Document RDn6gLOq6q0w5YpXYbaVoB1n

Monsanto E38H/ESC (Co./Dlv./Dapc./Location REPORT NO.: JOl/PROJRCT NO. DATE: TITLE: AUTHORS: ABSTRACT: Roooorch Ktport (Typa of Raport) MSL-7980 ESC-88-42 780.28-1222 Jana 20, 1988 RCEIV:D JUl 181983 * ' ar .n IT. LOWS .? ' t * Analysis of PCBe lo Kurny Plant Water Saaplee D. E. McKenile..I. M. Hughes, L. I. Minor, C. K. Trang Twelve I-llter water sasplaa vara received froa tha Kearny Plant for low-level PCS analyses. PCB formulations vara detected above 0.1 gg/L In aavan of tha twelve sanplas. This raport glvaa descriptions of tha methods and dlscoaaion of thaaa results. Am i l l n a ly s is o f PCBs In Kearny P la n t U a to r Saaplos M S I-7980 g jk O watei TECHNICAL APPROVAL: &&*"*-*/falKl P. L. Shaman Environmental Sciences Cantor Sanlor Group Laadar APPROVAL BT: rn. Jtt.___________ Environmental Sciences Cantar QC/QA and GLP Supervisor APPROVAL DATE: M 10W HONS 02*971 COMPANY CONFIDENTIAL This document < tha property of Monsanto Company and tha recipient responsible for its safekeeping and disposition. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorized parsons or sent outside the Company without proper authorization. DISTRIBUTION CQPX-ttUMBER abstract only 1. 2. 3. 4. 5. 6. 7. 8. 9-11. S. L. Emery A. M. Ford J. M. Lee B. S. Yere P. R. Michael D. E. McKenzie B. M. Hughes C. K. Trang Reports Liorary - (E2NP) - (U4F) (U4D) - (F2WJ) (A2NE) - (U4F) - (U4E) - A/1F) - (R2C) T. F. Evans P. L Sherman A. F. Uelner ;a3na) U1F) :A3NF) COMPANY CONFIDENTIAL TM* doenmeat is the property of Monsanto Company and ike recipient is responsible for its aafcknpiag sad disposition. U contains CONFIDENTIAL INFORMATION nkicfc nasi not be rcprottoccd, rescaled to aaaatborktcd persons or tent ontside the Company mtlxxa proper euthorintaon. HONS 024972 RESEARCH REPORT --------------------------------------------------------------------------DATE: May 27. 1988 --------------------------------------------------------------------------PROJECT NO: MUUtm TO: B. S. Yart (F2WJ) FROM: Environmental Sciences Center Monsanto Company 800 N. Lindbergh Blvd. Sl Louis, Mo. 63167 Phone No: (314)694-1464 TMe Analysis of PCBs in Kearny Plant Water Samples ABSTRACT M 1-Bur wmtr Mmfks mn raabat fvm dtt Kramy Plow far towdcwl KB mutfsa. KB formafmiams wara Bantu* aBot 4/ ag/L in jcwrw of Bit tmirt sampkx This report pros tescnyaons oflht mtthorb mdOhaaaiem ofthts* rants. INTRODUCTION Twdw water Mfln am ngari Iron the Kearay Plata for low-lcvet PCB aaalywa. Four UMM 14k> aainphs hWW #110 am mat br mo Afina mlyicr oat mo mm yim, aartfrn aria, lit ismasisg aanpka am kMM #101 #109 and #111 and lilt Sample wlaam ataia l-har. la order m obtain bi^dy rafiable dau (or PCB foonttlaooo concentration* between 0.1 and 100 ag/L, (be l*iter sample* were tandd with methylene chloride and (be extract volume was reduced to 1.0 L Tbe final moact* were aaalymd long a cspdhry GC/MS analysis metbod. This method produced detailed information on tbe emauntt of total CL|biph*ayf through total CL.g-bipbciiyi congener*. (For ibia report, CL-bipbeayi m abbreviated 'CU-BF\ Ct-bipbcnyt is abbreviated *CL2BP\ etc) Fstimetri of tbe probable PCB Inrmulatinni were obtained oy comparing tbe tfistribetiona of tbe total rblnriaeted bipbcnyl congener concentrations with tbe diatribution of concentrations obtained from tbe analysis of standards of Arodor formulation*. (Note: Arodor is a registered trademark of tbe Monsanto Company.) MONS 024973 Page 2, Analysts ofPCBs in Kearny Plant Water Samples (coat'd) EXPERIMENTAL One-titer met sanpica wen apikcd with I og sack of four iarrocate (^CAMW PCS coagcaara). Liquid/tqaid eanaka mag a total of 180 aLa aethykae cklorida wm Bed to aobu FCBa iato tka orpaaic earaet. Thh enact wn reduced to 1.0 nL oaf Kederaa-Dank-------- -- lota. Tkia afactioo aatkod aad aaractioa Hoar akaat art aaaaaarizad aa WSEXOS aad WSFSOJ la tkia umpie aet. Oaea tka 1-Otar aaaapica an canned. 200 aL of tka 1000 aL caract or 200 aL of dl ~ta--- aoMoaa aan coBkiacd with 200 aL aatkracaaa-djn (10 ag/aL) ia anntanphr Wa. Tka tanas aad ataadarda to which tka aathraceaa-dia iataraal ataadard kad baea addad aan tkaa aakynd oa a capflhty GC/MS analytical oynca uaiag Standard Aaalyii* Matkod MSAN2J. Brief dnrripticn of tkia tMtkod aad tka dear akcet (MSFS23) an abo (how* in Appaadh B. Tkaaa anthoda aha denribe ralrahtinn okick an aaad to oktaia hdhddaal PCB roagrarr roareatralioaa. total PCS --grnr coacaatralioaa far CLj-biphcayl tktoagk CLjgAipkcayl roagaarn, rod tka total PCI maftalitliiin RESULTS AND DISCUSSION Rapnaeatathe ckroBatopaoH aad lablea naafeiog bon Lotn/1-2-3 ralrahlion an htBad ia AppcadhG Tka Lotn cakalatioa reaaka an akoaa ia Bra aeta of takka akoa ia Appaadh C Takka 1. aad 2. laaatrirr1) total CL,-BP tkroagk total CL10-BP coagaaar cBnct coaceatraftaa* (ia of ag/nL), 2) total PCS camel wacaatmioaa (ia aaka of ag/aL), aad 1) total PCBa detactad ia eadl taapk (ia aaiu of ag/L). Siaca tktn it a oaa Ikoaaaad-Md daman a aohna boa tka mater taapk volant to tka cBract rokaa. Ikon ia aaactly a oaa Ifciaaiad Odd daman k coacanntioa boa tka aaaantd tana coaaaatraiioa to tka water uapk coaceatmlea. Takka L aad 2. ia Appaadh C ako akoar lacoaaciea of tka Ion UC labeied tampan whick wan added to tack water taapk kefan reranioa began, aad peatiaea iafnmaioo nhlag to Ne aaaaa aaed lor earaet aaalyaia, dHnioa factor*, aad ialcraal atadtrd ana anaaand. Takka Ia aad La tannnin Aaaraga Rehliaa Reapoare Factor* whkk were dalcrBiaad bon the roagann. Takka lb aad Lb aaaaarin tka ratka of ckaracteriatk/coaBmiag ioa raapnant tor rtndanlt aad earaet*. Takka l.e aad Lc aaamarhe tka wing* larrup*** itcorarfaa, tnadard dariatioa*. awainan recovery, aad auaaaan ncanry annoted Cor Ike tel of data akoan ia Takka 1. aad L, rcapccthcly. Tabk 3. nnnarrrri ncorariat of 24 aatha PCB rnageaert whick wan added la aanph #110 far qaakty coatrol pagan aad Takka 4, 4a, 4k. S, la,aailb maanrin total PCB reagrarr coMMfiliBM MMnrf far Arodof fanMfatios tHdvd icfatioM obttM Ctom fa Svpdco C*npaap. Al of Ikon data whkk am ihnwa ia Appaadh C an fartker madeaeril aad ahowo ia Tabk I aad Figara 1 10 of tka patatn report. Figm* 1 - 3 laanniaa tka total PCB coaccamion aad loud PCB eoageon cooctatratkaa Cor CL.-BP tkroagk CL.JJ-BP roegtetn Banned far anapka #101 tkroagk #UL (Non thel 0.1 g/L an delected Cor the CU-bipheayi caageacr h #103 which i* at on anthod dctecaioa laaL Tkk carea wn aaalyicd huacaately after tka earaet far tanptr #102 whick coataiaad ahaoat 100 ag/L total PCB*. We kan toaaned that tkia trace guanity of CLjbiphenyl congeaen i* dec to carry-over boa the aaalywc of #I0L) HONS 024974 Page X Anafysil ofPCBs in Keamy Plant Water Sampia (corn'd) la order to dctcnniae tka Win of the PCBa detected ia sample cambers 101,102,104, KB, UK 107, aad 100, the (oul FCB laagrtrt dttribalioat am compared to dbtribatiaaa maud boa tka Company a 100 ag/aaL Arodor fccaalatioa ia amthaaol Figaro 4 ikon ikat tka daribaica of FCB taagaaen for Arader 1240 a aaffined boa 0.1 to 10 ag/mL. (This ntntipcada a a coaaalfarioa raaga at Oil a 10 ag/L k a 1-Ottf water napla.) Therefore eoapariaaa of dlatribatioa of total FCB magram ia wear earactt witk datribatioaa froa Arodor final ahtina analyses ahoald ptoeidt valaabk iofomatioa oa tka fonaalalioa ideality. Figaro 3 ikowt tka tka dalribalioa for taaapla anabm 103, 106, 107, aad 109 appew to bo marly ideatkai to (bat tkowa ia Figaro 4 for Arodor 1240. Fattkcrmora, akkoogk #102 aad #104 art ary liarihr to Arodor 1240, tkia FCB coagaaa dialribatioa probably arias boa a lower fonaalatina tack a Arodor 1242. Figaros 6 aad 7 tbow ike FCB magratr ijaribaioa for dgkt formalalioa aad Pipes * tkowa that tka dblribetioa lor #102 aad #104 an eery similar to tka Arodor 1242 aacyaie of this sand is thowa ia Figaro 9. Along with thoa two dhtribatioat are tkowa datrdrotiooe for Arodors 1234,1260 tad 1262. It sppaaw tka aaple #101 caa best be described a a wheats at Coapaay an thowa ia Tables 4,4s,4bl,]Aaa4Ua Appendix C Fortkoa of tkea dau an abo saamswiaed ia TaUt 1 of thie raporL Figaro X) aanairitn Ike rtsaka of tkea tatlyaw For al atafard Aiodor fotaalalioa aadyail, the total FCB cowcralrilina drtrnaiaed wa eetkia 47% of tka inataalielhia rapartad by iaptlro If aaa eadeda tka 0.1 ag/mL Arodor 1240 madaid wkicfc wa at oa katnnweal laeol of drttclioa. only Aipdota 1202 aad 1260 tkow Qoeialioat a largt a IT*. Al other tlaadard tokaioa wan within 13% of tka coned raise. CONCLUSIONS Saatpie aaabtn US, 100,110, 111, aad 112 dM eot coataia any detectable FCB congeners skew the --*---*-* leeel of detection of 0.1 ag/L pa FCB coagtaa. Coaparitoa of FCB coagtacr dhtribariom iadirale tka tka roaaiaiag peedire itaplct consisted of FCB fwaalalioa liwdtr to Arodors 1242.1240, aad a amdarc of 1234.12M. aad 1262. QC RESULTS Tka proaaa aectioa aaaaariact OA/OC rcaaka lor tkia act of samples. Qaalhy Aaaaraaca aad OaaOty Control eeotm an caadaciad apoa sack at of samples which ESC is repealed to aaatyae. Tka tsgaeelor caa botar aadarataad what fcmeaicaa ahoald be placed apoa these retain Tka toOcu'ag paaagiapka deterbe wkat apcriwtnls wan coadactcd to estimate the precision aad accarecy of Ike a that ao falae positive or aegatire ealaes arc reported. HONS 024975 Page 4, Analysis ofPCBi in Ketrrty Plan Water SanpUs (cant'd) .Oxttp* Tb* predaha of the dau reported the tablca eta be otinicd froM It* rendu of aaalpit of dapBcaMMMpiea which coauiaaaaly'ee above the level of detectioaaodfroM Ike reaaba of rptUap Ika MMph* with aanopaM aad aaaiw ceMpoaada. Table* 1. aad 2 ia Appcadn C report Ik* reaaki of a ihtpOran tatlyta (ar #101 m which coMpoaafr an* preacal above th* level el *--*-- (Note ika lkl I* an* lie* fapgrale Mtiyia dace laylinl* l!------- r- m-ipler ~th am |ii nihhd fm ika Maple.) Tkcaa (able* alao report Ik* petceal nomiy of sarTCpate foapoaadi which van illil to each tawpie before tatlyva Tkaa* data oho* Ikal th* aaaljaial predrioa it beaer A*# 30* hr tbb *lol aaple*. Aaalyoaa l tM Arodor foraalalio* ataadarda raapiap a coaeeatMth* ftoa 11 lo 10 ug/aL readied ia total FCB ajacratratioaa withia 47% of the reported Arodor coaccatrarioae. U oae eaehdM Ik* 11 op/aL Arodor U*0 ataadard wkich waa a oar iartmaaa lead el dctatiioa. oaly Arodota UK aad 1288 ahow daviatioa* a laep* a *7%. A1 ether naadard tolaiaaa wen wiiha 15* **--" The accaracy of Ike data reported ia Ika tablea caa b* miauled froa Ike resalti of vpikuvp Ika oaapln with tarropate aad tatrvo roaipo--b Table* 1. aad 2 ia Appeadia C ahowihe iccovyict aaaaaaif whea d napln am ipW abb bar,u(MabcRed aanaa ceapeaaOi 3J,.