transmittal of fish study work plan for lake dupree ... · fishes^-, and the audubon society field...

HERCULES , Hercules IncorporatedHercules PlazaWilmington, DE 19894

-0 - - . . . --. (302) 594-5000-' ; . . , i ! • .). Telex: 83-5479

Writer's direct dialnumber: (302) 594-7066

September 1, 1988

Hr. Robert E. HannesschlaBer, Chief CERTIFIED MAILReturn receipt requestedSuperfund Enforcement Branch (6H-E)

U . S . Environmental Protection AgencyRegion VI1445 Ross AvenueDallas, Texas 75202-2733

Re; Vertac Off-site Areas - Fine Grid Sampling PlanJacksonville, Arkansas

Dear Mr. Hannesschlager:

Pursuant to paragraph 2 4 . 1 . of the CERCLA Administrative Order on Consent,CERCLA VI-07-88 ( O r d e r ) , for the above-referenced matter, HerculesIncorporated submitted to the U . S . Environmental Protection Agency (EPA) aFish Study Work Plan (Plan) for Lake Dupree on June 27, 1988. The Plan wasapproved by EPA on June 2 9 , 1988. Pursuant to paragraph 2 4 . L . of the Order,work on the Plan commenced within 10 days of approval of the Plan; fish werecollected from Lake Dupree on July 6 and 7 , 1988 by our contractor, the ITCorporation. Now, pursuant to paragraph 2 4 . M . of the Order and the schedulecontained in the Plan, we herewith submit the IT Corporation report for theFish Study Work Plan for Lake Dupree.

One ( 1 ) copy of the report and the analytical laboratory data reports (FinalDioxin Report for Jacksonville Offsite, Volume I , Report and Data Summary, andVolume II, Initial and Continuing Calibrations and Data, July 2 6 , 1988) forthe Fish Study Work Plan for Lake Dupree are enclosed with this letter.

Being transmitted under separate cover to Kate Arthur, EPA, Region VI, with acopy of this letter are five ( 5 ) additional copies of the report without theanalytical laboratory data report as requested.

Enclosures

cc; Kate Arthur (6H-EE)U . S . EPA, Region VIDallas, Texas 75202-2733(by Federal Express)

Florence K . Kinoshita. P h . D .Senior lexicologist

INTERNATIONALTECHNOLOGY

I CORPORATION

RESPONSIVE TO THE NEEDS OF ENVIRONMENTAL MANAGEMENT

REPORT OH FISH STODY WORK PLAN(FOR 2.3.7.8-TCDD)

LAKE DUPREEJAOTSOMVTT.T.E. ARKANSAS

REPORT ON FISH STUDY WORK PLAN

fFOR 2.3.7.8-TCDD)

LAKE DUPREE

JAgKfiONVTT.T.K, ARKANSAS

Submitted to:

HERCULES, INCORPORATEDWilraington, Delaware

Prepared by:

IT CORPORATIONKnoxville, Tennessee

August 1988

REPORT OH FISH STUDY WORK PIAM

(FOR 2.3.7.8-TCDDj

LAKE DOPREE

.TACKSONVTT.T.R, ARKANSAS

APPROVALS: IT Analytical Services

NAME; Dana SimerlyTITLE: Proiect Manager

SIGNATURE:

NAME: Bruce Wagner_____TITLE: Laboratory Manager

S IGNATURE: /^Z^t^ ^X^L

NAME: Carol A. Erikson_____TITLE: Program Manager_______

SIGNATURE: LOW-U. •CAtA^^'——

1.0 EXECUTIVE SUMMARY

Fish were collected from Lake Dupree, Jacksonville, Arkansas, on

July 6 and 7, 1988 in order to determine the concentrations of

2,3,7,8-tetrachlorodibenzo-p-dioxin (2 , 3 , 7 , 8 - T C D D ) in the edible

portions of fish in the lake. The fish were collected using gill

nets. A total of ten (10) fish representing five ( 5 ) species

were filleted in the field and submitted for analysis for

2,3,7,8-TCDD by high resolution gas chromatograph/high resolution

mass spectrometry. Analyses for 2,3,7,8-TCDD were done on the

left fillet, minus the skin, of each of the ten fish. The

results of these analyses showed 2,3,7,8-TCDD levels ranging

from 0.013 ppb to 0.48 ppb. The individual result for each

sample is listed below:

FIELDSAMPLENUMBER

WH1750LFMS*

WH1751LFMS

WH1752LFMS

WH1753LFMS

WH1754LFMS

WH1755LFMS

WH1756LFMS

WH1757LFMS

WH1758LFMS

WH1759LFMS

FISHSPECIES

Largemouth BuffalofishLargemouth BuffalofishGizzard Shad

Gizzard ShadWhite CrappieWhite CrappieWhite Crappie

Bowfin

Blue CatfishBlue Catfish

2,3,

0

0

0

0

0

0

0

0

0

0

7,8-TCDD(PPb)

.031

.25

.0099

.48

.046

.029

.031

.013

.068

.23

* LFMS: Left Fillet, Minus Skin

2.0 Introduction and Objective

In compliance with a portion of an Administrative Order of

Consent between the United States Environmental Protection

Agency (USEPA), Region VI, and Hercules Incorporated, Wilmington,

Delaware, IT Corporation, a wholly owned subsidiary of

International Technology Corporation, was comnissioned to prepare

a fish study work plan for Lake Dupree, a small body of water

located in a community park in Jacksonville, Arkansas. The

purpose of the plan was to determine if the edible portions of

edible fish were contaminated with 2,3,7,8,-tetrachlorodibenzo-p-

dioxin ( 2 , 3 , 7 , 8 - T C D D ) .

The collection plan was designed to allow samplers to obtain

several different species of fish from which a representative

number of each species would be selected for analysis. The

fillet portions, minus the skin, of representative fish from the

lake were to be analyzed for 2,3,7,8-TCDD using high resolution

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

3 . 0 Field Activities

3 . 1 Fish Collection

Upon notification by Hercules Incorporated, of the acceptance of

the fish study work plan, the Field Analytical and Sampling (FAS)

Division of IT Corporation commenced fish sample collection

efforts. Scientific collection permits issued by the Arkansas

State Game and Fish commission were used for the duration of the

project and all specified conditions were met.

Fish were collected from Lake Dupree on July 6 and 7, 1988 using

four, 6 ' mono filament gill nets, 125 feet long with 3/4 to 2 inch

mesh. The nets were strung from opposing banks in an East-West

pattern with one net in each quarter section of the lake. The

first net was strung West to East in the northernmost quarter;

the second net. East to West in the second quarter; the third

net. West to East in the third quarter and the fourth net was

strung East to West in the southernmost quarter. A 14 foot

aluminum boat equipped with a 5hp motor was operated in a random

pattern in the lake in an effort to increase the swimming

activity of the fish. The nets were checked hourly; fish were

removed and released, or kept for collection when deemed ap-

propriate for the purpose of the fish study.

Fish were keyed and identified using How to Know the Freshwater

Fishes^-, and The Audubon Society Field Guide to North American

Fishes. Whales, and Dolphins2.

After a period of over twenty-four hours and successful col-

lection of five ( 5 ) species of fish, it was decided that these

^ow to Know the Freshwater Fishes. Second Edition, SamuelEddy, Win. C. Brown Company Publishers, 1969.

^he Audubon Society Field Guide to North American Fishes.'•'hales, and Dolphins, Alfred A. Knopr, Inc., 1983.

species would be representative of the fish population in Lake

Dupree. The five ( 5 ) species collected were:

o LARGEMOUTH BUFFALOFISH, Ictiobus cvprinellus

o GIZZARD SHAD, Dorosoma cepedianum

o WHITE CRAPPIE, Pomoxis annularis.

o BOWFIN (aka DOGFISH and GRINNEL), Amia calva

o BLUE CATFISH, Ictalurus furcatus

From these species, ten (10) specimens were selected for

analysis, including two ( 2 ) Largemouth Buffalofish, two ( 2 )

Gizzard Shad, three ( 3 ) White Crappie, one ( 1 ) Bowfin, and two

( 2 ) Blue Catfish. Excess fish, which duplicated those species

selected for analysis, were returned to the lake.

3 . 2 Sample Handling and Documentation

Each fish selected for analysis was assigned a unique, field

sample number which was scribed on a metal tag; the tag was

attached to the fish using a self-locking nylon tie threaded

through the gills and mouth. Each fish was weighed, measured and

photographed; all measurements and observations were recorded on

individual specimen collection log sheets. Copies of the com-

pleted collection logs are presented in Appendix A ; they have

been typed from the original hand-written logs for clarity.

Table 1 lists the size of each fish specimen selected for

analysis.

Chain-of-Custody (C/C) records and Request for Analysis (R/A)

forms were initiated by the Sampling Coordinator for the ten (10)

samples in order to track sample transfer from field collection

to receipt at the laboratory, and ultimate disposal. The

originals of the C/C and R/A records accompanied the samples at

all times; a copy of each form was maintained in the field until

completion of the field effort.

After collection and identification, each fish was carefully

filleted on both sides; each fillet was then individually wrapped

in aluminum foil and placed back on the fish in its natural

anatomical position. Each "whole fish" was then wrapped in

aluminum foil and the field sample number written on the outside

of the wrapping with indelible ink. The fish were immediately

placed in a cooler of ice and later transferred to a cooler of

dry ice for shipment to the laboratory.

The single exception to this sample preparation procedure was the

right fillet of specimen WH1750, a Largemouth Buffalofish, which

was hand-delivered to the on-site USEPA representative (Region

VI) . This fillet was individually wrapped in aluminum foil, and

marked with the field sample number. It was kept frozen on dry

ice until its release, under chain-of-custody, to the EPA re-presentative. The remainder of specimen WH1750 (the "whole fish"

less the right fillet) was wrapped in foil with the left fillet

in place, and handled in the same manner as all other samples.

