Document reNBEDBQvX707OOgEwagEBkvr

^ Monsanto SiEH/ESC HTo.7P1vT7DepC./Location) M <0 ec e to i *A S 8 * . ** ML nro l ui $i I& A 10MIAI Ana lysis (Type ot Report) REPORT HO.: MSL-S621 ESC-UA6-86-33 JOB/PROJECT NO.: 6603 OATE: April 26, 1986 TITLE: ANALYSIS OF GREASE AND HATER SAMPLES FOR PCBs AUTHORS: B.M. Hughes, D. McKenzie, end C. Trang ABSTRACT: Hater samples and one grease sample from the World Headquarters were analyzed for PCBs. No PCBs were detected with water levels of detection of 0.01 pg/g and grease level of detection of l ug/g. TECHNICAL APPROVAL: r.i: Sherman Environmental Sciences Center Senior Research 6roup Leader APPROVED BY: ff.M. Mees Environmental Sciences Center Quality Assurance Specialist APPROVAL DATE HONS 02*006 COMPANY CONFIDENTIAL Thia document it the property of Monsanto Company and the recipient it responsible for its safekeeping and disposition. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorised persons or sent outside the Company without proper authorisation. DISTRIBUTION COPY NUMBER 1, M. Arnold - R3B 2. B.H. Hughes - U4E 3. 0. HcKenzIe - U4F 4. C. Trang - U4F 5. P.l. Shernan - U1F 6. W.M. Hees - U40 7-9 Reports Library - R2C 10. Chesterfield Information Center - AA3A ABSTRACT ONLY H.A. Wo Hermann - U4E This report has been assigned to you. When it is no longer needed, you art responsible lor reluming it to: c If you transfer it to anyone else, please let your librarian know, so the records can be changed. ItirOlMv !/! MOHS 024007 Time Stamp <860512.1434> I ANALYSIS REPORT DATE: April 24, 1986 LOG NUMBER: U-86-02-03-01 PROJECT NO: 760.28-6603 TO: Mike Arnold (WHQ Safety) FROM: Environmental Sciences Cancer Monsanto Company 800 N. Lindbergh Blvd. St. Louis, Mo. 63167 Phone No: (314) 694-1464 Title: Analysis of Grease end Veter Saaples for PCBs ABSTRACT Veter saaples end one gTeese sample fron the Vorld Headquarters were analysed for PCBs using capillary CC/EC analysis aethods. No PCBs were detected with water level of detection of 0.01 ug/g and grease level of detection of 1 ug/g. INTRODUCTION Four water saaples and one grease sample were analyzed for PCBs. No PCBs were detected with water level of detection of 0.01 ug/g and grease level of detection of 1 ug/g. Standard Extraction Methods VSEX05 and PCEX21 were used for sample extraction and Standard Analysis Method ECAN02 capillary CC/EC aethod was used for extract analysis. SUMMARY Table 1 summarises the results obtained from the analysis of four water saaples and one grease aaaiple for PCBs. Note that no samples contained PCBs with levels of detection of 0.01 ug/g for the water samples and level of detection of 1 ug/g for the grease sample. QC RESULTS Tables 1 and 2 contain QC results for this project. All samples were spiked with CL5-benzene and 2,4,d-CL3-blphenyl before extraction. Recoveries be tween 68 and 1131 were measured for these two compounds. Table 2 contains QC results froa the spiking of the Saaple 2 grease sample and the Sample 5 water sample with 10 ug/g and 0.05 ug/g, respectively, Aroclor 1248. This data shows that if these levels of Aroclor 1248 or other Aroclor forumlatlons were present In the water and grease samples, they would be properly detected. (continued) HONS 024008 Pag* 2, A60318 DETAILS Standard Sampling Method No(s): Samples supplied by Mike Arnold, VHQ Safety. Standard Extraction Method No(s): VSEX05 and PCEX21 (Also see flow sheets WSFS05 and PCFS21.}or Standard Analysis Method No(s): ECAN02 Final Report File No(s): A60318 Table File Ho(s): 860318, C60318 Also Included In this report are: 1) Summarise of Standard Extraction and Analysis Methods used. 2) Analytical Request Information recorded at sample login. 3) A copy of the UAC/CLP manual. ANALYST(S): B. Mason Hughes, David McKensl* and Chi Trang ANALYSE APPROVAL: HONS 024009 TABLE 1. Suanary of fCB Concentration. Water and Creaaa Saaplai using Standard Analysis Method ECAN02. ESC Frojact No: 760.2B - *603 Sample t.D. Surrogate Recoveries(tRecovery) CL5-benzene 2.4,6 CU-biphenyl Sample 1 " (DUP.) 79 82 79 82 Data: February 26, 16 Extractioni PCB Method Coneantratlon (ug/g) Total WSEX03 ' NDl(a) " Sample 2 - (DUP) 71 n 91 93 pcExn ND2(b) * Semple 3 Sample 4 113 87 113 91 WSEX05 NDl(a) Sample 5 103 110 Method Blank 98 100 Footnotaa: a. b. ND1- Nona Detactad (<0.01 ug/g) ND2- Nona Datactad (<1.0 ug/g) TABLE FILE NO: B031B:MH * HONS 024010 TABLE 2. Suauaary of Aroclor 1268 Spiking Concentration! and tienulu In