Document aJdgBpq3O584kndomGO8ner3e

Monsanto_ _ _ _ _ _ _ _ _ _ _ _ MONSANTO COMPANY / DAYTON LABORATORY / DAYTON. OHIO 4S407 ESC/DAYTON (Depertaent/Section) ANALYTICAL (Type of Report) REPORT NO. MDA - SUO m JOB/PROJECT NO. 484.2100 DATE 2 July 1984 PERIOD COVERED RECEIVED JUL 51984 MOMSANTO COMt'AMT MW MWI in 8T. LOW# TITLE ANALYSIS OF PNP FOR INCIDENTAL PCB's AUTHORS: b. H. Hughe*. AUTHORS! * . M. H ughes T IT L C : ANALYSES OF PNP FOR IN C ID E N T A L PCB I* ABSTRACT: samples of p-nitrophenetole from the Oueeny plant ware analyzed for possible PCB concentrations. The results of these analyses are shown in this report. TECHNICAL APPROVAL: 3 J. 17. Brd fcfrc^ Group Leader luor Reil -* -1 r; 3 APPROVED BY ______ R. F. Ivory & Environmental Services Center Service Project Manager APPROVAL DATE: RESTRICTED DISTRIBUTION; (see over) ORTPiPTTM r,r'rp*r#iiT;nsj C 0 uPpSf tt'V * ^c4)LN f i b: t*VI*t i A L This doctnt is the preperty of Nwtssnte Caspany anJ recipient Is responsible for its ssfsksepinp and dispeslti It ccntsins oaniMItt INPOMUIMI afcich nust net reproduced, reveeled te unauthorized persona or sent anti Hansante Csapeny eltbeut prsper tutherisstien. MONS 022939 $00 IrE f S' .j ; i o \ CORY NUMBER 1. 2. ). 4. 5. 6. 7. 9. *. 10. J. W. Baxer R. J. Doy M. E. Klaus N. Prange D. B. Reddington C. C. Sisler R. K. Ivory B. M. Hughes Central Tries Technical Reports Lbry. T3C T.1C T3C 1740 C2NJ 040 1250 1250 1250 R2C ABSTRACT ONLY H. A. Woltenunn NOTE: Distribution of this report is restricted Requests for additional copies should be made through the principal contact at the Monsanto location involved or the Manager, Environmental Sciences Center, Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGEMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: B. M. Hughes D. McKenzie C O M P A N Y CUNKUtN! IAL HONS 022940 ANALYSIS P0P7 0ArC: June 29. (904 IOC NUtlfiCQ: I-04-C3-O9-OI PROJECT NO: 404.?lOie RC*: 0ufeny/lvOry Environmental Science* Center Monsanto Co*Pdny/Da>ton ,,at*-'',ato- y ISIS Nicholas Road Dayton. 0r* 4r,4i6 Ptone Ng: (SI 3) ?60-34'. ' Title: Analysis of Incidental PCBs In p-nltrophenetole Standard Sampling Method No(s): Samples supplied by customer Standard Extraction Method no(s): PCCX06 Standard Analysis Method no(s): HSAN03 Final Report file Nolsl: A2I0I8 Table file No<s>: 621010. C21016 Tables l and 2 summarize results of incidental PCBs in p-ntroph*re:o e. Also Included are : I) A brief explanation of the tables. 21 Stannaries of the above referenced extraction and analysis methods. 3) Analysis request Information generated for this project. 41 A brief description of my Interpretatlor* of the Incidental PC6 regulation. S) A copy of the CSC/UAG GLP Manual. feel free to call If there are any questions concerning this report. i HONS 022941 Tiblt I. Rnwiti of InelbanUI PCI Inatym Project Not 464.21010 Oaiti Jm n, 1994 Sample Ident If1 cat Ion Congener Analytical lOQla) Class Method fug/g> P-nltrophenetle P-nltrophenetoie lot QD~040tS lot QO-OiOiS(Oup) ConcentratIon (ug/g) ClI-BP CU'-BP Cl 3-BP Cl 4-BP ClS-BP CU-BP Cl 7-BP cta-e*' CL9-0P Cl 10-BP NSAN03 " ' ' - - 1(N) " * ' ` - Surrogate Sp'fcing Amount Compound Addediug/g) NQ(b) NQ * * " " " Recovery (t) 3.4.?'4*-C.4-o6 1.0 IOC 76 Occident at ion CSC Extraction Method Date of Extract ton Smpit Amount Catr.cttO 19) Extract final Volixxe (ml) Extract Dlut >cn ESC C*tract or Sample Number Date or CGC/ns Analysis ns run PCCX06 5/1/84 1.144; 1.0 1:1 PCB-307 5/10.5/11 19267.19264 PCEX06 5/1/84 1.0126 1.0 1:1 PC6-306 S/10.5/11 19268.I920S footnotes: (a) LOQ - limit of Quantitation in ug/g. Signal-to-nfse ratio <5 greater than 10 when this amount Is analyzed using the above referenced Analytical and Extraction Methods. The following letters indicate how this value was determined: E - estimated from PC0 congener standard analyzed under the same conditions. N - measured from native spiking of sample matrix. S - estimated from surrogate spiking of sample matrix, v - measured In validation experiments of similar sample matrix. (b) NQ - Not Ouantltatabie. The congener concentration Is below the LOO value. Table stored In file: B2I0I6:MH Anotyst(t): 0. Ha Analyst Approval:, p McKern l e w /tpy 2 HONS 02*9*2 Tabla t. Mamltt T Incidental Ka Analysas Projact Hoi 484.11818 () Jin n. 1884 Sample Identification p-nltrppnenttoif nethod blank lot QO-JStlS Congener analytical LOQia) Clate nethod (ug/g) ConcentratIon lug/g) ClI-BP cw-eo U3-B* ci 0.9-0* Cl K-9* HSAN03 * " " " " * " l(N) NQ<0) NQ " - - Sv^'O^ate StUIng Amount Co^po*if>d Added(ug/g) Recovery (1) J.4.)'4-CL4-<5e 1.0 i: 47 Docuoentat Ion ESC Extraction Method Date f Extraction Sample Amount Extracted (g) Extract final Volume (mi) Extract dilution CSC Extract or Sample Number Date of CGC/MS Analyst* NS f*N PCEX06 5/1/84 1.0046 1.0 1:1 PCB-39! S/I0.S/I1 19269.19295 PCEX06 S/T/84 0.0 1.0 1:1 PC9-39? S/10.5/11 19270.19296 footnotes: la) LOO - llailt of Quantitation In ug/g. Signal-to-nolse ratio It greater than 10 whan thli amount It analyzed utlng the above referenced Analytical and extraction Itethods. The following letters Indicate how this value was determined: E - estimated from PCB congener standard analyzed under the tame conditions. N measured from native spiking of sample matrix. S - estimated from surrogate spiking of sample matrix. V measured In validation experiments of similar sample matrix. lb) NQ - Not Quant I tatable. The congener concentration Is below the 10Q value. Table stored In file: C2IOt8:HH Analyst(s): 8. lie NcKenzIe Analyst Approval: 3 HONS 022943 OCTAIUD EWUNATIQN Of IlCIOWT*. KB TttUS In an effort to streamline repeats generated by CSC on Incidental ACS* priitAl in o wide variety of material*, using a wide variety of technique*. Standard Extraction Methods (SCHs) and Standard Analyst* Method* ($AM*> nave been developed which can be easily Interfaced with each other. An abbreviated form of these SCNs and *An* ha* been stored on the HewlettPackard 33S7-LAS computer system used by CSC. In an effort to commjnicete these details with customers of CSC, this information I* supplied with each Incidental PCB analysis. However, many project* Involve a very yell number of sample* which are not necessarily the same matrix. Therefore, to reduce cost* of generating reports for these small projects, major infom^tion