45132802 Hexazinone ECM Soil - US EPA...Assorted laboratotY g1.,;sware including: gradlla!ed...

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TJ) a +-r Ccy

[~ 2 omiddotI 6

MORSE LABORATORIES INC

Remiddotrision 2 middotDate l 096

DETERMNATION OF HEXAZIJllONE AND ITS MET ABO LITES IN SOIL

Reasonfor nrviiicn middot To rltduc le initial sample size d amount of eluting solution in Section 42 Tne chaagcs were made to provide a clemeshyewaa for instrumcnation

10 INTRODUCTION

nu standaxd aperlling proccdme (SOP) is inlinded far the det=inarian ofresid of heuzinone md hcCJZinone metabolites A (IN-T393i) B (IN-A3928) C (INshyT3935) Al (IN-G3453) I (IN-JS472) arid G3 l70 (IN-G3 l70) in soil

20 EOUIVALJiICE STA TEMTIlt]

During the conduct of this anaiysis equivalent apparatui solvents glassware or techniques (such as sample conc=tion) may be substituted for those specified in this method e~cept-where otiilt=Wise noted +ii the Ctem m equivalent piece of

( equipmcit or m equivalent tecimique is used iS use will be documerued in the smdy records when appropriate

30 MATERIALS

31 Appiritns lDd Equipment

Assorted laboratotY g1sware including gradllaed cylinders short stem glass funnels pipeS vohimetric flasks evaportting llaskS mi=liter syringes

Gas Chromatograph middot Hewlett-Packard 5890E gas chromatograph equipped with m NIP detector an HP6890 Autcisampler and an HP 3365Il ChemStation middot

GCColumn 15 M x 053 mm id fused silica column cross bonded with 05 microm film thickness Rtx-35 shy

Balancs Analytical balanc cipable of weighing to =-01 mg

Top-toadiag halane~ cipable ofweghing to plusmn001 g

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~ _

C-middotmiddotmiddot

(

~middot

~middot-- bull

Ceitrifuge

Ceitrifuge Tubes

Evaporators

Evaporator tubes

Filter Pap-

EDP Electronic Pipets witi suitable tips

Reservoirs (75 mL 25 mL or 15 mL) and adapters for use witi SPE cimidges

Solid Phase Extraction Apparatus

Solid Phase Extraction Columns

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[EC clinical cemrifuge (lnrenational Equipment Co Needham Hts MA)

50 mL polyehyleie or poiypropyleie c-itrifuge tubes Widi scew-cip closures

N-Evap Models 112 and 115 attached to a nitrogen source (Organomation Associates Souti Berlin MA)

Turbo-Yap 200 mL unit (Zymarlc Corp~ Hopkinton MA)

Zymark 200 mL tnbes (Zymarlc Corp Hopkinton MA)

Wbatman541

VortexGenie 2 VWR Scientific Bridgeport NJ)

Rainin Ridaefieri NJ

Varian Analytictl Instruments Sunnyvale CA

Vac Elut Mode SPS 24 (Varian Analytical Instrwiients Sunnyvale CA) or

Y-tsiprepnlt Solid-Phase Extraction Vacuum Manifold (Supelco Inc Bellefonte PA) middot

SupelcI=nlt Envftrade-Carb SPE Tubes Custom 12 mL Polypropylene Tubes with Teflon Frits packed with 15 grim ofENVI-CARB (Supleco Inc Bellefonte PA)

C13 Mega Bond Elut 6 cdl grun (Varian Part1225shy600 I) (Varian Inc Harbor City CA)

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middotmiddot

Shake

Test Tubes

ultrasonic Bath

pHmeer

Actcne

Dimethyldichlorosilane

Ethyl Acetaie

middot Glacial Acetic Acid

middotHexane

Metianol

Potassium Phosphate Monobasic middot

Sodium Chloride

Toluene

Water

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BurreU Wrist-action shake- (Bureil Corp Pittsburgh PA) shy

16 x 100 ramborosilie3e silylared witi Teflon~-lined scew cips

Branson Model 3200 ffitrasonic Bati (VWR Scientiiic)

Beilanan ltjgt34 pH mere- (Beckman Instruments Inc~ middot middot Fulle-ton CA)

Pesticide residue quality

SlJlcca ClalogNo 3-3009 (Supelco Inc Bellefonte PA)

Pesticide residue qualify

Reigem grade



Reagent grade

Reigent grade


HPLC grade

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AaalyticU grade avtilabie Ocro DuPont Agricultural Produc-s Global Tecbaology Division E L duPoru de N=ours and Company Wtimiagton DE

Analvte

HeQZiaone Metabolite A Metabolite B Metabolite C Metabolite Al Metabolite I Metabolite G3i70

34 Rengent Preoirition

( 34I 3rru1 Acetic Acid

Standard ldenificition

DPX-A3674 IN-TI937 IN-A3928 IN-13935 IN-03453 IN-JS472 IN-03170

Add 173 microL glacal acetic acid per one liter ofHPLC grade water Record the pH of this solution This soluticn is stable for approximaiely two weeks at room tenperarure Discard the scimion when it starts showing signs ofturbidity

342 OlMKHP005lvNaC1 Sdution

Weigh 136 g KH2PO and92 gNaCl into al litervolumetric flask Dissolve the - compounds with HPLC gltUc water Bring to volume with HPLC grade waxer and mix well Record the pH ofthismiddotsolution (-pH 4) This solution is stable for one month at room temp= Discird the solution when it staxts showing signs of turbidity

343 Extraction Solution

Combine equal volumes of 2cetone and 0IM KHPOOtrade NaCl Solution weU Prepare fresh daiiy

MLx

34 + 9 l Acetone3nuv( Acetic -1-d

lYLx 90 mL aceone with 10 iL 3mM acetic acid solution Prepare fresh daily

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345 9 Methano13mM Acetic Acid

Mix 90 mL mehanol with IO mL 3miv acetic acid solutions Prepare fresh daily

346 Mixed solvent solution (20 acetonc50 ethvl acetate30 toluene GC Diiuting Solution) middot

In a 5( mL mixing cylinder add 10 mL acetone and 25 mL ethyl acetate Dilute to volume with toluene Mix well Prepare fresh middotas needed

35 Anilvticil Standard Preparation

35 Stock Standard Solutions

12S mg(corrected for puricy)degof each analytical standard is accurately weighed quantitatively transferred to a 25 mL volumetric flask_ and brought to volume with methanol to make individual stock standard solutions having a concentration of

500 microfmL Toese stack standard solutions are tii be stored at l-8 bullc when not in use Toese solutions are stable for approximately six months when stored under these conditions

352 Fortification ISoikina) Solutions

Typically mbed standard solutions containing all seven analytes per standard solution are prepared by adding the appropnate amounts ofstandard solutions into a volumetric flask and diluting to volume with methanol Store all spiking solutions in a refrigerator when not in use

For preparation ofvarious standard concentrations see form ML 47a in AppendL I

353 Intermediate Standard Solutions

Typically int=ediate standard solutions containing all analytes are used ta prepare the GC standards Toe intermediate standard solutions and the GC standards are prepared in volumetric flasks and diluted with mfaed solvent solution (20 acetone 50 ethyl acetare30 toluene) Store these standard solutions in a refrigerator when not in use

For preparntion ofvarious standard concoltrations see form ML 472a in Appendix I

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354 GC Calibration) Standartl Solutions

Typically GC standards contlining all seven analytes are prepared Store GC standards in a refrigerator when not in use

middot For prcparirion ofvarious standard concntrlrions see farm ~iL 4721 in Anoenclix I

40 AJfALxTICAL PROCEPURE

41 Princiole

Tne analytes arc dracted from the ~ail sample with an aqueans buffer-acetone solution The mrulting ellract is evapol2Ied lo the aqueous phase and passed tbrough a disposable graphetized CJibcin SPE column The analytes arcmiddot eluted frommiddot tlie carbon column with acid-acetonesolution Tae eluate is evaporated to dryncSs and brought ta the water phase far a second column cleanup uing a C8 SPE column middot