Quality Conttol Experiment! for Water and Creaaa Sanplea. ESC Project No: 760.2$ - 6603 Date: Februery 26, 19$6 Sample I.D. Surrogate Recoverlea (tRecovery) Aroclor 1268 CL5-benzene 2,6,6-CL3-Blphenyl .................................................. Sampl* 5 <H. Spike) 68 70 Amount Added Recovery <"8/S> () 0.05 160 Sanple 2 (H. Spike) ss 106 10.00 68 Method Blank 87 TABLE FILE NO: C60318:KH 90 ND ND MONS 024011 Tha following pagaa daacrlba Standard Sampling, Extraction, and/or Analyala Mathoda uaad for thla projact. MONS 024012 ESC Standard Extraction Method (SEM) TITLE: Vide scan extraction method for veter. MATRIX: vater ESC Standard Extraction Method*No: VSEX05 TYPICAL SAMPLE SIZE (Liters) TYPICAL EXTRACT VOLUME <1) 0.01 - 4 1 - 40 TYPICAL ANALYTES: Aroclors, PCBs, priority pollutants ESC Standard Analysis Method Nos: ECANxx and MSANxx INTERFERENCES: Various; See individual Interferences for Individual analytes. TYPICAL SURROGATES TYPICAL RECOVERIES (%) phenol-dS 20-80 CL-phenol-d4 20-80 CL?-bensena-d4 50-120 naphthalene-d8 50-120 I pyrene-dlO 50-120 chrysene-dl2 50-120 pontachlorobsnzene 50-120 2,4,6-trlchloro- ; blphanyl 50-120 APPARATUS AND MATERIALS: Burdick and Jackson methylene chloride Separatory funnel* Sodium sulfate for extract drying Sodium hydroxide and sulfuric acid for pH adjustments Nitrogen for extract volus* reduction Water bath and K-D apparatus for extract volume reduction LIMITATIONS: Sufficient eample amount to provide CC-MS LOD. SAFETY PRECAUTIONS: Saa Safa Laboratory Practices. DATES OP METHOD CREATION AND UPDATES: 5/16/84, 10/5/84, 12/7/84 HONS 024013 FLOW SHEET VSFS05 FOR ESC EXTRACTION METHOD VSEX05 SAMPLE ID: .............................................................................. MRC EXTRACT #............ .............................................................................. LOG NO: .......................... EXTRACTION DATE and TIME: ....................................................... /................................... RECORD NATIVE pH..................... WAS pH ADJSTED YES/NO IF YES TO WHAT pH PLACE SAMPLE INTO AN APPROPRIATELY SIZED SEPERATORY FUNNEL (] (1/2 HEAD SPACE SUGGESTED FOR ADEQUATE MIXING) t] SAMPLE VOLUME ......................................... SURROGATE SPIKE ............................................................................. IF pH ADJUSTED ( ) ADJUST WITH,50% NaOH OR H SO 24 ADD METHYLENE CHLORIDE IN ( THE APPROPRIATE AMOUNT (1 L SAMPLE 30 L SOLVENT, 100 ml. SAMPLE 15 bL SOLVENT) ) SHAKE SAMPLE ONE TIME [ AND VENT THROUGH STOPCOCK REPEAT DOUBLING THE NUMBER OF SHAKES BETWEEN VENTING SAMPLES UNTIL THE NUMBER OF SHAKES EXCEED 80 1 RECORD AMOUNT METHYLENE CHLORIDE ADDED FOR EACH EXTRACTION i i M/ i)......................... 2)......................... V 3)......................... OBSERVATIONS AUOW PHASES TO SEPARATE (i ........................................................................... REPEAT EXTRACTION PROCEDURE TWO MORE TIMES IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT. [ ii] [] . ........................................................................... ACID/BASE WASH COMENTS DRY EXTRACT WITH A INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 bL METHYLENE CHLORIDE) ( .[ ] EXTRACT DRYING NOT REQUIRED RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL { ) ' REDUCE EXTRACT VOLUME TO l aL BY K'D TECHNIQUE AND OR NITROGEN SOLVENT VOLUME REDUCTION [ ] ' [ ] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS EXTRACT NO: ..................................... DATE/TIKE COMPLETED........................../....................... ANALYST: ESC JOB NO: HONS 0240IA ESC Standard Extraction Msthod (SEH) TITLE: PCBs in Non-EC Active Matrices ESC Standard Extraction Method Nor PCEX21 MATR1(X),(CES): Soils and other non*EC active solids and solvents TYPICAL SAMPLE SIZE (S> TYPICAL EXTRACT VOLUME <!) TYPICAL ANALYTES: Atoclors 1232, 1242, 1248. 1234. 1260. 