 1.44 "' 0.40-'.90>-' 1.00^ 1.47^ 0.38.

1.0 1 .7 1 . 1 2.9

7 1 1 0

FORM 2 - MULTIPOINT CALIBRATION SUMMARY

TARGET COMPOUNDRESPONSE FACTORS

INTKWL STANDARDRESPONSE FACTOHS

INST. DATESTD. -——

TINE 10. TCOO PtCOO HiCDO HpCOO OCOD TCOF P»CDF HiCOF HpCDF OCDF •C-1COO •C-TCOF "C-HiCDO "C-HpCDIt "C-CCOO

Ctl-1 11-06-67 11:31 200 0.77^ 0.77-" 0.62^CW-1 11-06-87 10:54 MO Q.79-^ 0.80-' O.M^CN-1 11-06-87)2:1) 1000 0.80- 0.79'• 0.64-'•CW-1 H-06-87 13:15 2000 0.74 0.77 0.65 ICW-1 H-06-87 14:19 5000 0.76 0.76 0.58 1

1.05' 1.06' 0.89 / 0.97 ^0.83 ^ l1.08-- 0,99''0.95^ 0.9)-' 0.85 ^ 11.)! '' ).OZ-'" 1.00 -/ 0.98''' 0.94 - 11.11 1.02 0.92 0.90 0.89 11.08 1.02 0.87 0.90 0.80 1

1.91 v 1.15 I1.76 ^ 1.05 -/ 11.90- 1.10 i.- '1.85 1.07 11.81 1.10 1

1.48 11.391-- 11.42 /• 11.52 11.31' 1

1.79 ^ 1.00 -/ 11.72 ^ 1.03 ^ 11.67 / 1.0» - 1I.B4 1.05 - 11.62 1.05 " 1

1.57 ^ O.S8 y.51 •' 0.54 ^

1.54 - 0.54^1.56- 0.611.52 -/ 0.47

NEAN RESPONSE FACTORSSTANOARO DEVIATIONRSO

"C-TCDO•C-ICDF*C-H|]COO*C-H(CDF•C-OCDO

SO 200SO 500SO 1000SO 2000SO 5000

'ACTORS 0.77 0.78 0.62riON 0.02 0.02 0.03

1.J, 2. 4.^

STANDARDS

»11C12-2,I,7,B-TCOO•13C12-2.3,7,8-1CDF•I 3012-1,2,3,4,6,7,8-HiiCDD"13C12-l,2,3,4,6,7,8-HpCOF"13C12-1.2,3,4,5,6.7,8-OCOO

SHIFT STANDARD COMPOUNDS •

2,3,7,8-TCOO, 2,3,7,8-ICOF1,2,1,7,8-PaCOD, 1,2,1,7,8-RBCDF1,2,3,4,7,8-HlCDD, 1,2,3,4,7,8-H)<;OF1,2,3,4,6,7,8-HpCOO, 1,2,3,4,6,7,8-HpCOF1,2,3,4,5,6,7,8-OSOO, 1,2,1,4,5,6,7,8-OCOF

1.090.01

^

1.020.02

^

0.910.05

^

0.910.04

^

CONCENTW

0.86 1.850.05 0.066.1 3.4/ >/

iTION (pg/ul)

500500

1000

200500

100020005000

1.090.04

y

1.420.08

5.7

0 1 7

i1.730.095.1>/

1 1 1

1.030.02

2.Q/

1.540.02

1.1

0.550.05

9.6

FORM 5 - CONTINUING CALIBRATION SUMMARY

TCDD PBCOO H)CCO HpCOO OCOO 1CDF PtCOF HiCOF HpCOF OCOF "C-TCOO <C-TCOF «C-HpCDO «C-HpCOF "C-OGOO

0.80 0.63 0.42 1.06 1.07 0.96 0.77 0.56 1.75 1.07 1.42 1.88 0.99 1,45 0.58

STDDATE TIME ID. TCDO PeCOO HxCDO HpCDO OCDO TCDF PaCOF HMBDF HpCDF OCDF •C-TCDO "C-TCDF "C-HpCDO "C-HpCOF "C-CCDD

11-05-87 09:48 SO 500 RF 0.78 0.67 0.45 1,14 1.04 0.94 0.82 0.60 1.86 1.05 1.58 1.77 1.04 1.54 0.58RFO 2.5 6.2 2.4 5.4 2.8 2.1 6.5 6.9 7.2 1.9 2.9 6.0 4.9 6.0 0.0

S7DDATE TIME ID. TCDO PaCDO HiCDO HpCDO OCOO TCOF PaCOF HiCOF HpCDF OCOF «C-TCDD «C-TCOF «C-HpCOO "C-HpCOF •C-OCOO

11-05-87 16:16 SD 500 RF 0.77 0.65 0.45 1.08 1.04 0.95 0.79 0.60 1.74 1.05 1.42 1.86 1.00 1.47 0.59RPO 5.8 5.1 2.4 0.0 2.8 5.2 2.6 6.9 0.6 5.8 0.0 1.1 1.0 1.4 2.6

STDDATE TIME 10. TCDO PaCDO HXCDO HpCOO OCDO TCOF PeCOF HiCDF HpCDF OCOF •C-TCOO "C-TCOF "C-HpCDO «C-HpCOF "C-OCDD

»lSo5-fi? 00:10 SO 500 RF 0.77 0.70 0.49 1.06 1.10 0.95 0.85 0.69 1.68 1.06 1.57 1.74 0.96 1.45 0.48Y__—-^ RFO 5.8 10.5 15.4 1.9 2.8 5.2 9.9 20.8 2."» 0.9 5.6 7.7 5.1 1.4 25.5

0t-1CD 0 1 7 1 1 2

FORM 3 - CONTINUING CALIBRATION SUMMARY

TCDO PeCDO H)CDD HpCOD OCDO TCOF PeCDF H)CDF HpCDF OCDF •C-TCDO "C-TCOF *C-HpCDO •C-HpCOF *C-OCDO

0.77 0.78 0.62 1.09 1.02 0.93 0.93 0.66 1.85 1.09 1.42 1.73 1.03 1.54 0.55

STDDATE TIME ID. TCDO PaCOO HiCDO HpCDO OCDO TCDF PaCDF HiCOF HpCDF GGDF •C-TCDO •G-TCOF 'C-HpCDO «C-HpCDF «C-OCDO

11-10-87 13:57 SD 500 RF 0.74 0.83 0.64 1.16 1.21 0.91 0.96 0.85 1.73 1.06 1.41 1.74 0.99 1.42 0.64RPO 4.0 6.2 3.2 6,2 17.0 2.2 3.2 1.2 6.7 2.8 0.7 0.6 4.0 8.1 15.1

STDDATE TIME ID. TCDO PaCDO HiCDO HpCOO OCDO 1CDF PaCDF H)CDF HpCDF OGOF "C-TCDO •C-TCOF "C-HpCDO «C-HfiCOF "C-OCDD

11-10-87 18:55 SO 500 RF 0.84 0.80 0.64 1.15 1.14 0.94 0.94 0.89 1.79 1.12 1.43 1.83 1.08 1.56 0.64RPO 8.7 2,5 5.2 5.4 11.1 1.1 1.1 3.4 3.3 2.7 0.7 5.6 4.7 1.3 15.1

STDDATE TIME ID. TCDO PaCOO H)CDO HpCOO OCOO 1CDF PfCOF HiCDF HpCDF OCOF «C-TCDO •C-TCOF •C-HpCDO "C-HpCDF "C-OCDO

11-10-87 23:11 SD 500 RF 0.79 0.73 0.60 1.05 1.10 0.87 0.81 0.80 1.60 1.10 1.44 1.83 0.98 1.42 0.63RPO 2.6 6.6 3.3 3.7 7.5 6.7 13.8 7.2 14.» 0.9 1.4 5.6 5.0 8.1 13.6

0r'»o0 1 7 1 1 3

FORM 3 - CONTINUING CALIBRATION SUWWT

TCOO PaCOO HXCDO HpCOO CCDO TCDF PeCDF HKCDF HpCDF OCDF •C-TCDO "C-TCOF •C-HpCOO «C-HpCOf "C-OCOO

0.77 0.78 0.62 1.09 1.02 0.91 0.91 0.86 1.85 1.09 l.<2 1.71 1.01 1.54 0.55

STO0»TE TIME ID. TCOO PtCDO HWCOO HpCOO OCOO 1COF PaCOF H)COF HpCOF OCOF •C-1CDO •C-TCOF •C-HpCOO "C-HpCOF 'C-CCOO

11-16-87 08:59 SD 500 RF 0.79 0.81 0.62 1.08 1.06 0.95 0.92 0.86 1.78 1.02 1.44 1.85 1 .01 1.44 0.65RPO 2.6 1.8 0.0 0.9 3.8 2.1 1 . 1 0.0 1.9 6.6 1 .4 6.7 2.0 6.7 16.7

STO0»TE TIME 10. TCOO PaCOO HXCOO HpCOO OCOO 1COF PaCOF HXCOF HpCOF OCOF "C-TCOO •C-TCOF "C-HpCOO "C-HllCOF "C-OCOO

11-16-87 17:20 SO 500 RF 0.79 0.79 0.61 1.29 1.01 0.9 0.91 0.85 2.16 1 . 1 5 1 . 1 7 1 .74 1 . 1 7 1.78 0.46RPO 2.6 1.1 1.6 16.8 1.0 3.1 2.2 1 .2 15.5 5.4 1.6 0.6 12.7 14.5 17.B

0 1 7 1 1 4

FORM 3 - CONTINUING CALIBRATION SWHWY

TCCO P«COO HMCDO H|)Cl» OCDD TCOF P«COF HiCOF HpCDF OCDF •C-1COO •C-TCOF •C-HpCDO "C-HpCOF •C-flCOO

0,77 0.78 0.62 1.09 1.02 0.93 0.93 0.86 1.85 1.09 1.42 1.73 1.03 1.54 0.55

STODATE TINE ID. TCDO PaCDO HiCOO HpCDO OCOO TCDF PeCDF HiCOF HpCOF OCDF "C-TCDO •C-TCDF "C-HpCOD «C-HpCOF •C-OCW)

11-19-87 10:06 SO 500 RF 0.75 0.92 0.75 1.1 1.18 0.95 I.I I 1.8Z 1.1 1.42 1.76 1.1 1.56 0.68RPO 2.6 16.5 19.0 0.9 14.5 2.1 16.7 15.1 1.6 0.9 0.0 1.7 6.6 1.3 21.1

STDDATE TIME ID. TCDO PaCDD HiCDO HpCDD OCDO TCDF PoCDF H>CDF HpCDF OCDF "C-TCDD «C-TCDF *C-H(iCDO "C-HpCDF "C-OCOO

11-19-87 1 9 : 1 8 SO 500 RF 0.79 0.82 0.64 1 . 1 2 1 . 1 0.9} 0.97 0.87 1.82 1 . 1 3 1.42 1.73 1 . 1 1.58 0.56RPO 2.6 5.0 3.2 2.7 7.5 0.0 4.2 1.2 1.6 3.6 0.0 0.0 6.6 2.6 1.8