*.CL4-BP.uc12. Ctt aad 0TM-"^). Table 1 ia Appeadfc t ahsaa Ike rctovcricl at Mated aihea 2* IQ rnapaarri aete ipiked iato saapic 1H> a 11 tat U> H/l par coapoacM For tk* *0 aanafaM tecpvttic* reported ia Table I. ia Appeadbr C Recovery Meaa Recovery Slaadard Dcviatioa Recotcry Raapa Mialm lUcowy Mmmmm Rffftyfry - 98 % 77 % - 157* 50* 207* The haqacacy dbtribetioa hr Ikea* icartelici are alao rhoaia ia Table l.e. Tkia faitillolio* rkoaa Ika 1 of Ike <0 recover** i* above UK aad 1 ia bchw 30*. Tkirty-ciaht of the <0 taktea fall bctvtce SO lid U0% recovery. fm tkt 40 uarrogatc rwawki reported ia Tebfc 1 n Appcedii C: Rccorory Mats Recovery Siaadard Devialiea Recovery Roegs MUmm Recovery Maabaaa Recovery - 100* - 31* -170* - SB* - 228 * The kipriy daiiialna hr Ikea* rccoterrca are dao rkovva ia Table 2c. Tkia (hatrib'ttioe rhoo* that 1 of dOieaovoricaia above 180* aadlhal 37 of dOvalaca fadbctwaca 50 aad 150%. coaceatralioaa of 11 aad 1.0 ap/L aad aanopale spiking coaceatrathae of 1.0 ap/L: Recovery Meaa Rcoowy Mcdtai Recovery fiiidad Deviation Recovery Raape Mhmh Recovery Minora Recovery - 8138* - 86JO* - 14.11 * - 67.00% - 55.00* - 122.00* MOWS 02A976 Page S, Anafysit ofPCBs in Kearny Plant Water Samples (corn'd) wnrai Ha darn remain# ia this study includa ane cnrrectina far arvw.. I mvcte Hi. "* "----*U1~ -J th. --Nek rnM Its amUv anaemuialc recovery amlin. if he/m. I--I. itel--hmmwbm. ...# Ulna- The Recow? Mew (or surrogate rccowiex ia Tables 1. and 1 at Appendix C aad slaam above, are withia 2% of 100% aad therefore there are ao significant biases iatrodeced iato analyses. The Rccovety Meant lor native aad surrogate recoveries ia Table 3. of Appeadet C md show above, are withia 14% of 100% which farther substantiates that there ate no sigaificaat bimes iatrodaced into these analysts. MOTE! No data reported ia this report iarlades any rmaia In. Ihis hiss. Il is th rtianasihilitv of the analysis reoacrior lo anolv atwrooriae bias epereefom if h./w frrk ihar sarh rnrrcrtinm are warranted. rh PealHvee aad Nmarivee. The analyses of Organic Free Water shown ia Table 1. of AppaadmC shorn that the analytical sjateas intredaces no Use positive values. The resells of analysis of anaple #110 which was spilnd with 01 ug/L shown ia Table 3. demonstrate that ao false negative shirt have been reported. The reported levels of detection ia this study are apprummately equal to the concentration of the lowest native spiking itady reported ia Tabic 3. of Appendix C (0.1 ug/l). REFERENCES A am complete deeiriptioa of this method may be obtained from a Research Report pabiahed in Milaspain's Reports Library, MSL-7410 ESC-UAG-R7-174, issued December lg, I9f7 --uuu Ttewamy of tepnavameisst in fhrldriiwf KB Analysis Appmecter-, by D. E. McKenzie, L. R. Miaor aad I. M. Hughes. UST OF APPENDICES Appaadbl A, Mammary of project details far this report (This lection contains data processing information on the sawn of Hies, names of umpire. amass of methods, etc.) Appeadfal. Summary of Earaclioe and Analysis Methods used for this project. Ippaadhr C Summary of GC/MS Raw DaU aad Detailed Lolas/1-2-3 Outputs. Appendix D. Important analytical request aad ctem-ef-cuslody mformmion recorded at sample login. Appeadht I. Dssrriptiom of important terminology aaed in Quality Assurance/Ouality Control. Analyte Eatraoioa, end lastrumcmtl Analysis. ANALYSTffit David E McKenzie. B. Mason Hughes. La Shawn R. Minor, and Chi K. Trang ANALYST APPROVAL! HONS 024977 IK W /O 49(K 9 * 7* m ourns*** m~u I<M 1. IflWT 4# tMt PC* a I KK *tKti In Mttr MflN Irtm Hu iNny Plant an* Malar ataa Pralaat MMr M.M tttl nap 0, 1*44 I4t4l *C4 Cn*MP Canwntrat tana 1m4A> mi* 02-41 all* co*ip co- co-ip a2-p a*- CL9-4P CU4-IP tata( PC*a lit tw-* 1 1 4 1 4.S 1.1 1.4 4.1 l 1 1 4 4.2 9.9 11.1 2.* I.S I.S 14.2 S4.4 SI.2 19.4 1.4 1.2 1 4 4 (4.1) 4 * 4 4 9 4.1 2.4 M.t 4.4 1.9 9.1 4 4 4 1 4.2 9.3 4.) 4 4 * 4.1 4.2 9.1 4 9 4 4 1 1.4 9.9 9.1 4 4 4 1.2 I.S 1.2 4.1 4 4 1 14.S 2S.* *4.) 4 24.1 4.4 4.4 5.4 4 1 Pra4aM laraMlaOan ntaiwra nlatwra 41242 41242 4124* IIHI 412a 4124* 119*11 lN *r< tlar linUrn 412491.1) 4124*0) 4124*0) 4124*0*1 41*1441) 412210) 412)2(2) 412420) 412*4(2) 4WMI) 412*20) 4124*01 4 Ml ) Ml 1*44 iW 4.41 1 *.*4 1.0 **2 12 I.U MS 4.14 * * ai 2* 4.12 4.21 I.U 2.24 4.1 4.14 in I.M 4.42 4 4 4 1.2 1.2 2 1 2.4 *.*4 4.11 4.1* 2S4 1*2 4 *1 2 2* *.24 * 4.4* 4 in i 4.24 1.44 4.2* 1.14 I *-4 11 41 * 4.S3 4.9) l.n I 4 4.04 l.l* I.SS 1.4* 4 4 4.12 4 4.12 44 41 II 14 I.M 4.04 laaal/Carraat Carraet (1) 4.44 4.*2 4.14 f .44 I.V9 ). Ml 4.92 2.14 2.29 4.4 1.42 4.1 I* 1 *2 S *4 2 14 4*.* 1 * S 142 2 MS.) 1 4* > M* 2 m.4 1 4* 1 M* HONS 024978 Page 7, Analysis ofPCBs in Kemy Plant Water Samples (corn'd) Figure 1. Summary of Total HCBs Measured in Kearny Water Samples Simpl Number Menaurod In Kaarnr WMar Inmlii W!CT^5S5!TfWWBi!!iB WMmd In Kaaray WMar Samglaa JSBL & a Total PCS Cangonoro HONS 0 Page 8, Analysis ojPCBs in Kearny Plata Water Samples (coat'd) Figure 4. Summary of PCB Congener Distribution for Aroclor 1248 Standards A124MD BBBH A1241> L. I A1244H) ii A124800) Il HONS 024980 Page 9, Analysis ofPCBs in Kearny Plant Water Samples (corn'd) Figure 5. PCB Congener Distribution for Selec1t0e5dKearn1y08 Water o S10a7mples 108 12of lelative to Largest Congeners (%) 100 80 80 I 1L40 20- 0_CU-BP---------- CtJFBP---------- CCS-BP Total P QB CongenerS Figure 6. Summary of PCB Congener DistribA1u22tiKo6)nafiorAAlOrMcteOloor *S12t3a2n(2d) ards A1242(1) lelative to Largest Congeners (%) 100 80 80 40 Li.20 0_ L1-BP cU FBP----------CL5-BP--------- Total P CB Congeners HONS 024981 Page 10, Analysis ofPCBs in Kearny Plant Water Samples (corn'd) Figure L . Summary of PCB Congener Distribution for Aroclor Standards A125412) m A126(X2) A12621D o A1268(D 1 Relative to Largest Congeners (%) . || . . c13-bp i-w1 <3g. r-BP n CL5- BP Total PCB Congeners Figure 8. PCB Congener Distribution for Selected Kearny Water Samples 102 104 A12420) a HONS 024982 Page 11, Analysis ofPCBs in Kearny Plant Water Samples (corn'd) Figure 9. PCB Congener Distribution for Sample 101 and Formulations 101 m 101-dup A12S4 A12B0 A1262 m ^Relative to Largest Congeners (%) 100 0 > 0 40 20 . 0 CL4-BP ll J-BP CU- Ja. S-BP oi-BP Total PCB Congeners Figure 10. Total PCBs Measured In Aroclor Formulations Formulation HONS 024983 Appendix*. Summary of project details for this report (This section contains data processing information on the names of files, samples, extraction and analysis methods, etc.) Standard Semphof Method(s): Samples supplied by outside consultant. Standard Extraction Mtbod(s): WSEXQ5 (See WSFSQS Tor method flow sheet.) Standard Incremental Analysis Mcthod<a): M3AN23 (See M5FS23 for method flow sheet.) GC/MS Data Acquisition Method Name: PCSC2S Sample Identification^): #t01 #112. (See ranher information oa eared numbers, notebook pep numbers, etc. m Appendix D. Final Report F3e(s): \meword\pcojtctj\pcuj>222\nI222^oc, and -\aa8222.doc Table FUc(i): \m\profects\pcojS222\iaS222 MONS 024904 Appendix B. Summary of Extraction and Analysis Methods used for this project This section contains brief method descriptions and flow sheets for Standard Extraction Method WSEXQ5, copies of extractions sheets generated during sample extraction. Standard Analysis Method MSAN2S, and a copy of the GC/MS instrumental method used to acquire selected ion monitoring data for PCBs. HONS 024985 CSC ftsndsrd btraeelM ltotho4 (SEN) TITLE: Vida scan extractIon nothod for voter. MATRIX: water CSC ftenderd bmetlM Method Her 9SEX05 typical sample SIZE (Liters) tpical exiract VOLUME <i) 0.01 4 1 40 TYPICAL AJKALYTtS: Aroclors, KBs. priority pollutants CSC Standard Analysis Method Nos: CCAMxx and MSANxx IirrartUHCCS: Various; Saa Individual Interferences for Individual analytes. TYPICAL SURROGATES TYPICAL RECOVERIES (*) phenol-d5 CL*phenol*d4 CL2*bonsene-d4 naphthalene-dS B7tana-dl0 chrysene*dll pencechlorobenxsne 2,4,4-trlchloro* biphenyl 20*80 20-80 50-110 30*120 so-in 50-120 50-120 50-120 APPARATUS AND MATERIALS: Burdick end Jacluon asehylsne ehlortda Separatory (umm1 Sodlua eulfate for extract drying Sodlua hydroxide and aulfurlc acid for pH adjustments Nitrogen for oxcrace toIum reduction tfator bach and R*D apparacua for oxcrace volume roducelon LIMITATIONS: Suffielone tempi* emoune to provide GC-MS LOO. SAfTTY PRECAUTIONS: Saa Safa Laboraeory Practlcot. DATES OP HSTHOO CREATION AND UPDATES: 3/U/I4, 10/3/84, U/7/84 HQHS 0249*4 ruam shut vsrsos rot tsc ZXTtACTIOM METHOD VSCX05 U ID: mrc extract ................................... locno: .U:??:.C<?.5-te EXTRACTION DATE ut TINE: AfitJk.dfUjf.?....,.... * /& <t~r -7-RECORD NATIVE pH .......... WAS pH ADJSTED YEs(g{) If VES TO WHAT pH..................... PLACE SAMPLE INTO AM APPROPRIATELY SIZED SEPERATORY FUNNEL (1/2 HEAD SPACE SUCCESTED FOR ADEQUATE MIXINC) CXI SAMPLE VOLUME ...JL. ** ' ........ ____ UipjvK............. 1 H s M/jH u.. ivAA'p... OrA'c.'iL. .<tij/nv IF pH ADJUSTED ( ) ADJUST WITH.SO* NOH OR H SO 24 ADO METHYLENE CHLORIDE IN >0 THE APPROPRIATE AMOUNT . (1 L SAMPLE JO bL SOLVENT. . IOO nL SAMPLE IS >L SOLVENT) . SHAKE SAMPLE ONE TIME {>< AMD VENT THROUGH STOPCOCK . REPEAT DOUBLING THE NUUER . OP SHARES BETWEEN VENTINC . SAMPLES UNTIL THE NUMBER OP . SHAKES EXCEED SO . RECORD AMOUNT METHYLENE CHLORIDE ADDED FOR EACH EXTRACTION /r . 1D1 - I \l / V L'cb' 2)3).i.tt'M.. OBSERVATIONS ALLOW PHASES TO SEPARATE X] REPEAT EXTRACTION PROCEDURE TWO MORE TINES IF ACID OR RASE WASHED RECORD TYPE AND AMOUNT. [) .. () . ACID/BASE WASH COMEMTS DRY EXTRACT WITH 4 INCH SOOIUH SULFATE COLUMN (COUM PRESIDESB WITH 30 aL METHYLENE CHLORIDE) X] . . . . ( 1 EXTRACT DRYING NOT REQUIRED RINSE SODIUM SULFATE COLUMN WITH 2 130 aL XI . REDUCE EXTRACT VOLUME TO 1 aL SY K-D TECHNIQUE AND OR NITROCEM SOLVENT VOLUME REDUCTION EXTRACT tn-PCA^j^. XI . . X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS DATE/TIHE COMPUTED- '/................. ANALYST/^-4 ` ESC JO* NO: f.C-. %.: - i. '........................... HONS 0247 ftOJKT HM/MW 'J>$An m. UMtooc net w m moot must | SANTLI I iMniric*nan *{%...6iAp... ....... Pte&fyv.M(>JM9X ;..