bc.P lb '87 14:50 INbTv1-F'RINTb EAST JOHNSON ST. P · bc.P lb '87 14:50 INbTv1-F'RINTb EAST...

24
bc.P lb '87 14:50 INbTv1-F'RINTb EAST JOHNSON ST. P.l September 16, 1987 Mr. Douglas C. Premo Facility Coordinator GM-CFD Massena State Route 37 Roosevelt Tovm, NY Mr. Premo: On September 15, you received the "deliverables package" from California Analytical. This is the reporting format for dioxin/furan analysis which was asked for by EPA. Specifically, the reporting format or deliverables are shown in Exhibit B of the material you received. ' Exhibit B is a portion of the whole dioxin/furan methods package specified the Statement of Work. As you can see from the table of contents for the method the whole package consists of six parts and a preface. The Statement of Work is intended to provide methods to CLP labs conductive work unde.- the Superfund program. These methods supersede methods found in SW-846 for superfund projects If Lisa Gatton-Vidulich or Christine Visnic of EPA still do not understand thxs, then please have them contact Joan F*sk a (202) 382-3155> She is the P* ject Manager for the CLP program. Another contact within Region II is PHI Cokely at (201) 906-6921. These people should be informed as to the tequirements to use the methods specified In the Statement of Work dated 9/l/P£ for Dioxin Analysis. This is the method used by California Analytical. The method in SW-846 is different and inferior. However, if EPA Region II prefers this method, then Caliiornia Analytical is willing to analyze the samples in this manner. The question regarding intern*-1, standards is simply answered by referring Regies IT. people to the entire Statement of Work for Dioxin Analysis. This document should be available to them or to their QA officers, pie question about tne type of column was previously answered by California Analytical Very truly yours, Thomas R. Stolzenburg Applied Chemist dls 269.23 931:DLS:pr«mo8

Transcript of bc.P lb '87 14:50 INbTv1-F'RINTb EAST JOHNSON ST. P · bc.P lb '87 14:50 INbTv1-F'RINTb EAST...

bc.P lb '87 14:50 INbTv1-F'RINTb EAST JOHNSON ST. P.l

September 16, 1987

Mr. Douglas C. Premo Facility Coordinator GM-CFD Massena State Route 37 Roosevelt Tovm, NY

Mr. Premo: On September 15, you received the "deliverables package" from California Analytical. This is the reporting format for dioxin/furan analysis which was asked for by EPA. Specifically, the reporting format or deliverables are shown in Exhibit B of the material you received. '

Exhibit B is a portion of the whole dioxin/furan methods package specified the Statement of Work. As you can see from the table of contents for the method the whole package consists of six parts and a preface.

The Statement of Work is intended to provide methods to CLP labs conductive work unde.- the Superfund program. These methods supersede methods found in SW-846 for superfund projects If Lisa Gatton-Vidulich or Christine Visnic of EPA still do not understand thxs, then please have them contact Joan F*sk a (202) 382-3155> She is the P* ject Manager for the CLP program. Another contact within Region II is PHI Cokely at (201) 906-6921. These people should be informed as to the tequirements to use the methods specified In the Statement of Work dated 9/l/P£ for Dioxin Analysis. This is the method used by California Analytical.

The method in SW-846 is different and inferior. However, if EPA Region II prefers this method, then Caliiornia Analytical is willing to analyze the samples in this manner.

The question regarding intern*-1, standards is simply answered by referring Regies IT. people to the entire Statement of Work for Dioxin Analysis. This document should be available to them or to their QA officers, pie question about tne type of column was previously answered by California Analytical

Very truly yours,

Thomas R. Stolzenburg Applied Chemist

dls

269.23 931:DLS:pr«mo8

XfB WA86-K357 ATTACHMENT A

STATEMENT Of WORK

DIOKXM ANALYSIS

Soll/Sodlnont And w*:«r Katricoi Multl-Coneoatration

Soloetod Ion Monitorlac (SIM) CC/MS Analjili

S/X/S6

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STATIHEST OF WOt*

TABLE OP CONTESTS

mFACE:

EXHIBIT As EXHIBIT B;

EXHIBIT C:

EXHIBIT 0:

EXHIBIT E:

EXHIBIT Fs

EXHIBIT &'•

!«I!L

Seep* of 11

Summary of Dioxia SOW Change* ,....» . til

Suaaary of Xaquiraaauta A-1-5

Repotting Requirement* mod Deliverable* <>.•................. 0*1-20

Sample Rerun Requirement* * 6-1-3

Analytical Method* D-1-3S

Quality Aaauranea/Qual 1 ty Control Requirement* E-l-23

Packaging and Shipping of Saapla Extract*.* . V-l-1

Chain-of-Custody and Document Control Procaduraa. C-i-5

Q 3 3 o o £s»

'J1

'1 7

q p p , cSEP 15 '37. 14:45 INSTY'-PRINTS EHST JOHNSON ST. Otr I j or id. CI iwnl_ rllNHL-T i 1 tHL LHB PAGE.34 P

scon 0? wax

The purpose of thle contract is to provide EFA with ehanlcal analytical services using (fleeted ion Monitoring (SXM) |t« ehroaetography/aaas spenttonstry/data systen (GC/MS/DS) techniques tor the analysis ox 2,3,7,9-Tetrschlorodlbenzo-p-dloxln (TC0OV in soil or sedlnent end eater ssnplea. The

*' rrspls? arc £"*• •***» of suspected 2,3.7»8-TCD0 eontanl-netlon. The aethods required la this contract are effective for a concen­tration range of 1 to 1000 parts per billion for soil or sedlnent and 0.01 to 10 parts per billion for uater.

The Contractor shall use safe handling procedures and generally accepted good laboratory practices to prepare and analyse for the presence of 2,3,7,8-tetrachlorodlbenzo-p-dioxln <TC00) in soil or sedlaent tad voter saaples.

The data obtained will be used by EPA to deternlne the existence and extent of threats to the public and the envlroonent posed by haaardous vasts disposal sites. The date nay be used in civil and/or erlalnal litigation, therefore the strictest adherence of eheln-of-ctatody protocol, doeuaent control, and quality assurance procedures la'required.

1 1

c - n , = S E P 1 5 ; 8 7 1 4 = 4 6 I N S T Y - P R I N J S E A S T J O H N S O N S T . a c r I S o c 1 £ : £ i L H L H N H i r : H . H L ! _ H t i PAGE.05 P'5

KXHZ1IT 1

REPORTING REQUIREMENTS AMD DELXVQIA8LSS

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SEP i SEP 15 '87 14:48 INSTY-PRINTS EAST JOHNSON ST. PH'aE . C6 P.6

BthlbltS - Reporting Raaulreaants end Deliverables

The Cotcrtctoe shall provide rsports sod other deliverables as specified la tha Coottact Schedule. Tbasa raports sra described below. All reports shall be submitted la legible Cora oe resubmission shall be required. All raports and documentation required, iaciu«uag sr«»2L s« claarly labalad with tha EPA Caaa number, Batch number and assoelatad saapla/Dloxln Shlpaant Record nuabcc(a). If documentation is subalttad without tha raqulrad identification, as specified above, rasubalsslon shall ba raqulrad. Tha Contractor shall provide all raports and dalivarablas as daserlbad balow, Tha Contract Reporting Schedule (Section 2) specifics tha nuaber o£ copies required, delivery schedule and distribution of all required deliverables. 1.1 Dioxin Shlpaant Record* Copy of SMO Dioxin Shlpaant Record with lab

receipt information and original Contractor signature.

1.2 Sanole Data Package< Hard copy analytical data and documentation Are required as described below. NOTE? This analytical protocol is designed for rocalpt and analyals of saapla# by batch. Therefore, It la dealred that •ample data from aaaplea in one betch ba reported together, i.e., on tha sane reporting for®. However, contract accounting and billing are based on tha saapla unit.