1262. trichlorobiphenyl Isoaers through octachloro* biphenyl Isoaers 0.5 - 5.0 10 ESC Standard Analysis Nachod Nos: ECAN01, ECAN02 INTERFERENCES: Any electron capturing species in the retention tlae region of triehlorobiphenyl lsosers through octachloroblphenyl Isoaers that Is non acid hydrolyzable TYPICAL SURROGATES TYPICAL RECOVERIES () pentachlorobsrusne 2,4,6'trlchloro'* biphsnyl SO - 120 50 - 120 APPARATUS AMD MATERIALS: Burdick and Jackson benzene or hexane for suple extraction or dilution. Pierce vials. Sulfuric acid at varying concentrations. Ultrasonic beth. Disposable glassware. (See flow sheet for this extraction aathod in PCFS21.) LIMITATIONS: Method applies only to aatrices which do not contain Interfering electron capturing species in the triehlorobiphenyl through octechloro* biphenyl lsoaer retention tlae region. SAFETY PRECAUTIONS: See PCB handling protocols in laboratory aafety aanual. DATES OF METHOD CREATION AND UPDATES: 12/17/84 HONS 024015 FLOW SHEET PCFS21 FOR ESC EXTRACTION METHOD PCEX21 SAMPLE ID: EXTRACTION DATE and TIME: - SAMPLE COLOR AND DESCRIPTION MRC EXTRACT * LOG NO: ............ WEIGH OUT SAMPLE INTO A 14 OR 40 aL PIERCE VIAL (] . SAMPLE WEIGHT SURROGATE SPIKE OF SAMPLE . [) ADD 10.0 aL BENZENE TO SAMPLE. . [] ULTRASONICATE SAMPLE FOR 1/2 HOUR IN A SOUND BATH. (] . . PLACE 2 bL OF THE EXTRACT INTO A 7 aL VIAL % ADD 2 bL ............ SULFURICACID AND SHAKE . () . . (1 . . ALIOW PHASES TO SEPARATE REMOVE 1 aL FOR ANALYSIS. [] EXTRACT NO: .............. DATE/TIME COMPLETED ANALYST: ..................... ESC JOB NO: 10.0 aL FINAL VOLUME ............................ *QHS 024016 ESC Standard Analysis Mathod (SAM) TITLE: Aroclor Formulation* In Solvents ESC Standard Analysis Mathod Mo: ECAN02 ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-3680 Capillary CC/EC inter faced to an HP-3357-LAS Laboratory Data Syataa TYPICAL ANALYTE TYPICAL INSTRUMENT LEVEL OF DETECTION (LOD) (ug/ml) Aroclor formulations 1232. 1242. 1246. 1254. 1260, and 1262 0.1 TYPICAL PRECISION 10X LOD <%> 30 TYPICAL ACCURACY 10X LOD <%) 30 INTERFERENCES AND LIMITATIONS: Any alactron capturing apaclaa In tha ratantlon tla region of trlchloroblphanyl through octachloroblphanyl isomers ara potantial Intarfarancaa. Exact ratantlon tlmaa of moat llkaly PCS isomer* can ba abtalnad from tha analysis of Aroclor 1248, Aroclor 1234 or Aroclor 1260 formulations. CHROMATOGRAPHIC COLUMN: 30-matar fused silica J&W DD-5 (0.23 uM> with vide bora (0.32mm). COLUMN TEMPERATURE PROCRAM: 130(l)/4/300 INJECTION TYPE: Splitlass CAL1RRATX0N AND STANDARDIZATION: Usa intarnal standard quantitation tschnlqua and callbrata Instrumant raaponaa factors from authantlc Aroclor formulation standards. Uso a minimum of 10 PCB Isomers for tho detsrmlnatlon of foreulatlon identity and quantity. CALCULATIONS: Formulation coneantratlon (Isomer RRF)(Isomer area/internal standard area) where: RRF la tha ralatlve response factor for tho appropriate PCS Isomer In a given formulation. Formulation concentra tion la obtained from the average of at least 10 such cal culations. SAFETY PRECAUTIONS: See PCB handling protocols In laboratory safety manual. DATE OF METHOD CREATION: 10/25/83. 2/3/84 Time Stamp - <860424.1507> HONS 024017 Tha following pagaa daacrlba Analytical Raquaat Information ganaratad for thla projact. HONS 024018 Time Stamp <860424.1507> MONSANTO COMPANY/ENVIRONMENTAL SCIENCES CENTER ANALYSIS REQUEST DATE: 2-3-86 LOG NO: U-86-02-03-01 REQUESTER: ResCent Safety-Arnold PROJECT NO: 760.28 - 6603 REPORT RESULTS TO: F1LES/HEES, HUCHES, SHERMAN ANALYSIS REQUESTS SENT TO: FILES, MEES, SHERMAN, HUGHES SAMPLE PICKUP BY: McKenzie SAMPLE LOCATION: U-420 SAMPLE DESCRIPTION FOR S SAMPLES SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC (a) NUMBER(S) NBP 3333215 Sample #1 Crave Coeur Basin water 1 x 40 mL <b) NBP 3333213 Sample #2 Crave Coeur Batin gratae 1 x 40 mL Method Blank NBP 3333215 Sample 3 Crave Coeur Batin vater NBP 3333215 Sample #4 Crave Coeur Batin water 1 x 40 mL 1 x 40 ml PCB-1336 PCB-1537-DUP PCS-1544 PCB-1545-DUP PCB-1546-LS PCB-1547-HS PCS-1548 PCB-1538 PCS-1539 4 LS PCS-1540 NBP 3333215 Sample 5 Crave Coeur Batin water 1 x 40 mL FOB-1541 PCS-1542 4 HS Footnotet a DUP refera to duplicate analyte#, LS refert to a low level native aplke, and HS refer# to a high level native spike. b - Sample 2 was a grease sample while the other samples were water samples. It required a different work up procedure ao a complete aet of quality control staples (DUP, LS, HS and method blank) were Included in its analysis. RECORDED BY: McKenzie REQUIRED ANALYSES: PCBs ANALYTICAL TECHNIQUES: TECHNIQUE (EN) DATE COMPLETED TECHNIQUE(EN) DATE COMPUTED X GC/EC (It) 4/24/86 QUALITATIVE: x SEMIQUANT1TATIVE: REQUIRED QA/QC: SEE GOOD LABORATORY PRACTICES MANUAL QUANTITATIVE: x COMPLETION DATE REQUESTED: HONS 024019 COMMENTS: SAMPLE DISPOSITION: HOLD FOR JO DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME: AB603:LI MOWS 024020 Ih Manual. following it copy of tho ESC/UAC Good Uborotory Practices HONS 024021 Copy Number: COOD LABORATORY PRACTICES MANUAL A Culde toQuality Control/Quality Assurance Ultratrace Analysis Group March 19S4 paepB J. Er Group Leader Ultratracc Analyala H. A. Woltermann Manager, Environmental Sclencca Center laaued tot ________ Date .