0 1 7 1 1 5

FORM 3 - CONTINUING CALIBRATION SUMMARY

TCOO PaCCO HiCDO HpCDO OCDO TCDF PeCOF HXCDF HpCOF OCDF •C-TCOO •C-1CDF *C-HpCDO *C-H|)CDF "C-OCDO

0.77 0.78 0.62 1.09 1.02 0.93 0.95 0.86 1.85 1.09 1.42 1.73 1,05 1.54 0.55

STDDATE TIME ID. TCDD PaCDO HiCOO HpCDO OCDO TCOF PeCOF HiCDF HpCOF OCDF "C-TCDD •C-TCOF «C-HpCDD "C-HpCDF •C-OCDO

H-20-87 09:22 SO 500 RF O.B3 0.85 0.64 1.04 1.09 0.95 0.95 0.87 1.68 1.01 1.57 1.77 1.02 1.46 0.64RPO 7.5 8.6 3.2 4.7 6.6 2.1 2.1 1.2 9.6 7.6 5.6 2.5 1.0 5.3 15.1

STDDATE TIME ID. TCOO PeCDO HXCDO HpCOO OCDO TCOF PaCDF H)CDF HpCDF CCDF •C-TCDO "C-TCDF «C-HpCOD •C-HpCOF •C-OCDO

11-20-87 17:26 SD 500 RF 0.78 0.80 0.66 1.11 1.09 0.97 0.99 0.96 1.92 1.12 1.41 1.62 1.08 1.53 0.62RPD 1.3 2.5 6.3 1.8 6.6 4.2 6.2 11.0 3.7 2.7 0.7 6.6 4.7 0.7 12.0

010W 0 1 7 1 1 6

FORM 4 - (UALITY CONTROL REPORT

CASE: SAS 3354-F

WIRIX SPIKE RESULTS

CLIENT 10: SAS5354F-12-A4 CW|»: Y0021MS (~~-

ftU)P- ^~COMPOUND RESULTS ( aW" f RATIO SPIKE/IS ^_

2.3,7,8-TCDO 866 Z.70 " ^1,2,5,7,8-PBCDD " 4 06 )02< 's-

1,2,3,4,7,8-HiCOO 4 22 }06f 01,2,5,4,6,7,8-H(CDO 5 13 128)11.2,5,4,6,7.8,9-OCDO I .2 102»!2,3,7,8-TCDF 1 54 l;i4f1,2,5.7,8-P«CDF 4 1 7 104^l,2,S,4,7,8-HlCOF 3 74 94*;),Z,3,4,6,7,B-HpCDF 4 13 101»!1,2,3,4,6,7,8,9-OCDO 9 87 99f

CLIENT ID: SAS3554F-12-A4 CM: Y002WSO

COMPOIND RESULTS ^f»S{- % WTIO SPIKE/IS

2,3,7,8-TCDO1,2,3,7,8-PtCDO1,2,3,4,7,8-HXCDO),2,3,4,6,7,8-H)CM)),2,3,4,6,7,B,9-OCDD2,3,7,8-TCDF1,2,3,7,8-PBCOF1,2,3,4,7,8-HiCDF1,2,3,4,6,7,8-HpCDF1,2.3,4,6,7,8,9-(EDO

^7-27-0 .113.97 99f3.80 95)15.77 144»9.36 9*f1.00 iooy3.89 97 f3.76 94)<3.98 100?;10.3 103)1

TCOO RBCOO HxCDD HpCDO OCDO TCOF M;Df H)CDF HpCDF OC[

Y0021MS ^^BW 4.08 4.22 5.13 10.2 1.54 4.17 3.74 4.13 9.Y0021M60 O^t^T-" 3.97 3.80 5.77 9.36 1.00 3.89 3.76 3.98 10.RPD (») _JJ^-2.73 10.5 11.7 8.59 42 6.95 0.53 3.70 4.;

* Total TCDO was usad for RPD calculations.

^U^-(o^

A/w. ^nuL-r^ H-v ^v^r^ ^'7br^t (^nwoG^^ izfc«^wCoyz.iz.ex/rw Pt«2- S'ftrfvLlUr A -(M r7

./COLUMNi ^?

INSTRUMENT ID l

CURVE . TTIWIO

COmENTB t

13C-237B-TCDD

I3C-1234-TCDD

37C1.-237B-TCOD

237B-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HpC

HpCOD

XDD

13C-OCDD

13C-237B-TCDF9

2378-TCDr

TCDF

PeCDF

HXCDF

13C-123467B-HpC

HpCDF

OCDF

METHOD

c"?-\^w

SCAN*

is±LiW^

s li

BD'

J321vsy\

wJOS.-

/—•.

B2BO SAMPLE SHI

^

AREA

(332) tS'.ftT'fc

(332) l CIS

(320)

(320)

(3SB)

(392)

(438) • m0

(426)

(45B)

(470) ^0

(316) ^

(304)

(304)

(342)

(376)

(422) m^S

(410)

(442)

EET

(334).

(334)

(328)

(322)

(322)

(356)

(390)

(436)

(424)

(460)

(472)

(31B)

(306)

(306)

(340)

(374)

(420) 3W2-

(408)

(444)

DATE

INJ TIW

CHEMMEST tl

SAMPLE II

SAMPLE SIZf

^" oii[i-

(•n?to

VWZ.^

tiT.

^-^

6 1 1 '10

-n-?-^3?i^•oo^f

-TW3"-'Uoltl-

,^?-2-'l41^b

T?0

-Jl1-—

-Ji4—-" l{{>6

•^g^

"•-<. 11-

; « ii.y^>.^:.^RATIO

1^-

^2-

&.

ISh.O-H

^L

•i1?-^' 10

lo^fr^-^^^3.00^

RRF AMT

1&-J&-

. 10 „

Ji JL.^23--031

o.ft'ia-3S-J±l-—J.8 .

o-ss-^L±^-l0-fi;3l-

0^

B1H»

^-^Jt&L—.V<

DL

.ail

.1&-"O.t>05» ^

.^<0

9.oo?t>

8.0b-^4

l *^

o.a0tft,»,

O'^o «««

.^1

. 3.. H"fiort?-^

e-ooti *»O.Oo'1'? »«

.A-Q. p ***

O.o0f)»»»

<r>•V—

1--

^^(>4^

yft^A^

« Ar«* of ion u«Bd for quantitation.— Intcrrri ctandard uxcd to calculate RRF i« 13C-2378-TCOF.•*« IntTnal •tandard ux*d to calculat* RRF i» 13C-OCDD.»**» 37CL-2378-TCDO RRF calculated using IFB Mthod.IntTnal •tandard RRF'» calculated ucing 1234-TCDD a« intwnal •tandard.All ethT nativ PCOO RRF't calculated using 13C-237S-TCOD for Internal •tandard.

METHOD

COLUHNt ^^

INSTRUMENT ID « ^-\

CURVE, wwioic,^COMMENTS «.. ,

SCAN*

13C-2378-TCOD jafL

13C-1234-TCDD "L

37CL-237B-TCDD . J}-

237B-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HpCDD31jL

HpCDD

OCDD

13C-OCDD }W

13C-237B-TCDF ^Ob9

237B-TCDF

TCDF

PBCDF

HxCDF

13C-123467B-HpCDF«32. •

HpCDF

OCDF

8280 SAMPLE SHEET

,Cr

AREA

(332) 1^'-^

(332)1^^

(320)

(320)

(358)

(392)

(438) \-W^

(426)

(45B)

(470) IU>m

(316) 2-^%Z-

(304)

(304)

(342)

(376)

(422) ^(366

(410)

(442)

DATE

INJ TIMI

CHEMWEST II

SAMPLE 11

SAMPLE 8IZI

AREA*6.0 571

(334) ZKpV^

(334) 'W8«

(328) ^^<-

(322) .k ^

(322) jab \

(356) POO

(390)

(436) l?^-)^

(424) ^(r

('»60)—^A^———»?<r^

(472)^7?^

^H(>(318)' "•^-fS^

(306) ^0

(306) lyi ,(340) ^?-

(374) ^^

(420)l?.fel

(40B) ^^

(444) 5'S^,

, (i-zd-27

E , 10 :n-) ,^t>0|0^

i .^W-o 1 - ^ 1

. . .r^

RATIO RRF AMT

6-tD \.'<Z 10

J>^JI ^

M^ •<

O-

.031

^33.0,-C^

[^ J. . Zg,

.; ^

J,P

l -L o-sf- ^£OJgl Jj,S >.o

O.t?

D.1i

0.

<»•«»

^Ji ASt- &-^^vn

DL

^ &'

j »"

Ll 0 0

O-oo^

O^z-

P-oo$1 ,

i5fil ^

0.6<%»»» .

0.01^/7^ 'n^

(52&Jfc»*(.WP „

®-2°2l»»&^f»», ,..^^^lO.dfl?...

o.<"> „.• Araa of ion yd for quantitation. • »»• Internal ctandard ucd to c«leul«t« RRT i« 13C-2378-TCDr. yJ.^ 4u SinJ ^dC") /" v^-^• Infrn»l •fndard uwd to e«lcul«t« RRT i« 13C-OCOD. • w-^ ^•*«» 37CL-2378-TCDD RRF c*Icul«t»d using IFB —thod.Internal ktandard RRF'« calculated using 1234-TCDD as internal standard.All other native PCOD RRF's calculated using 13C-2378-TCDD for internal standard. -

• 201'

METHOD 8280 SAMPLE SHEET DATE :_J.L®-.. -

COLUMN:.J^fc$________ XMJ TIME «_l . 3:——

INSTRUMENT ID sJ^.^. CHEMWEST ID i.fl0.!1 .

CURVE iyr^w^F/r .SAMPLE ID . ilE^ diCOMMENTS :__________ SAMPLE SIZE ;_1..2i&-

5CAN» AREA ^AREA^ RATIO RRF AMT DL ^

13C-237B-TCDD .1 1 (332)_23=lak-_ <334)J^4^_1__ : 1 :- -1°-- 2>- ^

13C-1234-TCDD .1. (332?iitUS___ (334)_2ilil?-___ - ___ -S.6-

37CL-237B-TCDD jO»L (32a)_-a.a .»._ _„„ -0. . -^_ -2ll"*» o

237B-TCDD ___. (3205_________ (322) ...Hi__ ___ .0.22. .„„ 1°11

r-~

TCDD ___ <320)_______„ (322)..JL!J'___ -——- SL33, ——-- 0-^

PeCDD ___ (358)________ (356)...ill__ --—— L -—— °~^

HXCDD ___ (332)______„ (390)_J:^__. „„ C^_ ___. ^

13C-123467B-HPCDD.L?.!!! (43B)_!&1.1J .__ (436)J_t(U?i„ i ^>.. 5S_ Sll*** ci

HpCDD ___ (426)_________ (424).^;ij___ ___ J.6!. ___-OJl-*"^

OCOD ___ (45B)________ (460)._i2_^—— --__ ^~ ———o-!^-'t*f•

13C-OCDD a£L (470)Jll _._ (472)_So^____ 0_lL o.S?_ ^__ X3>

.^g10( y^ *J "• ~ __ -

13C-237B-TCDF ^ (316)_l. ijl __ OIB). .!? !- -0-' -1-15- i?-- 113

237B-TCDr .___ (304)..__.____ (306)._3Jj_——- -___ 0-3L ___- 0-^?2<*

TCDF ___ (304)._.______„ (306)__^lh——- -—— ^1- ———'L^1-**

peCDF ___ (342)________. (340)._[1^_... ___ L „-„<t>-!±*«

HxCDF ___ (376)._______ (374). J1__. ___ °.1L ___°^^ V^

13C-123467B-HpCDF l'i. (422) 1^ _ <420)_^J2^_. 0_Si i- L 1^_ I'il *

HpCDF ___ (410)________ <40B).±12: ___ ___ JtSL ___ 9- ll#<(#

OCDF ___ (442)_________ <444)_^L^____ -—— l-L ___ 1-"»

* Are* of ion used for quantitation. „»» Internal standard used to calculate RRF is 13C-237B-TCDF. ^/^(^, /»»J ^.C>C>C.(^ AtAWi«*• Internal standard used to calculate RRF is, 13C-OCDD. S•*** 37CL-237B-TCDD RRF calculated using IFB aethod.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-237B-TCDD for internal standard.