*......." ntucTion ma0t\ J^/EeioC. ,____________ ,, i wmiicaxnt// i VOUM ..... COmOfTS: 'dtiCsif' -u Vr JJb. / .CiCOjr. ..PM.r.fJ...... h0 r%**** /j, //* a/ ..PH.*.7...................... Afc________ 1 #602%. fcA&cX. .m..*&... i Pc&m)(....lU.................. .............. At.............. ...Pm.7.7........$&...... ..Mt.,7........... ................................ -\k-- ...PM.7.7............... xf7. UA'.-.au7`..&dtL.\juJSfZ. . J. XIm&Jr.L. .M~~.. 0*b--0*AH6-E J19UL i- CillkrulM nscas: class S weight lalanca Reading ' M-U6-tOLTINT OMD irnns laranunmi (ALL IANFLZS UCCTI *K AID ovlt Taon noicsTta ucun U M IS a AMRIOM TO l) (TUI lUAn-.sfe) or TUBS ICTRACT1B I AMOUNT: ^ FINAL TOLOMK BRNACT: Ay,, . Msaf ...........,U" U- lAjPdlO / ><> m- /AJPC/O SToCJi /MmX /C/u7 MOMS 02496& ROJZCT UB/MOO:'bhm/.....'..s&i.. . . !" .ifajkt.... m. uoaoaK rut --Mint "TM"'.... wa^.faS'.. rot otoor: BRVACT | 1AMTLI man | iDorririCATioH man/ voum &&4&3X I01 ............................... .. /o 1 ........................................ COMOrTS: dief .fi.H'.Z............ AWvyor-lJw.. ^y<* . P.P.* .71............<WW5. JjuC.-^lt*L. Mw: fyu&aty./os......................................... RP. T.l................ A&s&i\.1P.4......................................... .fiUf.7................jfiluvf'.................. Ad&^./as:...................................... .p.Pr. .7.......... .itileJ.rnma... ...................................... &ea3tf,yJ6l...................................... .flA'.7.................yAVv'..#m-y.. ............ c-a* t$rJwq--*---J-*-i?-t- 's,. J i(2^ycJu rH> ...X^.l()Ojoau..lliJiUU!MU AcnaL I * *"*^*l* *XtirrvA**"* j *U-l -I- Collbratlm Mtii: clui S might - lalane* luHa| "Ciyut. inxxao nroaiMTioa 135man. or ti otimtib z uemt riML TOLO0* tXTItACT: J . . m.j&iJ QnPe6--Z ...l&M UU imtui unm in *m oou non nomtn uctm U 00 M II AM1TIOO TO fR) (mi gUMO:ah) U- fOCjJ iUif/L' n- ioOjJ /dPcto eW. HONS 024909 C I CaltkratlM nocaa: ilui S Ml|ht lalmc* hadl<| or ion miAcm s amor d.1^. tram xarouHTiM (all umju isam snc am obu non noicAna uctrrt uotnii amxtim to ih> (TILS IIAAVO:all) FINAL IOIM STTIACT: C/a &4-Z' - /ST}JLS U'/stUrf /*JPP/0 n./W/uJ JtoCX 90 UC Standard Aulyaia Natho4 (SAM) CSC Standard taaljaia Method No: TITLE: Polychlorinated Cofin4a 1st llmea MSAN25 ANALYTICAL INSTRUMENT AND MODS OF OPERATION: HP-5915/5987 Capillary CC/M5Seleceed Ion Monitoring with RTC-VI operating aystea. Typical Run Tina: 15 - 40 aln. Typical Multiplier Voltage: 1100 - 2100 aV Typical Dwell Tlaes: 100 500 asec/aaas Haxlaua e of Macaco: 20 Boases x 5 ranges - 100 oasse* Electron Energy: 70 aV Maaa Spectrometer Tuning File: KT8402 Mass Spectxenetes Data Acquisition Method: PC3C25 TYPICAL ANALYTE TYPICAL INSTRUMENT LEVEL OF DETECTION (L0D) (ug/nl) TYPICAL PRECISION 4 10X LOO <%> TYPICAL ACCURACY 4 10X LOO <%> Organic Compounds eluting between toluene end n-C34eae 0.01 - 0.1 30 30 INTERFERENCES AMD LIMITATIONS: Anelyte characteristic ease ause be threattographically resolved Iron other eluting conpounda which produce the tone neas. CHROMATOGRAPHIC COLUMN: 30-aeter fused allies JAW 01-5 (0.2$ uM) with wide bore (0.32 m) COUMI TEMPERATURE PROGRAM: S0(4)/t/300 INJECTION TYPE: Spllelest CALIBRATION AMD STANDARDIZATION: Quantitative: Use Internal standard quantitation technique and calibrate inatmnent raeponsa factors Iron standard solutions of analytes of lntorost. Qualitative: Whan ulelpla characteristic nesses ere onltored for a given analyte, the retie of characteristic ness responses oust bo within 201 of tbooo for the authentic standard. For PCS analyses, tho eharoctorlatie assess which art aonltorod ere the aoleeulsr ten eoncslnlng all 33-CL laetopas end the aoiecular Ion containing one 37CL Isotope. The following table ouaaarixea the naaaes end approxineee retention tine regions nonitorad for tho anolyels of internal standard, surrogate standards, and chlorobiphenyl (CL-BP) through decaehlorobiphenyl (CLX0-BP) PCI congeners (continued) MONS 024991 Page 2, HSAH23 (cene'd) DATA ACQUISITION INFORMATION Analyta Masses C4LC-BLF*BFIs~e6Cn1e3rss, uarrnotgharatecene*dlO CCLU3-B-iPr laoaara loaners 118.190 1292*2..2m24 233.9.237.9 CLA-BP isonars 2(9.,291.I CCCCCCC23LLLL,.UU1321*l7f0-0-,-'->-W31--,iiBF>V3rr'.Pr.*lll1l-laaaaa'1.'oooooC2.aaaaaC5aaaaUa1,35rrrrraaaaa-'Ms.(u.-r(r1-o2CgCa1U3te-aMu-rr1e2gCa13tasurr.44**13333298323009177939319.........9B8t77(((.,,.,..,.*44*33333(29482091911933131.,.......779186(( Retention TUee (slnucai 13 1133 - 2222 22 222212222223 333000 3300 31330000 33333335 13 3353 CALCULATIONS: Analyte concentration (Analyte area)/((Anelyee RRF)(IS area)) uhero: Analyte araa la eha characteristic mass area of eha analyte. IV la tha relative reeponae factor for eha analyta. IS la cho intomal standard and la usually anehracene>dlO. RAF - (analyta araa In atandard)/((analyta cooc.MIS araal} K) eoncontratlona ara calculated In ana of two ways: 1) If an Aroeler fornulatlen can bo Identified froa eha pecterne of PCS loaners, so lac tad PCS laanara or elaaaaa of leaner* (1. a. all CtA-biphenyl iseners) ara uaad to quantify tha Areolar aaneantratlon. Relative Response Feetore ara calculated using tha caneantration of tha teeal Aroclor forulation in tha above Rtf aquation. 2) If no unique Aroclor fernulatlan la preeent, than tha eotal KB caneantration la calculated by using standard solutions containing known anaunta of chlarablphanyl through daaaahlaroblphanyl congeners to calculate Relative Raaponaa Factors far each chlorine clasa in the above RRP equation. The IBFs far tha eorreapendiitg KB laouer claasas ara uaad to calculate total KB 1saner concentrations of each clasa in unknown sanplae. (Far oore lnfematlen regarding standard#, sea Supplement to MSAN2S on the fallowing page.) SAFtTY PRECAUTIONS: See KB handling protocols in laboratory safety oanual. OATS OF HBTHOO CREATION: 12/9/13 Tina Scaup <880408.IS24> (continued) HONS 024992 Fage 3. KSAN2S (eont*d) SvppltMttil Information to Standard Analysis Hotbed NSAN23 The following describes detellt of Interne! stenderds, surrogate standards, end individual FCS congeners used for Instrument calibration: Intemei Stendard Anthracene-dlO Surrogate Spiking Compounds C-13 labeled 4-chloroblphenyl 13C4 3,3',4,4*-cecrschloroblphenyl 13C12 2,2*.3,3*.3,3*4,4*.-octeehloroblphenyl decachloroblphenyl 13C12 Native Spiking Compounds (used for native spikes end Instrumental calibration) 2- meoechlereblphenyl 3- monochloroblphowyl 4monochlorob1phenyl 2,2*-dlchloroblphenyl 2,3-dlehloreblphenyl 2,4*-dichloroblphenyl 4,4*-dlehloroblpbonyl 2.4.4- trlchloroblpheny1 2.3.4- trlchloreblpbonyl 2,4,4*-trichloroblphenyl 2,3*,4,4,-tetrechlorobiphenyl 2,3,3,4,tetrachloroblphenyl 2,2*,4,4*,-tatraehloroblphenyl 2,2*,3,4,S-penteehlevebipbenyl 2,2*,3,4,3*-pentachlorobiphenyl 2,2* ,4,3,3*-pencachloroblplanyl 2,2*,3,3*,4,4*-bexacfcloroblphenyl 2,2'.3,4,4*,3 *bexecbloroblpheny1 2,2*.3.3*.4.4*-haxaehloroblpbanyl 2.2*3,3*,4,4*,4-heptsctaloroblpheityl 2.2*3,4,4*,3*,4-heptaehleroblpfcenyl 2.2 *,3,3 *,4,4*,3,3*-ectachloroblpyhenyl 2,2*,3,3*,4,S,3,*.4,4'-nooechlocoblphenyl decachloroblphenyl (continued) *QNS 0^4993 Papa 4, HMN23 (coned) KI Windowing Coapwandl (ulad Co docwont proper dots ocqulalclon window*) 3-CL1- and 4-CU-blplMnyl 2.I-CL2 and 4,4`CU-blphanyl 2,4,t-CL3- and 3,4,4'-CU-blphanyl 2.2',.*'-CL4- and 3.3' ,4.4'-CIA-blphanyl 2.2'.4,<,t'-CL3- and 3.3' .4.4'.5-CU-blphanyl 2.2',4.4',*.*'.CU- and 3.3' ,4,4'.J.S'-CU-blphanyl 2,2'.3.4'.3.I.I'-C1.7- and 2.3,3' ,4.4' .S,3'-CI.7-blphanyl 2,2'.3.3'.S.S'.I.'-Cll- and 2.3.3' .4.4' .3.3' .l-CU-blphonyl 2,2',3,3',4,S,5'..'-CL9- and 2.2' .3.3' .4,4' .3.5' ,l-CU-blphonyl CLlO-blphanyl Choractorlaclc and Confining Nuhi Monleorad Charaeearlatlc (AMU) Confining (AMU) anthraeana-410 181 190 4-ehlorobiphonyl'4C13 3.3'4,4.eetroehlerebIphenyl12C13 2.2'3.3',3,3'.8,8'-octachloroblphonjrl-l2Cl3 d>MChlofblyhtiylHCl3 194 301.8 439.7 309.4 198 303.8 441.7 311.1 aonochloroblphonyla dlehloroblphonyla trlchloreblphanyli c* erachlorob Ipbaiqr la poneochloroblphonyl* haxachloroblphanyls hapcacbloroblphanyla octoehloroblptanyla MDMhlaraklfhMyla dacachlorob1phony1 111 222 233.9 289.8 323.9 339.1 393.8 427.7 481.8 497.8 190 224 237.9 291.8 325.9 311.1 393.8 429.7 483.8 499.8 HONS 024994 fh09 SHUT HSFS29 rot ISC AMALYSXS METHOD MSAN23 EXTRACT ID: ESC EXTRACT LOG HO: ............ MS LOCBOOK PACE WHICH: EXTtACT CQLOH AMD DCSCHXrTlOM CALIBRATE HASS SPECTROMETER ( ] WITH PPTlA AMD DEHOMSTVAtl . CAPILLARY CHROMATOGRAPHIC . HESOLUTIOM VITH SYSTEM . PERFORMANCE STAMOARD . PLACE IM A 1.4 L AUTO SAMPLER VIAL THE SAMPU EX TRACT OR STAMDARD SOLUTIOM COHTAIMIMC PCD COMCEMERS WITH ISO uL INTERNAL STAMDARD SOLUTION. THE IMTERIIAL STANDARD SOLUTION USUALLY CONTAINS 10 UG/L ANTHRACENE-DIO IN CN2CL2 OR BENZENE. PLACE VIAL III AUTOSAMPLER TRAY OP MP-39I5/S7. RECORD HASS SPECTROHSTRIC AND OAS CHROMATOGRAPHIC OPERATING PARAMETERS IN INSTRUMENT LOGSOOK. (] . [) CALCULATE CHARACTERISTIC ION AREAS Or ANALYTES OF INTEREST AND ANTHRACINE-010 INTERNAL STANDARD. .......................M | ) CALCULATE CONCENTRATION OF ANALYTES OF INTEREST USINC THE FOLLOWING EQUATIONS: PCS Chlorine Class Concentration Chlerlna Cisco RRF (Chlorine Clsso Ion Aria) (Chlorine Class RRF) (Incsrnsl Standard Area) (Charactarlacie Ion Araa Cor Chlorino Class) (Chlorine Close Concentration)(Internal Standard Area) Total PCS - CL1-SP Concentration CL2-BP Concentration Concontrselon CU-SP Concentration ... CLIO-BP Concentration MS FILE NUMBER: ................................. DATE/TIHE COMPLETED................................ / ANALYST: ....................................................... ESC JOB NO: ................................................ HONS 024995 METHOD FILE LIST Method file: PCSC2S Teeperetur*: Source 200.0 GC type: 3940 Colxan: Cop Isothereal M Run Typo: SIM, Splleleoe: Yoo Pose Run Tloo 0.0 CC, El Run tine: 40.00 Scon Store tlae: IS.00 Roloy ol Roloy 02 Trioo oO Trloc ol ON 327.0 327.0 327.0 327.0 OFF 327.0 327.0 327.0 327.0 Oil 327.0 327.0 327.0 327.0 OFF 327.0 327.0 327.0 327.0 Sin Paraaeters: ifunber of groups: 3 Multiplier voltage: 2400 Salsa Ion current: 300 uA Croup 1 Croup 2 Croup 3 Group 4 Croup S Stsrt/Seep IS.00 22.SO Seort/Stop 22.50 29.30 Seorc/Stop 29.30 40.00 Stort/Stop 0.00 0.00 Searc/Stop 0.00 0.00 m Dvall -II*.0 -140.0 -144.0 -144.0 222.0 -224.0 25J.4 -257.4 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 100 100 100 100 100 100 100 100 0 0 0 0 0 0 0 0 0 0 0 0 K/Z Owsll 255.4 -257.4 -214.1 241.1 301.1 301.1 -323.4 -125.4 -354.1 -341.1 -343.1 345.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 100 100 100 100 100 100 100 100 100 100 100 100 0 0 0 0 0 0 0 0 M/l Dwell -154.1 -341.1 -343.1 -345.4 427.7 -424.7 -434.7 -441.7 441.4 -443.4 -447.4 -444.4 504.4 -511.4 0.0 0.0 0.0 0.0 0.0 0.0 100 100 100 100 100 100 100 100 100 100 100 100 100 100 0 0 0 0 0 0 M/Z Dwell 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 M/Z Dwell 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 00 0 0.0 0 0.0 0 0.0 0 0.0 o 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 0.0 0 HONS 024996 Appendix C Summary of GC/MS Raw Data and Detailed Lotus/1-2-3 Outputs. This section contains chromatograms and Lotus outputs generated for this set of samples. All chromatograms are the sums of the intensities of the selected masses monitored for PCBs. HONS 024993 'I I *i rn i ft p4tv SlaaM (IS tt/al por co^Mt) "11 A|iiu|iiinAw|iiii|iiii|ii^iii|iiii|ii/|iiii|i Q| I?.0 lB.0 19.0 20.0 21.0 22.0 23.0 24.0 1.0 26.0 27.0 20.0 irocJor 124$ fauifolont to 5 ug/UUrj 4k. 29.0 ...............................................^...L...m...a.J..I..l..r..A..a..J...I..a.A..u......A.Aa.A._.<.w.......... ,...., 17.0 10.0 19.0 20.0 21.0 22.0 23.0 24.0 20.0 29.0 27.0 20.0 29.0 Arocior 1242 fauirtfont to I m/litorj 17.0 10.0 19.0 20.0 9nTjiimW|iinnni|iiMfiiinmi|iiupfW|innwpnnmi|nin 31.0 22.0 23.0 24.0 20.0 20.0 27.0 20.0 29.0 Arocior 1232 (equiwkhnt to 2 ug/UUr) fln.aT~ 17.0 ia.0 19 0 20.0 21.0 22.0 23.0 Arocior 1014 (equiraaJlooat to I Uuff//lliittaorrMj 24.0 2S.0 20.0 27.0 29.0 29.0 | 11 11 llWf I\ I'i'lTjV 17.0 10 0 19.0 20.0 21.0 22.0 23.0 24.0 29.0 20.0 27.0 20.0 29.0 9000001 Arocior 1221 (equiraiiat to 5 ug/UUr) 10.0 21.0 320 23.0 24.0 29.0 a 0 27.0 20.0 HONS 0 2 4 9 9 ft oil 1 CNVmr SUmdard (1 ag/mL par eaaapammat) 24.0 29.0 29.0 27.0 29.0 29.0 90.0 91.0 6 92.0 99.0 94.0 99.0 7"SgMAi-gttETT g 1Q A A kk k * a. kroclor 1288 (ofolvalcni to J ag/Uler) Hum hi. Him, *.- 24.0 29.0 29.0 27.0 29.0 29.0 90.0 91.0 92.0 99.0 94.0 99.0 60000'] j I Aroclor 1282 (iquinliolnnlt to Ji Mag//UUtloar) A/W_A 24.0 20.0 20.0 27.0 20.0 20.0 90.0 91.0 92.0 99.0 94.0 Aroclor 1280 (equivoaliecnt to 2 iOtrg/l/iltitaarr)) """ <|iiir^r -A, 1 ^ _m mL^JuuL^ --^ 24.0 29.0 20.0 27.0 20.0 20.0 90.0 91.0 92.0 99.0 94.0 | Aroclor ISA (jUuiral^it U 2 ug/lilar) M(U-*; MUM~~ 39.0 99.0 24.0 29.0 20.0 27.0 20.0 20.0 90.0 91.0 079 < v < < ......................| 1. , 92.0 99.0 94.0 99.0 MOMS 0 2 4 9 9 9 200000* * PCI-2302 f/101) 4 MM; mi IS .0 100000' * IS .0 40000* 20.0 21.0 22.0 23.0 24.0 29.0 26.0 1~ fCB-2300 f/J09) ~ l ttMW.MMti . T. ----Av----*A/a--^ 4 I'rrM't i * !-* 20.0 21.0 22.0 * (*j> _ 23.0 24.0 r' ........... .. n*nnM 29.0 26.0 , ,, M HI MMi Hu m - - - - i- - -______^ 20000* IS .0 100000* 50000* 20.0 21.0 " --_ KB-2308 (/107) 22.0 -- ___/i 23.0 24.0 29.0 26.0 *!. Mini} ma.m A 1. J LJ\^Va_~Ma___M-A--n,--A/ILJA^w^ 19 .0 20.0 21.0 22.0 23.0 24.0 29.0 26.0 40000* 20000* IS 0 pi K*'"7T 20.0 21.0 22.0 23.0 24.0 29.0 26.0 Mtfiiu - mmm t ma* iroclor 1249 Standard (equindant to 9 W/liter) i j|l . K i ^CLv^Jw_J\JL____ A/vLJU^_^_ 19 .0 20.0 21.0 22.0 23.0 24.0 29.0 26.0 MQNS 0 2 5 0 0 0 HONS 0 2 5 0 0 1 tMMTf if Nany m >l|iw mt MM Hr *} Nl IMS IMI rot 0*10041100; mmmam lM0> *ii nr Kt mr MM> (wo/M loMI 101 1102 noj Kt )W K 230) Kt 2SO* lOMI <w0/<4> (utSMt (W02M1 tw*Mt imi awMonM#0"Vl* WMooOMUMHVto totOhtOtOOt^MflO^O MnOtanMOOtio OOOMMotoM^MnttO MoOIOoott *............ 0 0 0 0 0.3 0 0.) t 0 0 0 0 0 10.2 0 0.4 4 0 0 0 1.2 0 0 30.4 0.1 0.3 9 0 0 3.9 0 S3.2 0 0.1 > 0 1.2 0 4.9 It.4 0 0.) 3 0 0 0.1 0 3.0 1.4 0 0.) 2.0 0 0 0 0 9.0 1.2 0 0.2 .t 0 0 0 0 0 2.3 0.3 0 0.1 1 0 0 0 0 0 0.1 0 0.1 T on mm mm w --mioiot too* mm m ami mai _j 11JBILi, 0 0 (i mi n 09 t M 0 tt MCI n t 90 U 0 0 It MO) 79 MO tot 139 2 2 It MCI II n 00 112 1 0 it MCI 09 119 no 120 10.3 10.S IS MO 02 no 129 202 ft.) ft.l It MO 44 m m 132 0.1 0.1 It too n oo MS 124 2-4 <- (t MO 111 04 m a 21.1 no ft MO tt to 04 M N WM mmmm mam aw awt Ml H9M0 I.OOt tOM H9t90 o.oot 1000 HS91 0.001 MOO H9IS4 0.001 1000 Hi199 0.001 1000 19144 0.001 1000 H9M9 0.101 tooo ninot I to I OkM put*. Man mM ho MariVfiM m i 0.1 uf/M. KSM4 0.001 MOO 19142 0.001 MM 19192 0 001 lOM Ml Milt tttf 01 Mfoa t-taplo Oolfotlw ft to ffllOtap 111 0*01 #102 ftoi tl M HONS 025002 IM* I. n-- ry ef loamy K9 Analyse* of Wacar far lreject M222 1AU *1 Avarafa lalattv* lasporae factors dwriiat far Cask conpansr Class Characteristic 1statfvs laspsnsa faetars iaipania laspsns* fra* frea standsrdi standard Cll b**onyl *2 CM bipeanyl S3 CM OipOsnyl * Cttbi^wnyl C19#1i aibifawnyt M CUbifksnyt 97 afelpMnyt M dTttpfcanyl M aSbipkanal *t0 ClMIpbcnyt *11 aSbi^MT'yl #12 aaiptanri ns awfAmri in (llki|ksnrl IIS CUfelfk 12C1XM* CDblptonyl 917 aSOlpMnyt 019 aSOlptonyt 919 UMipHanyl 20 ClAbipftenyi 21 CIOblpMnyt C22 Cl ytpiwyl 123 Cl Tbipfcanyt 121 Cltblpunrl *23 ClMips 1203*2* Cl1bif*ayl *27 CltObipfcinyl *2S CllObtf* 1203*29 fl.40* 0.4*3 9.74* 9.*09 9.241 9.447 9.33* 9.49 9.299 9.2*7 9.297 9.219 9.192 9.21* 9.179 9.0*97 9.0*11 9.0*27 0.133 9.1 0.09 0.0471 0.0413 0.0251 0.0*77 0.934* 0.93*2 9.910* 0.41* 9.4*1 9.7M 9.042 0.243 9.49* 9.3*2 0.491 9.293 9.2*7 9.291 0.219 9.17* 9.229 9.119 9.09*3 9.9941 0.95*4 9.119 0.99*1 9.9*73 0.9304 9.9343 9.9212 0.0341 9.9299 9.93 9.0139 laspanaa Iras nadari 0.44* 0.31 o.m 9.79 9.2* 9.47* 9.399 9.4*1 9.312 9.392 9.2*1 9.21* 9.174 9.229 9.144 9.0*93 0.9951 9.9533 9.111 0.0757 0.0993 0.0347 0.02*7 0.919 9.0302 0.925* 9.0249 0.012* Avarat* laspanaa Faster 0.424 0.409 0.7*3333 0.793333 0.249*** 0.4*9*** 9.3*3 9.454 9.297*** 9.209*** 9.29*313 9.217333 9.177333 9.223 0.153*** 0.9*51 0.09*7** 9.057533 0.129*** 0.M72** 0.9*953) 0.040133 0.0351 0.021433 0.057333 0.9207** 0.0313** 0.015 Avsrat* Canpanar Oaapanaa 0.9*1777 dl 9.793333 C11-C13 9.391993 CU 9.294222 tt) 9.2999M a* 9.153*** CM-C1S 9.9509 ft) 9.992155 a* 0.917*1* Ct7 9.921433 CIO 9.997313 a*-C13 9.9297** at 9.9313** al9 9.915 ai9*C13 HONS 025003 iiiin im iC E ttititiiifiiiitii tMMrv Iwn Kl M|iMt nmw iw mtn ----- CkaractarUtlc Ian lipwi / Canflnrtnt In I Ml II UtMMIIM HJ194 H9M2 >i)M uut hum HUS' W far KM Ntactal H$tM H.SM H9M4 >19142 HSW 4aM0<nMt) m tss Ctt-W-tK1S torr. MM-CirMl MM ni-IMKt) tor. MBlMlInil ttM UM*U CIW M IKD Mnr HONS 025004 I ToMt I. c S1ATIIIICM (VMUftlION Of SUftOtATC STUIVS tOVOMI fcmary of Koomy KS AmlyMt of Motor far 'rojoct *0222 MWU C8MMIMM MUCK MCMtlfl; (1 MCI SfMOMt NVIA1KM (I MO mihimi MCOMtT a mo NUMM MCOMtr It MO M1NM0MMM Harvcfclorfcipfconyl-K13 9 U At 111 It IttruMfOipfwnyl * 1X1) OS M *1 111 It kinilir*MNitri - 1X11 tt X St 12S It imrtlirilipiiinri * 1X11 11* 42 S3 207 M Wltfl NO Ail MOKAlfl ft 27 St 207 40 rtMUorr tisiiiMTiao mcomaiu rat t 4o -m- VAUftt ?/>/& t*N M-St St-70 7t-N to*lit 110-11* IN* IS* ISO* Itl a Mci (I MO ft MO ft MO ft MO ft MO ft MO ft MO ft MO MwcMfMMwwyl -XU lolrooMorofclplHwyt - 1X11 OKtaritlorofeiffcoffyl 1X11 NtKlIanfetfMnrt - 1X11 4 2 1 1 0 0 t 1 2 S 2 0 t0 1 0 2 S 2 0 t0 0 a 1 2 1 12t1 fOt U SUMOIATI VMUCS. i 14 2 1 HONS 025005 M(| I, Mam ll iMTHf K f MH*r far WH (MB UH FM CAIIBMHM: Hill} Him Htm mm M. IMMCT MNI IMMMB CUM iin*ii nnH na it im mr <m m* tt tit* am Klim KB 22tt KB IMS KB 2M Kl 23*2 KB 1M KB DM KS Utl KS 2M KB 1 (MMl <MMI (AM) (MMl (MMl (MMl (MMl (MMl Mil (MMl MiaiiaiMMU IHMirAiAMli IflAIWAIAMll ihinmvmiak* MMMtrM*ftoM<B MMMlBrMCMrl kiaMmlifiMMi mmMbmMbImM* B.1 2.1 l.l 1 1 .( 1.7 2.4 1 2 2.1 M.l 1.2 l.l 1 1 I 1 .1 1.9 *.* 1.9 t.2 l.l 1.2 1.2 1.4 l.t l.l l.l l.t 1 1.) 4.2 1.2 2.1 l.t 1 I l.l I 1.2 l.l 1 1.1 1 1 1.2 mi .1 l.t 1 1 1 i. l.t l.t 1 1 1 1 1 j l.l l.t 1 1 * mm, mm w nwcu^o l.f 21.1 24.2 l.l 1.4 S.l l.t B.t MMl KM t tMII IMU l.t M.l M.l . .4 9.1 t a.t iwMManMfiMRrf-mis ft MCI ft MCI AMD VMM n mm n mm Ji n w n m tit n n w mi M M IHI MUM MOM i Hint i 1*I4J I H4M2 : HSMB i HSMt : KIM : K51M : H9I12 . ONI t hSMT Ml .Ml B.M1 I .Ml I.M1 .MI B.Mt .M1 B.M Ml IMMO fMM MUM Ml MIMMIM IN IIBMI Ml* BM*I (WMMIlM rM I I IkHM K iMtffTMM N < 1.1 IBM tMr lOTMMMR C Mart I ImHi Mi fun mi m IM*ll lfc nir HONS 025006 tabu 2. lu--ry of laarny PCS Analy--a of Uiitf for PrajKt 90222 i--U a Av*raa aala'iv* IttponH Factora Control^ for Cacti Confonor Clooo Chorocioristfc lot it tv* lotpoMt Factors MpOMO iMfMM fro* iiofirtf Irm 'ardorS etc OipMorl CM tf--1 fl CM OfpMwyl it ClUtlpMvl CIM1 Clfot---- ClftlpNnvi IT Cl2tfMmrl -- 02019--1 09 01--9--1 i1 Cl)--vt fit Cl 1-9--1 f12 ClibipMnyt ill C14--p--ft fH Cltbi--aryl 15 Clt-- 1203919 05--9--'* 17 CL5--9--nrt fit CMbiftMnyl 19 CHiifMnyt i2t 09--yl f21 09--9--'* i22 ClTbffMnyl 923 07--pMnyt ttt Ol--pfcanyt #25 u--i-- 1203929 CltoipMnyl 22 CL lObipMoyt 2t CMO-- 12C1S929 9. tOt o.at 0.724 ** 9.251 9.449 9.551 1.02 9.291 9.525 9.501 9.259 9.195 9.259 o. tat 9.9299 0.0992 9.9200 O.U 9.11 0.0009 0.9522 0.0922 0.9209 9.0229 0.0521 0.0909 0.093 0.905 9.422 9.225 .Ml 9.222 9.599 0.555 9.502 9.210 9.201 0.292 9.215 9.125 9.209 0.12 0.0992 0.0595 9.959 0.0995 0.0295 0.0959 0.0425 0.9570 9.9252 9.9499 0.9545 0.0555 0.9191 la--an-- fra* HwdrO 0.450 0.519 0.204 0.952 0.255 0.441 9.545 9.44 9.504 0.519 0.292 0.222 0.109 9.251 0.171 0.0999 0.9919 9.9952 9.115 0.0915 9.07 0.0493 0.9415 0.0291 0.0572 0.0520 0.0349 0.9125 Avar--9 taaparaa Factar 0.415999 0.409999 9.745999 9.949999 0.229555 0.429555 9.545 9.429999 9.295999 0.500555 9.200555 0.229999 0.105 9.225135 0.125 9.021019 0.0922 0.094535 0.117455 9.093555 0.074055 0.049999 0.042199 0.029235 0.059933 o.oia 0.0371 9.017455 Avar--o Con--nor 0.5499-- CM 0.9499-- 01*05 9.557055 02 0.292444 05 0.212155 04 0.125 04-03 0.099055 03 0.0952-- 09 9.045419 07 9.929255 O0 9.059951 O0-C13 9.05a 09 o.7i a* 0.012955 019-03 HONS 025007 is x ttiS H