on the technical details of an analysis are presented In tabular form within the same table which reports the data. Cach table includes a general title, CSC Project Number and Dote on which the table was generated. The sample Identtf(cation i* the customer ident(Meetfon which was on the sample bottle. The next section of the table gives results for the particular PCB congener class listed. The level of Quantitation (LOO) using the Analytical and Extraction Methods shown In the table, is given for each congener class. This LOQ Is determined In one of four ways and Is described In the table footnotes. The next section of the table deals with quality control used in each sample analysis. The surrogate spiking compound (If used) which Is added to the sample before extraction and analysis. Is listed, along with the amount added and \ Recovery measured for each sample. The final section before the footnotes deals with how each sample was extracted and data documentation. The CSC Extraction Method, Date of Sample Extraction, Amount of Sample Extracted. Extract final Voluse, Extract OHutlon and ESC Extract or Sample Number give critical extraction details of the analysis. The date of CGC/HS analysis and the nass spectrometer file reference number (FRN) document how and when the extract or sample was analyzed and where the raw data is stored. At the bottom of each table, analysts involved in extraction and analysis are listed, along with provisions for signature of the responsible analyst. This table fommt is both compact ano precise. It was developed in an attempt to quickly and accurately generate data which the customer can quickly and accurately evaluate. It should include all required information for certification. If there are any suggestions concerning this format* please contact me at extensions 396, 209, or 409. 6. Mason Hughes Senior Research Specialist Mitt INCXPTtMHtSP Environmental Sciences Center Monsanto Company Dayton Laboratory ISIS Nicholas Road Dayton, Ohio 4S407 4 HONS 022944 The following pages describe Standard Extraction Methods and Standard Analysis Methods used for this project. 5 MOWS 022945 CSC Standard Extraction Method ISEM) TMtts PCBs In nltro group containing atrlc$ ESC Standard Extraction Retrod No: PCCXOt HATRI(X),(CES): p-ni*ropnanoto*. aromatic/ likyt n't'O containing compounds TYPICAL SAMPLE size < 0) O.S - 5g TYPICAL Extract volume l-rl) : - 10 TYPICAL ANALYTES: AlZ4?.A|Z40.AlZS4.AlZSO.and PCB I SCm*'S i*jrC through dC* CMoro biphenyl INTERfEPENCES: Any electron caoturIng toedes m cne retention time region of tr icMorodipnenyi isomer* through octacnioroolpnenyi Isomers for ECAnoi and CCANO:. Any species in the appropriate retention time region which give the same relative charac teristic mass responses as PCB isomers for RSAN03. TYPICAL surrogates ------------------ TtP!Cal reco/eies m ----------.................. pentad iorobenzene 2.4,6-trichloro- blpnenyI 3.3'.4,4' -CL 4- biphenyl-d4 .r, . 120 SO - 120 SC - 120 APPARATUS ANO MATERIALS: Burdick and Jacxson hexane for sample extraction Concentrated hydrochloric acid for reduction of the nltro group. ROSSy t *n for cotylyttc reduction of the nltro group. OistHied deionized water for dilution of the hydrochloric add. $od'vr> hydroxide pellets for freeing the amine salt. Silica gel columns Impregnated with potasslu* permanganate, sulfuric acid. and potassiu* hydroxide. Disposable glassware. UNtTATIONS: Method applies only to matrices which do not contain non-hydro* Iliable electron capturing species in the trichiorobiphenyi through octa* cl11 oroOlphenyl Isomer retention tine region for EC detection methods. SAFETY PRECAUTIONS: See PCB handlIng protocols In laboratory safety manual. OATES OF HETH00 CREATION ANO UPOATES: 4/24/04 MONS 022946 C now sheet pcrsoc ton CSC EXTRACTION NCTHOO PCCXOG SAMPLE 10: CXTRACTION DATC %nc T|C: mac extract LOG NO: HUGH OUT SAfir^C INTO A 40 i* VIAL () WEIGHT SAMPLE (I g) SlRXA'! $PIE O' SAMPLE SP|k AOO l.S 9 OSSr TIN. ANO 6 mL CONC. HCI TO SAHPlt AUOW TO STAND OVERNIGHT . () . ADO !*> "H. WATER TO SAMPLE ( J ANO BA?Ifv with NOH (4-Sg) . Extract ixu lot METwr- ( J I ) ( ItNt ChlORIOE/hCxANE . RINSE EXTRACT 1 X 10 AC JC1 SUL?U*IC ACIO . (J REDUCE SAMPLE VOLUME TO l) I-: H WITH nitrogen ano . APPLY TO COLUHN QUANT|TAT IVIY. .. ELUTE WITH JO ML HEXANE [) NITROGEN BLOW OON* TO I H ( ] EXTRACT NO: ............................................. OATt/TIHC COMPLETED ---------------------/ ANALYST t ............................................... ESC JOB NO: RINSE COLUMN w|Tn 2 X 20 ml { ) HEXANE CLEAN-UP column description 2S it OISPO PIPET \/ \/ I cm n* SO 24 4 cm II POTASSIUM PERMANGANATE SILICA GEL I c SILICA GEL 4 cm ACIO SILICA GEL I cm SILICA GEL 4 cm BASE SILICA GEL GLASS WOOL HONS 022947 7 ISC Standard Analysis Method TITVIi OrfanIc Gcapoiaidi In Solvents IX Standard analysis IktM No: RSAM03 ANALYTICAL INSTPUmEkt and nOOC or OPERATION: HP-59656 Capillary GC/N$-$irctei |<x> Monitoring with Revision-! Hiti-drive software. Typical Aon Hire: Typica' Multiplier voltage: Typical Dwel1 Times: Mo*Ihk/t ff of Masses: Electron Energy: 3-40 min. 1600 - ?800 ev ?00 - 500 msec/mass ?0 70 ev typical AKAt Y'r typical instrument lEVEi Of OtTECTION (IOC) <ug/ml) Organic Compound* eluting between toluene and n-C34-ane 0.01 - 0.1 typical PRECISION 0 I0X L00 (1) 30 TYPICAL ACCURArv 9 10r LOO It) 33 INTCRf ERENCES AND LIMITATIONS: Analyte characteristic mass must be chromato graphically resolved from other eluting compounds which produce the same mats. CHROMATOGRAPHIC COLUMN: 30-meter fused silica JAW 06-5 (0.?S uH) with wide bore <0.3? w) COLUMN TEMPERATURE PROGRAM: 50(0/6/300 INJECTION Type: Split'ess CALIBRATION AMO STANDARDIZATION: QuantItatIvc: Use Internal standard quantitation tecnnlque and caliorate Instrument response rectors from standard solutions of analytes of Interest. (feelItatlve: When aultlpie character Istlc aasses are aonltorrd for a given analyte, the ratio of characteristic east responses auet be within ?01 of those for the authentic standard, for PCS analyses, the characteristic aasses which are aonltored are the molecular ion containing all 35-Cl Isotopes and the molecular Ion containing one 37-Cl Isotope. Since the above referenced analytical mstruaent can monitor no more than ZO masses In a single analysis. Incidental