Document 7NpR4O84eK1L1NNRN99gRQMa

Monsanto MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ______________ ESC/DAYTON (Departaent/Section) ANALYTICAL (Type of Report) AUTHORS t U. m . I!u<|hf*n T1TUC: ANALYSIS fOR INCIDENTAL P C S '* IN VARIOUS PRODUCTS REPORT NO.: MOA-S04 received JOB/PROJECT NO.i 464.3110 DATE: 16 July 1964 PERIOD COVERED: JUL20TBW g|ON>`iS ^ ' ** TITLE: ANALYSIS FOR INCIDENTAL PCB's IN VARIOUS PRODUCTS AUTHORS: B. .V. Hughes' 004 t. z \y $ A-' ABSTRACT: Sarples of various products fror. the Chocolate Bayou Plant were analyzed for possible concen trations of PCB's. The results of these analyses are shown in this report. TECHNICAL APPROVAL: -v'vr-M ' VV\ AjnyfD|Y: &VC_________ Brooks Senior Research Croup Leader .3 , R. F. Ivory rJ Environmental Sciences Center Service Project Mana?er pT9!PTrn nir ,* ';iviJ.Li! JUit\i>v. i- RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL IMi dooeent is the property of Monsanto coop any and the recipient la responsible for its safekeeping and disposition! It contalan coNflBCNTlAL IMPORnation which nest net be reproduced rivalled to unauthorised persona or eent outside Monsanto Coopany without proper authorisation. HONS 022972 COTY NUMBER 1 J. N. Blanclurd 1200 a R. b. Cray 1300 i B. M. Hugh.* 1250 4 R. F. Ivory 1250 s Cantral rilaa 1250 ( Tachnical Raporta Library R2C : I V^ \ abstract only h. a. woittrnann 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. H. Hughes D. McKenzie B. Williams COVf'AW C O N r I D [ N r I A I HOMS 022973 ANUttlS K*T IOC NUfltC*' I-04-Q4-1O-OI 1-04-04-11*01 i-04-c4-:'-o: 0*Tf: July 6. 190* PROJtCT NO: *94.31!10 CKc;o-t t Bavr-j'lvc'y fR.*: n* ;ronme-.ta' Sciences Center h*nsr*tO Conper>/Oaytcn laboratory ISIS Niches Road Oaytc-. 0* 45*!6 N:: IS:31 ?66-34:i Title: Analysis of Inc I dental PCOs In Various Products $tt':rd Sa-::rt *evoc *:<**: Sa-t'e! suct'ies t>> Cu!ton* Sta*:r: *fs:ti* wor ko:?*: p:?7. p;c*:c 5t#*:r: **i >ss v. fine R*c?'t r i *e a?;s;: A):;ij te: es I tnrovo* 0 sunre-iee Incidence* PC6 Result! 'or t^e a^j y!s o' va-io-* C-cceiete fcayr- Plant D*odjctt. Also 'nclueeo are* l! a o*ier ep anat*on c# the tat'es. 2) Stymar its of the above referenced extraction anc analysis net'-oct. 3) Analysis request information generated for this project. 4) A brief description o# m> mte'pretatlor of the in-ider.ta? PCE regulation. 5) A copy Of the CSC/l:Aj 6LP Manual. PLEASE NOTE: I the results shown In the tables demonstrate that these products cent no quant IfIaote incidental PCOs. However Tables 6 ano 7 sho that the .rtractIon method used In the analysis of A-?!$ d6 0/h. a-230 t?3-I. and A^HO 0$ s/0 destroys CU-0P through Cl3*0P congeners and therefore HONS 02297* tn*t thrr* product* auft 0* rttnoiyztd for th*t thr** c!**. . > tonn^t. Du* tht hl^t ittbHIty of th* Mnp'f MtrW (uMeh contiit* p'lat'lly llndtr pUyl bonttnoi). th(lt thro* product* My not Do anolyltMt 'or Cl I-BP through ctJ-B* vttt< 100 o' l ug/g. Inciomtoi PCBi >u'e &t pnoiyztd m the ftortlng Mttrlpl* ultd to product thttt thrtt proouct* In o-r to ClrcVovtnt thttt preOltiM. M*ltST($)i B. n*o>.Nughtt. 0o/d NChtnzIr *nd lu'Mra mttltf. .<*! AhtOOvA. I to n~ Af-'-A'- HONS 022975 Table |. Oesuttt of Incident*I Pd Iralym Project Not 404.11110 Date: July t. 1104 Thtrmtnol VP-1 Tank SBTS Congener Analytical lOQlal Clast Method (ug/gl Cl 1-0= Cl?-BP CO-ge Cie-gn cis-gp C16-BP Cl 7-go Cl 0-0= ci-gp Cl 10-BP H$AK0? " " " " * " l(M * " NQIb) Surrogate Sr',n5 Amount CenoovM AMtaivg/g) *.4.r ! .0 te Sample lOtfttlftCOtlon Thermtnol VP-l (Dupitcate) Concentration (ug/g) nQ - " " " Oecove-y (1) 89 Documental ion CSC Extraction nethod Date of extracticn Sample Amount C*tr#cted (9) (tract Final Volume (ml) (tract 01 tut ion CSC Extract or Sample Nuaoer Oate of CGC/ffS Analy>l* Its FP* PCCKIC 6/20/84 1.0940 t.O III pcg-46i 6/79/04 19491.19496 PCEXlO 6/20/84 1.0633 1.0 1:1 PCB-46? 6/29/84 19492.19497 footnotes: <) 10Q ' Unit of Quantitation In ug/g. Signal-to-noise ratio Is greatsthan 10 4>en this amount Is analyzed using the above reference: Analytical and extraction Methods. The following lette-s indicate now this value was determined; C - estlaated freer PCS congener standard analyzed under toe sane conditions. N - Measured freia native spiking of sanrle Matrix. S - estlaated froa surrogate spiking of sanple matrix. V - measured In validation experiments of similar sample matrix, (b) NQ - Not Quant I tatable. The congener concentration Is below the LOG value. Table stored In file: B3IIia>MHsl Analyst(s): 6. nason Hughes and David McKenzie Analyst Approval:. HONS 02297* Hbtt ?. Besutts of IikIMI PCt Umlrtn. Projact Hoi 4*4.31118 Oatti July , lf*4 Dlpncnyl 0IC Tank S6T3 Sample Identification Hethod Blank (Thermlnoi 0P0) Cenganar Analytical LOQlal Cla* Hetnod lug/g) Concent ratipn (ug/g) ClI-BP CL7-BP CiJ-*P Cl 4-bp ecs-ap CLt-BP Cl7-*P Clt-BP cie-Bf CUO-BP *sak:3 " " " * MWi * " " " " * " NQ<b> " * * " . MC - * " " " " Surrogatf Spiking Amount Conpoyno Added(ug/g: Recovery it) 3.4.J-4'-Ci4-<* 1.0 79 95 Doci4*entet loo ESC (.tract ion netnotf Cate of Extraction Sample Amount Extracted (g> Extract final vour-e (*) Extract 01lutIon (SC (.tract or Same 1 c Nuntw Oate of CGC/HS Analysis W$ fRK PCCxiO 6/zo/e- I.OSIO 1.0 1:1 PC6-463 6/29/64 19401.19498 PCExiO 6/70/64 0.0 1.0 1:1 PC0-466 6/29/64 19402,19499 footnotes: () lOQ - limit of Quantitation In ug/g. Slgn*l-to-noise ratio 1$ g*eate* than 10 when thl* amount Is analyzed using the above referenced Analytical and Extraction Rethods. The following letters indicate how this valve was determined: [ - estimated from PCS congener standard analyzed under the same conditions. N - measured from native spuing of saxpu matrix. S - estimated from surrogate spuing of sample matrix, v - measured In validation experiments of similar sample matrix, (b) NQ - Not Quantltatable. The congener concentration is below the LOC value. Table stored In file: C3lll0iflH:)9 Analyst(s): 6. hason Hughes and David HcKenzie QAnalyst Approval*. NON S 022977 Table ). Mutt* of InclAnUI KS Analyses Srsjact *> au.lilio Dat*i July l, IM4 Sample lOrntlflest Ion Congener Analytical lOQ(a) Class Method (ug/g> formaldehyde Tank 8)07 roraaidehyoe (Duplicate) Method eianv (foraaldehyde) Concentration (ug/g) Cl 1-0* Cil-8 c.i-d* Cia-OP ClS-0* cit-o CO-OP et0-0*> c.vo* CU0-9 ASAS3J * - ' ' KM - ' * - NQ(t>) * " " * " " " NQ " " " " hO * - " Arrogate Spi^ng *"urt Coapouno Addedlug/gl Recovery (I 1.0 83 93 141 CaciMntat lc- ISC Extract to- Method Date of Extract <o* S4W0I* taognt extracted lg? Cxtract final volume |m*) extract 01 tut <on (X (street or Semple Number Data of CGC/NS Analysis ts twh PCEA0T 7/2/Oi 1.3494 1.0 1:1 f*C0-Sl5 7/2.T/3 19532.I9S6I PCEX07 7/2/04 I.ISI9 1.0 1:1 PC0-JI6 7/2.7/3 I9S33.19562 PCfKCT 7/2/e< 0.0 1.0 1:1 PC0-3I9 7/2.7/3 I9S34.I9S63 footnotes: (el lOQ - Halt of Quantitation In ug/g. Signal-to-noise ratio is greater than 10 uhen this amount la analyzed using the above references Analytical and Extraction Method*. The following letters indicate how this value was determined: ( - eatlaated from HI congener standard analyzed under the sane conditions. a - aeasured froa native spiking of sample metrla. S - eatlaated from surrogate spiking of swple aatrla. V - aeasured In validation eaperlaents of slallar saaple aatrla. (b) NO - Not Quantltatable . The congener concentration Is belou the 10Q value. TaMe stored in filet D3in0>i*til9 analytttsli 8. Nnason Hnugghnecsi anod Duaaviod HnccnKce* nzle i, 7t~-- ^jA- ansiyst Approval> HONS 022978 Ml* 4. Basalt* af Incldsntal PCS Wlym. Project Hoi 4B4.ll11* Bate: July 4. I**4 NtA lot A<0dlt* nltrliot'loctUtt) Sample Identification IDA lot 0 leeio. nolbn.0ry) Congener anaiytlcei 1001*) Class Method lug/g) Conceptr#tln fug/p) Cll-S C12-B* Cl)*BP Cl4-B= ClS-6* ClS-B' CL7-B Cl8-Be Cl-B CllO-6* NSANCJ " ' - " " ' * MM) ' * " ' ' " NQtb) " " * " * " " M0 " " " " * SvrroQAte Sc'^'^s Amount Compound added!ug/g) Pecovery 1X7 J.A.J'A'-CL 4-06 1.0 86 136 OoCmne^tAtion CSC extraction Method 0Att of ctrction Sample amount extracted (gl (tttrAct Mn<l Volt** (ml1 (atrec? DMutfor (SC (atrACt or Simple IMOr Date of CuC/ms analysis ns nts PCEX07 4/22/84 1.1418 1.0 HI PCB-A67 7/2.7/3 I9SI6.194*4* PCCX07 4/22/64 1.0669 1.0 1:1 PC6-468 7/2.7/3 I9SI7*19546 Footnotes: la) lOQ - Halt of Quantitation In ug/g. Signal-to-noise ratio la great*' than 10 uh*n this Mount Is analyzed using tne above referenced analytical and Extraction Methods. The following letters Indicate hou this value uas determined: C - estImated from PCS congener standard analyzed under the same conditions. N - measured from native solklng of sample matrix. S - estimated from surrogate spiking of sample matrix. V - measured In validation experiments of similar sample matrix, (b) NO - Not Quant Itatable. The congener concentration Is btlov the LOQ value. .Table stored In file: E3III*iMH:| analystis): >. "aasson Hughes and Oevld McKenzie analyst approval -D-7frgr* HONS 022979 1*1* t. Besults af IvMntol n Anatyaas. Project No: aba.Jills Oata* July 6. 