Document emmXwna495qoNKzxqZpegzVg9

Ir Monsanto MONSANTO COMPANY/ DAYTON LABORATORY / DAYTON, OHIO 6407 :! _ MDA-534___________ (Depertoent/ieetion) MS3^>5 REPORT NO. i KDA-S34 JOB/PROJECT NO.I 4B4.22iO _ ESC/DAVTOM (Type of Report) pDECEIVED j SEP 4 l&M DATE: 30 August 1964 PERIOD COVERED! ftMW It' rr. lows TITLE: ANALYSIS OF HUD AP'D WATER FOR AROCLOf.S AUTHORS: B. H. Hughes' ABSTRACT: Kud and water sar.ples fror the Trenton Riant were analyzed (or possible concentrations of Aroclor forrulations. The results of these analyses are shown in this report. 3 m rs ii H TECHNICAL APPROVAL: APPROVED BY: .'i&JL ________ Brooks Senior Research Group Leader gJ'-Ur,- ............ . R. P. Ivory Environraentel Sciences Center Service Project Mensger APPROVAL DATE: /- -ti RSSTRJCTED DISTRIBUTION! (see over) COMPANY CONFIDENTIAL tkis IsomU is Us prepsrty sf Meoesste Ceepeny eoi Ike siest is reigeoelkle fer its eefeketping sol iiepesltieo: SMPOSMSTIOM Rlck suet set Re rises pereeoe er lent sstsiSe estherisetlen. HONS 023105 oicT R .) T I O \ COPYMUMBCA 1. M. Barry mo 1. B. M. Nughos 1250 3. B. r. Ivory 12S0 4. Central Piles 1250 5. Technical Reports Lbry. R2C ABSTRACT ONLY H. A. Wolteraann NOTEi Distribution of thil report it restricted. Requests for additional copiaa should ba tada throughtha principal contact at tha Monsanto location involved or the Manager, Environmental Sciences Canter, Payton Laboratory. Dayton. Ohio. ACKNOWLEDGEMENT Contributions of tha following Payton Laboratory peraonnel to this project are gratefully acknowledged! Analystfi B. K. Hughes C. Trang haam> COM PAW CONFIDENTIAL HONS 023106 ANALYSIS AtPOST 100 HlPtfEC: i-C4-oe-le-oi 10: Tr ertc- DATE: August 29. 1984 psojcct no: e4.2?eie environmental Sc'encfi Center Monsanto Cont*any/De>-:on laboratory (5(5 N'c'oias &oac Oaytori. Onio 4$<;G Pnone No: (5(3) *6?-3<l! title: Analysis of Aroclor fornulatlorn In hud and Hater Sam-let Sta-oa-o Sam ms r*:noc Holt): Samples supp'ied Cy customer. Stand*-5 Est'actior Ket'-od Nolt): USEC5 Stand*-c Ana'>s:s net nee Noltl: ECANC2 fine' Retc-t rile hois): A228I8 la: 'e f"t hols!: B226ie.C228l8.D226l8. 122618 tablet I tr-roug- 4 Sknma'lze Aroclor analysis results for aud and water tarn-let 'rr tne Trenton Plant. Pleate note that the concentration of Aroclor I2S4 detected In the water tam-le. shown In facie I. Is **> near |t level of detection. Therefore these concentrations aay oe In error by a factor of two or three. Alto Table I shows appro*IhateY 1591 recovery for the Cll-blphenyl surrogate. This My be due to the pretence of this compound In the uater sample. However this recove-y would corres pond to an absolute concentration of approximately 0.0S ug/g wr.lch Is well below the St ug/g concentration which defines a hater la! as "PCB-Containing". The high recovery of 1881 for the Aroclor I2$4 low spite Is due to the presence of Aroclor I2S4 in the aanple. analyst(Sti A. n*son Hughes and cry Trang analyst appaoyali jk- 1 HONS 023107 1llt l, Result* of Capillary CC/tC Analyst* of Arocior foraulatlon* ' In Tranion Vat*r aenpte (K ProJack Mot 494.22919 Oat at August 29.1994 sahpu lOCNTiricarioN Site 2 Pond water Thomvllle ftd. Site ? Pood water Thomvllle Rd. Oupiicete "etT^d Bier* *s*.t*t esc AHl1ICl minoo 100 rc;IO' l?S4 Vlwtt He of Velvet Stc OavUHort 1 *et Sto Oe* CCAN02 * 0.01 - - - - .014 .00 14 .90S 39 COnCEntrat:cn tjg/9' .01? .09 14 .005 42 *C - - Su#W*U SPIMKO COn-OCSC *nous' *0010 IxO/e: CvS-t>*nsas* ft.l-t'pna'r! ccano; t.oi * 0.02 39 250 MCOVldr ID 30 2S3 is 39 OOCU"s3*3!On ISC Irtractlor nathoo Sant'a Ant extracted <o> (Btract final volim lal) (at'OCt Dilution (X (.tract NO. Protest me Nan* MSCxOS 10 1.0 1:1 PC8643 9P773 wsexos 10 1.0 III PCB644 0P774 NSEX9S 10 ! .0 111 PC6647 OR??? upiwtion or taextvuTiONSi tOO llolt of OateclIon In us/B O non* detected Kith a detection Halt Riven by tna LOO valua na a net analytao no of Valua* Total range of *roclor foroulatlon concentration* ataturtd frea Individual PC* Itoaer*. The iwtoer of Itoaar* utad in thl* calculation I* Riven by no. of valuat No of value* Umber Of PCI l*oaer* u*ed to aeature Arocior concentrat lor 1 Hal ltd Oca [CStd Oavlatlonl/IConcentratlonl) * 1901. TWU fill NOi KMItiltl 3 MOWS 023108 1ABIE 2. Result* or Capillary GC/EC Analyses of Aroclor foroolotloos In Trenton Hater sample (K Project No 484.22818 Oate: August 28.1964 M*lt IKNTiriCATION site 2 Pond uater Thornvllle Pd . lov spike Site 2 Pond voter Tnornvllle RO. High spike AKt.tu esc ANALYTICAL hOmoO 100 CONCENTRATION (ug/g) Arcticr 1254 *r.j c values o of va'ues Stc Deviation t Pel Std Dev ECANC2 - - - 0.01 - - .018 .09 19 .001 36 .05 .0? 