____ __________ JR3/J01 A Environmental Sciences Center Dayton Laboratory Deyton, Ohio 45407 MONS 024022 TABLE OF COKIEMTS I Objective* 11 Scop* 111 An*ly*la A. Method* . QA/QC Frogrem 1. Spl* Trcparttlon QA/QC *. Method Henke b. kepllcete* c. Spike* 2. Instrumental Analyela QA/QC t. Inatrumentatloo b. llenk* c. Quentltetlon Internel Stenderd d. Stenderd* C. Detree* of Quentltetlon 1. Quelltetive Analyele e. Tentetlvc b. Confined 2. Seml-Quantltatlve Analyela 1. Quantitative Analyela D. Quality Crlterle end Renedlel Action 1. Quellty Crlterle e. Slenke b. Recoveries c. Preclelon d. Limit of Detection e. Accurecy 2. Remedial Action IV Dete V Senple Dlepoeel FIGURES Figure 1 txenpl* of CC/MS Logbook peg* 2 Example of SC/EC Logbook peg* 3 Example of Dl*c/Tape Logbook page f*l ] l j I 2 2 2 2 2 3 3 4 4 4 4 7 7 7 7 7 S g g g g 9 9 9 9 10 pt* 5 6 11 HONS 024023 I. Objectives Th main objectives of the Ultratrece Analysis Group quality assuTance/qumUty control program are: 1) to aaaurt that our laboratory generates high quality rtaulta; and 2) to maintain tha otctaaary racorda that document laboratory performance. II. Scope Tha acopa of thle manual Includaa araaa of CLP oot epedflcally addraaaad in tha ESC aection manual and expanda upon certain araaa where QA/QC practlcaa differ from thooe daacrlbad in tha aection nanual. It ia intended to ba uaad along with tha taction nanual to provide a complete picture of the CLP within the Ultratrace Analytic Group. in. Analysis Tha generation of analytical raaulta withlo the Ultratraca Analytic Group routinely lnvolvet two procataaa: temple preparation and Inetrunental analytic. Semple preparation lnvolvet one or more of a variety of teehnlquct Including extraction, dilution, acld/baee vaahee, column chromatography, concentration and nuneroue other technlquet to render the temple ia a tultable condition for lnttrumental analytlt. Inatrunental analytlt taken the tultably prepared tample and introducet it into an analytical Inttrument to meaaure the detired parameter(t). Both of theae procettet can be detcribed by clearly defloed and teparable metSoda called cample preparation matboda (SPMe) and inatrumental ahalyela mathoda (XAMa). SPKa and XAMa may be combined In nuneroue waye (depending upoo the nature of the samples and the needa of tha customer) to produce a successful analytical protocol. Por example, several different SPMe nay be used to produce camples that are suitable for analysis by a single 1AM. Tha measures incorporated into each of theae experimental proceaaea to ensure that an assessment of the quality of tha results can be made constitute the QA/QC program for a project. The following subsections describe the eleaeots of the analysis process: A. Methods Methods are the written documentation that describe the analytical process. They contain sufficient detail such that a competent dentist or technician can readily perform the required analyses. The usual practice la to have methods that describe the sample preparation process (SPMe) and mathoda that describe the Instru mental analysis process (lAMs). Each method developed within the Ultratrace Analysis Groups la assigned a method number as described in the ESC Section Manual. Methods are obtained from various sources including in-house develop ment, modification/adaptation of literature methods, or specific protocol methods dictated by government agencies. Methods may be formally validated by a series of experiments that describe a classical validation protocol or may be leas vigorously proven owing to factors such as frequency or use, customer needs and 1 MOMS 024024 coat/tlalng restrictions. In any cist i QA/QC prograa 1* applied to tbs analysis process to provlds a asasurs of tha quality of the rssults. Unless a QA/QC prograa Is prescribed by a required protocol (e.g., EPA Dioxin In Soil protocol), certain alnlaua QA/QC Beasures (depending upon the analysis type) are Incorporated Into all Ultratrace Analysis projects. The following aubtectlon describes the Ultratrece QA/QC prograa: QA/QC Prograa An affective QA/QC prograa Incorporates experlaenta that provide Information relative to each of