Document evdOq9p34e8w1NxJMVd4ekJw9

E S C -U A G -8 6 -1 3 a rra e : ANALYSIS OF TOTAL PC8 CONGENERS IN KRtfM RICH PLANT SO IL SAMPLES ____ StEH/ESC rtoTOTV. /Dept./locafldin REPORT NO.: MSL-5452 ESC-UAG-86-13* JOB/PROJECT NO.: 6204 DATE: February 21, 1986 TITLE: ANALYSIS OF TOTAL PCB C0N6ENERS IN KRUHHR1CN PLANT SOIL SAMPLES AUTHORS: B.M. Hughes, 0. McKenzie and C. Trang ABSTRACT: Krunerlch Plant Soil samples were analyzed for total PCB congener concentrations using capillary GC/EC and capillary GC/MS analysis techniques. These samples are associated with the clean up of a chemical storage area. No samples contained total PCB congeners at levels above 50 ug/g. AUTHORS: b .M . H ughes, 0 . M cK enzie a n d C . T ra n g ti .gMIAI M SI-$452 TECHNICAL APPROVAL: P.L. Sherman ~ Environmental Sciences Center Senior Research Group Leader APPROVED BY: Environmental Sciences Center Quality Assurance Specialist APPROVAL DATE: ^ 0239LQ COMPANY CONFIDENTIAL This document it the property oi Monsanto Company and the recipient is responsible for its safekeeping and disposition. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorized persons or sent outside the Company without proper authorization. DISTRIBUTION COPY NUMBER J. Gloeckner - 1740 2. B.H. Hughes - U4E 3. 0. McKenzie - U4F . C. Trang - U4F S W.M. Mees U40 6. P.L. Sherman - U1F 7-9 Reports library - R2C 10 Chesterfield Information Center - AA3A ABSTRACT ONLY H.A. Wo Hermann - U4E MONS 023911 This report has been assigned to you. When it is no longer needed, you are responsible for returning it to: If you transfer it to anyone else, please let your librarian know, so the records can be changed. -ia;c> tarv. i/ot Time Stamp <860305.1219> ANALYSIS REPORT DATE: February 21, 1986 LOG NUMBER: U-86-01-29-01 PROJECT NO: 760.28-6204 TO: Jim Gloeckner/Krummrlch Plant FROM: Environmental Sclancaa Cantor Moneanto Company 800 N. Lindbergh Blvd. St. Louis, Mo. 63167 Phono No: (314) 694-1464 Title: Analysis of Total PCB Congeners In Erumnrlch Plant Soil Samples. ABSTRACT Krumnrlch Plant Soli samples were analyzed for total PCB congener concentretratlone using capillary GC/EC and capillary GC/MS analysis techniques. These samples ere associated with the clean up of a chemical storage area. No samples contained total PCB congeners at levels above 50 ug/g. INTRODUCTION Six soil samples were analyzed for total PCB congener concentrations. These analyses are required as a part of the Krumnrlch Plant cleanup of an area where chemicals had previously been stored. Initial extraction and screening CC/EC analyses Indicated that electron eepturlng compounds were present which lntsrferred with the low level analysis of PCB congeners. After column cleanup of the soil extracts, low levsl CC/EC scrsenlng Indicated that less than 50 ug/g total PCB congeners were present. Since the PCB congener pattern was not Identical to an Aroclor formulation, GC/EC analysis methods which require that the Aroclor pattern be very slmller to a standard Aroclor for mulation, could not reliably be used. Therefore, a GC/MS method was used which quantified each PCB congener class (1. a. each set of congeners with e given number of chlorine atoms). The total concentrations of the ten PCB congener olesses were determined from the capillary GC/MS analysis of the cleaned up soli extracts. Very good agreement was obtained between the total concentration based upon this GC/MS data and the GC/EC screening data. SUMMARY MOMS 023912 Table 1 summarizes the results of Initial capillary GC/EC screening of the cleaned up soil extracts. Note chat no soil contained greater than 30 ug/g total PCB congeners based upon this semi-quantitative analysis method. Tables 2 through 5 summarize In more detail Che results of capillary GC/MS analysis of the cleaned up soli extracts. The values reported In these latter tables agree very well with the results reported In Table 1. Refer to Standard Extraction Methods PCEX21 and PCEX03 for the details of how the samples vers extracted and claanad up and rafar to Standard Analysis Methods ECAN02 and MSAN03 for tha details of how the claanad up axtracts wera analyzad. This Information la Included In a lacar section of this report. QC RESOLTS Quality control results are shown In Tablss 1-6. Tables 1-5 show re coveries of surrogate compounds which wera added to each sample before extraction. This Information Indicates how wall each soil sample was extracted. Triplicate analyses of T 448262 are shown in Table 2; duplicate analyses of T 4445(4 are shown In Table 3; duplicate analyses of T 444251 are shown in Table 4; and duplicate analyses of T 44S47S are shown in Table 5. Table 5 also shows tha results of analyzing an Aroclor 1260 standard using tha same analysis protocol which was used for tha toll extract analyses. Vary good agreement was seen between the expected Aroclor 1260 concentration (12 ug/g) versus the detected total PCS congener concentration (13.6 ug/g). Finally, Table 6 summarizes recoveries of Aroclor 1241 which was added to a Blank Soil sample and T 444531. These data show that good PCS congener recoveries would be expected using these methods for the analysis of soils from the Krummrleh Plant. DETAILS Standard Sampling Method No(s): Samples supplied by the Krummrleh Plant. Standard Extraction Method No(s): PCEX03 and PCEX21 (See PCFS03 and FCFS21 for flow sheets describing these methods.) Standard Analyels Method No(s): ECAK02 and MSAN03 Final Report File No(s): A20418 Table File Ko(s): B2041S, C2041S, D2041S. E2041B, F2041S, C2041S Alto Included In this report are: 1) Summaries of Standard Extraction and Analyels Methods used for this project. 2) Analysis Raquest Information recorded at sample login. 