Document wpGK90YGEbQ0bKXBdJZgpk8J

Monsanto ESiH/ESC (Co./Uiv./dept./location SAMPLING ANALYSIS (lype of Report) . 3 S sw X 1 s sMl s*# c a * \ REPORT MO.: DATE: JOB/PROJ. NO.: TITLE: AUTHORS: ABSTRACT: RECEIVED OCT 23 1987 MSL-7Z23 ESC-UAG-87-M4 Octobr 9, 1987 7634 and 7636 Analysis of Montreal LaSalle Plant Haste Samples for PCBs. B. M. Hughes, 0. E. McKenzie and L. R. Minor The Montreal LaSalle Plant reguested that ESC conduct low level PCB analyses on six samples to determine proper waste disposal methodology. Samples Included organic wastes prlMrlly consisting of phthalate esters and a water/sediment aqueous waste. Two sets of samples were received for analysis. In both cases the organic matrix samples #101, #108 and #110 contained PCBs ranging from 3.7 to 7.7 ug/g. Aqueous phases and sediment from aqueous samples (102. (10BB, and #1108 ranges from NO to 3.9 ug/g. All analyses were conducted with a method limit of detection of 0.1 ug/g per PCB congener. i n IS ii i\ lemtai TECHNICAL APPROVAL: .. w Jjt,, a-- P. L. Sherman Environmental Sciences Center Sr. Research Group Leader APPROVAL BY: -TTY ________ Environmental Sciences Center QA and GLP Supervisor APPROVAL DATE: JlI, I<1V1 COMPANY CONFIDENTIAL Tide document is (ha properly of Moneento Company and the recipient ' responsible for its aafeteepinp and disposition. It contains CONPCBIVTIAL INFORMATION Which must not be reproduced, revealed to unauthonted persona or sent outside Pie Company without proper authorization HONS 02h6bl COPY NUMBER DISTRIBUTION ABSTRACT ONLY 1. S. L. Emery 2. A. M. Ford 3. 8. M. Hughes 4. J. M. Lee 5. 0. E. McKenzie 6. H. Plotnlk 7. C. Roy 8-10 Reports Library - E2MP - U4E - U4E - U40 - U4F - 5090 - 5090 - R2C T. F. Evans - A3NA P. L. Sherman - U1F A. F. Uelner - A3NA C O VI R A N Y COM IDF N TlAi This report has been assigned to you. When it is no longer needed, you are responsible lor returning it to: i you transfer it to anyone else, please let your librarian know, so the records can be changed Cllfltv 1/BQ) HONS 024662 Tima Stamp - <871013.1337> AMALTSIS RIPORT loc mmm: u-*7-o-o-02 U-67-09-U-02 TO: Christian Roy and Myra Plotnik (5090) Moneraal Plant DATS: October 9. 1917 R0JECT HO: 760.21-7(34 780.28-7836 FROM: Envlronaental Sciences Coneor Monsanto Company 800 M. Lindbergh IIvd. SC. Louis. Ko. 83187 Phono Mo: <314) 894-1484 Tltlo: amlysis of Montreal Lafalls float Vasco Semples for fCSs ABfTlACT Tho Montreal LaSalla float requested that ISC conduct low lrrol fCl analyses on six samples to dotsraino proper wsseo disposal aoehodology. Semplee Included organic wastes primarily consisting of phchalato eaters and a water/sedlment aqueous waste. TVo sots of saaplos wore received for analysis. Xn both eaaoa the organic matrix saaplaa #101, olOl and #110 contained Pels ranging fron 3.7 to 7.7 ug/g. Aqueous phases and sediaont froa aqueous saaplaa *102, slOIB. and ollOS ranges froa MD to 3.9 ug/g. All analyses were conducted with a nathod Halt of detection of 0.1 ug/g per PCI congener. XMTBOMCTXOV Six saaplos wore received froa the Montreal Plant for PCS analyses. Prior to analyses it was determined that a Halt of detection of 0.1 ug/g per PCI congener would be required, because the notarial in question was subject to a regulated level of 1 ug/g for disposal. Aqueous saaplos wore centrifuged prior to extraction and the voter end sediaont were treated as separate aaplee. Saaplos were prepared using Standard Extraction Method PCBtlS omitting the cleanup celuai stop. Tho aoehodology involved weighing tho seaples into a Teflon capped vial end spiking tho saaplos with carbon 13 labeled PCS congeners, and adding 10 aL 20% aqueous K0H eo the vials. The vials were capped and warned In a aandbath ae approximately 80 degrees C. for 1 hour. Semplos wero thon extracted with 23 xL Surdlek end Jackson UV grade hexane. The volume of tho extract wee reduced In s were sandbeth under nitrogen screen to a final volutes of 1 mL If possible. The extracts were chon subjected to capillary GC/MS analysis using Standard Analysis Method KSAM23. SeLeeted ion monitoring was utilized for ell analyses. Characteristic end confining lone wore monitored over epproprlseo roconcion time ranges end the ratio of ehersceerlseic to confining reponee was aohs a**663 calculated for all coapounda dataccad. (Saa PCSC25 for aero data acqulatclon Information.) Daca n aeeapcad tf the ratio aacched corralponding icandard conganar racloa of plua or alnua fifty percent. If a coaponant waa dataetad and the ratio waa out of thia range. It vae aeauaed thee the compound waa not a PCS conganar and the concentration waa not calc ulated. Standard Extraction and Analytic Hethoda are Hated In a later action of thla report. A Hat of aplklng coapounda uaed In ehla atudy and characcerlatlc and confining Iona aonltorod are llacad In the Additional lnforaatlon aactlon of ehla rapore. All concentration wore calculated uatng Internal ttandard aathodology, which la llatad In standard Analyela Method NSAM2S. Calculation ware baaed on a aarlea of raapona factora calculated for each chlorine data froa chraa atandarda each containing 24 known congenra. The aeandard eontalnd the cowponsnts llatad In the Additional lnforaatlon aactlon of thla report under the heading Heelva Spiking Coapounda. Actual Indivi dual and average chlorln claaa raapona factora uaed In concentration calculation! ara In Tablaa lb and 2b. Raaulea of anlyaaa ara given In Tablaa 1 and 2. Concentration ranged froa HD (< 0.1 ug/g) par conganar to 7.7 ug/g total PCI congenera In the unplkad aaaplaa. Thaee tablaa llat the concentration of PCBa doeecead par chlorln claaa In eha extract, the auaaad total concentration of PCIa in eha extract, tha concantration of total PCIa In ug/g (corractad far aaapla aaoune and extract voluaol and tha parcant recovery of labeled aurrogacea If they ware added to the eaaploa. following Tablaa 1 and 2 ara chair a and b councarparea which llat eha ratio of characcerlatlc Ion to confining Ion of coaponnta decocted, and raapona factora vhieh ware uaed to calculate concentration. Saaploa ara naawd with their Identification nunbar. DOT reform to duplicate analyela, SID rafera to tha aadlaant portion of an aquaoua aaapla- U rafara to a native eplka addition eo a aaaple of 0.1 ug each of 24 PCI congaaora, and * MS Indleatea eha addition of 1 ug each of 24 PCI congonra eo tha nerlx. Thoae aeandard aatarlala ara llatad In the Addelonl lnforaatlon Soctlon of ehla report. Tha ratio of CU-. Cl>-. CL5-, CL4-, and CL7-biphenyl congenra Indicate chat the cocal PCIa which ara preeont ara froa alxturoa of Aroclor 1242 and 12S4. QC USBLTS Saaplaa 0101 and 0102 a 0102-SID ware aplked with 4 carbon-13 labeled PCI hoaelaguoa. lecovertea ranged froa 4 eo 1214. Afcar careful 1nopaction of eha data eeveral very lew apurloua recoverlee ware actrlbucad to chromatographic lnterfarenta, and aaaa apactroaatar detuning during daca collection. Thla damning waa not daaaad eo bo aarloua a Inca It only occurred far the higher molecular weight PCIa (Ctl through CLIO), and aaaplaa that contained PCIa moat likely contained either Aroclor 1242 or Aroclor 1254. Neither of theea fornulatlona contain algnlflcane aaounea of eha higher molecular weight PCIa. Sana apurloua raaulea wara alee found In the native aplklng raaulea for lower chlorinated (CLI-CL2) biphenyls, which wara due to chroaacographlc lncarfaranca. It la aaauaed ehac these valuae do not affect tha conclusions of this rapore. In addition, low and high level native spikes (addition of 0.1 ug each for 24 native congeners and tha addition of 1 ug each for 24 congeners) wara performed on all aatrlcaa. Natlva spiking recoveries for tha vase majority of raporead recoveries ranged froa 50 eo 1504 recovery. A second group of saaplaa was extracted without tha addition of carbon 15 labeled surrogates due eo HONS 024664 lack af surrogate compound* at tha tine of oxtraction. Thaia samples vara alae spiked with cha nacin spiking atandard. Tha raeavarlaa froa chaaa atudlaa Indicated chac cha rapertad aaapla values ara rallabla. Individual aurrogata coapaund raeavarlaa ara llatad In Tabla 1. and natlva spiking raeavarlaa ara glvan In Tablaa } and 4. Saaa atandarda vara alae analyzed aa saaplas In ardar to eaae cha reliability of average congener roaponae calculations. Results ef snslysls of LS SFK (lev native splka atandard) and HS SK (high natlva spike standard) Indicate cha analysis Is rallabla. OITAXU Standard Sampling Method No(s): Saaplaa supplied by tha Montreal LaSalle Plant. Standard Extraction Method Ro(s): PCEX13 ISaa also flaw ahaat PCTS13} Standard Analysis Method No(s): MSAM23 (Sea also flow ahaat MSFS23) Mass Spectrometer Data Aqulaltlon Method: PCSC23 Saspla Idantlfleatlon(s): Sao login Infatuation Final Report Fils Mo(s): IA743A Tabla File Mo(s): a:\peb\TA743* and e:\peb\TA7434 Also included In ehls report ara: (II Irlef descriptions and flew diagrams of Standard Extraction, Analysis and Maas Spaetronatsr Data Acquisition Methods used In this study. (2) Rxanpls of a raw data output (CC/MS) chroaatograa obtained In this study. (71 Chaln-of-Custody documentation for this study. (4) Analytical Raquoat lnforaaelon generated at sanpla login. 