1.2.1 Case brrratlve (laboratory cover lettef)cflsrains fha_Case number> Dioxin Shipment Record numbers,Contract number/and deta.x«d docuaantation of any Quality Control., aSSyTa, ship­ment a-.4/or analytical problaaa ancountarad in a specific Caaa. Also Included should ba docuaantation of any inearnal decision tree proecsa used along with a summary of corrective actions taken, Tha Case narrative auat ba s -»i i» original signature by tha Laboratory Manager or his designees.

/ * " ) C o p l a * o f c o a p l o t o d D i o x i n S h i p m e n t R e c o r d s f o r a l l s a a p l e c reported in data package.

1.2.3 Results of Initial triplicate analyses of four (4> concentra­tion calibration solutiona, including all Selected Ion Current Profiles (StCPs), Calculated Response factors, plotted concewr tratl<a calibration curves (see Section 9.2.0.3.Exhibit D), and computer generated*quantitation raports.

I.2.* Coaplotod data reporting shoots (ferns 1-1, 1-2, 1-3, and 8-4 with appropriate SZCfs. Data results of levels less than 10 ug/kg or 100 ng/L shall be reported to two (2) significant figures; results greater than 10 ug/kg or 100 ng/L shall ba

•; •: p i =,cc.r ID a< it- « + c n o i r-rrcinia Lno i~ junnsun ai . n,-,-c a-? r. r i _ • u i w n i _ n i i n u i i L i X r i w r t - i ' a c . 0 7 •

[ 1.2.5

reoortad to three (3) significant flftttii. Apply the rounding rules found la Section 7.3.2, "Handbook for Analytical Control in Vator and Wastewater Laboratories, EPA-600/4-79-019. Each SICP auat inelnda tha following haadar lnforaatlon: data and tlaa of aaalyslas instrument ID; and sample ID, I.e., SPA eauple nuabor, eallbtation solution or CCAl or rolaan parformtnaa ehack i staples ara aaalyaad aora than onea, aU eanpla data shall be raportad. (Not*; Original and rarva data aaat ba tubalttad.)

SXCPa generated during oach parfomanca chaek solution analyst* and aaeh concentration calibration solution analysis.

1.2.6 A chronological list of all analyses performed. If aora than ona GC/MS systaa is used, a chronological list Is required for aaeh systaa. Tha list oust preside tha Data Systaa File Heme, the EPA saaple number, and (If appropriate) the contractor laboratory saaple number for each saaple, blank, concentration calibration solution, and perforaauec check solution. This Hat shall specify data and tlaa of beginning of analysis. All saaple/blank analyses perfotued during a H-hour period sust be accoapaaleb by two perforaance check solution analyses, one preceding and one following saaple/blank analyses. If multiple •mf. »*»- ""If TIT if-*"—«"•« »wlf nriM

f?r ,M. 11-h.ur »..l.d. 1.3 S.arel« n«t. 8IMI» helmi H»*d eon n.lytie.1 d»t» ud doe»..at»-

tlon ers requ.'--1 from the Ssapls Dste Package (Saetlon 1.2).

1.3.1 Case Narrative uyJ'X

1.3.2

1.4

Coapletad dat- reporting sheets consisting of Forms B-l, B-*. h-3, and B4. Original and rerun saaple data_shall be .provided on Fora B-l. """ "" — —nHM

GC/MS Raw Dot- "'anas: Magnetic tape containing raw GC/WSd--*ln appropriate'loatruiant manufacturers .foraat for all analyses (samples, blanks, concentration callbratloa solutions, ncrforaanee ™eck solutions, nnd performance evaluation staples) shall ba shipped to U5-EPA within eeven (7) days of request by the project officer or SMO. The Laborataw shall retain the innetliL tsoe dete knUiiU

Saunle extracts and Onuaad Sanola Portions t Unused port lot •* of Maples and alTT pla extracts shall be catalnad by Contractor for a period of ISO deye after analyses ars reported. Extracts. • • stored at 4*C; unused portlqpi_*' *