21 .02 3! S'JP?;'E S:K!kG co^pojv: anoun* AOOCD Iu0/l ClS-Den*en* Cll-V'or.fn/' ECAN02 " 0.0! c.c* NAt<f tolklng ttudy A-OClOr 1254 . o:..oe 5* 215 IS8 RECOVER (1) ti 263 18 DOCUMENTATION E5C Extraction Method Sanp'e ant extracted is* (tract final teliae <M (tract Dilution ESC Extract No. Process flit Naae VSCXQ5 10 1.8 III PC8845 8PT75 M5EK05 to 1.0 in PC8S46 BPTIt EXPLANATION Of AMNCVIATIONSl 100 Halt of detection In ug/g NO none detected lth a detection Halt given by the LOO value HA not analyzed no of value* Total rmoe of Aroclor forawlotlon concmtrMloni aeesured fraa Individual PCS Iscaers. The iwtei of Iscaers used In this calculation Is given by No. of Values No of Valve* * N*tr of pee Isoaers used to aeasure Aroclor concentration 1 Pel std Dev tistd Devlatlonl/IConcentratlonl] X 1001. TAKE flit HO. C226I8.HM 3 MONS 023109 TASLC }. Results Of CuHlirir GC/EC Analyses of Aroclor formulations In Trenton Hud sample CSC Project Hoi Hl.mit Oetei August tt.IttA SAhPU INNTIflCAUON ASA,,T( CSC ANALYTICAL KTHOf to: Site 2 Pond awd Tho'rwtlle Rd. to. spike Site 2 Pond mud Thorrwl1ftd. High %u\Kt COnCCnTNaTIOn (ug/gl Arcelor US* Png of Values me o' values Stc Oevlat lor. S Pe1 Sto Dev CCANOC - 0.1 * ' .IS .90 1) OS 31 .99 S9 V .13 13 SURROGATE STKING CONPOUS? a*Ojnt ADOCD lug/g) ClS-oenzene tlJ-Olpr<rr' CCANOC * 1.0 2.0 kat've solving study Aroclor use . io..ar 10! 103 Mfc RCCOv'Rr id 103 107 129 DOC~tOATIO CSC (.traction method Samp** Am* etracted ig) Cvtract final volure (ml) (tract Dilution (SC (tract Ho. Process rile Name WSCXOS 1.0 10 III PCD6S0 BP781 orExplanation mKvIationSi 100 Molt of detection in ug/g MSCX0S 1.0 10 1i1 PCBtSI BP702 M9 none detected ulth - detection Molt given by the 100 vslue HA not analyzed Hng of Valuai total range of Aroclor fornolet Ion concentration* Matured fro* Individual PCI Isomers. The nimbor of Isomers used In this calculation l given by Ho. of Values Ho Of Values Nmber of PCS Isomers used to measure Aroclor concentration I Pel Std Dev tIStd OevlatIon)/(Concentration)] X 100s. TAdtE flit NOi D2ia<NH A HONS 023110 TABLE 4. Results Of Capillary GC/EC Analyses of Aroc lor fornula: Ions In Tranton Dud sanp|t CSC RroJfCt Ho: 464.{{BID Datei August {8.1*64 SAIAE lOCNtlflCATION AMuiTi Aroclor l{S4 >* Y'vfl ho o* values Stc Peviatio* 1 Re! Sts lev HZ H'OC tcun: - ft* l fond oud ThornvIII * Rd. Sit* { Pond ud Thornvllle Rd. DuelIcat* Method Blank too 0.1 NO -- -*- CONCENTRATION lug/gl no n: .- ,, . -,, -. *** C: l-b*r.r*n* tO-t'R'e-.' *?oys' AOZ-iO IwS-'.J ECAvCi * 1.0 2.0 BOC ,,!*?AT l> 104 IDS RCCOvERr 111 102 107 10! 10* ISC !faction Hethcs Sanc'e at: e.tractec igl (fact final voluvc in') (fact Dilution (SC (.tract No. Rrocesi m* Have HSCX0S 1.0 10 m PCB446 BPTT* (XP.ANATIC* Of ABBRCVIATIONSl lOP llolt of dtttctlen In ug/g HSCXOS 1.0 10 III PCBC49 BPT80 VSEXOS 1.0 10 1:1 PC6CS2 SPT8) NO none Otttetad ulth a detection Halt glean by the LOO value NA not ana'ned Rng of Values Total range of Aroclor foraulatIon concentrations easured fro* Individual PCS. Isoacrs. The nater of Isoaers used In tMs calculation Is given by Mo. of Values No of Values Nuafcer of PCB Isoncrs used to Measure Aroc lor concent rat lor. t Bel $td Dev * ((Std Oevlatlon)/(Concentratlon)J x I00S. TABU fill MOt tmiBiHH V HONS 023111 DCTAIKD CWVAHUTION (J TASKS In an effort to itrunllw report* tmrttM by ISC on PCSi present In a vide iM*ly of Mlt'ltlt, using aide Witty of techniques. Standard (traction methods tStn) and Standard Analysis Hethodt (SAAsI have Scan developed which can be easily Interfaced with each ether. An abbreviated fora of tncsr SCHs and Saks have been stored on the Hewlett-Packard MST-ias laboratory automation systen. used by CSC. In a effort to commnlcete these details with customers of (SC. this Information It supplied with each PCS analysis. However, auny projects Involve a very tael I nurber of samples wMc- not necessarily the same matr I *. Therefore, major Information 0' the technical details of an analysis are presented In tabula' fo'a witnlr the same table wh.cn reports the data. (acn tacit includes a general title. (SC Project Number and Date on which the teb'e was generated. The sample Identification is tne customer Identification which was on the sample bottle. The next section of tne tat.ie gives results for the particular analyte listed, for Arocior formu lations. the formulation is Identified either visually or from (SC developed data analysis programs. Tne concentration of the forauiation Is calculated as tne average value of tne Arocio' fonmjlatIon, based upon the analysis o' a njsber of Indivld-a' PCD isomers In the formulation. Tne ramper o' Isomers used In tnls ca'cuUt ion Is given as "No. of Values* and the range of Aroc'c concentratIons fo- tnls mnber of PCD isomers Is given by *Ang 0* va'ues*. Tne s'.anda'd deviation ond t relotIve standa'o oevlation fo- this raysber of determinations