Document jykv05g1aoEBnZnne7DJxKXNQ

Monsanto (to:;iMvc.`ikrupU/rLvoc*t1w) ____________ Analysis (rypn or Report) REPORT NO.: MSl-6369 ESC-EA6-87-02 JOB/PROJECT NO.: 760.28-6275 DATE: January 14, 1987 TITLE: Analysis of Aroclor Fonaulatlons In ono Soil Saaple Iron tha Krtaarlch Plant AUTHORS: B.H. Hughes, O.E. McKenzie and B.J. Slnpson ABSTRACT: Ono soil saaple from tha Krtaanrlch Plant ms analyztd for Aroclor foraulatlons using capillary 8C/EC analysis tachnlquas. Tha saopla ms found to contain both Aroclor 1254 and Aroclor 1260. Tha Mjar coaponant ms found to ba Aroclor 1260. Basalts Indicated that Aroclor 1254 concantratlons warn fairly hqaogoneous throughout tha soil, ublla Aroclor 1260 concentrations uara aora varied. Tha total concentration of Aroclor foraelatloae In duplicate analyses ware approxlnataly 1000 and 300 up/p. Thareforo this sanplo should bo trantad as a PCS notarial. Please contact John Craddock and/or Paul Hlchaol concerning disposal regalreaents, etc. ESC-EA6-87-02 T I1 U : A n a lysis o f A ro c lo r h i w U t l o u In On* S a il S a f in ii Ii "'"UNece. TECHNICAL APPROVAL: Envlronaantal Sciences Cantor Senior Research 6reap Leader APPROVED BY: EEnnvvilronaantal Sciences Cantor QQuuaal lity Assurance Specialist APPROVAL DATE: ,a<//p/7 HONS 024500 COMPANY CONFIDENTIAL TMe document Is the property of Monsanto Company and the nclpicm <e raeponalbla for Ha safekeeping and disposition. H contains CONPBENTMl INFORMATION which must not be reproduced, revealed to unauthorltad pareona or sent outside tha Company, without proper authorization. I) ! S T HlliU I o\ COPY NUMBER 1. B.M. Hughes - U4E 2. O.E. McKenzie - U4F 3. B.J. Simpson - U4F 4. A.M. Ford - U4E 5. R. McEntlre - Kmemirlch 6-8 Reports Library - R2C 9. Chesterfield Information Center - AA3A 10. W.M. Mees - U4F ABSTRACT ONLY P. l. Sherman - U1F COMPANY CONI IIHMIA! This reoon has been assigned to you. When it is no longer needed, you are responsible for returning it id: i _ -1 i' you transfer it to anyone else, dlease let your librarian know, so the recordscan be changed. -l3Bt:C!tv I BOt HQNS 024501 Time Scamp - <8 70114 . U22> ANALYSIS IU0KT DATE: January 14, 1986 LOG NUMBER: U-66-12-08-02 PROJECT NO: 760.28-6275 TO: Ron McEntlre/Krummrlch FROM: Environ--ncal Sciences Cantor Monaanco Company 800 N. Lindbergh Blvd. SC. Loula. Mo. 63167 Phono No: (314) 694-1464 Titla: Analysis of Aroelor Formulations in ona Soil Saapla from the Krwlch Plant. ABSTRACT Ona toll aampia from Cho Kru--rich Plane was analysed for Aroelor formuladona using capillary CC/XC analysis techniques. Tha sample was found to contain both Aroelor 1254 and Aroelor 1260. The --jor component was found to bo Aroelor 1260. Results Indicated that Aroelor 1254 concentrations ware fairly bo--fonaous throughout tha soil, while Aroelor 1260 concentrations ware --ra varied. The total concentration of Aroelor formulations In dupli cate analyses were epproxl--tely 1000 and 300 ug/g. Therefore this sample should be treated as a PCS material. Please contact John Craddock and/or Paul Michael concerning disposal require--nts, etc. INTRODUCTION One soil sample m received from ehe Krunrnrlch Plant for PCI analysis. The sample was analysed using capillary CC/1C analysis techniques by diluting using Standard Bstraetlom Method PCIX02 and and analysing the resulting ex tract using Standard A--lysis Method ECAN02. These --thoda and flow sheets PCPS02 and ECFS02 are Included in a later section of this report. SUMMARY Table 1 s--rises results for the analysis of Aroelor fornulaelons in one soil sample. The sample was analysed in duplicate and concentrations of Aroelor 1254 were found to be 48 and 54 ppm respectively. Concentrations of Aroelor 1260 wore found to be 1015 and 250 respectively. These valuee in dicate that Aroelor 1254 Is fally uniform throughout the soil, while Aroelor 1260 is not homogeneous In the soil. QC RESULTS Table 2 Su--arles QC results for this project. The sample was spiked with Aroelor 1242 at levels corresponding to 1.5 ug/g and IS ug/g. Respective recoveries are given In Table 2. (continued) M0NS 024502 Page 2. A27518 (cont'd) Tabla 3 aiaurliu percent recovery ef surrogate spiking eoapsunds. Tha saaple was spiked with paneachlorobanzana and 2.4.6-trlchloroblphenyl. Tha respective recoveries ars llaead In Tabla 3. Tha unusually high recovery ef paneachlorobanzana Indicates that paneachlorobanzana or ioae other nonchroaatographlcally resolved lncarfarene was prasanc In cha saaple. Recoveries of 2,4.6-trlehloroblphenyl ranged froa 91 through 1079 Racovarlaa of tha native Aroclor 1262 In tha spiked saaplee along with cha recoveries of 2,4,6-trlchloroblphenyl surrogate spiking coapound lndlcsce chat the data Is reliable. DETAILS Standard 3sapling Method Ho(s): Saaple supplied by Ron McEnclra. Standard extraction Method Mo C s): PCEX02 (Sea PCFS02 for aaehod flow shoot.) Standard Analysis Hschod Mo(s): ECAN02 (Saa ECFS02 for aaehod flow sheet.) Ssapls Identification!s): BBU LOADING DOCK. Final Report Fils No(s): A27S1S Tabla Fils Ro(s): B27318, C27518, D27S1S Also Included ara: (1) Brief descriptions of extraction and analysis aethods used. (2) Extraction details for ssaples associated with this project. (3) Analytical Request Information recorded at login. (4) Discussion of Important teralnology used In quality Assurance/ Quality Control, Analyte Extraction and Instrumental Analysis. AXALYST(S): B. Mason Hughes, David McKenzie, and Brenda Slnpson. , Tlw^ ANALYST APPROVAL HONS 024503 Tibi* 1. Reaulca of Aroelor Concentration* decocted In on* Soil pi* Cora ch* Kruanrlch Plant ualng capillary CC/EC analyala. ESC Projact Ro: 760.2S - 6275 Data: Dacaabar 19, 1916 Saapl* ID. EXTRACT BBU LOADIRC DOCK PCB-1853 LOD(b) (ug/g) IS AMOUNT DETECTED ABOCLOR AROCLOR 1256(ug/g) 1260 (ug/g) 40 1015 BBU LOADING DOCK DUPLICATE PCS*IBS* 15 54 249 METHOD BLANK PCS-1855 15 ND(b) HD Fooenoea*: . b. LOO- Lisle of Dococclon was stlMCod on tha baala of Aroelor 12*2 aplkad In eha aaapla SO ug/g. HD- He Aroelor fonulaclona detected abov* th* llalc of dataetlon. Fomulatlona Include: A1221, A1232, A1242, A1248, A125*, A1260, A1262. TABU nu HO: B2731S:MH HONS 02*50* Table 2. Summary of Aroclor 1242 Spiking Concentration* and Recoveries In Quality Control Experiment* for on* Soil sample from the Krummrlch Plant. ESC Project No: 760.2S - 6275 Saaplo I.D. UU LOADING DOCK + LOU SPIKE MU LOADING DOCK HIGH SPIKE Date: December 19, 1916 Aroclor 1242 AaounC Added Recovery ("*/*> (%> 1.5 355(e) 15 166 Fooenoeo: a. High rocovory duo Co Ineorferrlng ruponsta froa Aroclor 1254 whleh l* prceonc In ehli staple. TABLE FILE NO: C273!S:HH HONS 024505 Table 3. Surrogate Seandard recoveries In on Soil fora the Kruaarlch Plane using Standard Analysis Method ECAN02 and Seandard Extraction Maehod PCEX02. ESC ProJcC No: 760.28 - 6275 Data: Dacaabar 19, 1986' Saapla I.D.