131 Description of laportant tornlnology uaod In Quality Asauranca/Quallcy Concrol. Analyte Extraction and Instrumental Analysis. ADDITTORAL IRFORRATIOR This section daacrlbaa eoapounds used In this study aa standards and provides Intonation an aaas ranges aonitored during analyses using aalsctad Ion aonltorlng. Internal Standard Anthracene-dlO Surrogate Spiking Coapounda C-13 labeled 4-chloroblphanyl 13C4 3,3',4,4'-eacraehloroblphanyl 13C12 2,2',3.3',3,3'4,t',-octachloroblphenyl HONS 024665 doeoehloroblphonyl 13C12 Motive Spiking Conpoundo (uood for rniclvt aptkes) 2'oonochloroblphonyl 3-nonoehloroblphonyl 4-nonoehloroblphenyl 2.2'-dlchlorob1phony1 2,5dlchloroblphonyl 2,4'-dlehloroblphonyl 4,4'-dlehloroblphonyl 2,4,4-erlchloroblphenyl 2.3,4*erlehloroblpheny1 2.4.4'-erlchloroblphenyl 2.31.4.4, -cocroehloroblphonyl 2.3.5.4,'Cocroehloroblphonyl 2,2',4,4',-cocroehloroblphonyl 2,2 *.3,4,3-poneoehloroblphonyl 2,2',3,4,3'-poneoehloroblphonyl 2,2',4,3,3*'poneoehloroblphonyl 2,2',3,3',4,4'-hoxoehloroblphonyl 2,2',3,4,4',3'-hoxoehloroblphonyl 2,2'.3,3',4.4'-boxochloroblphonyi 2,2'3,3',4,4*,4-hopCoehloroblphonyl 2,2*3,4,4',S',4-hopcoehloroblphonyl 2,2*.3,3',4,4',3,3'-oe tochloroblpyhony1 2,2*,3,3',4,3,3,*,4,4**noneehlorobiphonyl doeoehloroblphonyl Choroccorlocie and Confining Nooooo Honlcorod Choroecorloele (AKO) onchroeono-dlO 4-ehloroblphonyl 4C13 3,3*4,4*-cocroehloroblphonyl 12C13 2,2'3,3',3,S',4,4'-oecoehloroblphonyl 12C13 Doeoehloroblphonyl 12C13 nonochloroblphonylo dlehloroblphonylo erlehloroblphonylo eeeroehleroblphenyU poneoehloroblphonylo hexeehleroblpbenyio hopcochloroblphonylo oecoehloroblphonyl# nonoehloroblphonyl# doeoehloroblphonyl 144 194 301.4 439.7 309.4 144 222 233.9 249.4 323.9 337.4 323.9 427.7 441.4 497.4 Confining <AJ) 190 194 303.4 441.7 311.4 190 224 257.9 291.4 323.9 339.4 325.9 429.7 443.4 499.4 ANALYST(S): 4. Kooon Hughoo, 0. C. MeKonslo, ond LoShown Minor ANALYST APPROVAL: HONS 024666 Ml I. Ml M KS CMMMrMlM MUM M HMml ta^tw MMc llM latm'Mn MU )* NMImM KUIS Mi MMI9. |lr*U(tt IVM> IM4 MM Ml U4IMMIM: HUH HUM KUtl man mm MMMM CUM I M W IM MM M INI K4-XM4 n Ks-im M M'im Mi-1144 14 ms-iim it M4-4M4 (4 MS-1144 14 ti*U> (Mtt) Ii4> M4MI (M**> <M/U> (MS) -->liril|*Mli MiMnM0nMi lrMMMM0mrM tlllMIlMjilUli MMMnM0M|U MIMI>MMmMi MmMmMMmMi 444444 C.1 C.1 1 4414 c.r 4.V 4 1 4 4.1 I.I 4 i.i .* 4 4 4.1 1 4 i.i 1.4 4 4 4.4 1.1 4 t.i 1.4 4 4 4 4.4 I.I 4 i.i 4.4 44 4 4.1 1.1 4 4.1 4 4 4 4 4 4 4 4 4 4 4 4.1 4 444444 MMl MM M IIWKHMM 4.4 4.4 4 4 4.9 . 1.1 Mm MM M IMII IMil 4 r.t 4 4 4 1 1.4 4.1 l 1 it mm t*U> 9.4 4.4 I.I 1.4 a.4 4.4 i.i 4.1 1.4 4.9 2.1 4.4 1.1 4.1 l.t 4.1 1.2 SI 4.1 4.1 V 4.4 n 4.4 umiirMiMHnmn >iin>urMMm - n (S MCI n IV 41 M It MCI n 1M 41 M 1* MCI TV 1M m IM (1 MCI n m 1M m <1 MCI n n iv 44 IS MCI Ml 44 M n IS MCI 1} 44 Ml M IS MCI m n 1M 1M IS MCI in M IM M (4 MM HI M s M MMIfMMUM HCM MKC MMM Ml * H44M I H4444 i *1444? i turn t HUII i H4444 I HUM i HUM I HU1S i HUM C.M4 1.M4 4.m 1.141 1 1.194 1.4M 1 1 1 I.MV I.2M 1.14 4.Ml 1 4.9U 1.412 1 1 1 I MM IIM) HU i 17MM8 tmmt umw I MHI. WIWI M MM M MMfTMM M < MOMS 024667 iiu n iiiim iim m iiiiiiii T*ll_ la MM m aNMCiuttm im mimmi tt caw thim mmi mi mi iwui i-m m mtui ii cokutuinm tamii kM IB t*ta ft Nl CMMMrrtlM In MMpmI fmflft into* Itufw 4 IllfMIlM M|*li HIM KlltS i MINI. MMI NBB utmm mm u cpouimm It u ts M HUM HUM HUM HUff ra n Hum hum mu mi nnn HUM HtttI hum rr If HUM huh rt IM HtttI HUM mim , mm `mam MlnmHN M*M0Hnv fl m m 4*P-Mmmft`tCtJ at M)>m< fi m m M as imuMi ft M m iMmi *t m f! OI*W- MMI Mr. PI HMwyt fft * m PI >tWwt ft m fl pr-MfMnvt ft ft Pf MfUfl PMf-tKIS Mr. IMMwrl PtBMpMNlt OM-M-1Ktl Mr tm mi ON am ini im MM tin fair ftm ma M ttf M mta mm at IM aw i f f f t f f i mr ats St IM am in m am f t its i s t am am tn am m m m am t f Mt f f It] Ml am Mf am m m am m 2*1 IN am am IM in mr mf m m iaa m m Mf in m Ml t IB m MS f t # Mt Ml tm Mf m nr it* Mf tst tm f i I Ml im tm tarn tm Mf M| ur Ml tM IM nr mr Ml ns MS tm Mt tar tm f i f f t t Mt tm M Mt m n tr rr tts tts t MS f t t f rr rr rr tr m n tm n i t t f f ff IT IM n ar n tm at M m m i is f f til ts f f m IM ft fi m u m n i # f tm rt f ff fi Mt m as m a V it f t I f Ml m ft m m ar at m m n tm it it ft tm IM its IM It! tm Mf m tm tm M M sr m Sf fM f n If f ir N M sa m rt *1 M i f f f f sr If a M Sf M rt ta M SI M ff a m ta at M M II M M f i 1 IT n fl M St tt m If SI II f If It II ft Ml IIS fm Mf ISI Mf tm ISA fm 9f t tm i f rt tt f rt tf ftt Mf an tta fl M Sf tt fl a n It if ar a Ml n ft MS ts a Ml tSf Mf tm Mf I* M m i a i f f a a tm M at m m ff m 19 m ft m If ft N rr m M m m m m M tt 1 M i tm f f tit m If m n m tm til tas I t i t f f i m Mf tm tis IM tm Ht tn til tm lf m trr IM M* in tn itr ist tn m HONS 024660 T-U U ItMt If WM|I lllltlvi Nlpf< fKIVI twnfi* fir Ink Cwiwif CtaM OwrMtirliili tolMfM iMpOTM flttin MfNI tapm <rA Irm HWOrt MrM cm nymm m t.m CM Mflno* is cn ttfkmrt m .NO t.Mtt atMtfNmrt KtM 1.011 al#v4 M .MIS aJM^Nnrt or naMpMnvi m out #.113 aWfMvi t .Mil CHM0NN|rf o.oitr cuMfMori tn #.213 aM0NNrt til .ON# CUM**?! til .#3 aM^Mnri tu .111 aWpMwyt #15 INI aiMy# IKOtW .) aSMfMnrt tir .MN1 dSMfMnrl to mu ClSMMvl tit .mm C&OMflMMrt CN .mm acMpMnri tli .mm ttNtpMHyt #22 .mm gitlpMnrf til .Ml alWONl CM .0MN ClMIpMflyf #35 .Ml am#i iicij#2* .Ml cnupmwyt #22 0.00127 aiNiffwrt #2t .MS aibpr> iiciscit 0.0N5J 1.00 .DO .Mil .MS# .ON .Mil .MSI .MM .MSI .MS# .M# .Ml MIN .tin .MM .Mil .MU .NA#7 .MO MOM MMO .MSI .M5tS 0.M3M .ISS O.OKISt 0.M2M o.Mtn Mpm 1tm MOrO .MU .MM .NO .MM .MM .m .MtS .MS .MM .MM .MM .M .1M .Ml .MM .115 .MM .MM 0.M71 .M#27 .OM* .M72 .MTU .MSN .1M O.OMtt 0.MJ17 0.MM5 Iwrip llQ--l tutor .ason .mu .MUM# .MM# .MMN .MMSI .MUSS .MM* .MM# .M7SU .out .17SM .MM .tun .MM# .MM o.mm .NOS .00741 .Ml/ .MSM# .MMSI .MM51 O.OMOM O.OM7 .04021 0.MS4M 0.0MS7 Ovorafo tmiMr .MUM .MM .MOM# .MSM# .MS# .MOM# .MM* .MMM .mu .MMM .MOM .MA7 0.004021 .MS4M 0.MM7 MONS 0i*669 1M mt Ml CMMrMtM Na lllMIttM Mtf tMlflll NMIMU9 uatng . (9r*)tt ISM) Mi Ulll uion H(M) HUS KAMI firas ra-nn i rat mm n tits m. ran * mms m * nw m nm m n. wt m nmim Kt-tm Nt-tiM Mt-ttst m ini ms-hm ra nn imm.) tmm% (^u) <m*u) c*m> <**) /) .1 1.4 1.4 1.1 M 1.3 M . M I 1 1.3 9.9 M M 9.9 I.) 1.4 i.j t .9 r.i 1 9.9 9.1 |.9 #.t . i.r i.i I 9.9 i.i M 9.1 9.1 ts u rr i.r u i.r MS IM 99M9M9 Ml I-Mil rttxu I'lsrii I-MEM it wi It MCI (B MCI ill Mill 1991 1.991 9.919 H4499 9.911 1.999 I M19999 9.1 I HUM 1.199 9.999 1 1)94999 I H4M1 I.M 9.99 ( I119M9 T||tst iaTMpl} were. r>of spiked wiftv SLrroopte, irai 4.9 4.9 4.9 l.t 41.3 41.4 It. 9 HONS 024670 |abl* I1M1 #7 Ivtriff lalitlM InpanM I--1-- ImfKid #-- K--ft tm$*rmr Cto-- CftoroctorlMlt Mitlw --p-- fictan iMpMN Mp-- Irm Irm tM-91 CI1 M|*nrl ft CI1 MM A CI1 MM M awM ocu* awpiM m aM ? aWM 0 aM 0 CtMpMnrl 010 CUMpft--r' *11 aMMi cummv' on aiMpiM *u Ci4ip>wr> CUMffc 1203014 CUM--*! 17 aM fit amfiwyi fit aiMM n aiMM ai (UMM 2 ayWftM f2S CUMM ClMM CtOftipft 12OSf20 uotiMr' ClIObifMnr* Ml ClMtlpH 1203023 o.m 0.10 0.000 *"* .MS 0.400 o .277 .a 0.211 0.230 0.2S . o.mo 0.232 lit 0.0004 i.im 0.0002 0.00M 0.0*71 0.0401 0.0S0S 0.034 0.020 100 0.0)03 0.0271 100 0.209 0.201 0.340 0 0.t07 0.30 0.2M 0.17 0.100 0.101 0.102 0.1S0 0.110 0.131 o 0.0002 0.0447 0.0404 0.0424 O.OS4S O.OSOO 0.0340 0.0142 0.0103 0.021 0.01U o liip--i irm iwOifO 0.210 0.32 0.013 0.101 0.370 0.204 0.S9 0.10 0.210 0.213 0.100 0.10 0.210 0.0770 0.0070 0.0707 0.002 0.0403 0.0030 0.040 0.0420 0.0233 0 0.0320 0.0224 0 Avoroo* np-- 1--1-- 0.277HS o.no 0.011 M0 0.103000 0.302333 o.aoous 0.4 0.100 0.210100 0.213000 0.103333 0.133313 0.100000 M0 0.074400 0.004040 0.0711 0.037733 0.047000 0.047000 0.047033 0.044333 0.023133 100 0.0M7 0.021433 100 Av--aps Can*-- 0-p-M 0.277333 0.4M444 MO 0.31330 0.207777 0.10111 10 o.oooon 0.03000 0.04300 0.023331 too 0.0307 iimn too HOHS 0246 72 NMa 1. KiMriM c* Mtivt TO MCI t tana ta Nontraal Ca^la* Ustnt CtanNarC latraatlan anf MyiU MartuM PttllJ w* NMN2). (Frajaci: riH) It llw MMtlw # 1.4 iim topis ant M It* AcMItlan ( M t U topi* m out Nil: HUIJ it out NU: HUM citiot mm $m ***** coins iwhi cot phi rca-mi it 70*1157 <t 70 2142 It to-iisi it 70*1154 It 70-201 It <8 IK) It ICO IS tees ft MCI ft NCI IS MCI CM a d -tlpMnri Cl M* Cl CM* IS m at-Mpdanrl Cl CM* ct m cs m m CO a ai-McMM Cl CIS CM* C8 Ml ai-MfCmri m CM a a a CM a 07 CtSttfMnrl #1 CM a a * It* cs Ml CU-McManrl ct (Ml m Cl Cl ccs a nr-MfkMvi ct CC4 - Ct m Cil-MCNnrl NT a nf-pipMnyt act a no-tlfpanyt 48 tea ft 115 m 584 9% 04 t M7 12 IO Ct Ml 4 o S IS a ns 47 or 51 254 n 08 m 114 u 1M It is 41 05 tv 114 9M 17 MS 41 MS 47 ttt to 51 to ttt 04 n 40 TV 198 Ct its n its Ct IO M fl TV 1M o 04 71 ft 44 174 111 IO 44 44 M HI ot 114 to 157 117 40 114 to ICS ta lit 04 112 IO M 144 115 29t 02 o 47 1M t 04 02 o SI IIS ttt 545 io 1M m IN ftt SS US 117 u MS 157 171 114 n St 144 ttt 1S5 to vt 14 Itt 47 ISt 174 n St it tl It 1SS