of tne Arocior formulallor e-t given In the following two lines Of the tebles. Tne newt section of the toble deals with duality control used In tact lyr e analysis. The surrogate spiking compotvy) which Is added to the sample before extraction and ana'ysls is listed, along with Its amcnyit and l Recovery measured for each sample. In cases where PCR concentratlens are very nlgr and thus require extract dilution, no effort Is made to quantify this com pound. Tnls could be done If (SC knows that these deta ore Important. Put typically SO ug/g Is tire Important level to quantify accurately so t'at Surrogate data for concentrations larger than this value, from a regjiato-y stancpoir.t. are not Important. Trie neat section documents how each sample was extracted and analysed. Tr<e (SC (xtractlen Method, amount of sample extracted, extract final voitm. extract dilution factor. (SC extract ramber and the computer dete file In which the processed deta is stored e'c given in this section. The last section gives o brief description of abbreviations or gives any footnotes that give additional Information about specific samples. This table format Is both compact and precise, it was developed in an ettsapt to quickly and accurately generate data rfilch the customer can quickly eras accurately evaluate. If there arc any suggestions concerning this format, pltase contact me at extension !N. DCSCRIPT ION STORCO IN TDCXOKItl * HONS 023112 The following page! describe Standard extraction Method! and Standard enalyrl! Method! vied for thli project. HONS 023113 7 (SC Standard Extraction Method (SEN) IIUEi Wide aeon extraction aetnod for valor matrltxl.tces). HATAI<X),lCCS)t valor ISC Standard extraction Nethod No: MSEKOS TYPICAL SAMPLE sin is) TYPICAL (X1MCT volume (ml) 10.0 at -4 i io ml- 400 *L Typical ANALYTES: Aroclora, PCBi. priority pollutant* CSC Standard Analysis Notnod no*: IxTER'CRENClS: var lout: See Individual Interference* for Individual analyte*. TYPICAL SURROGATES TYPICAL RECOVERIES (1) duetprated surrogate* for Individual analyte* pentachlorefcenzene 2,4,t-tr IcMoro- blphenyl S0-I20 SO-120 SO-120 APPARATUS AND MATERIALS: Burdick and Jac*ton aetnylene cMorlde SSoedplaurrattourylfafutennfeolr* extract drying. Soolu* hydroxide and sulfuric acid for pH adjustment*. Nitrogen for extract voluxe reduction. Mater oath for K-D extract voliaxe reduction Lln|TATlON$i Sufficient sample amount to provide GC-RS LOO. Satcty PRCCAtfTionsi See Safe laboratory Practice*. SATIS or ICTMOO CKat ion mo UPDATES: S/IS/B4 HONS 0i31J4 now $cn wsrsos FOR ISC EXTRACTION KTHOO WSEX05 SAHPLC ID: INK EXTRACT f LOO N0> EXTRACTION DATE And Tilt: ........................................................... /...................................... . RECORD NATIVE pH...................... NAS pH ADJSTEO VES/NO IF VES TO NHAT pH PLACE SAMPLE INTO AN || APPROPRIATElT SIZED . SEPERATORT FUNNEL . 11H HEAP SPACE SUGGESTED . FOR ADEQUATE NIXING) .() SAMPLE KLUE............. SURROGATE SPIKE IF pH ADJUSTED I > ADJUST HltH.SOS NsOh OR H SO !a ad; methylene chloride in The appropriate ANO'JNT ii . ii i SAPP*! id ml solvent, . 100 ML SAMPiE IS t SOLVENT) . . . SHAKE SAMPLE ONE time AND VENT Through STOPCOCK () . REPEAT DOUOl ING Tit NUMBER . OF SHAKES BETWEEN VENTING . samples until the NUMBER OF . SHAKES EXCEEO BO RECORD AMOUNT METHYLENE CHLORIDE ADDED rOR EACH EXTRACTION : I)..................... : \:/ Z)..................... V ))............. OBSERVATIONS allow phases to separate i) REPEAT EXTRACTION PROCEDURE TWO MORE TIMES dry extract with t inch sooium sulfate column (COLUMN PRCRINSEO WITH SO ML ICTHYUnE CHLORIDE) t )(] .. [ ) EXTRACT DRYING NOT REQUIRED RINSE SOOIUM SULFATE COLUMN WITH Z X SO RC I) . REOUCE EXTRACT HUM TO I At RY K-O TEOBIIM M OR NITROGEN SOLVENT VOLUME REDUCTION I J. ( ) TRANSFER EXTRACT INTO UIAL FOR ANALYSIS EXTRACT NO: -..................------------- DATESTIIC COWlETED--........... .......... / .................................................................... ESC JOB NO.................................................... . HONS 023115 (SC Standard Analysis netted eSAn) tllltl Aroclor (orawlatlent In Solvents (SC standard Analysis netted no: (CAN? analytical instruncnt and NOOC or operation: np-SBBO Capillary a/tc Inter faced to an HP-JJST-lAS laboratory Data Systea typical ana.tU typical INST<Mn*T LCVCL V KTCCTION (too: (ug/al) A'OC'or forte'a*. Ions ::iz. itti. tin. i:se. izto. a- i:' o.i typical PRtCISION ( I Ox IOC 111 so TyPICAI accural, I0K lOD 111 i- IhYCPftsr\C!l lIn;?ATIONS: a-t electron capturing species In tr-e rete-- tion tlee reg'on o' trIchlorob'pnenyl through octachlorob'pnen> Iscoers * pete-tle' Interferences. (act retention tlaes of oost llke'y OC# Isoaers tan oc Obtalnec froa the