(a) BBU LOADING DOCK EXTRACT * FCB-1853 PERCENT SURROGATE RECOVERY Pentachloro- 2.4.6-Trlchloro Benzena(b) Biphenyl 707 107 BBU LOADING DOCK DUPLICATE METHOD BLANK PCB-1854 PCB-1855 917 101 96 98 BBU LOADING DOCK LOU SPIKE PCB-1883 1472 102 BBU LOADING DOCK HIGH SFIKI PCB-1884 1499 100 Poetnotas: a. Extracts war* which war# spiked with Aroclor 1242 as part of the QA/QC protocol aro indicated by a LS or HS. which Indicates the level of Aroclor 1242 which was added to ehe extract. b. The unusually high recovery of pentaehlorobensene in the soil saaple indicates that the saaple contained pentachlororobensene or soao ocher non-chroaatographlcally separable lnterferent. TABLE FILE BO: D27318:MH HONS 024506 Ths followtut PMM dsscribo Standard Saapllng, Extraction, and/or Analysis Hotbeds usod for this project. HONS 024507 ISC Standard Analysis Mathod (SAM) TITLE: Aroclor Fomulation* In Solvents ISC Standard Analysta Mathod No: ECAN02 ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-5880 Capillary CC/EC Inter faced Co an HP-3357-LAS Laboratory Data SyaCan TYPICAL analyte TYPICAL instrument level or detection (lod> (ug/nl) Aroclor fomulatlona 1232. 12*2, 12*1, 1254, 1260, and 12S2 0.1 TYPICAL PRECISION 9 I0X LOD <<) 30 TYPICAL ACCURACY 9 10X LOO <%> 30 INTERFERENCES AND LIMITATIONS: Any alaccron capturing apaclaa In cha ratan- tlon elna region of trlchloroblphanyl through octachloroblphanyl lsoasra ara potantlal lntarfarancaa. Exact retention tinea of aoat likely PCS laonara can be obtained fron the analyala of Aroclor 1248, Aroclor 123* or Aroclor 1260 foraulatlona. CHROMATOGRAPHIC COLUMN: 30-necer fuaad alllca JAM DS-5 (0.23 idl) with wide bora (0.32a). COUMI TEMPERATURE PROCRAM: 130(l)/4/300 INJECTION TYPE: Spllelaaa CALIBRATION AND STANDARDIZATION: Uaa Internal atandard quantitation technique and calibrate lnatrtaant reaponae factors fron authentic Aroclor fomulation atandarda. Uaa a nlnlnua of 10 PCB lsonars for the (lateralnation of fomulatlon Identity and quantity. CALCULATIONS: Fomulation concentration (laoner ERF) (leoner araa/lntamal standard area) where: REF la the relative reaponae factor for the appropriate PCB lsoaer In a given fomulation. Fomulation concentra tion le obtained fron the average of at laaat 10 such cal culations. SAFETY PRECAUTIONS: Sae PCB handling protocola In laboratory eafecy annual. DATE OF METHOD CREATION: 10/25/83, 2/3/8* Tina Stanp - <861219.0939> HONS 02*508 nmr sheet ecfso2 roa ESC ANALYSIS METHOD ECAH02 EXTHACT ID: ESC EXTRACT * LOC NO: ............ . EC LOGBOOK MCE NUMBER: ........................................................................................................................ EXTRACT COLOR AND DESCRIPTION .......................................................................................................... PUCE ISO uL EXTRACT OR AROCLOR STANDARD, AMD ISO uL INTERNAL [] STANDARD SOLUTION CONTAINING . 0.04 ug/nL CIA-BENZENE IN . BENZENE IN A 1.6 iL . AUTOSAMFLER VIAL. . PUCE VIAL IN AUTOSAMFLER TRAY OF HP-SSSO. RECORD ELECTRON CAPTURE AMD GAS CHROMATOGRAPHIC OPERATING PARAMETERS AND 3357-LAS FILE INFORMATION IN INSTRUMENT LOCSOOK. (] . [) CALCULATE RRFl TOR 10 - 30 PCB CONGENERS IN THE APPROPRIATE AROCLOR FORMULATION. USING THE AROCLOR CONCENTRATION AS THE ........................(I ANALYTE CONCENTRATION . FOR EACH PCB CONGENER. [ ] CALCULATE CONCENTRATION OF AROCLOR FORMULATION BY AVERAGING THE VALUES DETERMINED FROM THE 10 30 PCB CONGENERS. Whara: RRP - Raladva Rupnut Factor (conganor arta in Aroclor atandard) (CL6-banzana araa) (Aroclor concancradon) (conganar araa) Aroclor Concaneratlon - ......................................................... (CL*-banzana araa) (RRF) THESE EQUATIONS ASSUME THAT THE SAME AMOUNT OF INTERNAL STANDARD IS ADDED TO EXTRACTS AND STANDARDS. Tha abova calculation! ara parfonaad for 10 - 30 PCB conganara and cha valuaa avaragad to plaid an avaraga Aroclor fonuladon concancradon. MS FILE NUMBER: .................................. DATE/TIME COMPLETED................................../ ANALYST: .......................................................... ESC JOB NO: ........................................................ MOMS 024509 ESC Standard Extraction Method (SIM) TITLE: FCBs in Non-EC Active Natrleas MATRI(X),(CES): Soils and other non-EC active aolids and solvents ESC Standard Extraction Mathod Mo: PCEX02 TYPICAL SAMPLE SIZE (*) TYPICAL EXTRACT VOLUME (i) 0.5 - 5.0 10 TYPICAL ANALYTES: Aroclors 1232. 1242. 1248. 1254, 12(0, 1262. triehloroblphanyl isonars through octachloroblphenyl isoaers ESC Standard Analysis Method Nos: ECANOi, ECAN02 INTERFERENCES: Any alactron capturing spaclaa In the retention tine region of trlchloroblpheayl Isonara through oetaehloroblphenyl teeners. TYPICAL SURROGATES TYPICAL RECOVERIES (%) pantaehlorobansana 2,4,6-trlchlorO' biphenyl 50 - 120 50 120 APPARATUS AMD MATERIALS: Burdick and Jackson bonzana or haxana for sanple axtractlon or dilution. Ultraaonlc bath. Nitrogen for axtract voluaa raduetlon. Disposable glassware. (Saa flow ahaat for thla axtractlon nathod In PCFS02.) LIMITATIONS: Mathod appllaa only to natrleas which do not contain interfering alactron capturing spaclaa la cha trlchloroblphenyl through octechloro* biphenyl laonar retention tine region. SAFETY PRECAUTIONS: Saa FCB handling protocols In laboratory safety aanual. DATES OF METHOD CREATION AND UPDATES: 10/31/83. 2/3/84. 