1904 Sample Identification "6A Tpok 326TI2-2 *H6A(duP) <atImet Feed tuppt ) nethod 6'ant (MH0A) Congener Analytical lOOte) Clast Nethod lug/gl Cll-ftP CL2-0 cu-o Cl 4-8 ClS-0* Cit-BF CU-|P ClB-BP Cl-BP Cl 10-6? RSANC3 * ' ' ' - ' " t(N) ' " ' - " " NQ(O) " " * * * * Concentration lug/g) NC NQ ** " " " "" "" " " *" Surrogate Spiking Amount Compound Added(ug/gl Recovery (t) J.A.S`4'-ClA-dB 1.0 102 89 91 Doct*entat loo CSC extraction Nethod Oete of extraction Sample Amount extracted (g) Extract Final Volume (ml) Extract 01lutIon ISC extract or Sample hxor Date of CGC/hS Analysis Its FRN PCCX07 6/22/64 1.1626 1.0 1:1 PCS-469 7/2.7/3 16516.19547 peexo' 6/22/84 1.022? 1.0 1:1 PC6-470 7/2.7/3 19519.19540 PCEAD7 6/22/84 0.0 ! .0 1:1 PC8-476 7/2.7/3 19525.19553 Footnotes t la) LOO - limit of Quantitation In ug/g. Slgnal-to-nolse ratio Is greatethan 10 nen this amount It analyzed using the above referenced analytical and extraction nethods. The folloving letters Indicate ho* this value uas determined: I - estimated from PCS 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. lb) NQ - Not Quantftatable. The congener concentration It belou the 10Q value. Table stored In file: f3HI0:NM:l knalyst(s): B. Nason Hughes and David HcKenzIe Hfett . anuiu of IncMwAel KS Analyses ftajfct sat ew.Si it 1 A-215 df 0/H Sattt July t. IBB4 Sample Idenffleet ion A-7JC T?3-l method Blent C't CII-8P CL?-(= CU-!Ctf-I' Ct-* Clt-S: Cl-f: CLB-(= Cl*-B= Cl ID-BP IC*t lOOial HthO0 lug/gl R&ANC3 " " * * " ** . - mn; * * * " - Ss-rojate Sc'-'-; A - t Coxpojnc AO oeoiuj/j' Js^.J^'-CK-c* !.; K*|t) Ktc: * o Cf*c*tr*t o*' twg/g) NA KA * "" NO Aj ""** "" "" "" fie:?ve-r ?v i:? 6t DOClTfrtit if IK.(:: 'o- e*.-s: Bate cf tt'a:t:or Sa-C'e A-o.-t Ifa:te: (wart *tna' v;jre " leVBCt P` ut c(SC (.tract c- Sa-c'e t.te- Date of C0C/V3 anaiys's ns r*s pci* :. s/::/8c ! a c*: fc 5 1.0 .*: I Cft-47* 7;'.7/3 19S2S.19554 tu:;sc 1 t. C p ! .9 1:: KS-l'f V2.7/5 1952*. 19551- p:c ' 6/::/*c.c 1.3 :: i PCS-45* 7/C.-/3 19533.:?!59 Footnotesi (#' lOC - limit o` Quantitatlor in ut/a Sign.:-to-.-elte r.t'o > j-eatethen IC *f. this raun'. 1s e-aiyceO using tne aboe refere-cec Ara'ytlce' end (xtrectlon methods. Tht following lette-s Indicate how tMt value vat deterr'nee: N - measured fro* native spiking of sample *et-l. (t) NA - Not Analyzed. The (SC extraction method used In these ane'yse; destroys Ct-BP through CO-BP congeners. Therefore no IOC ce de established for these compounds In these samsie*.. tc) NQ - Not QuantItetable. The congener concentrjtIon Is below tne IOC value. Table stored in filet 6IUIBinh:i* Analystt lIsli B. Nason ttugr.es and 0avS6 NcxenjIe t Approve' i vl 7t^--_____ Analyst HONS 022981 Table 7. Results of IdcMmUI KB analytes. Project Hat 4B4.JIIIB A-JT8 S/D Congener Analyt lea : sOOia) Class Method lug/g) Ctl-B Ct?-8P C'.S-!= Clt*!= 1x7-8= Cl-f= ci-e* Cl:o-b; HSAKP? " " " " * . MV * " " ' Sr*98A! S:'.i'i A~.-t : Added! uj.'s' _ 4 - iC m:di * * V:c ' * " 12 Betti July *. IBD4 Set it lof'ti'iett'y A-TTe <K S/D (Oueiicete: CoCntr?1^ (ug/g> N* " ' 5e:;.r, :v 7; BaCkrtitave- IS: C-trstt s- ref*: Ov.t c# l**.'z Irfact I'.J' VO'ufe (- D N#t i O' ISC !fect c- Sarple srte- D*tt * CGC/** Ar* yf.% p;r y;: i .: i. * i:! C5-A?? 7/?,7/2 !W?0.!$55' p*r, ; ; /::/ 1.0 !:: D-a_ *s ?/:. 7;3 !9),,'9.:?*59 foetnotes: la) IOC - Limit of Quantltatlo* '* us/9- S'g-ai-to-roise rat c is g-es:*- tner 1C uhen this ao--nt is ene'yze: using tnt eoevt Anaiyt'cel and Extraction methods. t-.e ftiiou'ng !et:e-s indicate non this value was determined: N - measured from native spiting o' serx'e *e:-i. It! N* - Hot Analyzed. The CSC extract ion method use: m tnese , tti destroys CL-BP through C13-BP congeners. Tne-e'o'e ns lOO ca ge established for these eencour,-!. (el NO Not Quantltatable. The congener concentre:ion 's 6eia- t-e ,0C Table Stored In filet itillllimiiB Analyst(s)i B. Meson SiVgghheest and Davyi'd MnccKKenzie Analyst Approval &7 HONS 0229B2 TabIt I. tosults of Incldwrtal KB balytn, Project Msi AOS.31II# Obtai July t. IMA Sample Identification KSl so let CBC 0J $AK G lot CSO 031037 SA lot COC lOiSn Congener Analytic*' lOQ(o) Class fffthotf (ug/0) CofKtntrst ton lug/g) CU-8=> Cc2-#f CU-B CIS-#' as-s a*-# Cl7-= Cl#-#' CvlO-8* HS4SCJ " ' i(N) p " * Ss#'rp9te Soikins Afloat Co"eo*n Aooteiug/s) Note) * * * ** NQ " " " " " " Recovery d) NO " " * " " " " 3*4,J'4' -cc-d* 1.0 89 154 14 2 Cocimnu: ion tSC Ctr#ctlO Cate cf extractloSonpie Amount CKtrocteO (9) Cutrott Ftnoi Vo'i^*e (*') (troct 01 Jut Ion CSC extract or Sample ihm&er Date o' CGC/tt A-a'ytls NS FRK PCC*97 inn84 1.0266 1.0 1:1 PCB-A7I 7/2.7/3 I9S20.I9S49 PCEX07 6/22/Bs 1.0382 1.0 1:1 PCS-474 7/2.7/3 I9S22.I9SSI pcmo7 S/22/es 1.0590 1.0 l: 1 PCB-47S 7/2.7/3 19523.1955? footnotes" (a) 10Q - limit of Quantitation In ug/g. Slgnal-to-noise ratio Is greater than 10 uaft tMl amount It analyzed using the above referenced Analytical and extraction methods. The following letters Indicate ho* this value mat determined: ( - estimated from PC# congener standard analyzed under the same conditions. N - measured from native spiking of sample matrix. $ - estimated from surrogate spiking of sample matrix. V - measured In validation experiments of similar sample matrix, (bl NQ - Hot Ouentltatable. The congener concentration Is belo* the 100 value. Table stored In file: 1311161e*ti1* Analyst Is 11 6. Nason Hughes and torld NcKenzle Analyst Approval tn 7tfhj**' HONS 0229B3 RETAILED CWUNATION Of INCIOENTAL KM TAKES In an effort to straamHne reports generated by CSC on Incidental fCB* present In a wide variety of materials. using a wide variety of tectalques. Standard Extraction Method* iSErH) and Standard Analysis Method* (SAMs) have been developed which can be easily Interfaced with each other. An abbreviated for* of these SE"s and Sams ha* peon stored on the Hewlett' Packard 33ST*IA$ computer system used by CSC. In an effort to communicate these details with customers of CSC. this inforaotion is supplied with each incidental PCS analysis. However. evny projects Involve a very s*mII of samples which are not necessarily the same eptrU. Therefore, to reduce costs of generating reports for these small projects, major Information on the technical details of an analysis are presented m tabular form viti.fn the same table which reports the data. . Each table includes a general title. CSC Project H^ynber and Date on wsich the table was generated. The sample identification is tr*e customer identification which was on the sample bottle. The ne>t section of the table gives results for the particular PCD congener class listed. Tne level of Quantitation (L0Q> using the Analytical and Extract*bn Methods shon >r the table. Is given for each congener class. This 10Q is determined in one of four ways and is described in the table footnotes. Tne next section of the table deals with Quality control used in ea:n sample analysis, the surrogate spiking compound (if usee) which is added to the sample before extraction and analysis, is listed, along with the amt.*', added and l Recovery measured for each sample. The final section before the footnotes deals with how each sample was extracted and data doc**entato*. Tne ESC Extraction Method. Date of Sample Extraction. Amount of Sample Extracted. Extract final volume. Extract Dilution and ESC Extract or Sample Number give critical extraction details of the analysis. The date of CCC/rnaiys's and the mass spectrometer file reference number (FPN) ooc^mtent ho. *ns when the extract or sample was analyzed and where the raw data is steed. At the bottom of each table, analysts Involved in extracts and analysis a*e listed, along with provisions for signature of the responsible analyst. tris table format is both compact and precise. It was developed in an attempt to Quickly and accurately generate data which the customer can Quickly and accurately evaluate. It should Include ei reouired informal tor 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 Flic: |NXPT:MH:SP Envlronrentai Sciences Center Monsanto Company Dayton Laboratory ISIS Nicholas Road Dayton, Onto 45407 HONS 022984 Iht fol loxlng Mts d*scrib* Standard Extraction Methods and Standard Analysis Methods usrd for this project. HONS 022985 ISC Mjndrd Analysis Method ISAN) TITlIi Organic fBNiuntfi In Solwt ISC Standard Analysts HrtJwo ND< KIM) ANALYTICAL IN$T*uhCNT AND N00C Of 0PCMTI0N: HP-50658 Capillary GC/NS-Selected Ion MonitorIng with RevIsIon-t Nultl-drive software. Typical Nun Time: Typical Multiplier Voltage: Typical Owetl Times: heaimus f of Hasses; electron Cnergy: 3 - A0 min. IB00 - 2600 ev 200 - 500 msec/mass 20 70 ev TYPICAL AKA.YTC typical instruhcnt LCVtL or DCTecTioN aoo (ug/ml) Organic Compounds elutlog betee* toluene and n-C34-ane 0.01 - Cl TYPICAL PPCCIS10N 6 I0X LOO (11 30 typical accjna:* # ioy io: in 30 iNTCPf t*HNCS ANO LIMITATIONS: Ana'yte character l*t lc ** *uSt b Ch'Oratcgraohlca'ly rolved fro* ether eluting compounds which produce the ire nets. CM0NAT0G*A*HIC COLUMN: 30-meter fused lilies JU DS-S (0.25 u*) *,! ld bore I0.J2 an) COLUMN T(NprATUOC W0GANj 50(41/6/30! INJKTION TrP. SpUtles* ca.ibaation ANO STANOAACIZATION: Quantitative: Use interne! standard Quantitation tec^niQuC end calibrate instrument response factors fror standard solutions or a'a'ytt: of Interest. Qualitative: When Multiple characteristic masses a*e monitored for a given analyte* the ratio of characteristic mass responses must be within 201 of those foe the authentic standard, for PCB analyses, the characteristic aiosses which are monitored are the molecular ion containing an 3S-Ci isotopes and the molecular ton containing one 37-CL isotope. Since the above referenced analytical Instrument can monitor no more than 20 masses m a single analysis* Incidental PCB analyses reoulre two Injections of each sample tn order to analyse from CL-biphenyl through CLiO-btphenyi Isomers* anthracene-dIO and the surrogate spiking compound. The following summarizes the masses and approximate retention time regions monitored In these two capillary QC/H$-$|N analyses. HONS 022986 ANAirsiS fl IWsse* Cl-#8 lionrrt. anthr*Cfn-dlO CL7-#8 IHM'I J.a.3',4*-Ct**9P surrogate Ci5-#8 lion,.. Cl7-ir Isomers C;.9-0P isomers 166,190 277.224 796.290 323.9.325.9 391.