Tae analytes n-e eluted from the colwim with acid-mehanoL Tne eluate is ( evaoorated lo dryness and the residue dissolved iii a suitable mixed solvent solution

far~ cbromitographic ailalysis using NP detection

42 Sample Ertriction

Note Use disoosable laboratory equioment whenever possible All tlassware used far the ~ysis must be metic-tlously clemed prior to use shy

l Weigh a 50 g sample into a 50 mL centrifuge tube Fortify ar this point Allow the spiking solvent to evaporate under a fume hood

2 Add 20 mL eClracting solution Manually shake ten times Shake far an additional IO minutes using a wrist-action shaker at maximum speed

3 Centrifuge for 10 minutes at approximately 2500 rpm

4 Decant the mrulting extract through a filter into a siianized Zymark tube

5 Reneat stens 422 - 424 one more time decmting the extrJc tbroutli the sa~e fite into the same collection vessel Rinse the fiiter with 2 x IO mL acetone

This is a stopping point Refrigerate exrric~ for furthe- procSsing

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6 Evaporate the combined earac ta the water phase (- 15 mL) at 50 middotc using the Turbo-Yap e~1aporiror Use a template co deemine this endpoint

7 middot Dilute thee= to-50 mL with HPLC grade ware lvfix weU

Thi3 is i stopping point Refrig=e the extract far furthe proc=ino 0

8 Just prior to cirbon SPE column ceinup sonictte the extract for 5 minutes MixwclL middot

43 Solid Phase Ertriction ISPE)Pnrificition middot

L Pack the carbon column by gently pushing the column frit onto the carbon packing Condition the column with one column volume of9 acetone 3auVf acetic acid Eute to dry and dry the column far approximately 30 seconds more with vacuum adjusting the vacuum gauge to minimize loss of small middot amounts of cariJoL Continue conditioningmiddot the column with two coltimn volumes of water without allowing the column to go to dry Discard_all eutions

( 2 Attach a resevoir to the =ttidge and pass the samole eXIract through the

middot cirtridge Use vacuum to fucilitate sample elutioL Do middotaat allow the cartndge to go to dry Discard this sample load Remove the reservoir

3 Riase the sarnple cantaine with aae column volume (10-11 mL) of water and add rinsing to the calllmL Elute ta dryness and dry for approximately 30 seconds more with v3cttunL Adjust the vacuum gauge to minimize the loss of small amounts of carbaL Diseattl this wash middot

4 Rinse the column with one column volume ofhecme Allow the hexane wash to go to dryness aod dry for -30 seconds more with vacuum middotAdjust the vacuum gauge to miniiniZe the loss of small amounS of carbon Discard the heuoe wash

5 Elute the aoalytes into a 16 x 100 mm silanized glass test tube (marked at -1 mL aod -5 mL) with 10 mL of91 acetone3auvl acetic acid Elute by gravity However vacuum may be used to start the elution

Nore middotSee Appeidix II for detailed instructions for silylaring glassware

Tbis is i stopping point Refrigerate extracS for further proc~ssing

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Evaporue the sample emac to -1 mL at 40 - 50 C using be N-Evap

Wash the sides ofthe sample test rube with-2 mL a=ne and evanorate the ettrlct to 02 to 05 mL bull

Repcit washing the sides of the test tube with a s=nci 2 mL portion of acooe

Take the ettrlct tci dryness

Dissolve the rcsidne in200 microL acerone Briefly vortex the = and sonicate for 5 minutes Again vorteC briefly

1 L Add -1 mL ofwruer and evaporate to the water phase

12 Add-4 mL HPLC water and continue the evaporation step to 1SUIC removalmiddot ofall traces ofthe acetone

13 Adjustto-5 mL with HPLC water_ (

This is a stopping point Refrigerate the bull=ct for furthe- processing

14 Vortex Sonicate for 5 minutes Vortex The bull=ct is now ready for additional SPE column clemup

This is a stopping point Refrigerate the extract for furthe- processing

44 Additional Col~rnn Cleinup with C18 SPE Cartridge

Note To ensure unifomrity ofthe column packing in the Cartridge l2Jl the cartridge on the lab bench then gently pnsh the column frit onto the column packing prior to nse

L Poss 5 mL 91 (Methanol31ll1vl Acetic Acid) to the column Elute to dryness aod dry for 30 seconds more with vacuum Continue conditioning with 2 x 5 mL HPLC water without allowing the column to go to dryness

2 Load the aqueous extract from 4314 onto the column anc eure to -l cm above the column packing middot

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3 Rinse the sampie =tube with-2 mL HPLC water andadd this rinsing to the column Elure iust to drvness Discard the sample load and wash

4 Wash the colu= with2 x 5 mL helt3Ile Elute the second 5 mL hexane wash to dryness Continue drying the column for 30 seconds more with vacullIIL Discard the heme washes

5 Elute the analytes into a 16 x 100 mm silanized glass test tube caIbrated at 20 mL with 7 mL 91 Mebanol3mM Acetic Acid A suitable reservoimay be used for this step to facilitate elution Elute by gravity However vacuum may be used to start the elution

This is i stopping point Refrigeate the extract for further processing

45 Concentrition and frocessinltgt ofSample Eluites for GC Anolvsis

Evaporate the =ple e-mact to -I mL at appro_ximatey 50 bullc using the NshyEvip shy

i 2 middot Wash the sides ofthe samnle test tube With-I mL methanol and evaoorate the

eltlractto 02 to 05 nlL - shy

3 Repeat washing middotthe sides of the tesr tube with a second I mL portion of methanol

4 Take the extract to dryness Determine the final volume ofthe extract at this point so that he concentration ofthe sample in the final extract iS 25 gmL

5 Dissolve the residue in a vollime of acetone equivalent to 20 of the final volume ofthe extract Briefly vorteC the e-mact and sonicate for 5 minutes Again vortex briefly

6 Add a volume of ethyl acetate equivalent to 50 of the final volume of the extract and ensure complete solution ofthe analytes by vigorously vortexing the miCrure

7 Adjust the final volume of the sample extract with toluene Sonicate for 5 minutes iYix thoroughly for GC analysis The final concentration of the sample in the extract is l mL = 25 g

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( 46 GC Anilvsis

SOP Mem-101 0

Note The column md conditions stlted in the method have b= sarisfueory for the matrix being analyzed- The specific column pacldngicoating carrio gas column =i=ture and flow rare listed arc typical conditions for- this anclysis_ Specific conditions used will be noted on eich chromatographic run and will not othcrwise be documclted middot

461 Oo=ting Conditions

Instrument HP5890E gas chromatograph equipped with an NiP degtector electronic pxessure controlled inlet (packedpmgcd) an HP6890 autosamplcr and an HP 3365 II ChemStation_

Column 15 M x 0-53 tiJm id- fused silica column crossbonded with 0-5 microm film thickness Rlx-35

Inlet Liner 2 mm id- liner lightly packed with fused silica wool

Injection Volume 2 microL

Carrier Gas Helium

Flow Column Makeup

5 mUmin (constant flow) 15 mUmin

Temperature Injector 290 bullc

Detector 285 C

Column Initial Rate 1

Rale2 Final

1so middotc 25 Cmin to 275 C hold 22 minutes 10 Cmin 285 C hold for LOO minute

462 Sample Analvsis

Prepare a four-point staodard curve by injecting constant volumes of combined malyte standard solutions prepared in a mi-ced solvent solution Use constant volume injections for sample CxtrJCts as wen Sampie responses net bncketed by the stondard curve require dilution and reinjection

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46J Calculations

Calculations for instnuneital analysis are conducted using a validated software application to =re a standard curve based on lin= regression These regression functions are used to calculate a best fit line (from a SC ofstandard conceitrations in microglmL versus peak= response) and to det=ine con=trations of the analyte found during sample analysis from the calculated best fit line

The equation used for the leist squares fit is

y=mx+b

where

y = peak area response

x =microifmL found for peak of~terest

( m=siope

b = y-intercept

The calculations for ppb analyte found and percent reltovey (for fortified samples) for each ofthe seven analytes are