The prepared fish specimens were shipped frozen on dry ice by

overnight carrier, under full chain-of-custody, to the IT Special

Analysis Laboratory (IT/SAL), in Knoxville, Tennessee, for isomer

specific (2, 3 , 7 , 8 - T C D D ) analysis.

4 . 0 Analytical Program

4.1 sample Receipt

The ten (10) fish specimens were received at the IT/SAL on July

8, 1988. Immediately upon receipt, each specimen was checked

against the accompanying chain-of-custody forms to verify

documentation accuracy and sample condition, and subsequently

logged-in. The left fillet of each fish was removed, assigned a

unique laboratory number for internal tracking purposes and

forwarded for analysis. The laboratory (ITAS) numbers and cor-

responding field sample numbers are listed in Table 2 for

convenient cross-referencing where necessary. The remaining

parts of each fish ( i . e . , right fillet, head, and viscera) were

kept frozen and remain archived at the laboratory.

4 . 2 Sample Preparation

Each fish fillet was ground and homogenized after the skin was

removed. Ten (10) grams of each sample and ten (10) grams of

sodium sulfate, the method blank, were weighed into separate

jars. Each sample and the sodium sulfate blank were spiked with

lOOul of an internal/surrogate standard mixture, containing

5.0ng 1 3 C - 2 , 3 , 7 , 8 - T C D D and l.Onq 3 7 C 1 - 2 , 3 , 7 , 8 - T C D D , and allowed

to stand overnight for equilibration. After equilibration, ex-

traction by ITAS methodology was performed. The ITAS Standard

Operating Procedure for extraction of biological samples is

presented in Appendix B. The procedure used for each sample is

described, briefly, below.

After overnight equilibration, the sample was blended with lOOg

of sodium sulfate and 50g dry ice until homogeneous, dry and

powdery. These amounts vary slightly from the amounts described

in the work plan, but the amounts used were sufficient for drying

the samples, which is the purpose of the sodium sulfate reagent.

Acetonitrile (150 ml) was then added to each sample, and the

mixture was shaken for three ( 3 ) hours on a platform shaker. The

variation in agitation time from that described in the procedure

(Appendix B) was made based on the nature of the specific samples

and was approved by the laboratory quality control coordinator.

The resulting extract was then filtered into a flask and con-

centrated to approximately 5ml. The concentrated extract was

transferred to a separatory funnel using a ten (10) ml portion of

acetonitrile to rinse the flask. Approximately 15ml hexane was

then added to the separatory funnel.

4.3 Sample Cleanup

To aid in the removal of chemical interferences, each con-

centrated sample and blank extract was treated using separatory

funnel techniques detailed in Option C of the U . S . Environmental

Protection Agency, Region VII protocol for "The Determination of

2,3,7,8-TCDD in Soil and Sediment," September 1983 revision.

Briefly, the extracts were washed with 20% potassium hydroxide

(KOH) followed by distilled water (to remove KOH residues) ,

followed by three concentrated sulfuric acid (H^SC^) washes,

followed again by distilled water to remove acid residues.

Further routine cleanup consisted of two ( 2 ) column chromato-

graphy steps. The first step involved passing the extract

through a neutral alumina column; in the second step, the extract

is passed through an acid-modified silica gel column which then

flows directly into another neutral alumina column ("dual

column" step). The final extracts were concentrated to near

dryness, then raised to 50ul with isooctane.

4.4 Sample Analysis

Isomer specific analysis for 2,3,7,8-TCDD was performed using a

modified version of the EPA reference method described in "RCRA

SW-846, Method 8280", revised September 1986. The final extracts

were analyzed using high resolution gas chromatography/high

resolution mass spectrometry (HRGC/HRMS) scanning in the selected

ion monitoring (SIM) mode for enhanced sensitivity. A 60m SP-

2331 fused silica capillary column, demonstrated to resolve

2,3,7,8-TCDD from other isomers of TCDD, was used. Before

acquisition of the sample data, a seven ( 7 ) isomer performance

mixture containing 2,3,7,8-TCDD and the six ( 6 ) most closely

eluting TCDD isomers was run. In addition, a five ( 5 ) point

calibration curve was run in triplicate. The mean response

factors (RFs) obtained from this initial calibration were used

for all subsequent calculations; Table 3 contains the initial

calibration summary data. A shift standard was analyzed on each

day that sample analyses were performed, to demonstrate in-

strument stability. To be acceptable, the measured shift

standard RFs had to be within 10 percent of the mean RFs from the

initial calibration. Shift standard results are summarized in

Table 4. Method accuracy was measured by calculating the

recovery of 37C1-TCDD (surrogate standard) as compared to the

internal standard, ^C-TCDD, for each sample analyzed.

5.0 Analytical Results

The results of the isomer specific analyses for 2,3,7,8-TCDD in

the fillets (without skin) of fish from Lake Dupree obtained by

HRGC/HRMS are reported in Table 5. The "client sample number"

refers to the field sample number assigned at the time of

collection. The measured concentrations of 2,3,7,8-TCDD are

reported in parts per billion ( p p b ) . When no 2,3,7,8-TCDD was

found, a sample specific detection limit was calculated as 2 . 5

times the background signal in the general elution area of the

"C-TCDD internal standard. The additional information contained

in Table 5 ( i . e . , GC/MS analysis date and time, relative ion

abundance and surrogate percent accuracy) is reported as required

by EPA protocols.

6.0 Analytical Quality Control

To demonstrate that all analytical materials, i . e . , reagents,

glassware and solvents, were free from interferences, a method

blank was processed with the batch of ten fish samples. The

blank was extracted, analyzed and reported according to the same

procedures used for the accompanying samples. The blank was

designated BLK1195 and no 2,3,7,8-TCDD was detected at a de-

tection limit of 0.00l9ppb, successfully demonstrating the

absence of laboratory contamination.

One matrix spike/matrix spike duplicate pair was also prepared

with this batch of ten samples, to provide data for evaluation of

analytical precision and accuracy. The sample to be spiked and

duplicated was selected at random, by the laboratory, at the time

the samples were logged in. Table 6 presents the results of the

matrix spike/matrix spike duplicate analyses, along with the

corresponding precision and accuracy calculations. The relative

percent difference (RPD) of 15.4% is well below the upper limit

of 50% specified by the EPA, demonstrating excellent analytical

precision. The spike recovery of 109% is also acceptable,

falling well within the 60-140% acceptance range, and

demonstrates excellent accuracy.

10

Surrogate (^Cl-TCDD) recovery ("Percent Accuracy") was also

calculated for every sample and blank as a measure of the

accuracy of the overall extraction and analytical procedure. The

percent accuracy for each analysis is included in Table 5. In

every case, the accuracy is within the 60-140% method-specified

acceptance limits, demonstrating satisfactory laboratory

performance of the analytical method.

The 2,3,7,8-TCDD results generated for this fish study are

satisfactorily supported by all available quality control

information.

11

TABLE 1

SPECIMEN SIZES: LAKE DUPREE FISH STUDY

FIELDSAMPLENUMBER COMMON NAME

(SPECIES)

SIZEWEIGHT LENGTH(gran) (cm)

WH1750LFMS*

WH1751LFMS

WH1752LFMS

WH1753LFMS

WH175LFMS

WH1755LFMS

WH1756LFMS

WH1757LFMS

WH1758LFMS

WH1759LFMS

Largemouth Buffalofish(Ictiobus cyprinellus)

Largemouth Buffalofishfictiobus cyprinellusl

Gizzard ShadCDorosoma cepedianum)

Gizzard Shad(Dorosoma cepedianum)

White Crappie(Pomoxis annularis)

White CrappiefPomoxis annularis)

White CrappiefPomoxis annularis)

Bowfin(Anna calva)

Blue Catfish(Ictalurus furcatus)

Blue Catfish(Ictalurus furcatus)

540 32

520 32

140 2 2 . 5

140 2 2 . 4

70

50

420

370

460

730

16.8

15.5

30.2

53.2

38

44.1


TABLE 2

CROSS REFERENCE SAMPLE

LABORATORYNUMBER

BB0546

BB0547

BB0548

BB0549

BB0550

BB0551

BB0552

BB0553

BB0554

BB0555

FIELDSAMPLENUMBER

WH1750LFMS*

WH1751LFMS

WH1752LFMS

WH1753LFMS

WH1754LFHS

WH1755LFMS

WH1756LFMS

WH1757LFMS

WH1758LFMS

WH1759LFMS

NUMBER LIST

SPECIES

Largeaouth Buffalofish

Largemouth Buffalofish

Gizzard Shad

Gizzard Shad

White Crappie

White Crappie

White Crappie

Bowfin

Blue Catfish

Blue Catfish


TABLE 3

INITIAL CALIBRATION SUMMARY

TCDD/TCD?

JACKSONVILLE OFPSITE

Date

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

CC1CC2CC3CC4CC5

Instr.ID

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

Mean

37

61220

Sol.ID

CC1

CC1

CC1

CC2

CC2

CC2

CC3

CC3

CC3

CC4

CC4

CC4

CC5

CC5

CC5

RF Used (x) =

» RSD =

Cl

pg/nipg/nlP9/til

NativeTCDD

0.952

0.959

0.924

1.05

1.03

1.06

1.07

1.10

1.06

1.02

1.02

1.07

1.13

1.17

1.20

1.05

7.3

10 pg/ul50 pg/til

100 pg/H.11000 pg/ul3000 pg/ul

Measured RFNative

TCDF

1.88

1.86

1.91

1-99

2.03

2.04

2.10

2.33

2.28

2.09

1.82

2.30

2.42

2.63

2.74

2.16

13.0

Natives

Surrogate^'Cl-TCDD

0.931

0.923

0.846

0.956 c'

0.951

0.948

0.974

1.03

0.949

0.945

5.1

sm(bwlO)

TABLE <

ISOMER SPECIFIC CONTINUING CALIBRATION SUMMARY

JACKSONVILLE OFFSITE

BATCH 1195

Date

07-17-88

07-17-88

07-17-88

07-18-88

07-18-88

07-18-88

Inetr.ID

70-250S

70-250S

70-250S

70-250S

70-205S

70-250S

SolID

PC

CC1

PC

PC

CC1

PC

NativeTCDD

1.08

1.08

HgasSurrogate-"Cl-TCDD

1.00

0.972

ured RF RatioNativeTCDD

1.03

1.03

(He,Surrogate•"Cl-TCDD

1.06

1.03

as/Mean)

TCDD IsoraerResolutionPet. Valley(Applies ForPC Only)

7.9»

5.4»

6.8t

7.4»

Solution ID Codes;

PC ° Performance check solutionCC1 •" Concentration calibration solution #1 - 10 pg/ul

sin(bwll)

S g 3 E S ° S ^ s s i 5 s s i s s § i l 5

? ° . . . . ? a a a ^ a a a a a a a a a? » B - ^ - » ? ? ? ? P ? ^ ? ^ ! ! i ? P- ; S , B- S " 3 ; ; 5 5 5 5 5 ; ; 3 ;

z z S. o S 2. v » , » « » » » , » > » « , » »" •s?-6<? •° -

^I

3-g g i S S i i y y

•* 8 **

I

•o o» ^ o*

35- ° .3 .3 3 ° 3 3 ?• ?•g ° ° ° 5: g

^ i i ^ ^ I i i ^ j 5 !? S 3 3 g 3 . . . . . . . . . . . .