3) A copy of the ESC/UAC Good Laboratory Practices Manual. ANALYST(S): >. Mason Hughes, David McKenzie and Chi Trang ANALYST APPROVAL: HONS 023913 TABLE X. Suaaary of FCB Concentration* In Soil Saaplaa Estimated by Visually Coaparlng rCB Pattern Intensities with an Aroclor 1262 Standard. Standard Analyala Method ECAN02 was used for extract analysis. ESC Project No: 760.28 - <204 Sample I.D. Surrogate Recoverlas(tRecovery) CLS-benzene 2.4,6-CL3-blphenyl Date: February 20, ISIS Estimated FCB Concentration (ug/g) Blank Soil 113 63 T 448262 (DUF.) * (TRIF.) 109 100 102 133 95 92 T 444584 (DOF.) 85 109 176 103 T 444531 109 161 T 448251 * (DOF.) 50 44 94 84 T 448373 45 84 T 44B47S * (DUF.) SO 58 77 78 Method Blank 53 97 Footnotes: a. ND- Nona Detected 1.0 ug/g) TABLE FILE NO: B20418:MH ND (a) 23 2 2 5 10 5 ND (a) MONS 023914 Table 2- Results of Total PCBs Detected Oalng Standard Analysis Kathod MSAMOS. Tina Staap - <860221.0812> Project No: 760.28-6204 Data: February 20, 1986 T 448262 Analyta LOQ(a) (ug/g) CLl-blphenyls CL2-biphenyl* CL3-blphenyls GLb-biphenyls CL5-blphenyls CL6-blphenyls CL7-biphenyl* CLS-blphenyle CL9-blphenyls CLlO-blphanyl 1(C) * * " * * * * NQ(b) m m 5.0 S.l 5.9 2.4 0.5 1.5 Total PCBa (ug/g) 23.4 Surrogate Spiking Approx. Aaount Coapound Added (ug/g) Sampla Idantlflcation T 448262 (duplicate) T 448262 (triplicate) Concentration (ug/g) NQ NQ " " 5.9 5.5 4.1 8.2 6.2 3.8 1.5 3.9 1.0 0.6 0.8 0.6 19.5 22.6 Recovery <%) CLS-benxene 1.0 109 2,4.t-CL3-blphenyl 2.0 133 100 102 95 92 Documentation ESC Extraction Method Date of Extraction Saaple Aaount Extracted (g) Extract Finol Volume (ml) Extract Dilution ESC Extract or Saaple Nunbar Data of CCC/MS Analyst* MS FEN PCEX21 1/30/S6 1.2244 10.0 none PCB-1323 2/5/86 >L094S PCEX21 1/30/86 1.0899 10.0 none PCB-1524 2/5/86 >L0946 PCEX21 1/30/86 1.1777 10.0 none PCB-1523 2/5/86 >L0947 Footnotes: (a) LOQ - Llalt of Quantitation In ug/g. Slgnal-to-nolee ratio 1* greater then 10 when this amount la analyzed using the above referenced Analytical and Extraction Methods. Tha following lattara Indicate how this value was determined: E estimated from standard analyzed under the some conditions. (b) MQ Not Quentltatabl*. Tha congener concentration is below the LOQ value. Table stored In file: D2041S Analyst(*): B. Maaon Hugh**, David McKenzie and Chi Trang Analyst Approval^ ___ HONS 02391$ Table 3. Results of Total PCS* Detected Method MSAN03. 0lng Standard Analysis Tina Stamp - <160221.0812> Project No: 760.28-6204 Data: Fabruary 20. 1916 T 444584 Analyte CL1-biphenyls CL2-biphenyls CL3-blphanyla CL4-biphenyl* CLS-blphanyl* CK-biphenyls CL7-biphenyls CLS-blphanyl* CL9-blphsnyla CLlO-blphanyl Total PCS* (ug/g) LOQ(a) ("S/S) 1(E) * * ' " * NQ(b) m m " m " m " Sanpla Identification T 444584 (duplicate) T 444531 Concentration <"8/S> NQ NQ m m * N m Surrogate Spiking Approx* Amount Compound Added (ug/g) Recovery (%) CL5-benzene 2.4.6-CL3-blph*nyl 1.0 2.0 85 176 109 109 103 161 Documentation ESC Extraction Method Data of Extraction Saapl* Anount Extracted (g) Extract Pinal Volume (ml) Extract Dilution ESC Extract or Saapl* Nuabor Dat* of CGC/MS Analyala MS nut PCEX21 1/30/86 1.2991 10.0 none PCS-1326-a 2/5/86 >L093S FCEX21 1/30/86 1.2003 10.0 none PCB-1326-b 2/5/86 >L0936 PCEX21 1/30/86 1.1771 10.0 none FCB-1327 2/5/86 >L0937 Footnotaa: (a) LOQ - Llalt of Quantitation in ug/g Signal-to-nols* ratio 1* greater than 10 whan thl* amount is analyzed using the above referenced Analytical and Extraction Methods. The following letters Indicate how thl* value was determined: E * estimated from standard analyzed under the same conditions. (b) NQ Not Quantltatabl*. The congener concentration is below tha LOQ value. T*bl* atorad In file: E20418 Analyst(s): S. Mason Hughes. Dai/id McKenzie and Chi Trang Analyst Approval: Z4A- HONS 023916 Table Kesults of Total FCBs Detected Using Standard Analysis Method MSAN03. Tina Stamp <860221.0*12> Project No: 760.28-4204 Data: February 20. 1*84 Sample Identification T 444281 T 444231 (duplicate) T 448373 Analyte CL1-biphenyls CL2-biphenyl* CL3-blphenyls CL4-biphenyls CL5-biphenyls CL6*blphenyla CL7-blphenyls CLB-blphenyls CL9`biphenyl* CL10-blphanyl L0Q(a) <ug/g> 1(E) 18 " m a NQ(b) * " 1.4 0.8 0.4 NQ Concentration (vg/B) NQ a a 3.0 0.8 NQ a 0.7 NQ 2.2 3.9 0.9 1.1 0.2 0.3 Total PCBa (ug/g) 2.6 4.5 8.8 Surrogate Spiking Approx. Amount Compound Added (ug/g) Recovery (%) CL5-benzene 2,4,6-01.3-biphenyl 1.0 2.0 50 94 44 45 64 64 Documentation ESC Extraction Method Date of Extraction Sample Amount Extracted (g) Extract Pinal Voluae (al) Extract Dilution ESC Extract or Sample Number Data of CGC/MS Analyala MS FKH FCEX21 1/30/86 1.0353 10.0 none PCS-1530 2/5/86 >L0938 FCEX21 1/30/86 0.9917 10.0 none FCB-1531 2/5/86 >L0939 PCEX21 1/30/86 1.1089 10.0 none PCS-1532 2/5/86 >L0941 Footnotaa: (a) LOQ Limit of Quantitation In ug/g. Slgnal-to-nolsa ratio la greater than 10 whan thla amount Is analytad using the above referenced Analytical and Extraction Methods. The following letters Indicate how thla value was detsrmlned: E - estimated from standard analyzed under the same conditions. (b) NQ - Not Quantltatabla. The congener concentration la below the LOQ value. Table stored In file: F20418 Analyet(s): B. Meson Hughes. David McKenzie and Chi Trang Analyst Approval: HONS 023917 Table 5. Kotultl of Total PCBa Detected, Osing Standard Analysis Method MSAN03. Tina Staap - <860221.0840 Project No: 760.26-6206 Data: February 20. 