UNITtO ATM tNVIftONMENTAl MffrffhON AOCNCVHC4UON W

CftAMCMM6*MWOCQ ***•

MOUtfON. ttXAft 9M9 4

Subject:

Aby of th« laboratory rw data fop th»of th* UberatoryStrtlii! SaiJl *«*- ^*"

INQRfiANIC:

inr-vc-vOOO

The data t*as found:

; us* of data rtqulres caution. Problem; data should not & used, Probleas

retarding the review can be addressed to at.

aotedIn

fieuder

s i t e Koppers

O R G A N I C OA CHECKL I ST

Contract No a

No. _.5AS.#1811FRe v i e w e d By _M. L_*_Hitter

oats 4/3/86 ^ «f/^ftrfe

NO. F4045F4047

F4059F4051F4041

Cont ra c to r Cal Anal LabMatr i xAcct, /6TFAJNC1 3F TFAU79

F4062 F4065 C

OVERALL COMMENTS ( To 8e Comp l e t e d By £PA PERSONNEL )

VGA S/N Pest1 » Ho I d I n g T I ma s

2. T u n J n g /P a r f o r m a n c e

3. Ca I I brat ; arts

4 . B l a n k s

5* Sur roga t e s

6. Ma t r i x Sp f k e/Oup

7. Compound I d e n t i t y

3* Ca s e As s e s sm e n t

OR .CLAQI.fJCA_T_LOjl.S. fSee Attached)

Other(HxCDD)Ji5_A

A^N**l

ANR

At o v I a t Q n a I - .. J)a.t_a _u s_a fa l_e ;. rces s e n t l a l r ev l a i y ft em s . _n j g s_l .n g _o r c r_l t e r I a

not

Jj— T^UJ1 *P c o p t a b_l_e__° D_a_t a_ un u s a_ bj a_;_a 8 s e n t la I r ev^ ley 1 1 e m s _m |_ s j I n q or c rj t e r I a_n g_t_m e t *KR- Wot required or requested for this SAS submission.

REHXCN VI CLP OA REVIEW

3AS# 1S11F Site Koppers Lab CAL

The following is a sumnary of sarpie qualifiers used by Region VI in reportingthis CLP data!

No..VCftBNAPest

Acceptable Provisional Unacceptable

r-

Othsr (HxC DD). 0 0

Tne jjLb__hJ:s 1.'e"arLal.7zed samRles FJ»°45 and F4059i along vith_ appropriateQG in the form of standards and native spike addition for hexachlorodi-benzodioxin« Thg__data_ resubmission was very good and 6E_-HL now considersthat the data submitted by the lab for SAS#l8llF is to be consideredas acceptable. Sample F4045 on re-analysis showed 36 ppb of HxCDD;sampleF40 5 9 had no detect a ble^Hg DD^ wi t h a detect i^onj_linii t c a 1^ ul a ted to b eaboutJXl/f ppb for HxGDD, The native spike recovery for F4059 was about120$. _____________For what_ever_reas_on__that HxGDD was the rea^uestea^.parameter for this setof data, it was clear from the lab reanalysis of F4045 that HxGDD was,in fact, the minor component in the sample. Evidence was shown in the datathatvery substantial of heptachloro isomers of dibenzofuranand dibenzodioxin, HpCDF and HpCDD, as well as the octa-isomers OCDFand OCDD wei?e also present,

ORGANIC QA CHECKLISTCONTINUATION PAGE (

CASE NO. SAS 1811F Resubmittal SITE KoppersCOWIENTS;As the presence of other isomers of ._cfelorgdijen_2Qfura_ns and_dioxlns

was not a part of the SAS request for this set of data, 6E-HL recommendsthat this entire set of data and perhaps the site itself be re-evaluatecfor parameters of interest 4 The amounts of hepta and octa isomersbe determined by the lab either from existing data or by reruns under

...___ __ _ . _L u_ , _ ,., - - ,._, __ fr-rr.- ———— ——— -ii -i -n.:i. - . n i - i . . __ •-„_ __ ._ __ ——_—._.-.__-._ __ -i __ r— ̂—— j-^r-,-^-^— n - j— nr

a separate work statement 4 Similarly, the data from the other samplesin this SAS#1#11F done earlier and not a part of the resubmission are_ _ _ _ _^ ___________ __now suspect as to_their Qn^^r^y^9^^n^Jrs^_.(^!1A^s_a^^)^rate

analysis of this site for similar samples was done for hepta* and octa-isomers or others of this series).