PCD analyses require two Injections of each sample In order to analyze froa Cl-biphenyl through CllO-blphenyl leasers, anthracene-dio and the surrogate spiking compound. The following suaaarlzes the aasses and appro*Imate retention tlae regions aonltored In these two capillary GC/HS-SIM analyses. HONS 022948 I ANALYSIS 91 Analyte Hasses Retention Times (minutes) Cl-BP isomers. enthracene-dlO CL/-BP isomers 3.4,3*,4'-Cl4-0p surrogate ClS-BW ioneri CL7-0P Isomers 108.190 222.224 296.296 323.9.325.9 391.8.393.6 461.6.463.6 11 - 21 11-21 21-28 21 - 28 28 - 39 26 - 39 ANALYSIS ? anthracene-dll' CL3-0P som*rs CL4-0P isomers CL6-0P Isomers C18-BP l0*rs CHO-0P isomers 166.168 255.9.257.9 289.6.291.6 357.6.359.8 427.7.429.7 497.6.499.6 )4 - 23 14 - 23 23 - 29 23 - 29 29 - 39 29 - 39 CALCULATIONS: Analyte concentration (Analyte *re*)/(An*1yte RRf)(arM of IS) where: Analyte area I* the character 1stic mass area of the analyte. RRf is the relative response factor for the analyte. IS Is the Internal standard and Is usually enthracene-dlO. RRr (analyte area in stanoaro)/<conc. of analyte)(area of IS) PC9 concentratIons are calculated In one of two ways: 1) If an Aroclor formulation can be Identified from the patterns of PCS isomers, seleted PC6 Isomers or classes of Isomers (I. e. all Cl4-b)ohenyi isomers) ere used to quantify the Aroclor concentration. Relative Response Factors are calculated using the concentration of the total Aroclor for mulation In the above RRf equation. 2) If no unique Aroclor formulation Is present, then the total PCS concentration Is calculated by using standard solutions containing known Mounts of chloroblphcnyl through dacachloroblphenyl Isomers to calculate Relative Response Factors In the above RRF equation. The RRFs for the corresponding PC0 Isomer classes arc used to calculate total PC0 Isomer concentrat Ions In unknown samples. SAFETY PRECAUTIONS: See PCS handling protocols In laboratory safety manual. OATES Of IKTHOO CREATION AND fCTHOO UPOATES: 12/9/83 HONS 022949 0 The following pages describe Analytical Request Information generated for this project. HONS 022950 10 **C ENVIRONMENTAL SCIENCES CENTER ANALYSIS REQUEST DATE: march 9,1964 REQUESTER: $1. LOlIS/QUCENi/HUGHCS LOG NO: 1*64-03-09-0! PROJECT NO: Rt0*>T RESULTS TO: F UES/MEES. IVORY.BROCKS anal *b t S REQUESTS SENT TO: FILES, IVORY. BROWS. hjChES SAHO^E PICKUP eY: n. hu>EC SAMPLE LOCATION: LAB .**8 BullOlNG 2 sample DESCRIPTION FOR 2 SamPlES SAMPLE IDENTIFICATION NUMBER OF BOTTLES CSC NUMBER'S) P-MTROPmEnETOlE LOT OC-06CSS | PCB-30T.PCB-366 O.'P PCB*389*LS,PCb-39C*H; P-N|TQOPhnCTOlE LOT 0C-366IS l PCB-391 hCThoo Blank PCB-392 RECORDED BY: P. HUPP REOUI Rip ANALYSES: INCIDENTAL PCB*S ANALYTICAL TECHNIQUES: SEE PCFS06 AnO PCEX06 DATE COHPtETEO X a/EC (IB) 6/29/84 QUALITATIVE: US SCMIQUAHTITATIVE* QUANTITATIVE: US REQUIRED OA/OC* COMPLETION DATE REQUESTED: COMMENTS: SAMPLE DISPOSITION* X HOLD FOR 30 DAYS StfCTY PRECAUTIONS* ANALYSIS REQUEST FILE NAICi AAZlOOiLS 11 HONS 022951 Analysis of Incident*! PCBs In Monsanto Products. Vast* Streams. Emissions no Effluents of Closed and Controlled Waste Menufactur Ing Processes 6. Mason Hughes Environmental Sciences Center Monsanto Company/Dayton laboratory ISIS Nlchoias Road Dayton.Onlo 4$407 Tt>t October 21, 196? federal Register <voi. 47, No. 204) contains a very extensive Definition of PCB-conta*ning products, waste streams, emissions and effluents from menufacturing processes ana general descriptions of methods wMcn should be used for these analyses. The purpose of this present report Is to outline t*e approach taken by Monsanto's Environmental Sciences Center In turc'ying analytical data which can be used for certification of Monsanto products, waste streams, emissions and effluents. In order for the material to be certified as not containing PCBs. the CP* set various levels of Quantitation (lOQ). below which a product, waste stream, emission or effluent could be certified to contain no PCBs. The LOQ Is defined on the basis of the concentration per resolvable chromato graphic peak. Ouoting from page 46986 of the federal Register, vo>. 47, No. 204. "This means that for a process to be eligible for exclusion under the closed and controlled waste process exclusion, no single peak on a gas chroedtogram registers PCBs In excess oft ten micrograms per cubic meter In air emissions, 100 microQrams per liter in water effluents, and two micro* grams per gram In products and uncontrolled waste streams." Therefore there are very specific definitions which Monsanto can apply to Its products, waste streams, emissions and effluents which determine whether these materials may be eligible for exclusion. It Is the goal of the Environmental Sciences Center to supply Monsanto plants with the proper data and docusentatton for this exclusion. Capillary gas chromatography/electron Impact mass spectometry (CGC/MS) Is the Instrumental technique trftich the federal Register suggests should be weed In the analytical method for PCB congener analysis. However for most Monsanto products* most* streams, air emissions ond water effluents* this Instrumental aethod must be used in conjunction with an extraction method In order to determine what levels of PCB congeners* If any* are present In these various aaterlals. The remainder of this report will therefore deal with how IK will implement this Instruaental aethod for the raiysls of PCBs In various types of samples. In order to analyse a sample for PCBs. using CGC/HS techniques* a representative saaple of Interest* or a representative extract of a sample of Intarast oust ba Injactad into tha eapl t lory chroaatograahlc systea. Tha prassnea and quant It Itas of KB congeners present are deteralned by coopering tha PCB cengsnsr responses In tha sample of Intarast with the XX mons 022932 responses In on anelytlcal standard containing at least one PCS congener for eocn of the ten chlorine dosses (I. e. Cll-biphenyl through ClIOblphenyl). the analysts of Monsanto products end waste streets c*r> be devioed into two types of CGC/HS onolyses. the first Is for products ort waste streams which can be chromatographlcel ly resolved from Cll-biphenyl through Cl10-blphenyl congeners, when the product or waste streem Is present at ten million tines the levels of the PCS congeners. Thl* first type of onoiysls