the following questions: (1) Are there any iapurltles, background or contaalnatlon that will Influence the results? (2) Row reproducible are the results? (3) How well can the analyte be recovered froa the saaple aatrlx? (A) What Is the Halt of detection for the analysis? (S) What la the dynaalc range of the analysis? (i) What la the accuracy of the analysis? All of these questions are addressed by properly sclectlng/applylng the use of blanks, repllcatas, spikes and standards In a QA/QC prograa. The discussion of the use of these QA/QC techniques at they apply to Ultratrace Analysis Croup activities Is best done by considering the saaple preparation and lnstrtaental analysis processes separately. 1. Saaple Preparation QA/QC a. Method blanks - Representative glassware, solvents and reagents are used with saaple aatrlces which are slallar to those for which results are being reported, yet do not contain the analytes of Interest. Method blanks are analysed at a frequency equal to 10X of tha analysed Saaples for saaple sets which are aultiples of 10. At least one aetbod blank Is analytad for sample sets containing between 1 and 9 saaples. b. Replicates - If sufficient saaple amounts have been eubaltted for analysis, replicate frequency Is the ease as tha aethod blank frequency. If at all possible, replicates should be obtained from the saae saaple bottle In order to alnlalte aaaple lnhoaogenelty problems due to saaples being taken at slightly different tlaee. c. Spikes - If sufficient saaple Is available for each saaple type, the saaple Is split and spiked at two levele with 2 HONS 024025 th* native (unlabeled) analyte(e). The levela are typically 2x (lov) and 2Ox (high) tht anticipated detection llnlt and aerve aa a technique (or eetlaatlng the Halt of detection for each aatrlx. Theae low and high aplkea are conducted at a frequency equal to the Method (lank frequency. Obvlouely eplklng with the native analyte cannot be done for vldeecea anelyete alnce thla preauppoeee knowledge of the Identity of the analyte(a) In the eaaple. Other eplklng technlquee are ueed to evaluate the extrac tion/recovery efflclenclee for the analyte(a) of lntereet. Ideally extraction/recovery efflclenclee are deteralned for each eaaple, alnce, in principle, each eaaple nay repreaent a different aatrlx. Thla can be done very eaelly when the detection technique la aaaa apectroaetry If an leotoplcally labeled veralon of the analyte(a) la available. Docuaentatlon of extractlon/recovery efflclenclee la not required for each eaaple If the eaaple aatrlx for a eat of aaaplea la conetant. However, for a eaaple aet for which the alallarlty of aaaplee la not known, and for which adequate aaaple la available, each eaaple auat be apllt and aplked with a known aaount of the analyte(a) of lntereat to determine extraction efficiency. If adequate aaaple alae la not available or the Identity of the analyte(a) la not known before the fact (l.e., wideecan analytic), aurrogate eplklng compounda nay be uaed to aaaeaa extraction efflclenclee In each aaaple without actually eplklng each aaaple with the analyte(a) of lntereat. The choice of the aurrogate eplklng compound la tailored for each analyte. Thla aurrogate auat be choeen ao that It la either ehealcally Identical to the analyte of lntereat (for exaaple ualng leotoplcally labeled analoguee of the analytea), or la cloeely elailar In terme of llquld/llquld partition propertlea, chemical reaction propertlea, column elution propertlea or other aatrlx 1eola tion propertlea which are uaed to laolate the analytc(a) froa the aaaple aatrlx. Another property of the aurrogate eplklng compound la that It not be preaent In the aaaple being analyied Inetruaental Analyela QA/QC The final atep In obtaining analytical reaulta lnvolvea the uae of an appropriate Inetruaental technique to produce the analytical data Saveral QA/QC practiced auat be Incorporated In thle precede to enaure validity of the data. a. Inetruaentatlon . Careful docuaentatlon of lnetrtatent uaage, calibration, and aalntenance la eaaentlal for the generation of high quality reaulta. Each aajor lnatnaent within the Oltratrece Analytic Croup will be the aealgned rcopooelblllty of a profeeaional employee deelgnated aa the Inetrwent Steward. The lnetriMent Steward la reaponelble for making aura that logbooka are availeble and properly coapleted by lnetruaent uacra. It le the 1 HONS 024026 responsibility of each individual uln| th