L ppb analyte =

microgfmL analyte found x 1000 x mL solvent x mL find volume x GC diL fac g sample x ml aliqucc

where

microgmL analyte is calculated by linear regression based on pei1lt area response

1000 = conversion factor from microg to ng

g sample amount of sample analyzed

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mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

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middotso Metli-10 Page 12

voiume of extraction soiveit

volume oi sample e= taken through the proc-dure middot

volume of final excract submitted to GC

the magnitude of dilution required to bTacket the response of the sample within the standard curve responses When the sample requires no dilution the GC dilution fucor = l

2 The peccnt recovery for fortified control samples is calculated as follows

-shyoo ~overy = ppb fourti ui fortified canrrol - ppb fourti in control middot bull

ppo addd -x 100

50 REFERENCES

-Duoont Reoort No Ai1R 3883-95 (Draft) Analysis of Hexazinone and Metabolites in Soil and Groundwaternsing GClvlS receved 1122195

2 Dupont Report No AMR 2896-94

3 Morse Laboratories Inc SOP Meth-93 Revision- 4 Determinarion of Hexazinonc and its Metabolites in Water

r--middot

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Silylition of Glassware

Purnqse

Silylaiion is a proc= used to cheni~y tr= glassware in order to prcvcit or minimilte binding ofaoalyre residues to the glass surfuce

Caution DO NOT ALLOW DIMETHYLDICfilOROSILANE TO COME IN CONTACT WITH WATER CHLORINE GAS AND HYDROGEN CHLORIDE GAS WlLL BE PRODUCED

TBIS PROCEDURE MUST BE DONE UNDER A FUME HOOD THE TECHNICIAlf MUST WEAR REAVY I~TEX GLOVES

Procedure

Prepare 100 mL ofa 5 (vv) solutio~ of dimediyldicJlorosilane (DMDCS) in

h=e shy

To a glass stoppered glass container (approximately 200 mL volume) add 95 mL hexane Slowly add 5 mL DMDCS Stopper and inverr to mix

Larger volumes cm be prepared using the proportions discussed above however artenpt to prepare amounts that will be nearly totally used to avoid disposal ofexcess solution

2 Pour a small amount ofthe DMDCS solutioa into the glassware to be treUed Rotate the glassware to thoroughly coat the inside surfuces Pour exc= solution into the aexr piece ofglassware to be treated

3 Allow the tJetted glassware ta dry (approximately 20 minutes) Rinse with deOnized wacer then aceione Again allow to dry

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4 Glassware is now =dy for use

Note bull Arzy glassware thatis cemed with a brush afte- it has b= silylanized must be rcsilylanized

bull Store pure DMDCS arrcom t=peranire

bull 5 solutions ofDMDCS in ho-ane are stable for 5 days whei stored weU-stopp=d at room temp=rure

(

SOP Prepared by Frances Brookev

Kevin Clarl

rmiddot

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ANALYTICAL METHOD FOR THE DETERMINATION OF HEXAZJNONE AND

METABOLITES OF INTEREST IN SOIL AND WAT1 USING ELECTROSRAYshy

LCMSMS F W Brill Tom Gardn~r

10 SUMMARY A ~chic mchod is descnbcd for the eCtrlction pwificition lild quantitition o(bctWnonc (DPXshyA3674) md metabolites A (IN-T39ji) A-l Ctrade-A3453) B (n-A3928) C (IN-T3935) I (IN-15472) and G31i0 (IN-G31i0) in soil md W3tc-bullbull

Water samples (20 mL) wee fil~d concitrited ind purified using solid pbasc extriction eircridg=-s (Eivi-Cirb md CI3) The instrumrntoll malysis for detectionaJJd quantiotiou of the malyres was accomplished by LCMSMS Mrb m elecrnsproy intmu-e mmultiple t2Ctiozz mociroring MRJbull

Soil samples (Sg) were extractCd with OIM KHPOJ05M NaCl ~olution filtered conccncrated and purified urine solid phase extnctioa Qltridges (Envi-~ ind Cl 8) The instnimental anilysis for detection uid quuititatioa of the 3111iytes was iccomplished by LCMSMS with an cectrospray irireriace in multiple ~ction monitoring (MRf)

The limit ofquanticition (LOQ) formter was 0100 ppb for-hetlZinonc 2nd a1I 6 mct1bolitis Tue LOQ for soil was 20 ppb for hcxacinone and all 6 metabolites Test samples v-ue fortified at th tOQ 3Ild 5 t LOQ for cach analyte in both soil and water to vtliditc the cehod

To~ cortrpeted

20 INTRODUCTION Hccazinonc (DPXmiddotA36i4) is the 3cti~c ingmliot in Yelp~ habicidesmiddotre~ed for postenergence control of many annual and biennial wetds Allalyte sttu~ ciiemicl nuncs DuPont code oumbes and Chemical Absrrac registry Dumbets llC provided in Figure 1

In this method water smmles ue 2ciciified filte-cd purified md cooci~ted by SPE A combination of an ~vCarb and a C18 smiddotPE step ire used 10 mnove most mlcit ind substances that cay interie~e with the inmumcncaI analysisbull

The purified atncs were mtlyzed by ESI-ICMSMS llSing positive mode multiple re2ctioo moni1oriilg (MRf) for hewiJiooe md metabolites AAmiddotl B C 1 and G3li0 Qwntitltion wis based on the integtltion o(a single MRf trinsition response This anilysis quintictivdy detects heuzinooe and all 6 metlbolites the IOQ for e2ch determined 10 be 01 ppb ia w11er ind 20 ppb in soil

To ~ a1mpleted

30 MATERIALS Equivalent equipment and mueriah miy be substituted unless otherwise specified (see seition 53) note my spctificuions in the following descriptions before mUing substitutions The equivilencysuiubiliry of any substitution should be verified with 2ccepoble eoottol md iortifieltion recovery daa The nuteiils ue listed in order of first 1ppcu1I1e in the method

LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

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Matier AE 163 amlytictl bilincc r-1et1ir Insttumettt Corp Hightstown NJ) Ppctsipipcors and tips suiuble for p~cion of stlndJJlis acd sunpc fortifictions Assorted 11iili bcke-s ind volumc6c yiin~

Sartlc rn-lcrion Mettler P~460 top-loiding mtlyticLI bilmc (Menier InstruJCenc Corp)

250-mL higD density polypropylene cecrifuge rubcs (N3lgec)

RoapidVapraquo Evaporition System (Llbconco Corp Kms3S City Mo)

T~homog~Model FID-1810 (Tckmar Company Cin~noati Ohio)

0-15-lm ffitcr Unjt P_l I5()(l045 (Nalge Cocnp10y Rochester NY)

Somill RCC ccltritUgc with SS34 rolor (DuPont Company Sorvatrt Produc~ Wtlmingtou DcL) or IEC HN-Sil ccurifuge (DamocIEC Division Needham Mau) Buchner Fmmd Filter Papc- Wbamwi S Clt No 1005 070) to fit Buchner Funnel

Samifc urifiC3tion C18 Mega Bond Elu~ 20cdlg PN llli-6001 (Varian Hubor City CA)

Supekem11 Eivi-Drii SPE column 60mLJL5g CUSTOM (Supeco Inc Bellefonte P~)

15-mL op rr=ervoir empcy PN 1213-1010 (Variau) Luer s~oclc-l 1213-1005 (Vorim) Bomi EIur wptm PN 1213-1005 (Vgtrim)

N-Enp Amlytical Evaporator Model IJ1 (Beton Dickinson amp Co Franklin Ukcs NJ)

2-microm 13-mm Aero Disc 130 PTFE syringe filtcr P N 4412 (Gelman Sciences Ana Arbor Mich) bull shy

45-jlID 25-mmAcroOisc 13CRPTFE syringcttlter PN-419 (Gelroan Scicic= Ann Aibor Mich)