:18

COLUMNS "5

INSTRUMENT 10 l

CURVE tStW

COMMENTS l

13C-237B-TCDD

13C-1234-TCDD

37CL-237B-TCDD

237B-TCDD

TCDD

PBCDD

HxCDD

13C-123467B-Hp(

HpCDD

OCDO

13C-OCDD

13C-237B-TCDF«

2378-TCDF

TCDF

PBCDF

HxCDF

13C-123467B-Hp

HpCDF

OCDF

METHOD

<^M

^5

SCAN*

C04I-

121'L

^3:

:mWh

A

JS22.

^QL.

^J^

CDfjar

82BO

(r

(332).

(332).

(320)

(320).

(35B)

(392).

(43S)

(426)

(4SB)

(470)

(316)

(304)

(304)

(342)

(376)

(422)

(410)

(442)

SAMPLE SHEET

AREA

iH<y4^-^^

V-W^

\W>k

Z,T-?^1

.mi5' /•L.^-Y

n *?

(334)

(334)

(328)/'

(322)

(322)

(356)

(390)

(436)

(424).

(460).

(472).

(318).

(306).

(306)

(340).

(374)

(420)

(408).

(444)

DATE 8 /*'

INJ TIME i

CHEMWEST ID 1^0°

SAMPLE ID l^

SAMPLE SIZE ; 1J-

^ RAT"•z.zisiy o.^

(^ StV) Q^fl-

4^1SS3g3

53&^^o^Z-?^^b

/^OfS-Z- Ol'1)

, . ^ y - -w

37T5S—— ——li^^' 6.

r LPJl-^^ 'JL?-!S^'5^ 5^

z?^462-

zofo?-^ 0.14^

$-1;

^o

-20-^

2-?

(^^

y^f-

3-6*2 y

RRF

1^-

e^

±22-

-o3i

e. -

-0 '-

1^-

J-!

±91-

o.SS.

-l -

&:0.16

0^

o«b

i- -

±fcL^

»

^-

-o?-/

1 '

AMT

-l£—

-H-

- L-

5£-

ns

t0^

0,

&^

2X>"'\1£--i

) '

CL ^-

^ "r—

13^**" ^0 ^i»C.

^u^^c

0.00^

0 •oofc't ,——- ^re-^ija-0D^»,» •

0-°^

,-^

-s^^A^*7:"^^ ^y ••»"f t f t i i 'vP'-'^-^**&-oo^»«

• ——•„ ^^ol^1^o-o>}'*«»

.oJl3.««»» Ar.« of ion u.«l for qirntiftion. y/Lt^l^ "'Co^^-^^»• IntTMl Btandard uifd to calculate RRF 1« 1X-2378-TCDF. - c— U•** Int»rnal •tandard uxed to calculaf RRT i«. 13C-OCDD.»»•• 37CL-237B-TCDD RRT calculatuj using ire «ethod.Internal •tandard RRT'» calculated using 1234-TCDD a* internal •tandard.All other native PCDD RW'« calculated uling 13C-237B-TCDD for internal standard.

11

COLUMNi &ly*^

INSTRUMENT ID :

CURVE «mwiciCOMMENTS «

13C-237B-TCDD

13C-1234-TCDD

37CL-2378-TCDD

2378-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HpC

HpCDD

OCDD

13C-OCDD

13C-237B-TCDF«

2378-TCDF

TCDF

PeCDF

HxCDF

METHOD 8280

CuM

W^

5CAN«

LSll C332)

^ (332)

tO-^

(320)

(320).

(3SB)

(392)

"D- Ji t43B)

(426)

(45B)^zr^L- <470)

-S.081 (3161

(304)

(304)

(342)

(376)

SAMPLE SH!

AREA

\W^

uW-

1621^

ll-

26'\0\-J.

——————

EET

(334)

(334).

(328).

— <322).

(322)

(356)

(390)

(436)

(424)

(460)

(472)

(31B)

(306)

(306)

(340)

- <374)

DAT

INJ TI

CHEMWEST

SAMPLE

SAMPLE SI

^°,.11^^.6..

.- 21£:L162-?1/^

(<%!

iL^^^

-a^a-.7J-t-w

"•S-iT^S--•ii2-w&^s^8.^3?; 2.

5&3'^»0

- S-5' ,9-5^

E ; l(--?o '>

ME, IV."-

ID . >0/3^

TD ,^4$^f^1

... (^^yRATIO RRF AMT

^ . . 111- -i£-

0-10 J^

„-„ J i-l-.-0-£?-

„ - - o a . .^a

„ o^,o^ is v>

(.01

^ -Oil &SS-

„ - -1-15-1°-,

^ - fi5LCi i

0^

l>«t>

f^?-

DL ^

.^ 'r-

.isn.»»* °

.0-^!e-oo'v^Ovoti-

:^^^-J^"«( ]5»»» '

602^»«»

-^

-^

&>9^»«

6.90«{b^

0.00' »»

0 ,» ,t <-

13C-123467B-HpCDrJi>13.- (422) •Z.^^_. <420) t^ Q^L - --- i6^*'*

HpCDF ___ (410)_________ (40B) ___ ±fcS- ___ {- -<Ht*

OCDF (442). (444).• Ar»t of ion ucd for qirntitation. ^cL^tt lo»/ CeCSlO r^co^L^«» Int«rn«l BtandTd u—d to calculaf RRF i« 13C-237B-TCDF. ^^*^^ w*' /')««« IntTnal •fndTd uwd to calculate RRF i«. 13C-OCDD.««« IntTnal •tandard uwd to calculate RRF i«. 13C-OCDD.***• 37CL-2378-TCDD RRF calculated using IFB •ethod.Internal •tandard RRF'* calculated using 1234-TCBD ac Internal •tandard.All other native PCDD RRF'B calculated using 13C-237B-TCDO for internal standard.

METHOD

COLUMN! &6~^

INSTRUMENT ID s c^^.-

CURVE.WWIClC^f

COMMENTS t „ „ .

SCAN*

13C-237B-TCDD 10^

13C-1234-TCDD 12l2

37CL-237B-TCDO 1^1}

237S-TCDD

TCDO

PeCDD

HxCDD

I3C-1234678-HpCDDJy^

HpCDD

OCDD

13C-OCDD WJ^

13C-2378-TCDF 1SS1-v

237B-TCDF

TCDF

PeCDF

HxCDF

13C-1234678-HpCDFJjt21

HpCOF

OCDF

« Are* of ion u«ed for•• IntcrrrI standard u*** Internal standard«•*• 370.-2378-TCDD RRInt»rn»l •tandard RRF'All other n*tiv PCDD

8280 SAMPLE SHEET

.6-

AREA

(332) 'U>^T-

032) m^.

(320)^.,..,

(320)

(3SB)

(392)

(43B) /50^

(426)

<4SB),,,

(470) l0''?^

(316) f 4^

(304) .,.-

(304)

(342)

(376)^,^ ,^^ ,

(422) ^KeO^fc-

(410)

(442)

qucntitJtion.••d to calculate Ku—d to calculate 1F calculated using« calculated usingRRF'» calculated u

(334).

(334).

(328)

(322)

(322).

(356)

(390)

(436).

(424)

(460)

(472)

(318)

(306)

(306)

(340)

(374)

(420)

(406)

(444)

RF ifRRF iiIFB •1234-

sing 1

DATE

INJ TIME

CHEMMEST ID

SAMPLE 10

SAMPLE SIZE

AREA*?-»-^>(.ISSilL—/2ll3i

ifliT-^67-S

2^-—"?5-o

^

16^3-1-

^?(S

•i-2^'7^575—•7r7?z^—^'i.05^

^'^<C'5J1^•2^

^0

-£1' -

4?-^^7-°ll-?oy

^(?0

13C-2378-TCOI, 13C-OCDD.wthod.•TCCD as inte3C-237fl-TCDD

, /^Zo-^

^y-^, fooil^. ^3^

.-u .RATIO RRF

JLUlll-

0^

C^

0-3?

-—— -0-%

e^p^

Q^L^L-^ '•n,

^9-L

-° . ASS-

0- -HL5.1Lo i,0^

'.I'L6^ J i.

±s&.1-L

,-, ^i^-^

rnal •tandanfor interna.

>-

-OC-/-

AMT

10

-±-

'J

J^

'15-

lO

ZA»S-

lo^

d.1 stan

?2-

DL ^

^^ CM

.., r^-

""oOAy?-L^fr-®'o.o}i-

O.oT-7-

i ^1'OJ,',»»» -

I IL—^

-l?^

°±1 .**& & t t « «

^L**O.Olb^

,(,^ •^^^, IsiX.***0-0b0»»»

oo^»»»/l^.ol ''c-/1-ccc^ '

^ . 271

METHOD 8280 SAMPLE SHEET DATE :_[1.Z$_1±.

INJ TIME «. 22_

CHEMWEST ID t^.£jS!2LrNSTRUHENT ID ».^*J^V...

CURVE .in iSA&fCOMMENTS I___________

SAMPLE ID ,7A>^<Y^OC.^-

SAMPLE SIZE i_. ±2^——_.

AREA* RATIO RRF A11T DL^1)

SCAN* AREA A11T DL

^-^ Hi;- AQ iS^_^ ___ _(^_ ___

_ o.W ^ i jo 'Z^^^ ^(^)-^

1-(M^—^~•

0

•T-^i)(334) "^3^13C-237B-TCDD

13C-1234-TCDD

37CL-2378-TCDD

2378-TCDD

TCDD

PeCDD

HxCDD

t04l. (332) ^fc.g&j'

^L (332)_il SJ.

^Jl

mL ozoJ1? !(322)Ji5?_!L---0_lL -O . ).——^

(356)_2_S2.___ ___ OSS._ _____ 0_.0^1

To (320)_. ia.i2.___ (358).

___ (392). OSO).^____ ___ 0^_ _____ eJO^

(436). il?l__ 5J1 ASy__ 3S._ iilS.***"^

(424)..jlllj„__._ ___ _^_ _____ I)_0^1*»» 'HpCDD

OCDD

13C-OCDD

13C-2378-TCDFf

2378-TCDF

TCDF

PBCDF

HxCDF

(426).