Originally submitted data for the remaining six samples of this setj- — -^F404 7 > F40 51 > F40 62, F4Qo 5 r F40o_8 ,_ F404 1, was aga . 1 n r e-r e ̂vi . ewed and t heinitial findings of identifiable amounts of HxCDD in certain of thesesamples ( all except F4047 and F4041, as stated in the $/&5 <3A review).Points of objection to the data frnn the lab for the original submissionhave been settled and it is 6E-HL opinion that the lab has given thissample set its best effort. The sample F404 5 data,_ originally in doubt ,has been rerun (item #1 of 8/85 QA review). Lab blank interference (item#has been shown to be no J-onger_a__jproblem;_ the initial interferencewas for only the one isomer for which the lab was running as the standarand this amounted to about a calculated 0,2-0.5 ppb which was stillbelow what the requirement was bel^/ved to be of about Ippb for the blanFor values of HxCDD reported the lab had to assume a single response forthe measured isomer that would also be applicable to the other isomers

ORGANIC QA CHECKLISTCONTINUATION PAGE

CASE NO. SAS 1811F Resubmifctal ;iTE KoppersCOfrfclENTS:of HxCDD and this they did* Running all possible standards for HxCDDwould be outside of the scope of this work and the standards dont existin any case (item#3)* Native spike recovery for F4059 was shown in theresubmission to be satisfactory (item #4). Sample analysis data should^now be considered acceptable for HxCDD results as originally requested-(item #5) .

cvOO

Colifornio flnolytico! Loborotories, Inc.2544 Industrial Boulevard • UUest Sacramento, Cfl 95691 * (916) 372-J393

March 13, 1986Lab No: S6490SAS 1811F

Mr* William LangleyUSEPA Region VIEnvironmental Services Division6608 Hornwood DriveHouston, TX 77074Dear Mr. Langley:On February 11, 1986, Cal Lab received a letter and all thedata associated with SAS 1811F from David Lopez. I haveenclosed a copy of that correspondence, along with the othermemos that were attached, cal Lab was quite concerned bythis, and X immediately called Mel Kitter to dicuss thesituation with him. We both agreed after a lengthly discussionthat there were problems with the data, but that they were not"unfixable" and that the data should not have been classifiedas unacceptable. After a discussion of the problems, Cal Labagreed to repeat samples F4045, F4059, the native spike and themethod blank with our most current methodology (using a 13C-hexainternal standard) at our cost. We are re-submitting this newdata along with the original report to Mr. fitter for re-review;confident that the data will be acceptable. Had Cal tab beenmade aware of these problems immediately after reviev/, we wouldhave corrected the problems in a much more timely fashion. Itmakes it very difficult to respond to questions or criticism ofour work when the only feedback we get is to have the originalreport returned to us labelled "unacceptable" with no chance fordiscussion. In the future we hope that a better system can bedeveloped between your region and Cal Lab for resolving thesetypes of problems.If you have any questions, please give me a call.Sincerely,

oi—»or-OO

Michael J* Miille Ph .D.Director GC/MS Services

MJM:rthcc: SMOKendal YoungHarold TakenakaJoan Pisk

ytfof^

UNITED STATES ENVIRONMENTAL PROTECTION AGENCYREGION VI

I2OI CUM STREETDALLAS. TEXAS 7S27O

February 7, 1985

Paul A* Taylor, Ph .DCaliforn ia Analytical Laboratories2544 Industrial BoulevardWest Sacramento, CA 95691

Re: Special Analytical Services Case No. 1811FDear Mr. Taylor:

The EPA Region 6 Houston Laboratory reviewed the data for SAS 1811Fand found it to be unacceptable. Based on this evaluat ion, I am returningthis report to you for your d ispos i t ion .If you have any questions you may call me at 2 14-767-2720.