analysis of Aroclor I(40. Aroclor IZS4 o- Aroclpr mo for tel at lont. CwROHATOSRAPn'C COLUNN: JO-aeter fused silica JAN 00-S <0.?S uN| 't. :oe 00-f (O.lZnn.). COilNIX TCNR(RATiW PROGRan: 110(11/4/300 INJCCTION TPC: Split lest igat'iosCA. and Standardization: Use Internal standard quantitation technique ang ca''prate Instrimnt response factors froa aut'ientlc Aroclor fortelatIon standards. Use a ainlv of 10 PCB Isoaers for the determination of fo-te- lation identity ana quantity. CALCULATIONS: fortelat Ion concentration (Itcaer areel/Osoaer RRf) where: RRf Is the relative response factor for the appropriate PCS I soarr In a given fortelatIon. Fortelatlon concentra tion is obtained froa the average of at least 10 such cal culations. SAfITT PRCCAUTIONS: See PCB handling protocols In laboratory safety aanual. DATCS or HCtHOO CRtAT ion AND MCTHOD UPOATtSi IB/ZS/83. Z/l/04 10 MONS 023116 Ihc foliating pages describe Analytical Request Intonation generated for this project. U HONS 023117 MONSANTO COHPANY/DAYTON LABORATORY1 fNVIRONNCKTAL SC Itiers CUlYtR ANALYSIS RCQUISI OATEi AUGUST |(. 1*04 RtQUCSYCA: TREnTOn/IVORy LOG NO: I-S4-OB-IS-OI PROJECT NO: 4B4.22BI8 At RORY RESULTS TO: r lltS/NECS.BROCKS. IVORY ANALYSIS RIOOCSYS SET TO: t ILCS.MUGHtS. IVORY. BAOEXS SANPlC PICKUP BY: MCKCN2IE SAW>ll LOCATION: LAB Jl Samp.E OCSCRIRYION YOR ? SAMPLES SAMPLE IKMiriCATION NUMBER or BOTYiES esc NUM8CRIS) SIYC I - Ron: hoc TmORnvIuE RO siyc : - pos: wa*a y.ov/:lle re I PCBC4B RCB*4(0LP.ItAYj BCBSSOIl. SRIKCl RCWSIIH. SPIKE I RCBCS2I*. Blast:! I RCCOROCC 8y:R. RC6C4J RCB*44!0uRLlCA-Ci RCBS4SII. SPIKE) PCBS4SIM. SRIKCl RCBS4Y(h. Blaa>.> IVORy RCOVIRCD ANALYSES: RCB ANALYTICAL HChNIQUCSi TECHNIQUE OAYC COMPUTES X GC/tC I IB) S/2B/S4 OUALIYATIVtl StHIQUANTITATIVt: QUANT I TAT I vt f RCQUlRtO QA/QCt COMRUYION DATE BCQUlSTtOt YVO MtfKS THOM RCCEIY OT SAMPvtS. concurs! SAMPLE BISPOSITIONi X NOLO TOR IB DAYS SATCTY PRECAUTIONS: ANALYSIS DCOUST TILE NAME: AABCOBill 42 HONS 023118 Ih* following It copy of the CSC/UAG Good loborotory Practice* Ninual. 13 HONS 023119 Copy Sunken cooo lakmatoct nuciicis kakvai > hUi to liillli Cootral/Oualltr tugmm tlltrltIKt Analyst* Ctnp Notch ! Vnl J. rW> Croup UWit, Vltratraca Analyst* R. A. Kaltanann Nan*(*i, Imliwtu) Seine** Caul laiueA lai taut ____ JS1/J0S A brlr**MM*l Seine** Cnt*> bltw Sohoratary Roytoo, *klo AS40J u HONS 023120 uni of oontxis I Okjactlvaa 11 Seays HI talyili A. Hsthola >. QA/QC fro|ra 1. Iflt htpmilM QA/QC a. Hatkol Blanks k. Beylleatas c. Sylkea 2. laairiaania) Analysis QA/QC a. lasttanentatIon k. lianaa c. Quantitation Internal Standard 0. Standards C. tXfiaaa of Quantitation 1. Qualitative Analysis a. Tentative k. Ctaflntl 2. Seal-Quantitative Analysis 2. Quantitative Analysis 1. Quality Criteria aa4 Banalla1 Action 1. Quality Crltatla a. Blanfca k. Bacavatiaa . Btatlalns 0. Unit af Detection a. Accutacy 2. BanaOlal Action IV Data V Saayle Disyoeal nomas Haste I taanyla of QC/NS U|teM ya|a 1 Bumpiest QC/DC lailaal yna 1 Bnnayla al Bloc/Taya laokaak dad* IS I tSIf 1 A II HONS 023121 I. CM retiree TM mIb kjidlvti of the mtrotvteo ImI/iIi Crony quality iHiiriBct/^litj (H(r) fr|rM ov: 1) ? that mi lobovotofj |mrtM btyh %Mltty imbIii; end 2) to Mlntofo tM Mcmirjr tocorto tMt 4ocof>t laboratory yarforoaoca. 11. coyt TM o<oy of tM ainvil Includai oraaa of Cl? oot oyoclflcally addraaaad In tM ISC atetion mbvbI and axyanda vyoa cartaln araaa vhara QA/QC practical dilftr ftoo tfcoit daacrlbcd In tha taction oanual. It la ftnttndad to M Md a lent with the acctlon oanual to yrovlda a cooylatt ylctura of the CL? vlikln tM Vltvatraca Anilyali Crony. in.? The feneration ( analytical reavlte within tha Dltretrece Analyaia Crovp tovtinaly lavalvaa two practical: aa.pla preparation end l.atomnul analyaia. lacplt preparation Involvaa ana ar note af a variety af technique! Including a.tiactlon, ailvtlon, ecld/kaee vaehee, celuan chronetotrephy. caacantratlan and nunerour atkar technique* ta render tka aaapla la a aultekle condition for Inatrmcniel analyaia. Initrvnental analyaia takaa tka anltakly yrayarad aaapla and Intaadvca. It Inta an analytical iaatraaant ta aaaavta tka dtalrtd paraneter(a). loth af tkaaa practical can ka daacrlkad ky claatly daflaad and aeparakla net boda called aaapla ptepaietlon natbada (IFMa) and laatrmentel analyaia aathada (lAfla). (PMa and Un nay ka ceablaad la rnaama way. (dapandlni apan tka aatvta af tka aaaplaa and tka aaada af tha caataaai) ta pradwea a awacataful analytical pratacal. Fat aaaapla, aavaral different IPMa ay ka tried ta preduct aaeplee tkat are evitable fat aaalyala ky a alagla 1AM. Tka *taeutaa Incarporatad lata aack af tkaaa axpetiaeatal pracaaeaa ta anaura that an aaataaatnt af tka quality af tka raaulta can ka vide ceaatltuta