10/3/84 HONS 024510 plow shut rcrsoz FOK ESC EXTRACTION METHOD rctX02 SAMPLE ID: EXTRACTION DATE nd TIME: - SAMPLE COLOR AMD DESCRIPTION WEIGH OUT SAMPLE INTO A 14 OR *0 aL PIERCE VIAL SURROGATE SPIKE OF SAMPLE . {] MRC EXTRACT LOC NO: FINAL WEIGHT INITIAL WEIGHT SAMPLE WEIGHT ADO 10 aL BENZENE TO SAMPLE. . (j ULIRASOHICATZ SAMPLE FOR 1/2 HOUR IN A SOUND BATH. (] . . PUCE l aL OP THE EXTRACT INTO All/2 aL VIAL FOR ANALYSIS. . (] . NITROGEN BLOW DOWN IF REQUIRED [| EXTRACT NO: ............... DATE/TIME COMPLETED ANALYST: ESC JOB NO: FINAL VOLUME MONS 024511 Tha followInf pagaa ahow aatractlon datalls for aaaplaa aaaoclatad with tbla projact. HONS 024512 rLow sheet pcrso2 rot ESC EXTRACTION METHOD FCEX02 SAMPLE ID: BBO LOADINC DOCK DECEMBER 19, 1988 EXTRACTION DATE and TIME: DARK SOIL SAMPLE COLOR AMD DESCRIPTION PCB-1833 MRC EXTRACT * ........................ U-86-12-08-02 LOG NO: ........................................ WEIGH OUT SAMPLE INTO A U OR AO aL PIERCE VIAL (X] . SURROGATE SPIKE OP SAMPLE (X) l.oil g. SAMPLE WEIGHT .................................... 300 uL DEM 121483 - 02 (10&20ug/aL) ADD 10 aL BENZENE TO SAMPLE. . (X) ULTRASONICATE SAMPLE TOR 1/2 HOUR IN A SOUND BATH. (X) . . PLACE 1 aL OP THE EXTRACT INTO All/2 aL VIAL FOR ANALYSIS. . [) . NITROGEN BLOW DOWN IF RSQUIREO [) PCB-1S33 EXTRACT NO: ........................................... 12-19-86 DATE/TIME COMPLETED........................ SIMPSON ANALYST: .................................................. 760.28-6275 ESC JOB NO: ......................................... FINAL VOLUME 10 HONS 024513 FLOW SHEET PCFS02 FOE ESC EXTRACTION METHOD PCEE02 BBU LOADING DOCK SAMPLE ID: .......................................................................... DUPLICATE .......................................................................... DECEMBER 19. 1986 EXTRACTION DATE and TIME: PCB-1854 .IRC EXTRACT ..................... U-86-12-08-02 LOC NO: ....................................... SAMPLE COLOR AND DESCRIPTION WEIGH OUT SAMPLE INTO A 14 OR 40 aL PIERCE VIAL (X) . . SURROGATE SPIKE OP SAMPLE . (X) 1.138 g. sample weicht ........................... 300 uL DEM 121483-02(10&20ug/BL) ......................................................................... ADO 10 aL BENZENE TO SAMPLE. . (X) ULTRASONICATE SAMPLE FOR 1/2 HOUR IN A SOUND BATH. [X] . . PUCE 1 aL OP THE EXTRACT INTO All/2 aL VIAL PUR ANALYSIS. . (] . NITROGEN BUM DOWN IP REQUIRED . |] PCI-1854 EXTRACT NO: 12-19-86 DATE/TIME COMPLETED SIMPSON ANALYST: 760.28-6275 ESC JOB NO: 10 FINAL VOLUME .................................. aL HONS 024514 runr shut rcrso2 FOR ESC EXTRACTION METHOD PCZZ02 SAMPLE ID: METHOD BLANK MRC EXTRACT PCB-U55 DECEMBER 19. EXTRACTION DATE and TIME: CLEAR SAMPLE COLOR AMD DESCRIPTION 1986 LOC NO: ............... NEIGH OUT SAMPLE INTO A 14 OR 40 aL PIERCE VIAL [X| . . SURROGATE SPIKE OF SAMPLE . |X] 0.000 g. SAMPLE HEIGHT ........................... 300 uL DEM l2LA83-02(10U0ug/aL) ......................................................................... ADD 10 aL BENZENE TO SAMPLE. . [X] ULTRASOHICATS SAMPLE FOR 1/2 HOUR IN A SOUND BATH. (X) . . PLACE 1 aL OF THE EXTRACT INTO All/2 aL VIAL FOR ANALYSIS. . [J . NITROGEN BLOB DOW It REQUIRED [j PCB-1S5S EXTRACT NO: ........................................... 12-19-86 DATE/TIME COMPLETED........................ SIMPSON ANALYST: .................................................. 760.28-6275 ESC JOB NO: ......................................... 10 FINAL VOLUME ................................. aL HONS 024515 flow shut pcfso2 F01 ESC EXTSACTION METHOD PCEE02 SAMPLE ID: BBU LOADING DOCK ........................................................................ + LOU SPIKE ....................................................................... EXTSACTION DATE and TIME: DECEMBER 22. 1986 DARK SOIL SAMPLE COLOR AND DESCRIPTION PCS-1883 MRC EXTRACT a................... U-86-12-08-02 LOG HO: .................................... WEIGH OUT SAMPLE INTO A U 08 40 aL PIERCE VIAL (X) . . SURROGATE SPUE OF SAMPLE . [X] . 1.243 g. SAMPLE HEIGHT ..................................... 300 uL. DEM 121683-02 (10620 u|/aL) LS- 300uL. DEM 100886-02 (3ug/aL) ADD 10 aL BENZENE TO SAMPLE. . (X) ULTRASONICATE SAMPLE FOR 1/2 HOUR IN A SOUND BATH. [X] . . PLACE 1 aL OF THE EXTRACT INTO All/2 aL VIAL FOR ANALTSIS. . (1 . NITROGEN BIJOU DOUN IF REQUIRED . l1 10 FINAL VOLUME ................................. L PCB-1S83 EXTRACT NO: ...................... JANUARY S. DATE/TIME COMPLETED - SIMPSON ANALYST: -- 760.28-6273 ESC JOB NO: 1987 MONS 024516 rUW SHEET PCFS02 POE ESC EXItACTXOH METHOD PCEZ02 BBU LOADING DOCK SAMPLE ID: ....................................................................... + HIGH SPIKE ....................................................................... DECEMBER 22, 19BS EXTRACTION DATE and TIME: DARK SOIL SAMPLE COLOR AND DESCRIPTION PCB-1884 MRC EXTRACT ................... U-86-12-08-02 LOG NO: .................................... WEIGH OUT SAMPLE INTO A 14 Oft 40 aL PIERCE VIAL (X) . . SURROGATE SPIKE OF SAMPLE . [X) . 127* S SAMPLE WEIGHT .......................... 300 uL. DEM 121483-02 (10420 ug/aL) HS- 300uL. DEM 1008S6-02 (50ug/aL) ADD 10 aL BENZENE TO SAMPLE. . (X) ULTRASONICATE SAMPLE FOR 1/2 HOUR IN A SOUND BATH. [X] . PLACE 1 aL or THE EXTRACT INTO All/2 aL VIAL FOR ANALYSIS. . (I . NITROCEH BLOW DOUR IF REQUIRED :i FINAL VOLUME PCB-1SS4 EXTRACT NO: ........................................... JANUARY S. 1987 DATE/TIME COMPLETED.............................................. SIMPSON ANALYST: .............................................................. 760.28-6273 ESC JOB NO: ..................................................... 