(458). "60 ^'J-1 '.1,^ __ J.»i_ __O.oo6t»««

J l- (470) ll??^ (472) T^T^1~ ^S_ O.Sf_ ^J^^-S-yo^

-i L (316) ^Z^fc

J^S, (304).S3ll,l

l!Wi (304).a.3 .__ OOS).! .1!?!!... .02&. ti l.(°,

J!aW(342).'w«L-__ <340)_1^H-_-. I66, o^-^^———*^c

___ (376)________ <374)_5.2^————- ___ o^b __Ojo}}** ,^

. ^•2^^^- &-- 1^-

J^5_ ___ D-I L***

\.^ __g.oj>5]l»,

13C-123467B-HpCDF. LL- (422) .IJ-OJQ^'.,

HpCDT ___ (410).

OCDF ___ (442).

(420)^^2 .

<4oe)_l$ .(444)

• Ar«a of ion uxed for quantitation. i ^Se 01 {\\i ^a^aAa^i•* Int«rnal «tandard wd to calculate RRF i« IW-2378-TCDF. >/O>*A TO loi l- "i-UV tuw»^•** Internal •tandard wd to calculate RRF is 13C-OCDD. «•»** 37CL-2378-TCDD RRT calculated using IFB —thod.Intirnal •tandard RRF'B calculatBd using 1234-TCDD as internal standard.All other nativ PCOO RRF's calculated using 13C-2378-TCDO for intTnal standard, n

r

/-^ ^

METHOD 8280 SAMPLE SHEET DATE t t -l?,

COLUMN. J&5:_______ INJ TIME ...l

INSTRUMENT ID tJ^ lL— CHEMUEST rD I Qfl^^I

CUR^ .^W^F/T SAMPL£ ID . 1/^J?^^

COMMENTS »__________ SAMPLE SIZE , C^-My)

SCAN* AREA AREA* RATIO RRF AMT DL

13C-237B-TCTC ^O (332) -Z-^^0 (334) li)JlL__ .-21 1&- AP, ^^ 10

13C-1234-TCDD c0^ (332) J.fe, J_1 . <334)_ -_^_?S_ _0_^ ___ _l^»_ ___ c\1

37CL-2378-TCDD ^1 (32B) •Z'ft>y3o ___ J^ . __ t 2' »» r-s—

237S-TCDD ___ (320)________ (322? /it^ tf-Tg ___ .O ___<S£S;S?1 0

TCDD ___ (320)________ <322)_3Jl____ ___ .0 2. .__0;»0^

PeCDD ___ (3SB)_______ <3S6)J i2£f-__ -__ S^9, ___ <2££S^

HxCDD ___ (392)________ <390)-&C-S^—— ___ A! ___q,aog3

13C-123467B-HpCDDJ2S «38)^2^^.__ (436)_13.S.i6J__ O. L JL I- 5£_ 1°1^***

HpCDD ___ (426)_________ (424)_^*_^°__ ___ J. _ ^__o^xf)l*** '

OCDD ___ (4SB)________ (460)_Al- 5^^_ ___ J.OI .^o•olot*•*1 —2fe33^1 - ——— -^ ———13C-OCDD ^fe <470) 2.iil___ (472) I . TJg Z."." .°-12- O.Sy. < [.. ^3

'JilaM-13C-2378-TCDF 1° (316) •Z-^^P OIB).!5^ ... ML J..1?- L0 V^

»

2378-TCDF ___ (304)________ (306) - 30^ ___ Q^j ___066^*

TCDF ___ (304)_________ (306) Hr''^<\ ___ tl.1i_ __o,{>oV7,**

PeCDF ___ (342)_______. (340)J^S..Sa .__ ___ ft;^ __A00^**

HxCDF ___ (376)_________ (374) /»_^S . ___ 'Jit. O^o int

13C-123467B-HpCDFJ6^ (422) ^yfe&4 (420)_^21/2__ &J^ j. L !«_ l£3 .»»*

HpCDF ___ (410)________ (40B) .t^__ ___ J^5_ ___0£3&***

OCDF ___ (442)________ (444) /••J '. ___ 1^1, ———O.&S&f**

• Ar*a of ion u«Bd for qu«ntit*tlon.•« Internal •tandard u«cd to calculate RRF is 13C-2378-TCDF,•*« Internal itandard u*ed to calculate RRF is 13C-OCDD.»**» 37CL-2378-TCDD RRF calculated u«in; IFB —thod.Internal xtandard RRF's calculated using 1234-TCDO as internal standard.All other nativ PCDO RRF'« calculated using 13C-237B-TCDD for Internal standard.

- 3&8^

METHOD B280 SAMPLE SH

COLUMN! (A^

INSTRUMEUT ID t .'.L--

CURVE, WtWC.^F/r

LOMMtNTS «„. .

SCAN* AREA

13C-237B-TCDD ..•$, (332). ly '

13C-1234-TCDD 1^ (332) '1593?-

37CL-237B-TCDD j^*

237B-TCDD ... <320) „

TCDD .. (320)

PeCDD (3S8)

HxCDD ,... (392) „ ,„

13C-123467B-HDCDD 1^ (43B) <\w%<{'^.^

HpCDO ^.^ (426) . ^

OCDD ^ «SB> ^—.^

13C-OCDD W2- (470) T-^0t><(> .

13C-2378-TCDF lOO? (316) ^1^0y

2378-TCDr (304)

TCDF (304)

P«CDF ^ (342)

"*CDF' .^— (376) „.„.„

13C-123467B-HDCDF t.U0* • (422) 1^^^

HoCDF .... (410)

OCDF (442)

EET OA1

IMJ T]

CHEMMEST

SAMPLE

SAMPLE S:

AREA*Sl9?i-

(334) 1611 Ot.

(334) ^^'^

(328) ^(^

, (322) /y^-^$(322 ) !» i ^

(3=6) 7-^

(390) //^-S-/^

(436) 1^»^

(424) Hf'^l

(460) /l'/»51//TI1^

, (472) W^f

-^1-^(319) •U 'L'iSn

. (306) Hf^S

(306) / .W .

(340)itf'W

(374) h'/-- 63Z

(420) ^W

(408) ^-<&S3

<444) H^£3t>

— -/-^-——-•—————

re .JHW[ME , 1^°'

ID . It.

m , ^W^t-A^

tZE , ZO'0'^

RAT10 RRF AMT

2-31 1&- v0

0-^ ie

e^ ^0.

„ J H. —.P.-Wo.<^

0 ft ' >•»•» zo

— J L(•»T-

OW „<-^^A- O.SS.

0 • (. '.0

— fi-^ -

0^

0^

614. -

-UlI'-L

DL ^0

-^ "r~-

- ---- y-- t .»»»« oO.o0g^

e.(o^- —————— tAX? 5W.-V.

6-0^

lO.OQgl

- Sll««

°£22»*» >

O.O'SJ »*«

-^

- .s- iSSZS *aQo^»«

0^0^»

o^o/Sf**

-1^^"0.031 *—

0,o3J»«>

• Arc of Ion USK) for qmntltation.» Intcrrri standard wd to caleulatc RRF is 13C-237B-TC1)F.•*« Internal standard us«d to calculaf RRF is 13C-OCDD.•**• 37CL-2378-TCDD RRF calculatfd using IFB —thod.tntcrnal standard RRF's calculated using 1234-TCDD as internal standard.All other nativ PCDD RRF's calculated using 13C-2378-TCOD for internal standard.

METHOD 82BO SAMPLE SHEET DATE i-,1 .'

COLUMN! b<^ , , INJ TIME « >6^'7

i INSTRUMENT ID t C^~\ CHEMWEST ID « ^Ool'?^)'

CURVE .^TIWIOICM^ SAMPL£ ID , SfiW>^f^-^| COMMENTS l „ .. ' SAMPLE SIZE » ^vo<i'^.

1 - SCAN* AREA AREA* RATIO RRF AMT DL r~

13C-237B-TCDD WP (332) J^^T- (334) ' (^?5-n W ^ \o V^

13C-1234-TCDD ^OSS) W 1^ (334) ^5)2-3 0^\ (o r-

37CL-237S-TCDD JOll (328) 13) 0^ .*< lt(,^>^.0

2378-TCDD (320) (322) \y-' '^&^ 0-}7 o.efl?

TCDD (320) (322) ^ 0-7?. I? .01?-r'c-« - i^y-firr.

peCDD „ (358) ,„,.„, (356) ^ ) ... P-'M D-6^

HxCDD .. (392) „.^...^ , (390) Hf-SC'7- ^ 0.0' ^^^ O.off

1X-1234678-HDCDD IP^t' (438) (•T156/ (436) 7-"''°?-t> O.^J.OT. l£> j '^w

HpCDD (426) <424).^1^2—— -151- .....<:J-3/ **• <

OCDD „.. (458) (460) ^* 5%?, 1-»T- ,^ 0.^&"»«»'y T ?-"1'; 13C-OCDD ^W. (470) W^ (472)^^ l<fl0 o^ p.s5- '" -^

($?6^;13C-2378-TCDF 100 ) (316)(7t^''S (318)'"•fit O.H |. IU ^T <,

•

2378-TCDF (304) ,. , „ . (306) fl^.,^20 0^! 0.0t '«»

TCDF (304) (306) 7J5' „„ O-^ &-^ »*

PeCDr (342) " (340) ^ ^f^ Qt\^ o.oS3**

\ HxCDF „„„ (376) „„,.„ , (374) J-ft^ <^Q ^ .„ t^ .- Oiefi?** >| - . ^ —^ ^^ -^ ,-—— ^^^13C-1234678-HpCDr 1^1 • (422) (014' - «20) I^W b^ {.^ yp. \^w \J

HoCDr (410) ,,. (408) H^e'f2 (. O.-^i***

OCDF (442). .... . (444) Hf'" 3^ \-^ 0-V »*»

• ArM of ion uccd for ciirntitation. ./M^fo le^ ^0^0 uc^\** Infrnal •tandard u««d to c«lcul«t« RRF ii 13C-2378-TCDF. 'rMW:ru " " ' ' >•*** Infrnal ftandard ucrd to calculat* RRF is 13C-OCDD. U•*** 37CL-2378-TCDD RRF calculated using IPB —thod.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDO RRF's calculated using 13C-237B-TCDD for internal standard.

ji '342

l-2o -&9-METHOD 8280 SAMPLE SHEET DATE

COLUMN! .JS?! . INJ TIME » I'S-'6^

INSTRUMENT ID

CURVE .^TIt^^^f/r

COMMENTS i__________

AREASCAN«

13C-237S-TCDD 12'H. (332>___^j^_

13C-1234-TCDD '1. (332)J_'Jg??l_

^4_37CL-237B-TCDD2378-TCDDTCDDPeCDDHxCDD

___ (320)______

.__ (320)_______

___ (3BB)______

___ (392)______

CHEMWEST ID ;_^°l!i _____

SAMPLE ID , 9AS3^-01-A-'>

SAMPLE SIZE s ^•^^-

AREA* RATIO RRF AMT DLT.lg^l

(334)_m^21_ A2i 1&- -L0- ti3-(334)„22.i^:i.