only require* the sample to be Injected Into the CGC/ftS instrument and PC6 congener areas compared to standard PCS congener areas. The second type of analysis applies to Monsanto products and waste streams which cannot be chrof^tographicai ly resolved from PCB congeners and for a>r emission and water effluent samples. This second type of analysis must first Isolate Into a solvent ll PCS congeners which are present In a representative sample of cne product, waste stream, air or water sample. Hits extracting solvent can then be analyzed for PCB congeners as described above in ti.e first type of analysis, since the extracting solvent is chosen to be chronetograpMca* iy resolved from the PCB congeners of interest. Therefore an integral part of the PCB congener analysis revolves around the vuMowtion of the extraction method used to isolate the PCB congeners and voMdation of tne CGCnS method used to analyze extracts. In order for Monsanto plants to understand the data that is generated for incidental PCB certlftcation. the following sections outline how data will be obtained and validated for t*e presence or absence of PC8 congeners in various Monsanto materials. (xtraction of products, waste streams, air emissions and water effluents: If samples of Interast cannot be directly analyzed for PCBs using CGC/MS techniques, they must first be extracted with an appropriate solvent which can be analyzed for PCBs. This not only applies to the products or waste streams, but also to air samples or water samples which may contain large amounts of products and waste stream components. Two major properties differences of PCBs and major compounds In samples of Interest can be used to Isolate PCB congeners Into an appropriate extraction solvent. These are: I) reactivity: and 2) water solubility, low levels of quantitation for PCB congeners in samples which contain major components In tne PCB congener elution region cannot easily be obtained unless these major components can be removed by their reactivity or water solubility. The inherent stability of PCB congeners and their high affinity for organic solvents and low water solubility are chemical and physical properties which can be exploited for this separation. However It Is Important to demonstrate that, during this Isolation phase. PCB congeners have not been removed during the process. This Is done In two ways. The first way Involves the use of a surrogate compound which acts exactly like PCB congeners, yet Is mass spectrometriesMy different. This Is normally accomplished by using either deutereted PCS congeners or congeners which contain carbon-13 rather than carbon-12 In the biphenyl structure. These surrogate spiking compounds are added to each sample for which PCB congener extraction Is required, and their recovery Is reported along with any PCB congener detected. However this approach Is valid only If one has tsotoplcatly label led PCB congeners for each congener class. Since at this time there are no surrogate compounds for all efosses of PCB congeners (I. e. CL I-biphenyl through CLIO-blphenyl). a second type of extraction validation Is normotiy used. This validation step Involves adding at laost one native PCB congener for CLI-blphenyl through CLIB-blphenyl congeners and measuring the recoveries of eoch of these native congeners dwe the product* waste stream, air amission or water affluent la extracted. That# native spiking studios should be performtd on representative typos of motrices to demonstrate the validity of the A3 HONS 022953 results. If no previous dot* Is ovoltable for recovery of ail PCO COTgene' types fro* a specific Aetna, this native spike should be perforawo in order to validate the data being reported. Since it is not anticipated that incidental PCB generation win be de tected for Monsanto processes. It Is Imperative that the above quality control steps t* conducted on each sample or for each sample Mtrix type In order to va'idate the fact that if PCB coneeners had been present in the Monsanto sample*, they would have been detected at the levels required by this reguiation. CGC/MS anaiys't cf extracts, products and waste streams: As mentioned above, sample extracts, products and waste streams can t>e Injected directly into the CGC/HS analytical system If the major components do not elute <n the retention time regions of the Cll-blphenyi through Cl10-D'phenyi congeners. Data ouailty of this analysis step Is also otmunstrated by similar approaches outlined above for sample extraction. Ir, order to verify tl*at the lnstr\xxent is functioning properly for each sample injected, an internal standard Is added to each extract, product or waste stream cefore it Is Injected Into the CGC/HS system. AnthracenedlO is usually used for this purpose. The absolute areas of the fnterr>o> stancjrc in the extract, product or waste stream analysis must be within 30t o' the area of the internal standard which is added to the PCS congener analytical standard. This analytical standard, containing Cll-blphenyi through CUO-blphenyi congeners, Is analyzed under the same conditions as the extract, product or waste stream samples and from the Instrvexent responses for the ten PCS congener classes, levels of detection and quantitation are determined and the amounts of each congener class (If greater than the LOO) is reported. Ideally, each sample should also be analyzed after spiking with at least one native PCB congener In each congener class at the level of quantitation (lOQ) in order to verify that the 10Q concentration could be detected and quantified In the presence of sample Interferences. This is done In order to show that the CGC/MS Instrumental analysis Is valid for the sample matrix of Interest. However some products and waste stream samples are not miscible with solvents in which PCB congener classes have been prepared and there fore it Is not always possible to analyze a native spike of all products and waste stream samples. This Is not a problem with sample extracts, since the extracting solvent has been chosen to be compatible with surrogate and r*tlve spiking studies which occur In the sample extraction step, described Quantitation and Identlf1cat Ion of PCB Congeners: Tables I and 2 show how the 209 PCB congeners are distributed amoung the CL 1-biphenyl through CLtO-btphonyl classes. In