ss ft St 51 77 to M MtMMf riwfff ctt a a tipaMnri 4ci) MS 115 It 44 t to CO a 04'O* IlCtl turr. St 77 Ct M Itt At CM a OC-CC-mtS turr. St 44 Ct 52 1M M O CU4-C7-12C1J turr 4 21 21 11 124 24 M MW MIC t l441t t HUM : >14421 : >141)4 : >1441C : H4417 ala Inmriil arc riM ia <p mart Hala iwMr MC3NS 024673 '*< 4aawaflaa af Batlva PCI MMtlana ta NMrM( 10*1aa Uafr latradian ant Inalyala Natda* 7CI11S an! ONUS. (frajacti )J4) It > Ida MNtttan af 2.4 14 ta a Sa^ta anri at Dm Mrfttlan af 24 *4 ta a ta^lt m CMia Mil: HUa IS CM IS Mil: hum it UK m 11 tMfli m m mot as it ok is u M Ki-2in rcs*2tts ks*2isi rcs-tiis is via rt MO It MC) It MC> It MC> It IK) ISM) is Mia It IK) Ml Cl*MfHamrt il ms a m is at n m tt m is MS 14 its m-mm it Ml 12 Ml IS Ml CU-WM**' -l M4 - N MS IS Mr as>MM 11 MS - 12 Ml IS MS Cll*MfiWN|rt It Ml m - M n MS ClMIManrl 11 MS M MS ttl-MpHanyt MT at'MM MS CUS-SMianyt m MS MS MS 144 ft IS? MS 1S4 IIS MS MS 14S M4 MS ISS IS St ns 1 S4 1t 144 MS iss M4 tss MS MS MS MS 14S MS til 144 K 1st ISS its ISS MS ts Ilf 147 1S2 SSS MS 47 iss ISS ss Sit MS SS M ISS 44 1ft M4 It 1st ISS SI ISS m as tss M2 114 MS n ss 1S1 its fl ISS IS ss MS Ml 14S MS 12 4S ISS IS 212 MS 44 SS 144 MS 114 ISS 41 4t 141 M7 tst M4 K 14 12S Ml ISS ISS IS S7 S4 Ml 1st MS 44 7 m S4 ss ISS 71 s IS MS ss MS M 12 44 111 St MS IS 14 s MS 2t IK 44 11 41 1S4 24 MS IS mmosaii mww--t m l-a-Mpkaivl-ICIS S 0 S 4 S 4 #14 CU-M-IXII krr. s 0 4 4 4 MS a aS M fXII Surf. s t 0 S 4 S MS CIIS'M'IICIS Swrr # 1 4 4 4 4 NS ISM Pill : >1444) : 144tt : >14451 : >14442 : >14444 :: H44J1 Ml Iwsvtriii ara rtwM la Ida naara iSela nuMar HONS 024674 Th following pagoa daacrlba Standard Sampling. Extraction. and/or Analpala MOthoda uad for ehia projoet. MONS 024675 ESC Standard Analysis Method (SAM) ESC Standard Analysis Mathod Mo TITLE: Polychlorinated Coapounda In Solvents NSAR23 ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-59S5/59S7 Capillary GC/NSSalacead Ion Monitoring with RTE-TI operating syatea. Typical Run Tina: Typical Multiplier Voltage: Typical Dwell Tlaaa: Maxlaua a of Maaaea: Electron Energy: IS 40 aln. 1100 - 2(00 eV 100 - 300 aaac/aaaa 20 aaaaaa x S rangaa - 100 aaaaaa 70 aV TYPICAL ANALYTE TYPICAL INSTRUMENT LEVEL OF DETECTION (L0D) (ug/al) Organic Coapounda eluting between toluene and n-C3A-ane 0.01 0.1 TYPICAL PRECISION 10X LOO (9) SO TYPICAL ACCURACY t 10X LOO <%> SO INTERFERENCES AND LIMITATIONS: Analyte eharacterlatlc aaea auet be chreaategraphlcally reaolved fron ether eluting coapounda which produce the aaae aeaa. CHR0MAT0CRAPH1C COUM: 30-aeter fuaed a 11 lea JUI DE-9 (0.23 tdf) wlch wide bora (0.S2 aa) COLUMN TEMPERATURE PROCRAM: SO(4)/(/SOO INJECTION TYP1: Splltleeo CALISRATIOH AND STANDARDIRATION: Quantitative: Uae Internal atandard quantitation technique and calibrate lnatruaant reaponae factora froa atandard aelutlona of analytea of lntareat. Qualitative: When aultlple eharacterlatlc aaaaaa are aonltored far a given analyte, the ratle of eharacterlatlc aaaa reeponaea anat be within 20% ef theaa for the authentic atandard. Per PCI analyaea. the eharacterlatlc aaaaaa idllch are aonltored are the aelecular ion containing all 35-CL laatopea and the eolecular Ion containing one 37-CL laotape. The fallowing cable auaaarlaea the aaaaaa and approxlaate retention tine reglone aonltored for the analyala of Internal atandard, aurrogata atandarda, and ehloreblpbanyl (CL-IP) through dacachloroblphanyl (CL10-SP) PCS congeners. HONS 024676 T ttt Analyca Haases Retention Tines (aliiutes) Relative Retention Tinas (a) CL'BF 1jooer*, anthracene-dlO 4-CL-(P-(C13 surrogate CL2-BP laoaara CL3-BP laoaara CU-BP laoaara 3,4,3',4'-CIA-BP-12C13 aurr. CU-BP Laoaara CLB-BP laoaara CL7-BP laoaara (b) CLB-BP laoaara 2,2',3,3',3,5',.(-CLB-BP-12C] CL9-BP laoaara CLIO-BP CL10-BP-12C13 aurrogaca 188,190 194,19( 222.224 255.9.237.9 2S9.S.291.S 301.S,303.S 323.9,323.9 337.(.339.8 323.9,323.9 391.8,393.8 427.7.429.7 439.7,441.7 4(1.(,4(3.( 497.(.499.4 309.(,311.( IS 22 15 22 IS 22 15 - 30 22 * 30.5 22 - 30.5 22 30.5 22 30.5 22 30.5 30.5 40 30.5 . 40 30.5 40 30.5 . 40 30.3 40 30.5 40 0.40 - 0. 0.(0 0. 0.(0 - 0. 0.(0 - 0. 0.S4 - 1.12 0.B4 - 1.12 0.84 - 1.12 0.14 - 1.12 0.(4 - 1.12 1.12 - l.87 1.12 - 1.(7 1.12 1.87 1.12 - 1.(7 1.12 1.(7 1.12 - 1.(7 (a) Relative katanclon Tlaaa calculated ualng a rocanelan claa of 2(78 alnutaa for 3,,l',*'-CU-IF-((. <b) CL7-8P laoaara ara analysed ualng olehar CL2-loaa charactorladc tana (/a 323.9 and 323.9) or aolaeular Iona (a/a 391.( and 393.(). CALCULATIONS: Analyte caneancraclon - (Analyca area)/[(Analyca (APHIS araa>| uhara: Analyca araa la tha eharaccarlacle aaaa araa af eha analyca. U7 la cha relative reapeneo factor far tha analyta. IS la cha Internal ecandard and la uaually anchracana-dlO. U7 - (analyta araa In standard)/!(analyta cone.)(IS araa)I PCS eoncaneratlona ara ealeulacad In ona of ewa waya: 1) If an Araclar famulatlan can ha ldanclflod fran eha paccarna af PCS laoaara, aalactad PCS laaaors ar claasaa of laaaara (1. a. all CLA-blphanyl laoaara) ara used to quantify tha Araclar concentration. Relative Kssponaa Paetara ara ealeulacad using tha eaneantratlen of eha total Araclar fornulaclen In eha above (IT aquation. 2) If no unique Araclar fernulaelan la praaane, chan tha total PCS concentration Is calculated by using standard selutlone containing kneun ansunts af chlarablphanyl through daeachlorohlphanyl laanars ca calculate Kalaeloa lasponaa feeCoro far each chlorine class In eha above (IP aquation. Tha Ora far tha corresponding PCS 1sonar elassaa ara used ta calculate total KB laaasr concentreclone of each class In unknown aaaplaa. I For aora Intonation regarding standards saa Supllnane ce MSAN23 on cha following page.) SAPITT PRECAUTIONS: Saa PCt handling preeacela In laboratory safety nanual. DATE Of METHOD CREATION: 12/9/(3 Tina Scanp - <S71012.1S12> Tina Scanp - <871012.1S12> HONS 024677 SuppllMneal Information to Standard Aiuljaia Method HA1V23 Intarnal Standard Anthracene*dlO Surrogate Spiking Conpounda C-13 labolod 4*ehloroblphenyl 13C4 3,3*,4,4'totroehloroblphonyi 13C12 2,2',3,3',-oetaehloroblphenyl deceehlorebiphenyl 13C12 Native Spiking Conpounda (uoad for natlvo aplkoo) 2 --noehlorobIpheayl 3 --nochloroblpbeny1 4--nochlorobiphonyl 2,2' -dlchloroblphofiyl 2.3~dlchloroblphenyl 2,4*-dichloroblpbenyl 4,4'dlehloroblphenyl 2,4,4* trlehloroblphenyl 2,3,4* trlchloroblphenyl 2,4,4* trlchloroblphenyl 2,3' ,4,4,-tetrochloroblphonyl 2,3,3,4,tetrochloroblphonyl 2,2 *, 4,4 , * tetrochloroblphonyl 2,2* ,3,4,3-pencochloroblphanyl 2.2* .3.4.3>.peneoehlereblpbeiyl 2,2',4,3,3*pentoehloroblphenyl 2,2' ,3,3' ,4,4'*hasaehloroblphenyl 2.2' .3.4,4* ,3'~hexachloroblphenyl 2,2*,3,3',4,4'-hemochlorobiphenyl 2,2'3,3',4,4*,4-heptochloreblphenyl 2,2*3,4,4',5',4-heptachloroblpheayl 2,2',3,3',4,4*,3,3*-oetochlorobipyhenyl 2,2',3,3*.4,3,3,',4,4'-nonochloroblphenyl deeechloroblphenyi Characteristic end Confirming Masses Monitored Choreecerisclc (AMO) anthracene*dl0 4-ehloroblphenyl 4C13 US 194 Confirming (AMD) 190 19* HONS 024670 d1ehlocobiphanyIs trlchloroblphanyla eatraehlorobtphanyl* paneachloroblphanyla h&aehloroblphnyla haptachlorobiphanyla oceachloroblphnyl> nenehloroblphnyifl dcchloroblphanyl 222 295.9 289.1 329.9 357.8 323.9 427.7 481.8 497.8 224 297.9 291 8 325.9 359.8 325.9 429.7 483.8 499.8 HONS 02*679 flow sun nu rot ISC AMLTS1S UTHOD HSAM5 EXTRACT ID: ESC EXTRACT IDG NQ: HS LOGBOOK TAG! RUMSIt: .......... EXTRACT COLOR AMD DESCRIFTION CALIBEATS HASS SPECTROKETER | ] with rrriA and demonstrate . CATILLARY CHEOKATOGRAFHIC . resolution with ststih . rnroRKAMCR standard . riACt IN A I.S iL AUTOSAMTUR VIAL THE SAHFLE EX TRACT OR STANDARD SOWTIQN CONTAINING KB C0NCEN1R5 WITH ISO uL INTERNAL standard soumoN. THE INTERNAL STANDARD SOLUTION USUALLY CONTAINS 10 OC/aL ANTHRACENE-D10 IN CH2CU OR BSNXXm. FLACI VIAL IN AUTOSAHFLER TRAY OF HF-SMS/17. RECORD NASS SrECTRONRIRlC AND CAS CUOKATOCRATHIC 0MRAT1NC FARAIfETIRS IN INSTRUNENT LOGBOOK. [] . (| CALCULATE CHARACTERISTIC ION AREAS or ANALYTES OF INTEREST AND ANTHRACENE-010 INTERNAL STANDARD. .............( ! [ 1 CALCULATE CONCENTRATION or ANALYTES or INTEREST USING THE FOLLOWING EQUATIONS: FC1 Chlorine Claaa Concentration Chlorine Claaa SET (Chlorine Claaa Ian Area) (Chlorlna Claaa REF) (Intarnal Standard Araa) (Charaetarlaele Ion Area for Chlorine Claaa) (Chlorlna Claaa Coneantration)(Intarnal Standard Araa) Total FOB - CL1-SF Coneantration CL2-BP Coneontratlon * Coneantration CU-BF Coneantration * ... * CUO-BF Concentration HS FILE NUMBER: ................................. OATE/TIME COMPLETED................................./ ANALYST: ........................................................ ESC JOB NO: ................................................. HONS 02A680 METHOD riLE LIST Machod flit: PCSC2S Taaparacura: Sourea 200.0 CC typa: 5040 CoLusn: Cap Iaoeharaal If Run Typa: SIM, Splielass: Yas Post Run Tlaa 0.0 CC, El Run elaa: 40.00 Scan Scare tlaa 15.00 Rtlay l: Rtlay a2: TrUc *0: Trite al: Off 327.0 327.0 327.0 327.0 OFF 327.0 327.0 327.0 327.0 ON 327.0 327.0 327.0 327.0 OFF 327.0 327.0 327.0 327.0 Sla PiruMtears: Nuabar of groups: 3 Multiplier *oltaa: 2(00 Kalatlan current : 300 uA Croup l Croup 2 Croup 3 Croup 4 Group 5 Seare/Stap 13.00 22 30 Scart/Seap 22.30 30.30 ICart/Etep 30.30 *0.00 Se*rt/feap 0.00 0.00 Seart/Seop 0.00 0.00 H/Z Dmll H/Z Dmll H/Z Dmll n/z Dvall H/Z Dvall 101.0 100 -233.9 100 -391.1 100 190.0 100 -237.9 100 -393.1 100 194.0 100 -2(9.1 100 -*27.7 100 194.0 100 -291.( 100 *29.7 100 222.0 100 -301.1 100 -*39.7 100 224.0 100 303.1 100 -**1.7 100 255.9 100 323.9 100 -(*1.* 100 257.9 100 -323.9 100 -**3.( 100 0.0 0 -337.( 100 -*97.( 100 0.0 0 -339.1 100 *99* 100 0.0 0 -(39.7 100 309.( 100 0.0 0 -*41.7 100 -311.( 100 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 HONS 024681 ISC Standard extraction Hathod (SOI) TITLE: PCBo In bate hydrollxabla or lonlaabla aatlcea ESC Standard Extraction Method No: PCXX13 NATKI(X). (CIS): Chealcal products which are base hydrollxabla or lonisabla, la. ehloro acetyl chloride, chlero phenols, foralc acid, ate. TYPICAL SAMPLE SIZX (I) 0.9 Is TYPICAL OtTIACT VOLUME (al) 1 - 10 TYPICAL AMALYTES:A1232.A1242,A124I,A1234.A12(0 and A1262 and PCI laoaari none through deca-chloroblphanyl. INTESPUklMCXS: Any alactron capturing apoclaa In eha ratantlon elaa ragion of aonochloroblphenyl lioaan through dacachloroblphanyl lsaasrs for ECAM01 and ECAM02. Any apoclaa la the approprlata ratantlon tin* ragion which give the aana relative characterlatlc eaaa taaponaaa aa PCI laaaara for NSAN03. TYPICAL SUK10CATXS TYPICAL EECOVEBIIS () psntachlorobansans 2,4,(-crlehlsre- blphenyl 3,3*,4,4*-Cotta* chloroblphanyl*di 30 120 30 120 30 - 120 APPAEATUS AMD MATHXAU: Eurdlck and Jaakaen hananc far antractian solvent. KM aelutlena of variant atrengtha far hydrelyela and Ionisation of chealcal apoclaa such aa athera, acid chlorides, aclda, esters, etc. Silica gal coluana lapregnated with potasslua peruanganats, sulfurle acid, and potasalua hydroxide. Disposable glassware. (See flow sheet for chls extraction aethod In PCTS13.I UMITATIMS: Method applies only to aatrlcea which conCain hydrollxabla or lonisabla alactran capturing apoclaa In the aonochloroblphenyl through dacachloroblphanyl ratantlon tins ragion for EC dactlon aethoda. SAPITY PKECAUT10M: See PCS handling protocols In laboratory safety nanual. OATES OP NEIHOO CUATIM AMD UPDATES: 7/23/S4 MQNS 024602 flow shut rersij FOR ISC EXTRACTION METHOD PCEX15 SAMPLE ID: EXTRACTION DAT! And TIMS: MRC EXTRACT LOC NO: .............. VtlGH OUT SAMPLE INTO A 1* OR 40 aL VIAL (] WEIGHT SANTLX (1 g) SUUOGATE SriXE OF SAMPLE SPIKE ADO------ aL--------- KOH AND SHAKE NOTE baaa ahauld ba addad ilwljr or gridualy to avoid vlolont roactlona [] . . . . . REMOVE EXTRACT QUANTITATIVELY{ ] WITH S X 4 aL HEXANE RIMES . REDUCE SAMFLE VOLUME TO . 3-4 aL WITH NITROGEN AMD () AFFLY TO comm quartitativly . AMOUNT AND CONC. OF EASE ADDED [ ] RINSE COLUm WITH 2 X 20 aL . HEXANE comm DE3CRIFTI0N 23 aL DISFO FIFET I ------ 1 1 ca Na SO ----I 24 I I.....................4 ca It POTASSIUM | PERMANGANATE | SILICA CEL I ca SILICA GEL ELUTE WITH 40 aL HEXANE NITROGEN SLOW DOWN TO 1 aL [) [| 4 ca ACID SILICA CEL 1 ca SILICA CEL 4 ca BASE SILICA GEL \XXX/ \/ GLASS WOOL EXTRACT NO:................................... DATE/TIME COMPLETED................................./ ANALYST: ESC JOB NO: HONS 024683 Th following pi|'* *l>e calculation* or raw data doccaantatlon of raportcd rsrales. HOhS 024664 M'3 data file header from >L4413 p If IvL ISO ISO D10(10UC Operator MmSON hi sc ML) HS SPIKE (DIL 1 10) *21 *S2 BrL#2l ?/ 12/a 5y" MS model 87 SW/HW rev IA ALS * **t Method file PCSC2S Tuning File HTQ602 No of extra records Source temp 200 Analyzer temp 0 Transfer Line temp Chromatographic temperatures Chromatographic times, min. : Chromatographic rate, deg/min : 0 00 00 0 00 0.0 0 00 00 0 00 oo 0 00 00 HONS 024605 5000 4 0 0 (J- 400000 14 3 27 321 t JlK^J L__ ________________ u? 912 t , - 21 .0 21.2 21.4 ' 21.6 21.9 22.() 22.2 22.4 = UW and 190) pi 3000-] 1994 L 4094 194e| JtJhk_ 11372 4999- 5169 5804 4 /L, ?> 17.6 16.9 19.4 19.9 19.2 19.6 29.9 ludand 190)12-14 2500 2800 4699* . , 27 19 .1 74 53 i 2999- 1 | 1 1 1 | i i i > f 18.4 19.6 13.2 13.6 1 P 9| 29.9 4999 2999- 4 999 2999- 19.2 2660 i i4369 19.6 29.0 5442 1 3796 1 3A 3733 Li 5992 29.4 29.0 21.2 21.6 5393 i 36 ?9 22.9 22.4 HONS 024686 4499 1 5`5'Sl37 _iL 30di 2W 3449 5"-*501 111 1 i i m i r * r i i i i i I i i i i i i v i i i i i i i i i1^ 1 . . 24.4 29 >9 21.2 2t. 22.0 22.4 22.0 23.2 23.0 24.0 7TTS /iPJPMfl'L <^,5'9 & zvl'^ * **> *-*a c-toej lY* `ttfcr JLjl200<>j -1 fw H 11 n | ii n |m 11 i ii i| iWl |li il 11 i*6^ii .................... ............ HONS 024687 i .................... .... i| 2S.S 26.0 26.5 27.0 27.5 23.0 28.5 23.6 240*. iioe- l 365 i 1 ri_.r 3 62 i ,4 Trr _...mr n.v 1 T _L ?4r i 537 (.4 145 26.5 27.8 27.5 28.8 28.S 28.0 mmm waTM * 20.5 38.8 2ee* *' -- 602 aM A.^k A N. ,s* -- 3i '32 A A rv 3 333 A2900- k 29.2 29.4 29.6 29.8 38.8 38.2 38.4 wmmwi (mi,::i'j * 'jz5-y> ***-* 20OO- 3. "4 -29 --.-3l ISO* 2000- k JL 473 ** . 31.2 31.6 32.8 32.4 32.8 33.2 33.6 mmm m,7-7 ^ TM-T> **> 2623 . i. . 2000- a?02900- 1,.,. M,,,, 2133 ^A HONS 02M4688 29.2 29.4 29.6 29.8 38.0 30.2 30.4 38.6 38.3 mNttmm4*7 *** * 200* ia*o31.8 31.2 31.4 31.4 31.8 32.8 5 33 A-r-32.2 32.4 ' 32.4 ' -32.8 ' 190* 200* . 33.2 33.4 30? 34.8 399 m. 34.4 __ 34.8 -280* I W___ 1912 _ r, r290* 33.2 A--n , - - 33.6 34.9 34.4 34.3 mmpp-Mm <TM-6 nd 5iL6> ** HONS 024609 R'J,WAIT , 15 DiJ^CMU,! M III M I II | | t m I I i I M I I i I III THE FOLLOWING OUTPUT I I I I I n I II I I I I I I I I I I II I I I I I II I I M I I II { I I i i I I I ! I I I I I I | H M I l i t M I M I I I I I i I ! i i | I IS FOR the SAMPLE SHOWN IN THE mi LOSING nrftogp I I I I I I I I I I l I I II I i I I I I l I I I 1 I II I I I H M ! I II M I I I l I i | II | MS data Til header from >L44i3 Sample 1'jL ISO ISO DlQtlQUC Operator MASON Mite ML) HS SPIKE <DIL MO) *21 M32 *TL#21 9/12/87 0 Sy*. 2 MS Models 87 SU/HW reu IA ALS * *** Method file* PCSC2S Tuning file; MT8602 No of extra record* 4 Source temp. 200 Analyxer temp.: 0 Transfer line temp 0 **3 " Chromatographic temperatures 000 Q o Chromatographic times, min. 00 00 00 00 D U Chromatographic rate, deg/min 00 00 00 00 00 Anthracene-diO Area * 1197912 and Std. Cone = 10 ug/mL ii m i 11 i 111 n i i M ii I 1111 i i i i i i it m i i n i 11 n i 11 m i 11 u i m i n i i m m m i m 11 i n The following output uses the following definitions for Compound Number toi 102 03 04 oos 06 07 ooa 007 10 ii 12 *13 *14 US 016 17 in 017 20 *21 22 23 124 025 126 27 028 27 anthracene-dlO (m/e 188 area and m/e 190 area) CL-biphenyl *1 (m/e 186 area and m/e 190 area) 2 (m/e 168 area and m/e 190 area) " *3 (m/e 168 area and m/e 190 area) 4-CL-biphny1-6C13 (m/e 194 area and m/e 196 area) CL2-biphenyl 1 " 2 (m/e 222 area and m/e 224 area) (m/e 222 area and m/e 224 area) 3 (m/e 222 area and m/e 224 area) " 4 <n/e 222 area and m/e 224 area) CL3-biphenyl 1 (m/e 2SS 7 area and m/e 2S7 9 area) 2 (m/e 255 9 area and m/e 2S7.9 area) 3 (m/e 2SS. 7 area and m/e 257.9 area) CL4-biphenyl 1 (m/e 287 . B area and m/e 291 8 area) * 2 (m/e 287 8 area and m/e 291 8 area) " 3 (m/e 287 8 area and m/e 271.8 ar ea) CL4-6P-12C13 Surr (m/e 301 8 area and m/e 303 0 area) CLS-biphenyl 1 (m/e 323 9 area and m/e 325.9 area) " 2 (m/e 323 9 area and m/e 325.9 area ) 3 (m/e 323 7 area and m/e 325.9 area) CL6-biphenyl 1 (m/e 357 O area and m/e 359 8 area) 2 (m/e 357.8 area and m/e 357.8 area ) * 3 (m/e 3S7 a area and m/e 357 8 area) CL7-bxphenyl 1 (m/e 323.9 area and m/e 325.7 area > " 2 <m/e 323 7 area and m/e 325.9 area) CL8-biphenyl (m/e 427 7 area and m/e 427 7 area / CL8-6P-12C13 Syrr . (m/e 437 7 area and m/e 441 7 area > CL9-blphenyl <m/e 461 6 area and n/e 463 b area) CL10-blph*ny1 <m/e 477.6 area and m/e 499 6 area > CL10-BP-12C13 Surr (m/e 507 6 area and m/e 511 6 area / Compound CHRCTRSTC/dlO CNFRMNG/dlO Number (X 10) (X 10) Compound RATIO CHRC/CNPRM Delta-RT <x 100) ICLs om 0*12 )03 i) 0 4 005 006 007 000 007 010 10 00 0432 0 185 0949 0664 0364 0734 0493 0725 0288 120 01S1 0162 0334 0227 0222 04S8 0316 0443 0375 .0QE+Q0 0OE+00 OOEHJO .00E*QO 00E *-00 . 0 0E + 00 0136 00E*00 OOE+OO OOE+OO 8355 39 206.53 1 298.25 1 294.02 1 292.50 1 163.91 2 160 31 2 1SS 89 2 163 87 2 76 82 3 HONS 024690 Oil 012 Oi3 014 015 '1 V6 017 oin 01? 020 021 022 023 024 025 026 027 02U 02? 0326 0322 0160 0123 0162 0218 0115 0091? 0106 00720 00627 00490 00720 00783 0039? 0183 00491 00317 0 0845 RIJ,CR1\,AL,FF . 0423 0433 .0164 0135 0177 0173 0202 0164 0177 0114 0079? .00791 00503 . 