tka QA/QC pretraa far a prejact. Tha fellevlai eukeectieat daacrlka the alaaanta af tka analyaia procaaa: A. Matkada Metheda an tha writtan deemantatloa chat daacrlka tha analytical pracaaa. They cmtala aufficlaat detail auck tkat a cany ateat ecleatlac ar technlclaa cm readily parfarn the required aaalyeea. Tha ueual practice la ta have aathada that daacrlka the ample praparatlm pracaaa (fMa) and nethede that daacrlka tka luetrvantal analyaia pracaaa (UHa). tack necked daralapad within tka Vltretrace Analyaia Crmpa la aaaltnad a nethod nunkar aa daacrlkad In tka Etc tactlea Manual. Matkada are aktalaed frm variant eeurcet lacludlnp la-kauaa deviloyant, codification/adaptation af literature nathada> at epectfic pratacal mthada dictated ky powermint agential. Matkada nay ka larvally validated bp a aarlaa af arparinanta that daacrlka a claaefcal valtdatlan pratacal ar nap be laaa vltaravalp praam avfaQ ta facteta auck aa frequency at uaa, cnatanar aaada and 1C MONS 023122 coat/ctaiat rutrlctlHi. In aoy cjii a QA/QC p|na la ar^)M la tka antlyait pkmi la ptnvlCa a Mama af tka af tlx tanlta. Wwt a QA/QC prigm la pamlM ky a taialtaC ptotacol (e.|., DA Malta la toll pratocal), canal* ainiau* QA/QC Maniac (CtpanCtai upon Ika analytic typo) > intotpotatnC lato all Vltiatiaea Analytic projacta. Tka lollovlat nkaactln Caaciikaa tka Plttattact QA/QC piopm: QA/QC ll|laa la affective QA/QC pta|tn Incorporate! aiperlncnta that provlte lafaiBillon illative to aack of the follovlai met lone: (1) Arc tkcri any tapvricleo. kackgtnunC or cootaalnatlon that vlll iafluiaca tka itaultt? (1) Rov teproCudkle an tka reaulta? ()) How nil can tka enelyta ka recovered fro* tka tuple Mtllll (A) Wkat la tka Halt of Cetectloo for tka analytic? (1) Wkat la tka Cynanlc 1*0|C of tka analytic? (1) Wkat la tka accuracy of tka analyala? All of tkaat mctlool aia aCCraaieC ky properly aalactln|/ayylylnl tka ace of klaakt, rayllcotaa, aylkaa ail atanlaila in a QA/QC progran. tka Ciacuaaleo of tka uaa af tkaaa QA/QC tacknlQuet aa they apply to Oltiattaca Analyala Cioup cctlvltlaa la kaat tone ky cnaMailai tka aaapla piaparatin a*C iaatrokental analyala piacaaaaa eipecettly. 1. tanpla fraparetlon QA/QC a. Httkod klanka - kepreaentetlve glaaevate, aolvanta an4 taatnta arc cad trttk aaapla nattlcaa Mick aia alallat ta tkoac fat uklck raaalta aia kal*t reported, yat to not cntaln tka analytic af lntaiaat. Hetkod klanka aia analyte/ at a fiapuancy anal to 1H af tka analytic aanplaa foi aaapla aata Mick an nltlplaa af 10. At laaat ana MtkoC klnak la analytaC fat aaapla aata cntalnlnc katwan 1 aaC I aanplaa. k. Replicant - If aofflctaal aanpla aaounta kavc kata nukaltteC fai analyala, rapllcata ftapaancy la tka aaaa aa tka MtkaC klaak fraQueacy. If at all pMitkla, lapllcataa akanlC ka aktalaaC fin tka aaaa anpla kattla In aiCac ta atnlnlaa aaapla lakoaogaaelty pnklan Cm to anplai kalat takan at allpktly Clffamt tinea. 1 r a. (plkaa If aafffclaat aaapla la avaflakla for aack aanpla type, tka aaapla la apllt aaC aplkaC at too lavala trttk 17 HONS 023123 the native (n)iM(i) TIM Imh are inlullj h (lw) and lOx (tliD'lk) HlklHIli tilKtln Halt and nrn u a technique ( oeti- netlng Ik* Halt al Imttln far each wattle. Thete law aM high eplkea art conducted at a frequency equal to tkt Method blank Ititwetir. Obvloualy a|ltl>| with tkt aatlwa analyte cannot kt tone for vtdeecea analytic alntc tkla preeuppoeee knowledge of tkt Hoot it; of the analyte(a) In tkt aanple. Other oplkln| techniquee art weed to ovalwatt tht extrac* tlon/recovery cfflcltnclta for tkt analyta(a) of lnttttat. Htally extraction/recovery tffIcitncltt art deccralned for tach aanple, alnct. In principle, oack people aay repreatnt a different ottrli. Tkla can ke done very eaally when the detection technique la aaaa apetmetry if an leotopically labeled veraloa of the analytt(a) la available. Docuncntatlon of cxtractlon/recovery afflclencica la not requited for each aanple If the aanple oatrix for a art of eaaplet la conetant. However, for a aanple aet for which the alnllarlty of eaaplet la not known, and for which adequate people la available, each eaayle nuat be apllt and epiked with a known aaount of the analyte(a) of Interact to dettrnlnc extraction efficiency. If adequate aanple alte la not available or the Identity of the analyte(a) le not known before the fact (l.e., vldeacen analyalc), aurrogate oplking couponnda nay be weed to aaaeaa extraction afflclencica In eack eeople without actually eptklng each aanple with the nnalyte(a) of Intereat. The choice of the eurtoiate aplkln| conpound la tailored lor each analyte. Tkla aurrogate nuat ke ckocen eo that It la either ckanlcally Identical to the analyte af Intereat (for exanple ueln| laotoplcally labeled analo|uea of