<32S)Jf lL

<322)._l'?:l__

(322)

j^_ ___ J_e__ ___

_ J^ J__ i?a^__ _oj2_ __ &_^_o

_—-o-% __-aJl-l0

__ ^g_ __ o-oofe0(356)__48£.

(390) ^2 0.0, 0 •00fcf

(436)„(.5Z: L^_ 151 J. .. Zff_ ll l***

(424).. .lfc___ . __ ^_ _____ 0_S_**» 'HpCDDOCDD13C-OCDD

13C-237B-TCDF237S-TCDFTCDFPtCDFHxCDF

(426).

(45B). (460)_^^:y3____ ___ ^V__ _____ &.0^»««

(472)"1^2otf~ P_n_ 0_S$_ ' s' %'

_^f^<316)_^.l'^^__ (31B)_.il]I3$_. P_ . J. . iP___ _1U

<304)__._______ (306). 2±__. ___ 0^_ 0_0i »*

0_06}_1»«

0^ __O.06}]**e-«^ 0-66%««

2A

(304) _._______ <306)_?.i^____ _„_ O .

(342)_________. (340)_^_'21

(376) _______ (374)

13C-l23467B-HpCDFly^:- <422)_Z$6^&.,

HpCDF ___ (410).

DCDF ___ (442)

(40B)_I°i.

(444) ^g

• Ar«« of Ion used for quantitation.•• Int«rn*I •fnd«rd u««d to calculate RRF is 13C-2378-TCDF.•*« IntTnal standard UKd to calculata RRF is 13C-OCDD.•»** 37CL-237B-TCDD RRF calculated using IFB —thod.IntTnal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using I3C-237B-TCOD for internal standard.

METHOD

CllLUMNi b^

INSTRUMENT 10 l C*

CURVE, WWI C ,f,F,6-

COMMENTS l —„—-

SCANH

13C-2378-TCDD i j-

13C-1234-TCDD ' h

37CI.-2378-TCDD WJ^

237B-TCDD

TCDD

PeCDO

HxCDD

13C-1234678-HpCDDJ i2

HpCDD

OCDD

13C-OCDD J fcl

13C-2378-TCDF j;00fe«

2378-TCDF

TcorP«CDF

HxCDF

13C-1234678-HpCD^jf?J•

HpCDT

ircDr

8280 SAMPLE SHEET

AREA

(332) -z-^yi 1

(332) lfS^t>

(320)

(320)

(358)

(392)

(438) U>\

(426)

(458)

(470) t-Wl-^

(316) W^ .

(304)

(304)

(342)

(376)

(422) ^b^O

(410)

(442)

DAT

INJ TI

CHEMWEST

SAMPLE

SAMPLE SI

AREA*.Wf-^

(334) 32.1^1

(334) z3a,S-8

(328) z-TTS®'/

(322) W

(322) .. fIL..

(356) ^

(390) ^'

(436) W^

(424) fc^-0

<-»60).Jr-3?-%?(472) •Z 'V'FT-

l2-iy3T(31B) tloS^L

(306) 6H^'

t 3 0 6 ) 6 . ? J .

< 3 4 0 ) 3 £ . ^ — —

(374) '

(420) foof? 1 -

(408) ^

(444) ^ l

E »-lHfc:^-..--..-

re •IIL1'2--...--.-.ID » ^oofcb^fcTID « (» t(r1<<)J?^l>l« ;ZE « C' 00 )

RATIO RRT AMT

- 1?°- lai- J0-- o-11 i»

o. 4o.»0-33.

- . . ?;%. ....-, 0.0-

- 6t6' ' —j S J. . ZO

'•I,

J.»l

0-^ o. 'r?

C-'^ (.-»!. lO

,- -- &^- -

6 ^ „

oycmb

^0.1(7 1 .

.1 . -..-

l.

OL

-i^

q^*«»,. o.011^^

O-oo^

&.ooq^0, }.l f- ^o***

p-oo"^*.333

.-1^^ff^»»0 -01>g;%*«

t),OQZ^«»

D.OOj-^

.i^***

.00^»»»Q.oWm

• Ar** of ion U«MJ for quantitation.•• Infrn*! ctandTd wd to c«lcul*t> RRT i« 1X-2378-TCDF.«*• Int»rn«I •t«nd«rd u««d to calculate RRF !• 13C-OCDD.•*•• 37CL-2378-TCOD RW caleulatwd using IFB —thod.Infrnal •tand«rd RRT'* calculatBd using 1234-TCDD •• intfrnal •tandard.All othT nativ PCDD RRF*» calculat«d using 1X-2378-TCDO for internal •tandard.

COLUMN; ^^

INSTRUMENT ID l

CURVE «97V^\0COMMENTS i

13C-237B-TCDD

13C-1234-TCDD

37CL-2378-TCDD

237B-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HpC

:OS?

OCDD

13C-OCDD

13C-237B-TCDF

2378-TCDF

TCDF

PeCDF

HxCDF

13C-123467B-HpC

HpCDF

OCDF

METHOD

Cu?-\

^W

SCAN*

iSiD-^

i .

——

DDJTfl

CU?

100^

DF.i.67!"

8280 SAMPLE SH

^

AREA

(332) ^W-?-

(332) 1^600

(320}

(3205

(358)

(392)

(43B) ?-5(!>UT-

(426)

(458)l.T,o It

t o^s. g^ '

(316) f1!^^-

(304) „

(304)

(342)

(376)

(422) ^

(410)

(442)

EET DAT

INJ Til

OEMWEST

SAMPLE

SAMPLE SI

AREA*Wiao .(334^1?-^

(334) t^Oth^

(328) ^1 7^^

(322) HF- ^^-

(322) ^^<5

(356)JW:J'l5:

(390) h*1- 403

(436) •Z.y^O''1-

(424) m'-sig.(460) H+, 'KoO

(to3t'2. (472)'^•T>1?-'•/

12.142.1(318) ^T^r-

(306) Ht'S&Z.

. (306).H.t'5S2:. .

(340) Hr'-Ste?

(374) Ht' =14

(42Q) ^l'f«

(408) H»-»<«°1

(444) Hi-'5-b§

E

ME

II

II

Zf

-

-

. --Ib,;, ^'0\

) : ^oo n^, ,^^5^yF; .. (2-.s-7s.

RATIO RRF

Ml lll-0.%(>

o<si.o-JZ

- -o^t&;g0.0-

OA^ J;01

—— JJ1-Jl,»l

-0- . -o-SS-

^L ±1^-&^-c ,Oft»

o«b

0^ j^

— - a s -\.

S7-

-10-/I'/

AMT DL

AO ^

^

-tL- L -"**

0^0^

5,^q6£>^fO.SQa^

2S— J ***.0)&»»«

"c'-o-y?^g^»»»»'

^L-2fi-

10 ^J^

C'CT(5-/4*

.0. *«

(2.tX>^0»»

C3.L>gg?««

^ •,,

a^»»»

o.Di7 ••»

0^1

r~

0

xpc-

• ArM of ion Ufd for quantitation.»• Infrrri cfndTd uswd to calculate RRF is 13C-2378-TCDF.•*• Internal standard uced to calculaf RRF is 13C-OCDD.•*•* 37CL-2378-TCDB RRF caleulattd using IFB •ethod.Internal standard RRF's calculated using 1234-TCOD as int«rnal standard.All other nativ PCOD RRF's calculated using 13C-237B-TCDD for internal standard.

r~,

DATE -.Jl-^J^L

INJ TIME »__L1L

METHOD 8280 SAMPLE SHEETCOLUMNS Jfifc .

INSTRUMENT ID 8 . L-

CURVE «5[!®J^A&f -

COMHENTS «__________

CHEMMEST ID , OZ^

SAMPLE ID «5Al fH±_ii

SAMPLE SIZE 8__Z_^6^_____

AREA* RATIO RRF AMT DLSCAN« AREA

13C-2378-TCDD W t332i (T-O^O __ <334) ''TT' P-' - It!;. JO

13C-1234-TCDD ."L C332).j2£W__ (334).1^^L. HL „._ J^

37CL-237B-TCDD

2379-TCDDTCDDPeCDDHxCDD

(320).(320).(3SB).(392).

___ _0_<S^ _^_

__ _0j2. _„._ -o±l ..„___ 93$._ ..„

__ p_.e^ __&_ _ J_y»_ tg,_;_ _\^i_ _

l-o-i.

(390)_l6 .

(436).1J21^<5HO(424)

(460)

HpCDDOCOD13C-OCDD

13C-237B-TCDF2378-TCDFTCDFPeCDFHxCDF

(426)

(45B)11 r ' J"^^^^^""™^"^^^ ^ "" ^nsv '™ ^ ™ ""^^^^ ^^^^JM- <470)„6i.lS£»_ (472) '^-wr^ J>J.l o-SS- L

W^O ,liS- <316) ZZ^OO (31B) iE-_ _&^ _L1L l.

(304).(304).(342).(376).

(306).

(306).

(340).

. i2 !****,<?_o^_. o-olt

0_o^

()_0^_

l

r<^

r~

o

•f:^."*

. °-j3-**«°. -"«.jai.^l. L3.1!**'^-?21»*^-^1-

O-o^T- „

13C-123467B-HpCDFJ£32.- (422)_^I' _

HpCDr ___ (410).

OCDF ___ (442).

JaL__(

11.__,/ ^(^-te ' 0 ^^1

»«••*. Jl-**11

M^ ...

• Arc of Ion ufd for quantitation.•• Infrnal ctindard wd to calculate RRF is 13C-237B-TCDF.•*« IntTnaI standard UBKJ to calculate RRF is 13C-OCDD.»—» 37CL-237B-TCDD RRF calculated using IFB »>ethed.Internal Btandard RRT»« calculated using 1234-TCDD ac internal atandard.All other native PCDD RRT'a calculated using 13C-237B-TCDD for internal standard.

METHOD 0 SAMPLE SHEET

COLUMN;. ( '

^'^••Jl^-SL

INJ TrME !__^____.

CHEWIEST ID : YO°^_L

SAMPLE ID ,^^..^.

SAMPLE SIZE !_^?. ll_.___

INSTRUMENT ID : ..___L'-L—

CURVE iSLW_hC^^(r

COMMENTS :„___„___„_

SCAWt AREA . AREA* RATIO RRF AMT DL

13C-2378-TCDD W?__ (332).1^_2. -—— (3345:_-t.L;g.&____ _°.-2i l.ll_ .LO._ 3 .

13C-1234-TCDD L00^ (332)_J_8X1_>___ <334)_'j^:°?_6.-. —11- -__ J.0-- __--

37CL-237B-TCDD J0^_ (32S)_tl2£5__:__ .___ _o..<?i . _ S .****^

237B-TCDD _____ (320)________ (322)___^59___ _____ _0.32_ ____ Owfi^ ^

CMm

TCDD _____ (320)_.._______ (322)___T^C'_.__ „—— -&_% _____ ^J^

PeCDD _____ (3593 __________ (356)^__'__'/?____ ____ &.?•?_ ____ i0.0.'.:'1'

HxCDD ____ (3925__________ (390)_A^_32?__ ____ _)..&_ .....O."