u tim J trirlilH li iunry #1 *vrwy KB tatlfMi *t VMtf fr Mtt OMrvttvrUtU 1n li i ib utOMfian / CmflraiK In I Ff KS MNlrt m Cl IlBinyl VI HJ1U HSin >ism HSIU lSI*l KIM! nSMB lSMV HSI7B U1B VIM BMB MB' tsrc Him *ism fta MB ism m *-Q VlyMwI M1l m m-iiyMKi MB Ctl VIMlM VI IM fit* IS ID CU-BIpMM BIB tU-W-WCU torr. V ft! MBwrl VI mb ob mbmki it m cu-wmm IBB ai'B-WII tor. Mi mt'iton* MB OIHHKI) tor HONS 025008 fM 2. t SIAMSTICAi (VAIUAMON Of SUMOfiATf SPtKtM COMPOMt lilify (f Ktamy K0 Amif*-- f Wlir fw PnjKl 10222 MHMAft caecum mmcOlfU<A**Anyt-AC11 lMrMOlrm#iHAri 1X11 OmtMmMpNnrl * IKU nifMwyl 1X13 MtiUCf m AU MMNHAKt AtttAM III MCSWRIII IX MC) 97 94 94 112 too IIAMN MVIA1IOI IX MC) 12 H M 40 11 NIOinM RCCOMRV IX MC) 70 74 01 30 30 NMIMtM MC0MRV IX MC) 117 MS MS 221 220 WM Of MICROHMMM M M M If 40 INMKT RISIRtRUtlON Of MCOMRIlt in i 4o 7/\/ig ^T VAMCS ( R-30 M-M 30-21 n-u 90-110 110-110 130-130 ISO-MO >100 ix mo IS MC) IX MCI (X MC) IX MC) IX MC) (X MC) IX MC) IX MC) NnMM*rmfMnvl MIS iwricAtfMIpMwyl - 1X11 onuMweiewri * iXU wwOlorAiRMnyl IXU 0 0 1 24 1 R00 00 0 2 4 1 0 0 1 0 01 3 1 0R 1 0 01 02 3 1 0 1 100 AU U0OOMI1 VAlUit 0 0 H 4 1 2 1 HONS 025009 Mat tv* Sefkiflf 0A/CC laswita lor Caarnv Pd in Malar Analyaaa Ofwra MS Addition ( 24 u and LS - Addition af 2.4 o# fCSa> Mrojd MS CAUS MUi HStt? It CAUS MU: h)IM I110NS fCS 2299 it MC> MS tK it MCC) MS SMC (1 SIC) #110 IS MCt 2299 it MC) IS SMC < ACC) IS SMC it BCC) 002 Cl'Oipfcanyt 01 M3 12 104 IS 104 Cl2`fci|Mnyt 1 mr - 2 M S 09 4 ill cis-o40Mnr* 1 ill 12 ill 3 u CU-ttfMnyl II 0U 2 IIS 3 ill ft>4l|Aatyl 1 ill 12 119 * IS Ml (iHIfAanvi II 21 2 22 n 23 CUbiffcanyl ii 24 2 m ClO-OfMAonyi 27 ClO-MtfMwnyt 21 ClM'ttflwnyl 07 too 10S 9S too MO OS 100 10S 12 100 94 07 too 10S 7 100 97 14 too 94 42 too 92 OS too 94 OS 110 09 07 100 9S 114 MO 90 M too 90 90 100 04 00 100 104 79 MO MO 91 too 107 07 MO 4S 00 too 104 04 100 99 00 100 104 IS too MO 00 too 107 00 MO 99 00 too MS 01 too 94 7 too 10S 07 MO 94 91 too 114 70 MO 92 92 MO 112 7S 100 94 00 too 90 43 100 79 99 too 104 43 too 79 too too 104 70 too 2 97 100 121 77 100 MO tot 100 m 70 MO 92 IIS too 12S 70 100 MO too too IIS 79 too 99 ns too 114 $9 too 91 SUMOMIC COWAN*1 009 4'Cl-OiMMnyl -4CIS 91 too 102 14 C14 W-12C1S Surr. 104 too 12S 24 tlOI9-1K1S Surr. 99 100 104 29 ClMOMWCU St*t 122 too 127 90 too 01 too 56 MO 55 too 94 94 74 07 NS MAM MU s H51SJ : *15157 : >lS17S : l5152 : >15154 : >15174 Mote locovorios aro tat I to Dm noaraat Mieli i HONS 025010 t *4 irUr ImilillM >w>yi< *tA tm iHliri IM l iMmy Kl In Matr Myili Mm ' eaiiAMticti tsm Him Mill . I1MAC1 Mil IIMI IHHI IIMlNM IIN2 (1 rbI Mm is mm *m* <> mm A IMA (A.IPAM AIMA IS ppO AtMA (I rm AMI* 11 MB> Aim 11 MM (MAI KAMI lM) (l) I4M) It***) </*! iiani) ii*i tmtmt Mlkl>*l|>W|U lliMir<i)>wrU MfNMmfeMMl MllfelMM#in|fll milMlMlIIHH** iMMnMiiM'ii MmiKwni T"""I--| |- A A A.At A.AA A A A A A A.AA A.11 A.S1 A. 14 0 A A A A.AI A. If 1.11 l.SA I.A7 A.AA A A A A.AS A.S2 1.2* A.AA 2.2* A. 1* A A A A A A A A.A A.AI t.m A.ir A A.If *. A.AI A.2 A.S A.M A A A A A l.M 1.U A.tf A.AA A A A A A A.JA IIS A. If A.M A A A A A A MM *.at 1A AJA A.At A A mm mm w oiaaciii^m mu* tm w mm tmtu A.AA A.AA A.AA A.W A.ft t.N AM t.m 2.2A 2.2A A.* A.Af f.SS 2.11 2.M A.* A.M f.SS 1.11 l.M MAAAAMA MM tW>MI*IAin>IMI AlMMAMfMrl IR1I AAMMlArMIM"A - MC1S It MCI A A A A IS MCI A A A A IS ACC) A A A A (SACO A A A A IS ICC) A A A A IS c> A A A A IS AC) A A A A IS MCI A A A A IS MO A A A A is sacs m tm mi AMWMAA IMW 1 HSIf* iMtif mm <a> IBfAACt MAM M <*) mmmm am nmi > HHt (MMfMlM ar r 1 1 1 UMA 1 1 1 Hfltl 1 1 1 HS1A2 1 1 1 tSIM 1 1 1 HftAS 1 1 1 Him i t k imirpni^ m A.) /. UNI KSHV l 1 1 1 1 1 DIM 1 1 1 IjM MMfMM* C aii mu mi MGNS 025011 Table 4. a yu--ry if Aracier Ferwlatiane Imlytia vilh Cwymif Oeepanaa Factors Used In Ceerny PCI in Water Analysis Quantitation 1*<e al Average Relative Response Feelers Oenereted Far face Cenftner Claes Characteristic Relative Response Facters Iren standard! Ires stem Averape Retpenee Faster Cll biphenyl 1 Cll biphenyl PS CM biphenyl P4 ClAbl0kenyt SCIMl Cliblpbenyl M Qiblphenyl 07 Ct{biphenyl AQ Cl{biphenyl IF CllMphenyl 014 CllMphonyI #11 ClSblphenyl P1{ ClAbiphenyl PIS CUbiphenyl 014 Cttblphanyl PIS CMM0> txiiaia ClSbi^enyl 017 ClSbiphenyl 019 ClSblphenyl P19 CtAbiphenyi 020 ClAbiphcnyl 021 CtAbiphenyi P{{ ClFbiphenyt 021 Cl Fbtphenyl 024 CtPbipnenyl 23 CtPbii* 1201024 ClOMfhenyt P27 CllObiphenyt 020 CltObiph 1201029 0.404 o.ai 0.724 0.A4V 0.231 o.4a 0.131 0.4A2 0.294 0.123 o.sot 0.230 0.191 0.239 0.104 0.0704 0.0497 0.0700 0.14 0.11 0.0004 0.0322 0.0472 0.0209 0.0720 0.0171 0.0400 0.0191 0.403 0.472 0.721 0.440 0.222 0.399 O.SU 9.107 0.20B 0.201 0.247 0.214 0.17} 0.204 0.17 0.0447 0.0344 0.049 0.0991 0.979} 0.9449 9.0474 0.0170 0.0232 0.0490 0.0S4S 0.0S33 0.0141 0.410 0.314 0.7S4 0.432 0.233 0.441 0.143 0.44 0.104 0.119 9.297 9.227 0.199 0.231 0.171 0.0409 0.9419 0.9412 9.111 9.0913 9.07 0.0441 0.0413 0.0241 0.0372 0.0120 0.0149 0.9173 0.41344* 0.401444 0.741444 0.449*44 0.229111 0.429133 0.141 0.42944* 0.293444 0.300333 4.2001S3 0.224440 0.1PS 0.223113 0.173 0.071004 0.0*27 0.0*4311 0.117413 0.091311 0.074011 0.040444 0.04214* 0.024/31 0.039911 0.0140 0.0)71 0.017411 0.34944* ftl 9.419444 ai-CIl 0.137113 at 0.297444 ftl 9.212111 CM 0.173 CU-C13 0.044033 Cll 0.0932*4 CM 0.043414 a 7 0.024733 CM 0.039933 C10-C11 9.9140 C19 o.oiTi aio 0.017411 ClIO'Cll HONS 025012 3 i )S S S iS 3 2 2 2 2 2 3 1 2 2 lltll> llI is ia tiiiiittia m tiin iin iii IlM* . I Iiit--h to ItkIit ImdiltM tmlVlrt ** (pr >i>wi IKIWI Wm# in iNrnr Kl in Mtc *"**<* ImmIImIw -- ................... OMfMiiriHic i inm / maM wcc* w catcuiiiiton 1 42 <S M 12 f) t)t*S Him Him 1)129 tSIM HSMI iw HtwiM m ir km iMtttd mi mm* 14 IS 14 17 19 >1)192 ism >15149 HSI91 >1)194 ................... 19 IM H5I92 Him mwmm imm hm mm mmmm nm m mnrmmm-rn m #n M MH m m 4-n M0wwi mii M MllMI)nl ! MM m Mt M MM>Ctl'MMMv> #11 Ml MM (Ml* #19 MAI-MUmI #M Ml MM #M - M CU-M'MII tor. #1? m Ml MM #1* m M(U'W#Ml Ml Ml Ml# Mf " Ml M-CMI#iiM Ml Ml MM m MMU-Mmr1 CM (iHI-lKtt lurr. Ml M9 HI Cl W*to* MCI) Mrr 1M Ml 10* m m IS) is* is* m $ 94 H 11 n 19 ii a M *S 121 1M 1M 19) 10) 92 91 29 111 111 9S2C 2M 299 >91 lit 1S9 m is# IS# 1M 99 91 U 1) 19 M 9* 92 92 119 1)9 1)1 m 9S 12# 92 9 12) IM 9S21 MS M9 M9 M9 1SS 111 IS) IS# 9# 95 95 M 1 1 1 99 42 45 129 in 12) IM 105 92 91 12 IIS 11# 935# 9 9 9 9 9 9 9 99 9 1 M 9 9 9 9 9 9 9 9 9 9 9 9 IM 9 0 199 nu 9 9 9 9 22) 9 9 9 99 9 9 M 9 9 9 M 9 9 9 9 9 9 9 0 9 9 9 9 922# 221 9 9 9 142 9 9 9 99 9 9 M 9 9 9 M 9 9 12) 9 9 9 9 9 9 9 9 9 9121 SM 9 9 9 144 9 9 9 94 9 9 91 9 9 9 9 9 19) 9 4 4 4 4 4 9 4 4 9494 4 4 4 9 9 9 9 9 9 4 4 4 4 4 1)4 4 4 199 4 19 9 9 4 9 9)71 4 9 4 4 4 4 4 4 9 4 9 9 9 4 9 9 4 129 9 4 11) 4 4 4 9 9 9 92SS m 9 9 4 142 9 4 9 99 4 9 91 4 4 9 9 4 4 4 9 4 9 9 4 9 9 4 HU MS 4 4 4 1S9 4 4 4 94 4 9 41 4 4 4 9 9 4 4 4 4 4 4 4 9 9 4 9)71 M7 9 4 4 IS* * 4 4 M9 4 * 9) * 4 9 9 9 9 9 4 9 9 4 9 * 4 4 9U* 4 4 4 4 4 9 9 4 m 4 4 99 4 4 4 9 4 121 9 4 217 4 9 4 4 4 * HONS 025013 >tiri MM* tn 9--my Kl In tM*r AMtyvIa 9wamltMli AIMS (t (p tUU (1 M lt#MI liMI MHMOTMflNHrta MMmkKiwirii UMttw^HfMnyU Wmiiirti)>wiiU NiMMinM|kvit toawMrfcMi*nirli tmMilmtlMunrli 1.11 9.19 t 9.M l.lf 9.94 9.99 9.9* l.4 9M m* nm m amcus+m) Wm NM II MM <**) 1.4/ 1.4/ 9.N l.ff m cuiauritt; hsms mnwiiimii ixu Mw9UHM|lH-- * IXII <1 MC) 9 9 9 9 9 9 9 9 m mm mi : llll9 t Him mmm tmm li MM MMM (> 1t IMMT1 MMM MUM mi - 1 i MMMMMM IIIIMI MM* 14999999 14999999 Ml* (MMfMlM fM>4 rt fMlri li i MtMil |km. Wuh M 9 MmmII b* fmirfrititf m < 9.1 ugM* Mi Mk mil Kll 01 HStn Hill* MONS 025014 labia 5. Tttit * Aroelar Pernuletlane Analyiad witb Cumr lupin (Ktiri UMtf In iMnv K> In Meier Anelyata tamlutlw Table al Averape Oeletlve iNpmt factor* (mralid lor Kacb Cantener CIOM Cbaracterleiie MlMlw laapanaa Factor* inpanae laapanaa fro* atanOerbl Iran nawbrfl CI1 blpbenyt M Cll biphenyl fl CM biphenyl ft CUbipbanrl K1)fS Cl2bipbenyt 00 CUbipbanyl *7 Ci2blMenrl M CUbipbanrl i* Ci5btpbenyl * CUblpbonyl 111 CtSbiphenyt P12 CUbipbanyl PIS OAbipbanyl *W 04bi*anyl 015 CUbiph 12C1301* CUbipbanrl tr ClSbipbenyl *10 CUbipbanrl fit Cl4bi0enr1 Ml CUbipbanyl Ml CUbipbanyl 22 CtTbtpbenyt #2) ClTfeipbenyl *24 CUbipbanyl MS CUbipb 1203*24 Citbipwirl #27 ClIQbipbanyi *21 Cl IQbipb 1201*29 0.401 0.401 o.m 0.049 0.211 0.440 0.551 0.400 0.205 0.525 0.501 0.2S0 O.tlS 0.259 0.104 0.0700 0.0407 0.0700 0.14 0.11 0.0000 0.0522 0.0472 0.0209 0.0720 0.0571 0.0409 0.0195 0.409 1.472 1.723 1.449 0.222 0.100 0.55) 0.507 0.200 0.201 0.207 0.215 o.m 0.200 0.17 0.0047 0.0505 0.050 0.0991 0.0793 P.0AS9 0.0475 0.0570 1.0252 1.0490 .9345 0.0155 0.0141 Avaraft 0.450 0.510 0.704 0.052 0.215 0.441 0.I4S 0.44 0.504 0.519 0.207 0.227 0.100 0.251 0.171 0.0090 0.0010 0.0452 0.115 0.091S 0.07 0.0405 0.0415 0.0201 0.0572 0.0320 0.0349 0.0175 0.415440 0.100040 0.745000 0.040400 0.22*553 0.4295S5 0.545 0.420040 0.295400 0.500555 1.200533 0.220000 0.101 0.22555) 0.175 0.0710*0 0.0027 0.004555 0.117453 0.09)533 0.074053 0.040040 0.042140 0.020755 0.050933 0.0340 O.P371 0.017453 0.540000 01 1.040000 ai-oi I.5570S5 ai 0.297444 03 0.212)5) 04 0.175 04*0) 0.04MS5 05 0.0952*0 a* 0.045410 07 0.020755 CU 4.059955 0*05 4 4344 09 o.oiTi aw 4.417453 OII CU MOMS 025015 MM* ft. ft Ummry *4 ftraclar rmilMlM Mwiytaft tritft Cift--r fti^--i Itturi UMft in cnny Kl in Mtr Wiyala fciant Italian Httti hm Him Him Him >isu< i Mft Far Pdi MkM MN MVW Mm Him hitM Him him Him Him fiiiiiu its itiu c n iiis iiiiii is M iiH H tim HONS 025016 Appendix D. Important analytical request and chain-of-custody information recorded at sample login. MONS 025017 Tlaa Staap - <660327.0913> Monsanto cohpant/xnvirobmintal jciincis cun Aiuu.ni* request DAT*: AftlL 23. 