Vacmmimmifold PJC S-i030 (Supcko Inc Bellefonte Pi

bull 3200R-J Brmsonic11 UltrLYinic Clcmcr (Brwonic Ultrasonics Corp Dailbury Conn) LC~S Analvsis T=e foilowing HPLCJMS systen was used for this method including equipmcit necessary to diven the flow going into the mass sp~mcgta to wistc and ofpost-column splittiDg oi the HPLC flow

Miao-Mass Quartro Il criple sector quadrupole instrumeit with AP SOtm=tintcrfJc collfigured for ESI opmtion

bull Masslynx dm Jequisition so~ rwming under Windows NT Wates Model 1100 HPLC system including pump module iutosampler dcg3Sing module cohmm comparcmint module (Watm Corp Milford Mow)

bull ElCCtricilly-actuated high-pmsure 6-port switchlng valve with 1116 in fittings EC6W used for eflluctlt diversion from MS (4-port nlve would be Jdcquate flECiW) (Valeo lnstrumcni C1 Inc Houston TX) High-~minless steel J16 in fitting tce llZTlfor we in post-column flow splitting Split r1tio adjusted by tltering ~ccion on waste-side ofte by ttltering length ofopilluy OJbing (Valeo lmttumcnt Co Inc) Zorbubull 46 mm id)( 250 mmRx-CS S-microm particle size PN 88096i-901 (MAC-~IOD Antlytical Inc Chadds Ford Pi) Substitute columns may ivc sub-optimal pufonmnce

Reag1uus and StllltdardJ

~ OmniSolv gbss distilled lc1onc betlDc mcblnol

DRAFT 4

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Baker Anal)-cd Rcigeu pocssium phosphate dfoasic cryml p_ 1252-01 CHPO (1T Bake Pbillipsbtttg SJ)

Baleer Aillyze~ Rcigilt soriium chloride c-r~ul P~ 3252-01 K-Cl (JT 3ake- Phillipsburg NJ)

bull GR glad~J aeerie acid (EM Scicic)

bull All wuer-ns Milli-Q distilJed deionized water ()ofilliporc Cori E--1-ford ~iss) Sunduds All sandirds wee synthesized by DuPont Agriculturu Prociucs Wilrninrc Del S~dirds should be greitcr than 95~~ purity

DPX-A3674213 (hexazinoac

INmiddotD937-3 (mctlbolitc A)

bull INQ345J-2 (metiboUrc A-1)

IllmiddotA392S-i (metibolitc B)

bull IN-13935-3 (metlbolitc q bull IN JS4n2 (metabolite 1) bull IN G3I7~2 (mealxilite G3i0)

JJ Safety and Heallh

No un~y~~~Is arc used in this method AU appropriite matcill Uey di~ shces should be red ald followed md proper peronal pnicCCrivc cquipminc should be Uled

40 METHODS

41 PrincipUs ofAnalytiW lfaltad

4 I Samofe Extraction

The OlM KH~005M NaO soil extrlctioo solutiaa yicl~d high recoveries and has~ demonstrated u m effeetive extr3Ctiou agent for bexuinooc ind its mecbolites Witer is not ext-11middotd it is direly filtered concentrated and purified on the SPE colwnm

t Urract PJrificarian

Clrboo phase~) md Reverse phase (ClS) Bond Eiucll SPE procdlUes in Sed to provide ettensive cxttact purificitioo The water md the soil atricts ire passed onto aad ribcd on Envi-Carb eolumos The column is thei washed with water aod bcxioe to remove most of the macit material Elution is with an acetone-3 mM 3crie icid (9010 vv) solution The acooe in theeluate is -=ovid md the sample is brought up in water md loaded onto 1 C18 column The ClS is then washed with w1ter md heune following wbid1 it is cutcd with medwioL The sample is blown dowtl to ~ through 1 series of procedure$middot designed to minimize Jou of uWytc on the container walls ind is brou~t up to a final volume in water for a final iiJcration acd LCMS malysis

4 I 3 lOMS Anavs-is

The method utilizcs cleetrospriy ioni3tion (ESO md is oper1ted in positive ion mode wing Multiple Reaction Monitoring (MR) on the ~icromus insaumentuion (or all o(thc malytcs A single trmsitioo ~monitored for C3eh llWyte (MH+l JCngmcnting to the IJl-eyclohexane moiecyj Selection of these cransitions was based upon the nws spcctr1 generttcd durittg the method devclopmet rocss with the instrument in scinniog mode The ~cen gCllcrited by ESI-LOMS for the milytcs ~--shown in Figure ~ The Oue ion ~Hr for eii JlLllyte ~ s~lec~d for qUladcufoa The sezicivities ofeici inafyce vWed the GJ l 10 showing the leut sesiriviry in the positive ESI SRf mode the he-~one showing the most

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Duoot Rrort ia 1292

J~ Analyriclll Procirdurir

J Glassware -rid poundauiornfrr Ctaning P-Jcerpound1re1

Dispostblc Wiware ire used whcieve Ossible ill this meod Reisable labwirc whieb includes the evaporation vesscJs md volwletrics for stmdmi soluriocs ire deincd by washiIig with a labornary gride derrgct followed by t1p water rinses (3) and distilled v11w inses (3) A fin31 iceone rime rnay be used to rcnove the residual W3te- md promon drying Coic it~ oiglassware must be tre11ed silanicd 10 preveir 3b3orptioo of ~ies ooto hc gWS

J Prmtlration and Stobilirv ofReagmt Solurfons

0IM KttPOJOSM ~foC Solurion Acd 1J6g KHPO wi 291g NaCl into a 1 liur voiumcric flasic Dissolve ibe Compounds with HPLC or MillimiddotQ wittt Brig to volume ind mix well Record the pH of the solution (should be -t) Tais solution is stable for I momn discmf eirlicr if it show signs ofUrbidity or bactcia growth Scie volume as necssary

3 mf Aeerie Acid Add 1 i3 microL of glWal acetic acid pc 1 L of fllgtLC or MillimiddotQ water Tne solution is stable for l month Dis~ e3tlier if it shows signs of turbiciity or bacteria growth

110 diluted Glacial Acric Acid Prepm 1 110 dilution ofgl3cUJ 3ctic acid by placing 9 rnL of HPLC or Milli-Q water into a IS ml pbstic CC1trifugc tube or ary other suicable conuinerwith a cap Adrl 1 mL of glacial acetic acid mi~ circUUy Clp w~cu noc in use

Ett3etion solution for Soll is prepared by combining icone ind the 0IM KHPOJOSMNaCl Solution in a 9010 vlvtatio This solution is prparcd dUl~ as netd-d however will be ~ble for 1 tnonth middot

9010 Acetone-3mM Ace~c Acid Solution Mix 90 mLofutone with lOinL of3 mM Acetic Acid solntiaa This solution is used for SPE column conditionbg md elution S~e volume as needed stible for l month

9010 Methanol3mM Acetic Acid Solution Mix 90 mL ofncWnol with 10 mL of3 ml Acetic Acld solution This solution is wed for SP column conditionittg ind eiution Sc3lc volume as needed sable for l month

HPtC Aoucoll Mobile Piase A OOlM ictic acid solution for we as mobile phase is prepared by filling a I L volumetric flask with distilled d=ionizcd water addpoundng 600 microL ofcot1ccutrated acetic acid gently agititing the iUxture and diluting to volame in distilled ddonizcd witer This solution should be prepared is needed or scone if turbidity or baccial grolilth is observed

J23 Stock Soluriora Prrnarario11

IfpOUlble stuidlrdJ with t puriry gtdter th3ll 9S ~ tD be wed Individual l 002-microgml ~ stindards ~olutions for heUZinooe md the 6 listed mettboli~ were preparM by weighing 501 mg oi =ch stlOcbtcl in a sepuite ~d SO-mL volumetric flask md diluting Itgt volume iD acetone Sample weighrs were detcnnincd to 3 signifie3UC figures The malyricil ~Imcemuse provide a weight precision to 3 significinc figures or he 3mount ind volume bas to be idjusted to meet this criteria For eumple inctC3Se the unount 10 10002 mg ind use a 100-mL volumettic flislc Cleirly bbel cach stock solution with dite prepued mklyte ind coocilrltion Stock soiutions are stored uoder rcfiigeratioo (42 degq ind must be replaced 3t cist cvery 120 dlys or when approximitely hill-volume Kc= stock solutions stoppacl 10 nmict solve=c evaporation