10 MONS 024517 Thm following pagas show calculations or raw data docunancacion of reported raaulta. HONS 024518 Top Raw: BR337 Bottoa Raw: BR340 ( 20.0- 30.0) ( 20.0- 30.0) (Enlarged x (Enlarged x 20.0) 30.0) HONS 024519 Top Raw: BR337 Bottoa Raw: 8R340 ( 30.0- 41.0) (Enlarged x ( 30.0- 41.0) (Enlarged x 20.0) 30.0) HONS 024520 MOWS 024521 Top Raw: BH33B BottOM Raw: BR340 ( 30.0- 40.0) (Enlarged x ( 30.0- 40.0) (Enlarged x 20.0) 30.0) HONS 024522 Tha following pogos show ehain-o-eoatoiy information for thla projoce. HONS 024523 ___________________ iqia shipping oatw Monsanto -(omm________________ *tt*i nn^n ( mk ) "1ST m ___ 1_ Sell SmmIm FlbrtoMrt Bra (X t 8m.) a 3# cjv NOTlCf TO CAMIMtW w pod amt mmm THU SHIM0VMT It MMmT TO MQM MMfO INlHlNt iooahom tv mm mrnirnmmmm phn7mi i Ml tH m MB MTI MlWIIltO FOR CMIMCAL EMEMMNCT VU.IHM StesKMwaszv3a ; (vmum on acomnt cau. cmmtnmc o*r m mour 14 CMCANVTfC MU I MONS 024524 Monsanto iiqhmuw wcuttma. ot--via oa. MOt ft*** IffM 171-MM CBAIM or CUSTODY SAWFLIIC tfCOiP SMoltof Identification: bJtiS'G. Do>l. tiUsn BSd Lc+v-^i* Dock. Lot ta>br: 0CC73 Data: tl/r/ru Analytaa Kaqulrad: ~7Cb HM.WJT Mcom . (i/Ofcl Data: /3/.XL Data: itklyi /^, teUwtliM Tn P>tO CamMata ibob or umno tiU Uport Ho. Author WTIUCTIOW Tha paraoa taklag tha tarlt coaplataa tha Information la cha Stapling acord araa. each paraon to nfeaa tha aapla la rallaqulahad ahould alga tha fora aad forward aa aacaaaary. Analyaaa parforaad ahould ba llatad with taaaaata. Whoa all analpaaa aro eoaplata, tha orlglaal ahould ratun to tha "acalvad y" algaatura. mi f Mmhn eapiT HONS 024525 Th following pogos doscrlbo Anolytlcol goqnose Information gnrtd for this project. HONS 024526 Tina Scrap <870114.1135> MONSANTO COMPANT/ESVIKONMENTAL SCIENCES CENTEE ANALYSIS REQUEST DATE: DECEMBER I, 1986 LOC NO: 0-86-12-08-02 REQUESTER: SAUCET, ILLINOIS PROJECT NO: 760.28-6275 LOGIN NOTEBOOK PACE: 47 REPORT RESULTS TO: FILES/MRES. SHERMAN. HUCHES. HeKENZIE. SIMPSON ANALYSIS REQUESTS SENT TO: FILES. MEES, SHERMAN, HUCHES. HeKENZIE SAMPLE PICKUP BY: SIMPSON SAMPLE LOCATION: U420 SAMPLE DESCRIPTION FOR OMB SAMPLE SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC NUMBER(S) BBU LOADING DOCK Method Blank 1 X 1/2 pc. PCB-1833 PCB-1834 PCB-1S55 RECORDED BY: SIMPSON REQUIRED ANALYSES: PCBs EXTRACTION LOGBOOK NOTEBOOK PACE: 1SS6Z1 ESC STANDARD EXTRACTION METHOD! S): PCEX02 ANALYTICAL TBCHNIQUBS: TECHNIQUE (EH) DATE COMPLETED ESC STANDARD ANALYSIS METHOD INSTRUMENT LOGBOOK PACE a SC/EC (IS) 12-19*86 ECAN02 137286 FINAL EFFORT NOTEBOOK PACE:: 3,434,440 OTHER NOTEBOOK PACES: QUALITATIVE: X SEMIQUANTITATIVE: QUANTITATIVE: X REQUIRED QA/QG: SEX COOD LABORATORY PRACTICES MANUAL COMPLETION DATE REQUESTED: CMBBNTS: SAMPLE DISPOSITION: HOLD FOR 60 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME: AA275:U HONS 02452 7 Th follovlns nctloni daacriba important terminology used In Quality Aasurancs/Quality Control, Analyta Extraction and Instrunantal Analyala. ISC and ESC/QAO Good Laboratory rractleaa Manuals can bo obtained by eontaetlns Bill Haai <U4) HRS 54A-UM. MOMS 024528 Quality Aaauranca/Quallty Control Terminology Thla (action daaerlbaa commonly used terminology and phraaaa which ara uaad In conjunction with Quality Assurance/Quality Control (QA/QC). Thla infor* nation nay ba helpful In underaeandlng aoaa dacalla of Qa/QC procaduraa which have boon lncorporotod In tho proaont report. The following two sacclone alao give uaoful Information concerning carninology uaad In analyca extraction and instrumental analyale of aanplaa and aanpla extracca. Quality Aaauranca/Quallty Control - Terminology uaad to deacrlbe activities which ara daalgnad to produce analytical result* of known quality. In an effort to alniaize coata of environmental analyaaa. apeclflc QA/QC alananta hava bean Incorporated Into ESC/UAG extraction and analyala atapa which ahould not unduely burden analytical atudlaa with large development and method validation coata. Thla approach haa been taken ao chat aaca of aanplaa can be analyzed for varioua analytea without extenalvaly validating aachoda over wide conean* tratlon rangaa and without ualng nachoda which ara daalgnad for only one matrix. One price which one paye for thla approach la chat analytical pro* clalon and accuracy are aacrlflced, aonewhat. However, In many caaaa, whan clearly defined regulatory limlta have been aet, confirming that the analyte la praaane at levala well below or well above the limit dona not need the type of accuracy chat la required when the regulated analyte concentration la In the vicinity of the regulatory limit. In theae latter caaea, more extanalve QA/QC proceedurae are required than are included in the preeent acudy. Preclalon - Terminology uaad to evaluate the reproducibility of a certain determination. Paranmcere which affect analyala preclalon range from aanpla acqulaltlon, to aampla acorage, to aanpla extraction, and finally to aampla extract analyala. Normally, the major factor which affacta the preclalon of the analyala la the aampla extraction acep. Thla acep normally reaulta In aampla analyala preclalon on the order of + or - 30*. The preclalon of a reault can be determined In a maker of waya. Replicate analyaaa of the aame (ample, followed by the calculation of a percent relative atandard deviation for chat determination la Che moat popular method of aaaeaalng preclalon. However, thla cal culation ahould not be made whan chara ara laaa chan three replicate polnta from which Co calculate the percent relative atandard davla* cion. In addition, replicate extraction* end lnatruaencal analyaaa nuet be performed. Therefore obtaining percent relative atandard deviation data can be very exponaive and la noc normally obtained un- lesa large atudlaa are being conducted. A second method of aaaeaalng preclalon la with the uae of duplicate analyaaa. The praaane report lncludea reaulta of at least one sample which was analyzed In dupli cate. HPT811 It lx the responsibility of the analyala rtguaator CO review theae data and draw hla own conclusions concerning the erecl* Sion of the determination, and, more Importantly If Ch* nttclllaa at the determination meets hla needs. (continued) HONS 02*529 Fag* 2, Quality Aasurenca/Qualicy Control Terminology Accuracy Terminology used to determine the "corracrnan" of tho data. The accuracy of aoic acapa In tha analysis of samples ts typically on tha order of 10*. However, whan analyta eoncantratlona In ths saapla extracts approach ch* laval of datactlon of a determination, accuracy as wall as precision can approach 100* or greater. The accuracy of a determination of an analyte which Is peasant at concentrations which at* such greater than the lnstruaantal level of detection Is aost strongly affected by the hoaoganiety of tha sawple aatrlx and tha precision of tha extraction stop, which results In typical accuracies In environmental analyses to be on the order of 30*. Normally, che accuracy of standard solutions which are used Co cali brate analytical Instrumentation is wall below this amount, and therefore is normally not an important factor in producing inaccurate data. From time to time, analyte responses of standard solutions from different sources will