1886 Saapla Identification T 648478 Analyte CLl`biphenyl* CL2-biphenyl* CL3-blphenyls CL4-biphenyl* CLS-biphenyl* CL6-blphenyl* CL7-biphenyls CUblphenyla CL9-blphenyls CLlO-blphenyl Total PCBa (ug/g) L0Q(*) (ug/g) 1(E) a m n m N n a NQ(b> ft " ft ft a Surrogate Spiking Approx. Aaount Coapound Added (ug/g) T 448478 (duplicate) 12 ug/g Aroclor 1260 Standard Concentration (ug/g) NftQ NQ ft ft ft ft ft ft ft ft ft ft 6.6 8.1 0.8 NQ ft 13.6 Recovery (t) CL3'benzene 2,4,6-CL3-btphenyl Documentation 1.0 2.0 80 38 58 78 * BSC Extraction Method Date of Extraction Semple Amount Extracted (g) Extract Final Volume (ml) Extract Dilution ESC Extract or Saapla Number Date of CCC/MS Analysis MS FRN FCEX21 1/30/86 0.9979 10.0 none PCB-1S33 2/5/86 >L0942 PCEX21 1/30/86 1.0311 10.0 none PCB-1534 2/5/86 >L0943 2/5/86 >L0850 Footnote*: (a) LOQ - Limit of Quantitation in ug/g. Slgnal-to-nolae ratio la greater than 10 when thia aaount la analyzed ualng the above referenced Analytical and Extraction Methoda. The following lettera indicate how thia value waa deternlned: E - eatlaated froa atandard analyzed under the aaae condition*. (b) NQ - Not Quantltatable. The congener concentration la below the LOQ value. Table atored in file: C20418 Analyat(a): 8. Haaon Hughe*. David McKenzie end Chi Trang Analyst Approval HONS 023918 TABU 6. Suaery of Aroclor 1248 Spiking Concentratlona and licon^ln In Quality Control Exparlnanta for Soil Saaplaa. ESC Frojact No: 760.2S - 6206 Data: February 6, 1916 Saapla 1.0. Surrogata Rccovarlaa (tRacovary) Aroclor 1268 CL5 benzene 2,4,6* CL3-Biphenyl Blank Soil (L. Spike) 85 * (H. Splka) 100 121 90 Aaount Added Recovery (Ug/g) <%) 0.91 8.1 76 83 T 466531 (L. Splka) (H. Splka) 85 50 91 100 0.76 9.1 110 90 Method Blank 53 TABU HU NO: C20416-.MH 97 HONS 023919 Tha following pagaa doicrlbo Standard Extraction Mathods and Standard Analysis Mathoda usad for this projact. HONS 023920 ESC Standard Extraction Method (SEM) TITLE: PCBa In Non-EC Active Matrlcaa ESC Standard Extraction Method Ho: PCEX21 MATRI(X),(CES); Soli* and othar non-EC activ* olid* and solvents TYPICAL SAMPLE SIZE <g) TYPICAL EXTRACT VOLUME (al) TYPICAL ANALYTES: Aroclora 1232, 1242. 1248, 12S4, 1260, 1262, trlchlorobiphanyl ieonera through octachloroblphanyl laoaara 0.5 - 5.0 10 ESC Standard Analyala Maehod No*: ECAN01, ECAN02 INTERFERENCES: Any electron capturing apaclaa In the ratantlon tine region of trlchloroblphenyl laoaara through octechloroblphenyl laoaara that la non acid hydrolyzable TYPICAL SURROGATES TYPICAL RECOVERIES (%) pontachlorobonztno 2,4,6-trichloro- blphanyl 50 - 120 50 - 120 APPARATUS AMD MATERIALS: Burdick and Jackaon banzana or haxana for aaaple axtractlon or dilution. Plarca vlala. Sulfuric acid at varying concantrationa. Ultraaonlc bath. Dlepoeeble glaaavara. (Saa flow ahaat for thla axtractlon nathod In FCFS21.) LIMITATIONS: Mathod appllaa only to aatrlcea which do not contain Interfering electron capturing apaclaa In the trlchloroblphenyl through octachloroblphanyl lsoaer retention ttae region. SAFETY PRECAUTIONS: Saa PCB handling protocola In laboratory aafaty nanual. DATES OF METHOD CREATION AMD UPDATES: 12/17/84 MOMS 023921 FLOW SHEET FCFS2I FOR ESC EXTRACTION METHOD PCEX21 SAMPLE ID: EXTRACTION DATE and TIME: SAMPLE COLOR AND DESCRIPTION WEIGH OUT SAMPLE INTO A U OR AO aL PIERCE VIAL (] . MRC EXTRACT # LOC NO: SAMPLE WEIGHT SURROGATE SPIKE OF SAMPLE . [] ADD 10.0 aL BENZENE TO SAMPLE. . (| ULTRASOH1CATE SAMPLE FOR 1/2 HOUR IN A SOUND BATH. [] . . PUCE 2 aL OF THE EXTRACT INTO A 7 aL VIAL * ADD 2 aL ............. SULFURICACID AND SHAKE . (1 . . (1 . . ALLOW PHASES TO SEPARATE REMOVE 1 aL FOR ANALYSIS. [] EXTRACT NO: ............... DATE/TIME COMPLETED ANALYST: ...................... ESC JOB NO: ............. 10.0 aL FINAL VOLUME............................... HONS 023922 ESC Standard Extraction Mathod (SEM) TITLE: rets In Non-EC Active Matrlca* ESC Standard Extraction Method Vo: PCEX03 MATRI(X), (CES): Soils and other non-EC active solids,solvents and oils. TYPICAL SAMPLE SIZE (8) TYPICAL EXTRACT VOLUME <al) 0.3 5.0 10 TYPICAL ANALYTES: Aroclora 1232, 1242, 1248, 1234, 1260, 1262, trlchloro blphenyl laoaera through octachloroblphenyl laoaera ESC Standard Analytic Method Not: ECAN01, ECAN02 INTERFERENCES: Any electron capturing apeclaa In the retention tlae region of trlchloroblphenyl laoaera through octachloxoblphenyl laoaera which are not removed by the three-phaae allleagel column. TYPICAL SURROGATES TYPICAL RECOVERIES () pentschlorobenzene 2,4,6-trichloro- blphenyl 50 - 120 30 - 120 APPARATUS AND MATERIALS: Burdick and Jackeon hexane for aaaple extraction or dilution. Sodlua aulfata for drying the aaaple natrlx. Silica gal column, lapregnated with potaaalua paraanganata, aulfurlc acid. and potaaalua hydroxide. Nitrogen for extract voluae reduction. Dlepoeable glaaavara. (Saa flow cheat for thla extraction method In PCFS03.) LIMITATIONS: Method appllaa only to aatrlcaa which do not contain lnterferrlng electron capturing apeclaa In the trlchloroblphenyl through octaehloroblphanyl laoaar retention tine region when electron capture analytical aethods are uaad. Thla llaltatlon doea not apply to aaaa apectroaetrlc aethoda. SAFETY PRECAUTIONS: See PCB handling protocola In laboratory aafety aanual. DATES OF METHOD CREATION AND UPDATES: 2/13/84, 9/23/84 HONS 023923 FLOW SHEET PGFS03 FOE ESC EXTRACTION KETHOD FCEX03 SAMPLE ID: EXTRACTION DATE and TIME: MRC EXTRACT LOG NO: WEIGH OUT SAMPLE INTO A 14 aL VIAL (J SURROGATE SPIKE OF SAMPLE . [] FINAL WEIGHT INITIAL WEIGHT SAMPLE WEIGHT DRY SAMPLE IF NEEDED EY . ADDING ABOUT 0.1 | t) Na SO TO VIAL . 