00528 00489 0219 00522 00258 00488 . OOE+OO OOE+OO 00E*-00 Q0E+00 OOE+OO 00E 00 OOE+OO 00E+00 QOEtQO OOE+OO - 0204 OOE+OO OOE+OO OOE+OO - 0204 OOE+OO OOE+OO OOE+OO OOE+OO 77.55 3 74.44 3 97.56 4 ?4 50 4 91 66 4 126 15 4 56 9 Li 5 56 03 5 59 65 5 63 IS 6 62.74 6 61 99 6 143.19 7 148 42 7 81.57 8 83 26 8 94 08 9 122.98 10 173 29 10 HONS 024691 Tho following pogot (how chaln-of-cu*tody Information for this projact HONS 024692 Mnwnt C|N m. 429, 'ue ft. Metrxb September 15, 1987 Monsanto Company 800 N. Lindbergh Boulevard St.Louts, Missouri U.S.A. 63167 Attention: Mason Hughes ^0^ Re: Maste Plasticizer Mr. Hughes: Enclosed ere samples 108, 108-8, 110 and 110-8 for PCI analysis by GC/mass spec. As per our conversation, I have separated the organic (top layer) from the Mater phase (bottom layer). Sample 1108 and 110 contain the top layer, and sample 108-8 and 110-8 contain the water layer as well as solids. The organic phase contains long chain (CT-CU) esters of phthallc acid (PAE). It nay also contain traces of adipic acid esters. The aqueous phase Is mainly water containing grey-white settleable solids. The solid phase Is filter aid (dlatomeceous earth) containing approximately 301 of absorbed plasticizer asters. The charge nimfcer for this work Is 04-000-1910906. If you have any questions, please do not hesitate to contact me. Sincerely End. MOWS 024693 Monsanto CANAOA INC. si.iso*r>ct iu*fusviNrc toutft'to OCMkNOf M Christian Roy s* TO: . iiNmiu MORSAHTO COWARY owraicT aus omn aunc/wx oc vent kcoouux O3B *AQBiTU>0 .>0 K 717 STXtTrjlrttU. MOSIMAUO*. OWT UM2QA Kill RUBI mil M-21NSI < "Ul ST-PATWCX. LASAU.I. OUfMC HflN JHJ (*>> Ml 10 TCI.EX Ml mil <*mvtnaioano. 2. wonrom ic vzsma 1104) HS-4S73 TEUX; Mm S*ptb*r 15, 1587 800 R. Llndbirgh Boulavard - Bldg S Ricilylng St.Louis, Missouri, U.S.A. 63167 ATTENTION A (.'ATTENTION OE Mason KRMtl Npyw Hughas my-- (U4E) {tIRyInRyW SHU VIA: Tn cT nrYomi aa |_| ass TfLI^HONlQ ZS? K.W ______ Wasta Plasticizer Oil (saavlas for experlaental purposas) iutok stoca""? STOCK EM( l Sample Order Commande d'echantillons NO CHARGE ATITREQRATUIT %7c9/6 AtLay*,- f7oc)/^- loP ' n'09.Hf &TT T0P ^ Monsanto JU^uxo\ 0 //& wncu+jj /OZ 4 fot CUSTOMER'S CORY / COPIE DU CLIENT MONS 024694 Monsanto MMsoaftw CanaM inc. September 3, 1987 Monsanto Company 800 N. Lindbergh Boulevard St.Louis. Missouri U.S.A. 63167 Attention: Hison Hughes Re: Haste Plasticizer ^7,0 </ Enclosed ere seaples *101 end #102 for PCS analysis by GC/mass spec. As per our conversation. I have separated the organic (top layer) from the water phase (bottoa layer). Sample # 101 contains the top layer, and sample # 102 contains the water layer as well as solids. The upper organic phase (#101) contains long chain (Cj-Cj,) esters of phthallc acid (PAE). It may also contain traces of adipic acid esters. The lower aqueous phase (#102) Is aalnly water contain ing grey-white settleable solids. The solid phase is filter aid (dlatoMceous earth) containing approximately 301 of absorbed plasti cizer esters. The charge maaber for this work If you have any questions, please do not hesitate to contact Myra Plotnlck Industrial Hygiene Chemist HONS 02*695 SALKS 0*CI U*CAU Of VCNTE Monsanto CANADA INC. zMoISgSAISWSOAEUHGTAiAOMNOT. UrMq XsJo4x 797sr^pffrsvsxt. <41# *3+9322 TELEX 0.}tMSt 42S RUE ST RATRICK. LASALLE. OUESEC MEN 2KJ (St4) 399-4900 TELEX OM <EJ4 494 RIVERSIDE AO R R 2. AMQTSFOAO 1C mtf (604| 993-4973 TELEX: 04-3E3S33 RMtnetv^uNHuZioi Myra Plotnlck JHt# TO: , surSort"* MONSANTO COMPANY 0* T| Seotwber 3, 1987 800 N. Lindbergh 8ou1everd - Bldg S Receiving St.Louis. Missouri, U.S.A. 63167 T/T/T? *Ltt9*'tWLi ,4r ATTENTION ,, u. A L'ATTENTION OE M,,on ""S"** (U4Eiw pWCHMSI '** hesauiA 'WMNl HhUMW If# uwS*nr*nD HINW WWW C4wrr*r M"** RW mtxM 53 mknrdon tclcphoncai. i^ifcnhirnU: W'WWM oTuOoC***t*tVo'c*t Lo>iiviAvW(aYOiMiMMCtVTU9to I'WWrtS* WL0MTENAOT Sample Order 2 Neste Plestleizer Oil Commande (seaplts for experleentel purposes) d'echantillons NOCHARGE A TITRE GRATUIT Monsanto l CUSTOMER'S COPY / COPIE DU CLIENT HONS 024696 Tha following pagas dascrlba Analytical laqnatt Information for this project. MOMS 02469? Tlaa Scaap - <071012.1621> MONSANTO COMPANY/ENVUONHZNTAL SCIENCES CENTER A1ULTSIS REQUEST DATE: Sapeaabar 0, 1907 LOG NO: U-07-09-00-02 REQUESTER: Myra Ploenlck/Canada LOGIN NOTEBOOK PACE: 3759209 PROJECT NO: 70O.34-703* REPORT RESULTS TO: FILES/HEU.HUGHES,SHEJWAN,HCXDIZIE,MINOR ANALYSIS REQUESTS SENT TO: FILES HESS,SHERMAN,HUGHBS.HCKEKZIt.MINOR SAMPLE PICKUP BY: MINOR SAMPLE LOCATION: U-A20 SAMPLE DESCRIPTION FOR 2 SAMPLES SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC NUMBER(S) 101 UPPER ORGAMIC PHASE 1 X 30 aL PCS-21*9, PCB-2150-DUP PCB-213UU, PCS-2132+HS 102 MATER CONTAINING CRKY-WHITE SETTLEABLE SOLID I X 30 aL WATER ONLY PCS-215*. PCB-21SJ-0UP PCS-213+LS.PCS-2157*HS SEDIMENT PCS-2139, PCE-2M0-DUP PC1-211+LS. PCR-21t2*HS NETHOO BLAMK(S) PCB-lltS, PCB-216* RECORDED BY: MINOR REQUIRED ANALYSES: PCS (Incidental) EXTRACTION LOGBOOK NOTEBOOK PACE: 151639 UC STANDARD EXTRACTION METHOD(S): PCSX13 ANALYTICAL TECHNIQUES: TECHNIQUE (EN) DATE COMPLETED ESC STANDARD ANALYSIS METHOD INSTRUMENT LOCBOOK PAGE x- CCCC/HS ( ) 10-12-07 MSAN25 157533-15733* FINAL REPORT NOTEIOOK FACE: 34*04*5 OTHER NOTEBOOK PACES: QUALITATIVE: X SEH1QUAMTITATIVE: QUANTITATIVE: X REQUIRED QA/QC: SEE GOOD LABORATORY PRACTICES MANUAL COMPLETION DATE REQUESTED: MOMS 024698 COMMENTS: SAMPLE DISPOSITION: HOLD FOR 90 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME:AA7634 HONS 024699 Tin. SCaap - <*71012.1S19> MONSANTO COKPAMY/ENTIRONMENTAL SCIENCES CENTER ANALYSIS REQUEST DATE: Sapcaabar 11,1917 LOG NO:U-S7-09-18-02 REQUISTEK: ROY/MONTEIAL PROJECT N0:7*0.2*-763S LOGIN NOTEBOOK PAGE (To bo flll.d out at login. >: 3759212 REPOST RESULTS TO: F1LES/NEES.SHEEHAN.HUCHES,MCKENZIE,MINOR ANALYSIS REQUESTS SENT TO: FILES NEES.SHERMAN,HUCHES,MCKENZIE SAMPLE PICKUP BY: MINOR SAMPLE LOCATION: U-420 SAMPLE DESCRIPTION FOR 4 SAMPLES SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC NUHBER(S) 170913 BOTTOM LAYER 110-B 1 X 40 oL HATER ONLY PCS-2114.PCB-21I5+H5 SEDIMENT PCB-21BB, PCB-21S7+HS B70915 TOP 110 1 X 40 aL PCB-2171, PCB-2179+HS B70913 BOTTOM LAYER 10B-B 1 X 40 oL WATER ONLY PCB-21S0. PCB-21IUHS SEDIMENT PCB-21S2. PCB-21S3*MS 870913 TOP LAYER 10B t X 40 oL PCB-2173, PCB-2174-DUP PCB-2175+LS. PCB-217S*HS METHOD BLANK PC*-2 US RECORDED BY: MINOR REQUIRED ANALYSES: PCSa EXTRACTION LOGBOOK NOTEBOOK PAGE: 13BB40 ISC STANDARD EXTRACTIOH NXTHOO(S): PCZX15 ANALYTICAL TECHNIQUES: TECHNIQUE (EM) DATE COMPLETED ESC STANDARD ANALYSIS METHOD INSTRUMENT L0C100K PACE X CCCC/MS ( ) 10-12-17 NSAM25 157533-157334 FINAL REPORT NOTEBOOK PAGE: 3440446 OTHER NOTEBOOK PAGES: HONS 024700 QUALITATIVE: SEMIQUANTITATIVE: QUANTITATIVE: REQUIRED QA/qC: SEE GOOD LABORATORY PRACTICES MANUAL COMPLETION DATE REQUESTED: COMfENTS: SAMPLE DISPOSITION: HOLD FOR 90 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME: AA73S:U MOMS 024701 Tha following section* daacrlba Important terminology used in Quality Asaurance/Quallty Control, Analyte Extraction and Instrumental Analysts. tfl6 and KtC/QM Good laboratory Practices Manual* ean ba obtainad by eon* taetlng Janat Laa (040) KITE 344-1273, CLP and QA/QC Supervisor. MONS 0^4 702 Quality Assurance/Qualley Control Terminology This taction describes commonly used esralnology and phraso* which arc uaad In eonjuneelon with Quality Assurance/Qualley Control (Qa/QC). This infernation aay be helpful in understanding soma datails of QA/QC proeoduraa which havo boon Incorporated in tho proaont roport. Tho following two tac tions also giro usoful information eoneomlng tarminology uaad In analyca axtractlon and instrumental analysis of sanploa and saapla axtraees. Quality Aesuranco/Quallty Control - Terminology used to describe aceivltlas which are designed to produce analytical results af known quality In an effort to mlnlmlro coots of environmental analyses, specific QA/QC elements have been incorporated Into BSC/UAG exerection end analysis seeps which should not undusly burden analytical seudles with large development and method validation coats. This approach has been taken so that sets of samples ean be analyzed for various analytes without extensively validating methods over wide conceneraelon ranges end without using methods which are designed for only one aaerlx. One pries which one pays for this approach Is that analytical pre cision and accuracy ere sacrificed, somewhat. However, in many eases, whan clearly defined regulatory limits have been set, confirming that the analyte is present at levels well below or well above the limit does not nood tho typo of accuracy chat is required when the regulated analyte concentration is in the vicinity of the regulatory limit. In these latter esses, more extensive QA/QC pro* eeedures are required than are Included in the present study. Frselslon - Terminology used to evaluate the roproduclblliey of a certain determination. Parameters which affece analysis praclalon range from aamplo acquisition, to sample storage, to sample extraction, and finally to sample extract analysis. Normally, cha major faceor which affects the precision of the analysis Is ths sample extraction seep. This step normally rosults in sample analysis precision on the order of or 30%. The precision of a result can ba determined In e number of ways Replicate analyses of the seme sample, followed by the calculation of a percent relative standard deviation for that determination is ths most popular method of assessing precision. However, this cal culation should not be made when there are less than three replicate points from which to calculate the percent relative standard devia tion. In addition, replicate extractions end instrumental analytes must be performed. Therefore obtaining percent relative standard deviation data ean be very expensive and is not normally obeainsd un its* large studies ere being conducted. A second cached of assessing precision is with Che use of duplicate analyses. The presene reporc includes rssults of at Isaac one sample which was analysed In dupli- eat*. WQT1I i It 1. eh. r.non.lbUltv of th. n.lvl. nauaitor to rvtw th... H.c. .