Sincerely,

OOf-O

David Lopez, On-Scene CoordinatorEnvironmental Services Div i s i on (6E- £F )

cc: Kieth Bradley - 6E-SH

"| UNITED STATES ENVIRONMENTAL PROTECTION AGENCYf REGION VI

MEMO

Date; 8/13/85Subject;From:

To: Joan Fiak, Project Officer, WH-548A

by Cal Anal Lab for SAS 181 1F .

The data submitted by Cal Anal Laboratory is questionable. Werecommend reanalyais under better conErolled analytical conditionsThe procedure under preparation by BiSL/Cinn for analysis of Octa-chloro dioxin could be a model for resolving problems encounteredIn Ehe data for this case.

The results suffer from several problems which should not be ex-ceptions to the usual CLP requirements. These points are dis-cussed in the attached report. Corrective action is recommendedao that subsequent data will be acceptable.

oo

cc: Sample Management OfficeU .S . EPAP .O . Box 818Alexandria, VA 22313William Langley, DPO, Region VIHarold Takenaka, DPO, Region IX

California flnalytical Laboratories. Inc.2544 Irtduscnol Souievofd • UJest Socromento. Cfi 95691 * (916) 372-1393

July 23. 1985Lab No. S6490-S6497Received: 7/9/85SAS 181IF

Mr. William LangleyU . S . EPA Region 6 laboratoryEnvironmental Serv ices Div is ion6608 Hornwood DriveMonterey Park Plaza, Bldg. CHouston, IX 77076Dear Mr, Langley:Enclosed are data summaries and documentation for the samples and QA/QCcomprising SAS 1S11F which we received July 9, I?35. The soil samples werelogged in under CAL Lab numbers S6490 through S6-97 and analyzed for totalhexa dioxins only. The correlation of ID numbers is shown below.

oop-oo

EPA ID

F4047F4051FA059F4062F4065F4068

CAL i:S6A9CS649156*925649356494S6A95S6A96S6497

The analysis was fairly straightforward, although we would like to call yourattention to sample F4G45 (S6490). Our internal standard (13C-TCDD) shiftedsignificantly in its retention time and the recovery was low compared to thsother samples in this case. Since it is not known how well 13C-TCBD recoveryrepresents hexa dioxin recovery, the value we reported (84 .7 Pg/g) may or maynot be the true value. The results we are reporting are contractually correctand in an effort to get the SAS out on time, we are not repeating this sample.However, if the value seems unusual, we would recommend that the analysis berepeated since this sample was so different from the other seven.If you have any questions about the data, please call.Sinewe1.

Paul A. TaylorxVPh.EPresident Michael pMi i l l e , Ph .D

fi-rector of GC/MS ServicesOrbanosicy

Senior Chemist'

cc SMOEMSL

*UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

REGION VIHOUSTON BRANCH

66O8 HORNWOOD DRIVEHOUSTON. TEXAS 77O74

ORGANIC QA CHECKLIST

KQPPERSCase No. SAS

Reviewed By __M^L.RitterDate

Contract No. 3ASContractor ANAL LASMatrix _Soil/sedAcct.

Sample No. F4045 - F404?F4062

F4051F4Q65

SFF4059

F406S F4041

OVERALL COMMENTS (To Be Completed By EPA PERSONNEL)1 .2,3.4.5.6.7/'8.9.