I

B - 2

o o

07 'vO

n

ccp i =?=-r _J-P ar 14-<40 ims i rtkih i b uhsi jui-trtoun •; Sir 1J OI it.« <wI-II_ nnfiLr i II.HL LI-IO PHQE.08

snblent tonoerature. When directed is writing by the Project Officer or Sanpla Management Office, the Contractor shall ship (not at Coatracpoc* a Jpenae bat la accordance with Department of Transport ntlSe tegulatloaa) specific saaples and/or extracts to a specified location

l 6 Document Control and Chala-«f-Cuetody Pschags: The Oocunent Control and Chain-oCustody Jackage induces ail or generated for a specific Case or seapla batch, that have not beea previously subaitted to EPS as a deliverable. These Iteas include but are not United to: sanpla tags, custody records, aaaple tracking r.rafda analvsts logbook pages, bench sheets, chronatographic ".".Vc ut.r /rtSto".! !» te. !.««..« lojjboob pagea, correspondence, and the docuaent inventory. (See Exhibit 6.)

1.7 Monthly Seaolo Stetus Report? The (loathly Senple Status Report shall prSvld; the statue of all sanplaa the Contractor haa received or has had la-house during the calendar nooth. Required Includes: seaolss received, seaples extracted, samples analyze*.

»bUl b. umum b, .,„oprl.t. p* Sanpla, Case and Batch/Shlpnent nunbeea.

i a n*iry Senple Status Report: lu rasponaa to verbal request from the SSI.i££g...« 0*v". « ch« t Otttcr. th. C«tr«tor «m.« verbally provide sanpla status information on a s me-dey cv-,.14 confirmation be coqueetsd, the Contractor 1aa—. J.WJM!!IAI mjoSKtlne il l JH«*A t'oik bhat saaa y using

shall Inline thafTtSr?otad for the Monthly and, in addition, shall require Information on sample analysis raporta la pregraas aad analysis reports aubnltied/nailed.

In accordanco with applicable dslivary raqulranoata, thaContrsctorahsll deliver specified itene par the following Contract Reporting Schedule (Sectloa 2.1). Recipients include the CUJ Unplo EMS1/LV QA Division, and the appropriate Regional and NtIC Contract Evidence Audit Team (complete caoo file purge/.

2.1 Contract Reporting Schedule

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a - 3 M u G\

SEP 15 '87 14:49 INSTY-PRINTS EAST JOHNSON ST. S E P 1 5 ' 8 7 1 2 : 2 3 C A L A N A L Y T I C A L L A B P A G E . 0 3

P . 9

ITEM NO. REPORT

comtract-reportibs schedule

# DELIVERY COPIES SCHEDULE

REPORT DISTRIBUTION SHO IMSL/lV REGION METC

1 Dloxln Shipment 1 Record

2 Sample Data 3 Package

I 3 Sample Dote Summary Package

4 Sample Extracts

Complete Case Pile Purge

6 Hagueklc T-. pr t

lot

1 Pkg.

Lot

7 Days After Receipt of Sables

IS D—» Afo... v;iia*tsd Sample Receipt Date

H)R-30 Daye After Validated Sample Receipt Date

IS Daye After Validated Sample Receipt Date

•OR-30 Days After Validated Sample Receipt Date

7 Days after Written Roqueat by Project Officer or SMO. Hay dispose of 180 days after analysis unless requested

180 days After Date of Data Submission

-OR-7 Days After Written Request by Project Officer or SMO

Within 7 Days of Request By Project Officer or SHO

X

X

X

X

X

X

As Directed

X

X

Monthly Sample 2 Status Report

Dally Sample 1 Status Report

5 Days following End of Each Calendar Month

Verbal and/or Written; Upon Request by SMO or Project Officer; Maximum

Frequency la Dally

As Directed

NOTE: ALL RESULTS SHALL BE REPORTED TOTAL AND COMPLETE.