#.393.# 461.,463.6 ANALYSIS |2 'K>'*C*n*-dlO Cl 3-BP Isomers Cw4.gr t$eme*s Cl#-#8 !*'$ Cl#-#8 CLIO-#8 1 >**: 166.198 255.9,257.9 . 269.6,291.9 357.#.Ji,.e 427.7,429.7 497.6.499.6 Retention T imes .11 21 II - 21 21 - 28 21 . 28 26 . 39 28 ' 39 ! _ 23 14 . 23 23 . 29 23 . 29 29 . 39 29 - 3 CA;CUlA7|0nS: Ana'yte coxe^'#*.lO-> (Analyte ar*a)/(A-iaiyte M'Ma'ea ' l w^re: A~.*'yte a-ea ts character!**ic nasi area of the analyte. Pf i the rentlve response factor fo* the ane'yte. 15 is the intern*' standard and is usuala^tn-acere-ci?. wf (analyte a'a n standaro)/(core. of ana;yte)(aree o' IS PCS concentrations *'* calculated in one o' t*c ways: 1) If an Arocior formulation ca** be ident'fled fro** tne patterns o' PCS <loner*, seieted PCS (some's 9r classes of isomers d. e. e'i Cl4-oiphe~>' isomers) are used to ouaMify tne Arocior concent rat ion. fteiative Pesponse factors are calculated using tne concentretin of th* total Arocior for* mutation in tne above Mr equation. 2) If no unique Arocior formation Is present, tnen tn total PCS concentration is calculated by using standard solutions containing know* amounts of enlorobiphenyi through decacniorobipnenyi isomers to calculate Peiative Response factors in the above Mr equation. The RPf s for tne corresponding PCS Isomer classes are used to calculate total PCS Isomer concentrations In unknown samples. SAFETY PRECAUTIONS: See PCS handling protocols In laboratory safety manual. OATES Of TCp CREATION ANO METHOD UPDATES: 12/9/93 HONS 022987 ISC standard extraction Method <SCM> TITLIt Kti In aatrleat contalnlro acidic (roup* ISC Standard extraction Mailed to; KCXO) NATRI(X),(CIS)i carboxylic adds. Chloropnenols. and any alkyl or aromatic compound tnat U acidic in nature TTPICAL SANPU SIZE <g> 0.5 - Sg TYPICAL CATftACT VOLUNC (*) 1 - 10 TYPICAL ANALYTES: A 1242,A!2*8,AI?S4,A!260.anc CB Isomers mono- through de:aCMoro-DIphenyl. IhTCPfCPfNCCS: Any electron capturing spedet in the retention time region f tr Ichlorobiphenyl Isomers through octaehloroblphenyl Isomers for ECANO1 an CCANC2. Any spedes in t*e appropriate retention time region whicr give the same relative characte'istc mass responses as PCe isomers for HSANO). Typical surrogates typ;c*. RECOVERIES (t pentacMc'o&en^e * s: - 123 2.4,6-trIchloro- bipr.e* > ' SO - I2C 3,3'.4,j'-tetrac O'C- b:phenyl-06 SC - I2C APPARATUS AND HATtCjA.S: Bwrd^cA and Jackson heane *of sample etract'r.. Potass^ nydfo*oe toiud* 12 n> to ionize acdc functional groups. Distilled deionized water for dilution of the potasslu* hyd'oise. Potass1h/droKloe pellets. Silica gel collars impregnated w*tn ootass*ur per^nganate, jjruric ac o. and POtaSSi^ hydro*`0e. Disposable g'as*a*e. .IMITATIONS! Netnoe applies only to matrices which are hyC'o`izatie usf'g a ?* POtatslu* hydro*|oe solution, tc $As m-t valid for Cl 3-BP througt Cl0B. S SAMs are velld for all PCBs from Cl I- through CLIO-BP. $Af(Tv PRECAUTIONS: See PCS handling protocols in laboratory safety manual. DATES Of KTHOO CPCAT ION ANO UPDATES: S/I4/B4. 6/20/04 MOMS 022980 non sen ttnai FOR ESC EXTRACTION IC1MOO PCEXOT SMFlt ID: .................................................................... IC EXTRACT I ................................................................................... LOG MO................. EXTRACTION DATE and Tint: NEIGH OUT SAMPLE INTO A <0 at. VIAL |) WEIGHT SAMPLE II gl SURROGATE SPIKE OF SAMPLE [ ) SPIKE .................... A IS HA 2 M KOH SOLUTION TO VIAL M ' Snake until SOlIO is into SOLUTION EXTRACT )ISK HEXANE I) 1)111) REDUCE SAMPLE VOLUME TO [) 1-2 at WITH NITROGEN AnO . ARPkV TO COLUMN QUANTITATIVE*. .. ELUTE WITH }0 nL HEXANE () NITROGEN IlOW OOWN TO I *L 1) Extract no* DATE/TIME COMPLETED ANALYST t...... ............-- CSC JOR NOi RINSE COLUMN WITH i ?0 m. I ) HEXANE . ClEan-up COLUMN DESCRIPTION 2S IN. DISPO P1PET I CN N SO 2A t cm II POTASS!J" PERNA3AN<* SILICA GCl I c SILICA GE'. 4 c* ACID SI.IC* GEL I cm SILICA GEt. 4 CIA DASE SILICA GEL / \/ GLASS WOOL HONS 022989 (K Standard extraction IMM IXN) TIIUi KM In blpnonyl and areaatlc Ultra ISC Standard Extraction artnod KOI KtxiS MATRKX).(CfS): oil and ell mixture* typical sample SIZE typical extract VOLUME (ml) O.S - Ig 1 - 10 TYPICAL ANALYTES: Al242.AI248.AI2S4.AI2S0.ano PCS liomcr. nono throws'. OrecMoro biphenyl INTERFERENCES: Any electron capturing species in the retention time region f trlcMorotlpnenyl Isomers through octocnioroplphenyl Isomer% for CCANOI 0*0 (CANO?. Any spec If* In the appropriate retention 11me region which give the same relative ch*r#cter 1stic pass responses as PCB isomers for NSAN03. TTPICAl SURROGATES ttpica^ RCCOVCRtCS III pentachlorobeniene 2.4.6*tr IeMoro- blphenyl 3.3*,4.4*-tetra chioro biphenyl 5C - I2C SC - l?G ST * I2C APPARATUS AND MATERIALS: Burdick #no Jackson hexane for extraction solvent Sulfuric aclO filing MSI) to oxidize tne matrix Sulfuric ac<0 for acid wash Sooiv* sulfate to ary the sample matrix Silica gel columns impregnated with potassium permanganates su>fv.Mc add. and potassium hydroxide. Disposable glassware. SO me centrifuge tubes LIMITATIONS* Method applies only to matrices which do are hydrolyzable using a filing sulfuric acid MSI) solution. EC SAMs are valid for Cl 3-BP through ClIO-BP. NS SANs are valid for all PCBs from ClI-BP through CllO-BP. SAfETv PRECAUTIONS: See PCS handling protocols In laboratory safety manual. DAT(S Of NEThOO CREATION ANO UPDATES* 0/20/84 HONS 022990 no* Kn KTSI9 rm isc cxtmction icnco rctxio SAMPlC 10: CATBACT10* 0At( #r* Tint: WEIGH Ol/T SANPlC INTO A 40 L VUt t) 5UOOOGATC slE or SA-^U |j M*C CATBACT f IOC NO: ............. WEIGHT SAHPIE H 9) ADD 10 Pi HtAAst t) ADO $ Pi ruttlNC SUt'VRIC ACID list) SKA*! foa SO SECONDS AMD RE novt h(aanC By I hiwjTC IJ . PIPCT NCKA\E AkoG W! Th 2 * 5 *. '; B!*$ES tOC *C* SHA<t> INTO A At IK . VIAL . BINSE COtO*?. pITm 2 * 2C r l ) hExanI . CLEan-op CGLWN 0E5CB|P*;>. 25 me 0I5PC P.H' was* cktsact pith eot smru*!C acid ( ; BOCvC lAtftACT OwAKTlTA-tvCit INTO . A 50 A. CC^PiruGC Toes . BCDXC 5Aie%t volume TO 3-5 <k WITH KlTAOClN AMD APP*.Y TO COLUMN QUANTITATIVE (} . . I Cr KM SC 2 *c- :i P0'a15;. PCa^ANGAKATr sus;a gel I cr SI.ICA G*. (LUTE PITH 4C C HCAAKE NITROGEN BlO DOWN TO I PC l) l) 4 C" ACID Sl-lCi GCl I cm SILICA 6. .4 cm BASE SILICA GCl \XXX/ \/ GLASS WOOL EXTRACT NO:------- ------------------ DATC/TINE CONPIETED......................... ......... /--.............. ANALYST*-------------------------- ----------- CSC JOB NO: MOMS 022991 The folloalng pages describe Analytical Request Infonaatlcn generated far this project. HQkS 022992 me ENVIRONMENTAL SCIENCES CENTER ANALYSIS request OATEi APRIL 10. 1*64 IOC NO: 1-64-04-10-01 REQUESTER: CHOCOLATE BAYOU/IVORy PROJECT NO: 404.31116 REPORT RESULTS TO: FItCS/NEES.IVORY.BROOKS ANALYSIS REQUESTS SENT TO: f 1LES.IVORY.BROOKS,HUGHES SanlE PICKUP Ry: n. hugheS SanplE LOCATION: LAB *6. BUILDING ? SAMPLE DESCRIPTION for 3 SAMPLES sample identification THCRmINOL VP-I TANK 5BTS FORMALDEHYDE TAW 630? RERUN mcthoo Blank for rerun diphenyl oil DC TAW S6T3 NUMBER OF BO'TlES ESC NOMOERlS) I PCB-46I.PC0-4S?-DUP. PCS-464-iS i Pce-4StvPCB-4s?-o,jp. PC6-45fl-LS.PCfl-4SB-H PCB-SIS.PCB-5IS-D0P PCB-SIT-LS.PCB-SIB-HS PCB-Sl* I PCB-463.PC6-4SS-HS rethoo Blank for tmermimo. and diphenyl oxide PCB-4S6 method blaw for FORmalDEhyoe PCB-46C RECORDED 6Y: P. HLPP REQUIRED ANALYSES: INCIDENTAL PCB'S ANALYTICAL TEOBIIQUES: X GC/EC (ID) OATE completed 7/4/64 QUALITATIVE! YES SCHIQUANTITATlVE* QUANTITATIVE: YES REQUIRED QA/QCy DUPLICATE ANALYSIS ANO HIGH AND LON SPIKES COMPLETION OATE REQUESTED: CCRRCNTS: IS AND MS REPRESENT LOW AND HIGH NATIVE SPIKES, RESPECTIVELY SAMPLE DISPOSITION: X HOLD FOP 30 OAY$ MOWS 022993 sarin mccmtionsi set res morocas Musis kquist nu nmci msiiohi HONS 02299V MC ENVIRONMENTAL SCIENCES CENTER ANA* TSIS REQUEST OATEi ARRIl II. I VBA REQUESTER* CHOCOLATE SATOO/IVORY LOG NO* 1-64-04-11-01 PROJECT NO: 4B4.3IIIB REPORT RESULTS TO: rilCS/MEES.IVORY.BROOKS ANA*.TSIS REQUESTS SENT TO: PILES. IVORY.