19*6 LOC NO: U-66-04-23-02 REQUESTER: MARTIN PROJECT NO: 760.21-1222 LOGIN NOTEBOOK rACI (To bo flllad out ot login.): 3739239 REPORT RESULTS TO: FILES/HEES, HUCHES,SHEEHAN,MCKENZIE,MINOR ANALYSIS REQUESTS SENT TO: FILES HUS. HUGHES, SHEEHAN. MCKENZIE .MINOR SAMPLE PICKUP BY: MCKENZIE SAMPLE LOCATION: U-A20 SAMPLE DESCRIPTION FOR 13 SAMPLES SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC NUMBER(S) 103 1 E 1 L 103 1 X 1 L 103 1 X 1 L 107 1 X 1 L 109 1 X 1 L 101 1 X l L 110 1 X 1 L 110 1 X 1 L 110 1 X 1 L 110 1 X 1 L 106 1 X 1 L 10S 1 X 1 L 111 1 X 1 L 102 1 X 1 L 10A 1 X 1 L 112 1 X 1 L RECORDED BY: MINOR REQUIRES ANALYSES: CC CHRCHATOCRAPHASLES EXTRACTION LOGBOOK NOTEBOOK PACE: 13S.646 ESC STANDARD EXTRACTION NETMOD(S): USEX05 ANALYTICAL TECHNIQUES: TECHNIQUE <EN) COMPLETED ANALYSIS METHOD LOCBOOK PACE X CCCC/MS ( ) 5/27/8E MSAN2S 156.603 - 156,604 NONS 025018 FINAL REPORT NOTUOOK PACE: 3.434,412 OTHER NOTUOOK FACES: QUALITATIVE: X SEMIQUANTITATIVE: EiqUIXEO QA/QC: SEE GOOD LABORATORY PRACTICES MANUAL QUANTITATIVE:X COMPLETION DATE REQUESTED: COmEVTS: SAMPLE DISPOSITION: HOLD ION 90 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME:AAt222:L! 025019 MOMS CHAIN OF CUSTODY RECORD - tfflJS/Wrd'l Project Mo. 0(>O^_______ Project Title MwSAPTP - kM*>y Sample Source . ^***ia/Ctonec<- CoNoetore Nome < ' **** /_____ ,--, y(sft|Cri Field Informotlon mJ_______________ Method Of Shlpplnp ^ elpo -------, tor tdUiL A944C.. Ddte/Tlme v/z/lt <S> OfiZO leceWed B, elgn______ for_______ Oete/TIme Sample DealBBatiea m \D in IQ1 Semple Leoatlee K>/* \1 Date Time vhilrt mo im m* \ mo Analyte iisUsotcb " Me. Of Ceetatnere - UJ~ \ Commenta: ^ jlvvtl~ /pu-***^ HONS 025020 CHAIN OF CUSTODY RECORD - t1l>P/b>7Z> - ^ Project No. DMoS- Projoct Till* - frBAWy mol* Soureo . P/*______________ C.Hsw /I.Chmeli / CoNoctoro Homo print PloM Information Motkod Of hlfflif By: for. Oato/Tlmo ft* -------------- -> looolvod ) *lgn_____ for_______ Dato/TImo DMMnotloa /^/ Somplo Location vU y*" XCIIt \1 Oato Tlmo Ml/tf UJo lies an; \ ' I&S Analyto ' No. Of Contalnaro hti^jL 1f Commonto: HONS 025021 CHAIN OF CUSTODY RECORD- HWS4*>7V Project No. 06Mf______ Frojool Title MM*A7Z> kT&M* y I anipplnf /gfl &C. Date/Thoe V/w/M <__ 3*20____ Doto/Tlmo DOOOlOMPPOIOtlOO Soioplo Location Date Time Analyte /\0b ' IDi no m /a \1 Hk/n II K t tizr 1*110 V )HOO LxfUit1ict< No. Of Ceatalnoro /^ Commanta: tUOMyyg /7 t7m4*~ LL- 025022 hons CHAIN OF CUSTODY RECORD - Prolaet No. _______ Protect Title MMSWTd - IrtMSy____ ____________________ - Lf M/+Sample Soarea _ ________________________________________________ 6 &Colloetorc Nome , /Ct*h.uL. rlrft Field Information v//t____________________________________________ Method Of Shloolna__ /SV__ &C_____________________________ ftoHoqolahod By: alee /^yy i^tvfc"-- IOf A*S*<=-_______________ Doto/TImo g- 2la..... By: elf a lor----------Data/Time tomato Daalaaatleo \DV- /z>V IIX Sample Location /'/a i1 Data Time V/az/i? /f/* \1l I7I& Analyta hishiottk* + No. Of Coalminera f- //#A i Jr Commanta: 7tn**JT U- HONS 025023 Appendix E. Descriptions of important terminology used in Quality Assurance/Quality Control. Analyte Extraction, and instrumental Analysis. HONS 02502* Quality Assurance/Quality Control Terminology Thu lection describee commonly used terminology and ptirasea which are need in rnnjanniun with Quality Astaraace/Quafity Control (QA/QC). This information may be helpful in imitrinsating tome details of QA/QC procedures which here been incorporated in the present report. The blowing two sections also grin useful information concerning terminology used in analyte catraetion and instrumental analysis of samples and sample extracts. f|--IIIT illUrimil'TTHII flllrj - Terminology used to describe activities which are desgncd to produce analytical rcsuki of known quality. In an effort to minimize costs of environmental msl) i. specific QA/QC elemcats have been incorporated into ESC/UAG extraction and analysia ueps which should not unduly burden analytical autfics willi large development and method validation costs. This approach baa been taken so that sets of samples can be analyzed for various analytes without extensively validating methods oner wide concentration ranges and without using methods which arc designed for only one matrix. One pries which one pnys for this approach is that analytical precision and accuracy are sacrificed, somewhat. However, in many caaec, when clearly defined regulatory limits have beca set, confirming that the analyte ie present at levels we* below or we* above the Kmit does not need the type of accuracy that is required when the tegaiated analyte concentratios is in the virinhy of the Hgsimoij limit, la these latter enact, more extensive QA/QC procedures are required than arc included in the present study. IIbUh Terminology used to evaluate the reproducibility of e certain determination. Parameters which affect welyiis prerieion range bom temple eequiaition, to sample storage, to sample extractton, and firmly to sample extract analysis. Normnfiy, the major factor which affects the precaioa of the analysis it the sample extraction step, This step normally results in sample analysis precision on the order of or - 30%. The precision of e rank can be determined in e number of ways. Replicate analyses of the same sample, followed by the ralcalelioa of e percent relative standard deviation (or that determmation is the moat popular msthod of amcmiag precision. However, Hue calculation should not he made when there are less than three repficale points from which to calculate the percrat relative standard deviation, la adiitiea, repfieme cstractioaa and teplicate instrumental analyses mum tin ha sot anrmafiy obtained anlem large studies am being conducted. A second method of aaaeamag p~hi-- ie with dm nee of duplicate analyses. The present report iadudei results of it lead one - - -- - - - - . J|it|sample which wee enalyiad in dnohcme lUOTt:; Is to the rasanarthitu of the i ' ' iwimbififa HOMS 025025 Page X Quality Assurance/Quality Control Terminology (corn'd) Aeramrv - Terminology med to determine the 'correctness* of the data. The accuracy of moat Step* in (ha analysis of samples is lypiray oo the order of 10%. Hosew. whea aaalyte concentrations ia the i--pie ssracts approach the lead of detection of a detenuinatiou. accuracy as weft pn rains cm approach 100% or peeler. The accuracy of a detenoiaatioa of aa analyte alack is preaenr at coacentratioaa which are much peeler thaa the instrumental level of detectioa ia oaoat stsotyly aflaeted by the hoeaofcaeity of the sample matrix and the precision of the cmractioa step) which results ia typical accuracies ia caviroaateatal aaalyies oa the order of 30%. Normally, the concernraiom of staadard tolulioaa which are used to calibrate analytical instrumentation are withia 10% of the correct coaccatratioaa, aad therefore staadard sohMioa coacentratioaa are aot aa important factor ia producing iaaecerate data. From time to time, aaalyte responses of standard sohaioaa from dMereat sources will be compared to staadard lolatioaa ased for instrument calibration. Thia iaformatiaa a normally included ia the lection entitled *OA/QC Results' The accuracy of a result caa be estimated ia a aamber of ways. The current study uses surrogate standard recovery aad native aaalyte recovery information to aid ia atenaiag the accuracy of a resah. sample matrix aad performing the various extractioaa. dean ups, aad iaatruiaeatai aaalyam amedmed with the determination. The me of sutrogail also assumes that the spiked surrogates are bouaf ia the mania in tha same way m the analytes of interest Surrogate standards are added to every seatpie while aaliue saalytas are added to only 10% of each set of rampics. Therefore setingiii -y-farf recovery data could ha used to correct the reported results of aa aaalyls concentration, if the aaer of Jhl - Terminology used to describe how the accuracy of a determination may be affected, a negative him maim that values below the correct value are normally measured. A positive him astern that values shove the correct value are normshy manured. The instrumental inelyais step of extract analysis normally does not contribute significantly to ascslysia bias. Most bias ia rmirnamamal snafysis is inroduted in the sample extraction step. A negative him ia introduced when the sample is nos tomplltaly extracted and tha caract docs not comaaa 100% of the analyte. A poauive him ia hniodared whea the Anal volana of the caract ia lam thaa the correct volutes. Surrogate Tiserial da (SSX which ate dbcaaecd ia the asm section. caa be used to determine the asaoam of him which ia NOTE! Nat Lnvat af DHncilaa (UTOt Terminology aaed to indicate what aaalyte concentration wig peedace a tigisaf Tit ~t`t~ ratio of 10. For the present report, thia value is aot tsperimsatariy determined. Noratady, a Uadi of Qeantitattoe is used to determine the threshold concentrution above which aa aaalyte caa be detected. ___ . Terminology used to indicate the lowest analyte concentration which caa rchcbly he quantified. The precision of the delcrmiuatioa of the analyte concemralioa at the LOO ianormaly oaths order of 100%. The LOO ia normally determined experimentally by addutg a haown amount of aaalyte to the sample matrix aad measuring the percent recovery at the LOO. In some cases, when there ia maufTieieat sample quantity, or rof convenience, aa LOQ wM be determined using other methods. These methods should be dearly described ia this report. ICONS 02502b Page 3, Quality Assurance/Quality Control Terminology (corn'd) tmtmPmmkhu.. Termmokgy used lo indicate the inmasfl repotting of the pmtn of compounds la mmif eaeoe, the soara at these fake positive stakes caa be traced to the snalysh of very high level standards or temples ksasediately prior to the rampie ia which poahrie nhel are reported, la order to aaaan against reporting lake potkivct, attempts an made lo inject cleaner uaipici before dhtier laapka. Whea high level compooenO an detected hi lamplca immetfiately prior to low leni -tmfln. then lower lent unplH an rena ro that it caa be docamented that the poahrie values are rent. ],, addition. organic bee water and other aimilar maleriala which an known to be organic free an aaed to document that then an no other nnkaowa tonrcea of contamination which wooid caaac the reporting of falae positives. JEUhJSmIIIB * Terminology aaed 10 indicate the incorrect reporting of the abacace of targeted compounds The coerce of take negatives ia many huiances ia dae to maaking of the --i [inssili of iotcreal by the aaanrie matris or from iaatraaicnl malfunction, la order to determine, eiprrhwtntady. that al oomponenu