2 * . (] RINSE COLUMN WITH 2 X 20 aL HEXANE DILUTE SAMPLE IN VIAL WITH HEXANE AND PLACE ONTO CLEAN-UP COLUMN. [] . . QUANTITATIVELY RINSE VIAL ONTO COLUMN WITH 4 X 1 aL RINSES. . (] . ELUTE SAMPLE INTO 30 aL . CENTRIFUGE TUBE WITH [ ] 40 aL HEXANE. . NITROGEN BLOW DOWN TO . aL [ 1 EXTRACT NO: ............... . DATE/TIME COMPLETED ANALYST: ....................... ESC JOB NO: CLEAN-UP COLUMN DESCRIPTION 25 aL D1SP0 PIPET 1 ca Na SO 24 4 ca It POTASSIUM PERMANGANATE SILICA CEL 1 ca SILICA CEL 4 ca ACID SILICA GEL 1 ca SILICA GEL 4 ca BASE SILICA GEL \/ \/ GLASS WOOL HONS 023924 ISC Standard Analyala Mathod (SAX) TITLE: Aroclor Foraulatlona In Solvanta ESC Standard Analyala Nathod No: ECAN02 ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-5880 Capillary CC/EC lncarfacad to an HP-3357-LAS Laboratory Data Syataa TYPICAL ANALYTE TYPICAL INSTRUMENT LEVEL OF DETECTION (LOD) (ug/al) Aroclor foraulatlona 1232, 1242, 1248, 1254, 1280, and 1282 0.1 TYPICAL PRECISION 9 10X LOD <*> 30 TYPICAL ACCURACY 10X LOD () 30 INTERFERENCES AND LIMITATIONS: Any alactron capturing apaclaa In tha reten tion tlae region of trlchloroblphenyl through octaehloroblphenyl laoaera are potential lntarfarancaa. Exact retention tinea of Boat likely PCS laoaera can be obtained froa the analyala of Aroclor 1248, Aroclor 1254 or Aroclor 1280 foraulatlona. CHROMATOGRAPHIC COLUMN: 30-aatar fuaed alllea J&U DB-5 (0.25 uM) with wide bore (0.32aa). COLUMN TEMPERATURE PROGRAM: 130(l)/4/300 INJECTION TYPE: Splltlaaa CALIBRATION AND STANDARDIZATION: Uae Internal atandard quantitation technique and calibrate lnatruaent reaponae factora froa authentic Aroclor foraulatlon atandarda. Uae a alnlaua of 10 PCB laoaera for the deteralnatlon of foraulatlon Identity and quantity. CALCULATIONS: Foraulatlon concentration (laoaer RRF)(laoaer area/lntemal atandard area) where: RRF la the relative roeponra factor for tha appropriate PCB laoaer In a given foraulatlon. Foraulatlon concentra tion la obtained froa the average of at laaat 10 auch cal culation#. SAFETY PRECAUTIONS: See PCB handling protocola In laboratory aafety normal. DATE OF METHOD CREATION: 10/25/83, 2/3/84 Tlae Scaap - <880221.0804> MONS 023925 ESC Standard Anelyil* Method (SAM) TITLE: Organic Compound* In Solventa ESC Standard Anelyala Method Mo: MSAMO3 ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-5985/5987 Capillary CC/MSSelaeted Ion Monitoring with RTE-VI oparatlng eyeten. Typical Run Tin: Typical MultiplierVoltage: Typical Dwell Tinea: Maxlnua of Maaaaa: Electron Energy: 3-40 Bin. 1800 - 2800 eV 200 500 asac/nass 20 naaaea x 5 rangaa - 100 aasaas 70 aV TYPICAL ANALYTE TYPICAL INSTRUMENT LEVEL OF DETECTION (LOD) (ug/Bl) Organic Coapounda eluting between toluene and n-C34-ana 0.01 - 0.1 TYPICAL PRECISION g 10X LOD <*> 30 TYPICAL ACCURACY g 10X LOO (%) 30 INTERFERENCES AND LIMITATIONS: Analyte characterletlc naaa nuat be chroaatographlcally raaolvad froa other eluting coapounda which produce the aaaa Bate. CHROMATOCRAPHIC COLUMN: 30-aatar fuaad alllca J&U DB-5 (0.25 uM) with wide bora (0.32 an) COLUMN TEMPERATURE PROGRAM: 50(4)/8/300 INJECTION TYPE: Splltlaaa CALIBRATION AND STANDARDIZATION: Quantitative: Uae Internal atandard quantitation technique and calibrate InetruaenC reaponae factora froa atandard aolutlona of analytea of Interact. Qualitative: When aultiple characterletlc naaea are aonltored for a given analyte, the ratio of characterletlc aaaa reaponeea auat be within 20* of thoee for the authentic atanderd. For PCB analyaea, the characterletlc naaaea which are aonltored are the aoleculer Ion containing all 35-CL leotopae and the aoleculer Ion containing one 37-CL laotope. The following table euanarlzea the aaacee and approxlnate retention tine reglone aonltored for the analyala of Internal atandard, aurrogate atandarda, and chloroblphenyl (CL-BP) through decachloroblphenyl (CL10-BP) PCB congener*. MONS 023926 Analyte CL-BP laooera, anthracene-dlO CL2-BP laoaer* Pentachlorobenzena aurrogate CL3-BP laooera CL4-BF laoaer* 3,4,3',4*-CL4-BP-d6 aurrogate CL3-BP laooera CL6-BP laoaer* CL7-BP laooera (b) CL*-BP leoner* CL9-BP laoaer* CL10-BP Hessee 188,190 222,224 247.9,249.9 255.9.257.9 289.8,291.8 296.29S 323.9,325.9 357.8,359.8 323.9,325.9 391.8,393.8 427.7.429.7 461.6,463.6 497.6,499.6 Retention Tine* (nlnutee) 16 - 22.5 16 - 22.5 16 - 22.5 16 - 22.5 22.5 - 30 22.5 - 30 22.5 30 22.5 - 30 22.5 - 30 30 50 30 - 50 30 - 50 30 - 50 Relative Retention Tinea (*) .0.60 .0.60 .0.60 .0.60 .0.84 .0.84 .0.84 .0.84 .0.84 .1.12 .1.12 .1.12 0.84 0.84 0.84 0.86 1.12 1.12 1.12 1.12 1.12 1.87 1.87 1.87 1.12 - 1.87 (a) Relative Retention Tinea calculated ualng a retention tine of 26.7* nlnutea for 3,4,3* ,4'*CU-JP-d(. (b) CL7-BP leoner* are analyzed ualng either CL2-lo*a characterletic Iona (n/e 323.9 and 323.9) or nolecular Iona (a/e 391.( and 393.(). CALCULATIONS: Analyte concentration - (Analyte area)/[(Analyte RRF)(IS area)] where: Analyte area la the characterletic use area of the analyte. RRF la the relative reaponae factor for tha analyte. IS la the Internal atandard and le ueually anthracene-dlO. RRF - (analyte area In atandard)/[(analyte cone.)(IS area)} PCS eoncentraclona are calculated In one of two waya: 1) If an Aroolor fornulatlon can be Identified fron the pattern of PCS laooera, aeleeted PCS laoaer* or claaae* of laoaer* (1. a. all CLA-blphenyl laooera) are uaed to quantify tha Aroclor concentration. Relative Raaponae Factor* are calculated ualng tha concentration of the total Aroclor for- aulatlon In the abova RRF aquation. 2) If no unique Aroclor forauletlon la preaent, then the total PCS concentration la calculated by ualng atandard aolutlona containing known aoounta of chloroblphanyl through deeachloroblphenyl laooera to calculate Relative Reaponae Factora for each chlorine claae In the above RRF equation. The RRFe for the eorreepondlng PCS laoaer cleaeee ere uaed to calculate total PCS laoaer concentration of each claaa In unknown aanplee. SAFETY PRECAUTIONS: Sea PCS handling protocol* In laboratory aafety aanual. DATE OF METHOD CREATION: 12/9/S3 Tloe Stanp <860220.1442> HONS 023927 Th following pagaa daacrlba Analytical Raqua.t Infornatlon ganaratad for this projact. HONS 023928 Tina Scamp - <860220.1432> MONSANTO COMPANY/ENVIRONMENTAL SCIENCES CENTER ANALYSIS REQUEST DATE: 1/29/86 LOC NO: U-86-01-29-01 REQUESTER: Gloc.cltnar/Krummrieh PROJECT NO: 760.28 - 6204 REPORT RESULTS TO: FILES/MEES, Shaman, Hugh.., HcKanzla, Trang ANALYSIS REQUESTS SENT TO: FILES, Maaa, Hugh.., HcKanzla, Shaman, Trang SAMPLE PICKUP BY: Hughaa SAMPLE LOCATION: U-420 SAMPLE DESCRIPTION FOR 6 SAMPLES SAMPLE IDENTIFICATION NUMBER OF BOTTLES ESC NUMBER(S) T 448262 T 448478 T 444564 T 446251 T 444531 T 448373 Mathod