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DuiCllc R9ort No 2292

44 Intermediate Standard and Forrificirion Soiurion ~~ararion

WaterSoil lnterediue Starnbrd An ln~t O microgimL nitd scndJrd soiutioo ~ lde from the 7 iodivicillll 100 microymL stock soiurions P3c 03 ci of elciJ oftle 7 indivi~l 100 microg~ srod solutions into a SO mL voume=-c flask using a pipe~ Pbc C volumcric oato the N-Evap and 3JS llitrogen through the 1all 10 blow off lll of the xonc c=ove immcdiuely Add HPLC or Milli-Q water md fill to the SO rnL line Vonet sonicte for S itlln

Wate Fortiticrion and Standird Solution A SO n~inl Vi2ter fortifiction and standard solution is prepared from the milted t~microydegmL Intcmcdiatc Stmdard Rcllove the Intemidia~ S12alhtd from the refrigeritor ind allow it to retch room teJlCr3~ TJlCI sb1ke by lund to insure san6rd cotisistCllC) before naking dilutions Pllce 2j mL of the 10 microgill intrnnediate stock solution into a 50 mt volumeric fluk Fill up co the line with WUC md =ix Libcl the solution with the d3te rreparcd malytes and conclct1tion Store the solution in the rcfrigrtor It is sable for 90 days

Soil ForrifioriCn and Stmdmi Solution A 200 n~ water fortificuion and miubrd solutio~ is prepared from the mlxerl tOmicroglmL Intmnediar Standanl Rcmrvc the Intemcdiue Standard frnm the refrigirtor and allow it to reieh room tcmpenrurc Tho slukc by bmd to insure stuldud consistccy before making dilutions Place 100 mL of the I0 microglmL ~ $toCk solution into a 50 mL volmnetric flask Fill up to the line with water and mix Ubel the solution with the date PfGllred amlytCS 20d conc~tration Store the sulution n the refrigciitor Ir is St3blc for 90 diys

middotf15 LC Calibration Standard Sol11no11 S~t fttpcratio11

Water The olibnticn stmdud set is made from the O ogiml Watci FoniiiC3tion and Stlcdard solution Recovc the Wi~ Forrificcfon md Stuubrd soluCcn from the rcjigeltor lCd illow tt o reach room teoperarur Then shikc by bmd to immc mcd2ni consistency before makihg dilmions Reier to the able below Place the specfied aliquot of the 500 pgmt WucrFortiiiction ind Stmdard solution into a 10 mL volumetric flask Fill to the line with HPLC or WW~bull wate Ube as calibrarioa sruidard solutions with dace prepared analyte$ md concitntion Storr these solutions in the refrigcritor They are stable for 90days

Iceitiiier Aicuot of 50 nefmL Sd(uL) F~al Vol Stindud Cooc~trlrion fnfrnL) WSI 1000 OmL IO WS2 1000 IOmL 50 WSJ 400 IOmL 20 WSbull 134 OmL 06i

Clearlt label the clhDruion solutions with he dlte ~ malytcs aad concitrition Autosamplermiddot vials should be filled to ipproximuely 113 cspaciry mi crppcd to minimizc solvent ~viporation The 10 ml volumetric flasks of stmdirds Will be stable for weeks Use (resh illquots from thcn for e01cb analysis set

SQit The clhbration scadard set is made from the 00 ngmL Soil Fortifiation and Scaadard solution Remove the Soil Fortific01tion and Stmdard solution rom the rcfrigeruor md allow it to rcacb room temperature Then shake by bmd to insure stmd3rd cinsistcncy before imlciog dilutions Refer to the uble below Pbce the specified lliquot of the 2000 pgmL Soil Fortifieltioo and Stmdard soiution into a IO mL volwne~c flask Fill to the line with HPLC or ~Q viter Label is cWbration standard solutions with dire pteatcd milytes lDd concotrition Scorc th~ solutions in the refiigeralor They ire Stlblc for 90cbys

Idcltificr Aiouot of00 nimL Stdfut) F~al Vol Stindird Concetlrion (nmL) SS 2500 OmL 500

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CuPon Reorr ~a 192

SS2 120 Om ZSO SSJ 500 Om 100 SS-l 16i 10 =L middot3

Clearly label the C3lfonrion solutions with the d3te p~ued imlyts 3Jld ccncintion Autcsamo~ vWs should be filled to appioximately 213 cIpaeliy md ~ed 10 minimiz soivec cvipor3rioo The JO mL volumcric flasks o(stmdirds will be sable (or 2 lCe~ Use fresh iliquots from then for eui

anal~is set

4__ 5 SourtI and Ciu1raqqiJdorr afSamulc

4 Storage arid Pt11roctging ofSamola

41

WatC All W1ter test samples arc fortified with bcnrinone md the 6 listcd mcuboli1cs froai the 50 Ilgml Watei ForiEcation and Stmdald ~lutions The tpprcpriuc- orrificstioo volunc is drawn into a pipetlpipettor and pbcd into 10 ml of Water The water is then tllixed Refer o the tlblc below fer the volumes ofVater_ Fortifiotion 3lld Stutdard solution to use for miking the LCQ ind 5 x LOO fonificitioos

sectQlli 4ll sOil test samples ue fortified with hcmiDonc middotuul the 6 lised met1bolites from-the 200 ngrtL Soil FortiDQtion ~ Stmdard solutions The ipproprUtc fcrtiiiiiPon voh1mc is drlbulln into a pipelpipcttor and p~into 5g ofsoil The soil is allowed tD nmd for 10 nlinntes Ref a tQ the t1ble below for rhe volums ofSoil ZortiBctdoa md Stactdmf solution co USe fer mtling the LOQ and Sx LOQ fortiiicitiocs

Amount to Vofrme Fortificition Soln Volume ForrifiCJriOD Soln Leyels ill anilvtes LOO

fQnin1 Low Fortificirio11 ClOOl Hiob Forrificirion (LOO ands x LOO Water 20mL 40 microL 200 microL 01 ppb 05 ppb Soil lg so 250 20 ppb 10 ppb

Concvitration and Prrification Procedu~ for Water

Soiutioa Requjmnc11~Samplc (exiraaioa + purificatioa) Milli Q waccr 50 mL mctlwiol 10 mL hcone 10 mL 9010 acetoa~ J mM Acetic Acid 10 mL 90 10 mcthtnolJmM Acetic Acid 10 mL

SAMPLE CONCENTRATION AgtID PURIFICATION

l Remove simples from refrigeruor or frcaer uid illow to wmn to room tcnpcrirure 2 -reisue 20 mL of the wrtcr smiplc 10d plice it inro a 250 rnL ciaifuge bottle 3 Fortify tczt s~la if required 4 Add SO mL of)4illimiddotQ ~let md thet1 jcfdify by jdding 200 microL oithe 1110 diiutcd

gLu~I ictic icid solution ~p md briefly vont nit

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Duocc Rron gtIo 2292

I PJic the 15 EYiCarb Beed Eluts~ iico the vaCium mmiiold ind condition them by pbcng 10 mL of9010 icconc-3 mM lCtic icid soiurion into the tubes and adjwting the flow to a fiJsl drip (-IO mLminute) Using l geitlc vacuum to pull through all of the liquid let tbc columi dry for 30 seconds after the alt of the liquld lw exited Load and condition the coiumn with two 10 mL volumes of oviccr Do not et the liquid level drop below the top of tilt sorbent Wt the second witer load has passed hrougb Do not aUow the tube to dry

2 ampQ the watC simple oncO the column in seveTJl pcrtiom ifni--ssary due to column rcscrvoir iipacy Tum on the V3cuum and 3llow Cc sample D pass through the column u a slow drip Do 110t allow the column to go dry Do not collce the liquid