be compared to standard solutions used for instrument calibration. This information is normally included in the section entitled "QA/QC Results". The accuracy of a result can ba estimated in a number of ways. The current study uses surrogate standard recovery and native analyte recovery information to aid in assessing che accuracy of a result. This recovery Information, normally reported as percent recovery, glvee you information concerning the percent of surrogate etenderda and native analytes which wars recovered after adding to your sample matrix and performing che various extractions, elean-ups, and Instru mental analyses associated with tho datarmlnaclon. Tha use of sur rogates also assumes chat che spiked surrogstes are bound in the macrlx in the same way as tha analytes of Interest. Surrogate scandarda are added to every sample while native analytes era added Co only 10* of each sac of sample*. Therefore surrogate standard recovery data could be used to correct che reported results of an analyte concentration, if the user of the data feel such corrections era warranted. wnrn m dare reported in rMa .t-i.Mw to^i.wto correction for surreaaca standard recovery.___Tr t. rh taanonaihlllcv of the Person reouoarlne tho analyses to am.lv annrooriara racewerw corrections. If ha/aha fools that such corrections are warranted lias - Terminology used to describe how tha accuracy of a datarmlnaclon may be affected. A low bias naans that values below tha correct valua are normally measured. A high bias means chat values above tha correct valua are normally measured. Tha instrumental analysis stap of extract analysis normally does not contribute significantly co analysis bias. Host bias in environmental analysis is intro duced In tha saapla extraction stap. A lew bias is introduced when tha sample is not completely extracted and tha extract does not contain 100* of tha analyta. A high bias is Introduced whan the final volume of the extract is less than the correct volume. Surrogate Standards (SS), which ax* dlscuaaed in ch* next section, can be used to determine ch* amount of bias which is incorporated in eh* reported reeulc. WOTRH Wo data reported in this report includes anv correction for this bias.___It H tilt IIIWMmiln of tha parson raouastlns the analyses to SOPIt appropriate bias corrections, if ha/sha feels that such corrections are warranted. (conelnu*<i) HONS 024530 Page 3, Quality Aasuranee/Qualley Control Terminology Level of Detection (LOD) Terminology used to Indicate what analyte concentra tion will product a signal-to-nolse ratio of 10. For tho proaane report, this valua Is not experimentally determined, normally, a' Limit of Quantitation la uaed to determine the threshold concentre, elon above which an analyte can be detected. Limit of Quantitation (L0Q) - Terminology used to indicate the lowest analyte concentration which can reliably be quantified. The precision of the determination of the analyte concentration at the LOQ is normally on the order of 100%. The LOQ is normally determined experimentally by adding a known amount of analyte to the semple matrix and measuring the percent recovery at the LOQ. In some cases, when there la insufficient sample quantity, or for convenience, an LOQ will be determined using other methods. These methods should be clearly described in this report. Further Information The general area of Quality Assurance/Quality Control, along with much of the terminology described above, is very complex. The following references nay provide further information which may be useful in understanding the validity of the results reported in this study. ||Tf Ittndird B4110-I3 entitled "Intraleboratory Quality Control Procedures and a Discussion on tsporting Low-Level Data". amm ifwiarJ Fractlea B1777-77 entitled "Determination of Precision and Dias of Kathode of Committee D-19 on tfater". to artlei, " <-' authored by 29 mil-known environmental (Clantlaca. Thla artlcla waa funded by a (rant fron the Environmental Protection Agency and acknowledges 2A additional aelantlata In industry and (insurant who mra Involved In the review of tho article. Its citation is: -Principles of Environmental Analyele*. L. H. Keith, ec. el.. Anal. Chan. 1983, S3. 2210 - 2218. an rra Parr ill entitled "Guidelines Establishing Teat Procedures for the Analysis of Pollutants Under the Clean Water Act; Final Rule and Ineerla Final Rule and Proposed tula*. This docueent Includes details of EPA's 600-serlea analyele eathods. A current copy of those nothodo can bo found In tho October 28, 198A Federal Register. QAQCTE:MH HONS 024531 Analyte Extraction Terminology This (action describee cononly used terminology and phraeee which ara uaad In conjunction wlch analyte extraction. Thla Information nay ba halpful in undaratandlnf some datalla of how analytae In your samples ware laolatad for Instrumental analyala. Instrumental Analytic Terminologies ara glvan In tha following aactlon of thla report. Saapla - Terminology uaad to reference the naterlal which you tubalt for analyala. Samples aay be aolld, liquid, and In aoae caaea, gaaaa. In ganaral, when a sample la received for analyala, It la logged lneo the (SC aaaple login book and proper chain-of *cua Cody docuaenta ara maintained In the event thla Information aay be required for litigation purpoeee. Analyte Terminology uaad to reference (pacific compound! or fornulatione of eoapounda. When an analyala la requeated for a certain analyte within a certain (ample matrix, normally aoae type of extraction procoaa la required. Extraction - Thla terminology refara to tha atep which laolataa the analyte of interact into an appropriate tolvent. extraction la required for aeveral raaeona. In many caaea, the concentration of the analyte la below the level of decoction of tha lnatruwnc which will ba uaad for analyala. Iharefore, extraction involve! re moving tha analyte of lntareat from a relatively large volume of aanpla and placing It Into a relatively email voliaa of solvane. Thla placea tha analyte In the lolvenc at a concentration which can eaally be detected by the analytical Inatrumenc. A aacond reason that extraction la required, la that the aampla aay not be appropriate for direct lnatnmMntal analyala of the analyte of Interact. Thla can be eaally understood