~t M. ~~ ennc.mln. th. nr.ei- <I" of eh. dc.TMiaElan. ind. or. iartntlY. If eh. pr.cl.iUn af th. rf.fc.giln.clon --1 hi. nd. (continued) HONS 024J03 Pag* 2, Quality Assurance/Qualley Control Terminology Accuracy - Terminology used to determine tho "correctness" of eho doc* Th* accuracy of most stops In cho analysis of samplss la typically on ths ordar of 10%. However. whan anaiyca concsncrsclons In cho ssisple extracts approach tho lsvol of dotscelon of s determination, accuracy as wall as prods ion can approach 100% or greater. Tho accuracy of a determination of an analyte which is prosont at concentrations which aro such greater than cho instrumental level of detection is most strongly affected by the homogcnloty of the sample matrix end the precision of Che extraction step, whieh results In typical accuracies in environmental analyses to be on the ordar of 30%. Normally, the aeeuraey of standard solutions which are used to cali brate analytical instrumentation is well below this amount, and therefore is normally not an important factor in producing inaccurate data. Free elms to time, analyte responses of standard solutions from different sources will be compared to standard solutions used for Instrument calibration. This information is normally included in the section entitled "QA/QC Kesulcs". The accuracy of a result can be estimated in a number of ways. The current study uses surrogate standard recovery and native analyte recovery information to aid in assosslng the accuracy of a result. This recovery Information, normally reported as percent recovery, gives you Information concerning tho percent of surrogate standards and native analytes which were recovered after adding to your sample matrix and performing the various extractions, clean-ups, and Instru mental analyses associated with cho determination. The use of sur rogates also assumes that the spiked surrogates are bound in the matrix in tho same way as the analytes of Interest. Surrogate stan dards are added to every sample while native analytes are added to only 10% of eech sec of samples. Therefore surrogate standard recovery data could be used to correct the reported results of an analyte concentration, if the user of the data feel such corrections are warranted, mnrtl l me dace ramorrod in ehla seudw InrllMlm gllT correction far eurreasts standard recovery. It is the raamonalhlllev of tho ooroon roonootlnc the onolvooo to oanlw onnrooi-Ugn recovery correction* If ho/cho fools thot ouch corrections are warranted. Bias - Terminology used to doserlbe how tho accuracy of a determination may ba affected. A low bias means chat valuaa below the correct value ere normally measured. A high blae noons that values above the correct value aro normally measured. The instrumental analysis atap of extract analysis normally docs net eontrlbuts significantly to analysis bias. Hose bias in environmental analysis Is introdueed la the temple extraction stop. A low bits is introduced when cho cample Is not complstsly extracted and ths extract docs not contain 100% of ths analyte. A high bits is introduced when the final volume of tho extract le lees than the correct volume. Surrogate Standards <S$), whieh ere diecuesed in the next section, cen be used to determine the amount of bias which is Incorporated in the reported result. MOTtlf Mo data reported In this fsnort on, correction for this bias. It Is tho responsibility af tha Parian rimiMtlni tha uuWm to dbLy aporonrlata hlM carractlana. If ha/aha f.al. that auah carractlana r. v.rr.nt.d (continued) MOMS 024704 Page }, Quality Aaeuranca/Quallty Control Terminology Lnil of Datact Ion (LOD) - Terminology uaad to Indicate what analyta concant ra don will product a elgnal-to-nolae ratio of 10. For tha praaant report, thla value la not experimentally dataralnad. Normally. a Llalt of Quantltaclon la uaad to dataralna tha thraahold concentra tion above which an analyta can be detected. Llalt of Quantitation (LOQ) - Terminology uaad to indicate tha lowaat analyta concentration which can reliably be quantified. Tha preclalon of tha determination of the analyta concentration at the LOQ la normally on tha ardor of 100*. Tha LOQ la normally dataralnad experimentally by adding a known amount of analyta to the aaapla matrix and aaaeurlng tha percent recovery at tha LOQ. In aoae caaaa. whan there la lnaufflclent aaapla quantity, or for convenience, an LOQ will be dataralnad ualng other aathoda. Theae oethodj ahould be clearly deacrlbed In thla report. Further laforaetlon The general area of Quality Aaauranca/Quallty Central, along with much of tha taralnology deacrlbed above, la vary caoplax. Tha following refarancaa may provide further Information which may be uaaful In underatandlng the validity of the raeulta reported In thla etudy. "vu a--ammo awootlaa D4110-gl entitled 'Intralaboratory Quality Control Froceduree and a Dlacuoaion an kapartlng Low-Level Data*. aeon Praecipe Mill.11 entitled 'Determination of Freelaton and laa of Mathoda of Caanittae D-l* on Qatar*. am artle.1 - - *e^ffl`| ttlg'*tT authored by 29 wall-known environmental eclentlete. Thla article waa funded by a grant from the Environmental Protection Agency and acknowledged 24 additional eclentlete In lnduatry end government who ware Involved In tha review ef tha article. Ita clcatlon la: 'Prlnclplea of Environmental Anelyale*. L. H. Keith, et. el.. Anal. Chen. 1911, 55, 2210 2211. 40 CTX Fart lid entitled 'Culdellnee Eatabllahlng Teat Procedurea for the Anelyale of Pallmcanca Under the Clean Qatar Act; Final tula and Interim Final tula and Prapeead tula*. Thla document lncludea detail* of EPA'a 600-earla* onalyala aathoda. A currant copy of theae aathoda can be found In tha October 26, 1914 Federal Kegietar. QAQCTI:N1 HONS 024705 Analyta Extraction Terminology This Merlon dsserlbcs cuamimly uMd terminology nd phraeas which ara uaad In conjunction with analyta extraction. Thia Information may bo halpful In under,tending ecas da Cal la of how analytaa In your samples wara laolacad far Instrumantal analyala. Instrumaucal Analyala Tatmlnologlaa ara (Iran in eha following faction of thla report. Sample - Terminology uaad to reference the aacarlal which you submit for analyala. Samples may be solid, liquid, and In soma cases, gases In general, whan a sample Is recelvod for analysis. It Is logged Into tha ISC sample login book and proper ehaln-of-custody doctaenct ara maintained In tha awenc this Information may be required for litigation purposes. Aaalyta - Terminology uaad to reference specific compounda or farmulaclono of compounds. Whan an analysis Is requested for a certain analyte within a certain sample matrix, normally earns typo of extraction process la required. Ixtractlon Thla tarminology refers to tha stsp which Isolates tha analyte of Interest Into an appropriate solvent. Ixtractlon Is required for savmral reasons. In many cases, tha concentration of eha aaalyta la below tha level ef detection of tha Instrument which will be uaad fer analyala. Therefore, axtracclon Involves re moving the analyte ef latarest from a relatively large veliae of sample and planing le Into a relatively aaall voluae of solTone. Thla places eha aaalyta In eha solvent ae a coneaneraeioa vhleh ean easily bo dotoocod by tho analytical inacruaant. A ascend roaaon that axtracclon la required, la that tho sample nay not bo appropriate for diroec lnaerunontal analyala of tho analyto of lntoroot. Thla ean bo anally understood for analytaa in aolla. Vary few analytical lnaerunonta allow soils to bo dlrectl" inserted into tha inotruaent. Therefore tone typo of isolation atap (1. a. extraction) la roqulrad in order to place tha analyta In an approprlaca natrlx for Inatrunantal analyala. When tho analyto of lntoroot la praaant at sufficient concentra tion, end the staple natrlx eon be directly Inserted into the analytical Instrument, the staple, or tho diluted staple, ean bo directly analysed. However, thla eaao represents a nlnorlty of saapla analyses which BSC is asked to perforn. (continued) HONS 024706 Page 2, Analyte Extraction Terminology Matrix - Terminology usad to reference tho major components of a sample. In moat eases. major components ara noc of diroce incaraat except as they offset tho