3 Plice S mL of _~nt inlo the empty 50 mL ciaifuge rube vona Pacc this rinse onto the Bond Elut and 2llow to pus through Jt a Slow drip Pull aD the water through allow to dry passing air through for abont 30 seconds 3fta last drop has come oft

4 Place S mL ofbaanc into the Bond Elut md allow to pass through at a slow drip Allow co dry passmg 3ir throuJh for about 30 seconds after bst drop has come off

5 Open the vacuum manifold md plae plastic 15 cl Cilttiuge rubes into the manifold in order to coDect Cc elua~ middot

6 Place 10 mL of9010 ~ctond mM 3tricaCd solution into the Bond Eut tllbe wd alloW to pass dJr)11gh at a slow drip Pull all of the liquid through into the collection tubes BrcU the vxmm middotmd remove the tubes coacainiDg the cuatc

7 Pbcc sample on an NmiddotEvap and ev2p0ra1e to approximately l mL at 4()50 deg 8 Wash the sides of the sample test tube with approxiJmnly 2 mal of ictone md

eV3poran the anato 02 to 05 mL ~t this wuhing with a ~d 2 mL volumc bf3Cetonc EV3p013tc the sample to dryncss bull ~middotmiddot

9 Add 200 IL ofacone to the tube vortex mdmiddot1onictc f~r S minutes Vona 3gain Add approximalely l mL owatcr md ~tc to the walctphase Add approximately 4 mL ofBPLC watc md continue the evaporation sty ID cmurc removal of all traces of 3CCtone nis is 2 Ytry critlciJ Sfep the prtience O( 211) tlaquot0ne will prevent the polar analytes Crom belng reuined ao the CIS column in btcr steps)

10 Adjust to approxin=tcly 5mL with HPLC witcr Vortex soniatc for 5 minutes vortex

11 Proce=d direcly to he Cl8 SPE cl~middotup This is J napping point Sanpcs C1U be pbcd into the nfrigcritor for storage for up to I wck

CS BOND ElUT CLEltIUPFJNAL PREPARATION l Plice theClS Bond Elu~ tubes onto the ncuum mmifnld and condition them by

placing 5mL ofmcbmolJmM Acetic Acid (9010 vv) solution into =ch tube and adjusting the Oow to a fast drip Driin the mbe md lllow to dry for 30 seconds more under vuuum In the same mimer cODdition next with 10 mL of ~tcr in two 5 mL incremems wUting until the first 5 mL is completely below the frit before adding tbe second 5 mL Stop the flow when the level of the water drops slightly below the top of the sorbrot mthe boaom tube Do nor let the tubes dry

2 Pl3Ce the En-i-Cub cluue solution (step 11 ENVl-CARB cC111up above) into the Cl s Bond ElurZ tube APIY vacuum open tbc stopcock ll1d load the cluite onto the column with a vcrv ~low dritt Step when the level of the liquid is 1 cm ahove the top of the sorbcnt Discud the 3qUCOW ctDucnt

3 Biclcrinsc the origiil Envi-C1rb elmlc contiincr by pliciDg 20 mL orw11er into it vonct miOg for J w seconds Pour this rinsatc in10 the ClS cutridgc Allow this (riruc)witc-~to pw through the ClS and discud Allow ill of the bullvucr to be driU ou1 of the mCc Immcdii1cly shut off vicuwn discird lo3d volume

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DuPoor R~orr -lto 2292

i Pl3c 50 all oiicunc into the CtS Qrttidgc Allow the hcunc o pw through ll i roode-itc driptier the bcunc w completely pused tltrough he column ldd ~othc 50 mL ofh~c lDd 3ilow tbt Q complccy pus through ilic coiumo as ~cu Allow the vaclutn 10 rull air thrcusb- the crnidgc witil thae is no more dripping

5 Brelt vactmm lnd place a new tS mL plastic curifugc tube iito the vacuum manifold under the Ct S ubes 10 collect the Juate

6 Pbcc 10 mL ofctbanolJ m Acetic Acid (9010 vv) soiurion into the colwm Allow the cluuc to pass through at a moderate drip 3lld coUct Diliud tbe Cl 8 oolumn

i Whci elution is Onishcd pbcc the tube containiDg the extract onto the N-Evat1 ind blow ii doMJ o approximately 1 mL middot

8 Wash the sides o(thc tube with ipproximatcly 1 ml mcthmol 3nd blow down 1o approximuey 02 t 05 mL R~t with uiotlut 1mL ~a llld blow down co dryness Immediately stop the nitrogt111low uid remove the tube from the N-Evap

9 Add~ 1aml o(HPLC or Milli-Q waeer to cbctube containing the evapol3tcd C18 eluate Verex mix for S seconds and place into the ultnsanic bub Allow the sample to rcmJit in tbe bath (set at 30 to 45 degres) for S to to minutes

10 Filler apptoxllnatily tO mL of lhis final volume solution through a 01 micron ActoDisc filtc inlO in appropriate autQsamplcr vial Cap

11 This sample is now rcidy for LCMSMS malysis It em be stored for up to 3 weeks iD a rcfrigaUor 214 bullc

429b Conc~rration iind Purification Pr-oceduTc for Soil

Solution ~qufrmiddotcotsSample (cxnction + puriOctionJ ~tilli- Q lvltr 50 ml Eitriction solution 20 mL tnethtnol 10 mL bexmc 10 mL 90 l 0 acetone 3 rni Acetic Acld 10 mL 9010mcthanol3mMAccticAC-d 10 mL

SA[pLE COSCENTRATION A41) PURIFJCTION

SAMPLE PREPA~TION AND E-ltIRACTION

1 Remove umpics tram rcfiigcntor or frcect ind allow to wirn to room tcnperirurc 1 Weigh ouc a 5 g gmplc o(thc soil and place ic inro a 50 mL c=iMgc bottle 3 Fortify samples ifmiuircd 4 Add 20 mL o(OJ~( KH~005MNa0 cctractionsofutioo Manually shake 10 times

Placc onto a wtst-action shaker uid shake for 10 aiinutes at maximum speed 5 Centrifuge tbe simplc for 10 minulC3 at approximately 2500 rpm 6 Attlcb a 20 mL syringe to a OAS microm Acrodisc filttr Decmt the supemucnt into the 2

syringe Filler into a 50 mL cottifugc tube Place tube ilmncdiately onto lD N-Evap 31 40 to SO bullc md begin cvaporition

7 Rcpcit steps i through S When there is sufficient room in he O mL centrifuge rube (on the N-Evgtp) filter the secocd supernucnt into it Rinse syringe with 2 x IO mL volumes of icone ~d place ice1one into the 50 ml centrifuge tube conuining the filaire

8 Evaporate the cmbined ettracrirue to the watc-piuse (3pproximatdy 5 mL) 9 Adcf HPLC Vll-unriI tbc volume is approxinutey 50 ml I0 Jusl prior ti iroceding to the SPE cC30up sonicie ttrlct for 5 min and vortct mii

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DuPorI R~orr So 2291

I Place the l5 g Eivi-U-i Bond Eluts- into the YlCUum manifold acd cocdition them by placing 10cIof9010 acetooe3 mM uric acid solution into the tubes md adjusting the flow to 1 fast drip (-10 mlminute Using 1 geitle VacIUm to pull through all of the liquid let Ce colwnn dry for 30 seconds aftt the last of the liquid has ~ted Load md condition the column with two 10 mL oiumcs of water Do not let the liquid level drop beow the top oftbe sorbent after the sctood wttcr load has passed through Do not allow the rube io dry

2 Load the soil eurict onto the column in Stl-eiI portiocs ifnecsury due to column r=ervoir =P3Cit) Tum on the bullr11uum and allow the sample to pass tlrough the column at i slow drip Do not allow the column to go dry Do not eollct the liquid

3 Place S mL ofwata inco tb~ empcy 50 m c~gc rube vortex Pace cltis rinse onto the Bond Eutmd allow to pass through at a slow_drip Pull all the W11C through allow to dly passing air through for about 30 secoods after last drop has come Ocr