13C-123467e-HDCDDr.'^o_ <43B)_J_^___2.__ (436)__lf_0_?i2.___ .IL J_ l_ !£__ L0.! ***

HpCDD _._._ (426:1 _„___.„.„ (W)Jf^^___ ___ j_l___ ___.(....L1:*** •

OCDD ___ (45B)_________ (460)_^/i2T^.___ ____ J..." . _____o__>?_2;**x

13C-OCDD t L <470)J_-?:.._..___. (472). l. .-.... O. - SSE, - -i .

^t^?13C-2378-TCDF W__ (316).1(_^3.1&._. <319).^^_E.-- M- -1-1L -l0

^

2373-TCCF _____ <304)___________ (30S3__»fc._^:____ _____ fi.3L __.

TCDF _____ (304)_________ <306)__/_'6._!.s5.._ .„__ 0_^_ _____ l5_0(_tl.»-

PeCDF __„_ (342) „_.„._„„ <340).__w_.__ _____ ll.. __„.o__tll!**

H:<CDF .__„ (376.1.________ ^74)_ft^_W___ ___ fit. ____3..P__1"*

13C-1234678-HpCDF_.<5_ (4225.?5y______ (4203_^_??5-l-t—— -O.. . _.L'i_ ISL_ to_T__»»»

HpCDF ___ (410)__________ (40B)__.---'—'L.__ __- J- - -___{>_^h^.^

OCDF ___ (442)_________ (444)_W?.2/JL—— ___ _—1. ____'?-ooc^**•

* Area of ion used for quantitaticin.*»* Internal standard used to calculate RRF is 13C-2378-TCDF.**•* Internal standard used to calculate RRF is 13C-OCDD.»•»** 37CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.Al l other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard.

r^-HETHOD &. ^ SAMPLE SHEET

COLUMN; „_&;$._„_______

INSTRUMENT ID : _^J^._.

CURVE sinS.I -0^

COMMENTS !____„_____-

SCANft AREA

DATL^A-L^^-...

INJ TIME s.J^^f.____

CHEMWEST ID «_w•>2:l——_._„„

SAMPLE ID :J ll$yf_--fcH

SAMPLE SIZE :.2___'?'__.

RATIO RRF AMT DL

13C-2378-TCDD 1&M__ (332)_JZa^3...__ (334)^lf7?iL—— -P-' 1.1?=- -^-- 1 . '- ^

13C-1234-TCDD 1(0.5 (3325 ^.f^__. (334)_J2.?^__ i?.V\

^<r1tt /»»./.„37CL-237S-TCDD 1^S._ ' (SSai.i'-jJ"-0-

2378-TCDD I25__ OSO).. .!.__ <322?..2;2: S.

TCDD TO_^J (320)_«12°JS..

PeCDD _____ (358)_____.

HxCDD ___ (332)_____.

13C-1234678-HDCDD^y^_ (4385 .U^JtS..

(3225_1L12J±___ •Z.f- -OJa^!iL-/——--/

^^*~" 1^ /(356)_tf/a_^31L___ _____ B1.' . ____ ._»s__r ^

(390)J____'_1__.

(436)_llL20-(_—.

<4245___"__3^>_

(460) ?- <> 1 _""ggfOfa

(472) ll^loo

-•sia/_____ _0_&1 _____ A50JO

0-lL — .- 2£-_ -'—^***_ H^ _ a. oiS *•»«

o_l__ J^L^0 ,. -___ (426).

^0-- (45B)_•_tLL,

1?53— <470)___^_tl.

HpCDD

OCDD

13C-OCDD

13C-237B-TCDF

2373-TCDr

TCDFPeCDFHxCDF

-_^L o-s?_-!„-'J-^ ^

C. Ot? »+*-7 ci.^' J.JLJ.

L—— J?-?] -1- - -l-0—— -!l !/

L'L—— 0; - 0.../...{\.£:l„.3 2••r''

.1___ (3w_i1^___ (3ia)_Iw[_»

I060— (304?__?J^______ OOS)..!...?.'

(306)_1^^.._. t-XL -'-'-I. -:lLt

(340)._>_^_.0fc____ ^__ 0_^_<_-t0/l

(374)_Hr___1^2__ _____ 0^_ ___ o0-(376).

"20 >—??——'——-&^-- i?-1!- Ifil-' A-

(408)___t__^_3.

13C-123467S-HoCDF_l^_ C 4 22) . iA5 -.

HpCDF _____ (410)_______

OCDF ____ (4423. (444)._/___A5±

* Area of ion used Tor quantitation.** Internal standard used to calculate RRF is 13C-2378-TCDF.«•«» Internal standard used to calculate RRF is 13C-OCDD.»*" 37CL-2378-TCDD RRF calculated using IFB method. ' (• JL J <Internal standard RRF's calculated using 1234-TCDD as internal standard, t^-^u^.All other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard. /V\.U

^ ^ .i .0 SAMPLE SHEET DATt. ; lj-10-j^-METHOD I .0 SAMPLE SHEET

COLUMN; __^:5.______..- INJ TIME s^SSt ^JTJ5'

INSTRUMENT ID i. LlL... CHEMHEST ID : L3 :1."! ————.

CURVE siTLWJOG^J.. - SAMPLE ID i! !! 2:!!."? •t> •

COMMENTS :___________ SAMPLE SIZE ; _lS.^J[^._____ -^^L

SCAN# AREA AREA» RATIO RRF AMT " DL

I3C-2378-TCDD \SS'_ (332) ..W3J..._ <3345.L^L<JL- l.-l1: j-1?:- -£.. 3l /j^

13C-1234-TCDD l«i_ (3323 J}0.!6!---- (334)J^1M^___ 0_?3_ ___ _^0__ ____'" v-

37CL-237B-TCDD ^_ <328)J6iM——- -__ -o-$l -^-- l? "*

237B-TCDD \<&H. (3^.^^___ (322)_\JH<1S.___ .O. . ±2?- (l r' 'l- ^y

TCDD ____ (320)______._____ (322)__^n:_____ _^__ .O l - 5cKl':;.-''i

PeCOD i»:J^05B) 1'L .L.... <356)_6iJJ£——— -c>. - &:Z-L ii. - w^

HxCDD L?^- <332)Sfc6Sfc.____ (390)_t.232£-—— ?-2?- -o.ftl It1!- -l0.

13C-123467B-HDCroS(iL ('*3S'-S?i?-L——_ (4363JH.lfO^___ _____ __».•__ JLO__ ^0___»»- V •;

HpCDD ^/ 2_^ <42e)j_Z_^____ (424)^1L22_____ ..__ J:°l_ llLJ.- l* ^

OCDD ^ _lte.- (''so.lif?!.... (46o)_i_51&._._. _ ±y1:., ll.ir .'l.'J"- l<n

13C-OCDD lf?l. (470) vtv[^ (4725 1^0? __ _. 0-___ ns _ - Q,^ - ^

13C-2378-TCDF ^L_ Olfc). '1!'..___ (3ia?_Z^^OO____ ____ _\^_ _l0___ j^

2373-TCDF .WL_ (304).?:lll .____ (306). 1152^-—— ——- O.tL jL. '1' --4'-* 1^^

TCDF _____ (304)_________(306)_nr___..._ _. &.ll_ ____ ___**

peCDF _t2?h (342)_i.«ly:„_._ (340)_.j,A6______ ___ 0.1_. .li..(?: l0^*

HxCDr IM. (3765_?2^E-—— <374).311^J,___._ „__. 0_<b_ l-Vf_ l *

13C-1234e7^-H^CDF_l<•66_ (^S^JSWt'L-__ C420)_2^^(,_rg____ _____ __^l_ |_p-__ J_8—»

HpCDF ^_. (410)_4_.10_,____ (408)_<i2_<[l5___ ____ J. _ .H. . _l ^»*

OCDF _l..fc_ (442)_fl-?1.1--_-- (444).__lll<_'_•_._. _._„ _ 5__^ _^@»»-

* Area of ion used for quantitation.»* Internal standard usetl to calculate RRF is 13C-2378-TCDF.*** Internal standard used to calculate RRF is 13C-OCDD.»»M- 37CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using I3C-2378-TCDD for internal standard.

~~ METHCC 3i SAMPLE SHEET

COLUMN; _J)fc^_____-__-

INSTRUMENT ID i. lL--

CURVE :Sr\W]0_^^(r

COMMENTS :______„___

SCAN# AREA

DATE -_ih°l -

INJ TIME it-e>:10

CHEIWEST ID :S^.^L

SAMPLE ID 6M^l3--A±.^

SAMPLE SIZE !_Z^.-J3——____

AREA* RATIO RRF AMT DL

13C-2378-TCDD Ml- <3325 J2:*l'id_.__ (334)_ZiO^_

13C-1234-TCDD 1%-- <332)_ilf_4iA_—— (334) Jt2_c.lL

37CL-237B-TCDD l3_'L (32B).^tjjoM„

Wl_ <320)_W£1_____ (322)_ tJL?2.?0

inr^

____ (3205___________ <322)__^____.

{w- (35B)__\[2Jg..4__ (356)__&yZ,1?_.

l- .1-- <392)_______3____ (390)__£._L.°.

2378-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HDCDD^_ (436) _\^^0!.^•__ (4365JJ<l5_OJ|.

HpCDD J?lL (426)_._C2.S_____ t424)________L.

OCDD W?. (45B5__?S'«J___ <460).y^^°._.

13C-OCDD . (4703.i1.J.%_.._ (472)„?_01<11

- -°-% -'i- ^^***» r-~ ~~~ "1 •LT'-"^^ D-^^qit— -°:22L JL—^ __— O'1

Ji-35. ...m. A^- -^_o_^ ^^^ _^3>-!. ZP l; * »MI

j-a- s^ i ^±^^--^-:-^ ^'

o.sy ^ 5^

13C-237B-TCDF ^-- (316?-2£ife3±__ (31S)_Ujki6.f.___

2373-TCDF "L. (S04)_7^.^^?____ (306)_3^^$____

TCDF _____ (304?_________ (306>__^-__——

PeCDF 1!?2._ (342)__?__lS.____ (340.1__l_-J__il____

H..CDF ll l (37e)__^A^____ (374)_ly:?_»_.

13C-123467^-^JpCDF_^„6i_ (422)__if^'____._ (420)__l'f___l.

HPCDF ^L (4.10)_>fm_._„ (40S5_?«.._<L?_„

OCDF ._._ (4423_y._4l.%_____ (4445_^?_l4j_.

* Area of ion used for quant it at ion.** Internal standard used to calculate RRF is 13C-2378-TCDF.»••"» Internal standard used to calculate RRF is 13C-OCDD.»*«» 37CL-2379-TCDD RRF calculated usino IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard.

m <-o ^--— —--^-^-B^L L&r—--b^_ ___ ___**

-L i-fl -'-13**".i'—i—L li- **

. T-6 •r)-L'L 2-S-— L-^-*^*

-—- ±iL L - -i00' ^-—-- J-?-- 1°J- *»-

^ i ,

METHOD 8280 SAMPLE SHEET.COLUMN. j '.'L

DATE :JlS:13:.