»„; , • • • • • • • • • • • •X 0 0. 0. Mt A 0 • W

8 a c ^ r > J 0 ^ 0 0 0 0 0 0 0 0 0 0 0r t ^ B M ' r ' ' ? ' ' ^ * ^ ' ^ ' ? * ' ^ ' ^ ' ^ ' ? 1 ^ 1 ^ ^r~ A •— ^ • . ^ . ^ . ^ _ A ^ « > ^ _ k _ * ^ ^ _ i _ J

S 8 5 S S B S S S 8 8 S S

— * f ^ ~ * » K V l m o w ^ m w ' ^ ' f »• " o « t e * o « « o w i r u - 4 o ! — • o S *

a r ^ t ^ ' ^ . p ' - ^ ' ^ O ' O f ^ t ^ l

S —* fiJ -* ufe M 0*• u * u — O f t O ^ f O o r s J o u t r u. • ^ O . - . - ^ . O - . f t . - t ^ - V l - . o l ^s s

?

_ * | \ J - « _ * _» _• r^ _• -i _* _*f r i r u ' V« 0» •0 -• C^ 0 -^ 0- •»1 <\*i.n a ™ o o •o -> M -* — -^ vim r u - o u * - « f > u i o > — • 4 0 ' ^v - k U t h J L n f ^ ^ C f f O i ' i ^ O l U *w < - c » . t ' t > ' - o o - . f > i ^ - ' . - * o y

Table 6OA/QC REPORT

Project Nane Jacksonville off«lt»_____Coda HF»a»5B

Batch limber 1195___________________________HBHS

Simple Hatrix Fish_______Extraction Method spec I •I______

Report D.t« OB-1Z-M___________________________

GC/MS Run [iaf (I»OIMT») 07-17-M________________

Surrogate Percent AccurBcy

tuitier of Daf Point* - 17Hean Percent Accuracy « ___107X

Ranae' • 9a-Hni

Sanple * BB055;

Preclilon of Duptlotel

Splk« Dup. Vlue (i) •

Splk« Value (b) •

2,1,7,8-

TCPO

0.12

0.14

Precliloo- |a-b| « 100X - 15.W

l*b2

EPA Ringe • SOX

'• 2,3,7,»-

Accuracy of Spike Tcoo

OInervJd Spile Value <b) - 0.14

Orlg. Valir (a) • 0.031

Spike livel (c) • 0.10

Accuracy • b'l x 100X • 109X

c

EPA Rerioc • 60-140X

EPA Ranga for turroaata percent accuracy of 60-UO» applle* to laomer apecffic analyafa only.

«m(bnU)

APPENDIX A

EE3 SPECIMEN CULLECTIUN .06 DATE8

TIME 10

1

73

0fi

65

8 8PROJECT NAME: JACKSONVILLE/

LOCATION: , OFFSITE „ ,jacksonvilie,ArkansasPROJECT ff 480078 01 09 01

SAMPLE # WH1750LFMS

Largemouth Buf fa lo - f i sh Specimen Type

SpeciesI c t iobus cyprineTIus

Collection Method

Preservation Method

Gin riets

Dry Ice

Sample Location Description LAKE D U P R E E

PI Prep Lab AU = Austin CE = Cerritos DI = Directors ED = Edison FH = FAS MobileHK = Hiddlebrook PI = Pittsburgh SC = Santa Clara

01 Analysis Request: 01 = 2,3,7,8 TCDD 02 = Total PCDD/DF03 = Total and ISOMER specific PCDD/DF04 =

Fi lm RoU Ho. M Frame No- 22

Sample Team D.Peery, D . S i m e r l y( imt ia i s ;

Prepared By P. Peery Ck'd By DSS(Initials)

E53 SPECIMEN CULLECTIUN 3G DATE'

TIME 1n1

74

01

6Z

8 8

OFFSITELOCATION:„ Jacksonville,Arkansas

PROJECT 3f 480078 01 09 01

SAMPLE ft WH1751 LFMS

Laroemouth Buffalof ish

Ict-iobus cyprinellus

6 1 1 1 Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method

Sample Location Description LAKE DUPREE

PI Prep Lab AU = Austin CE = Cerritos DI = Directors ED = Edison FH = FAS MobileMK = Middlebrook PI = Pittsburgh SC = Santa Clara

_0^ Analysis Request: 01 = 2,3,7,8 TCDD 02 = Total PCDD/DF03 = Total and ISOMER-specific PCDD/DF04 -

File Roll No. 04 Frame No- 23

Sample Team D.Peery, D.Simerly'Ini+isis)

Prepared By D- Peery Ck'd By DSS

SPECIMEN CULLECTIUf .06PROJECT NAME: JACKSONV I LLE/

LOCATION: , OFFSITE , ,Jacksonville,ArkLOCATION: , OFFSITE , ,Jacksonville,ArkansasPROJECT ff 480078 01 09 01

DATE'

TIME--01

74

n2

R5

8 8

SAMPLE # WH1752LFMS

Gizzard Shad

Dorosonia cepedianum

Gill Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method


^01 Prep Lab AU = Aust in CE = Cerritos DI = Directors ED = Edison FM s FAS MobneHK = Hiddlebrook PI = Pittsburgh SC = Santa Clara

_^_ Analysis Request: 01 = 2,3,7,8 TCDD 02 = Total PCDD/DF03 » Total and ISOMER specific PCOD/OF04 =

Film Roll No. 04 Frame No-

Sample Team D.Peery, D.Simerly(Initi.i?c'l


SPECIMEN COLLECTION G DATE8

TIME--01

74.

04

63

8 8PROJECT NAME: JACKSONVILLE/LOCATION- OFFSITE——-"• * — vii • - , •ii n iJacksonvil le,ArkansasPROJECT ff 480078 01 09 01

SAMPLE if- WH1753LFMS

Gizzard Shad

Gill Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method

LAKE DUPREESample Location Description

PI Prep Lab AU = Austin CE = Cerritos DI = Directors ED = Edison FM = FAS MobileHK = Hiddlebrook PI = Pittsburgh SC = Santa Clara

_^_ Analysis Request: 01 = 2,3,7,8 TCGD 02 = Total PCDD/DF03 = Total and ISOMER specific PCDD/DF04 '

Film Roll No. Frame No. 25

Sample Team D.Peery, D.Simerly^^mtials)


SPECIMEN CULLECTIUN J6 DATE-

TIME80

1 .

7

•i

0

0

65


OFFSITELOCATION:„ Jacksonville,Arkansas

PROJECT ff 480078 01 09 01

SAMPLE ff WH1754LFHS

White Crappie

Pomoxi's annularis

Gill Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method


PI Prep Lab AU = Austin CE = Cerritos 01 = Directors ED = Edison EH = FAS MobileMK = Middlebrook PI = Pittsburgh SC = Santa Clara

Analysis Request: 01 = 2,3,7,8 TCOD 02 = Total PCDD/DF03 = Total and ISOMER specific PCDD/DF04 =

Film Roll No. W Frame No. 26

Sample Team D.Peery, D.Sinierly(Initialsl


EJJ SPECIMEN CULLECTIUN •J6 DATE8

TIME'

0

1

75

03

60


LOCATION: OFFSITEJacksonvil le ,Arkansas

PROJECT ff 480078 01 09 01

SAMPLE f f M H 1 7 5 5 L F M S

W h i t e Crapp ie

Pomoxis a n n u l a r i s

G i l l nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method

_tl&_

NA

Age

Sex

50 qr Weight1 5 - 5 cn1 Length

NA Girth

NA

NA


PI Prep Lab AU = Aus t in CE = Cerritos DI = Directors ED = Edison FH = FAS Mobi leMK = Middlebrook PI a Pittsburgh SC = Santa Clara

01 Analysis Request: 01 = 2,3,7,8 TCDD 02 = Total PCDD/DF03 = Total and ISOMER specific PCDD/DF04 =

Film Roll No. Frame No.04 27

Sample Team D.Peery, D-Si 'mer ly( I n i t i a l s )

Prepared By D- Peery Ck'd By DSS/ T - i- + < -

03 SPECIMEN COLLECTION JG DATE'

TIME'0

0

7q

00

7

0

8 8PROJECT NAME .'JACKSONVILLE/LOCATION- OFFSITE——•"—' " •J" • •, , • i ^ A iJacksonville,ArkansasPROJECT # 480078 01 09 01

SAMPLE # WH1756LFMS

M h i t e C r a p p i e

Pomoxis annu la r i s

Gin nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method


PI Prep Lab AU = Austin CE = Cerritos DI = Directors ED = Edison FM = FAS MobileMK = Itiddlebrook PI = Pittsburgh SC = Santa Clara