for analytes In soils. Very few analytical Instruments allow soils to be directly Inserted Into tha instrument. Therefore some type of isolation atop (1. a. extraction) la required in order to place the analyte la an appropriate matrix for Instrumental analysis. Whan tha analyte of Interest is present at sufficient concentra tion, and the sple matrix can be directly inserted lneo the analytical inatrumenc, the saapla, or the diluted aampla, can ba directly analysed. However, thla case raprasanes a minority of sample analyses which ESC is asked to perform. (continued) HONS 024532 ra| 2, Analyta Extraction Taralnology Matrix - Taralnology used to rofaranca eha aajor eoaponants of a sample. In oat caaaa, aajor components ara not of dlraet lntaraat except aa they affaet tha typoa of axtractlon atapa and othar laolatlon procaduraa which must ba uaad to laolata tha analyta froa tha aaapla aatrlx. For tha aajorlty of environmental aaaplaa which ISC la aakad to analyta, tha aatrlx la noraally watar or aoll. Howavar, aaoy environmental aatrlcaa contain relatively high lavala of organic eoapounda which aay lncarfor with tha Instrumental analyala of tha analyta of lntaraat. Tharafora, daponding upon tha analyta of lntaraat, tha required level of detection, and tha aaounta and typoa of othar organic aatarlala which aay lntarfar wlch the lnjtruaantal analyala, axtractlon aathoda auat ba davalopod which ara vary specific for a given tot of aaaplaa. In ordar to daal wlch alaosc a lialtlesa aac of aacrlcas, analytes, extraction aathoda and lnstruantal aathoda, an organized approach to aaapla extraction, followed by Instrumental analyala, haa boon davalopod at ESC. Extract - Taralnology uaad to Identify tha analyta-containing aolvane which waa obtained froa the extraction of a certain aatrlx. Extract Clean-up - Taralnology uaad to Identify chaalcal stops which ara required In order to reduce tha concentration of organic eoapounda which aay ba extracted with the analyta of lntaraat. Ihasa coextreecad eoapounda aay be at such high lavala and/or produce responses to that they lntarfar with tha lnseruaantal analysis of tha analyta In the extract. Ixtraetabla Coaqwunda - Taralnology which refers to eha ability of a coapound to ba Isolated froa tha aaapla aatrlx and placed Into eha extract solvent. When the aaaplo aatrlx Is primarily aoll which contains lltelo organic natter, aoat organic eoapounda are extractable com pounds. Howavar, whan tha aaapla aatrlx la primarily watar, only those eoapounda which ara hydrophobic ara extractable eoapounda. eaadard Extraction Method - Taralnology uaad to rafaranea an organized description of the stops Involved in Isolating an analyte from a given aatrlx, Thaaa methods ara assigned short names which can also bo uaad as computer file names for thaaa aathoda. The names of spocclflc Standard Extraction Methods which ara used In this study ara listed la tha final report In tha section entitled "Details". In addition, coplaa of thaaa Standard Extraction Methods ara shown In a separate section of this report. Standard Extraction Methods also Include details of aaapla clean-up. If required. Extraction Flew Sheet Terminology uaad to rafaranea a graphic daserlpeton of a Standard Extraction Method. This flow shoot la filled out by tha analyst In tha laboratory and aarvos aa a detailed record of what occurred In the aaapla axtractlon acap. Flow shoots of In dividual sample extractions aay be included in a secelon of this report. (continued) HONS 024533 Fag* 3, Analyte Extraction Ternlnololgy Surrogate Standard* (SS) - Ona laportanc alananc in tha extraction of an analyte fron a matrix, la ch* dataralnatlon of what parcanc of cho analyta was actually axtractad fron cho natrlx. For aathoda which Involve liquid/liquid axcraetlon of vacar with an organic aolvanc, or llquld/aolld axcraetlon of tolls with an organic solvent, It la Imperative that data b* obtained which glvaa ch* analyal* raquaacor lnfornaclon eonearning whac parcancag* of ch* analyta waa laolacad In Ch* axcracc during ch* axcraetlon acap. Surrogate Standard* sarva thla lnporcane purpot*. Tha philosophy on ch* uaa of Surrogac* Standard* Is as dlv*rss as eh* analyses who us* than. If cost war* no object, analyta raeovary lnfornaclon could b* obealnad by ch* ua* of atandarda addition analy sis method*. However. sine* nany sawplas require extensive labor co Isolate an analyta Into an extract, standards addition analysis methods ar* too costly for nose studies. (A standard* addition ana lysis requires each saapl* Co bo extracted and analysed at least thro* Class.) Surrogate Standards glv* th* saaa type of Intonation, with only ona analysts being required. A "Surrogate* Standard Is a coapound which Is chosen to bah*** exacely as tha analyta. It la a surrogate for Chat analyta and thus lnfornaclon obealnad for this surrogac* can b* asstasd to also apply to th* analyta of Interest. For the analysis of regulated analytes, It la inportent that when data Is generated that shows chat th* analyta la not presant, that w* can also show that It the regulated analyta were present In tha sample natrlx. It would have bean detected. This la especially true when coaplex extraction and lnatruawntal analysis steps ar* Involved In this determination Therefore, when an extraction is perforaed, a known anount of a Surrogac* Standard Is addad to th* saapl* before any extraction step* taka place. Whan ch* extract is then analysed for th* analyte of Interest, tha anount of tha Surrogac* Standard 1* also determined. Fron this lnfornaclon on* can docwant, for each sample, what recoveries were aaaaurad for this Surrogate Coapound. Froa this, one can dascrlb* sons level of confidence on the data genaraead for tha analyte of Ineereefc. A detailed discussion on how Surrogate Standards ar* chosen la be yond tha scope of this section on Analyte Extraction Terminology. SC normally use* two types of Surrogate Standards. Th* first Is when th* surrogate la exactly ch* sane as tha analyte of Interest, except that th* naturally occurring carbon, hydrogen, or halogen atoms In ch* analyte have boon replaced with non-narurally occurring laotopos. That* surrogac** can be expected co act exactly aa ch* native analyte*. One good oxaapl* of thla type of surrogac* Is the 