addition these tables show the cnerecterlsttc masses and theoretical relative abundances for each of the ten congener classes. In order to routinely obtain analytical data with levels of detection on the order of 0.1 ug/ml per congener, the mass spectrometer detector Is operated In the Selected Ion Monitoring node (SIM), This node Is a screening mode and monitors at least two molecular Ion characteristic masses aver the elution time region of the corresponding PCB congener class for ai l ton congener classes. PCB congeners are tentatively Identified from the ratio of the peek areas of the two molecular Ion chromatograms. If the ratio agrees within 14 HONS 022954 301 o' the exper i mental rat to obtained fro* the PCB congener st*4ard analyst*, and the two peaks maximize within two ness spectrometer scans, then the sample Is reanalyzed while monitoring all messes o' interest 'or positive Identification o' the PCS congener. )' the peak area ratio does not agree within 301 o' the experimental ratio 'or a particular PCS congener, then this response Is not due vc a PC8 congener. St*V*ery! The above aoooach a1lows 'or rapid, routine analyses o' extracts and samples of interest. Since 'ew positives are expected, adequate Quality control Involving the use o' Internal standards, native soikes and Surrogate spikes will be used to validate that the data car be used 'or the certifi cation c' the absence o' incidental PC8s in Monsanto products, waste stream*, air emissions and water effluents o' closed and controlled waste Manu facturing processes. 1e* f >e: lNr*C0' :*H:Sr Tabic rues; Intbo::hh, inTB0?s*m HONS 022955 IS Table I. Characteristic a*ses and Isotope patterns Of the characteristic nesses for cnoroopr>enyi through pentacniorobipheny* congeners. PCB Congener Class INi^Oer of Congeners) Car*ctfr |*t lc Nvf*t>er of Hasses CMo' ines CU-BP (3) CL2-0P < 1?) CL3-0P (?4) C14-0P (4?) Cl^-BP Me 192 193 iec 107 IBB 109 190 220 222 2.' 226 253.9 299.9 257.9 299.9 207.6 269.6 291.6 293.6 299.6 321.6 171.8 32S.6 171.8 179.8 0 *<-) *(-) 0 *(-) 1. x(100) 1 *(100) 1 x(IOO) *(32.4) 1 *(32.4) 1 *(32.4) - 2- *(100) 2 *(100) *(64.0) 2 *(64.0) *00.9) 2 *(10.9) - 3 - M)00) 3 *(100) *(97.2) 3 >1(97.2) (3I.5> 3 *(31.9) - 44 *(77.2) 4 *(100) 4 *(40.6) 4 x(IO.S) 99 *(61.7) 9 *(100) 9 x<64.6> 9 *(21) HONS 022956 1C Teble 2. Characteristic messes ond Isotope patterns of the characteristic ostses for heach)orobtphtny1 through decochlorofctphenyl congeners. PC0 Congener Class (Nurfcer of Congeners) Cl*ercter 1st i( N\y*fcer Of nesses O'lorInes C16-BP (47) Cl 7-BP (24) C18-6P (12) C19-BP (3) ClIO-Bf ID 287.0 269.6 791.6 793.6 371.6 373.0 3:5.0 377.6 379.6 399.0 397.0 399.6 361.6 363.6 369.7 391.7 393.7 399.7 397.7 473.7 479.7 477.7 479.7 4)1.7 43J.7 45*.t 441.1 441.4 445.4 447.4 4*1.4 4*5.4 4*7.4 491.4 $41.4 4 *<77.71 4 KtlOO) 4 *(48.6) 4 i10.9) 9 *(61.7) 9 *<100) 9 *(64.6) *(?U 9 6 6 *(51.4) 6 xflOO) 6 *(011 6 *(39) *(91.4) *(100) *<61) *(35) 7 *(44.|) 7 x(44.|) *(100) 7 *(100) *(97.2) 7 *(97.2) (17) 7 *07) 8 *(34) 6 *04) *(86.7) 6 *(88.2) *(100) 8 *(100) *(64.8) 8 *(64.8) *(26.7) *(26.7) 9 o(24.S) 9 o<77.2) 9 o(ltO> 9 0(75.4) *114.7) 10 0(21.2) it o(4t.4> it oUtt) it o(t4.4) 10 Xdt) 13 HONS 022957 The fol lowing I* copy of the ESC AMO Good laboratory Practices Manual. It MOMS 022958 Ifcahort 0000 UBOtATOCT PUCTICtS MANUAL A to Quality C--trol/Quality Aiwwi Ultratrace Aiulyila Croup (torch 19*4 Croup Leader, Ultratrace Analyaia 1. A. *>ltHn Ikuiir, twlnamil Scitaett Caottr Iimd to: Data! JU/JOD A raaaaatal tclaacaa Caatar Daytaa Laboratory Daytoo, Ohio 4SA07 1* HONS 02295' tails or coin ms 1 OljKdvti XI lcor 111 Analysis A. Methods I. QA/QC Pragma 1. Staple Preparation QA/QC a. Method Hanks h. Replicates e. Spikes 2. Instrumental Analysis QA/QC a. Instrumentation b. Ilanks c. Quantitation Internal Standard d. Standards C. Degrees of Quantitation 1. Qualitative Analysis a. Tentative b. Confirmed 2. Seal-Quantitative Analysis 3. Quantitative Analysis D. Quality Criteria and Remedial Action 1. Quality Criteria a. Hanks b. Recoveries c. Precision d. Limit of Detection e. Accuracy 2. taaadial Action IV Data V laaple Disposal FICHUS i bmtU .( oe/w Ui>m> r*i> l iwfii < ec/oc ukMk m* } tafli f HK/bfi Uftook m* 20 r*n las 5 4 11 MONS 022960 l. 9M1<W Dm Min tkjKilm of the Oltratrace luljrili Croup ihIIijt unniM/taaltt; cnlKl irtiTin art: 1) to man that our liWatar; generalee kl|k quality raaulta: and 2) to maintain tha aacaaaary records that decneat loboralory MiltnaiK*. II. Icoot Tke itayi ol tkla manual luladat araaa of CL? not apeciflcally addressed in tko CSC auction manual and expands upon cortaln araaa wkoro QA/QC practices dllftr froa tkoao doacrtkod lo tko auction nanual. It lo Intondod to ko uaad along with tko section annual to provide a coaplete picture of the CL? within tka L'ltratraco Analyala Croup. III. Analrala Tko gonoratlon of analytical raaulta within tha Ultratraca Analyala Croup routinely Involuoa two proccaaao: aaapla preparation and lnotrunontal analyala. Saaplo proparatlon Involuoa oaa or nora of o variety of techniques Including attraction, dilution, acld/hase waakoa, colin ckronatography. concentration and niaarowa other techniques to render tka aaapla la o aultabla condition for lnatnaental analyala. Inatruaontal analyala takea tka aultakly prepared aaapla and introducoa It Into on analytical laetrtmnt to aaaoure tha doalrad paraaotar(a). loth of theoe proceeeee can ka daecrlkad by clearly defined and aaparaklo aethodo called aaapla proparatlon aethode (SPMs) and lnatrwantal analyala aathoda (UMa). SPMs and LAMa aay bo coak load in ntaoroua waya (depending open the nature of the aaaploa end the needa of tko cuetoaer) to produce a eucceaaful analytical protocol. Tor axaapla, eeveral different IPits aay ko aaad to produce aaaploa that art aultaklo for aaalyelo by a alogle 1AH. Tha aaaaurao Incorporated into each of ckooo cnparlaantal proceaeea to cnaure that an aanaaaaent of tko quality of tha raaulta can ko aada conatltuto tko QA/QC prograa for o project. Tka following awbaoctlono deacrlbe the olaaonto of tko aaalyala proceae: A. Natkoda Matkoda ata tha wrlttaa docwantatlon that daacrlha tha analytical procaaa. They contain aufflclent detail aach that a coapitant acloatlat at technician can readily perfeta tha moulted analyeee. The aaaal