_^_ Analysis Request: 01 = 2,3,7,8 TCDD 02 = Total PCDD/DF03 = Total and ISOMER specific PCDD/DF04 =

Film Roll No. Frame No-W 28

Sample Team D.Peery. D.Simerly('"•'tials)

Prepared By 0. Peery Ck'd By DSS(Initials)

SPECIMEN COLLECTia. .06 DATE-

TIME8Q0

79

00

70

8 | 8PROJECT NAME: JACKSONVILLE/

LOCATION: , 01:FSITE . .Jacksonville,ArkansasPROJECT ff 480078 01 09 01

SAMPLE ^WH1757LFMS

Bowfin

Ami a calva

Gill Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method

_UA_

NA

NA

NA

Age

Sex

370 qr Weight

53 .2 ^ Length

NA Girth


PI Prep Lab AU = Austin CE = Cerritos 01 = Directors ED = Edison FM = FAS MobileHK = Hiddlebrook PI = Pittsburgh SC = Santa Clara

_0_ Analysis Request: 01 = 2,3,7,8 TCOD 02 = Total PCDO/DF03 = Total and ISOMER specific PCOD/DF04 =

Filni Roll No-

Sample Team D( I n i t i a l s )

04

-Peery,

Frame No-

D.S imer ly

29 & 30

Prepared By D. Peery Ck'd By DSS(Initials)

SPECIMEN COLLECTIUl _OG DATE-

TIME'01

70

00

70

8 8PROJECT NAME: JACKSONV I LLE/LOCAT I ON: OFFSITE

„ Jacksonville,ArkansasPROJECT if 480078 01 09 01

SAMPLE H- WH1758LFMS

Blue Catfish

I c t a t u r u s furcatus

Gill Nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method


01 Prep Lab AU = Austin CE = Cerritos DI = Directors ED = Edison FM = FAS MobileHK = Biddlebrook PI = Pittsburgh SC = Santa Clara

_m_ Analysis Request: 01 = 2,3,7,8 TCOO 02 = Total PCOO/OF03 = Total and ISOMER specific PCDD/DF04 =

Film Roll No. Frame No.Ot 31

Sample Team D-Peery, D . S i m e r l y( I n i t i a l s )

Prepared By D . Peery Ck'd By DSS(Initials)

SPECIMEN COLLECTIL LOS DATE-

TIME'0

1

7

n0

?7

n8 8

PROJECT NAME: JACKSONVILLE/

LOCATION: , OFFSITE , „,, Jacksomnlle.ArkansasPROJECT ff 480078 01 09 01

SAMPLE S WH1759LFMS

piiio Catfish

[c ta lurus furcatus

Gin nets

Dry Ice

Specimen Type

Species

Collection Method

Preservation Method


PI Prep Lab AU = Austin CE = Cerritos DI ° Directors ED = Edison FH = FAS MobileHK. = Kiddlebrook PI = Pittsburgh SC = Santa Clara

_M_ Analysis Request: 01 = 2,3.7,8 TCDD 02 = Total PCOD/OF03 = Total and ISOMER specific PCDD/DF04 =

FiTn Roll No. t)4 Frame No- 32

Sample Team O.Peery, D.Sjmer1y_[ In i t ia l s )

Prepared By P. Peery Ck'd By DSS(Initials)

APPENDIX B

STANDARD OPERATING PROCEDURE

ITAS-SPECIAL ANALYSIS LABORATORY

TITLE:

EXTRACTION METHOD FORBIOLOGICAL SAMPLES

SOP NO: SALS 09DATE INITIATED: 01/15/86REVISION NO: 3DATE REVISED: 10/23/87PAGE 1 OF 5

PREPARED BY APPROVED BY DATE QA CONCURRENCE DATE

^^•^^ ^^^< ^//^ c^i-Q^w- ^sr

/ ^1.0 PURPOSE

This analytical method describes the procedure used to extractdioxins and dibenzofurans from biological samples.

2.0 APPLICATION

The biological tissue sample is spiked with an internal/surrogatestandard mixture and blended with dry ice. The sample is jar-extracted with acetonitrile and concentrated by standard K-Dtechniques in preparation for cleanup steps.

3.0 REFERENCES

3.1 RCRA SW-846, Method 8280 (September 1986 revision)

3.2 EPA Method 613 Federal Register; Vol. 49, No. 209;43368-43373.1984

3.3 Bruailey, W. C. , J. A. G. Roach, J. A. Sphone, P. A.Dreifuss, D. Andrzejewski, R. A. Niemann, and D.Firestone, 1981, "Low-Resolution Multiple Ion DetectionGas Chromatographic—Mass Spectrometric Comparison ofSix Extraction—Cleanup Methods for Determining2,3,7,8-Tetrachlorodibenzo-[-dioxin in Fish", J. Agric.Food Chem. 29, 1040-1046.

3.4 Harless, R. L., E. 0. Oswald, and M. K. Wilkinson,1980, "Sample Preparation and Gas Chroniatography--MassSpectrometry Determination of 2 ,3 ,7 ,8-Tetrachlorodibenzo-p-dioxin", Anal. Chem. 52 ( 8 ) , 1239-1245.

SOP NO: SAL309DATE INITIATED: 01/15/86REVISION HO: 3DATE REVISED: 10/23/87PAGE 2 OF 5

4.0 ASSOCIATED SOPS

4 . 1 ITAS-SAL SOP No. 312, "Caustic and Acid Cleanup".

4. 2 ITAS-SAL SOP Ho. 1001, "Safety Procedures".

5.0 PROCEDURE

5.1 Reagents

5 . 1 . 1

5 . 2

5 . 1 . 2

5 . 1 . 3

5 . 1 . 4

5 . 1 . 5

5 . 1 . 6

5 . 1 . 7

5 . 1 . 8

Cautions

5 . 2 . 1

5 . 2 . 2

Spiking standard solutions; for isoroerspecific and totals analysis, samples will bespiked with C^-2, 3 , 7,8,-TCDD internalstandard at a concentration of 500 ng/ml and"d^^iS^ ,a-T!CDD surrogate standard at aconcentration of 100 ng/ml, plus ,,C-labeledPenta CDD, Penta CDF, Hexa CDD, Hexa CDF,Hepta CDD, Hepta CDF and Octa CDD, at aconcentration of 500 ng/ml and all in thesame isooctane solution.

Sodium Sulfate - ACS, granular, anhydrous.Prepare by heating to 450-C for 16 hours.After preparation, store in glass jars atroom temperature.

Dry ice.

Acetonitrlle; UV grade.

Methylene chloride, pesticide quality orequivalent.

Hexane; pesticide quality or equivalent.

Acetone; technical grade.

Toluene; pesticide grade or eguivalent.

Samples received for this preparationprocedure are of unknown composition, but maybe of potentially carcinogenic, mutagenic,toxic or in other ways hazardous.

It is mandatory that the initial weighing ofthe samples, addition of isotopically labeledcompounds and mixing of the sample beperformed inside the designated dioxin hoodin the high hazard laboratory.

SOP NU; SAL309DATE INITIATED: 01/15/86REVISION NO: 3DATE REVISED: 10/23/87PAGE 3 OF 5

5 . 0 PROCEDURES (CONTINUED)

5 . 2 . 3 Personnel involved in this sample preparationprocedure shall be thoroughly familiar withlaboratory SOPs on the processing of highhazard samples. (See ITAS-SAL SOP No. 1001,"Safety Procedures".)

5.3 Glassware - All glassware and stainless steel (blendercups, spatulas, etc.) used in sample preparation andcleanup procedures are solvent rinsed. The solventsused are acetone, toluene, methylene chloride andhexane, in this order. Allow to air dry in a hood.

5.4 Equipment and Materials

5 . 4 . 1 Blender.

5 . 4 . 2 Amber colored glass jars with teflon linedscrew caps - 240 al.

5 . 4 . 3 Platform shaker.

5 . 4 . 4 Snyder columns, three ball macro.

5 . 4 . 5 500 ml round bottom flask.

5 . 4 . 6 Heating mantle.

5 . 4 . 7 Concentration device; nitrogen blow downapparatus, N-EVAP.

5 . 4 . 8 Glass funnels, short stem.

5 . 4 . 9 Filter paper, Whatman No. 4 or equivalent.

5.4. 1 0 Analytical balance.

5.4.11 Separatory funnel; 125 ml volume.

5.5 Extraction

5 . 5 . 1 Prepare designated dioxin hood as instructedin laboratory SOP for processing high hazardsamples.

5 . 5 . 2 Weigh out 10 grams of the sample and transferto a stainless steel blender jar.

SOP NO: SAL309DATE INITIATED: 01/15/86REVISION NO: 3DATE REVISED: 10/23/87PAGE 4 OF 5

5.0 PROCEDURES (CONTINUED)

5 . 5 . 3 Spike sample with 100 ul of spiking solution,containing both internal and surrogatestandards, adding the solution to severalsites over the surface of the sample.

5 . 5 . 4 Add 100 grams of anhydrous granular sodiumsulfate into blender jar and blend mixturefor approximately 1 minute.

5 . 5 . 5 Add 50 grams of dry ice and blend until thesample is thoroughly powdered.

5 . 5 . 6 Transfer powdered sample into 240 ml ambercolored glass jar. (The screw cap for thisjar must have a teflon liner.) Rinse blenderjar several tines with acetonitrile. Therinsings plus enough additional acetonitrileto make up 150 ml are then added to the glassjar.

5 . 5 . 7 Shake mixture on electric platform shaker for2 hours.

5 . 5 . 8 After shaking, filter mixture through glassfunnels lined with No. 4 Whatman filter paperinto 500 ml round bottom flask. Rinse theglass jar 3 times with small amounts ofacetonitrile, adding these rinsings to flask.

5 . 5 . 9 Concentrate extract volume down toapproximately 5 ml in the round bottom flaskusing Snyder columns and heating mantle.

5 . 5 . 1 0 Transfer the concentrated extract to a 125 mlseparatory funnel. Rinse flask several timeswith acetonitrile, then several times with atotal of approximately 15 ml of hexane andadd this to the separatory tunnel. Proceedto caustic and acid cleanup of extract, SOPNo. SAL 312.