equipment to rteotd all tha pertinent data required In tha logbook, in example of a gaga fro* a GC/MS logbook la glvan In rigura 1 and that of a GC/EC logbook la glvan In Figure 2. Instruments will ba callbtatad according to tha lnstruant manufacturers' specifications or according to tha mathod balng uaad with tha lnatrtaaant. A log of Inetrunant calibration will ba nalntalnad with tha Instrument. Tha InatruacnC Stavard will ba raaponalbla for anaurlng that preventative and corractlva nalntananca programs art carrlad out on all lnetrtaente undar hla/har rcaponalbll1ty. If a specific problem la notad by an inetrtmnt user, It ahould ba notad In the logbook and tha lnatruaant Steward notified ao that appropriate corractlva action can be taken. b. Slanka A advent blank will ba analyaad at a frequency equal to the aethod blank. The aethod blank can aerva aa tha aolvent blank provided It la clean In tha area of tha analyte(a) of lntaraat. Thla practice ellalnatea tha poaalblllty of background Instraaental contamination. c. Quantitation Internal Standard A quantitation Internal atandard will ba added to each aampla following aampla preparation but prior to Inatrumental analyeia. Thla compound will aerva for determining relative raapooaa factora and for correcting for verlatlooe In aampla injection voltacs and evaporation of aolventa. d. Standarda Standarda ara aolutlooa of tha analyte(a) of lntaraat uaad to determine tha reoponee of tha detector over tha range of analyte concentTat Iocs found In tha eamplee. Tor Quantitative analyses. eufflclent standards and replication of standards will ba run to demonstrate linearity and precision of tha detector response over tha range of analyte concentrations. Should sample concen trations fall outside the demonstrated linear range, either additional standarda are prepared to expand the range, or appropriate dllutlon/concsntratlon of the sample la done to place It In the proper range. Degrees of Quantitation The Information provided for any particular analysis la tailored to the needs of the customer. In actual practice these needs vary across the broad continuum from the grossly qualitative to the precisely quantitative. It la Informative to examine what la Involved In providing the varying degrees of quantitation required by our customers. 4 AQNS 02402 7 HP 5985A ton_ kuttNi_ . __ MUtottoMilltol ha . .. ... toil. . .. MftCDA Mf IUM HONS 024020 HPS68 Gt/ffC in_ MMNI____ - - --- MftCDA Nf inn; NCUM 7. of GC/MC l*feook HONS 024029 1. Qualitative Analyela Qualitative analyela lapllee no quantitation at all but rather eeeke only the Identity of the compound(a) prevent. CC/MS la particularly applicable to thin type of analyelo problen. Two typee of ldentlflcatlona can be nade: a. Tentative A tentative Identification la nade on the baele of the analyot'e Judgement of a natch batwean the naaa epectrt* fron the aaaple and a naaa apectrua froa a reference library. Thia la often done for the large number of coapounda found In a wldeacan organic analyela. b. Confined A confined Identification requlrea that the ehroaatographlc retention tine and the naaa apectrua of the unknown compound natch tboea of a known atandard of the tentatively Identified conpound Thin la often done in wldeacan analyaea when etandarde can be obtained for tentatively Identified coapounda that are of concern. The nonal QA/QC raqulraaenta for qualitative analyela are (1) analyela of a blank. (2) analyela of duplicate aaaplea and (3) aac of a calibration compound (oaually Decafluorotrlphenylphcephlne, PTOP) to nature that the aaaa apectroaeter will produce aaaa apectra that can ba coapared with library apectra. 2. Seal-Quantitative Analyela Seal-Quantitative Analyela extenda the Information provided by a qualitative analyela to Include aoae eetlaate of the amount of analyta(a) praeent. The aethod of aeal-quantltatlon lnvolvea the coaperlaon of detector reaponae of tha analyte(a) with that of an Internal atandard. Tha aetlmated concentration la obtained by eeeualng a unit reaponae factor between the aoalyte(a) and the internal etandard(e). An Indication of recovery from the aaaple aatrlx la obtained froa the recovery of the aurrogate Internal atandard(a). 