Blank Blank Soil Blank Soil plua LS Blank Soil plua HS 1X4 oz 1X4 ex 1X4 oz 1X4 oz 1X4 oz 1X4 oz PCB-1523, PCB-1524-DUP, PCB-1525-TJ PCB-1533. PCB-1534-DUP PCB-1526-A, PCB-1526-B-DUP PCB-1530, PCB-1531-DUP PCB-1527, PCB-1528-LS, rCB-1529-HS PCS-1532 PCB-1533 FCB-1520 PCB-1521 PCB-1522 NOTE - DUP rafar* to dupllcata analyses, TRIP rafara Co Crlpllcata analyse., LS rafara to low lavol natlva aplka, and HS rafara to high laval natlva aplka. PCB-1526 vara labalad tha aaaa but kapt aeparata and aaalgnad -A and -B In ordar to dlffarantlata batwaan Chaa. All aaaplaa wara elaanad up ualng PCEX03. Extracta vara ldantlflad with an *C* following tha abova ESC nuabara. RECORDED BY: HcKanzla REQUIRED ANALYSES: FCBa ANALYTICAL TECHNIQUES: TECHNIQUE (EN) DATE COMPLETED x CCCC/MS (18) 2/21/86 X CC/EC (18) 2/21/86 QUALITATIVE: X SEMIQUANTITATIVE: REQUIRED QA/QC: SEE COOD LABORATORY PRACTICES MANUAL QUANTITATIVE: X COMPLETION DATE REQUESTED: ASAP HONS 023929 COMMENTS: SAMPLE DISPOSITION: HOLD FOR 30 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL ANALYSIS REQUEST FILE NAME:AA204:LI HONS 023930 Th Ninui1. following it 4 copy of th ESC/UAG Good Icborctory 1 Prctlcs HONS 023931 Copy Nuabr: GOOD LABORATORY PRACTICES MANUAL A Guide to Quality Control/Qualltv Aaeuranct Ultratrace Analyala Croup March 1984 Group Laadar, 01eratract Analyala . --------------------- - B. A. Woltenann Manager, Envlronaantal Sclaacaa Center laaued toi Date: JR3/J0B A Environsental Sclancet Canter Dayton Laboratory Dayton, Ohio 45407 HONS 023932 TABLE OF CONTENTS 1 Objective* 11 Scope 111 Analyal* A. Method* B. QA/QC Frograa 1. Saapi* Preparation QA/QC *. Method Blank* b. Replicate* c. Spike* 2. Instrumental Analyal* QA/QC a. Initruaentatloo b. Blank* c. Quantitation Internal Standard d. Standard* C. Degraa* of Quantlt*tlon 1. Qualitative Analyst* a. Tentative b. Confined 2. Seal-Quantitative Analysis 3. Quantitative Analyal* D. Quality Criteria and ReaedlalAction 1. Quality Criteria a. Blank* b. tacoverle* c. Precision d. Limit of Detection *. Accuracy 2. Reaedlal Action IV Data V Saapl* Disposal FIGURES figure 1 Baaaple.of OC/MS Logbook page 2 Example of CC/IC Logbook page 3 Exaapla of Dlac/Tape Logbook page Hi' 1 1 ! 1 2 2 2 2 2 } ] * 4 4 4 7 7 7 7 7 S g 8 g g 9 9 9 9 10 *Stf 5 6 11 HONS 023933 I. Objectives Tha sain objectives of the Ultratrace Analysis Croup quality aeauranca/quallty control pro|raa arai 1) to aaaura that our laboratory |anarataa high quality results; and 2) to nalntaln tha oeccaaary racorda that document laboratory performance. II. Scope The acopc of thla nanual Include! areaa of CLP not specifically addreaaed In the ESC aectlon nanual and expanda upon certain areas where QA/QC practices dlffar froa those described In the section nanual. It is Intended to be used along with the aectlon nanual to provide a conplete picture of the CLP within the Ultratrace Analysis Group. 111. Analysis The generation of analytical results within the Ultratrace Analysis Croup routinely Involves two processes: aanple preparation and lnstrunantal analysis. Sanple preparation Involves ooa or nore of a variety of techniques including extraction, dilution, scId/base washes, coluan chronatography, concentration and nuneroue other techniques to render the aanple In a suitable condition for lnstruawntal analysis. Inetrunental analysis takes the suitably prepared aanple and Introduces It Into an analytical lnstrunent to neasure the desired paranetar(a). Both of these processes can be described by clearly defined and separable nethode called aanple preparation netbods (SPMs) and lnstrunental analysis ncthods (IAMa). SPMs and IAMs nay be conblned In nuneroue ways (depending upon the nature of the aanplea and the needs of the customer) to produce a successful analytical protocol, for exanple, several different SPMs nay be used to produce aanplea that are suitable for analysis by a single 1AM. The neasuree Incorporated Into each of these experlnental processes to ensure that an asaessnent of tha quality of the results can be nade constitute the QA/QC progran for a project. The following subsections describe the elenente of the analysis process: A. Methods Methods are the written docinwntatlon that describe the analytical process. They contain sufficient detail such that a conpetent scientist or technician can readily perform the required analyses. The usual practice la to have netbods that describe the sanple praperatlon process (SPMs) and netbods that describe the lnstru nental analysis process (lAMs). Each nethod developed within the Ultratrace Analysis Groups la assigned a nethod niaber as described In the ESC Section Manual. Methods ars obtained froa various aourcas Including In-house developaent, nodlflcatlon/edaptatlon of literature netbods, or specific protocol netbods dictated by government agencies. Methods nay be formally validated by a aeries of experiments that describe a classical validation protocol or nay be lass vigorously proven ovlng to factors such as frequency or use, customer needs and 1 HONS 023934 coet/tlmlng rtetrlctione. In any case a QA/QC progran la applied to tha analysis proeaka to provide a measure of the quality of tha raaulta. Unless a QA/QC progran la praacrlbcd by a required protocol ETA Dioxin In Soil protocol), certain elnlM QA/QC aeaauraa (depending upon tha analyala type) are Incorporated Into all Ultratrace Analyala projecta. The following aubeectlon deacrlbea the Ultratraca QA/QC program: S. QA/QC Program An effective QA/QC progran Incorporatea experlnenta that provide Information relative to each of tha following queatlona: (1) Are thera any lapurltlee, background or contaalnatloo that will Influence the reaultaT (2) Bow reproducible are tha results? (3) Bow well can the analyte be recovered froa tha eanple matrix? (A) Vhat la the limit of detection for the analyala? (3) Vhat la the dynamic range of the analyala? (6) Vhat la the accuracy of the analyala? All of theae queatlona are addreaaed by properly eelectlng/applylng the uae of blanka, repllcatea, aplkea and etandarda In a QA/QC program. The dlacuaalon of the uae of theae QA/QC technlquee aa they apply to Ultratrace Analyala Group actlvltlea la beat done by conalderlng the aample preparation and lnatriaental analyala proceaaea aeparately. 