INJ TIME s 1 ! - ! 1

AREA KifBS** RAT10 RRr AMT DL

13C-2378-TCDD ____ (332)Jl?l51__. (334)'tlltt63 J__^ __>U__ _JO__ __6%

13C-1234-TCDD ^_ <332)_1_:<C.6J___ (334). j00 ... .-l1. ___ _\Q__ ____

INSTRUMENT ID 8_C^__

CURVE «.?[BMA^C ._

COMMENTS :____________

SCAN«

37CL-237B-TCDD \n^_

237S-TCDD ___ (320).

TCDD ___ (320).

PeCDC ____ (35B).

HxCDD HD- (392) ___

13C-123467S-HpCDDJ3S._ (438)_^2.^ .s'l.

HpCDD JLD. (426)______.

OCDD 13dL (45B)___7 .5_a,.

13C-OCDD £S^_ (470)_^S3?^.,

A'__S. (342)_,

A-'-CL <376)_.

13C-123467B-HpCDF__B?l (422)_^2_^^

HpCDF _/_[b_ (4.10)______

OCDF

— -0_3l- --1-- illl****

^0r^•s"r-

o

CHEMUEST ID :. .l3.______

SAMPLE ID sj ll l'll-JLL

SAMPLE SIZE s___JLl.§-^-_.__

EA» RATIO RRF AMT

(328) .S0. ?.0..

(322)_B3--IL1 -.

<322)J^_r::l l6_

oso.h.tJJ ISS'L.(390) -<.^^

6_-i0_ __

0_<0_ __

_&A2>_ __

Ml- --

0_WM6

I.OMt.

^%

(436)_^^^1J__ ^h. _0_13_ _^__ IS ***

(424)

(460)

-^

-•-££!,*•*

fi.0212**.- -L- *

i'll: "L***

1-dT. 'i:<»-'l*»»———————- ^•J——— -————y- t--———J,*""

^ .M^Ss-11'?^(472)Jl: l J^_.

' iS?-

13C-237B-TCDF _%!._ (316)^111^2—— (SISl-I m'L- -0.10. _W.

237B-TCDr ____ (304)______^___ (306).Ht:...<9i23___ ____ .Ofj .

TCDF ___ (304)_________ (306)__.J[l0__ _____ .OA(.

PeCDF _^__S. (342)_____„__ (340)___J^_Z£__ --__ -0• ?.

HxCDF ,;J . (376)________ (374)__^^__ _____ _0;.J_

— <420)__11f__.J__ .0.1T: _Lyi _y__ l_£3-*»*

__ (408)___^_L_?___ ___ __.l. ____ ilL- Jfc***

J3-7 <442) „_„;_?._„ (444)_.^.__.^__ . L .i_. -„.( ___**»

* Area of ion used for quantitation.«• Internal standard used to calculate RRF is 13C-2378-TCDF.»•»» Internal standard used to calculate RRF is 13C-OCDD.»••» 37CL-237S-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-237B-TCDD for Internal standard.

METHOD 8290 SAMPLE SHEET

COLUMN! .j LE.

INSTRUMENT ID ••-°^1.

CURVE j grtgH^^C ,

COMMENTS ;.

SCAN* AREA

SSsL (332).i2.yiii.13C-237B-TCDD

13C-1234-TCDD

37CL-2378-TCDD

2378-TCDD

TCDD

PeCDD

HxCDD

}W^_ (332).?OJa.&g_

l d-___ (320)______

__„ (320)_______

____ (35B)______

(392)

(426).

(458)

HpCDD

OCDD

13C-OCDD \^1 (470) 'H'

13C-2378-TCDF j O. (316).?_7L2l3_

237B-TCDF

TCDF

FeCDF

HasCDF

(304).

(304).

(342).

(376)

13C-1234678-HpCDF^]_ (422)_yjlf.l.

HpCDF ___ (4.10).

OCDF (442)

DATE iJhl:?!————.

INJ TIME ;_H.^J.6______

CHEMMEST ID !_^}^——_——

SAMPLE ID ;4^1'a.L-ll-Al

SAMPLE SIZE ;__^.•^.^„_____

AREA* RATIO RRF AMTWZf.

<334)_nHt»___ &A°_ _W:_ J0__

(334). 5.^___ JL"10- ___ -A°_-

(328)_6^5_t^S.___ _____

(322)Ht:-5>3 ___

<322)__t_J^O_. „__

<356)_+t^'gfr._^___

(390)JH.r:..__3... ___

<436)___£^il_„ i. _6_13_

(424)_!j__aLl____ ___ _V_L_

(460) HC'-<'2&__

(472)^_^_L__ 0-1 -0•S»- -2?-- -'i -

-_' 1 .• _ -——————• . /l« .... • fTtiff^)

csia ti'i&gjL'.... _L-_1'1-_'_'_'__ .I".

oooJAL.JQfi.-- —„ .^. —.

(306)_H_r^^<-'___ ____ _0flt_ ____

(340)_ht»^(l___ .___ .°:32. _...

(374)_H.t:_2^a.__ ____ _0.5&. ___.

(420) 'mYSS _0^_ _^_ _LO,

(40B)JttU!t$3—— ___ -Itl- --„

<444)Jl£-_i _. ___ .1.0 . .„.

DL

H2<.r—K\•^—r~-

,— it.O.W , ,-&-CTb iv^<«?S

->:3i- -Jl.- J1-?-***PL _____ _,J»OB2

P-l0- —— £i.'i°.V-&-CTb ii"

- L --—- -sa^___l_ _____ __OJt

^__ fill***«>af? *»»

J_0fc_ ____ fl;Q_._T»»«

o.«a7f««

n. ceho ««

. 4;££6l**

. iSd-**

. l ?!***

$ ' 3»»»

. feSSI-***

* Area of ion usBd for quantitation.»• Internal standard used to calculate RRF is 13C-2378-TCDF.*•* Internal standard used to calculate RRF is 13C-OCDD.»*»» 37CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-237B-TCDD for internal standard.

METHOD 82SO SAMPLE SHi

COLUMN: M-?

INSTRUMENT ID ;£ii.:l

CURVE 8 TISW)AJ^

COMMENTS ; „. ,„.„„„

SCAN* AREA

13C-237B-TCDD ^^ (232) ^W^ll

13C-1234-TCDD ^B1^ (332) 'i8°'W

37CL-237B-TCDD ^^L-

237B-TCDD (320)

TCDD (320)

PeCDD • (35B).

HxCDD (392)„

13C-1234678-HpCDD'la- (438) Z?5H?

HpCDD (426)

OCDD (458)

13C-OCDD Q*?? (4705 ^K-?^

13C-237B-TCDF ^2. (31£) G^ syL-

2378-TCDF ( 3 0 4 ) „

TCDF (304)

PeCDF (342)

HxCDF (376)

13C-123467S-HpCDFlfc<ii- < 422) J i .fi .

HpCDF (410)

OCDF (442)

SET. DATE ; 11-5-2^-

INJ TIME ;J5J(5

CHEMWEST ID : lOff2-^

SAMPLE ID :5^^TMP-»?-^

SAMPLE SIZE ; . tljc-

' AREA* RATIO RRF AMTIJI-H J.

(334) "Wl- l 0-^1. W 10

(334) '^fr^1 O-IO 10

<32S) ^^"S-fc 0.11 ^

(322) Hr'-Z '8' a-^o(322) JJJ; HT-& „ O.<0

.. (356)iltiJaaCL-- -0^- -——-

090) Jyr- 6;?? . o->(i(7'VS

^ (436) •Z-6?^L4- ^Ada. ^^L ^

(424) Hl»5-<<>i>' W

(460). lit' 3ll»-? ^6(,&^»{0

„ (472) V^T-f Q,.y[ 0-y •2?

fwr^(3lS) 'MS^?6% Ot" W lo

.- (306)..4.t*.L-&3&... „ .OIL „

(306) M^S^ 0^1

- t340)JitUf" - (>•'^';L - -

(374) 0!"- fc<;!'7- °5&.

.- <420)&llir^ JL32; -L-4 - -y-(40B)HT--(*M W

(444) HfJiS^ -- {•0<1'

DL CO

as-r~

L^A"®.- r<^feSS.7?

o^SSQ

t'^Si

1^»"'

<1^^**

g;55T»<H1^^

6^

^S^

^221'°**0.60 <«««

0. OO/fc ««

^^S2!**

\S1^-»ft 0^»»»

»-£5&3***• Area of ion ueed for quantitation.»* Internal standard used to calculate RRF is I3C-2378-TCDF.*** Internal standard used to calculate RRF is 13C-OCDD.»»•» 37CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard.

METHOE

COLUHNi bfr" ,,...,...

INSTRUMENT ID i. " .

CURVE .WtW^^Ai

HJHHEMTS 1

SCAN*

13C-237B-TCDD t0^^-

13C-1234-TCDO t.*- -

37CL-2378-TCDD C£^L

237B-TCDD

TCDD

PeCDD

HxCDD

13C-123467B-HpCDD2^

HpCDD ———

OCDD ———

13C-OCDD J3 -

13C-2S78-TCDF lS£l

2378-TCDF

TCDF

PeCDF

HxCDF

13C-1234678-HpCDF.K£.

HpCDF

OCDF

) 8280 SAMPLE SHEET

^

AREA

<332)l2iH2^-

032) l3>^^

(320)

(320)

(3595 „

(392)

(43S) t^l^

(426)

(4SB) „

(470) R l-l-

(316) •t-^^

(304)„

(304)

(342)

(376) ^

•(422) WST-

«10) . .„ . ,

(442)

DATE

INJ TIME

CHEMWEST 10

SAMPLE ID

SAMPLE SIZE

6&2.S/^(334)^15)^.^—

(334) .i O' lL-

(323) tV17'9"^

(322) £,0?^Z. „

(322)„(11L-——

(356) ^1^

oso.J^(436) 'islfife

( 4 2 4 ) t ^ & „

(460) 990

(472) ^^8 -

^^(31B)1.^:1[7S^

(306) 601- .

(306) ,1 ^

(340). ^ l^

(374) ^J .

(420) ^<?^16

(40B),A^——

(444) ^^ .

, If-Zo-^

, [6-'f<>^oozsf^.^y^^'^-e'. . ...,-

RATIO RRF AMT

±^111-J£-

J^ J^

o^ 4032

£ . - 3 3 . -&^ .O-O-

£^«. J,%- 5£-. .HI.

Jl;o1.

. &S?- -

-O. z .LIL i£-fit -l-o^fj»b

oJ^ wi iaJas-

. . k -L

DL <^

1" ^r~

j l"*» 0

O.oz1-0ooV-o.o^

^ L/yM^

6-0^ »*« •

0oMl..,

j-il

^L

o^ojjx&-jpgi «0 •tift **O-ooffi.,, . i

: wl ^6 ,««

0<%»«»

• Ar«* of ion u«*d for quantitttion. Jl i / , /ll <aDP- (&**&S•• Int»rn*l •t«nd«rd ucd to c»lcul«tB RRF i« 13C-2378-TCDr. •rfi f» £'<yw ^•*• Int«rn«I •tandard ucd to calculaf IW i«. 13C-OCDD.•*•» 37CL-237B-TCDD RRF cilculatfd using IFB —thod.Intrrn*! standard RRT'* c«lculat«d uaing t234-TCDD •• infrnal »t*nd»rd.All other nativ PCOD RRT's calcul«t«d u«ing 13C-237B-TCDD for int«rn*l »t«ndard.