3. Quantitative Analyela Quantitative Aaalyala provldee for the accurate aeaceeaent of the amount of analyte(a) preaent In a aaaple. To be able to do quanti tative analyela one aunt know the Identity of the analyte eo that atandarda can be prepared for eplklng and for the generation of calibration eurvee. The aethod of quantitation la baaed on a three-point calibration curve ualng atandarda of tha aaalyte(a) of internet over the range of concentratloae In the aaaplea. A onepoint calibration aethod can be uaed (aa with the laboratory data 7 HONS 024030 eyeten) provided that linearity baa been deaooatrated over the concentration range of the aanplee uelng ttandarda of the analyte(a) at three concentratlone In the rente. Thle calibration curve la then need to provide concentratlone of the analyte(a) la the aanplee via an external atandatda nethod or nore preferably via an Internal atanderda nethod. for the Internal etanderda nethod, the quantita tion Internal etandard la added to eech of the etandarde (juat aa with the aenplea) prior to lnatruncntal analyale and relative reeponae factora are determined. For quantitative analyale the naaa epectrooeter la operated aa a tea chromatogrephlc detector. The KS la therefore tuned and operated In a nanner apecifled In the approved nethod rather than uelng a calibra tion conpound aa required for qualitative anelyeea. D. Quality Criteria and henedlal Action Tba lnclueien of QA/QC ncaeuree Into an analyale prograa baa little neanlng unleae the reaulta are Interpreted and appropriate action la taken when neceaaary. The ability to do thle aaaunea none act of criteria that will trigger a reeponae or rencdlal action. The following aubaectlona deacrlbe the criteria that are uaed In the Vltratrace Analyale Croup to evaluate when quality control data Indicate e need for corrective ncaeuree and what remedial action will be taken. 1. Quality Criteria The overriding quality criterion above all othero la: Op the reaulta neet the needa of the euetoper. Thle determination will be made jointly between the euatoner and the analyet. The analyat nuat exerclae caution In not allowing the euatoner to overetate, nlelnterpret or unintentionally nlarepreaent the data. In addition to thle prlne quality criterion, the following eondltlona nuat be net: e. Slanka - In the event that a blank producea a poeltlve value. It nay not be uaed aa a valid blank If It exceeda 101 of any reported value for a aanple. b. lecoveriee - kecoverlea for all aurrogate and native aplkee nuat lie In the range of SOX<kccovery<l SOX. c. Freclalon - Freclalon will be calculated baaed on the recoverlea of aurrogate Internal atanderda. Average recoverlea will be calculated with t atandard deviation for each aanple aet. hepllcate analyeca and low and high native aplke recoverlea nay alao be uaed to provide additional lnformatlon/lnalght Into the preclelon of the analyale. HONS 024031 S d. Limit of Detection - The Unit of detection (U) vlll normally be ototed at *i the value of the low level native spike If It la recovered and quantifiable. Should the low level native spike not be recovered, the LOD will he atated aa >1 the value of the high level native spike If It la recovered and quantifiable. Should neither spike be recovered, a decision oust be Bade retarding the advisability of reprocessing tbo aaaple. Should all aauplea contain such large quantities of the analyte(s) that the levels of the lov and high spikes are insignificant (<10Z) by comparison, the value of the LOD becoues lees important and la sleply stated as the LOD for the Instrumental analysis process deternined by the analysis of standards and the ability to recover the surrogate spikes. e. Accuracy - The accuracy of the analyses Is best determined by analysing some aaaple uhleh contains the analyte at some predetermined level (e.g., an IDS standardised aaaple). If this type of standard Is not available then the lov level and high level spikes can be used as a aeaaura of the accuracy of the enelyses. kesulta oust fall vltbio a range of 75X to 1201 of the excepted value for the analyses to be considered valid. If the above quality criteria are not met the analyst vlll Immediately assess the need for and extent of remedial action that may be necessary. 