1. Sample Preparation QA/QC a. Method blanka - kepreeentatlve glaeeware, advance and reagenta are uaed with aample matrlcee which are almllar to thoee for which reaulta are being reported, yet do not contain tha analytea of lntereat. Method blanka are analysed at a frequency equal to 10Z of tha analysed samples for aample seta which are multiples of 10. At least one method blank la analyzed for aample sets containing between 1 and 9 samples. b. kepllcates - If sufficient sample amounts have been submitted for analyala, replicate frequency la the same as tha method blank frequency. If at all possible, replicates should be obtained from the earns sample bottle In order to minimize sample lnhomogenelty problems due to samples being taken at slightly different times. c. Spikes - If sufficient sample la available for each sample type, the sample Is split end spiked at two levels with HONS 02393S 2 tb native (unlabelad) analyte(o). The levala are typically 2* (lev) and 2Ox (high) tha anticipated detection Halt and atrva aa a technique for eetlnatlnt the Halt of detection for each natrlx. Theae low and hl|h aplkea are conducted at a frequency equal to tha Method Blank frequency. Obvlouely aplklng with the native analyte cannot be done for wldeecan analyele elnce thla preeuppoaee knowledge of the Identity of the analyte(a) In the aaaple. Other aplklng technlquce are uaed to evaluate the extractlon/recovery efflclendee for the analyte(a) of lntereat. Ideally extraction/recovery efflclendee are detenlned for eaeh tuple, elnce. In principle, each aaaple nay repreaent a different natrlx. Thle can be done very eaelly when the detection technique le aeea epectroaetry If an leotoplcally labeled veraloa of the analyte(a) la available. Docuaentatlon of axtractlon/recovery effldenciea la not required for each euple If the aaaple natrlx for a act of eaaplae la conetut. Bowever, for a aaaple aet for which the alallarlty of aaaplea la not known, and for which adequate auple la available, each auple auet be apllt and aplked with a known aaount of the analyte(a) of lntereat to determine extraction efficiency. If adequate aaaple alee la not available or the Identity of the analyte(a) la not known before the fact (l.e., wldeecan analyele), eurrogate aplklng coapounda aay be uaed to aaaeaa extraction efflclendee la each aaaple without actually aplklng each auple with the analyte(a) of lntereat. The choice of the eurrogate aplklng coapound la tailored for uch analyte. Thla eurrogate auet be cboaen ao that It la either chulcally Identical to the analyte of lntereat (for axnple ualng leotoplcally labeled analoguea of the ualytea), or la cloaely elallar In terma of llquld/llquld partition proportion, chulcal ruction propertlea, coluan elution propertlea or other matrix 1eola tion propertlu which are uaed to leolate the analyte(e) froa the Maple matrix. Another property of the eurrogate aplklng compound la that It not be preamt In the eaaple being analyzed Inatrmental Analyele QA/QC The final atop In obtaining analytical raculta lnvolvea the one of u appropriate lnetnxeentel technique to produce the analytical data Several QA/QC practlcea auet be Incorporated In thla proceao to enaure validity of the data. a. Inatruentatlon Careful docuaentatlon of lnetruaent uuge, calibration, and maintenance la eaeentlal for the generation of hlth quality reaulta. Bach aajor lnetruaent within the Ultratrace Analyala Group will be the aealgned reepooelblllty of a proftealonal uployee deelgnated aa the lnetruaent Steward. The Inatruent Steward la reaponalble for aaklng aura that logbooka are avail able and properly coapleted by lnatruaent uacra. It la the 3 HONS 023936 iiifOMlblllCy of ucb Individual using the equipment to rteord all the partlnant data required la the logbook. An example of a page from a GC/MS logbook la glvan In rigura 1 and that of a CC/IC logbook la glvan In figure 2. Inatruaanta will ba callbratad according to tha lnatrument manufacturers' specifications or according to tha aathod balng uaad with tha lnstriaent. A log of lnatruant calibration vlll ba nalntalnad with tha lnatruiant. Tha Inatruaant Stavard vlll ba raaponalbla for anaurlng that preventative and corractlva nalntananca progreme ara carrlad out on all lnatnaaanta under hla/her raaponalbllltp. If a apeclflc problaa la noted bp an Inatruaant uaer, it ahould bo notad In tha logbook and the Inatruaant Stavard notified eo that appropriate corrective action can be taken. b. Blanke A eolvent blank vlll ba analpaed at a frequency equal to tha method blank. The aathod blank can aerve aa tha aolvent blank provided It la clean In tha area of tha analyte(a) of Internet. Thla practice allalnatee tha poaalbllltp of background lnstroaantal contaalnatlon. c. Quantitation Internal Standard A quantitation Internal atandard vlll be added to each sample follovlng aaapla preparation but prior to Instrumental analysis. Thla compound vlll serve for determining relative response factore and for correcting for variations In sample Injection volumes and evaporation of solvents. d. Standards Standards are solutions of the analyte(e) of Interest used to determine the response of the detector ever the range of analyte concentrations found In the samples. Tor Quantitative analyses, sufficient standards and replication of standards vlll be run to demonstrate linearity and precision of the detector response over the range of analyte concentrations. Should sample concen trations fall outside the demonstrated linear range, either additional standards are prepared to expand the raoge, or appropriate dllutlon/eoncentratloo of the aaaple la done to place It In tha proper range. C. Degrees of Quantitation The Information provided for any particular analysis la tailored to the needs of the cuatoner. In actual practice these neede vary across the broad contlnuimi from the grossly qualitative to the preclecly quantitative. It la Informative to examine vhat la Involved In providing the varying degrees of quantitation required by our customers. HONS 02393 7 4 (Mil HP 5985A *11______ .. -------------ilM*aMiMaifMlI*M MaitlM__________ . - _____*?!