ia al lampka have been reported if they wen prcacat above a certain level of quantdaWm, a rrpraarntatrie laaapic of each nutria type k spiked with the aaalylea at the eahaeted keel of gucraaallna aad at tea Ikaca the rathaated level of quantitation. The recoveries of these cornpoaadi are then nauand far these two native spiking audios. If recoveries between 50 aad 1 % an eteaaeaed ia Iheae two nadirs, thea the louwr level native spike ia reported to the level of gaoalhnioa for the datermiaolioa, If roeoverka ia this range caa only be reported for the higher level of tpikiag, then ihk higher level wig be gaoled ae the level of gaaatilaiioa. In certaia instances, whea the aaalyte being spiked k ako present ia the inaepk at eowcentrations greater than the level of gaaathellna. corrections will be applied ia order to enhaale the recovery of thk compound, laatnanent etaWaaciioa u a toorca of Fake Negatives ia minimized with the vac of internal Ilsadaidl Internal naadarda mean no Fake Nepalivas an reported dec to Hwtnimcaial oiallaanioa aad tarrogate naadarda iasan ao Fake Negative! an reported dae to eatractioa malfanction. Farlkdr Information The general area of Qaatty A intcsacr/QuaBty Control, along with much of the terminology described above, ia very compies. The fodowing references otay provide farther kforataiion which may be aaelol ia uademaadiag the vafidhy of the resahs teported ia thk uody. MTM ItssSwr risrlht ttaiiM entitled latrakboratory Quality Control Procedures aad a Diecatsioa on Reporting Low-Levd Dau*. A.CTM Standard barllre P27TM7 entitled *Oetermiitation of Preckioa and Bias of Metbode of Coamktea D-1* oa Water'. An nrrlrk la A--hlVst rhrmktrv. authored by 29 wefl-kaowa environmental scientists Thk article waa funded by a pant from the Environmental Protection Agency aad acknowledges 24 addhieaa! icieatista in industry aad gomterwtnl who were involved in the review of the article. It's citation is: -Priacipka of Eaviroamsatai Analysis-. L. H. Keith, ct. al, rinml. Own. I9U. M. 2210 2211 JO CPM Pan ia entitled -Guidefines Establishing Test Procedures for the Analysis of Podetaata Uader the Ckmi Water Act; Feud Ruk aad laterim Fatal Ruk and Proposed Rak'. Thk denaarat isrhtder drtaik of EPA'a MPtttiq aaalytk methods. A current copy of these methods caa be found ia the October 2R1984 Federal Register. Chaaese 11 BlRjlUli I li TTkWIlBItn A--t~ds la Ch--ilfll Thllnll by Herbert A. Laitiaca. published by McGraw-Hill Book Company, Inc MQNS 025022 Analyte Extraction Terminology This section describes commonly used terminology and phrases which are ased in conjnncsion wish analyte extraction. This information stay be helpful in understanding same detada of how snalytti in your samples were isolated for instrumental analysis. Instrumental Analysis Teminotofics arc irien in the following section of this report. - Terminology used to reference the material which you submit for analysis. Samples may be solid, liquid, and in some caeca, gases, la general, when a sample is received for analysis it it fogged into the ESC sample tagm book and proper chiia of-emtody documents are maintained in the esent this information assy be required for litigation purposes Angfati Terminology used to reference specific compounds or formulations of rompoaads Whcaaa analysis is requested for a certain analyte witbin a certain sample matris normally some type of appropriate sohmt Extraction ia required for srrerai raaeoua la ntaay eases tha concentration of the analyte is below the level of detection of the iaalraatcut which will be used for analysis Therefore, coocaatratioe which can easily be detected by the analytical foxtmiitciti. A tamed ruaeon that extraction it required, ia that the sample may not be appropriate for direct inatramralil tealyih of the analyte of interest. This can be easily aadctaiood for analytes in toils Very lew tnalytlral inatrumemi aflow soils to be dbcctly inserted into the inalrumcm, Therefore some type of notation step (i. s cmnetion) ia required in order to place the analyte in an appropriate matrix for instrumental analysis When the analyte of interest ie present at saffidem eoocrxtraoou. and the sample nutria can be drectly inserted into the analysirul iaatruuical. the sample, or the darned sample, can be dbcctly analysed. Huuevci, this case represents a minority of sample analyses which ESC is aahed to perform. Matrix - Terminology axed to reference the major components of a temple. In am cates mayor compaacmi are not of dbect imereti except at they effect the types of extraction slept and other notation proaudurus which mam bn used to holme the analyte from the sample matrix. For the majority of eusitoamental samplxs which ESC is asked lo analyse, the matrix it normally water or sod. Hoamrer, euny environmental matrices contain crlauvrly high levels of organic compounds which may interfere with the instrumental analysis of the analyse of interest. Therefore, depeadmg upon the analyse ef irnrrem. dm repaired level of detection, and the amounts and types of other crpaic materials which may interfere with the instrumental analysis extraction methods mutt bt devefopod which arc very specific for a given set of samples Is order to deal with almost a Kmitkat act of matrices analytes extraction methods and inatntmeatai authods aa organized approach to sample extraction, followed by instrumental analysis has been developed at ESC HONS 02502ft Page X Analyte Extraction Terminology (cant'd) Stott - Terminology aaed to identify the analyte-containing sotvenl which wm obtained from (he earactioa of a certain matrix. .EttKLCkatdU Terminology used to identify chemical step* which are required ia order to reduce the concentration of organic compounds which may bo caractcd wiih the aaalyte of interest. Thcae coeauacted compounds aay be M auch high leach aad/or produce reapoaaea so that they interfere with the instrumental aaalysia of the analyte ia the extract. Exlmctahln Camnaaada - Terminology which refers to the ability of a compound to be hoisted from the saapte taatrix aad piaccd into the earsct solvent. Whea the sample matrix ia primarily soil which coaaiaa little orpair aatlcr. mow orpaie coapooads are extractable compounds. Howe'er, whea the sample matrix ia primarily water, oaly those coapounds which we hydrophobic are extractable - Terminology used to reference aa organized daacriptioa of the uepe ineobied ia iaotatiaf m aaalyte tram a pen metric These taeihodl we assigned short semes which can also be aed a compact file seats for them Methods The awaea of specific Standard Extraction Methods which are aaed ia this atudy we hated ia the final report in the section entitled 'Details' la addition, copica of them Standard Earuction Methods are shorn ia a separate section of thm report. Standard Etfractioa Methods also include details of sample clean-up, if required. Extraction Flow Sheet. TeralaoloeY used to reference a aranhic deacrifainn of s .Sis.d..d Swmh. Method. Thia Qow sheet is filed oa by the analyst ia the laboratory and senes w a detailed record of what occurred in the sample extraction step. Row sheets of individual sample cxlractitaw any be iarludrd ia a section of this report. joaUlMMLlSS) * One important cicmaw ia the earactioa of aa aaalyte from a nutria is the dsteraiawioa of what percea of the analyte wa actually earaclcd from the matrix. For methods which bnohm Bqmd/Squid earactioa of water with aa organic solvent, or tquid/aofid earactioa of sods with aa organic solvent. is is iasperalia dut data be obtained which gives the analysis requestor lalnrawloa conearning wha prrrraap of the aaalyte wa iaolwed ia the extract during the extraction ttps Sino|Mi Stwtfvdi hm this NRportiM pwpoK, The philosophy oa the aa of SonogMc Standards ia a diverse a the analysts who me thcae If coat were no object, analyte lacoacy iafaraalioa could be obtained by the aa of standards addhioa analysis methods. Ilnwarui, sfaca many sampha require eacaeno labor to iaolate an aaalyte into aa extract, naadwdi addhioa aaalyeia methods are loo coaly tor aunt studies. (A standanh addhioa saalyels requiroa each sample to he caractcd aad xaalymd a team three times.) Sarrogsm Slaartwds give the same type of iafnrmatinn, with ooly one saalytia being required. A "Surrogate* Standard is a rowpound which ia chosen to behave exactly w the analyte, h is a arrogate far thm analyte aad than information obtained for this surrogate can be msumed to also apply to the analyse ofimarsa For the aaalysia of regulated analytes, a ia important that when data a generated thm theme thm the aaalyte ia not present, thm we can also show that if the regained analyte were present la the sample maria, h would have been detected. This is especially trim when cumplia earactioa and instrumental aaalysia steps are involved in this determination. Therefore, whea aa earactioa ia perforased, a known amount of a Surrogate Standard is added to the sample befttte any earactioa steps take place. Whea the earact is then analyzed for the aaalyte of interest, the amount of the Surrogate Standard ia also determined. From this information one caa document, ter each sample, what recoveries were measured for thia Surrogate Compound. From this, one caa describe soma level of confidence oa the dwa generated for the aaalyte of interest. HONS 025029 Page 3, Analyte Extraction TermmoU>& (cant'd) A detailed fciMH ea boo Surrogate Standards arc cbosea beyond the scope ot tbia --* oa Analyte Earactioa Terminology. ESC normally aaca Mo types at Surrogate Standards. The first in stheu tba aam(aM ia aaaclty tba tarns aa tba analyte at interest, except that tba aaturriy occurring carbon. hydrogen. Of halogen atomi ia tba aaaiyta bava been replaced with non-nsturady ~~.;-g iaotopaa. Tbaaa anrrogatet caa be expected to ad exactly aa tba native aaaiytea. Oaa food example at tbia type of surrogate ia tba U^TCDD surrogate ia which aO carboa atoms me carbon-13 or ad cblortae atoou are chionac-37. Tba aeeoad type of Sample SUadard is oaa which does aot have the aaate chemical itractatc aa the aaaiyta at interest, bet ia known, or latemrd to ad chemically identical to the saalyte of meerca