SOP NO: SAL309DATE INITIATED: 01/15/86REVISION NO; 3DATE REVISED: 10/23/87PAGE 5 OF 5

5.0 PROCEDURB (CONTINUED)

5 . 6 Cleanup of Glassware

5 . 6 . 1 After use, glassware is solvent-rinsed withtoluene and methylene chloride. Wash withdetergent and rinse with copious amounts oftap water and several portions of distilledwater. Place glassware in oven and heat to400'C for 30 minutes. Remove from oven whencool and store in clean environment.

I INTERNATIONALTECHNOLOGY

I CORPORATION

FIBAL DIOXCT REPORT

TOR


VOLUME I

KEPORT A11D DATA SUMMARY

PREPARED BY IT ABALYTICAL SERVICES

KBOXVILLE, TEBBESSEE

JOLT 26, 1988


Case Narrative

Ten (10) fish were received on 07-08-88 for the analysis of2,3,7,8-TCDD (please see Table 1 ) . The samples and blankwere spiked with an internal standard/surrogate mixturecontaining 5. 0 ng 13C-2 , 3 , 7 , 8-TCDD and 1.0 ng :i7Cl-2,3 , ' J , 8 -TCDD. The samples were extracted utilizing ITAS developedprocedures. Sample extracts were analyzed using a modifiedversion of the,EPA reference method described in "RCRA SW-846, method 8280," revised September 1986.

sample Preparation

Fish samples (fillet only) were ground and homogenized. Ten(10) grams of the sample and ten (1 0 ) grams of sodiumsulfate (a blank) were weighed into separate jars. Thesamples and blank were spiked with the internal standard/surrogate mixture and allowed to stand overnight foreguilibration, followed by an extraction utilizing ITASmethodology.

Sample Cleanup

To aid in the removal of chemical interferences, the samplesand blank were first treated using separatory funneltechniques found in Option C of the U . S . Environmental Pro-tection Agency, Region VII Protocol for "The Determinationof 2,3,7,8-TCDD in Soil and Sediment," September 1983 revi-sion. Extracts were washed with 20% KOH and distilled waterfollowed by three concentrated HySO^ washes. Further clean-up consisted of two steps of column chromatography, Thefirst step involved a neutral alumina column while thesecond was a dual column system utilizing acid-modifiedsilica gel followed by neutral alumina. Final extracts wereconcentrated to near dryness and raised to 50 p.1 with aisooctane.

GC/MS Analysis

Isoner Specific TCDD - The sample extracts were analyzedusing HRGC/HRMS scanning in the selected ion monitoring modefor enhanced sensitivity. The column used for this isomerspecific analysis was a 60 m SP-2331 fused silica capillarycolumn. Before acquisition of the sample data, a sevenisomer performance mixture containing the six most closelyeluting TCDD isomers was run.

In addition, a five point calibration plot was run intriplicate. The mean response factors obtained from thisfifteen point calibration were used for all subsequentcalculations (see Table 2 ) . The shift standard, analyzed onthe same day as the samples, produced a response factorwithin 10% of the fifteen point curve for TCDD (please seeTable 3 ) . Accuracy of the method is obtained by therecovery of ^Cl-TCDD versus ^C-TCDD.

GC/MS Results

Isomer Specific TCDD - The results for the isomer specificanalysis, shown in Table 4, are reported in ppb. Adetection limit is calculated from 2 . 5 times the signal inthe area of the elution of ^C-TCDD whenever a samplecontains no detectable 2,3,7,8-TCDD.

QA/QC

Table 5 lists the results of the QA/QC samples. In allcases, precision and accuracy are within the limitsestablished for acceptance of dioxin/dibenzofuran data.

sm(bwlO)

APEEBDIX A

CROSS REFEBHICE U:ST

TABLE 1

CROSS REFERENCE LIST

IT SAMPLE

BB0546

BB0547

BB0548

BB0549

BB0550

BB0551

BB0552

BB0553

BB0554

BB0555

# CLIENT

WH1750

WH1751

WH1752

WH1753

WH1754

WH1755

WH1756

WH1757

WH1758

WH1759

SAMPLE

LFMS

LFMS

LFMS

LFMS

LFMS

LFMS

LFMS

LFMS

LFMS

LFMS

MATRIX

BUFFALO FISH

BUFFALO FISH

SHAD FISH

SHAD FISH

CRAPPIE FISH

CRAPPIE FISH

CRAPPIE FISH

BOW FIN FISH

CATFISH

CATFISH

sm(bwlO)

TABLE 2

INITIAL CALIBRATION SUMMARY

TCDD/TCDP


Date

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-02-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

11-03-87

CC1CC2CC3CC4CC5

Instr.ID

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

70-250S

Mean

37

61220

Sol.ID

CC1

CC1

CC1

CC2

CC2

CC2

CC3

CC3

CC3

CC4

CC4

CC4

CC5

CC5

CC5

RF Used (x) =

% RSD =

Cl

pg/nipg/îpg/î

NatTC

0.

0.

0.

1.

1.

1.

1.

1.

1.

1.

1.

1.

1.

1.

1.

1-

7.

ive:DD

952

959

924

05

03

06

07

10

06

02

02

07

13

17

20

05

3

10 pg/ul50 pg/iil

loo pg/îl1000 pg/(xl3000 pg/|il

Measured RFNative

TCDF

1.88

1.86

1.91

1.99

2.03

2.04

2.10

2.33

2.28

2.09

1.82

2 .30

2 .42

2.63

2.74

2 .16

1 3 . 0

Natives

%

0.

0.

0.

0.

0.

0.

0.

1.

0.

0

5

ogate-TCDD

931

923

846

956

951

948

974

03

949

.945

.1

KPPSSDJX C

ISOMBB SPHGIFIC COH'nBniBG CALIBRATIOH SUMMARY

TABLE 3

ISOMER SPECIFIC CONTINUING CALIBRATION SUMMARY


BATCH 1195

Date

07-17-88

07-17-88

07-17-88

07-18-88

07-18''-88I

07-18-88

Instr.ID

70-250S

70-250S

70-250S

70-250S

70-205S

70-250S

SolID

PC

CC1

PC

PC

CC1

PC

Measured RFNative SurrogateTCDD —Cl-TCDD

1.08 1.00

1.08 0.972

RatiNativeTCDD

1.03

1.03

o rrleas/Mean)Surrogate-'Cl-TCDD

1.06

1.03

TCDD IsomerResolutionPet. Valley(Applies ForPC Only)

7 .9%

5 . 4 %

6 . 8 %

7 . 4 %

Solution ID Codes:

PC = Performance check solutionCC1 = Concentration calibration solution #1 = 10 pg/ul

sm(bwll)

APPEHDIX D

ISOMER SPEGrFTC DATA SUMHABI

fABLE 4

2,3,7,8-TCDD RESULTS

Lab: IT/SAL

Case No; Jacksonville Of fs i te

Batch/Shipment No. 1195

Column: 60 Meter Sp-2331

Instr. ID. 70-250 S

Sample

Client

UH1750LFMS

"H1751LFHS

UH1752LFMS

WH1753LFMS

UM1754LFMS

MH1755LFMS

WK1756LFMS

WH1756LFMS

yH1756LfMS

KH1757LFMS

UH1758LFHS

UK175tLFHS

RB

a Corrected

RB - Reagent Blank FB - Field Blank

0 • Lab Duplicate FO - Field Duplicate

BS • Blank

MS • Matrix

MSO - Matrix

»

IMS

BB0546

BB0547

BB0548

BB0549

BB0550

BB0551

BB0552

BB0552HS

BB0552MSD

BB0553

BB0554

BB0555

BLK1195

for contributi

Spike

Spike

Spike Duplici

Uet Ut.(q)

ND - Not Detected

DL • Detection Limit

Aliouot

10.0

10.0

10.0

10.0

6.76

6.46

10.0

10.0

10.0

10.0

10.0

10.0

10.0

ion by native

ate

PPB T

Meas.

O.Oil

0.25

0.0099

0.48

0.046

0.029

O.OS1

0.14

0.12

0.01!

0.06S

0.23

ND

TCDD;

OL Date

(0.0019) 07-17-88

I:DD GC/MS Ana

07-17-88

07-17-88

07-17-88

07-17-88

07-18-88

07-17-88

07-17-88

07-17-88

07-17-83

07-17-88

07-17-88

07-17-88

0.9% of m/l 322 subtracted.

lysis

Time

13:46

14 :19

14:51

15:26

1'.;17

1*:32

17:05

19;20

19:54

17:40

18:13

18:46

13 :11

Ret. Ion

320/322

0.83

0.82

0.80

0.83

0.75

0.87

0.75

0.81

0.79

0.85

0.72

0.76

.»t'"nd...332/334

0.76

0.80

0.85

0.77

0.75

0.80

0.75

0.72

0.80

0.82

0.80

0.77

0.81

PpB Sl

Meas.

20.2

20.7

21.5

23.4

21.2

22.4

20.8

22.3

21.6

20.3

20.9

19.5

21.9

Ji-rogate

» Acc'v

101

103

108

117

10*

1 1 2

104

1 1 2

108

102

104

98

1 1 0

320

66.25

621.84

27.71

1402.34

100.38

53.83

58.79

196.88

169.39

36.98

155.88

840.46

Relatf

322

79.58

759.77

34.42

1680.30

133.36

61.65

78.27

244.24

213.71

43.54

216.92

1098.60

ve Ion Abur

259

50.55

601.35

25.96

1304.06

101.87

46.35

61.77

189.85

217.40

31.08

156.48

707.37

ufance

32Sa

421.28

520.59

607.16

668.79

713.10

628.22

410.04

327.93

296.38

551.54

517.21

744.74

620.72

332

956.36

1188.69

1369.55

1311.88

1521.37

1314.14

894.75

653.61

642.44

1292.28

1164.67

1753.62

1343.44

3 '.