2,3,7,8-TCDD surrogate In which all carbon acona ar* carbon-13 or all chlorine stoma are chlorine-37. (continued) HONS 02*53* Page *, Analyte Extraction Terminology The eond type of Surrogate Standard la ona which doaa not hava tha aaaa chemical atructura aa tha analyte of lntaraac, hue la known, or assumed to act cheeically Identical to tha analyte of lncaraat during tha extraction and clean-up atapa. Exaaplaa of thla type of aurrogataa are dautaraced compounds which aay ha addad to a matrix In which any ehromatographabla natarlala are to ba Identified. Thla approach can only ba applied Co GC/MS analyaea, a Inca the aurrogataa can bo differentiated from tha nadva coapounda from thalr dlffarant aaaa apactra. Since It la not known bafora aampla extrac tion and extract analyela what analytaa aay ba praaant, aurrogataa auat ba choaen chat could not poaalbly ba praaant In tha aampla. In addition, elnee only ltquld/liqutd or liquid/solid extraction would ba Involved, with no clean-up (alnca clean-up would rewove compounds In which the requester la Intaraatad) any hydrophobic dautaratad compound could aerve aa a aurrogata. Normally, phanol-dS. 2-CL-phanol-dA, CU-banxena-dA, pyrana-dlO and chryaana-dl2 are uaad aa Surrogate Standarda for the analyela of a wlda variety of hydro phobic natarlala In environmental ramplee. A eub-aet of thla aecond type of Surrogate Standarda are tha aurrogataa which are uaad In tha capillary OC/tC analyela of Aroclor fornulatlone. Since aaaa apaccroaatrle detection la not uaad, aurrogataa which contain unique laotopaa cannot ba dlatlngulahad from chair native countarparta. Therefore, other campounda are uaad aa Surrogate Standarda alnca they hava bean obaarvad to act exactly aa tha polychlorinated blphanyla (PCXa) in the Aroclor fornulatlone. Any halogenacad compound can ba uaad which acta exactly aa PCBa in tha extraction and clean-up atap. ESC normally uaea CU-benxena and 2,1,6-CL3-biphenyl for thla pur pose . Native Analytaa - Terminology which references tha analytaa of lntaraac which contain naturally-occurring Isotopes of carbon, hydrogen, halogans, ate. Native Spike - Terminology which refarancaa tha addition of a known amount of native analytaa to tha aampla aaerlx. Normally, at least ana sample will ba spiked with tha native analyte at tha reported level of de tection (law native splka) and sc 10 tinea the level of dataction (high native splka). Recoveries of tha nadva analytaa provide fur ther documentation on tha quality of tha analysaa performed. For aampla sacs which contain aora than 10 samples, tha frequency of low and high native spikes la 10% of tha number of aaaplas. (continued) HONS 02^535 Fag* S, Analyte Extraction Tirwinology Method Hank - T*mlno logy which refers Co a saapl* which 1* known to contain non* of eh* analyt** of lnc*r**c. for wacat analy***, chla 1* nor ally Burdick and Jackson Brand Water, da-Ionized, or dlatlllad ' watar. For aoll, It any b* toll which haa boon previously analyxad and known to contain non* of th* analyt** of lntaroat. All extrac tion atop*, using randomly selected glaaawar*, aolvanta, and all aurrogata spiking solutions Bust ba used. This provide* docuaencation that Ch* analyt** of lnesrosc v*r* not inadvertantly prosonc In axcractlon glaaawar* and aolvanta uaad In the analysis. A alnlaia of on* aaehod blank auat b* generated with each cat of >capias - for saapl* sacs containing wore than 10 aanplaa, aaehod blank* ar* gener ated at a frequency of 10% of th* nuabr of saapl**. Duplicate Analyses - Teralnology used to Indicate the duplicate extraction and duplicate extrace analysis of a saapl*. This provides docuneutlon on the precision of an analysis, (tonally the precision of environaental analyses of heaogeneou* saapl** Is on the order of 30%. A alnlaua of on* duplicate analysis Is required for oach saapl* sec. For saapl* sets containing aore than 10 saapl**, duplicate analyse* are generated at a frequency of 10% of the nuaber of saaples. Further Information The general area of Analyte Extraction, along with auch of Che teralnology described above, Is very coaplax. The following references aay provide further Intonation which aay be useful In understanding extraction fundsaental* and teralnology. *0 Ok Fart 13i entitled 'Guidelines Establishing Test Procedures for the Analysis of Pollutant* Under th* Clean Water Act; Final Rule and Incsrla Final Rule and Proposed Rule". This docuaent Include* details of EPA* s 600-aerles analysis aethoda. A current copy of chase aacbods can be found in th* October 2(, 1914 Federal Register. ItsMSMt at Work tr- '--tract Laboratory Froeren which la used In conjunction with CPA's Superfund Bite studies. A current copy aay be obtained by contacting: Joan F. Flak, Project Officer Analytical Support Branch Baxardous Response Support Division USEPA Washington, D. C. 20460 AHEXXE:HH HONS 024536 Instrumental Analysis Terminology Thla a ace Ion describes commonly used terminology and phraaaa which ara uaad In conjunction with extract analysis. Thia information nay ba helpful In understanding soma dacalla of how lnatruaantal analyaaa of sample extracts warn performed. Tha prawloua aoctlon of thia report daacrlbaa terminology aaaoclatad with analyta extraction. Sample Extract - Terminology uaad to deecrlbe tha solvent containing tha analyta of lntaraat which la obtained froa aoaa type of aaapla extraction atop. Detailed Information on how thia extract la pre pared can ba found In tha Standard Extraction Methods and flow ahaata aaaoclatad with tha aathods. Suaaarlas of thasa aatboda which ware used for this project can ba found In a separate section of this report. Internal Standard (IS) - Terminology uaad to reference a compound which la added to tha aaapla extract and atenderd solutlona of the analytes of lntaraat twalilatoly before lnatruaantal analyala. Tha purpose of tha Internal standard la to provide data which can ba uaad to correct for variations In lnjaccad volumes of extract and standard solutions which nay occur during lnatruaantal analyala. Tha Internal standard must not ba present In tha aaapla extract. Typical Internal standards uaad In aaaa apectroaetrlc analyaaa ara benzene-d6, naph thalane-dS, anthracene-dlO and chrysene-dl2. These deucarated compounds produce unique mass spectra and