(ROWS,HUGHES SAMPLE PICKUP By: h. HUGHES SAHPlE LOCATION: LAB 78 BUILDING 7 SAMPLE DESCRIPTION TOR 3 SAMPLES SAMPLE IDENTIFICATION HUMBER Of bottles es: nume-sis: NT A LOT A (SODIUM NITRtlOTRI ACE TATE) IDA LOT B (ACID.NIOBN.ORTI NMBA TAMt 374TI7-7 (ALINETR PEED SUPPLEMENT) METM05 BLANK I PCB-467 I PC0-44B I PC8-44V.PCB-470-0U0 PCB-4Y4 RECORDED BY: P. mjpp REQUIRED ANALYSES: INCIDENTAL PCBs ANALYTICAL TECHNIQUES: GC/EC (IS) DATE COMPLETED 7/4/84 QUALITATIVE: YES SEN (QUANTITATIVE : QUANTITATIVE: YES REQUIRED QA/QC* DUPLICATE.METMOO BLAMT ANO HIGH ANO LON NATIVE SPIKES COMPLETION DATE REQUESTED: COMMENTS* SAMPLES MERE PROCESSED ALONG WITH THOSE LISTED ON AC3IIO ANALYTICAL REQUEST SHEET DUE TO SIMILARITY OP COMPOUNDS (ALL HERE ORGANIC ACIDS OR SALTS). HIGH ANO LON NATIVE SPIKES ARE LISTED ON AC3IIO. SAMPLE DISPOSITION: X HOLD FOR 30 DAYS SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES ANALYSIS REQUEST FILE NAME: AB3II0:LI MOMS 022995 me environmental sciences center WAITS I $ REQUEST WUt APRIL I?. 1184 REQUESTER: CHOCOLATE BAYOU/IVORy 10G M>: 1-84-04-12-02 PROJECT Noi................................. 494.31116 tw results toi fiics/mces. ivory.brows ANALYSIS REQUESTS SCNT TOt FILES. IVORT.BROOKS.HUGHES SAMPLE PICKUP 6T: R. NUQKCS SAMPLE LOCATION: LAB 28 BUILOINO 2 SANRLC DESCRIPTION tor S SAMPLES SAMPLE IDENTIFICATION number OT BOTTLES ESC n'j>*E:S) A-IIS 01 C/" A-230 123-: a-2?b os s/3 method B.anSl SO LOT C6C 1029 SAK-0 LOT CBO 031031 SA LOT CO: 1025II RCTHOO Blank l PCB-411 i pcs-4ie I PCB-47S.PCD-480-DL'P PC8-48I-LS.PCB-4B2-mS PCB-483 I PCB-411.PCB-4T2-LS PCB-413-ns I PCB-4T4 I PCB-4T5 PCB-470 RECORDED BY: P. HUPP REQUIRED ANALYSES: PCB ANALYTICAL TECHNIQUES: X GC/EC (IB) DATE COMPLETED T/t/84 QUALITATIVE! YES SEN I QUANTITATIVE! QUANTITATIVE: YES REQUIRED QA/QC: 101 DUPLICATES. 101 HETWO BLANKS.101 HIGH ANO LOW NATIVE SPIKES COMPLETION DATE REQUESTED! COMMENTS! SAMPLES MERE PROCESSED ALONG WITH THOSE LISTED ON ANALYTICAL REQUEST SHEET AB3II0. DUPLICATE ANALYSIS FOR THE ORGANO ACID SAWLES ARE YOUNO ON SHEET AB3II0. SAMPLE DISPOSITION! X HOLD FOR 30 OATS HONS 022996 Win NKMfflONSi KC W( UKMTW MUCTICU MlVtlS KQUttT nu HMKi ACJIItlll HONS 022997 N foliating It a drtatlad dltcuttlon of tht Incidental Id Rogulatlcn. HONS 022998 Analysis of InciaanUI PCts In Nmo Product*. Motto StriM. Itliiioit ond Effluents of Clotod and Control lad Motto Ncnufectur Ing Procottot 0. hoson Hughes Environmental Sciences Center Honsento Compa^y/Dayto^ lebC'atO'* ISIS Mcno'os Road Ooyton.OMo 4S40* The October 2l. 1902 federal Register ivpi. 47, 2c*i contain* * r, extensive definition of PCB-contalning products* waste streams, em'jsio^s o*d efflve-.ts fro* ma^ufactur ing processes ono gene'a I de* r * 'c* i nr\. c' nev-y?* Men should be used for these analyses. The Puf&cse of f s p*ese**t rec:**. is to outline the approach toxen oy honsonto's Cnvf-onmtr*:* Sciences Ce*tf in supplying analytical data which ea' be used for ceft if at io'. o' v;*ss**.c products, waste streams, ee- tsioni r>c effluent*.. In oroer for the *ater la! to be certified as net conta n*g C3t. t'e C*A set va-ious ieve;s o' Quantitation uOQ). be*ow wrrich a prosit, waste st'ea*. emission or effluent cow'd be certified to co^toi*-. -*> PCS4.. Tn* LOO Is defined on the basis of the concentration pe' resoUatie ehronutc9rophic peat. Quoting from page 46996 of the Federal Register, yci. 47, ho. 204, "Tr.is meohs that for a process to be eiigit'e for exclusion u'-de* the dosed pnd controlled waste process exclusion, nc sing'e pea- on a gas chromatogram registers RCEs In excess cf: ten microg-e->i pe~ cube met#* i* air emissions. 100 microgrons per liter in water effluents, one two t!c'ugrams per gram In products and uncontrolled waste streams.- Tn+re'or* ft-* are very specific definitions which nor.sonto can apply to "ts preducts, waste streams, emissions and effluents which determine whetne* these materia *, may be eligible for exclusion. It Is the goal of the environmental Scie-ces Center to supply Monsanto plants with tie proper data and odcuwnte: ion 'or this exclusion. Capillary gat chromatography/e 1 actron impact mass tpectometry (CGC/rt) It the Instrumental technique which the federal Register suggests should be used In the analytical method for PCB congener analysis. However fer most Monsanto products, waste straams. air emissions and water effluents, this Instrumental method oust be used in conjunction with on extraction method In order to determine what levels of PCB congeners, if any, are present In these various materials. The reaatnder of this report will therefore deal with how CSC will Implement this Instrumental method for the analysis of PCBs In various types of samples. . In order to analyte a sample for PCBs* using CGC/HS techniques, a representative sample of interest* or o representative extract of 0 sample of Interest must be Injected Into the capillary chromatographic system. The presence and quontltltas of PC0 congeners present are determined by comparing the PCB congener responses In the sample of interest with the MONS 022999 rnponm In m far ascn af tna atannaclyntiicaarllnastaenldNaridtico(fn.taain. inagi-taipt ftaanasyt)ontheroawctntaonIffi*Nr biphenyl). tha analytic of Nonaanta products and watt# itrNM can ta divided Into two types of CGC/HS analysts. The first ft for products and tact* streams whieh can ba chromatographtcally ratolvad from Cl I-biphenyl through CltO-btphenyt congeners. dan tht product or waste stream It present at tan all Hon tlaaa tha levels of tha PCS congeners. Thlt flrtt type of rwlytls only requires tna sexplt to Oa tnjactad Into the CGC/tt instrument and PCS congener artat coaartd to standard PCS eonganar areas. Tha mono type of anaiytit applies to Monsanto produett and waste streams which cannot be chremetographleel iy ratolvad fro* PCS congeners and for air emlssIon and water effluent samples. This second type of analysis oust first Isolate Into a solvent an PCS congeners which are present in a representative sample of the proAict. waste stream, air or water sample. Inis extracting solvent can then be analysed for PCS congeners as described above in the first type of analysis, since the extracting sowc**: is cnose^ to be chrometographically resolved from the PCS eongenert of inte'tst. Therefore an integral part of the PCS congener analysis revolves around the validation of the extraction method used to Isolate the PCS congeners and va'ldatlon of the CGCn$ method used to analyze extracts. In oroe* for Monsanto plants to understand the data that Is generated for incidental PCS cert ification. the following sections outline how data will be obtained ano validated for the presence or absence of PCS congeners in various Monsanto attarlais. (tractlor of products, waste st'ea^s. esr emissions ano #te* e'fiue-ts: If s**oie of interest cannot be directly analyzed for PCSs us;ng CGC/nJ techniques, they must first be extracted with an appropriate solvent Men ca*' be analyzed to* PCSs. Tni$ not only applies to the products c* waste strear.s, but also to e*r samples or water samples which may contain large amounts of products and waste stream components. Two najo- property differences between PCSs and majo' compounds In various samples can be usee to Isolate PCS congeners Into a* appropriate extraction soWen*. These a*e: I) reactivity; and ?) water solubility. LOW levels of quantitation for PCS congeners In samples which contain Mjor components in the PCS congene* elution region cannot tesliy be obtained unless these major components can be removed by their reactivity or water solubility. The inherent stability of PCS congeners and their high affinity for organic solvents and low water solubility are chemical and physical properties which can be e*P oitea for tMs separation. However It Is Important to demonstrate that* OK'ing this Isolation phase. PCS congeners have not been removed during the extraction. This Is done In two ways. The first way Involves the use of a surrogate compound which acts exactly like PCS congeners, yet Is mass spectrometrlea*:y different. This Is normally accomplished by using either oeutcrated PCS congeners or congeners which contain carbon-l3 rather than carbon-12 In the biphenyl structure. These surrogate spiking compounds are added to each ample for which PCS congener extraction Is required. and their recovery Is reported along with any PCS congener detected. However this approach Is vol Id only If one has Isotop I tally labelled PCS congeners for each congener close. Since at this time there era no surrogete compounds for all classes of PCS congeners (I. e. Cll'blphenyl through Cl! 0-b I phenyl ) a second type of extraction validation is normally used. This validation s.teo Involves adding at laast one native PCS congener for Cll'blphenyl through CUO-blphenyt congeners and measuring the recoveries of eaen of these native congeners when the product, waste stream, air emission or water : affluent Is extracted. These