1^1.34

1476.60

1617.11

1711 .61

2028.83

1615.44

1194.26

901.89

805.56

1580.24

1456.58

2<.. .I*

1655.53

sm(bu14)

APPBBDIX E

QA/QP SUMMARY

TABLE 5. QA/QC REPORT i

Project Name Jacksonvi I Ie Offsite______Code ITFK25558___ Surrogate Percent Accuracy

Batch Mumber 1195______________________________MRHS Isomer.

Sample Matrix Fish________Extraction Method Special_______ ^ec1 lc

Report Date 08-12-88______________________________ Muntier of Data Points = ____17____

BC/MS Run Date CIsomers) 07-17-88__________________ Mean Percent Accuracy = 107%

Range' = 98-117%

Sample » BB0552_______

2,3,7,8-

Precision of Duplicates TCDD

Spike Oup. Value (a) » 0 .12

Spike Value (b> = 0.14

Precision = |a-b| x 100X = 15.4%

a»b

2

EPA Rang;- = 50%

^ 2,3.7,8-

Accuracy of Spike TCDD

Observed Spike Value (b) = 0.14

Orig. Value (a) s 0.031

Spike Levrl (c> = 0.10

Accuracy = b-a x 100% = 109X

c

EPA Range = 60-140%

EPA Range fo; surrogate percent accuracy is 60-140X for 2,3,7,8-TCDD only.

sm(bu14)

•"I '•

INTERNATIONALTECHNOLOGY

I CORPORATION

FIBAL DIOXCT REPORT

FOR

JACKSOHVILLE OFPSITE

VOLUME 11

IBITIAL ABD CONTIBUIBG CALIBRATIONS AHD DATA

FREPAEED BY IT ANALYTICAL SERVICES

KBOXVILLE, TEHBESSEE

JULY 26, 1988

ISOMER SPECIFIC IHITIAL CALIBRATION

11-03-87

•111^15 £-NO'rS? 12.34PH53S (uO Sus^OSTD;F: 1 . 31S.373£ K . 313.8378 U 321,3349 ^ 32?.3e4? N . 331.3363T.;.:t^lJLSTD I - 18PG/ULRUN ^

tnr-LE 1 INJECTION 1 G R O U P 1 CHANNEL 3t5. 94.

AREA RETENTION TIME

i 1. &St'?A'?E*<i3 i t ;29:37

.2 S. &925S2E*®! »:3a:i»6

AMPLE 1 INJECTION 1 5ROUP i CHANNEL 317.9»

A R E A RETENTION TIME

1 2. 17748»E<-»3 i.'i:29:37

£ 1. 137177E-162 »:3i»:»&

3 3. lS7?53E»ei B:31:42

'U1@£I5 £-NOV-3? 1^34?8-250S CEI^) S^ISOSTD;? 1 ^ 249,163£ B ^ £42,9343 ^ £53.9c98 [ 30£,965£ E ' 303.S93?'.;.:;t UL STD I - 19PG/UL.RUH #1ir,'.'i

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l Q ^ C S l , n , G l , hOCI ' ^ = 214,93 T = ^ 4 B 4M.?^-

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1 1. 18'?3B2Ei-<il »:27:'»A

2 8.73283»E*S£ »:29:'tl

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1 1. 14.9A4SE-93 a :29 :41

?MFLE I INJECTION 1 GROUP 1 CHANNEL 331.9t

AREA RETENTION TIME

1 4. 8l»'H72E-n»3 «: 2A: 39

2 5. 18A1S7E**! i>:31:t i

•MFi-E 1 INJECTION 1 G R O U P i CHANNEL 33S. 93

AREA RETENTION TIME

1 fe. i89153i»E*t3 «: 24: 39

2 5. 3931S7E*B1 i?:31:i?l

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AREA RETENTION TIME

1 2. <;&239&E»iiiS »:2&:il«i

: 1 lS3*37E*ai ii..31:iiil

,°LE i IMJECTIOri l ^fiOJr i ::•; ••.;>IKEL 33'3 °3

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2 c a"il-^^lE-»-'-'-l ^ 'I ''"

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AREA RETENTION TIME

1 &. a3173.i»E-i-<ll »:27:ii7

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1 4. S&*57lBE*a3 » :2&;39

2 4. 3593ME-HM <i:31: '»t

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1 5. a»l»178E»e3 8:26:39

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2 q.. 7«i83&5E*<ll <i:3a:llii

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@ /^ 162,16 1=23^ 42:^

.BSJ 31,11,61i © ^ = 136,75 T = 2 3 ^ 7

a|_______i_,_______i98,L 31,11,61 ^ ^ 1,

47.6S® f f l = 166,85 ]-- 23^47

r // •

ffl= 171,57 T=23 " t 7 ^ 43i

198J 31,11,61(g)^= mi 1=23^6

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MllSUl .G l^ = 557,81 T = 2^5

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; '•..O S 1 , I 1 , G 1

= 1CT.53 1=23 :45

2345 23:3§ SS^S E^^B ^15 24:39

'm 13-JH W MM (EI*5;' ! ^ 248,9378 B' 242,3349 C' 258,9298 D' 382,9652 I'- 383,9816.•; 2 UL 7-MR m

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HS1, !1 ,G1 ,@1^-- 1738.83 T = i 3 ^ 4 4

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23:15 £3:^ 23:45 £4'i 24:15 24^

^ <9 - an A/^ •7-/?-1"

% 13-JI-SS 14^1 ?e-258S (EI^3 Sus^ISOSTO^ 249,3373 B ^ S42,3349 C ^ £58,3233 ^ 38S,3652 E ^ 383,9816

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= 360,53 T^45

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DATA

BATCH 1195

TCDD ISOMER SPECIFIC

DATA SUMMARY

IT SAMPLE «_____^__- DATE ANALYZED:,

TIME ANALYZED:

^et 2,3,7,8-TCDD Detection Surrogate Surrogat>Weight/ Con^. Limit 320/322 332/334 Measured PercentVolume n<t .PPtr' npt; nq ppb opt ro.67-0.90) (0.67-0.90) (PPb) Accurac-.

Area Area Area Area Area Area*-3.32 334 320 322 259 _m

-,-,:-.- , . - - • " - ~^~2^ Z^^ ^c'•~><s~

COMMENTS: /^,/y /y ^ ^••,•7 ^^ ^^ /.-> ^y<

'D - Not DetectedS - Native TCDD SpikeD - Duplicate (Intralab)

Corrected area 328 [328 - (0.009 x 3 2 2 ) ]

Checked By=__^^__2l^l^-

Vi\

(\

ft^i

.Jj •'•'!•

ex.* oi~« »"^~» ——^-

r*--- — • z« •-"—- =:

—rS- CJJ , ••"•-I -I~

1 -———- ^

t 'n'". --;::; .-"- i. •I Ti"'" l^f'.r I"-' i '.O V.»~~JI ~~\t ' ""l ""•.J •i———" --M-

. \

^ -

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<£-«-:•\J •€==:• -r--:-<->. *—' -' '^s-''<S •—• c' «

•«-t - -:=*"i-ii

••-:•<-««ucr-•ix:-•=^ ——=============C»-JI•2S "•~-~B

<————1

+ •c•="•———< •=•-•

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W 17-JUL-8813^4S ?6-25eS i:E!^5 S^LSOSTD;' 1 K ' 31S,83?8 L ' 321,5548 B' 327,^ ^ 331.33S8 0' 333,9333al^TI'f'E TCDO, 3?i;L, ffi 13C-TCDD

3

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fl = 66,£5\

fl = /•'3,5SR^ 9,:33£5

\-- 422,66\ - - '• -

^

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^Ul^ 1251,34 T = 23:44' •i-'/i1 \ 8,7643

_>' '•_


DATA SUMMARY

IT SAMPLE f ^;<^—,-^/7DATE ANALYZED:

TIME ANALYZED: / ' - / . / /

Net 2,3.7,8-TCDD Detection

Weight/ Cony. Limit 320/322 332/334y01""16. n<7(J3pB pp<- ncr ppb ppt (•0.67-0.901 10.67-0.901

-• "- C^ ,•••'. '

SurrogateMeasured(PPb>

^. 7

Area332

Area_334

Area320

c^t, y /

Area322 „

^^"^

Area259

Area*328

COMMENTS;

'.0 - Not DetectedS - Native TCDD SpikeD - Duplicate (Intralab)

Corrected area 328 (32S - (0.009 x 3 2 2 ) ]

Checked By: ^^^ 7,/^^

'! IS'II 'IS^WHSIJ 381 «3 H\

mm ^3 m'm ••Q m'^ ••••! wî ••s m^ ^ws w^ww-i\ t

^sî'^- rv^ •)y

^s- ^y < c^ J/ô


DATA SUMMARY

IT SAMPLE < ^'6-^-y DATE ANALYZED: ^^-^

TIME ANALYZED: /. S-/

Net 2,3,7,8-TCDD Detection Surrogate SurrogateWeight/ Cope. Limit 320/322 332/334 Measured Percentvolume M fab pp» nq ppb ppt f0.67-0.90\ f0.67-0.90L fPPb) Accurac\

rea Area Area Area Area Area*——— - 2-i 320 322 259 328

-/v^ tjd2_iL 77,7/ ;c/ Js-^ ,^.^,

COMMENTS; ^ ; , , .3<,'-y ^ ^-^ /3 '

0 - Not DetectedS - Native TCOO Spike0 - Duplicate (Intralab)

Corrected area 328 (328 - (0.009 x 322 ) ]

Checked RV. ^/^

+ r-.c.~*~» rxJ -c .