4 Ptlee Sall ofhcxme into tile Bond But md allow to pus through u a slow drishyAllow to dry pauing iir through for about 30 setoods after last drop bas come off

5 Qom the YlCrum manifold and pbce pbstic lS mL centrifuge tubes into he manifold m order tO collect the eluate

10 Place 10 mL of9010 acctoccJ mM actic acid solution into the Bond Elut tube ind illow to p3SS thfoujh at a slow drip Pull all oftbe liquid through intothc iollectioo tubes Break the vacunm md mnove the tubes containing the ehate

11 Plac smple on ID NmiddotEwp md ~~to 3pproxilmtely I ml at ~50 deg 12 Wash the sides oftbc sounple ~ fllbc wilh approxim3tely 2 lXlal ofacoae ind

e--rporate the etnct to 02 to OS mL R~ot this washingwith a seotid 2 mL volwne of icctooe Evaporate the sample to dryness middotbull shy

13 Add 200 microL of actooc to the tube vorta and sooiClf for S minutes vanex again Add 3pproximitey 1 mL of water md evaporate to the water phase Add approximitely 4 mL of HPLC waler md continue the evaporation step to cDsurc removal of all traces of actooc This is 2 very critial step the presence of 2ny acetone will prevent the poltr in2lytes from being reuiocd oo the CIS column io later steps)

10 Adjwt to approximitcly 5 mL with HPLC wwr Vortet sooicte for 5 minutes vonet

I Proceed dirtJy to the ClS SPE clt=middotup This is a stopping poiDt Sunpe cm be placd into the refrigcritor for storage for op to 1 week

Cl8 BOND ELUT CLEANVPmNAL PREPARATION 1 Pbcc the CIS Bond Elurlgt tubes onto the vuuwn mmifold and condition them by

pbciDg 5 mL of metlwiolJmM Acetic Acid (9010 vv) solution into C3Ch tube md adjusting the flow to a fast drip Drain the tube and illoW to dry for 30 seconds more under vacuum Io the same manner coodition next with IO mL ofwate in two 5 mL Uicoemena waiting Utltil the first 5 mL is completely below the frit before adding the se-ond 5 mL Stop the low when the level of the water drops slightly below the top of the sorbent in tbe bottom tube Do not let the rube dry

2 Plac the Eivi-C3lb eluate solution (step 11 ENVJCARB clcanup above into the ClS Bond Elut1 rube Apply VlCJUm open the stopcock ind loid the chute onto the column with a verv slow drio Stop when the level of tht liquid is 1 cm above the top of the sorbenl Disclrd the iqueous effluent

j Sickriose the original EJvi-Cub euate cocuinc by placing 20 mL of water ioo it vonet rni-cig for i few seconds Pour this rinsue into the CI 8 cutridge Allow this

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DuPont R=ort No 2292

(rinse)wuc 7ash to pass thrcu~ chc CIS md disud Allow 311 of the water to be drrWll out of the ube lmlIebciy shut 011 vaCJUIl discird 1011d vulurne

i Plc o mL ofbe-~e into ClS cirridge Allow the beonc ~o pass throu~ lt J

mod~ drip Afterthe beuu has complerely passed through the column lcid anether SO mL ohtunc wd illow hJt to compkrely pw Uirough We column as wclL Allow the vacmID to pull lir through ll cutridge until thee is no men dripping

5 Breik vaCutlIl ind place 3 IlCi LS mL pllstic centrifuge rube illto the vacuum nanifold under the CtS cubes to collec e eluitc

6 Plac IO tnL ofmetlunol3 ml Acetic Acid (9010 vv) soiuticn into the column Allow the eluitc to p3$S through at i modmte drip and collcet Discrd the C18 coiwm

10 Vhei elution is finished pltc he tube coritUning the extrlct onto the N~Evip and blow it down co approximately I mL

11 Wash the sides of the rube with ipproximaiely l mL medunol and blow doWD to approximalcly 02 t 05 mL RlcI With mother J mL wuh aad blow down to drycess lmmcdi2tey stop the nicrogei flow md remove the tube from the N-Evap

12 Add~ 20 mL ofHPLC or ~-Q water to the tube containing the ivaporated Cl8 chute Vortex mit for S stt0cds and place into rhe ultrasonk liath Allow the sample to mniin in the bath (set at 30 to is degrees) for 5 to 10 minutes

10 Filter t=PfOxllmtely 10 mL of this final volume solution throuzb a 02 micron AcroDisc filter into an appropiUte iutosimpler vW Ctp

11 This sample i~ now r=dy for LCMSIMS anUysis It an be stored for up to 3 weeks in a rcfrigeritor it 4 bullc

fJ InruumeruariJJn

JJ I DecriDrion

This method requires an LCIMS1-S insttumelt equipped with an electOspray interface for the IWysis of water and soil An autosmplcr is also required fer the unatteided analysis of multiple samples and cilibruion s0Iutions The malyticl d3t1 in this IIrbod wu obtained from i Micromass Quattro Il LCMS equipped Nith the HP Sci~ 1100 gt-fociular HPLC Systcn which includes i dual channel PWIp autosunpier vacuum degasser tempearure-ccctreiled cOlunm ccmpllttnot and 3 UV-Vis deteccr (not required fer thi3 method) The HPLC md Mass Sferometer operatirlg paruneers for theie systcns arc given in scetion 432 The chtoIIJatographic column and mobil phases SCcified provide good pcik shapes and resolution of the anllytes This- illows tttffii-=zl iinle w switcz nuJ specroaicric 1cquisitioa paruica thereby allowing bettr optimizicion ofcaclgt ch3zmeL The HPLC solvct program includ~ a period of high-organic solvent flow to purge mitrix mateais from the column mi allows suffiCent re--equiliDration time between runs Do not 4ltcr these periods In generu instrument respOnsc is good to eiceUent for the mat)tcS on the positive EsI SRf cbanncs Always use the combirlrion of HPLC conditions and mass spectrometer panmctes specified for cicb lll3trit

JJ1 Oa~raring Conrfirions ficromass Ouam-o fl with HP sm~s f 100 HPlC

A~ALTilCU CONDITTONS FOR SOIL AiO WAIa

High Perarmanc~ Liquid Ciiromarography (HPLC) ~labile PhJse A Aqueous 001 ~I Jctic icid

~fobie Phise 3 At~tonittii

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Mobile~ Prosnm

On-eohmm Flow Rite lnjeciOD Volume Column

uass Sp~craMeta (MS) lonizition Mode

HVIcm Capillary Voltage Cone Voltage COllisicm Voltigc

GenmJ pumism CollisUm GuPr= MSl lJdlBM ~olution MS2 UllBM Resolution Some T cnpmllre

AcauisitiOt functions

ESP+ Sbrt 7Carin End 95 Int Chan Dea~ 00 sec

2 ESP+ Stirt 9Smin End 120 lnJ Cim Ocby 002 $Ce

3 ESP+ Stan l20min End 170

Int C1Wl Dcby 002 see

DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100

10 mLIItin spiit sr Diven 0-69 155-30 min 50 microL Zorbax RXO 25 c1 )C 46 mm id 5 microm ~th guard column ateched 30degC

Positive Esr 026V 40KV 32 Volts 18

Pooririv_ESt Mode 17-20xlOc-3 both JO both 12 SS degC

Set is shown below

Pawit Dauehrer Dwell IiiI 711 012 see

Pire~t Diu2hter Dwell 2553 1571 012 sec 26i1 1710 012 269J l ilO 012

Pireit Q3u2hter Dwell 2391 1570 008 25- 171l 008_

Approximite Rttcntioo Tim o( the 1 Anilytes

Anilvte Atgtorot Rctcnrion Time (min Accuisirion FuncrionTrinsirion metibolitcG3170 8S9 I litI -710

mc=iboli1c bull 1063 2 2693-lilO mctibolitc Amiddot I 1162 2 2693-lilO

DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547

DuPont Rcon gtlo ~92

ceiOolice I 1117 2 2672middot170 meaColi1c C 102 2 25S1-1570 heuzinoce 14 J6 2532- l il0

mcibolite B 1362 3 2392middot1570

Alurnate JIass Splaquorromdn (MS Conditions Confirmarion Channeamp

lfco-eluting matrix componca ioterfrn with Jtt) of the malytcs on bri pfUwry positive cearospriy MSMS chmaes 11SC the folowirg e1wrosprry ccnditioos md Ueate chumes ro both cotuinn Wt these co-eluting peiks ~ fn bet intcri~cs md to qumtiote the uiaiyts Alterntc channes C3D be detemiDcd from ccunining the full SclD spectra Of the diughtcr ioQ Sp~ Of ~CJi imiyte sboNtl in Figure 2 The 3l1cmate eleerospriy pannwm (ince3sed collision gas energy) speJied will iJso signitiC3Dtly reduce or climimte che intmering peiks on the origiml dunnels Re maJyu S3tllplei using the 3lcmate channels along with the origixuls for comparison