_-- _________ MRC-Oft Nt IS4M MONS 023938 Hr $66o oe/rc tolKIt----------------------- -------------- toll-------------------------------------------toMMItMlttt __________ _____________kWitHI____________________________toll ___ ,, . . . ... W IMM; NOVU 2. bMfl f OC/BC le|tofc Ml** HONS 023939 1. Qualitative Analyst Qualitative analysis implies no quantitation at all but rather aeaka only th* Identity of the compound(a) present. CC/MS la particularly applicable to thla type of analyala problas. Two typea of Identifications can be aadat a. Tentative A tentative identification la aade on the basis of the analyst's judgement of a aateh between tha aaas spectna froa the sample and a aaas spectrua froa a reference library. This is often done for the large nuaber of conpounds found in a vldescan organic analysis. b. Confined A confined identification requires that tha ebroaatographlc retention tins and the Base spectrua of tha unknown compound aateh those of a known standard of the tentatively identified conpound. This la often done in wldescan analyses when standards can be obtained for tentatively Identified coapounds that are of concen. The nonal QA/QC requlrenencs for qualitative analysis are (1) analysis of a blank, (2) analysis of duplicate saaples and (3) use of a calibration cocpound (usually Decafluorotrlphenylphosphlne, DFTTT) to assure that the mass spectrometer will produce ease spectra that can be coapared with library spectra. 2. Seal-Quantitative Analysis Seal-Quantitative Analysis extends the Information provided by a qualitative analyala to Include aone estlaata of tha aaount of analyte(a) present. The method of aeel-quantitation involves the comparison of detector response of the analyte(s) with that of an Internal standard. The estimated concentration la obtained by assuming a unit response factor between tha analyta(s) and the Internal standard(a). An Indication of recovery froa the sample matrix it obtained from the recovery of the surrogate Internal standard(a). 3, Quantitative Analyala Quantitative Analysis provides lor the accurate easeeaaent of the amount of analyte(s) present in a sample. To be able to do quanti tative analysis one aust know the Identity of the analyte so that standards can be prepared for spiking and for the generation of calibration curves. The method of quantitation la based os a three-point calibration curve using standards of the analyte(a) of interest over range of concentrations in the samples. A one- point calibration nethod can be used (as with the laboratory data 7 HONS 0239AO ayitea) provided that linearity bo* boon deaonetrated over tbe coneentracloB range of the eeaplee ualng atandarde of the analyte(a) at tbrea concentration# In tbe range. Thla calibration carve la then naad to provide concentration# of the analyte(e) In the eeaplee via an external atandarde aethod or aora preferably via an Internal atandarda aethod. For the Internal atandarde aethod, tbe quantita tion internal etandard la added to each of the atandarda (Juet aa with the aesplee) prior to lnatruaental analyala and relative reaponae factor# are daterained. For quantitative analyala the aaaa apectroaeter la operated aa a gaa chroaatograpblc detector. The MS la therefore tuned and operated In a aanner epecifled In the approved aethod rather than ualng a calibra tion compound aa required for qualitative analyeee. D. Quality Criteria and Reaedial Action The lncluelon of QA/QC aeaeurea Into an analyala prograa hae little aeanlng unlaae the reaulta are Interpreted and appropriate aetlon la taken when neceaaary. Tbe ability to do tbla aaeiaea aoae act of criteria that Mill trigger a reaponae or reaedial action. The follovlag aubeectlone deacrlbe tbe criteria that art uaed la tbe OltTatrace Analyala Croup to evaluate hen quality control data Indicate a need for corractlva aaaaurae and vhat reaedial action Mill be taken. 1. Quality Criteria The overriding quality criterion above all othera lat Do the reaulta aeet the need# of the cuatoaer. Thla determination Mill be Bade Jointlybetveen the cuatoaer and the analyet. The eaelyet auat exerclee caution In not allovlng the cuatoaer to overatate, alalnterprat or unintentionally alerepreaent the data. In addition to thla prime quality criterion, the follovlng condltiona auat be aat: a. Hank# - In tbe event that a blank produce* a poaltlve value. It aay not be need aa a valid blank If It exceed# 101 of any reported value for a aaaple. b. Recoverlee - Racoverlea for all aurrogate and native aplkca auat lie In tbe range of 50X<Recovery<1JOX. c. Freclalon - Precision will be calculated baaed on the recoverlea of aurrogate Internal atandarda. Average recoverlea Mill be calculated vlth t etandard deviation for each aaaple act. Repli cate analyaea and lov and high native eplke recoverlea aay aleo be uaed to provide additional lnforaatlon/lnelght Into the predeloo of the analyala. HONS 023941 8 d. Llalt of Detection - Tht Halt of detection (LOD) will donull? be Kitid ii H the vain* of tha low laval native aplka If It la racovtrtd and quantifiable. Should tha low laval oatlva aplka not ba tacovarad, tha LOD will ba stated aa S tha valua of tha high laval oatlva aplka If it la racovetad and quantifiable. Should