the analytea), or le cloaely atelier In tame of liquid/liquid partition propcrtlee, ckenlcal reaction propertlaa, coln elution propcrtlee nr ether natria leolatlon propertlea which are need to lealate the analyte(e) free the aanple natrix. Another property af the corrugate eplklog coopound la that it not be preaent In the aanple being anelyicd. Inetriatentel Analytic QA/QC The final atop In nbtnlnlng analytical taanltn lavelvet the nee af an appropriate laetrrnatal techalqoe to pradvee the analytical data. Several QA/QC prectlcaa nuat be incorporated In thin protect to anawra validity af the data. a. laetrvneatetloo Careful docmaaatatlan af laetnMat naage, calibreclan, and nalntaoance la aaaontlal far the genatatlaa of high quality feoalta. Sack nejor teatraneat within the ntratrace Analyoie Cranp will be the aaalgnad reapanalbUlty af a prafaaalenal enplayae deelgneted aa the laetnaaaat Steward. The laatrtmat Steward So raapanalbla tar waking aura that loghooka are avail* able and properly caaplatad by Inowiat ueere. It le the U HONS 02312b reaponelklllty of tack MlfMul ualnt tba xhIimii to record all tht riiilHM data regoired'ln tka ls|kook. An unrlt of a Ml* lm a CC/MS lagkeek la glean In figutt 1 end that of a CC/tC l|tool la (loan In Titurt 1. laetruaeate will ka calibrated according to tke laettw neot aaaufactorere* eyedf Icet loot or according to tba MlW kalaf need with tba laatnaaeat. A la* of laetro* ant callktation will ba aalatalaed wltk tka laatrwaaat. tka hatnaanl Itevard will ka reayooelkle for anaorla* tkai yreeentatiee and corractloa aelateaaece yragraaa ara carrlad owl on all laatrwnanta wndar kla/kar reeyoaelklllty. If a aycdflc yroklao fa ootad by ao laatrwoaoi oaar, li akoold ka aotad to tka lo*kook aod tba Inetroutnl ttaward aotlflad ao tkat ayytoyrlate corractloa actloa cao ba taken. k. blaoka A aoloant blank will ka aoalyted at a fragueacy egoel to tka oatbod blank. Tka netkod blank cao aaroa aa tka aoloant blank yroelded ft la claaa In tka araa of tka aaalyte(e) * tntoraoi. Tkla atactica allalnataa tka yoaelklllty of backfroond Inatro* nantal contanlaatteo. c. Quantitation Internal Standard A guaatltetloo Internal atandard will ba addad to aack aan*le followte* aaayle *rtaaratloo but allot to laatnmatal analytic. Tkla eeayound will aaroa for detemlala* ralatloa raoaonaa factora and for correcting for oarlatIona In aaayle Injection oolwee and aoayoratioa of aeloanta. d. Itandarda btaadatda ora aolotlooa of tka aoalyta(a) of latereat aaad to dotarnlaa tba raoaonaa of tka detoctor ooar tka tamf of analyte concenttatlane fooad In tba aanylea. bar Qoaatltntioo annlyaaa. onfftclant ataodardo aod raallcatlan of otaadarda will ba ran to deoooetrata linearity and yracleloa of tba dotactor raeyeoae ooar tba range of analyte concantratlana. Skaold oaaalo cancan* tratiooo fall oatalda tba doaoootratad linear raa*a, eftbar additional ataodardo are a>a*rod to oraand tba ta^o, nr amofrlat' dllntlan/concantratlon nf tba aaayle la dona to ylace It In tba yrnyar range. battoat of Quantitation Tka Infatuation yrooldod for nay yartlcoler analyala la tailorod to tka anode of tba Coatoner. In actual yractlce tbaat noado wary acroaa tka broad cantlauun Iron tba srnaaly guelltotlee to tba yrecleely Quantitation. It to lafornetloa to eaanlna wbat la lnooload in yrooldlag tba onrylng dtgroaa of guaatltetloo regulrad by our coataoara. 19 HONS 023125 t*no___ HP 5985A mi___ kUMWI, ill ______________ MKM M IMM llillilT T T lO PICVU I. bNfll ( CC/ME U|Uk . HONS 023126 M*..______ HPSMO GC/rc Mmin --------------- ---- IHC B it nan ricoi i. b>iia ti cc/ec ixwm hi*0lS 0*3127 I. Qualitative Analyala Qualitative tuljiii lap)lee ao twiiltilloi at all but rather MM Mil the Mwtlt; ( tin tfinMIi) fltHM. cents la M'tlnlnlt wllciUi t* title tree ef aaalyela problem. two typee *1 Identlflcatlnne can M watt: a. Tentative A tantatlvt Identification la mada an ttie koala of tka anal;at'a Judgement of a match katvaan tka aaaa tractruo fton tka aeaple and a aaaa epeettua Itoa a tafataoca library. Tkla la aftan Anna for tka lartt naakar of compounds found In a vldtacan ot|anlc analyala. k. Confirmed A confirmed Maatlflcatloo requites tkat tka chromato graphic ratantlon tint aad tka aaaa tract ran of tka known coapound aatek tkoat af a known atandkid ef tka tentatively ldantlflad coapound. TMa la aftan done In vldtacan enalyeet vktn etenderda tan ka attained for tentatively ldantlflad coapoundi tkat art af caacaro Tka aoraal QA/QC requlrenenta far qualitative analyala art (1) analyala af a blank, (1) analyala af duplicate aaaplaa and (!) uee af a calibration coapound (oanelly DacafluorotrlpkcnylpkoapMna, Wlff) to assure that the aaaa spectrometer will produce aaaa apactra tkat can ka coaparad with library apactra. 