A ^^•^l.- - 'C- l <-€:• IC-"-" f--- €-«-? "C__•——^ OC« ~---S f~~

'—_ CO" I———

•——- CS? ___ •3C:«-—__ <=-' (30 OOi

<.«-• -»^>- --—i— r«L:» •CJTI

S-c«<-•_• '- -1-«=»- •zss'€£:• I

m-"c-an

-——)• <33i-- CJO

^r>c«£*3i

%r-»J__ «->•^^•L_,_« •———•

cs:« <-•-*•!.•>_> •~^3i PS ^

•C-f-H 1" ^: C- \

SS 9 c,^l^

U•ftA '•'"

^

» 17-J1JL-S3 14'51 ;'H58S (Eh5 SusW..•' 1 ^ 313,83?3 U 321.S348 B ^ 32?,3W ^ 331.936S 0' :B3,333SH t ' H f l T I ' / E T e [ D , 3 7 C L , W D 1 3 C - T C D D

' / ^/ , .«/ ' • "

3ELC S1,I1,C1 i.. Y : 33:^; C2^ / \

3BJ 31,11,01 ^1 T = ^: , '/ i''' 'i^^_y\___

.88 ,LS1,I I ,51^34,^ T.^

.§@JS!,I1,G1; ;


DATA SDHMARy

IT SAMPLE »__i;%/" $""' /9 DATE ANALYZED:_____7- / ^•'.-^

TIKE ANALYZED:____/^~ ' ^ {:

NetWeight/Volume

2,3,7,a-TCDO DetectionCone. Limit

rcr^D&.Dpt nq ppb opt

Surrogate Surrogate320/322 332/334 Measured Percent

f0.67-0.90> (0.67-0.90) _fppb) Accuracy

^-^'L /.7.-77 ,yf,'/ ,/•</'-

Area332

Area*328

Area334

Area320.

Area322

Area

•/: /, /"/'// l'/^ ^'/ //•• S'"'- J/0

COMMEMTS: / ^ / ' ' ' ' /^ •S f > ' i / ' f ' ' : ' l ' L -'^ ^l^

SD - Not DetectedS - Native TCDD SpikeD - Duplicate (Intralab)

•corrected area 328 (32S - (0.009 x 322)]

Checked By: ^^} ••7-/^'P'

i^c- .^-.y ^ 7 -• /

(5^ ' ^ p-/?-^

3 17-.JIJL-3S 15^6 ?8-258S (EI») SUS^ISOSTD^ 313.897S L ^ 321,S94@ t 327.SM7 ^ 331,336S 0' 333,93;I BB8549 18G FISH

N^C 31,11,01

17-11-S315^6 78-256S (EH^ mm [.••• 3E1.3948 B' 327.SS47 H: 331,9368 0^ 333,S33S

COD, 37CL, M 13C-TCDO

yHH C S l , I l ^ l f j ; 13 T;23 ;47

11/\.

,MJ 3 1 , 1 1 , 0 1 fl.^i y.-s^ .2 -

/ \- '^/--" _____.'' '-^,______/ \._____________________

^OS1,I1^, i;u,6i T .

^/Ef 8,7665


DATA SOMKARY

IT SAMP3

NetWeight/

Area. 332

/^/. 3^

-E <

2,3

P<7

(

^?^5-^

,7.8-TCDDCone./055> ppf

y.^yfa

Area-32A

^^S--^3

7

DetectionLimit

ng Dob not

Area320

/C€>.'^y

E

I

320/322r0.67-0.901

^.^

Area322

/33.

>ATE AN?

THE ANA

332(0.67

£>•

J&

iLYZED:

.LYZED:

/334-0.90)

7'3'

Area

/(5/5

- ? - / & - -

^ ' - / , / ~ ^

SurrogateMeasured

<DDb)

31-^

Area*-328

1 ;;> 77-?, /^

^^r

Surrogat'PercentAccurac'.

/;<%.•'

COMMENTS:

. " D - Not Detected5 - Native TCDO SpikeD - Duplicate (Intralab)

Corrected area 328 [328 - (0.009 x 3 2 2 ) ]

C.ec.ed By: \^

IS'II ' IEO^HHSIJ 3^'3 (i]nigno]]ii esseag in'

W^ ••] m'W ^ S636'8S3 ^ 3 6t£6'3t3 ••3 SCT3 ^QISOSI'^S M3) S8S3-8^'I^I 88-if-EI f!

^t-^/-^ / z. ^ ^^9-, -<i ^ -' ^^

"M 1S-J11-331-M7 PH58S (EMU 321.SWJ [ SEW N' 331,3363 0' 333,3333

i?CL, M 13C-TCDD /

y ^ ^^W ft /-^ 191,8? ].^ '....l;

-/' \ si^-a ^ - J' \---

i 3 H . K S l , I l , 0 1 © ^. 1^^ T = ^

91______^ V____•M^S1,I1,01 D ; 133^ T : a ; 4 3

i i — -,—-..-,— r i i i i — i r T i l — I r ——r- i » i ( i i

^3 I! S l , I I ,i31 ^= ?M,39 T = £ 3 ^ - t: / \ ,..7/5."' fi

ai _ _ _^ ^ ^^,99 J 31,11,01 ^ 1^1^ y:^

\

8S«0 31,11,61y il LULUIV.' I L.' 71.

/R = 'W 5-


DATA SUMMARY

IT SAMPLE f ^/'u>~•,'/ DATE ANALYZED:

NetWeight/Volume

(-.>/{-

Area

,' ^ ; /^/ -/'

2,3.C

P?/<r"^

•"?.-;7. •^Area

7,8-TCDD^n^.DDbippt--ryi•^ ^

DetectionLiait

ncr Dob oot

Area320

TI

320/322(0.67-0.90}

^7

Area322

^ --^'

ME ANALYZED;

332/334(0.67-0.901

rr>.•^'

Area259

; -- -•

/^ • J;

Surrogat<Measure<

<DOb)

.^.'-/

^

e Surrogati3 Percent

Accurac'.

/•/J>

Area*328

,/-y ^ --

A-^ A '^'7 /••-' ":-''''COMMENTS:

'0 - Not DetectedS - Native TCDD Spike0 - Duplicate (Intralab)

Corrected area 328 [328 - (0.009 x 322 ) ]

Checked By: /^^ -7^^f-

•\ lO'll 'ISS^NMSIJ 39t'9 IS6933 Tl ;

m'^. m'i.K ••\\ eiwsie ^ OT'ses 'J mm ••]m^ W) Wi 3£'9188-lfir-^I ti

/f*/-^ /^'&';lc'<,<^ ^:1 ?"'-"

•3.:" .••=ra •:::;:• <•£::" "-a.:" C£:» :;..;; " 1001« *-- • « *-- • • ~- a •"•-1"» •" "B g "-„ » a "-- • • ~- a • ~-. « iCS^ * "~- • • ~-- • •—"~ &——»- •3^Jl

• • • • • • x a l BM Hliaiirl iMmRBl ••ruail U B B X B K B B I l u B k R I I B K l " •'—I

-

«-.-:• -•-)•-;•

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r-«a --1-—-•3=« --S3i

r-« . ---

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r-«^« --IP—•<• -"3S«

"

r';- -M ~'

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< -'• v: •~~' "or" i^~^'t^" C^J '«=• ••

"""'-v- - . - .sa r—" I-B ^ •- —— ' . <-•-)• 100

r'" ^^""^f ., -— • ) • • •3T:"

or •-1L:J" "-.J•f =!=• •——- »---:•.-^ ::: '= - r'0'

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•L^'•~--^'

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•=•?•—:' i-<"«. d ^—• .--> •-•-••:..-> cr:«

« - o"-«/ <c-«r" —ii • <:.-• •==.«

'1 '^-^ ^\^ ^ -

TCDD I60MER SPECIFIC

DATA SOHMARY

IT SAMPLE «__j^^ DATE ANALYZED ••________-£;

TIKE ANALYZED : / / , < '

Net 2,3,7,8-TCOD Detection Surrogate SurrogatfWeight/ COP•?- Limit 320/322 332/334 Measured PercentVolume Jig ^pb ppt- nq ppb ppt CO.67-0.90) /0.67-0.90) fppb) Accurac-.

rea Area Area Area Area Area*-——'- - 21 320 322 259 328

'//1'/-'' //7'-/:^.- ^->"/ ~?£r.^7 ^7 7 ? - . . - 7 . ^ .

D - Not DetectedS - Native TCOD SpikeD - Duplicate (Intralab)

corrected area 328 [328 - (0.009 x 322) ]

Checked By: ^L^£^_

TO- ML-8S 17^ ?B-253S (EM S IM• J ^ 246.33?S 8-' 242.3343 C ' ^SSS D' 38E.3E52 E' 393.9'

I-' ___<______A _L_._.____.___I..___-_W'-^ ''—"•.-.••.'.I •.——.•'-.',——.-,•,

m 17-JIH'S 1/^570-E5BS (EM Sus.'M1 ^ 313,3978 L 321.S348 B^ 327,8847 t^ 331.336S 0' 333,3338

;i t™"ETCDD,3?CL,M)13C-T(;;..'.

,£(i

338

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9.M

£i,i

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^ \.

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L, 1

61

53

78,6,7

4186

894

11^6,7-

1111.1

77i.1,'

,73

27518

,74" i'\

75

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T = £ 3

T = 2 3

T = 2 3 '

T = 2 3 ^ia"'i

T = £3;46

; 1 = 2 3 : 4 6

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:43

47

47

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————^-1.1 ''

A/-/ ' * L

/}^

Lc,'-

<1 1• "^'y

2;N5 ?4^3 2445 2^@ £4^5 £5^66


DATA SUMMARY

IT SAMPLE ( ,/W;: _ DATE ANALYZED:

NetWeight/

/A

Area-212

12J^1

2,3.7,8-TCDD( 9 .

nq/bpb ppt-

.•?75-^,>-<

7 " '

Area-13^1

%-/,5'/

DetectionLimit

na DDb Dot

Area320

//^

320f0.67

^.

^.sv

TIME

1/322-0.90) »

sy

Area322

ANA

332.).67

^

/^.-5

LYZED:

/334-0.90)

"

Area

/'/': ''••'

SurrogatMeasure..-(PPb) .