Q 2 •2

o c r i ; a . r . i 3 ; a i ' i ' + ' O y i i j i o j r - r K i n i ^ L h 3 i ; 3 u n i ' D u r i 3 1 . r ' l - . ' a t . i y r .

Addresses for Distribution swo

%

CLi Saspla Management Off let P. 0. Box 318 Alexandria, VA 22313

Toe overnight dellverlea, uso «tcoot addressj

300 H. Ua St., Suit* 200 Alexandria, VA 22314

EMSWIV

USSPA SMSL/LV QA Division Box 13027 US Vegas, HV 89114 ATTH: Dot* Audit Staff

Tor ovomight dellverlos, uso •troat address:

944 E. Hanson Ava. Exacutlva Cantor, Ra. 228 Us Togas, HIV 89109

Deputy Project Officer: Following contract award and prior to Con-tractor's receipt o£ the first batch of saaplos, tha Saaple Manegeaent Office will provide tha Contractor with tha list of Deputy Project Officers for tha 10 EPA Regions. SMO will provide the Contractor with updated Ragloual address/naae lists as necessary throughout the period of the contract.

HEIC N&IC Contract Evidence Audit Teen (CEAT) 12600 Vast Colfax, Suite C310 Ukewood, CO 80213

bLP lb 'b7 14: bid 1Mb rr-PKINTS LAST~JOHNSON ST.

S E P 1 5 ' 8 7 1 2 : 2 5 C A L A N A L Y T I C A L L A B P . 1 1

P A G E . 0 1

Dollverablea Index

I. Case Narrative The eaea narrative suet contain: Caca nunbar; contract nusbar; inmr? of any QC, aaaple, sblpnant, and analytical problana: and documentation of all internal daclaion tree processes used. Outline problana encoun-

lutiona. Be ae apocific and detailed ae neea«a<»r*

II. Tabulated Data (Bom B-l to Form B-4)

III. Standard Data By Instrument A) All quantitation raporte, and SIM naaa ehronat|raaa for concentration

\ calibration eolutiono 1. Organised la order: Triplicate rune of CC1

Triplicate rune of CC2 Tii Ueate rune of CC3 ate.

B) All quantitation raporte, and SIM aaae ehronatograne for routine calibration 1. Performance check aolutlena organised in chronological order

«

2. Concentration calibration solution fl organised in chronological order

IV. Sample Data A) All quantitation raporta, and SZM naaa 'hromatogtsas for nathod

blank(s) organised in chronological ord«r

B) All quantitation raporta, end SZM mas. .fcreaatogtams for samples (organised by increasing EPA nunbar)

7. Chain of Custody and In Bouse laboratory Control Docunants

A) CPA Chain of Cuttody Kecorda

B) SMO Dtoxin Shipment kecorda

C) Sanple Log-in Sheets

D) In-House Dtoxin Bench Sheet

E) GC/MS Standard and Saapla Bun logs

• ^

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as LO

)

!.Si&SS608 249 0716 SEP 15 '87 14:57 INSTY-PRINTS EAST JOHNSON ST.

SEP 15 '87 12:27 CAL ANALYTICAL LAB P.l

P A G E . 0 2

bb:

Caoa/Batch V6ta

Xnatrunaat IP*

POEM B-1S. TGPD SOIL DATA IXPOBT FOBM

la port 0atafM

- Coluaa:

hl« 2 of 2

tel. !PA latoonaa latloa

Saapla Busbar

3207 322

3357 334IS

3337 3341S 320 322

laaponaa (Araa)

328 332IS 334 IS 332KS 3341S

{

KB N 0 PE MFC

Mathod Blank PB • Plaid Blank Matlva TCDD 8plk« IS m Xntarnal Standard fuplleata/Portlflad Plaid Blank 11 m lama EMSL-1V Performance Evaluation Saapla m> m Bee Dataesad Maxima Poaalbla Concentration 18 m lacoaary Standard