typo* of extraction stops ond oehor isolation procedures which mist bo usod to Isolots tho analyte from tho sempl* matrix. For tho majority of onvlronmontal samples which ESC la oakod to analyte, tho matrix la normally waear or soil. However, many environmental matrices contain relatively high levels of organic cexpounds which nay Intarfer with the instrumental onolysls of the analyte of Interest. Therefore, depending upon the analyte of Interest, the required levol of detection, ond the taounts and types of ocher orgonle materials which may Intarfer with the instrumental analysis, extraction methods must be developed which are very specific for a given sat of samples. In order to deal with almost a limitless set of matrices, analytes, extraction methods and Instru mental methods, an organised approach to sample extraction, followed by Instrumental analysis, has bean developed at ESC. Extract - Terminology used to identify the analyte-containing solvent which was obtained from the extraction of e certain matrix. Extract Cleem-wp * Terminology used to identify chemical steps which ara required in order to reduce die concentration of organic compounds which may be extracted with the analyte of Interest. These eoextracted compounds may be at such high levels and/or produce responses so that they lnterfer with the Instrumentsl enelysls of the analyte la the extract. Extractable Compounds Terminology which refers to tho ability of a compound to bo lsoiatod from tho sanplo matrix and placed into tho extract solvent. Uhon tho sanplo matrix Is primarily soil which contains little organic matter, moat organic compounds ere extractable eon* pounds. However, whan the sample matrix la primarily water, only those compounds which ara hydrophobic ara axtraccabla compounds. Standard Extraction Method - Terminology usod to reference an organised description of the stops involved in isolating an analyte from a given natrlx. Those methods ara assigned short names whieh ean also be used as computer file names for those methods. Tho nemos of specclfle Standard Extraction Methods which ara used in this study art listed in tho final report in die section entitled DotalIs". In addition, copies of ehoao Standard Extraction Methods ara shown In a separata section of this report. Standard Extraction Methods also include details of sample clean-up, If required. Extraction Flow Sheet - Terminology used to reference a graphic daacrlptien of a Standard Extraction Method. This flow shoot is filled out by the analyst In the laboratory and serves aa a detailed record of what occurred In the sample extraction step. Flow sheees of in* dividual sample extractions may be included in a section of this report. (continued) HONS 024707 Pag* 3, Analyte Extraction Termlnololgy Surrogate Standard# (SS) On* laporeant olenane In eh* axtracelon of an analyte from a maerlx. La th* deteralneelon of what pareane of eha analyta was actually extracted from eha aaerlx. For method* which involve liquid/liquid axtractlon of water with an organic soivone, or ilquid/aelld axtractlon of aolla with an organic solvene, le la Imperative that data ba obtained which glvaa th* analyaia raquaator Information concerning what percentage of the analyta wee laolaead in the extract during the axtractlon atop. Surrogate Standard* serve ehla important purpoaa. The phlloaophy on the uaa of Surrogae* Standard* la aa diverse aa the analyata who uae them. If coat ware no object, analyta recovery Information could be obtained by eha uaa of aeandarda addition analvala method*. However, aInca many temple* require attentive labor to laalae* an analyta lnee an extract, aeandarda addition analyaia method* are too coetly for moat *tudle*. (A standard* addition analyala require* each sample to be extracted and analysed at lease throe times.) Surrogate Standard* give the same type of information, with only one analysis being required. A Surrogate* Standard la a compound which Is chosen to behave exactly aa the analyte. It is a surrogate for that analyte and thus information obtained for this surrogate can be assumed to also apply to the analyte of Interest. For the analysis of regulated analytes, it Is la^ortant that when data is generated that shows that the analyte la not present, that we can also show that If the regulated analyte were present la the sample matrix, it would have been detected. This is especially true when complex extraction and lnatrumantal analyaia stapa are involved in this determination. Therefore, when aa extraction la performed, a known amount of a Surrogate Standard ia added to the sample before any axtractlon steps take place. When th* extract is then analysed for the analyte of interest, the amount of the Surrogate Standard Is also determined From this information one can document, for each sample, what recoveries were measured for this Surrogate Compound. From this, one can describe acme level of confidence on the data generated for the analyee of interest. A detailed discussion on how Surrogate Standards sre chosen 1* biyood the scope of this section on Analyte Extraction Terminology. ESC normally uses two typos of Surrogate Standards. The flret la when the surrogate la exactly the seme as the analyte of Interest, except that the naturally occurring earbon, hydrogen, or halogen stems in the analyte have been replaced with nom-natuxally occurring laetopee. These surrogates cam be expected te ace exactly aa the native analyte*. On* good example of this type of eurrogaee la the 2.3.7.S-TCDO surrogae* In which all carbon atone are carbon*13 or ell chlorine aeons ere chlorine-37. (continued) HONS 024700 Fags 4, Analyte Extraction Terminology Th second typo of Surrogate Stondord la on# which does noc have the tamo chemical stroccur* a eho analyto of lntarest. but Is known, or aseumed to act chemically Identical to tha analyte of lntaraat during tha extraction and clean-up stops. Example* of chls type of surrogates ara dautaratad compounds which eay ba added to a aacrlx In vhleh any chromatographabla aacarlals ara to ba Idantlflad. This approach can only ba applied ta CC/MS analyses, since the surrogates can ba differentiated fron tha native compounds from their different aaaa spectre. Since it is not known before sample extrac tion and extract analysis what analytes may ba present, surrogates muse be chosen ehac could not possibly ba present in tha sample. In addition, since only llquld/llquld or llquld/solld extraction would be Involved, with no clean-up (since clean-up would remove compounds In which the requester Is Interested) any hydrophobic doucerated compound eould serve as a surrogate. Normally, phenol-d5. 2CL-phenol-dA, CL2-bensene-d4, pyrene-dlO and ehrysene-dl2 are used as Surrogate Standards for the analysis of a wide variety of hydro phobic materials in environmental samples. A sub-set of this second type of Surrogate Standarde are the surrogates which ara used la tha capillary CC/tC analysis of Aroclor formulations. Since mass epectrometrlc detection is not used, surrogates which contain unique Isotopes cannot be dis tinguished from their native counterparts. Therefore, ocher com pounds are used as Surrogate Standards since they have been ob served to act exactly as the polychlorinated biphenyls (PCS*) in the Aroclor formulations. Any haloganated compound can be used which acts exactly as PCS* In the extraction and clean-up step. ESC normally uses CLS-bensone and 2,4,6-CL3-biphenyl for this pur pose. Native Analytes - Terminology which references the analytes of interest which contain naturally-occurring Isotopes of carbon, hydrogen, halogens, etc. Native Spike - Terminology which references the addition of a known amount of native analytes to the sample matrix. Normally, at least one ssnple will be spiked with the native analyte at the reported level of de tection (lew native spike) and at 10 times the level of detection (high native spike). Recoveries of the native analytes provide fur ther documentation on the quality of cho analyses performed. For sample sots which contain more chan 10 samples, the frequency of low and high native spikes is 10% of the number of samples. (continued) HONS 024709 Pago 5, Analyte Extraction Terminology Method Blank - Terminology which refers to a sample which la known to contain non* of tho analytes of ineoroat. for watar analyses, ehis is nor mally Burdick and Jackaon Brand Water, da*lonizad, or distilled water. For soil, it nay be soil which has been previously analyzed and known to contain none of tho analytes of interest. All extrac tion steps, usinp randomly selected glassware, solvents, and all surrogate spiking solutions must be used. This provides documen tation that the analytes of Interest were not Inadvertantly present in extraction glassware and solvents used In the analysis. A minimum of one aethod blank oust be generated with each set of samples. For sample sets containing note than 10 sanplss, method blanks are gener ated at a frequency of 10% of the number of