native spiking studies should be performed on representative types of matrices to demonstrate the validity of the HONS 023000 results. If no ortvIout doto It ovtlltblt for recovery o ail PCS tenotntr (l|iOtt fre* o epeclflc matrix, this native tolkt should Ot performed >n srdtr to vel ldata tno data Mina rtporttd. Slnct It It not ontleloottd that Ineldtntol PCS generation >111 be dettcttd for nontonto procettet. It it Ioperative that lha aeo>a quality control ttaot oa conducted on oocn temple or for aocn tarnpir matrix trot in order to validate the fact that If net congenert had barn present In the nontonto tanpltt. they M*>td have bean detected at the levtla required by thlt regulation. C6t/US tntlytlt Of eatraett. product! and uotte ttreant: At eientlonee above, temple eatraett. product! and aaite ttreemt can be injected olrect*y into the CGC/ns analytical tyttem If tne mejo- toroyertt dc not elute In the retention tine region! of the Cil-blp*<r,,' t'-oug' CLlO-bip'nyl congenert. Data quality of thlt analytlt ttet. It * to 3rnenttrated by tlnllar approechet outlined above for tample extraction. In order to verify that the Inttr^aent It functioning properly fo- earn tanpie Injected, an Internal ttandard It added to each extract, prodo:t or vatte ttream before It It Injected Into the CGC/ns tyttem. tithrecmrdlO It wtually uted for thlt purpose. The ebtolute preet of tne interna' ttandard In tne extract, product or vatte ttream analys't mutt be ".vlet of tne orea of tne internal ttenoerd uricn it aooea to tne KS corgeneenelyticei ttenoerd. Tnlt analytical ttenda-fl, containing Cll-b'phenyi through CLI0-siph*-> congenert, It analyzed under the tame condition! at the extract, p-oe.tt c* vatte ttream templet and from the Inttriitent retoontet for tne ten PCS congene' cletiei. levelt o' detection ond ouantltotion are determine: anc the anountt of each congener c'att (If greoter than tne lOO) It recorttj. loeaiiy. each temple thouid alto be ano'yzed after tpiking >itn ot leatt one native PCS congener In each congener dais at the 1ee' of quantltatlb(LOCI In order to verify that the 10Q concentration cou'c be eetecte: an: ouantlfiec In tne pretence of tample Interference!. Thit it done In ordeto thou that the CGC/HS Inttriaxentel analytlt It valid for the tempi* matr'x o' Interett. Hovever tome product! and uotte ttream samples -e not > i:i: < ulth toI vent I In uhleh PCS congener clattet have been prepared end there fore It It.not alueyt pottlble to analyze e native tpite of el I p'oductt end vatte stream templet. Thlt It not e problem ulth temple extracts, since tne extracting solvent hat been chosen to be compatible itn surrogate eng native spiking studies uhleh occur In the tample extraction step, describee above. Quantitation ond Identification of PCS Congenert: Tablet I end 2 thou hou the 20* PCS congenert ere distributed emojng the CLI-blphenyl through Cl 10-bI phenyl clattet. In addition these tables snow the character I at I c mattes end theoretical relative abundances for each of tht ten congener clattet. In order to routinely obtain analytical data ulth levelt of detection on the order of b.l ug/ml per congener, the matt spectrometer detector le operated In the Selected Ion honltorlng mode (Sin). Tnlt mode It screening mode and monitors at least tuo molecular Ion character Ittlc mattes over the elution time region of the corresponding PCS congener class for all ten congener clattet. PCb congenert are tentatively Identified from the ratio of the peek treat of the tuo molecular Ion chromatograms. If the ratio agrees ulthln HONS 023001 SOI of th* experimental ratio obtained from the K# conger*' standard mlrtli, and th* tvo rnki maximise within tuo wi spectrometer scans, than th* sample It reanalyzed mhll* monitoring all aatut of Interest for aotltl** lotntiricatlen of th* tea congener. If th* peek are* ratio does not agree vlthln }0t of th* experimental ratio for a particular PCO congener, then thlt retponte It not due to a PCO congener. iiwnoryi The above aopoecn aiion for rapid, routine analyses of extracts and templet of interest. Since f* positive* are expected, adequate quality control Involving the use of Internal standards, native spikes and surrogate spikes xlll 0* used to validate that th* data can be used for the certifi cation of th* absence of Incidental PCS* In Monsanto products, vaste strea-s. air emissions and voter effluents of closed and controlled vast* manu facturing processes. Text f Set INC0I :S!n:S<> Tet.lt 'lies! ISiTJJI :VH, IkTJOJ :Mh MONS 023002 T*lt |. Character I >tlc aassas and Isotopa aattarna of tf charactarlatlc aassas far ctilerablaMnrl fJireu*i pantecMorablaNanyl wamri. KB Congflr Class INtHfccr of Cengcncri) Cnaracttrlstic N*6r Of CMoMnS CII-0P (3) C12-0P (12) CIJ-0P (20 C14-0P (a?) C15-0P UC) 15? 153 iot 187 108 109 190 ?;o ??? 22 4 m ?33. 255.9 257.9 259.9 207.0 ?e.a 291.0 293.8 295.0 321.8 323.8 325.8 321.8 329.8 0 *<-> *(*> 0 *(-) 1_ H(I00) 1 x(IOO) 1 (100) *02.0 1 (32.0 1 32.*) ' 2_ *(100) 2 -(100) *(84.0) 2 *(64.0) *(10.5) 2 110.5) - 3 - x(100) 3 *(100) *(97.2) 3 197.2) *(31.5) (31.5) * 4_ 4 (77.2) 4 M(100) 4 (S8.5) 4 00.5) 5- 5 (41.7) 5 *(100) $ (M.B> 5 (21) HONS 023003 Table 2. CharacterltIt aaatat and ItoUpe pattarna of tha characterlatlc aaaaaa for hanachlorablehenyl through decachlorcblahanrl eoamri. PCI Congener Clait (IMfcfr of Congenert) ChOfOCtfHitlC Hsrotr of Rtffttft CMorlw CL4-BP (4?) CL7-BP (24) CLB-BP (12) CL9-BP (3) CL 10-BP (1) 287.8 284.e 241.8 24).8 321.8 323.8 323.8 323.8 324.8 333.8 337.8 334.8 3(1.8 3(3.8 384.1 341.7 343.7 345.7 347.7 423.7 423.7 421.7 42*. 1 431.7 433.7 434. ( 4(1.( 4(3. ( 445.4 4(7.( 493.4 443.( 447.( 444.( 301.( xt?7.?> acC 100) *(40.4) *(10.5) . *(51.4) x(100) *(61) *(35) >1(1.7) >1100) *(44.B) *(?i) - *(44. 1) *(100) *(97.2) *(17) *(51.4) *(100) x(8!) *(35) - - *(34) >(88.2) *(100) >((4.8) >(2(.2) *(44.1) *(100) *(97.2) (!7) * >(2(.5> *(77.2) *(100) *(7$.4) x(M.7) >(34) *(00.2) *(100) *(44.B) >(2(.2) * 10 10 10 10 10 ' 3 >(21.2) x'6B.4> *(100) x(06.4) >04) HONS 023004 n following I* o copy Of tho ESC/UMS Sood Laboratory Proctlcas Ngnuot. HONS 023005 .eoco UMunn runieu nmvu * CM * ftwlltl Cwiwl/ftnlItT Aliarlntl Vltritmi Cwiip March 1M* Crovp U<ir, Dltmnei iMljrala #ru)U--______________________ I. A. VtlttraMin MM|, torl--111 tCtOCM Cmiii ImviA to: km ____ iu/m a InlrNMiul Iciaui Cutir D*TtM UWntirr DlftM, Ohio 45407 HONS 023006 tailz or comns 1 MJnilm II Icepa III Aaalyala A. DtlMl 1. QA/gc mira 1. laaple riipatailn QA/QC a. Hetbod llanli A. teplicatae c. Iplkee I. laetriaantel Analytic QA/QC a. laetruaaatatlon k. Alanka c. Quaatltatlon Internal Standard d. Iteadardt C. Dagreea a( Quaatltatlon I. Qualitative Analytic a. Tentative k. Confirmed I. taal-QuantItatIve Analytic ). Quantitative Aaalyala I). Quality Criteria aad taaadlal Action 1. Quality Criteria a. Ilaaka k. kacavarlaa c rtaclaloa d. Halt at Batactloa a. Accuracy 2. taaadlal Action IV Data V taaple Dltpottl nevus flaara 1 tkaapla.ef 0C/18 Logbook page . 2 tuayli of OC/IC Logkotk pat* J tnaaple of Mac/TapaLagkoek page Xus 10 f 1 * 11 HONS 023007 1. Th* Hit rtjKlhM ( th* Oltratrac* kilrili (rv m11I| M*araac*/*w*llty cmtrnl rntm mi 1) to mm that m ItWinnj |mih kick *w*llt? twitl! Mi 2) te MlatlU tta Mcrnuy racntd* that fctmM Utontm ftrtnMKI. 11. low Th* m ! thla Mil liclirfN am* of eu **t iHtlllulln *ddr****d in Ik* IK MCllM Mnwal (Hi *x?*oda n?oo certain mm* wh*r* QA/QC ?ractlc*t ii((*r ftM Ik*** dMcrlbed In tk* **ctio* naaual. It 1* Intended t* k< M*i alenf Vltk Ik* MCllM s*nv*l I* rrovld* con?l*t plctur* of Ik* CL? within th* Oltratrac* Anal?*l* Crow?. 111. iMlwli Th* |Mt*tlM *f analytical raojlta within th* Oltratrac* teal?*!* Crow? (MtlMl? lavnlwo* two ?rncM*a: a*a?l* ?ra?aratli>n and lnatrwMntal an*]?ala. Im?1* ?ra?aratlon lawolv** on* nr nor* of a **rl*t? of tockal*u* Including alraetlo*, dilution, acld/baa* wnahaa, coImb chroaato|ra?h?, eoncaotratIon and aun*reva *th*r l*chal*w** to raodar th* aan?l* la aultokl* condition for lnatrM*nt*l anal?al*. laatruncntal analyole tauo th* ooltahl? ?r*?ar*d *aa?l* *ad latroiwc** It lace an aa*l?tlcal lannoant to naur* th* i**lrd ?*ran*t*r(*). Both of than* ?roc**a*s cm h* i*crlb*d h? clearly d*fln*d and **?*takl* Mthoda called aaayl* ?r*?*ratloo nathoda (S?Ha) and laotrtetntal M*l?ala natkada (UK*). f?M* and UH* na? h* c*nbln*d la avMroo* wo?* (deycndlng **** th* Mtor* of th* mb?1m and th* aa*da of th* c**t*n*r) te ?r*dac* ooccaaofwl aa*l?tlc*l yrotocol. tot ananpl*. **w*rl differtnt CM* M? k* wood to ?todoc* o*n?l*a tkat ar* owltakl* f*r *n*l?*l* b? aln(l UH. Th* Moowr** lncor?arat*d Into each of tk*a* exycrlncntal ?roc*o**a to ananr* that an atHamat *f th* nuallty of th* r**wlt* can h nada cmatltwt* th* QA/QC ?r*|rm fee a ?roJ*ct. Th# followlai aukaactlona daacrlk* th* *lan*nta of th* aaalyala ?roccaa: A. Ntthoda Nathoda ar* th* written docMMtatlon that daacrlk* th* anal?tlcal ftncM*. Th*? contain nnffldMt detail onch that a c*n?tant MlMtlot or tochnldaa can rnadll? ?rforn tha r**wlrad anal?