1. Senl-Quantltatlvc Analyala Seal-Quantitative Analyala ax troda tka Information provided by a qualitative analyala ta include aaaa aatlaata af the amount of analyta(a) praaant. Tka atthod af aaml-quant ItatIon involute tka cooper!ton af datactor rtapaata af tka analyta(a) with tkat af ao Internal atendard. The eat lotted concent rat loo la obtained by resuming a unit taapaaat lactat katvaan tka aaalyta(t) and the Internal atandard(a). An Indication of recovery from tka aample aettli la obtained free the recovery of tka surrogate Internal atandard(a). ). Quantitative Analyala Qwantltatlva Analyala provldtt far the accurata aaaaaaaant af the amount af aaalyte(e) praaant In a aample. To be able to da qwantl tatlva analyala ana awat kaev tka Identity ef the analyte aa tkat ataadarda can ka praparad far apiklng aad far the generation of calibration cwrvaa. Tka method ef quantitation la kaaad on a three-point calibration curve wolag ataadarda ef tka analyta(a) af Interaat aver tka range af eeoeentratlone In tka aamplaa. A onepolat calibration method can ka aired (aa with tka laboratory data 22 HONS 023128 >!) ptovMnd till linearity ku km ImnimuI mr the concentration range af tha sesplss hIh tiMnli >1 the mltu(i) at three concentrations la tka tM|i. Thin callkratloa nrta la tkaa Mil ta imMi MKHtmiMi of tka mljti(i) Is tka HMlM Til aa nmiil ataalatla MtM ar aara riilnibly ala an lataraal standards nethod. fat tka latataal atwlnli Bathed, tka guantltatlan lataraal standard la adial ta aach af tha standards (last aa vltk tka senples) prior ta laatraaantal analysis and relative reaponie lactara ara dataralnsd. far Quantitative analysis tka Mas apactronstar la operated as a gas chronatographlc datartar. Tka M la tkarafara taaad and operated la a Mnnar specified ta tka approved Mtkad ratkar tkan aalag a calthratlaa cenpeund aa regulred far gaalltaclaa analjrsas. 0. Quality Crltarla and taaadlal Action Tka laclasiaa af QA/QC Maaataa late aa aaalyala yrsgraa has llttla saaalag anlaai tha raaalta ara Interpreted and appropriat* act lea la takaa vkan aacaasary. Tka aklllty ta do tbla aeeunee none act of crltarla that will trlggar a raapoaia ar raaadlal action. Tha following aaksactlona daacrlka tka crltarla that ara usad la tka Oltratrace Aaalyala Croup to avalsata whan Quality cootrol data ladlcata a aaad far corractlva aaaturat and what raaadlal action will ka titan. 1. Quality Crltarla Tka auatrldlag Quality crltarloa abowa all ethars la: Do tka results Mat tka aaada of tka cultsoar. This datarmlaatloa will ka Mda Jointly between tka castoMr and tka aaalyat. Tha analyst mist aaarclaa caution la not allowing tba cuatonar to awaratata, alelnterptat at unintentionally nltrapraaant tha data. In addition ta tkla prlna Quality crltarloa, tka following conditions oust ka Mt: a. glaaka - la tba avast that a blank producaa a positive value, It My net ka naad aa a valid blank If It axcaada 101 a( any raportsd valwa far a aanpla. k. Kacovarlas - gacavarlaa tar all surrogate and native aplkat nutt 11a in tka range of MHaecovery<lS01. c. Precisian - Incision *111 ka calculated based an the recoveries of surtsgs -v lataraal standards. Average recoveries will ka calculated with * standard deviation for aach aanpla sat. Aepllcats asalyaaa and lew and high native spike recoveries My also ka weed ta provide additional internetloa/laeight lata tka precisian af tka aMlpals. 23 HONS 023129 4. U>ll #f hlKIlM Tka 11Bit ( iMKtlN (IW) Vlll (mtllt M Mitd at % ilka tralaa af tka lav Iml utiaa aflit if it ticniial aa< fMtlllaUt. Nnll Iki lav 1ml sattoa aalka at k rataantad, tka LOO will ka Halil aa H tka aalaa af tka kl|k laatl aativa aalka If It la racaaarad nl gaantlflakla. tkaalt aaltkat aalka ka tacaaarad, a daelaleu Baal ka salt rtgarding tka adaluklllty af raaraeaaalat tka aaatla. Ikould all aaaflaa casta la Back lat|a tamtltlaa af tka aMlata(a) tkat tka laaala af tka law and kl|h aaikaa ata laalgatflcaat (<10t) ky caaaatlaan, tka aalaa af tka LOO kacaaat lata laaattaat anil la alBtl) atatal aa tka LOO fat tka laatruantal aaalyaia pracaaa datarslaad k; tka aulyala af ataadarda itl tka ability ta racaaat a. Accuracy - Tka accuracy af tka analyaaa la kaat datarviaad ky analytint bom Hayla nkick caatalaa tka aaalyta at aaaa pradatarnlnad laaal (a.|., aa ns ataodardlicd aaapla). If tkla type af atandard la aat aaatlakla tkaa tka lav laaal lal ki|k laaal aplkaa can ka waad aa a Baaaura af tka accuracy af tka analyaaa. kaaulta auat fall wltkln a raa|a af III ta 1101 af tka axcaytad aalaa fat tka analyaaa ta ka canaidarad aalld. If tka akaaa auallty ctltatla ara not Bat tka analyat vlll Inudlataly aaaaaa tka natd fat and antant af tanadlal actlan tkat Bay ka nacaaaaty. 