samples. Duplieats Analyses - Tsralnology used to indicate the duplicate extraction and duplicate extract analysis of a sample. This provides documentLon on the precision of an analysis, normally the precision of environ* mental analyses of homogeneous samples Is on the order of 30%. A minimum of one duplicate analysis is required for each sample sec. For sample sets containing more than 10 samples, duplicate analyses are generated at a frequency of 10% of the number of samples. Further Info tlon The general area of Analyte Extraction, along with much of the terminology described above, is very complex. The following references may provide further information which may be useful in understanding extraction funda mentals and terminology. an era Part 136 entitled 'Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Veter Act; Final tule and Interim Final tule and Fropoeed tule*. This document Includes details of CPA's 600*soriee analysis methods. A current copy of these methods can be found in the October 26, l*S4 Federal teglscer. IfTB--nr for which is used in conjunction with EFA'e Superfund Site studies. A current copy nay be obtained by contacting: Joan F. Fisk, Project Officer Analytical Support Branch Hasardous tosponse Support Division US ETA Washington, D. C. 20460 APEXTS:MI M0NS 024710 Instrumental Analysis Terminology This section describe* commonly used terminology and phrases which are used In conjunction with extract analysis. This information nay be helpful In understanding sons details of how Instrumental analyses of sample extracts were performed. The previous section of this report describes terminology associated with analyte extraction. Sample extract * Terminology used to describe the solvent containing the analyte of interest which is obtained from some type of sample extraction atop. Detailed Information on how this extract is pre pared can be found in the Standard extraction Methods end flow shoots essocletod with the mothods. Susmarles of choso ntthods which wero used for this project can bo found in a separate saeeton of this roport. Intamal Standard <If) Tsrmlnology uaod to roforonco a compound which la addod to eho aampla extract and atandard solutions of tho analytes of lncaraac 1 mediately boforo inatrumontal analysis. Tha purpoae of tho internal atandard is te provide date which can be used to correct far variations in Injected volume# of extract and atandard solutions which may occur during lnatnaontal analysis. The internal standard must nee be present In the sample extract. Typleal Internal standards used In naaa speetrometrie analytes are bensene-44, naphthaleno-df, anthracene*dlO ead chrysene-dl2. These deuterated compounde produce unique naaa spectra and are net present in naturallyoccurring samples. A eoemonly used internal standard for GC/1C analysis la hoxachlorobenzono. Intamal Standard Quantitation (lathed - Tamlnology which refers te e msthed of data analytic. This method roquiroo that a known amount of an intamal standard be added te the sample extract prior te Instru mental analysis, Responses of ell analytes ere calculated relative te the internal steadied using the following relationship: (Analyte Area) 1A telatlve Response - ............................................................ (Internal Standard Area) If different volumes of tho semplo extracts and standard solutions are Injoetod, those differences are reflected by differences In tho internal standard area. In addition. If Instrument sensitivity changes, those changes are also reflected in changes in tha Inter nal standard area. Tho calculation of tho relative response cor rects for those typos of fluxuatlons. In order to determine tho snalyto Concentration-Relative Response relationship, snalyto Relative Response Factors are calculated using tha following relationship for data obtained from the analysis of standard solutions: (continued} *ONS Page 2, Instrumental Analysis Terminology (Ineomal Standard (Analyca Area) Concancreelon) RAF Riltclvi Response Factor - ................................................................................ (Internal Standard (Analyca Area) Concentration) Whan identical --ounce of cha Internal etandard are added Co both extraces and aeandard solutions , Che internal aeandard concentration can In the above equation ean be eliminated. When chia la dona and Ralaelve Reaponae ia aubacituced for che redo of analyca area to internal aeandard area, che Ilf aquaelon becomes: RAF - RA/(Analyte Coneantraelon) Analyca eoneenerationa In che extracca are calculated fron che folloving equation: Analyte Extract Coneantraelon - RR/IRF In order te obtain the coneantraelon of che analyte In the a--pie, the following equation la uaed: (Analyca Extract Concentration ) (Extract Volune) Analyte Sampls Concentration .......................................................................... (Anount of Sampls Extracted) The area tame in the above equaelone nay be cecal Ion arena, FID peak arena, EC peak arena, or extracted ion arena. The details of how the internal aeandard quantitation nothod la applied to apoelfic methods are described in the various lnacrunoncal Standard Analysis Methods. The following equation shows what calculations should be node eo correct for analytical bias: (Analyte Saaple Concentration) Analyte Sanple Concentration - ............................................................... (Corrected for Analytical lias) (Aiaiaed Analyca Recovery) The Assumed Analyte Recovery can be obtained froa an average of surrogate recoveriee or native analyte recoveries, measured for che saaple la question. MOTE 11 Mo data reported in this study Include any correction for surrogate standard recovery. It Is the reopens 1 blllty of the person requesting the analyses eo apply appropriate recovery corrections, if be/she feels ehat such corrections ere warranted. External Standard Quantitation Method - Ternlnology which refers co a method of data analysis. This method requires chat a known amount of che analyte standard be analysed under che seme conditions as che sample extract. In order to dotormino tho analyte concentration- analyte response relationship. Response Factors are obtained froa che following relationship: (continued) HONS 024712 rtg* J. Instrumental Analysis Terminology RI - Response Feccor (Aneiyes Aree)/(Analyto Concentration) Analyte concentrations In the extracts ere calculated froa the fol lowing equation: Analyte Extract Concentration - (Analyte Area)/RF In order to obtain tho concentration of tho analyte in the sple, the following equation la used: (Analyto Excract Concentration) (Extract Volume) Analyte Seal* Concentretlon - -............................................................................ (Aaount of Seaple Extracted) The area terns in the above equations nay be total Ion areas, FID peak areas. EC peak areas, or extracted ion areas. The details of hew the external standard quantitation aethod is applied to specific aethede are described in the various lnstruaental Scaaderd Analysis Methods. The following equation shows what calculations should be aede to correct for analytical bias: (Analyte Seaple Concentration) Anelyte Seaple Concentretlon ...................* --............. ........................ (Corrected for Analytical Slae) (Assuned Analyte Recovery) The Assumed Analyte Recovery can be obtained froa an average of surrogate recoverlee or netive anelyte recoveries, aeaeured for the seaple la question. MOTE! I Mo data reported In this study Include say correction for surrogate standard recovery. It is the responsi bility of the persea requesting ehe analyses to apply appropriate recovery corrections, if he/she feels that such corrections are warranted. Standard Analysis Methods - Terminology used to reference an organised description of tho steps Involved in the instrumental analysis of a sample or a sample extract. These methods ere assigned short names which earn alee be used as computer file names for those oatheda. The names of specific Instrumental Standard Analysis Methods which are used in this study are listed in the flnel report in the section entitled "Details*. In addition, copies of these Standard Analysis Methods are shewn in a aoparate section of this report, new sheets of the Standard Analysis Methods are usually also provided in this section. Analysis Plow Sheet - Terminology used to reference e graphic description of a Standard Analysis Method. This flow shoot gives specific Information on how extracts and standards are enalyzed and what types of data reduction methods ero usod. (continued) HONS 024713 Faga 4, Inetruaantal Analyala Terminology Further Information The general area of Extract Analyala, along with ouch of tho terminology deacrlbed above, la vary cooplax. lafarancaa provldad In tha pravloua (action entitled 'Analyte Extraction Terminology" any provide further Information which nay bo uaoful In undaratandlng Inatrumental analyala fundaaantala and terminology. IMNTElMI HONS 024714