56)

METHOD 8290 SAMPLE SHEETCOLUMN! .J&JL

DATEINJ TIME Ib-.S)

INSTRUMENT ID i. . L—

CURVE .JIl^tCAgf^

COMMENTS i._________—

SCAN*

CHEMMEST rD ; •^CloMrlS.^t.

SAMPLE ID > -aAS^J^P-1^-61

SAMPLE SIZE

AREA*SCAN* AREA AREA* RATIO RRF AMT DLtg'gt,o4 0-^

13C-2378-TCDD ioaS. (332>_L'Ei2S£—— <334)_3?S5S— ±3^11^- •A0— -3^0^ft—

r-^—o

13C-1234-TCDD

37CL-237B-TCDD

237B-TCDD

TCDD

PeCDD

HxCOD

13C-1234678-HpCl

HpCDD

OCDD

13C-OCDD

13C-2378-TCDF*

237S-TCDr

TCDF

PeCDF

HxCDr

13C-1234678-HpCI

HpCDFOCDF

\a3&.JtiifcL

3DJaal

JflAfc-

JSS&.

VJ^.-

(332)

(320)

(320)

(358)

(392)

(438)

(426)

(458)

(470)

(316)

(304)

(304)

(342)

(3765

(422)

(410)

(442)

i. ^

———

-aQlfib--

-i assa..

a.i4&34fc

———————

a-mms

(334)

(328)

(322)

„ (322)

(356)

(390)

(436)

(424)

(460)iteW^

(472) Ifc3.fe%> .

(318)

(306)

(306)

(340)

(374)

. (420)

(408)

(444)

^gS^S152.4 Ifc

l«4fe50

- ^15-

- l .

S s s ...,.- ...

4S.l- l>-ISEPS

WO

•5,^-

fytb%%%3.a5,

^5

J ^ .

—5§5---^^

J ! ^ l.

—.5;tl-.

. ^v

o-IOAaas^

O.'Sf?

o-^„ .a-33L. e,5L

o.e-0. J^

--'•''l-

I.9-1.

^T- o-sy

O-^ 1.

O.V.

0H2.

0.

0-»t»

±fe^

l-»^

-Lt--tL

2£-

-X5-

1.0

Zo~&S--

-1^****- -°^.- ,-£.£32

O.OI~ i v-TW(

^>. 6H»»»~T?rv

B.fl'ld »»j

Lyi-

6,0j »«

-^L»*ff.<?2'!-»«

- e(3^**l»»*

-^^&-<)' *»

• AFM of ion ufd for quantitJtion.»* Int«rn*I <fnd*rd u»«d to c«Icul«te RRF i« 13C-2378-TCDr.**• Int«rnal •tandTd uc«d to calculate RRF is 13C-OCDD.»*«• 370.-2378-TCDD RRT calculafd using IFB WBthod.Infrnal standard RRF'B calculat*d uxing 1234-TCOD as infrnal standard. V\All other nativ PCDO RRF'« calculated using 13C-2378-TCDB for Infrnal •tandard. /J

578

METHOD 8280 SAMPLE SHEET.

COLUMN: __M^.

DATE :_iL-i--!?_.

INJ TIME U.I.L07-

INSTRUMENT ID :_CW.:__

CURVE sW^A^A

COMMENTS :__________

SCAN«

13C-237B-TCDD

13C-1234-TCDD

37CL-237B-TCDD

237S-TCDD

TCDD

PeCDD ' ___ (3SB)

HxCDD ___ (392)

AREA

I?1'!- (232)^30S3-JL_

1°?-- <332)_'___0___

»__>__

l&ZC, (320) fco 19-?--»/f-/02^ -»1»^1

ta<C?"320) _^fec_>L._.

.CHEMMEST ID i. ^ -

SAMPLE ID s S l .Jll

SAMPLE SIZE ;__M_52.V

AREA*ia.V733

RATIO RRF

_q3_^ __a_

-0.1.1 --.

AMT DL

-J2-- 50.?2

10

(334}_ .i2.AJI

<334)J^±.llh-

(32a)jlil±^^____ __„ _0_.3i_ __!__ J »»»«'

<322) ?_i?_gy o_2^_ i:io/o.i^_,___<322)__^L3.t23___ 5..? P_«0_\^_l5/'___

(356) ... I__ --—— -^AL --—— 0^

(390)_titiij».U_-__ ___ SSL- —__ 5--fi£?

• -^—r-T~o

13C-123467S-HpCDDQS:L <438)_^6^5J(1___ (436).'SL2i2^——o-.tL -'LIL -t?-- l ?a***

HpCDD _____ (426).

OCDD ___ (458).

13C-OCDD

-w----—.^-^^J_tk_ __ a-0*.'-***

13C-237B-TCDF

(304? 9'? 2-^T- (3065 ~X> T-^S- _ .„.•___ M^ O.

C304):3g_5.: (306).5^ .0.?_,.0^?)

l6_3_- !'(?342).J. n:___. (340)__t.l^.3^-__.^: .^\W'.___<*KAf'-

____ (376)________„ (374)__r_^a____ _____ _og__ ___A£e_.^»*

2378-TCDF

TCDF

PeCDF

HxCDF

13C-l23467B-HpCDF__'__ <422)___H______ (4205_J.____i.__ &_ft__ __M_S_ _y_ __^»»»

HPCDF ._ (4io>_____ (4oe)_Htl i3— __ J_tl_ __tii- iS.***OCDF ___ (442)_________ (444)_t___to___ ___ -__' '_ ___ • •-'-1***

* Area of ion used for quantitation.«* Internal standard used to calculate RRF is 13C-2378-TCDF.**•* Internal standard used to calculate RRF is 13C-OCDD.»*«» 37CL-237B-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.All other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard. 595

METHOD S280 SAMPLE SHEETCOLUMN; M-5

INSTRUMENT ID :_0^;L__

CURVE iiTL^A --

COMMENTS :____________

SCAN* AREA

13C-2378-TCDD I?!-4.. (332)_^^oilS-.

13C-1234-TCDD W^_ (332)_ .?H1.

tOTff37CL-2378-TCDD237S-TCDDTCDDPeCDDHxCDD

HpCDD (426).

(458)OCDD13C-OCDD

13C-237B-TCDF237B-TCDFTCDF (304).

(342).(376).

PeCDFHxCDF

r-

o

^35- (320)_^^:___ (322)_^«SS . _0.y. 64_0/ ^?_;

I61!- (320)J^Jt___ (sssi.Jmh.._ .i . o_<o[ .

-'£13- (470).!.51J .L

110 (316) ^HiLLb

DATE iJL5:!?-

INJ TIME :_JJi_'2l__.

CHEMMEST ID : 00l-&

SAMPLE ID Jfl.jt.il.

SAMPLE SIZE :"'•<'^-S-CM•stRATIO RRF AMT

<334) ][2:ll2...fe___ OJ^ J_'tt._ _j0_

(334) l-.l. "5.____ _6_3JL __— -A0-.

(32B)_^&'il5_^:„_. .___ _0.3l_ _^ IL'A,,,'.'

DL

1A

(436)'^fefet" 051_ _»_13_ .tS.. _U^»»»

(424)J^^y3_— --__ !&- ___- i -***

(460)_^/'-^7____ ____ J_6fe_ ___o_2i3_»«»(460) Ht'SOf~SSKJF^T?^ .... _ _.,«>

(472)_J33i^J___ &_»0_ _o. »_ _75__ JT^_

U^feoOIS^'2-'1191' 0 fl ^

aa.o_ (3o4)__ .g,i5^_ (3o6)_Ji^(£(2___ ^_y>_ _o?_(.( o._< .

13C-1234678-Hp CDFJJJfc. (422) J=lfeSI?_

HpCDF ___ (4.10)______

OCDF (442)

- <408).fcfe .S-

._ (444)_(J^3,&^_.

JM-(.Ofc

0,0 II »«»

ft OtS «•»»

* Area of ion used for quantitation.*» Internal standard used to calculate RRF is 13C-2378-TCDF.*** Internal standard used to calculate RRF is 13C-OCDD.»•»» 37CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard,Al l other native PCDD RRF's calculated using 13C-2378-TCDD for internal standard.

METHOD 8280 SAMPLE SHEE1

COLUMN; W-'5

INSTRUMENT ID : W-\

CURVE : TlSW^eC^

COMMENTS :

SCANtt AREA

13C-2378-TCDD ^fv' (332) 3?^X2-

13C-1234-TCDD [% (332)yi2?Ja

37CL-2378-TCDD {v^

2378-TCDD (320)

TCDD (320)

PeCDD (358)

HxCDD (392)

13C-123467B-HpCDDl2SS C»38) llOtH

HpCDD (426)

OCDD (458)

13C-OCDD fl5'l (470) l^O^fc

13C-237B-TCDF ^1 (316) fHl W»

237S-TCDF (304)

TCDF (304)

PeCDF .. (342)

HxCDF (376)

13C-1234678-HpCDF l^W (422) 13- 4^0

HpCDF (410)

OCDF (442)

DATE

INJ TIME

.CHEMHEST ID

SAMPLE ID

SAMPLE SIZE

AREA*132.111

(334) 4ZS-^

(334) 5 11. .

(32B)2d2.£2.o „

(322)Jlt^lfill

(322) ^1

(356) 32-^

(390) Uh-^lZ.

(43G) 15 (»

(424)Ji£22ST

(460) m-'1^2f.T&T5V-

(472)lltK>•!i^

>?(>30^01B) 55W&

(306) LllH-

(306)Bt;:3.53——

040) m"- 'no(374) H^%a

(420) Uo'^<.

(408) H^^l

(444) Mr-Hi^

; H-5-^. 16: T-

: 00^

s^J^j^

« 2.S ,RATIO RRF

Ml Jd?--o-3P

„— A-3i-6.40

O.<0

0^

O-fZ

lo> ey

— -w„ ±.ofao.y)- o.

O-^ WO^tofKO.T?

--—— -O-Sfc.

laT: L-yiWl.Db

••

.'2*'- (2,2,

————— (i<-

AMT DL •

J0 W. ^-

-A°-. —— o-1- -l s3;****

£W&

0^(°[""", ,-^5a

o.»y<0. OS»

-Lp— -»*»e.^ •»*«

lAAPl0.33 *»» '

^ ^1

w iz&<»iM »»

f < * »—— - &£-&-**

flifiiJfe**

zo q' ..***Si£3te.***0-fi.te***

* Area of ion used for quantitation.*» Internal standard used to calculate RRF is l3C-2378-TCDr.**•» Internal standard used to calculate RRF is 13C-OCDD.*»»» S7CL-2378-TCDD RRF calculated using IFB method.Internal standard RRF's calculated using 1234-TCDD as internal standard.Al l other native PCDD RRF's calculated using 13C-237B-TCDD for internal standard.

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