daring tba extractioe aad dean-up steps. Exsaiplci of Ibis type of sanogatea are dettterated - jinaub which auy be added to a matrix ia which My chroiaatograpbabtc taatenaia are to be identified. Tba approach caa only be applied to GC/MS analyses, siaca tba aarrogales caa be diAcreatialed from the native coapoaads froat their ddtereat aaaa tpoctra. Since it is aot baowa before taaplr extraction aad earact saslyeis what aaalytas may be present. sarrogates aatt be cboaaa that could aot poaably be preaeat ia the taapis. la adtfilioa. tiace oaly iqwd/liqutd or liqaid/tolid exlraclioa woald be iavolvcil. with ao ckaa-ep (siaca dcaa-ap would reatote taatpoaads at which the requester la iatarested) say hydrophobic daetaratad coatpound caald tone aa a tarrogala. Normally, phcnoi-dS, T T1 pltamil ill. CU-bcaaeac-dn, pyreae-dlO aad chrysene-dtf are ased aa Sarrogata Standards (or the aaalyaa of a wide satiety of hydrophobia materials ia teviroaaitalil samples. A tab tat of this aeeoad type of Sarrogata Standards are the aarrogatae which are aecd iw the capihary GC/EC aaalyaia ef Areder (onaalatiana. Siaca maaa ipeewoaiciric detection ia aot aaad, antigens which roaleia unique iaotopca reseat be dwtiagaiehed froat their native rmmurparta. Therefore, other caatpoaada are seed as Sarrogata Standards tinea they have been observed to act exactly aa the polycMorfaatod biphenyls (TCBa) ia the Arador fonaalallcaa Aay balopaatrd rnia|inead caa be aaad which acta exactly aa PCBs ia the earactioa aad deaa-ep step. ESC aonaaBy aaaa CLS-baaaeaa aad 2,dd-CL3-biphsayi far tbia propose. bgfal_Aiabttl - Termiaoiagy which tefereacas the analytes of iatercil which contain nataradyoccecriag iaotopaa of carbon, hydrogen, balopaa. etc UghtSgfa Terminology which references the addition of a knows aaaonat of native aadyin to Ida itanpli srafruL Normady, at least oaa aatapia eel be apibad with the aalive aaaiyta at tba repotted Isvci of drtattiaa (law native apike) aad at 10 thaea the lend of detection (high native ipdtc). Recoveries of the native aaaiytea provide Anther doenmratation oa tba quality of the aatdyaas tpibra is 10% of tba JlgyUblb Tcrntiaoiogy which refers to a sample which ia known to contain none of the anoiytea of iawraal, Ear weaar analysts, this ia normady Burdfek and isckaoa Brand Water, da-waned, or dWBednmar. Ear end. it map be soil which baa bean previously aaalyaa d aad known to contain aaaa of the analytes at iataiaal Ad erection nape, eaiag randomly teheted glaatwate. toKenta. tad ad eorregate apddag tohniona araat be aaad. This provides doewuentslain that the aaaiytea of interest warn not ianAmtsatly present ia extraction glassware aad toimala aaad ia the analysis. A aaahatna of oaa method Mask maat be generated with each tel of templet. For temple sett roatamiag amts than 10 itaaplei. awlbod Maakt act generated at a frequency of 10% of the number of tampica. Jbggggjllglgl Terminology eaed to indicate tbs duplicate extraction and daplirali extract aaaiyia of a sample. Tbit provides documentation oa the precision of aa aaalyaia. Normally the precision of inihomncnial analysra of homogcneons temples ia oa the order of 30%. A minimum of oaa duplicate analysis ia required tor each temple set. For sample sets roaiammg more than 10 samples, duplicate aaalyata are generated at a frequency of 10% of the number of tarnplea. HONS 025030 Page 4, Analyte Extraction Terminology (corn'd) Farther lafonsiatloa The geaeral area of Aaalyta Eztradioe, aloag W*h mock of the termiaology described abost, ia wy complex The foduwmg rcfereaces may prooide further infomatioa which may he aefol ia aadsrataadlag caractios faadaairalala sad terauaology. O CTK fart 13d aatitled "Goidehaes Estabfahiag Test Procedures for the Analysis of Pirlhtaaii Uader the Clcae Water Acs; Fiaai Rale aad lateriai Piaal Rale aad Proposed Rule'. This docauieat iadades details of EPA'i 600-series analysis asethods. A carreat copy of these aicthoda caa be fouad as the October Mb Mt4 Federal Register. r--RsataaMat af Weak hr a | |ghm|gn Praaram which is used ia conjuactioa with EPA's Sepcrfead Site studhe. A carreat copy saay be nhstjar H by contacting: Joaa P. PUt, Preyed Officer Aaalyrieal Support Rraach Hazardous Response Sapport Division USEPA WiiH.plos. D. C 20W0 HONS 025031 Instrumental Analysis Terminolojy This icctioa describes commonly used (erminoiopy sad phrases which are ased ia coajaaoiaa nhh ndrect analyse. This ialioraMlioa say be helpful ia aaderalaadHig soaM details of how awrasMatal analyses at temple eternal were performed. The previous lection ot this report describes lerwasoiopy aaaorielrd with analyte mrarrioa obninrd ha soma type at sample ehnetiea step. Detailed iaforaulioe oa how this earaet a prepared can be foead la the Standard Emaction Methods aad (low sheets saaaciatrd whh the aadads 3awssarias at these aasthoda which were seed lor this project caa be (oaad ia a separata icctioa of this report. JMBML&MdMlilS) Tarmiaelopy aacd to reference a roatpoaed which is added to the --y*t ahract aad asadard aohaioaa ad the saslytra af iatereat anmrdinlely before iastnaaratal analyse The parpnaa ad the iataraal alaadard ia to pcaaida data which caa be aaed to correct for virilism ia iajsaaod rehears ot eatract aad slaadard tahstiaas which stay occac dacitu iaatraaicatal aaalyaia. Tbs haaraal ataadard am act bs preacat ia the taatpla earaet Typical iatcraal ataadards aaed ia aaa ipaetraamric saaiysai ara blames d>, naphthalene ill, aathraccae-dlO aad chryaeac-dU. Thasa daatataled tompoinds pradara aaiipta auaa spectra aad ara aet present ia aatamlly eecarrlag apha. A camaaaaly aaed hdcraal standard for GC/EC atulysia is hcaachlorobeaaeac. I a aMthod of data analyse. This esthod reprices that a inane aanaat of aa haaraal asadard be added to the taatpla carnet prior to iaananratal analyse Responses of ad analytes are calcalatcd relative to the iatcraal asadard using the feflcnriag tahdsaahipt RR Relative Response - (Analyte Area)/(leraal Standard Area) reflected by dMftttarei ia the adaraal asadard areas, la addhioa, if iasirntacat scas*wily chaappa, relative respoaaa corrects for these types of Ihsctaatinn la order to daUrnriao the analyte concealration-Relative Retpenac relatinmliip. analyte Raiativa Response Facaoti ata catenated aalap the foMowiap relatinaahlp for data obtained troin the saalyale of rrP . (Iatcraal Standard (Analyte Area) Concentration) Raapsaaa Rcspoaae ------------------------------------------------------- Paccar (Internal Standard (Analyte Area) Concentration) HONS 025032 nt Pag* 2, InstrumentalAnalysis Terminology (corn'd) When identical amounts of ike internal standard arc added to both extracts aed standard solutions, internal standard coarnairatioa term ia the bore equation can be eliminated. Wken thm is dene Relative Response is sabstitnted for tbe ratio of analyte area to internal standard area, the * equation becomes: RRF RR/(Aaalyte Conceatralioa) Analyte concentrations ia the extracts are calculated from the following equation: Analyte Extract Concentration - RR/RRF la order to obtain the concentration of the analyte in tbe sample, the blowing equation is used: Analyte Sample Conceatralioa (Analyte Extract Concentration ) (Extract Volume) ----------------------------------------------(Aasonat of Sample Extracted) The area terms in the above equations may be total ion areas, FID peak areas, EC peak ana, or enraeted ion areas. The details of bow dm internal standard quantitation method ia applied to specific methods are dearribsd in the xenons instrumental Standard Analysis Methods. The fplowing equation shows what catcdalioae should be made to correct lor analytical bias: Analyte Sample Concentration (CorrncSed lor Analytical Mas) (Analyte Sample Conceatralioa) ----------------------------------------(A named Analyte Recovery) The Aaaaaeed Analyte Recovery can be obtained bom an average of surrogate recoveries or native ImUlHiglAHlIMhlikM Tcmiaolofy which refers to a method of data analysis. This method requires that a known amount of the analyte standard be analysed under the tame tondhlens an the auaapln extract, la cedar to dstorariun the analyte couceaumioa analyte niptime reletiouehip. R eipouaa Factor! are obteiued from the Mowing relationship: RF - Response Factor - (Analyte Area)/(Analyte Concentration) Analyte concentrations in the carnets are calculated from the following equation: Analyte Bdract Concentration (Analyte Arca)/RF HONS 025033 Page 3, Instrumental Analysis Terminology (corn'd) b order to abate the coactauatioo of the tnalyte ia ibe temple, ike foOowteg eqeeiioa a wed: Analyte Sapk Coaoeelredoa (Analyte Eared Concentration) (Edna Volume) ---------------------------------------------(Amount of Seapic Earaocd) Tke one term ia ike ebon tqaMteaa may be total ioa area, FID peak aw, EC peak treat, or tweeted tea ante. Tke driailr of how Ike carnal madard quantitation method ia applied to ipcdlic metkodt an dcacribed ia Ike nrteaa teatnaaeatal Staadnd Analytic Mctkode. The Moaiag equation akoaa what calcalalteaa tkoeld be ande lo coma for analytical bin; (Analyte Sample Coaceatraltea) Analyte Sample Coaetmraltea ---------------------------------------------------------- (Corrected for Analytical Bice) (Anamed Analyte Rccmry) Tke Aaaaaed Analyte Recently caa ba obateed bom an enrage of tunoqale lecomlta or emtee jlMdKl^Mfeak-kklfeldi - Tinaiastep end lo nferean aa orpaned deacripltea of Ike Hope iaaotndte dm tawmaeatal aanlyaie of a lempla or a temple Cdred. Theta airikote an nrigaad ikoit aaane which tea ateobe Bead m lompami be aaatee ter them atdkoda. The amacaef pecifie iadrmaranl Sltadard Aealytie Mnhodt alack an eaed ia ikit Body an kited ia Ike (iaal lepott ia Ike natea aadded Detafc\ Ia eddkloa, coptee of them Standard Analytic Metkodt an tkoaa ia a mparale tedtea of ikia report. Ftewiheeta of tke Slaadard Aaalytia Metkodt an ataady ateo prowled a graphic descriplioo of a Slaadard Hatknd Tfcie Rear teeaf pina tprrillr iafonaetioa am bow attracts sad ifdsnfc arc aaatyied lil types of dtta rcdactioa methods arc ini Farther lalbfttM provide Mar oldch my be ascAd ia cadcrstaadiap imtnaacatai aaalytis I HONS 025034