oalthat aplka ba racovarad, a dacialon nuat ba made regarding tha advisability of reprocessing tha aaapla. Should all aaaplas contain auch larga quantities of tha analpte(s) that tha lavala of tha low and high splkaa ara lnalgnlflcant (<10X) bp comparison, tha valua of tha LOO becomes lata lapottant and la alaplp atatad aa tha LOD for tha Inetnaental analpala procaaa dattTalnad bp tha analpala of atandarda and tha abllltp to racovar tha surrogate aplkaa. a. Accuracy - The accuracp of tha analpaaa la beat determined bp analptlng aoaa aaapla which contalaa tha analpta at aoae pradataralnad level (a.g., an MBS atandardlxad aaapla). If thla tppa of otandard la not available than tha low level and high level aplkaa can ba uecd aa a aeaeure of tha accuracp of tha analpaaa. kaeulta auat fall within a range of 75X to 12OX of tha axceptad valua for tha analpaaa to ba conaldarad valid. If the above qualltp criteria are not not tha analpet will liadlatalp aaaaaa tha need for and extant of remedial action that map ba neceaearp. 2. Remedial Action Tha flrat couraa of action will be for tha analpet and/or group leader to contact tha customer and dlaeuea tha reunite pointing out tha llaltatlona of tha data Indicated bp tha qualltp control raeulte. At thla point tha overriding qualltp criterion of customer needs will be addressed flrat. It could ba that the customer's naada ara act without masting one or more of tha other criteria. In such a case no remedial action la necessary. It could also ba that tha customer has such a demand for tlghtnasa In the results that his needs are not net even though the other qualltp criteria ara. This would trigger further analyses with tighter qualltp control designed around the results obtained (e.g., replications of positives to better establish precision or spikes of non-datactad samples to batter establish tha llalt of detection). In consultation with the customer additional experiments will be designed Including the appropriate qualltp control to ultimately provide the results of sufficient qualltp to meet the customer's needs. IV. Pats This section deals with the subject of data and how they ara obtained, recorded and reducad so aa to be useable la a report and pat readily available for referral and Inspection. HONS 023942 9 The samples will be labeled with a lot number at saaple login according to the procedure daacrlbad In the CSC Section CLP Manual. When delivered to the reaponslble technical person, the aanplee nap then receive additional labeling aa deased neces sary. Thla additional labeling will be docuaented In a laboratory logbook and/or notebook. Theaa logbooka and notebooka will be need bp the analpata to record all pertinent work and reeulte obtained (roa the aaaplet. The laboratorp notebooka will be filled out In accordance with Koneanto Uniform Notebook Procedures. All raw data generated for a given project, which cannot be convenlentlp placed In the laboratorp notebook (e.g., chroaetograaa, coaputer output, etc.), will be filed under aoae prescribed order (l.e., log nuabet) In a central file under the eupervlaon of the Project Leader and/or QA Speclallat. Moat of the data generated by the Ultratrace Analpela Croup are coaputer data atored on aagnetlc dlaca. In order to archive theoe deta the specific file nine and dlec auaber associated with the analpela will be written down In the laboratory notebook and/or lnatruaent logbook. When the disc la coapletely full of data an entire unedited disc laage ot copy of the files on the disc will be transferred to aagnetle tape. A logbook will be kept for recording the disc nuaber, naae and prefix associ ated with It, along with the associated tape and file nuaber to which the dlec wee transferred. An exaaple of such a logbook la given In figure 3. When the data are transferred e verification prograa la used to check all transferred records for correctness. When tapes are filled (they typically hold seven to ten disc Inages) they should be atored In a fireproof vault. All calculations of the results of the data will be specified In the aethod used. These calculations will be entered In the analysts laboratory notebook unless they are coaputer generated. In thla ease, a copy of the coaputer output will be filed with the raw date. The Project Leader will be responsible for checking the correctness of the data. V, Saaple Disposal Saaples will be disposed of la accordance with the Instructions on the Analysis kequest fora. The only exception to this would result when the analysis reveals a problea which requires saaple disposal In a Banner other than that originally specified. If the Project Leader notes froa the reeulte of the analysis that a potentially toxic product was present In the saaples then the saaples will be disposed of In a asnner deaaed safe by the Safety Department. The date of saaple disposal and the Banner should be noted on the request form stored with the rev data coapletlng the chain of custody of tha saaple. HONS 023943 10 (Hltl-Ortn Nfm 0u MlfMttMl) OM*M tow* HrMu Oat* Tapat Tapo* Tin P (nu #) /*> t>\ &-Laj> <** Qw*-) om> viywf0t . I Mi >/>/n t>Hl I <H>6VI 6e>WiO GMCi) Gi>Wt) 135 Jhto 8*fJI 130 (*$ Crtfl iwt j/b 131 CRRi) Citd Sfl i>r (i*#t) Lm$ s 3-11-0 / <v*t*>jiAO ~ - in> OWiiV>Ki - ft&Vfti-rti*. t&K. "MW 3/iy/6 S/n /$} l ?MI& //'n3 ttiujOr*! 6h- V^vb 4^ I <rt>4*9) dOU(x) C*)W$ CtMW) &>?!(/) Oof/ (is &>ft (f) 134 (HR9i4))CCwQQ 110 (**l# SM /V/ *1 ^ /yz, OW*) /*> <W/*) #}fo A w/*a s2> s&> ?$ 601)M 6*73 (S) 63>f&( e&i*(y) /V/ <7WoV) -s>i *!/ >73 <$/ (V5 (*fcS) *!*>!& //7 /VJ ftMeO ('Afctf) /ft ft**) <5*> 0f) 3 -3 33 3-3 quits Unhs i/s>hu <.I*tIv <j3lll3 453 (M) JrCAfVya-*** .S/J /St (AtoOfeZ f*lh Shafii tsx- (#*s> | j -C/u/b #/< efJK n/fW1Mhi Q>03 Qy C3>YA, (A* (3 V (33 e> p- y* 0>-rs-Cc) (0 <&V-W bbO)1ixlXllfil))t M'i V4 " &K FIGURE 3. Exaapla of DISC/Tapa Logbook paga. HONS 023944 11