1. tanadlal Actlan Tka fltat cauraa at actlaa will ka far tka analyat and/at group laadat ta cantact tka cvatovar and dlacaaa tka taavlta pointlag But tka llBltatiana af tka data ladleatad ky tka auallty canttal taawlta. At tkla paint tka overriding goalley crltarlan af caatanat naada will ka addtaaaad fltat. It caald ka tkat tka caataaat'a naada ata sat vltkavt Batting ana at Bata af tka etkar ctltatla. In auck a caaa no tanadlal actlan ta nacaaaaty. It canid alao ka tkat tka caatanat kaa sack a dasand lat tliktaaaa la tka taanlta tkat kla naada ata sat sat even tkaafk tka Btkat guilty ctltatla ara. Tkla vonld ttluat fattkat analyaaa vltk tlgktar guilty canttal daalgacd atavnd tka taaalta aktalnad (a.|.. tapllenttana af paaltlaaa ta kattat catakllak pracfalan at aplkaa af nan-datactad aanplaa ta kattat aatakllak tka Halt af dattctlan). Is cooaaltatlan vltk tka cutover addltlanal cxpatlaanta will ka daal|nad Including tka apptoptlata gaallty canttal ta altlaataly ptaalda tka taaalta af aafflclaat guilty ta Mat tka caataur'a uada. VI. kata Tkla aactlan daala vltk tka ankjact af data and kev tkay ata aktalnad, tacardad and ttdatad aa aa ta ka aaaakla to a tapart and yet taadlly aaatlakla fat tafattal and toapactlan. 24 HONS 023130 Hh aaaplea Wll W liMW with lag ntn at io>li login ictHllii ta tka (iNilni leecrtad la aha ISC Sactiaa Of Manual. Mm* dellvard ta tka raafaaalkla tatkalcal pereon, tka aaaplea aajr tkaa receive additional lakallag aa loaned aacea- ary. Tula ddltlonal lakallag will ka fcnantil la a laboratory logbook ad/ar aatakaak. Han la|ktU ad aatakoaka will ka wag kg tka aaalpala ta Iatari all *>* raevlte aktalatl (ta* tka aaaplea. tka laboratory aatakoaka will ka llllal awt la accatlanca with Naaaaata Dalian Dotakaak Procdwrea. all >aw lata generated fat a given frajact, which caanat ka conveniently filed ta tka laboratory aatakaak (a.|., chreaatatraaa, coaputar awtpvt, ate.), will ka fllal walar aaaa ptaatrlkd ailar (l.a., lag awakarl la a caattal Ilia valet the awparvlaoa of the project ladar ad/at QA Spatiallat. Hoat of tha lata gaaatatad by tha Ultrataaca Analyale Croup ara coaputar lata atarad aa aagaatlt dlaca. la ardar ta archiwa thaac lata tha apaclflc Ilia aaaa aal live awakar aaaoclatad with tha aaalpala will ka wrlttaa lawa la tha laboratory aatakaak aal/ar Inaimeni logkaak. When tha llae la caaplatalp full of lata aa aatlia waadltad Hat laaga at copy al tha fllaa aa tha llae will ka ttaaafarral ta aagaatlc tapa. A logbook will ka kept far recarllag tha llae auaker, aaaa ad preflv aaaaclatal with It, aloag with the aaaoclatd tape aal file auaker to which the llae waa traaiferrad. An axaapla of euch a lagkook la given la fl|ure ]. Whan tha lata art traaaftrred a verification prograa la waad to check all tranaferrd recorli for cailtclaaai. When tapet art filled (they typically hold etvtn to tan llae laagat) they ahauld ka atorad la a fireproof vault. All calculation! of the raiulta of tha lata will ka apectflad la the aethd weed. Ihtat calculation! will ka aatartd la tha analyata lakoratary notebook aaleae they are caaputer generated, la thla cate, a copy of tha coaputar output will ka filed with the raw lata. The Project Leader will ka ratpenalklt for checking tha torrectntai of tha lata. T. iaapUjyiP!*1 gnplei will ka liepoetl of in accordance with tha lnetructloaa on tha Analyeie gagueet fan. The only eiceptlon ta thla would raault when tha aaalpala ravaala a praklaa which regvlrae aaapla dlapoaal la a aaaaer other than that originally opacified. If tha Prajact loader voice Iron the reaulca of tha onalyaio that a potentially toxic product woo praecnt la tha eoaplee than tha ooaplee will ka liapaeed of la a wanner laaad aofa hy the Safety Deportaent. Tha lata of aaapla liapaaal ad tha wanner ahovll ha natal aa tha regveet fan atarad with tha raw lata coapletiag tka chain of cwatdy of tha aaapla. 25 HONS 023131 t*1tl*art MtfNtto*) Hnm UH fH # CHU f) itrv> iyw fcM* i/if/o Gt>Wr\ r>i (*yfr) tX* Hit ot>t*(sy )v $*) i *N*i J 6t>HU) /J> 0*3>/ I Ct>HO) feo WV'' CftiVf) V(fe hn* V>/{ru* 6t0f*) i >5 (*t#5>U0 .jMj ~&t* V'V<J 6T>i*9) OCr CM*) Cfl <**H UK S/mn fejoart) iV? (3**"0 C]S\ 3-11-0 !> (M*l)t0 ' >'"*> / TM*o)t/H} ~ * -tn> fiMV*<3 - (WOm yibv &K 3K W (toU l j>htts i/O'Jti 4t>7if3) C>f) )){$> CfHfio) r>7/f/) /<3 to> Vki /N MOMO - ' l 07 0 ImQ ybfhj $6K no (**!t) in i i>*fu> XK. Hi 'A?-''1 ftl& G#1 s/v/l* St /y;. sl> /*> />/>>) 33 l *W7/*3 Gl)lf('i) 6?J3(5j >7-5 .) G3>ns(7) P7><r> ,0/ //) ->3 /Vs t*tes) -*> s}y>hf> /Vb (MO*) S3 Wilts /V7 (Hat) n> U>hs /V? (Hal> m ftt*) . /*> (Hi*) i 3} l/lT/V ji L/32/fJ jIS ) JTT>>f'y-3K 331 V-J3 41 (Hu) (m2 to* tfri/ii teu ('<**'> 4/t>/b M*3 ^J - '>WMhtfi 1cJinr ton (<Jy Q>o3 <jv CiYJ, (J.) J> V (3> <> > (A> Co ( bbh1AA *O1/) J ft MCUU J. baoplf of DllC/Tapt Logbook HI*- HONS 023132 2b