T> S, IS o 3 •C*

I • 8 9/86

4

SEP 15 '87 14:57 INSTY-PRINTS EAST JOHNSON ST. S E P 1 5 ' 8 7 1 2 : 2 7 C A L A N A L Y T I C A L L A B

P . 2 P A G E . 0 3

Ub:

Caaa/Bateh *01

"olihOMtlC 1Tj%

TOW B-IV. TCDD lum DATA KSPOKT 70KM

BtpOVt PfltH

Colons

7«g« 1 of I

{

MS -m m D « PS B MPC « •NoC.s

i Mathod Blank ItatlTo TCDD Splka Duplleata/Fortlflad 71 old Sink EMSX.-L7 Parfornaoea Evaluation Saapla Maalaua Poaalblo Concantration Kalatlvo to 43Cj2-i>2#3,*-TCDa

71 " Plaid Blank XS <• Xmtornal Standard Mi • Karua IS • lacovorp Standard HD • Mot Dotaetod

1 - f J/Bd

wi x x i iij i i ri\AMia C-n T* j "w'ni 1 3 i SEP 15 '8? 12:27 CAL ANALYTICAL LAB P A C E . 0 4

tebt

Caae/lacsh 8oia

Znetraent IDi

IOBM B-lVo TCDO KATXB DATA BSFOBT TOWH

' Beport Datet " Colon i

Pag* 2 of 2

Bel. B?A Baaponea Ratios ' i 20/ Staple

Kuaber 322 1527 33HS

3327 33ARSl 23»' m. 322

Iaaponae (Area3

328 332 IS 331 IS 332RS 331RS

MB N D

H MFC

i Method Blank HittiWa TOO Spike Duplleace/Fertlfled Field Blank RMSL-LV Perfonanee Bvaluacion Staple K<ixlsua Foealbla Coneaattatlon

FB - Field Bleak ZS • Internal Standard ** • Benin RD " Rot Detected BS - Beeoverj Standard

B - 10 9/16

SEP 15 '87 14:59 INSTY-PRINTS EAST JOHNSON ST. S E P 1 5 ' 8 7 1 2 : 2 8 C A L A N A L Y T I C A L L A B

P . 4 P A G E . 0 5

A. TCDO UPOKX PDBH (for* 9*1)

This for* 19 ueed for tabulating and reporting case results.

Complete tho header information «c the top of tho page including inatru-none ID, laboratory name, ease/batch number, report date, and column uaad.

EPA aaapla number la tabulated along with data sample waa extracted, and weight (wet) extracted to the nearest tenth (O.i) of a gran or volume extracted (water) to the nearest 10 milliliters.

Calculate the concentration of 2,3,7,3-TCDD using the foraula:

c* . *» * Qts . UUP, . tf

C* - 2,3,7,3-TCDO concentration la ug/kg or ug/L

- the sum of Integrated Ion abundance detected for m/s 320 , and 322

" the sum of integrated ion abundances detected for m/s 332 • and 334 (characteristic ions of 13C.j-2,3,7,a-TC00 the internal standard),

Qt, • quantity (In ng) of addad to'the aeople before extraction

RR?a • calculated mean response factor for unlabeled 2,3,7,3-TCDD relative to uCi2-2,3,7,: TCDO

U • The weight (in g) of soir'sediment extracted or volume of watr~ oxtrected (in mL)

Positive samples are queatlteted with values >10.0 ug/kg or 100 ng/L recorded to three (3) significant figures and those values <10,0 ug/kg or 100 ng/L reported to two (2) sign if tear,, figures.

• ' for samples In which unlabeled s.vt *-TgBQ e eut«e*

the eatlaatod possible concentrate . which la rtmlrBd wnronua a »«..! with . ...I. '

Use the formulai

Ql« I. \y «u . upa . v

where: MPC * maximum pesaible concentration of unlabeled 2,3,7,8-TQjO required to produce Hx,

B - 11

SEP SEP 15 '87 14:59 INSTY-PRINTS EAST JOHNSON ST.