Data CompletenessInstrument TuneChromatographyBlank Analyses

!&.Matr ix Spike!Dupl icatesSurrogateFie ld Bl ankOther

. . .. . . . AcceptableAcceptable

_ _ . _ Acceptable_ . . , , Acceptable

, , , Acceptable— . — __ Acceptable

Acceptable_ . . .- . . . _ _ Acceptable

Acceptable

OTHER COMMENTS OR CLARIF ICAT IONSOverall dataalthough theinterferencesevaluation of

for this Ca.qp ^A^lab blank must be. As there was nothis dataT~orTr\n^

—J^_^ Provis ional_ . . . _ _ . X Provis irtrtf l l

X_____ ProvisionalProvis innal X

X Provis iona l_ _ _ Provis inr,^]x

Prov i s iona lProvis iona lProvis iona l

^HE....!? GoagM££M-^^4^ojconsidered as unacceptable"•"''"''" •• "— • — ^-_ __ ^^^^criteria for 6ES-HL to foil-~~~-: ~— i— ̂ - —— •--- r.a.,- I7&-* .q n1* i A>T *-«av» .^,. — ~- j. ̂ i —t — — «~

UnacceptableUnacceptableUnacceptableUnacceptableUnacceptableUnacceptableUnacceptableUnacceptableUnacceptable

sciai£nal_because of

Low in

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ORGANIC QA CHECKLISTCONTINUATION PAGE

• CASE NO. SAS lailF___________ SITE K°PPer s

F4045,F4047,F4051 ,F4059 SF #

COMKENTS: F4062, F4065 1F406#, F4041-^1 . _p3ta f-rom this sample set must be used, with cautig_n._The case narrati

relates as to- the shift in retention time/scan for the frighest amcunt-cf hexa-dioxin found,namely that of F4045 where 85 ppb was ̂ reported,In this sample, the internal standard showed a large shift and the ^area was low for the m/e 334 ion,about 26 ,500 as compared to the otheC"samples I .S . area for m/e 334 of about 500,000 counts. If~ the loss oro

low recovery "was only for the internal standard because of low additiPto the sample or instrument problems, then the value for F4G45 maybe too hi g h b y^so me f a c t o r 6 f~ 10-20 and the" true ftva 1 u e clo s er t c t ho s ereported for some other samples such as F4065 ( about 5-10 ppb ).

ID This case data suffers from the same problems as did an earlier setof data from the same lab, that the method blank and several samples

showed an interference in the scan ran^e_expected_for the one .standardhexa-isomer used for determining response values. The lab ran two setsof standards wnere~tne hexa isomer used,1, 2,3,4", 7, 8-hexa,"h~ad~ret"entio;scan numbers of 992 and 996 with RFs of 0 >50 and 0.46 relative to theI .S. of 13CirCDD. The method or lab blank was given a very low (0.011 ;detection limit for hexa, but an obvious interference was present thatfor the hexa-isomer in question for which the standard was run. Forsome reason_the_ lab did not take this_ interferenc.e__intQ. account... Arecalculated limit by 6ES-HL gives a much higher value.

"S, """''^ ————————————~i—————————-.,.. __^-,r ,-. l rT . ———,- —————————————— -———T J———————^——————————————————————————————————————'————• '- ———————""

r 3). For the samples which show some hexa-dioxin,namely F4045,F4051 tF4062,F4065,and F4063 ( the values for F4047 and F4041, less than 1 ppb, .should not be considered ) the values were derived by summation of var:peaks in the. ...spectra _and_ getting, a total area for m/e. 3.9.0 .__Manv_of__.the tpeaks were far removed from the one standard run by the lab and thusraise mof5~7iTrestioris"5s to "jus'i'wnat is being counted. Hexacnlorodlbe n:d i o xi n ha s a _1 ot of po s si b 1 e is ome rs _a nd_ ̂ he la b__ itself may ha v_e a _. _1 o tmore knowledge of the chemistry and GC patterns of hexa-dioxin, but

ORGANIC QA CHECKLISTCONTINUATION PAGE

CASE NO. SAS_________COMMENTS: F4062,' F4065 ,' F4063\ F4041

3. continued

SITE

the data present iation of an unequivocal'lSnner^

spike r e c o v e r v . » . , . » , r_interference tha t , sho^fo^he" particular isomer of

— _about 115^, if you try to take into account the

^47 was spiKed with native ^*lab listed the recovery as be€>

to subtract it out.5. Recommendations:Reanalysis of

4tJELdiL