***. Ik* nanal ?ractlc* 1* to kaw* nathoda tkat doocrlka tk* *m?1* ?r*?aralien ?roc*aa (ttlio) and nathod* tkat daacrlko tk* inatrwnantal aa*J?ala ?roc**a (UHa). lack a*tkod dr**l*?*d wltkla tk* Oltratrac* Aaal?ala Cr*w?a la aaaliaal a Mtbod nwnk*t aa daacrlkod la tk* UC faction Haawal. Nathoda ar* oktalnad fren warloua aaarc** lnelwdln* la haan* d***le?nant, nodlflentl*a/ada?tation of UtMatnr* nathoda, or afaclflc BCOCOMl nathoda dictated k? a*amn*nt afaoclaa. Notkodo na? k fanall? validated k? a Mtlaa of asyMlnoat* tkat daacrlk* a claMlcal walldatlon orotocol or aa? h* l*o !coronal? yrouen win* to factor* aweb a* fr**w*nc? or woa, cuatooar aaada and HONS 023008 mi/tWai raetrlctiaoe. la aj aoea a QA/QC ptfra fa applied the aaalyeie la provide a aaaaara af ibt quality af the raaalta. Onleoe a QA/QC itafna ta rmnlM by a pretocel (e.f., DA Hull ta (all protocol), cartala mining QA/QC aaaaraa (dependlaf open tka aaalyale typo) ara Incarcerated lata all ntratraaa Amalyele prujetta. Tka following aakaactlaa deecrlhee tka Vltratraca QA/QC pragree: QA/QC Prograw Aa effective QA/QC program laaerporatee aaptriaante that provllt Information ralatlva te aack af tka following quaetIona: (1> Ara tkara any lnpurltlea, background er contamination that will lallutnct tka rteulta? (2) Mow reproducible ara tha reaulte? (1) tow wall aaa tha analyte ha recovered fraw tha eanplt matrix? (1) What ta tha limit of detection far tha analytic? (5) What ia tha dynamic range af tha analytic? (t) What la tka accuracy af tha analytic? All af thaaa queatloat ara addraaaad by praytrly eelacting/epplylng the naa af klcaka, rapllcataa, aptkea and atandarda In a QA/QC prafraa. Tha dlacnaalan af tha aaa af thaaa QA/QC tochniqoaa aa they apply ta Dltratraca Analytic Croup actlvltiac la beat dona by eaealdcrlnf tha aanpla praparatlaa and laatrumental anal/all praaaaaaa aaparataly. 1. taapla Preparation QA/QC a. Method hlaaka lepreaaatatlve Ilaaawara, aolvonta and raacaata ara mead with aamplc matrlcaa which ara atallar ta tkoaa for which raaulta art balaf reported, pat da not cantata the amalytee af latoraat. Method hlaaka ara analyaad at a frequency aomal to 10X of tko aaalyiad aamplaa for aaapla aata uklch art multlplaa of 10. Ac laaat aaa mathad blank la aaalyiad for aaapla aata eamtalalac between 1 and t aamplaa. k. lapllcatta . If aafflclaat aanpla anouata have beam euhulttad for analyala, rapllcata frequency la tka name aa tka mathad blank frequency, if at all poaalbla, rapllcataa ofconld be afccalmad from tha nano aanpla battle la order to mlmlnlaa aaapla lnhonotaaalty problae due to capita balaf taken at alightly dlffaraat tinea. a. Iplkaa - If amfflclaot aaapla la auallable for each aanpla type, tka aanpla la apllt and aplkad at two laaala with HONS 023009 Ik* Mil** (aliMil) aMlyt*(*>. Tk* Imli ni typically h (law) aad Ml (ki|k) tk* HIltlHlW d*t*cttm limit mi ***** t*ckai*v* In **tl* Mtlog *k* IMl *1 iHMtt** far **ck Mtrla. 1k** 1 *d kl(k owlkoo ** coadwctod *t * limm> **o*l t* tk* Natkad Blaak Infancy. Otvionoly *fUli| iriik Ik* **ti** aMlyt* ****** k* In* In ulliitn ntlrili i*c* IM* |t*nmMI ksovlodgo *f Ik* limit]! *f ik* Mlyto(a) 1* Ik* oaapl*. Otkar tockoi*ii*o * un to ***|*i* tk* mttac- tloo/nconry afflclMd** for tk* OMlyto(a) *f l*tt**i. Woolly oxtroc cloo/roconry *lfjcl**cl*o * d*l*rol*l fa* **ck ooofl*, at***, 1* principle, **ck aaapl* ooy **pr***ni dlffarmt Mtrlx. TM* eon k* In* my Molly ofcoo tk* d*t*ctlM t*ckoi*uo 1* moo *pet**B*t*y If *a lootopinlly 1ok*1*0 **r*lo* of tk* *ulyt*(*) to *o*ilklo. Docmbc*i1m of **tr*ctlM/r*coT*ry offlcioncioo 1* oot r**utr*d far **ek inylt If tk* anylt motrU to* mi of **101 1* coBOtoot. Bowovor, fo* a ooayl* oot for oklck tk* alallarlty of ampl** 1* hi taovo, *od fo* wklck 4**u*i* *ooflo 1* avoilokl*, oock oaapl* Boat k* apllt and yU*d vltk Moon momi of tk* Molyto(t) of Intotoot to dotorBioo Mtroctlon *fflcl*ncy. If ado*uot* ampl* also fo oot orolUkl* n tk* ldmtlty of tk* *nalyt*<o) to not Mown kofoto tk* fact (l.*., trldoocoo onolyoto). aorrogoto oylhio* coayowod* My k oaod to null Mttoctloo *ffltl*ocloo to oock ampl* witfcoot actoolly oylklo* **ck Maylo vltk tk* Mlyt*(*> of lott**t. Tk* ckolc* of tk* oo*TO|*to oyloioi cMyoood la tollorod fo* oock Malyt*. Tkl* Oorro|oto Boot k* ckoMo tkot It 1* oltkor ckMltolly Idootlcol to tk* Mlyt* of latoTMt (fo* BXOoplc ooing lootoylcolly lokl*d ooolotooo of tk* (MlytM), * lo cloaily Hallo* to i*ibo of ll*old/ll*iild partition pop**tl, ckMlcol rooctlon propottl**, coltom olotloo propottloo o* otkar Mtrlx loolo- tlM p**p*rtlM oklck or* m*4 to l*ol*t* tk* *Mlyt*(*> froa tk* uoyl* Mtrlx. knotka* proporty of tko aorrogoto piking coapoood 1* tkot it oot k* promt lo tk* *aapl* kalog *ooly>*d. loatnuoatol daolyal* Qk/QC Tk* flMl *t*p la oktalolog analytical r**olt* laoolo** tk* m* of M opproprlot* iMtttMMUl ttckal*** to prodoco tk* noolyticol data. (*o*r*l Qd/QC practlcoo Boat k* lacorporatad la tkl* proc*** to bob** oolldlty of tk* data. a. loatnoomtotlao Coiofol dt of IBtotloo of iMtnmat bm|, calikrotlM. dad Mixtooonco 1* MMBtlal fo* tk* goMratlM of klgk aoollty tooolto. Bock Mjor Intrant vltklo tk* Ultrattoco dMlyol* Croop will k* tk* ooalfood t**pM*lklllty of a profmolOMl aoployM dMl<Mtod M tko iMtrant Itoward. Tk* laot*M*Bt lt*wo*d la caapaMlkl* for aoklog awr* tk*t l*kook* oro avail- kl* mi proporly c*apl*t*d ky laatnamt M*r*. It 1* tk* HONS 023010 IIMMIHIU; (I aack UMtUul Mt>| tho OQultuoat W Mm! all Ik* fntlMM toti taawlraA la tka Iqteot. 4a aaflt at a ya|o in* a QC/M laQkoak it |1VM la W| > a4 tkat af a 8C/K latkaak la |lna la ttfn 2. laatrwaaata will ka callkrataA accorllaa la tka laatrw ast uaaafactarara' ayaclflcatlaua ar accorllaf ta tka Baikal kalaf uat altk tka lMttawt. 4 lag at laatruaaat callkratlaa will ka aalatalaa4 wltk tka laatmont. Ika iMttwiii (toward will ka raataaalkla (ar aaaarlat that yravaatotlaa aa4 carrotlira aalataaaaca yrofraaa art carried awl aa all laatnaaata talat kla/kar loapoatlhlllty. If a aaaclflc (takla la aatod ty aa laattwaaat aaar. It houlA ka aatod la tka lofkook aal tka laatruaaat ttawar4 aotlflol aa that ayproprlat* corraetlvo aetlaa caa ka takaa. k. Ilaaka A aolaeot klaak will ka analytad at a fratuaaey ayual to tka watkaA klaak. Tka aatkod klaak caa aarva aa tka aolvaet klaak yraaldad It la claaa la tka araa of tka aaalytafa) of lataraat. Tkla atactica allalaataa tka aoaalklllty of kackfround lnatruaantal coataalnatloo. c. Quaatltatloa lataraal Itasdard A aoaatltatloa lataraal ataaAarA will ka addad to each aaaplt followlB| aawala aroaaratloo kvt arl*r to laatnaaatal analyala. Tkld taayoiad will oarva for Aatatwlalai ralatlwa raaaoaaa factora aad far corractlai for warlatloaa la aaaala lajactlon woltBoa aad awaaaratloa of aolwaata. A. ItaaAarAa ItaaAatAa ora aolutloaa of tka aaalyto(a) of lataraat aaaA to Aotatwlaa tka raaaaaoo of tka Aatactor awar tka raa|t of aaalyta caacawtratlaaa fawaA la tka aaaylaa. Tor Quaatitatlaa aoalyaaa, aofflclaat ataaAarAa aaA roallcatloa of ataalarAa will ka rwa ta Aanoaatrata ltaaarlty aaA yraclilaa af tka Aatactor raaoeaoa owor tko roaw* af aaalyta coacaatratloaa. (haul! tapla coacaotratloaa fall awtalAa tka AaaeaatrataA llaaar roota, altkar aAAllloaal ataaAarAa aro ynyaraA ta aafpaiiA tka raaaa. or ayrropTUtt Allatloa/coocaatratloa af tka aaaala la Aoaa to aloca It la tka araaar raa|a. katraaa of Quaatltatloa Tka laforuatlao yrawldad far aay aortlcolar aaalyala la tallaraA to tka aaola of tka caataaar. la actaal atactica tkaaa aooAa wary acroaa tka kraaA taatlaw (raw tka graaaly Qualitative ta tka araclaaly Quaatltatloa. It la iafataatlwa ta iMlaa wkat la lawolwaA la yrarlAlai tka aarylai Aaarooa af ouaatltatlaa roQulrad ky our caotawora. HONS 023011 _ MauM fcw _ HP 5985A - nr Menu i. t>MfU ( a/m Ufkoot mi. HONS 023012 mpsMo Ce/rc MMIMimNlttt H - MQNS 023013 i. 4**1 itaiia* <uiriii Qaalltatta* aaalyala tayllu a* yaaatltatlaa at all hi titkti mu ealy tk* Ideality f tk* ayaalta) ytuat. (e/M li yartlcalatly affllnUi ta tfcia In* *1 aaalycla yraklcs. Two In** at ilaatlflcatlaaa ta to aada: a. Taatatla* A taatatla* ldaatlflcatlaa la asla aa tto toil! at tka aaalyat'a )i*|iani at a aatck tors*** tka aaaa ayactra* traa tka aaayla at a aaaa aaattna tiaa a raferaec* likrary. Tkla la aftaa Aaaa tar tka lar|a aaakar at coayouela feual la a viltaeaa argaale aaalyala. k- Caaflraad A caaflraad ileatlflcatiae rttvlraa tkat tkf ckreaatoirayktc rataallao tlaa aaA tka aaaa ayactna at tka aataevn cooyoul aatck tkaaa at a Maw ataalarl ef tka taatatlaely ilaatlflal ceayaand. Tkla la aftaa Aaaa la vldeecaa aealyaaa kaa ataalarle caa to aktalaal far taatatlaaly llaatlflad ceayeaaAa tkat ara at caecara. Tka aarval QA/QC ratalraaaata far yualltatlaa aaalyala ara (1) aaalyala at a klaak, (2) aaalyala at Aayllcata aaaylaa aaA (1) act at a callkratlaa ceayoual (aesally Sacaflaaratrlykaaylykaayklaa. WTTt) te aaaura tkat tka aaaa ayactraaatar *111 yraduca aaaa ayactra tkat caa to coayared with llkrary ayactra. 