practice la te have aathoda that daacrlha tha aaapla preparation preceea (SPHa) aad aathoda that daacrlha tha Inserts* aratal aaalyala procaaa (lAHe). tack aathod davelopad within tha Ultratraca Aaalyala Creepe la aaalgnod a aathod uuabar aa daacrlhad la tha ISC Sactlaa Hsnusl. Hathade are obtained fraa various aourcas Including la-heaaa develop* aaat, aadlflcatlan/adaptatlan of lltaratara aathoda, ar apaclflc prececal aathoda dictated by paiaiaaant apanclaa. Hathade aay ha fanally validated by a aarlaa at aaparlaaata that daacrlha a alaaaftal validation pretacal ar aay bo leee vigaraaaly provan autag ta factora each aa freqaancy ar wee, caotonr aaada aad 31 HONS 022961 cail/tl>la| restriction*. la any uh a QA/QC pregrsn la afallal la tk analyala pracui to pmUa a aaaeure of iko quality of tka taaalta. Oelaaa a QA/QC prugran la pitacrlM by a reqvlred protocol D1 Jloila la tall protocol), certain elniaua QA/QC aaaauraa (dapoodlnt upea tka aaalyal* type) ara incorporated lata all Ultratrace Analyala prcjacte. Tka fellovlat aubaactlaa daacrlkee tka Ultrattaca QA/QC pro|r*a: t. QA/QC Pragma An affective QA/QC progrea Incorporate* axperlaanta that provide lnfaraatlan ralatlva to each of tka fellovlat question*. (I) Ara thara any lapuritiaa, background or cantaalnatlon that vlll Influence tha raaulta? (J) How raproduclhla ara tha raaulta? (!) How veil can tha analyte be recovered fraa tha aaaple aatrln? (A) What la tha Halt of detactlon far the analyala? ( What la the dynaalc range of the aaalyele? (t) What la the accuracy af the analyala? All af theee question* are addteased by properly aelectlng/applylng the uae af blank*, rapl lea tea, aplhea and atandarde In a QA/QC pragma. The dlacuaaloa af the uae of theee QA/QC technique* a* they apply to Ultratrace Aaalyali Croup actlvltlea la beat done ky canaldertng the aaaple preparation and Inatriaental analyala prectaata aaparately. 1. Saaple rraparatloa QA/QC a. Method blaaka - kepreaentatlve glaaavare, aolveata and raagaata ara aaad with aaaple aatrlcaa uhleh are alallar to theaa far vhleh raaulta ara being reported, yat do aat coatala the aaalytaa af lataraat. Method blaaka are analyead at a frequency equal to 101 af tha analysed aaaplaa far aaapla aata uhleh ara aultlplaa at 10. At leaat aua aathed klaak la aaalyead for aaapla aata cuutalalac betuuaa 1 and f aaaplaa. k. lepllcatea - If aufflclaat aaapla aunauta have keen euhalttad far analyala, rapllcata fraquaacy la the aaaa aa tha aathed blank fraquaacy. If at all paaalhla, rupllaataa ahauld ha obtained fraa tha aaaa aaaple battle la atdar ta alalalaa aaapla lahaaagaaalty peak! me due to aaaplaa bulag taken at allgbcly different tinea. c. Splkaa - If aafflclaat aaapla la available far each aaapla type, tha aaapla la apllt aad eplhad at tun level* vltk 22 HONS 022962 tk win (alitaliO uilrnU). Ill Imli ut Wleuir 2a (low) aad 20a (hl|k) tho aatlclpstrd detection Halt tat Hm u tachalQw* for ootlaotlag the Halt of (itlctlM for oath aotrla. Tint low aad kl|l Op11os aro cendwetad at a (totWK) oqwoI to tho Method Uaak froguoncy. Obvloualy BfUlBi with tho aotlvo aaalyto caaaot bo doaa for vldaacaa analysis loco thlo preeuppoeos knowledge of tho Identity of tho analyto(o) la tho aaaplo. Other oplklag tochalqwoo oro wood to owolwoto tho oxtroctloo/rocevery offlclcacloo for tho aaalyte(o) of lotoroot. Ideolly eitrectloo/recovery offlcloocloo oro fotenlMl for ooeh HOflc, olocc. In principle, each ooaplo nay represent a different aotrla. Thlo coo ho done vary ooolly whoo tho dotoctloo technique lo aaoo opoctroaotry If an lootoplcolly loholod version of tho aaalyto(o) lo ovalloblo. kocuaoototloo of extractloa/rocovery affleloncioo lo not required for oach ooaplo If tho ooaplo aotrla for oot of aaploo lo eonotaat. Howcaar, for a aaaplo act for which the olallarlty of aaaploo la act kaowa, aad for which adequate aaaplo lo available, each aaaplo auot be opllt and plkod with a haown amount of tho aaalpto(o) of Interest to dotoralao extraction efficiency. If adequate oaaplo site la not available or tho Identity of tho aaalyto(o) lo not known before the fact (l.o., wldoacan analyata), surrogate aplklag cowpounda nay ho wood to aooooa attraction affleloncioo In oach aaaplo without actually oplklag oach aaaplo with the aaalyto(o) of Intoroat. Tho choice of tho aurro|oto spiking coapouod la tailored for oach aaalyto. Thlo ourro$ote auot bo chooon oo that It la althor chaalcally Identical to tho ooalyto of lotoroot (for axample uolaa laotopically labeled analogues of tho analytoo), or la cloaaly aiallar in torn of liquid/liquid partition propottloa, chaalcal reaction proport loo, colaan olutlon proportion or other aatrlx leolatloo proportion which ara wand to looloto tho analyto(a) froa tho aaaplo aatrlx. Another property of tho aurrofato aplklni caapoond la that It not bo present la tho aaaplo being analysed. 2. laetnmatal daolyela QA/QC The flail atop la obtainlag analytical raawlta lavolvoa tho aao of aa appropriate iaetnaaatel tochalgwo to produco tho analytical data. Several QA/QC pvactlcoa aaat ho laeerperatad la thlo procoaa to aaouTQ validity of tho data. a. lnotfontatloa Careful dsfsatatloa of lnotrvasat wanta. callbratloa, and aalntaaaaca la aoaoatlal for tho |oaatatlaa of high Quality renalta. Bach aajor laatraaaat ttlthla tho mtratraca Aaalyola nap will ha tha aaaliaad raapaaalblllty af a profaaalaaal oaployee daaltaarad ao tha laatraaaat Itaward. Tha laatnaaat naward la raapaaalhla for aahlaB aan that lopbooko ara avail* able aad properly ooaplatad by daatcoaaot wears. It lo the 23 HONS 0229*3 raepooelbUlty of uch MMlwl Iilai tW iail|nt to iir< all the rtrtiMt hu la tka logbook. An aaanpla at a Ml* from a CC/MS logbook la |ln la Figure 1 asl that of a CC/tC lagWooI la |lm la Mgata 1. laatrvaeoce will ha calibrate accordlag to tha iaetruaant manufactureTM' epeclflcacloae or accordlag to tka acthod being aaad vith tha 1net treat. * log of laetrueent calibration trill be aalatalaed with the lnatrtsent. The Inetrreat Iteward will be reeponelble for onaurlag that preventative and corrective aalntmance pro|m are carded oot on all lnatruaenta aader hle/her reeponeihlllty. If a (pacific probloa It noted by an laatrraaent aaer. It hould be noted In the logboot and the lnatrrent Steward notified ao that appropriate corrective action can be taken. b. Blankt A