. 7 ^

^

^-;

id PercentAccurac\

//J •

Area*328

•'./??-9 Z

COMMENTS:

-0 - Not DetectedS - Native TCDD Spike0 - Duplicate (Intralab)

Corrected area 328 (328 - (0.009 x 3 2 2 ) ]

Checked By: /^/^ -7^ / f-'FS^

•,/-•—•—•\-^ r- • " • - • • • •"- '••• ---•.

13'U'IS^W3)lidS HSIJ 38155588

Mm ^ mx. ei^e'sis 'o fles'seE '•J SIBE'EOlSOSl^^S M33 Wi 83^1 SS-llT-^l

„/ -\TO

W S^3 W SH; 1 W• • • ' • • ' • • ' • ! I iiiti.i.ir •

weV^sî w;=^,aQ|i

1 i i i i I i ,—' ,..«ini -,Y T ^ i ^" . / ;i"'^.'''"' - I TQ'i'-r'u - 11 'i'7 i

" '^"1 . ^ ^ "X II IS H ii^ ^ ' / ' -

(-L^" i '

MS'-'l W, I^Î ' ' I ' -, ! f—;-

w iMS'e \^ ft ,N3=1 CT3 ^W^^

f:1 v i k' i '.'-K^VW^WS^-^Xt!S!-S^——————JlSiiiiMiiif-fia-tfT. „

\ ,;1 /8 ^H ^ G = I ra îg'îiii'eo

a ; G = l fiS-SSI ^'^fr^^S


DATA SUMMARY

IT SAMPLE « /-,',•-•'.' "•;'< ' ^ DATE ANALYZED ••_______

TIME ANALYZED: . ' ' - ' / . -.

NetWeight/

2,3,7,8-TCDD DetectionCong. Limit

no ^PP^ pp«- nq ppb ppt

Surrogate Surrogat*320/322 332/334 Measured Percent

(0.67-0.901 (0.67-0.90^ (ppb) ACCUC^C\

,' •'. .T'--

. /Z- /ft^

Area332

Area-224.

_ygS , L-

Area320

/(.L/ ?/

Area322

-,'7? ?/

Area259

^y?^'

Area*328

. 3'

COMMENTS:

D - Not DetectedS - Native TCDD Spike0 - Duplicate (Intralab)

corrected area 328 [32S - (0.009 x 3 2 2 ) ]

Checked By: fr^ ^/^

, ;^r---)--"-•^-

<<? 6 /^ ?-/ ^

£ P-JJL-8819^ 78-2583 (El*)- ' ' ' F' 305,8387 G ' 315,9419 H ' 317,93:

,•.__-''—,—— ..'„_______-___•__."». '"—"t.•-..—,« ———•j


DATA SUMMARY

IT SAMPLE f /•^^'-'•S'^ DATE ANALY2ED:_

TIME ANALYZED:_

7 / / -•'-

/^-•/'-g'

Net 2.3,7,8-TCDD Detection Surrogate Surrogat.Weight/ Conq. Limit 320/322 332/334 Measured Percentvolume ncr PD^ pot nq ppb ppt JO. 6-7-0.90) l0.67-O.SO) fPpb) Accurac1

Area Area Area Area Area Area*332, 334 3,0 322 259 328^320 322 _259

^/- -. ^•/ /'- ^•^ ^ -COMMENTS: A"" '-

SO - Not DetectedS - Native TCOD Spike0 - Duplicate (Intralab)

'Corrected area 328 [328 - (0.009 x 322) ] „

^1^ l^if^Checked By :_<//•" ' -————

• —.--, r- - .,,. ——,, )..

l a ' I I ' IS 3^041168'HSIJOBITSnfS^K

36i:6'8i£ 'i m'iK ••\\ m'w 's mm 'J siBe'ses ÔiSOSI^^S M33 SeS3-Bt BtÎ 38-TÎ »

^-l-fr/-^ roa/O' ^y , '"., ., ^2< - ^<. "t,.-"

f> s-^ / -<^ — c - '

^ . . . > ' •N3=1 CTSI ^lE'n'isoto

^ ^ B E 11 .1 / f'. I

^ , .•Is' \L 'I se'lssîg.i i ' isy^-1 -^C. •. ' -i ...-I Pr-'

» / --"/•

•J——'—c^

"c1^' \ / /^ Ef ^ 9 ^ £ 3 = 1 8e'9£ ' • ' • p

H I 18 1 ••-

••, I'-T 'T r .T '•, l / i'^'. bt 'i / i'^

L ^ 3 = l 88'IE î^ts^

iffiS'SÔ S3£6'1£^H ASS'a^l W^ ••-} W6!£ ^ 1 ÔISOSI^^ M35 WL \ 88-1PKI t£SK

TCDD rSOMER SPECIFIC

DATA SUMMARY

IT SAMPLE ( /\;-'C'"'''^'^/ DATE ANALYZED: ,7- ^,' .'j.'y-

TIHE ANALYZED: / y / .

Net 2,3,7,8-TCDD DetectionWeight/ Cone. Litnit 320/322 332/334Volume nq pvtv ppf nq Ppb ppt (0.67-0.90) CO.67-0.901

^

Surrogate Surrogat.Measured Percent

fppb) Accurac'

Area332

/ I W.i.: 7

Area..331

^A-/.-^

Area320

s /^. .yy

Area322

^.

Area259

/y7 ^

Area*328

COMMENTS:

-.D - Not DetectedS - Native TCDD SpikeD - Duplicate (Intralab)

Corrected area 328 [328 - (0.009 x 3 2 2 ) ]

Checked By:

_t- o.-.~? ESS"-•-• .rs.:" -•on CA:.*-':• c-n •3.:'

C2.:« ___ «=0i•:=-• "- i oo

•————• •~-J^ •X>

f-'-f •33 "=x= c-yi "—-

• •'-•^f•=•=•CJDi ~---Jcc* •:s?"- _« i

ri_)«CJ1

c r <5S"- - •-•"t

ic.-z»• iriC-i .,-•—-.

(-«=••---•00<JO

• •-"•—»-£=:-- •- »

P-JH 13^131W (EM: 1 1 f.:- 310,8978 L 321.S948 ^ WM ^ S31.336S ^ : :i33,333Ea^ffiTIVE TCDD, 37CL, ffi 13C-TCDD

r.( T < ^.^ ^ ,, SiB C Sl,[l^ Q ; 1^3 T = S^S

i ^ s l ? I l ! G l f l = 155.S8 T = 2 3 ^ 3W/ \ î•

•; ••--.

3 S L 31,11,01^ y :g3:ÎL I - L.I'

,/136

- 9 e . B S l , ! l , G l R = 5^ ^33;^ ^/ \ ^^/f^ ^

î11!61^ 11M,6? 1 = 2 3 ^ 6. ' / y ,.' i.

i 1

[1£l iôs l |n |Glfl= H56.53 1=^6, . — - — - _ B . , ^ ft '

11 ,-/•• 'J^6

£N5 M ^15 ^ ^ S^y


DATA SUMMARY

IT SAMPLE « / , ' y S 5 5 ' DATE ANALYZED:

TIME ANALYZED: /-=?. < '-

Net ^^.P.s-TCDO Detection Surrogate SurrogatiWeight/ 'OS- Linit 320/322 332/334 Measured PercentVolume per/fob ppf- nq ppb ppt f O . 67-0.90) (0.67-0.901 fppb) Accurac'

/ .. ^^7 — . ^6- ^1. >^ /^< y'.'y^

Area332

Area334

Area320

JW.W

Area Area Area*328

COMMENTS:

<D - Not DetectedS - Native TCDD Spikeo - Duplicate (Intralab)

Corrected area 328 [328 - (0.009 X 322)J

Checked By: M^ /^

; •

-

"-

1^ ex-"-\J •—« r--^-^- .\ I—— QT-..^ - f-'~•V Q\ <==:« '~XJ•^ '-'.-.-« -.—>

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c---^•in --(=..:• • r-uc-"•n-J

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__l •_oi ^ "==:• -.—« i-c-«—:• ess ix~-"

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—-" «-•-• • i'5* '+^;^ ^

•-•_1

^3 ^ ^K SI^ 66^3 SKi

^/

f .

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m ^/y)

9 K 3 = 1 ti'SSS ^ih'iso—————————————

\ 1 h))iU.i''"1 - 1 IQ'r ' r ' /T - U L1^ i:

, : - " ^ ' . ' I O I U S H

K^- ' V

^3=1 E^s^y^n' is i@s9L'e \a/^

?=1 rai ^ [g ' n^s^"'••. /•"'\ / -"^

il^!2=l 3t''et'S ^'[^I'lS:^

"\ / ©

^ r £ 3 = l ffi'^ ^[s'li 'is:-/'

[8

ins; H

S8[S

0"re

i

Se'| U

86| B

ee


DATA SUMMARY

IT SAMPLE «__y/ //^DATE ANALYZED: •?- / ~' -•-•--'

TIME ANALYZED: /? . ' / /

Net 2,3.7,8-TCDD DetectionWeight/ Cone. LlSlt

Yolmn.e, M pb ppt ncr ,j-ipS pptSurrogate Surrogati

320/322 332/334 Measured Percent! 0 .67-0.90) ( •0 .67-0 .90) fppb) Accurac'

r'. d' /

Area332 Area

_33^4

A-^i ^^

Area320

Area322

Area259

Area*328

•r-. '^

COHMENTS:

.<o - Not DetectedS - Native TCOD Spike0 - Duplicate (Intralab)

•Corrected area 328 [328 - (0.009 x 3 2 2 ) ]

cnec^ BV: ^

'J3

r--\

c<

^1

o~t

•Si^<a

cri••-••-•"^

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C.0i«33iU-><-•«

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——••'

r---.

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3(1195 17-JUL-8S 13:117H58S W SUS^ISOSTD? 1 K ' 319,8978 L 321,8948 11^ 327,8347 H ^ 331,3368 0 ^ 333,3333»t^f f iTIVETCDD,37CL, i013C-TCDO , /

transmittal of fish study work plan for lake dupree ... · fishes^-, and the audubon society field...

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