2. taai-Qiaaatltatis* Aaalyala lwl*Quaatltatl*a Aaalyala axeaada tka laferaatlaa ytoaldad ky a Caalitatls* aaalyala ta laclada aaaa aatlaat* af tka aaewt at aaalyta(a) yraaaat. Tka aatkaA af aaal-tnaatltatloa laaalaaa tk* ceayatlt** af Aatactat taayaaa* af tk* aaalyta(a) vltk tkat ef aa lataraal ataalarl. Tk* aatlaatal coacaatratloa la aktalaal ky aaawlat a aalt raayaaa* factor katvaaa tka aaalyta(a) and tk* lataraal araalarl(a). la lallcatlos af tacaaary froa tk* aaayla aatrla la aktalaal free tk* racaaary af tk* surrogate lataraal ataalarl(a). ). Qoaatltatlra Aaalyala qaaatltatlra Aaalyala yraallaa for tk* accurate aaaaaaaaat af tk* aaaoat of aaalyta(a) yraaaat la a awyla. Te ka akle ta la raaatltatlr* aaalyala aa* aaat Me* tk* Uaatlty ef tka aaalyta a* tkat ataalarl* caa k* yrayaral far aylklag aal far tka aaaaratlsa of callkratlaa ana*. Tk* aatkaA af yaaatltatlaa la kaaad aa a tkraa-yelat callkratlaa cacao aalaf araalarla af tka aaalyta(a) af lataraat east tka raac* f caacaatratlsaa la tk* aaaylaa. A aaayalat eallkrstloa aatkal aw to aaal (aa with tk* lahoratery lata HONS 02301k eyetea) primal tkat Ibault; kae lm laaeeetratel mr tka aaacaMrsttoa raaga af tka saarlae aelag itaWaria a( tka aaalyta(e) at tkaaa aascaatratlaaa la tka raa(a. Ikla callkratiea caraa ta tkaa saw ta atarita tsaaaattatlsaa af tka aaelrte(a) la tka min rU aa aatataal staalarla aatkat at aors preferably rla iattaaal etaalerle aetkel. rat tka latanal etaalerle aetkel. tka aaaatltatlaa lataraal etaalar! la aMat ta sack af tka ataluli (Jaat aa *ltk tka aaarlaa) rtlat ta lastnaaetal aaalyele aal talatira taataaa* faetata ara letetalael. fat Qeeatltetlwe aaalyelt tka Bata aracttaaattt la ererstel aa a kreasie*rerklc letecter. Tka MS la tkatafara twael aal ererstel la aaaaar ayeclflel ta tka arrrewel aetkel tatkar than aatag a callkratlaa taataaa! aa regalral far aaalltatlva aaalyete. Quality Criteria aa! Baaellal Action Tka latleelea af QA/QC aaaaaraa tala aa aaalyels yro|raa kat little aaaalat aalaaa tka retails ara lateryretel aal attraprlata act lee la teaae akaa aeceeeary. Tka ability ta la tkla aitiaat aeaa atl af crllaria tkat trill trl|far a recreate at raaadlal attlaa. Tka fallawlaa aakaactlaaa leecrlke tka trltaria tkat ara aaal la tka Dltrstrac* Analytic Crauy ta aralaata akaa aaallty teatral lata tallcata a aaal far eartatllaa aaaaaraa aal ahat raaellal attlaa will ka tatan. 1. Qaallty Crltarla Tkt ararrlllat aaallty crltarlea akeat all athara la: Be tka retain aaal tka aaala af ika taataaar. Tkla lataralaattea will ka Bale jelatly katweae tka taataaar aal tka aaalyat. Tka aaalyat Beat aaarelaa cattles la aat allewlag tka taataaar ta araratata. alslattryrat ar aalatestlaaally alarayraaaat tka lata, la aMItlsa ta tkla prlaa aaallty crltarlea. tka fallawlag taalltleaa aaat ka set: a. Blaeka - la tka sweat tkat a blank ymincea a poeltlwe walaa. It say aat ka aaal aa a aalll klaaa If It axcaalr 101 af aay reyertef walaa far a aaeyla. k. kacawarlea - Becewerlea far all aarratata aal aatlwa ayleaa Mat 11a la tka range af SOTtlacareryclSOX. c. freclslse rraclalaa will ka caltalatal kaaal aa tka racaaarlaa af aatTagata lataraal ataalarla. iwaraia raterarlaa will ka caltalatal Mtk I ataalarl laMatlea far aack aaasle aat. Ttpllcata aealyaaa aa1 law aal klgk aatlwa aylka recewerlee aay alee ka aaal ta yrewlte ellltlsaal laferaatlea/laalgkt lata tka rraclalaa af tka aaalyale. HONS 023015 d. Uill af NlicitM " Th* Halt af taMilM OOO) >111 aaiaillj k* atatad * tk* nltt *1 th* law lml wtln irIM If It 1* VMmrW al aaMtlflahla. OmM tk* law lml aatfw* wplka t k* rac***rad. tk* LOO will k* atatad * k tk* wtla* af tk* kl*k lml Mtiw* *flk* if it la racavarad aad *a*att(Ukla. Ikaall Mltkar *fik* k* recantad, laclaia* Mat k* aada r*|*Nla| tk* adwlMhlltty *f raffoceoalat tk* aaafl*. tkoala all aaafl** total* *wtk l*t|* taaatltlaa af tk* aMlyta(a) tkat tk* l*w*l* af tk* law at* klgk tflua at* laalfalflent (<lot) ky ceafarlaea, tk* aala* af tk* LOO kacowaa It** la*orient aad la atafly *t*t*l * tk* LOO (at tk* laatmmtal aaalyal* proem dataralaad ky tk* Malyaia af *taa4*rla and tk* ability te raaaatr a. ccat*cy - Tk* Mcaracy af tka aaalyaa* la bait dataralaad ky nalyllai lew Mafia Mick caataUa tka aaalyt* at aca* yraat*rala*4 lrati (a.|., aa m ataadardltad aaaplo). if tkl* Iff* af ataadard la aot available tkn tk* lew lraal and kl|k lraal aylkaa can k* aaad * a aaaaura af tk* acewtacy af tk* *Mlya*a. (Malta Mat fall wltkla a range at 111 ta HOT af tk* aacaptad walk* fat tk* aaalyaia ta k caoald*t*d aalld. If tka aka** taallty erltarla at* aet wt tk* analyat will iMtdlataly Matt* tk* Hid far *al ataat af raa*dlal action that way be atetatary. 2. tamdlal letIan Tk* fltat caata* af actlaa will k* fat tk* aMlyet and fat group latter ta eoatact tka caatoacr aa* dlacaee tk* rcaulta yointln* out tk* llaltatlm* af tk* **ta ladlcatad ky tka taallty caattal raaalta. At tkla yafat tk* avarridla* *Mllty criteria* af caatoacr Midi will k* addrana* fltat. It caal* k* that tk* ewataacr'a aaadt are a*t without aaatlag aaa ar ware af tka ether criteria, la each a caa* ao rMedial actlm 1* aaCMMty. It ceald alto b that the caatoacr k*a each laud far tlghtaM* la th* raaalta that hla aaadt era aot a*t eras thoafk the athat *aallty criteria ar*. Tkl* weald triu*t farther aaalyaa* with tighter M*llty CMtral daalgnad areaad th* raaalta *btalaed (*.(., replication! af fealtlva* ta Mttar aatakllah fractal** ar OfiM* af aaa datactad aaaplae ta batter aatakllah th* Halt af datactlaa). la caaaaltatlm with tka caitaMr addIt local azfatlaaata will h dMl(**d lacladla* lb* affrayrUt* taallty coatrol te altteataly provide th* raaalt* af aafflclMl taallty ta aaat th* caniHr'i aaada. H. hat* Thia MCtlM d**l* with th* aahjact af data tad how they ar* aktalaad, recorded **d tadacad M * ta ha aaaakl* la a rafert aad yat raadlly awallakl* far rafarral aad laayactlM. HONS 023016 ft* taaylee rtll M lakelet ritk ley Makar at aaayla layla eccertiai t aba Ktcafcn teecrlket to the nc Cm lea CU toaail. toaa telleerat ta tka aaayeealklt laatotoal yereee, tka aaaalaa Bey tkaa receive attitleaal labelto# aa taM aeceeaarr. Ikle attitleaal lakallai will ka luaiatak to a lakeretery lathee* a>4/ii aatakaab. Theee lathaaka aa* aatakaaka will ka aaa* ky tka ea^lyete ta not* m aaftteaal aart aa* raaalta abtatoa* fraa tka aaaalaa. Tka lakeretery aetafcaeke will ka ftlla* aat to accar*aaca with Naaaaata kdlan Wetekeek hacatim. kll raa tota seaerated lar a |l*aa arajaet, ahtch caoaat ka ceaeealeatly pOnced to tka lakeraiery aatakaak (a.*., akraaatagraaa, caafatar eatpet. ate.), rlU ka died eater aaaa yreecriket ar*ar (l.a., lag aaakar) ta a caatral (11a aatar tka auyervleen a( tka (reject leaker aaf/ar 4* tractallet. Matt at tka tala (aaarata* hy tka Ultratraee taalyele Creuy ata caayuter Mata tiered aa aaiaatic (lace. In attar ta artklee thaaa tata tka erectile file aaaa aa* tlac maker aiaaclata* will tka aaalyala will ka arlttaa tawa to the lakeratory aatakaak aat/ar taatraaani le|beek. When tka tlac la ceayletaly (all e( tata an aadra aaatlta* tlac laat* ar ceyy al tka (llaa aa tka tlac will ka tranafarred on aatattle tape. A legkoek will ka kayt (at racartlni tka tlac maker, aaaa ana prelaw aaaaclata* wltk It, aleef with tka aaaaclatat taya ant (11a aaakar ta which the tlac waa trate(erre*. An aaaayla a( each a leybeek la (lean 1a riyura ). When the tata arc traaalerret a warlflcetlen yragraa la neat ta check all traneferre* recarta lar carractaaaa. Whan cayaa are (Iliad (they typically halt reran ta ten dire lmagaa) they ahealt ka atarad la a (Irayraaf vault. All celceletlene a( the raawlta a( the data will ka ayecllled In the aethadt wind. Tkaaa celceletlene will ka entered la tka aaalyete lakeratary aatakaak unlaaee they are canyatar yaearatad. In thia caaa, a cayy e( tka caayuter autyut vlll the (Had with tka raw tata. The (reject Lander will ka raeyeaelkle (ar checklny thaa tarractnaaa al tka tata. . frrT- itr**1 taaylee will ka dtayaaad e( ta accerdanca with tka taetmctleaa an tka AnaCyala layvaat (era. The aaly ancaytlaa ta tkla wawld raault whan the aaalyala teruli a yreklaa which rayalraa aaayla dlayeaal to a aaaaar acker thaa that eriytatally eyectiled. II tka (reject Laatar aatae (raa tka raaulta a( tka aaalyala ckat a yataattolly taalc prelect waa yraaaat to the eaaylee tkaa the aaaylaa will ka tlayaaat al to a Meant taaaet tala by the tolaty Dayartmant. The tata af aaaplt tlayaaal aat tka aaaaar ahaelt ka aetat aa the rayaaat Ian atarad with thar raw tata caaylatto( tka chain ef ceacaty al tka aaayla. HONS 023017 Wit**1*,t kna (H N* <aa| trm-i Utmt IM ka * (nit n /* at <**> . bm (**/*) tfr 9%. to**} ay />/ fc* fit) i (*tgM* lrf)> IK tftUi) C*3 im l r*r -*Hj j/^4, bn Ai/o 0Wrt II .- 6*f4r) 6WiO Cl>4Vf) */ fV///if% 6*N W' ti V*f'\ CrZ>M<t) UK SM n% 6*7*5 oi (k*t> u*} sn 3*11-0 |> (**1)0*0 sn ' s-ii-e> &K. 1 itniU) 6> W, / i. " Bf# 6Co) JrvAMnyHQ.jMoftMK. A|tf Vr/fj tfD'/O'i /O rMiAMQ ftm) ** /N 4ftuf)&g " ^ 'U 4 ft>7/ (j) <?7/ (*j Ok (S*lHwn iltf (<**!*) Ckftl sn )/*> >9< IV/ '**} /*& HflH` - i/'V/J Unity **- **> /> f/**) (V <*) A 36 A2> *MJU hi* *1*1* /Vf fMtf) /H (rnr) f*l /Ve?) t*J m 0**) 00 o*; J JJ, a n ti Sfyyt* w-i/Aj Uihs cVu k/>/^3 i (M) JK**v3K A* f*$*)$*J ftw* jl) <*3 */*/ i #*3 ***> ir . 