2. Kemedlal Action . The first course of action vlll be for the analyst and/or group leader to contact the customer and discuss the results pointing out the limitations of the data Indicated by the quality control results. At this point the overriding quality criterion of customer needs vlll be addressed first. It could be that the customer's needs are net vltbout meeting one or more of the other criteria. In such a case no remedial action la necasaary. It could alao be that the customer has such a demand for tightness la the results that hla needs are not met even though the other quality criteria are. This vould trigger further analyses vlth tighter quality control designed around the results obtained (e.g., replications of positives to better establiah precision or aplkea of aon-detected samples to better asteblish the Halt of detection). In consultation vlth the customer additional experiments vlll be designed Including the appropriate quality control to ultimately provide the results of sufficient quality to meet the customer's needs. IV. fte This section deals vlth the subject of data and hov they are obtained, recorded and reduced so as to be useable In a report and yet readily available for referral and Inspection. . HONS 024032 9 The eamplea vlll be labeled with t log number at eample login according to tha procedure daacrlbad In tha ESC Sactloo CLP Manual. Whan daltvarad to cha raaponatbla tachnlcal paraon, tha eamplea way than receive additional labeling aa datnad aacaaeety. Thla additional labeling will be documented In a laboratory logbook and/or notebook. Theae logbooka and notebooka will ba uaad by tba analyata to record all pertinent work and raaulta obtained froa tba aaaplaa. The laboratory notabooka will ba filled out In accordance with Honoanto Uniform notebook Froceduree. All raw data generated for a given project, which cannot be conveniently placed In tha laboratory notebook (e.g., chromatograaa, computet output, etc.), will be filed under none preecrlbed order (l.e., log number) In a central file under tha eupervlaon of tha Project Leader and/or QA Speciallet. Moat of the data generated by tha Ultratraca Analytic Croup are computet data atorad on negnetlc dleco. In order to archive thane data the apeclfic file name and dlec Disbar aaaoclated with the analyala will be written down In the laboratory notebook and/or lnetrisent logbook. Whan tha dime la completely full of data an entire unedited dlec Image or copy of the fllea on the dlac will be tranaferred to magnetic tape. A logbook will ba kept for recording the dlac nisber, name and prefix aaaocl ated with It, along with the aaaoclated tape and file usher to which the dlac waa tranaferred. An example of auch a logbook la given In Figure 3. When the data are tranaferred a verification program la uaed to check all tranaferred recorde far corractnaaa. When tapea are filled (they typically hold eeven to ten dlac lmagea) they ehould ba atorad In a fireproof vault. All calculation of tba resulta of the data will be epcclfled In the method uaad. Theet calculation will ba entered la the analyata laboratory notebook onleae they are computer generated, la tbla caaa, a copy of tha computer output will be filed with the raw data. The Project Leader will be reeponelble for checking the corractnaaa of tha data. V. Sample Dlepoeal Sampled will be dlepoeed of In accordance with the lnatructlone on the Analyala gegueet fora. Tha only exception to thla would reault vhxo tha analyala reveala a problem which regulrea eample dlepoeal In a manner other than that originally epcclfled. If tha Project-Leader notea from the raaulta of tha analyala that a potentially toxic product wea prxeent In the aamplea then the aaaplea will be dlepoeed of la a manner deemed aafa by the Safety Department. The date of eample dlepoeal and the manner ehould be noted on the regueat form atored with the raw data completing the chain of cuatody of tha eample. HONS 024033 10 (Mltl-Ortn Hrtort htc CM k|t|NlM) Nfw hU T*h4 TtM Tim t (Ml* ) r*> ((**>) jyw <4(4* / (tot_yri) *0 fa/u 0Mij Ao*\SfS*itsir *>Hft i/if/o 1 ObWr} Gb6li) 6*> HA) GfiWd) Gt>Wt) 6*<*\ I ys tKT> J/Wl) 8#fM i*0 (.*) Crtfi iwrt 3tih> LSK 1*1 (*r0 CmJ *t 3*ti-3 l>T (*R*l) Lftrf) sn -n-f / '- "BIH 3sv CnoiVH^ - (WcVjM-^Vw PfitA />} W3)r*3 6* Ab /w tihuv)A<3 ' ' 4' SM/t} l t>MI& */rtn \r CrT*lC9) v*A &>7/M &>(*) 134 *a#l) tAl S>1 yhi/ts %SK 110 (A*iy) Cftlf sr\ 3 /*%> shifts M <Mt.cn l*K *st> Hi'ilty N> W>) /y> f/*>> &> *J*1H Sh Sfii/l* /V/ ->3 /*? wcs) *2> 5jiO> /& (m>) rfl (*u>i) rfl (M&) a lrl*l/*3 y/hs OB `U>k> M (it*) 33 IrfiTlV ISO (Mfi) 4* <t()lH3 xso ) jtrjtfiyrM sn V-J#s /s i (Me/) 0*2 *hnfo K '/Mu <- (At**} I i ffe/fe gx i vi (/#**> <y 4 obK r G075W S?73(5) W>14 (0) Gns(j) *&r}3.<P) $>13 (<f) GM3 Qv &2>YA^ ta> 6*-w (43 * tj. Ul Sir*. Or) <;*. 6>U (1) 4 ft F1CUU 3. Exaapl* of DISC/T0 Lojbook 7<|l. 024034 HOHS 11