I S * 8 7 1 2 : 2 8 C A L A N A L Y T I C A L L A B

P . 5

PAGE.08

Hk poak bright for n/s 320 or 322 in the aero group of >9 Kiu w«d to aaaeure A a.

Hia • peak hoight for tho appropriate ion eharactarlatie of tho intornol atandard, n/* 332 whan 320 ia used to doteralne A*, and n/a 334 when 322 ia naod to dotorviao Ag.

Qu - quantity (in ng) of 13Cl2-2,3,7,8-TCDD addod to tho oefore extraction.

2A?tt • calculated oaaa roaponao factor for unlofeolad 2,3,7,8-TCOD relative to cj,2"2»3»7»8"Ta,D.

V • weight (in g) of wet aoil/eediaent aanple or voluna of weter extracted (in al).

Report CC/MS Inatrunent ZD, the date and tiae the analpola waa perforaed, and the elgnal to noiae ratio for the aurrogate coapound.

-3 o o £=>

» - 1 2 £ ON CD

Str ID dr- liiUkj irto I T-PKiN IS EAST"JOHNSON ST. S E P 1 5 ' 8 7 1 2 : 2 9 C A L A N A L Y T I C A L L A B

P. 6 P A G E . 0 7

VOKN M

INITIAL CALXS8ATZ0M SUMHABT *»!• I at }

t.a bo r • £ nrn* i

Caaa/8ateh No,: — *olueiou Altarnaclva: Xnetruaone ID:

Soluciaw rn Codna:

CCX • Concentration CC2 <• Concentration CC3 • Concentration CCA * Concentration

calibration eolutlon #1 ealibraeloa eolutlon #2 calibration eolation #3 calibration aoltitloa #•

* ftat proaont In CC Solution Alternative Ona.

I - H 9/8*

bU" ID 'Br ID: Id! IHbl Y-I^ K i l N I b LHb r"jUMIibOh bl.

SEP 15 '87 12:29 CAL ANALYTICAL LAB

H.Y

P A G E . 8 8

row H 3 Of 2

1H1T1AL GAL1MATX0N SUM1AXt Laboratory: - CC Solution iltumtlTi: _________

Caaa/Setch Wo. t Xastnwettt ID:

Data Tine Sol„ ID

Heaaured Itfg

Mean Meaeured Itfl

Mean 11*1

CCl CC1 CCl

CC2 CC2 CC2

CC3 CC3 QC3 •

i

CC4 CC4 CC4

"olutlon IP Codec:

CC1 • Concentration calibration eolation *1 CC2 - Concentration calibration eolation ii CC3 » Concentration calibration eolation #3 -34 • Concentration calibration eolutlon #4

XRFi o 3 3

Watlee Mean IS Mean § of He ana? of Meanos

• • 14 »/•«

v-1 (-j -j o

SEP 15 '87 15:01 IMSTY-PRINTS EHSr~J0HN50N ST. S E P 1 5 ' 8 7 1 2 : 2 9 C A L A N A L Y T I C A L L A B

p.a P A G E . 0 9

9. Initial Calibration Suaaary (Form 9-2)

bcocd all loutlu calibrations (PCS end CCl) p*(f6lMd during Initial ealibratloa on fora 9-3.

Coaplata all header information Including laboratory* case/batch aumbac, and lnstruaent 10 and EPA CC Solution Alternative,

Date and tine along with responae for each ion la recorded for each cali­bration solution. The responee factors are ealevlacad with the following aquations:

a Factor) RRF (internal Standard Response Factor)

w.iecet

AX • the sum of Integrated ion abundance of a/a 320 and 322 for unlabeled

Ars " f$a sum of integrated ion abundance of a/a 332 and m/. 3?i for cUwi ,2,3,4-TCDO

Qn " quantity of unlabeled 2,3,7,8-TOD injected

Qu • quantity of C -2(3,7,ft-TCDD injected

Qrs • quantify of ^Cj2-i,2,3,4-TC00

Calculate the mean RRF and the percent relative standard deviation' for the triplicate runt of each ealibratloa solution.