aolvent blank will be analyied at a freguency equal to the net hod blank. The aethod blank can nerve aa the aolvent blank provided It la clean la the area of the asalyto(a) of lntereat. Thla practice elialnatte tha poeelblllty of background iaatronental cootanlnatlOD. c. Quantitation Internal Standard A quantitation Internal atandard will he added to each aanpla following oaaple preparation but prior to iaatrunental aaalyala. Thla confound will aerve for detaraintng ralatlvo raaponaa factora and for correcting for varlatloaa In oaaple Injection voluneo and evaporation of oolventa. d. Standarda Standarda are aolutlooa of tho aaalyta(a) of lntereat need to determine the raaponaa of the detector over the reage of analyte concent rat Iona found In the oaaplao. for Quantitative aaalyeee, eufficleat etaaderda and replication of atandarda will be run to daaoaotrata linearity and preclalon of tha detector roopoooe over the range of analyte concaatratlana. Should eanple cancan tratlona fall outalda the danonatratnd llnaar range, either additional atandarda are prepared to anpaad tho range, or appraprlate dilution/concentration of the eanple lo done to place It la the proper reage. Bogreee of Quantitation The information provided for any particular aaalyala la tailored to the noeda of the coeteaer. Xa actual practice thaae aaade very acrcea tho broad ceatlauaa (ran the greoaly qualitative to tha praclaaly qaaatltativu. It la informative to ananlno nhat lo involved la providing tha varying dagrnaa of quantitation required by our cuatoaara. 24 HONS 022964 hpsmo ec/fc. fcw - *. IIH*MMMHtMt> MutM,liM MHC-fM m non I 4*. h 1 1 a __ __1 Sa_ I 1 L, 1 sL 1 _3 u_ r r 1 _ L ML __1 1__ M Atn a* 11 L_ lax* 1_ AX atvaa... mvvti!tamat !**. ww MW *m. m,. I.M*. i.Mmmmmmm...vmmitwma mmmm(... hmit*mi..aiSim*., iit..nStttaZ.l i ZS55 "*****&*>*** *"* 1MM5MK..a5Ma.*.. i.Iit..aMtataMt*... ii|...aMtanM5a II i M tr r _* H mm-m . a. rm mm. vatt hm> tm.m. i.taaa i.5 IT 1 r $ f Ji _U JL 1 _*4 1 1f V Mi g r /I f1 r 1__ J2 r r _l ,t r tifi -- rtGNt 2. Eaaaplt ( CC/IC Ufboak p|t. HONS 022<6 1. Qaalitatlua Mull MiUtin MllllU MIn m kmiIimIm at *11 tot tattot to* >J tto Identity l tto nfM^d) preeeat. Mm la particularly (ftlluU* to tfclc tm af aaalyala prablea. to W af Idantifltatlana ua to cadet a. Tentative A tentative IdeatIfleatlea la aade aa tto toala at tto uljit'l Judgement at a aatch totwaaa tto aaaa irattrw freu tto Maple end a aaaa epactruu fraa a rafaraaca library. Thin ia attaa Aaaa far the large amber at cnaynuade found la a wldeacan organic aaalyala. b. Cootlraad A conflraad ldaatlflcatlon requlree that tto chroaato* trayhtc rataatlaa tlaa aad tka aaaa apartrua of tto aakaeua coapouet aatch theaa af a known atandard af tto tentatively ldantlflad coayouad. Thia la oftan dona In vldaacaa aaalyaaa whan atandarda can to oktalaad for tantatlvaly ldantlflad coapounde that ara af ceacarn. Tha normal QA/QC requlrauenta far yullutlra analyala ara (1) analyala af a blank. (2) aaalyala of duplicate aaaylaa aad O) uaa af a calibration compound (uaually Decafluorotrlphenylptoaphiae, Dm?) to aaaara that tto aaaa apactroaatar will produce aaaa apactra that can to coaparad with library apactra. 2. Sml-Quaatltatlve Analyala Saal-toaatltatlwe Analyala aataada tha Intonation provided by a qualitative aaalyala to include aaaa eetiaate af tha aaaunt af aaalyta(a) preeent. Tto aothod at eeal-quantltatlon lavalvaa tto coaparlaaa af datactar raapoaaa af tha aaalyta(a) with that af an Internal ataadard. Tha aattaated concentration la obtained by aeaualat a aalt raapoaaa factor totwaaa tto analyta(a) aad tha iateraal ataadardfa). Aa Indication of recovery froa the ample aatria la abtalaad froa the recovery of tto eurroiate Internal ataadardfa). 1. Qi|aatltatlve Analyala Quaatltatlva Aaalyala prawldaa far tha accurate aaaaaaaaat af tto aaomt of aaalyta(a) praaaat la a aaapla. To to able to da quautltatlva aaalyala aaa auat know tto Identity of tto analyte aa that ataadarda caa to prepared far aplklng aad far tto |aaeratloo af eallbratloa curvea. Tto nethod af quantitation la haead aa a tkrea-pelat eallbratloa curve uniat ataadarda af tto aaalyta(a) af lataraat ewar tto route af annaoutretlone la tto eaaplee. A ouepolat calibration aethod caa to aaad (aa with tto latoratary data 27 HONS 022967 Tt) imiM tht ItaMTtty km tom toaomtratto iw to hkMiiiim ram* ! (to wf>N HlH itobrii of tto mlnili) C tkM NMMtnUoN to tto r|. Tklt calibration ttm it tto* to to provide ercMtntltn of tto 0Mlyte<e) ii tto nmUi vU " **ornel ittoiNi tttlii tv tm pnfttiUy via Umia) tatoria Ntto4. tor tto iitaml atatoNi tattoo, tto naatlti* tiM internal ata^aN it aMa< to toed of tto ttandards (jm u iritd tto oa^lai) trior to laetiMoetal aaalyale and relative raaaowt foctoro oro detemlaed. tor guMtltetive aoalyala tto moo epectroneter 1* pereted aa o tot c^rtoto$rapdlc detector* Tto NS lo therefore tuaed ood operated In Maiar opacified la tto approved Mttod rathar than uai| a calibta* tloo cenpound oo ratairad for guelitetlve aaalyaaa. 0. Quality Crltorlo and RaMdlll Action Tto lecleeloe of QA/QC Maouroa Into ao aoalyalo pregran too little Maolag ualaaa tto raaolta aro lotorprotod and appropriate action 1* taka* when aeceeeery. Tto ability to do cble aaawaa aaa* aet of crltorlo ttot will trlggar a raapoaao or ranedlal action. Tha folloving eubeectlena daacrlto tto crltorlo that arc uaed In tto Oltratraca Aoalyalo Croup to evaluate vton quality control data indicate a need for corrective oaaauraa and vhat ranadlal action vlll be taken. 1. Quality Criteria Tto overriding guallty criterion above all other* la: po the remit Met tto Mode of tto cuetoner. Thle determination vlll be Mde Jointly botvaco tto cuatoner nod tto analyat. Tto aoalyat nwat aaerclae caution lo not allowing the cuatoner to overatato, olalnterpret or Mlnteotlonally olarapreaeot the date. In addition to thi* prlac goalIty criterion, the following coodltlona nuat be net: a. ilanka - In tto event ttot a blank producee a poaltlve value. It My not to uaad aa a valid blank If It exceede 101 of any reported value for a aanple. b. Becoverlea - Becoverlea for all ourrogate and native eplfce* suit lie In tto range of 50X<Bocovery<l}0Z. c. Proclelon - froclalon vlll to calculated baaed oo tto recoverlea of ourrogato internal atoadarda. Average recoverlea vlll be calculated with t atandard deviation for each aanpl* act. Bepli~ cate OMlyoaa and low and high native aplka recoverlea nay elee to uaad to provide additional Infomet'on/lnclght Into tto preclaioo af tbo onalyale. 