4 - efJK #m I r Gblffr) G)13(5j *TS (fc> G3>13(7) 9P1*(P) >13 (V GM3 Ci; G2>fu CJJ tov U> ** 'J- i1' V0 6i-. C0 62) IP-'O') fc&13 (1) i fV> mw 1. hafll ( IUC/Tih U|kMk Mt. HONS 023018 Ml (tlltrtlta: fiM W-BBST tollNtK'i I--It M. Tit Ctlltcttr't 1--it M. TMt Mk-6 _______ _______________________________ Ctlltctar'i *--it M. Ttl itcttita *r s--all--: cp Q3ioutrt<ttr^fct|'i|/f imiirkshmI *tu Mm> StatMaf: Mxyi^fn /.. Tjr-- Ktctai prMcliil (--la* Mttrial: fr _______________ /?>! 1 comcTot Ntaiaata Caawr 1.1. h m >!/ Taui m 57s TlltMat: tiWi t 93- YT?/ Caattct: . 6r* j Ctlltctar'i Mat: Dtaala Havton_____________TtltKO": (fjtl 5>/- ?/// (tlltcttr'i HfflllttItt: /"A Cs>i..,f* C(K//| ,, AMrtti: / 0, So* Hi 41 t ia. > T* j > " Ctapaajr Ctattct: (raj Intwlat: Y>~ ?! *' tat, ttarttt. tat mtftt aafttr m trt:ntlon rtctWIm atalt *' lat, t<lrtat. tal ItlgKit aattf a tcftaimita raettiit uapit tuom iot a w or w w n iw HlMUrt----------------------------------rrtTi laclutlat #aft HONS 023019 oummomT omims w isii'm OBUIg CDSTOOT Kt if tolltcttw: CtllKttr'i lwii *. Tit CtHtcttr'i Iwii it. Ttt CoUttttr's 1--it it. _S4____________ __________________________ _________________ ItctMtn if SttH>t:CC 101}llfritf<^y<' NwltrBliftut Sltt Mtrttt tf Swtntf: fAte el. t, A. j. . - Tjth tf tftCMt irtfedi* M*lt* tittrltl: Q-^c. it_____^ ^b-.vmi Nnintl Ct> f. 0. It* BMI i" T 11 Mtr. Nui NMT Al.i*. *?r/ -------------------------------77j----------------------------------- Ttltthtot: (W *)i- *>)/ CtfitKt: .6 (ri j CllllCttf'l lOl: ^avlon Ttlttheot: (?/J) }*>-}> i/ Ctllacttr'i MflHttltn: ^Afn^ig Mtrtti: P.OAt* ?// /fU:,, . T* i 9 > // CftMf Cmtact: /P.A Ca>u IstMffOA: /**/ ------------------------------7----------------- *-- Mlttttt t^tr tf r|nimto nmum wtU " hi, tilrui. hi Unp-- wur tr naiim wpi* tounoiw MiitKtM m awo HONS 023020 c a u tc m a i w i iwoamTioa owuft Of CUTOOT ate Of Clltcta: Colttctar'i Iwwu . T*-- Caltetter'l wim. Tit Cel letter'I SaarleOa. ___ _______________ __________ Tit ___ lecetlen af leaellaa: CTC 01 tniwur SMfilC HaulerDItaaI Jlta Otliar (iirleln) AMrail af SaaaHaf: Mft.ta.ti. CUmUt-t A*yt^ Tjrpe #f rracatl p-edaclt* *r'W aattrlal: Cry.:c di,~ . ( f... >n Neateata Coapeyr t. 0. In HR 7// . Tam 7tn/ Cal latter11 Peae: Baiwtla Have an Cel letter ! Afflllttlea: tr MrMI: t. 0 ttf ?// Al . : Ceapey Central: $. 6 /- J Telephone: (aR) >7 J- /-// Contact: /* S. 6r*y______ . Telephone: (jfA) Sit' l/(/ C. ___________________________ & ./JP''_____________________ [tendon: 7 * ! L. liaa, aHraaa. ml UiafMaa Mitf at orpaaUatlea rocolelne nap`a m w tiw cm m or mstmm sipuurt' TTTTT Incivslae ratal HONS 023021 M U M M M I IM AM S M 1 1 W Jkisslasm Oiti r CallKtlMi CilljcMr'l Iw1ti. Tit \0bb tollictw'i *>l in. Ttu Clllltttr't Iwim. t< UCItlU If SulHlAfe-Q^ fUtfO\Q|l5aJhnil,UfDliUtal SIU _____ Ottir (tMUUI ~___________ aojtmi k sminr VO. BOX nW .1^511 Am if incut jnJiclaf uaplM uttrill: Qv\wA\liC. ChfiVflxCIlA- ____ _______________________ _ Mututl CNV f. 0. Oh uuft/ 1i ii OUy. lull W /II.:., _____________rrf'fHh CllItctor'i I--t: *' TlliphOM: () *T7- l / Cutlet: f 6 , _____________________________ J T*l***""*: 0^ s&SST Clllltttr't WUttlu:lht^gt!M ______________________________ ,^,jay nu ' ^ilMiii ^-s, Tisn Curt"/ Cutlet: Vvt*. Utiulu: ^-5 H\ *' Im', tJJrttt, im ItltfMM mtr or irptnimiO" nctlrlnp MapIt lui. uarttt, m tinpmti wmtr if iryuumii rtctmij tupit MlinOVN M K S X S O J JO MIMO HONS 023022 MiiwMMM aM4iM inisnxD MU *f Cellectlee: Cel teeter`t I ,W flBHB! Cel letter'! Shlllhe. Tit MlKtlf'l iwllli. Tit lccitlm if SeapHef 4klSuL >n*wi -----Other (t^TP. MOretl if MMif?.o.So7nw Awe if KpreKcIeIiIi KkUuuidhf Mele4 tthrill , 0 liter , (I(till Site \ p, Chfi.Wci^- Nentlftte Cot*"/ r. o. lei-wn >" Miti etty. Tun ftwe /tr,k >rf ~T7T Telephone: (400) 1 M - Centect: * 0 rt * c1 Utter LV_S\i. Til them: fl\H sg\^\U Collector^ Afrit letten: tMtteMayp g.v_ Bf)K *\\\ iCUi\j _:Vfe^\s..ntnr Ctne*/ Centect: * Litemlee: ______ " eet. etrett, it telephone --her er erpeouetion reeeitit title eet. eeertii, et mep^ot wtr v erpenmtten recelelnp eetu m iin m r ^eoitaJhoe ioVinb MONS 023023 au*m cwtot Nt Ollccttw: t- i\-%* C*1tocMr'i C*1Ucttr'i --< * -Tfri < M______ CtUKttr'i ***' . Tta LacttlM Prp^^NlMttfTOllNiIlfDIihm' Sltt **rt taplliif: ^ 0. "So* -ni .msF Uf prpcatf pr*Kt*( MaplM MMrUI: frW5A\e. CtetMCH \YfrCttSfr: n Ikniiiti CmftKj t. o. m M*t ?// ii ii nij. twi mmr rtlwi* f9X!t 'I lt?\ CdlKtlf Hliphoni: [m) 21L1SJ' CantKt: $.6 Qt^'r Ttltphont: fifi) Silw'^i CsllKtW * rnninw: ^tteamTy CO-____________________________ ^\\ 0,V-V1M,T^ DwS T15\T Clli| Cwtict:^v\^___________btmlM: U-S ^ iMl'i'lUrill, * MlapMiM MMr or rpinliitlon rtcitvlnp iwpl* < *' Ii, mrm, am MipMm n> f fptnhitio* nttuim Mfi HONS 023024 Witt of Collection: C*>1ict*r`i si--i*wo. tit own m awrcPT */i/tV Collector's Si--lo Wo. Tit Coltocter's Si--It WO. Tit WOIMMOJNI IlddlM S HOIDIIKW m lecitlon Of Si--1I0WrodutrM.t..i/ Multr_ A--r (noli1n)_ Addrtis of Si--n: fit). Rdi 111. Ak*. tuts list! Typ* of procnt producing u--led ttcrlil:_______________ QfjfdQtMtirJr ptebrre/ ir ftrm/'r GlkfLJ ftit/e AxvJ JL (fTLrm-il WP-I it mklf-j ff DP6 anj bx'fir.. / Oliooxl Sit* N--sinto Cl--Mjr t. 0. lo< MH7" Tin Hi)| Tun 1HW <*!" -Tn.i msII ->rrr Ttlcphone: (--0) 39I-VC7/ Contict : fir/jt_______ Collector's Wit: M..le. L*n.pk.'-> Telephone: pS) JM V2 It Collector'! Affl lilt ton: /)tnn.fc pntttttr Addrnt: /fo. ftp VI. filvU .Tn*i Co--iny Contict: ftfrrs Wturns Ion: 313-VS79. VJK <!ifi^iw./^n<Mi.//^i7//r^AM>i?fyi 7>t*/ Tit* Ml Mil, Mdrtts; and tutpMM mtir of orfifiliitlon racttvlnf I. ^Oyir^dfcn-* ./* Ar W -p/T-fri- Wit, oMrtss. ind telephone ou--tr'or orginlntlon receiving so--It 3. Wit, Mdriss. ind tr Ifphono nui-Orr or orginlntlon receiving stepIt few/* il^HTro /) Slgnoturt SlfAUuH fnjnt,n -----------rrrrf^ A>fT TTtTr H-to-rr TUT*" Inclusive Ortrt jLjJt-- Inclusive Mtts Inclusive Mtts HONS 023025 H0UV3011* WOISSKSOd JO wiwO Ntt If Collection: Collector'* It*l**o. If* _fi____ JSL own er CTSTBCT 'y-lO'tH MlKUr'i Sotlom. Tit ________ ____ bllicur'i hulifc ________ Tit ____ XPAlocation Of ltlll:._f.i ln*Kir ttkar (ta*llTl H*vler Olasotal Ilta ~ "' AOOren of Sat1lt: . . 4.Bay*v Tyt of kkih protein* a'*0 aUrlil: Arthts n Ho.oooM.RitOmC-uothR--"jf m. Tom CMy, Toms ..`il.tm__________ 9>L- Talophona: M. Contact: A, D G>rg ^______ Colloctor'i It * y p*t TelopNone: (___) 2ZJJLL3J Colloctor'i Affiliation: ,*a >, /~8 jj| AOOroai: />.Q. A., 7// A/.,* *X 77?" CtV CantKt: Catenated: UfH It*.' otraai. at to updam atir if iiantiatton rocatilnf tat1* *' lot'. ooorm, 0*2 tefepat wtor if orpinltatton rocamnp ut'i m. otroii, at mopRooa atr of orpanuatlon rocouir.p at' ^zlaZ IfOROtOf* ha t lac loti to Data* 3-le-t? IRC llltl <0 Mtoi J/.U-S'S inclusive Mtll SIIUU^i f-*-pr imr Inc loci* Dates HONS 023026 ate if CillKtlm: Cellettar's Staple e. flat ft W HjUULflBIg' 300* $ + Cellacter'a Staplem. T-- _____________ _______ Collecter't Sfpltde. _____________ lit _______ Lacitlao ef SfaUat: SSA-t Pradecer AfT~fj HaalarDlipetal Site Older (upltla) Mdrm ef Saapllat: .o- fo C*r S*At is Type ef precast predactap stapled aattrlal: eAt^. c*/ /fr-a/vti h opi ti i w ctuktw m io c p t iw i -------- Neattnte Ceapen* , ?. 0. Ie ** >" lain -Wly. Taut )iy ^7j TtltpHeaa: fe*) f f J - fn / ,, Contact: * . o 6/-._______ Cal latter'I daw: ? ^r.t eTaltphena: () Callactar'i Affiliation: /tant*,.-/!>; Addrttt: ^0 /?t Iff A t.-- "77^11 Ceapanjr Contact: ^i. ./i // ^>ij/litentlon: 7/ laat,~addrtsf, aril telephone auaftr of ortanliatlon focal flap Mapia- laae, iMraii, aaj taiepnoee Mar ar orpenliatloa recelvlnp staple Ian, iMriii,' ana telephone nunetr of erpenlxatlon rtcT*1p "ttnplt V2U? /iA , r Slpnatare sipnaiure tt d. a THle TfTlt' C-b laclHlia Detea 1 -3 d -*/ lnclaslre Mtas iKiusiva aatti IKintn eaU* HONS 02302? own r w a o s ta i Mt M MIkIIm: OW or OSTOPT 3-*?-0 f Collector's tttloOo. Tit Collector's Stole N. Tit Col Itctor's Stilt Oo. ______ 2L__________________________________________ Tit ______ lecetlon of SotHot: W W-f freducer >fsmarp NmltrDisposal Site ______ Other (uplaln) Address of Soap*Inf: CrroctW are _____________ Type of process produclnp stapled otter 1*1: OltAA/uic c/teJ*i c*c /*ra*r- new SHIPPtO IwrootTIOQ COUECTOO u W.mTI(W Monsanto Coapany f. 0. lot HOB 7// 'Altm Toms 17 Sit nt Telephone: (OH) rBi-Zi(/ Contect: fatcpAiL 6tzy Collector's Maoe: Smoaua Telephone: (7'3) S&l'ilj / Collector's Affiliation: fikut**r-P__________________________________ Mdress: P- ^Ox 7/1 ,4t>.W K* 7 7i J________ Coapany Contect: pAHQAtt dm*rEitenston: VS 7/_______ net, adoress. end telephone woer of orpantmlon receiving staple Hot, eooress. end telephone wooer of orpanliatlon rtctlvlnp staple J. law, . nymr or orpariuatton rtctWln$ staple /f.W,fr T Title jnlS^QJLJL-- EMfr 3 *7-IV Inclusive taut SifMtvrayj . nti* Inclusive tits fltolSo * ---'***&**' " Hili------------ -- fWJ?/ Inclusive Petes STfttlufo-----------------------------------1----- rme---------------------- Inclusive Ntes HONS 023028 C tln Q O possession