2,3,7,9-TCDO

A , • ted Ion sbuadancces of a/a 332 and a/a 334 for

B - 13

oc.r is or IIBI r-PRiino LHSI jyniioun 01. SEP 15 '07 laiOO CAL ANALYTICAL LAD PAGE.10

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SD

x . „.n .< ..*>> .1 th. thr.. U.,oc..T.«— ...«««l.«l»

tt„ eb. * roapouaa factor*: calculate tha »aai otjaa«»»

§ 3S o o ifh.

1 - 1 6 h-j vj M

a

SEP 15 '87 15:03 INSTY-PRINTS EAST""JOHNSON ST. S E P 1 5 ' 8 7 1 2 : 3 0 C A L A N A L Y T I C A L L A B

P. 10 P A G E . 1 I

Laboratory*

£aa«/Batcn rio.i

roni s*3

BOVTlin CALtSXATZOIt SCMMA1Y _____________ CC Solution Alcaroaelvvi

XnotvuMAt ZOi

(CC1) (PG3) 'ERPORMi JtCS CHECK SOL. CON. C IALIB. SO >L. #1

Data 1

Tlaw 1

Xesooaaa

fa 320

322 .

328 , V.

332Z3

33411 . •

332RS •

i 1 '

334X3 •i

Ratlea

320/"(22

332/334IS «

332/334RS -

lir. —

RRP* . — • — 1

X VaUaT — — — 75 2 2 o o 4^

r - 17 9/3*

u>

*5

SEP 15 '87 15:03 INSTY-PRINTS EAST"JOHNSON ST.

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P. 11

Routine Calibration Suamery (for* 8-3) CwLt. tto hud.r laf .nation incladini tha laboratory. la.twniot IB Case/latch number and CPA CG Solotion Alt amative. for aach performance cheek aolution analyzed conplete tha date and tine of analytic, tbt raapooaa for •/* 239» 320, *" 322 fo onlabalad 2,3, ,8-TCDO- .328 for *™Cl4-2,3,7,8-TCDD, and 332 and 334 for Cx2-2,3,7,8 TCSD and Ion ratloa for a/x 320/322. n/x 332/334 for J"fll 3 V* 332/334 for CJ2-1»2,3,4-TCDD are to ba calcnlatad and recorded.

Raapooaa faetors ara to ba calculated aa tn tha Initial Calibration Suaaary (Section B). For calculation of valley percent aaa Saetlon 0, Section 9.2.6.1. For each Concentration Calibration Solution #1 need in Routine Calibration, coaplete all tha above inforaation.

7) 5 3 o o

8 - 1 8 * Vj

r2',k

SEP 15 '87 15:04 INSTY-PRINTS EASf~JOHNSON ST.

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P. 12

form i-4

QUAUTT CONTROL SUMMARY

I

I

I

Uboritory Haao,

Xnatnnent 10

Caae/Bateh Ro.

Accuracy» Fortified/ Spike Field Blank:

Relative Difference (1), Duplicate Analysia:

SOIL

WATER

DA Sample Number: DA Sample Number:

Accuracy! Fortified/ Spike Field Blank:

Relative Difference Duplicate Analyaia:

DA Sampla Humbert

DA Sample Humbert

1 - 1 9 9/86

o 3

o o

-J in

SEP 15 '87 15:04 INSTY-PRINTS EAST JOHNSON ST. SEP 15 '87 12:31 CAL ANALYTICAL LAS PAGE.14

9> QC Sunaary Coaplote *11 th« header information. Eaport the oaaple auaber for cho fortlfiod flold blank ond eho X accuracy

of-the fortified/spike flold blank by using cho following equation: aaouat aaaaured

X accuracy • ——————- x 100 1.0

Eocord cho aaaplo used for duplicate and cho Relative Vopeont Olffaronco which la calculated aa followa:

$1 and S2 represent sample and duplicate aaaplo results.

B - 20