29 HONS 022966 d. Llalt af tilKtlM Tka limit of IttKtlM (LOO) will aaraally ka ititil aa 4 Ik* Vila* ( tka lam Inal aatlaa aylkt II ft la rKtntal and faatlllaUa. Daall tka law Inal aatlaa atlka aat ka rocovarad, <ka 1M will ka atataa aa 4 tka walaa at tka ki|k lawal aatlaa aplka If It la recnerod aal taaatlflakla. tkaalf aaltkar aflta ka racnered, a dec 1a1oa aaat ka node ra|atlU| tka adwlaakillty af reyreceallaf tka aaaple. tkaalf all aaaalaa ceatala aack laria taaatltlaa at tka aaalyta(e) tkat tka Inala af tka law aad kl|k aylkaa ara laalpaltleant (10t) ky ceaperieoa, tka walaa af tka LOO kacaaaa laai Important a*4 la Imply Hated aa tka LOO fat tka laetrtaeatal aaelyeia yroceaa determined ky tka amalyala af otaadarda aad tka aklllty to ikdvk a. Accuracy - Tka accatacy at tka aaalyaat la kaat dtttrained ky aaalytlmt aoaa aaayla wklck caata laa tka amalyta at aaaa predetermined Inal (a.p., aa nt ataadardltad aaayla). If tkla tyya al ataadard la aat nallakla tkaa tka law lewel and ktgk Inal aylkaa caa ka uaed aa a aaaawta af tka accuracy af tka aaalyaat. kaaalta aaat fall wltkla a raa|a af 711 ta 1201 af tka encoytod walaa far tka aaalyaat to ka considered valid, valid. If tka akovv yuallty crltarla ara not aat tka analyst will lnedlately atian tka ated for and axtaat of raaadlal action tkat aay ka necessary 2. kamadlal action Tka flrat cnraa of action will ka for tka aaalyat and/or trowy loader ta caatact tka cuatoaar and dlacuaa tka raaulta yolatlng out tka llmltatlamo of tka data Indicated ky tka auallty central raaulta. At tkla point tka narrldlay yuallty criterion of cuatoaar aaada will ka addraaaad flrat. It canid ka tkat tka cuatoaar'a aaada ara aat wltkout moot log ana or aora of tka etker criteria. In euck a caaa no raaadlal act loo la aacaaaary. it could aleo ka tkat tka cuatoaar kaa auck a daaaad for ticktoast ta tka raaulta tkat kla aaada ara not aat nan tkougk tka etker duality crltarla arc. Tkla would tripper further aaalyaaa wltk tlpkcar duality control daalpned around tka raaulta ektalaed (a.., rayllcatlaaa of yoaltlwee to kattar aatakllak yraclalaa n aylkaa af non'detectad aanylaa to kattor aatakllak tka . llalt at datectloa). la conanltatloa wltk tka cuatoaar additional cayarlaanto will ka daalynad lnclodlng tka appropriate duality coatrol to altlaataly prowldr tka raaalta af enfflcleat duality to aaat tka cuatoaar'a aaada. IT. kata Tkla eectlea daall wltk tka aakjact of data pad kow tkay ara ekutaad, racordad and radacad aa aa ta ka aaaaklo la a report aad yat raadllp awallakla far referral and laapoctloa. HONS 022969 29 Th* aaaylae *111 h* labeled *itk 1*1 Makar at aaayle login according t* tka yrncakare kaacrlkak la tka ISC Sactlaa W Maaaal. Wkaa kallvarak t* tka raayaaalkla tackalcal paiwa, tka aaayl** aar thn racalvn aMltlaaal lakallag aa kaaaak aataaary. lkia aMltlaaal lakallag will ka linaaitat la a laboratory lagkaak aak/ar aatakaak. Three lagkaaka aak aotakooka *111 ka aaak by tka aaalyata ta ratari all yartlaaat vara aak raaalta ohtaiaak fraa tka aaayla*. Tka lakeratary aatakaaaa all] ka fillet eat la accerkaac* vltk Itoaaaato Balkan getakaek fretakaraa. All raw kata gaaeratak far a glaaa yrejact, *blch caaaat ka ceanraalaatly ylacek ta tka lakaratary aatakaak (a.|., chraaatograa*, caayutar aalfat, ate.), will ka filet eater aaaa yraacrlhok arkar (l.a., lag aaakar) la a caatral file eater tka eeyerrleea at tka yrejact leaker aat/er QA tyaclaltat. Heat of the kata taaaratak ky tka Oltratraca Aaalyata Creep are coayater kata atarak an aafaatic ktace. la arkar ta arcktaa tkeee kata tka ayaclfic file aaaa aak klac aaakar aaaociatak !tk tka aaalyata *111 ka written town ta tka lakaratary aatakaak aat/er Inatroant lagkaak. Wkaa tka ktac la caaylataly fall af kata aa aactra aaellted klac iaaga ar cayy ef tka fllaa aa tka klac *111 ka traaafarrak ta magnetic taya. A lagkaak will ka kayt far racarklag tka klac amber, am aak yrafla aeeoclatat with It. alaag with tka aaaaclatak taya aak file aaakar ta wklck the klac waa traaafarrak. An aaaayla of each a logbook la glean la rigvre 3. Wkaa the kata arc traaafarrak a verification yrograa la aaak to ckack all traaafarrak racorka far carractnaaa. When tayaa are flllek (they tyylcally kolt erven ta tea klac laagaa) they chowlk ka atarak la a flreyroef vaalt. All calcalatloaa al the raaalta ef the kata will be eyed flak la the artkok aaak. Theee triolet lane will bo aatarak la the aaalyata laboratory aatakaak walaaa they are ceaywtat gaaaratck. la thla caaa, a cayy ef tka coayater outywt will ka flick with tka raw kata. The Project leaker will be reeyoaalkle for checking the cerrectneao af tka kata. V. Scania Pleoocal Smylaa util ka kleyoeek af la accarkaaca with the laetrectlene aa tka Aaalyala legweat fan. Tka aaly axcaytlon ta thla aaalk raault whoa tka aaalyala ovarii a yroblaa which mini aaayl* klayaaal la a aaaaar ether than chat arlglaally ayaclfiak. If the Project Leaker aataa fraa the reeulte af tka aaalyala that a yotmttally taalc yrakwet waa yraaaat la tka aaayl** than th* amylaa *111 k* klayooak ef la a aaaaar kaaaak oaf* ky tka Safety kayarnaat. Tb* kata ef aaayl* klayaaal aak tka aaaaar ahoalk k* aotak aa th* rageeat fen atarak with tb* raw kata caayletlag th* chata ef cuataky ef tka aaayl*. HONS 022970 30 tm lnMttn) (mi* n /*> i_ /J> />v **> 0KJ Om) *f a* . I *M Mi A/3 I . J I J' l 0mm G*Hc) C*>Wt) G*Wi> foWt) >*** f BO iiJ ti*3 Im3 IK* *, lMd [Hfi *H** jM> j^yfc, B#fl is* Wfi 0*f*\ V'V/ti 6MQ) J-Ai /|J >31 (trO t**l 3-ii-tJ i> (<*) t/*J sn ' / r*t4)i/*0 - - 4r<McjiyM4-ftgPntf.*h. 394 <V*M / i/arin 6 0 n(s) %S& SD?0) "3 (rBAi3/Kl |nl Vfyb /n flb*) f<*cj - ' -i' Jr <k>*/ tf <*) (3* (#i) liwQ 5*1 3*Arj iiu (**#) C*al s 3/*to >$K i*// '*i0 W** >4^ Jtyl s/;Uts Hinlt* W}M Hi. (Ho*) /f> i . / i s2> *rm* 03*13(7) 1 33 >73<P> /<// Ml*) | | | 3.3 > (<J7 HS ws) y//3 Q>13 (iV /Vfc (mo) m (Moi) HJ (Mel) ffl (Jt+) ,, <50 * 4* (U) / < M*/j ^cj fcn* tcu 6*> | . M?i (***> 4l ss U*ths Units ->3 l/**ho 31 i/jtfu St 1 ifcVb ijkvb x\Jsih3 *S -7// otX " &K c*tt. (jJ tb v (J> ** *- y b - v 6*-*. (0 W> ?*($ fe>i* (1) f ft) ncou 3. Caaapl* of lUC/Iin L|koM mi. HONS 022971 31