ara not present In naturally-occurring aanplsa. A coaonly uaad Internal standard for CC/IC analysis la hexachlorobenxens. Internal Standard Quantitation Method - Terminology which refers to a method of data analysis. This nathod requires chat a known amount of an Internal standard be added to the aaapla extract prior co Instru mental analyala. Responses of all analytes axe calculated relative to the Internal standard using the following relationship: Ut - Relative Response - (Analyte Area) ............................. -.............................. (Internal Standard Area) If different volumes of Che aaapla extracts and standard solutions are injected- these differences are reflected by differences In Che Internal standard area. In addition, If Instrument sensitivity changes, these changes are also reflected In changes In the Inter nal standard area. Tha calculation of the relative response cor rects for these types of fluxuatlona. In ordar to determine the analyte concantratlon-Ralatlve Response relationship, analyta Relative Response rectors ara calculated using the following relationship for data obtained from the analysis of standard solutions: (continued) HONS 024537 * 2. Instrumental Analysis Terminology (Internal Standard (Analyta Araa) Concantracion) RAF - Rslatlva Response Factor - .................................................................................. (Internal Standard (Analyta Araa) Concantracion) Whan identical Mounts of the Internal standard are added to both extracts and standard solutions, the Internal standard concentration tan In the above aquation can be eliminated. Whan this Is dona and Relative Response Is substituted for the ratio of analyte area to internal standard area, the RRF equation becones: RRF - RA/(Analyte Concentration) Analyte concentrations in the extracts are calculated fron the fol lowing equation: Analyte Kxtract Concentration - RR/RRF In order to obtain the concentration of the analyte In the staple, the following equation la used: (Analyte lxtract Concentration ) (Extract Voluae) Analyte Sample Concentration -........................ ................................................... (Aaount of Saaple Extracted) The area tens In the above equations nay be total Ion areas, FID peak areas, EC peak areas, or extracted Ion arena. The details of how the Internal standard quantitation aethod is applied to specific methods are described In the various instnseental Standard Analysis Methods. The following equation shows what calculations should be made to correct for analytical bias: (Analyte Saaple Concentration) Analyte Saaple Concentration - ................................................................ (Corrected for Analytical Bias) (Assumed Analyte Recovery) The Assisted Analyte Recovery can be obtained from an average of surrogate recoveries or native analyte recoveries, aeasured for the saaple In question. NOTH I No data reported in this study Include any correction for surrogate standard recovery. It Is the responsi bility of the person requesting the analyses to apply appropriate recovery corrections. If he/she feels that such corrections are warranted. External Standard quantitation Method - Terminology which refers to a aethod of data analysis. This aethod requires that a known aaount of the analyte standard be analysed under the seam conditions as the aaaple extract. In order to determine the analyte concentrationanalyte response relationship. Response Factors are obtained from the following relationship: (continued) HONS 024538 r*. 3. Instrumental Analysis Terwinology Rf - Response Factor - (Analyte Araa)/(Analyta Concsncraelon) Analyta concontraclona in eha axcraccs ara calculatad from tha fol lowing aquation: Analyta Extract Concantratlon - (Analyta Area)/RF In order to obtain the concantratlon of tha analyta In tha sample. tha following aquation Is used: (Analyta Extract Concentration) (Extract Voluna) Analyta Sanpla Concantratlon - ................................................................................ (Anount of Sample Extracted) Tha area tana In tha shore aquations nay be total Ion areas, FID peak areas, EC peak arose, or extracted Ion areas. Tha dacalls of how the external standard quantitation nachod la applied to specific nathods ara described In tha various instrumental Standard Analysis Nathods. The following aquation shows what calculations should bo suds to correct for analytical bias: (Analyta Sanpla Concantratlon) Analyta Sanpla Concantratlon - ------------------ --------------------- ----------- -- (Corrected for Analytical Bias) (Assuaed Analyta recovery) Tha Asswad Analyta Recovery can be obtained from an average of surrogate recoveries or native analyta recoveries, neasured far tha saapla In question. NOTE!I Ho data reported In this study Include any correction for surrogate standard recovery. It la the responsi bility of eha parson requesting the analyses to apply approprlaca recovery corrections, If hs/she foals that such corracelons are warranted. Standard Analysis nathods - Terminology usad Co reference an organised description of eha stops Involved In tha lnstrusantal analysis of a sanpla or a sanpla extract. Those nathods ara assigned short nanas which can also be used aa computer file names for those nathods. The nanas of specific instrumental Standard Analysis Nathods which ara used In ehis study ara Hated in tha final report In tha section antleled "Details*. In addition, copies of thesa Standard Analysis Nathods arc shown In a separate section of this report. Flow sheets of tha Standard Analysis Nathods era usually also provided In this section. Analysis Flew Shoot Terminology used to reference a graphic description of a Standard Analysis Nachod. This flow sheet gives specific Information on how extracts and standards ara analysed and what types of data reduction nathods are used. (continued) MONS 024539 Page 4, Instrumental Analysis Terminology Further Information The general area of Extract Analysis, along with such of the terminology described above* Is very complex. References provided In the previous section entitled "Analyte Extraction Terminology" nay provide further Information which may be useful In understanding Instrumental analysis fundamentals and terminology. INANTS:MH HOMS 024540