Iouizition Mode Pcririmiddotc ESI HY= 01 i Cipillary Volbge 36KV CC1nc Voltage 25 Volts Collision Voltage 30

Gcnerai~ Positive ESI Collision Gas Pssttrc 17-2()xl0emiddot3 MSl Lwmf Rcsolution botl18 ~[S2 LiHM Rsoiutioo both 12 ampiurcc Tempc13t1IIC 85 middotc

Acauisition FtIDcioas set for selected alternate MR~ trmsitions

433 Cilibrition ProceOttes lnstrumcitiiion per~ ll2S britially eilt11U3tcd for eaJbrltlon ruponse linciriry by the following procedures

1 Tue LCMSl~iS insrrumcit WlS ruiied in positive clerospriy mode to optimize the (lshycyclobcune moiecyr pclk while still showing the bise peak (MH]bull For the oegative electtospray compounds the instrument was tuned to maximizc th (M-1 r peik

2 Full-scm ou-ltolumn malysis o a 4-microgfmL cahOruiou solution containing eich of the analytd ltl3S pdormed to verify appropriate mz responses and ahundanc ratios

3 Analysis of cWOration solutions (see section 41S for prcpiration) and co~ctioo ofa 5-point clfbrarioo curve wu pcrformed to verify linority (R1 098) ov~ the analyticll t20gc md ~u1tc detector response (low cahbratioo solution response Sil signal-toshynoise)

Routine manufacturer insuumoc chbratioo md mtinlclulc procedures should be foUowcd u neccss~ to oprinize perfonnanc It is ilio ieessuy to ensure that he eeettospriy intcrfae components are de~ A dirty SoWC can ciuse driti in iimument response

4 3 J Samrile frtafrris

Initially u lcist I md prce~bly runs ofa mattit-om1iaing sample should be ~de to equilibrate the ESI-LCMS system prior 10 r~g a simpfe se uniess instrument pcrformanc allows otherwise

DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547

DuPont le=ort gto 2292

Ctlibntion sourioos llld saoplcs should be 3ltc~tciy amir--i through the inalysis set so icst samples cm be qcntiiei using the lv~ge respoI13C oibmcliIlg mncilrd (ie bull sendMd supie stlttdud sample mnciarci e) Ifinstrmdt performmce is ~ie it is ~issibic o run 2 smpci berwci eic stu1dud r6vidcd a suridltld ~~ tbe ~ smpe ofihe set JDd follolV the 11st sacrple of the sct Ac 3 mininmm i chcic samolc consisting of a control forriDd 11 plusmne LOQ and -rocessed through the mcchod should be 1lD with ev~ sampic set

4 J middot ferhods

The ppci found md percit ofapplied mocries ire denined from ClkularioClS wiriei compare the pell ue3 responses of each malya to the rcspoase ofbrackctingmiddotuuiyticll stin~ds Use onlv the primary ~ cwmel for quzntiwio_n Do not use the Toed Ion Cbromito213m ~cl ari inpoosc values should be cnteredmiddotin an EltCEL bull spradlhect tcxpiatc designed to peform the iypnipriate calculations

The response facor (RF) is cdailated for euh malytc in all cili0r1tion sundard anal)lcs by dividing the peak arc by the inalytc concuntion One may use either the avcrigc response facor of the entire set of stmchrtls if the ri-spomc has be= mblc over the period of mUysis or one mlY use the 3VCrJgc of the closer two stanriard1 hhlcb ~the sample being qttalltitlted ifin~int drift bas bcei noted In either C3Sc valid recovery dara ire gcucntcd ittbe p~t relative stlJdanl deviation (1oRSD) for the pcalc arc rtSpOD$CS oftbe stmdardsuscd bless than or Cqu3l to 20oo Values for the unowt (ppm) decc-ed in samples arc dctcmiaed by comparing the peik uca of =ch saniplc ~lytc detected with the avcrigc ~ocsc Uc+or and comQng for aliquots weight of sample md fimJ volume Tac p===ir o(applicd recovcri= Ibr ortiiicd simplcstre clc-lated by dividing pPm fodegUnd by ppm applied md mulriiying by 100 middotbull

C (conebullbullof sample pgfml) bull Arca(samplc)RFavg)

ppb (=cpk) bull CW bull (IAF) FY

W bullweight of sample (g 1 mt lg) AF bullaliquot frlction (voL iliquottoul vol) FYbull total volume of final analysis solution (mL)

Sample Cilcubciont (Brack-ting Smdards) For a bypotheticil malytc

~O mL (bull20g) watcr smple fortified at 0100 ppb aliquot fricion bull 1 F1I13l Vownc 2 mL

Respocsc of067 ogimL Std bull 700 area counts Respocsc of20 ogimL Stdbull 2200 ~counts Response of0100 ppb fortifiQtion 1200 3tC3 counts

RF(ltvg [(220020 aglml) + ltOOI06 bullml)J2 bull 1072(mJag) Cone S31Dple bull 1200ll072(rnUag) bull 1119 ogmL AF 20ml20ml bull LO

ppb simple bull l119 (oVml)20g) bull (11) bull 2 mL bull 01119 nSf~ 01119 ppb reovc-1 01119101000 bull 100 111~4

DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547

DuPont Repor -middoto 2292

FGUR 1 CiiEMICAL STRUCTURES AND NAMES

~none Dext COe 1b middot DPX-ASi4 c=rz1 Nsre= S-Ttiazine-24-(1H3Hcicne ~

cfCdiexyl-Sdrethyfarrirc bull 1-rre~

~~iteA QPQf Cedbull No middot T393i cr-eijnt Nambullmiddot STriazine-24-(1H3H)-dione 6shydimethylamino--3-4-hydroxyc-ftigt hexyl)-1-methyl

CA c R-strt Na bull rone

Mtaciile A1 bull [) bullPmt Ode b bull G3453

Omira S-Trmre-24gt1-31-0cre i1ra-sshy~delt)l-~rrEtyenaiiro-Cdc Pelttry middotncoe

WetlttoliteB a rPNrt rcro tti middot 1N-A3928

eemr1 Nare= S-Triazine-24-1H3HQcne 3shyoCd1exyl-1~~no)-CAC imy b middot 55611middot54-2

Wetaxtile C D poundmf Oce tb middot IN-T3935 Qerriral Nzrremiddot S-Triazine-24-(1H3Hdicne 3shy(~)-1-rrelh)iS (rrelh)iamno)-

DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292

F1GURO 1 (CONTINUED)

CHEMICAL STRUCTURES AND NAMES

OB

~r-(- t JI

o~N1iCR3I ell

r-1 ~--I middot I o~~o

I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex

Mtaclite C1 Dfn rr middot tN-G3454

CP7ic3 N=rremiddot S-Triazine2+1HH-ciaie 3shy(2~00Egt)l)-1-irelhyl-Q (rrelllyianino)shy

CS PeSQr middotrcoe

MaxiileD QrpotCcdbull Nemiddot lN-82338

CA$ pntrr Nomiddot none

Mtaiciite E shyDre=xrt ore tt bull JNT3936

Cibull1 N2rmiddot S-Triazine-246-1 H3H5H)shytrione 1-4 hytroxycjcohexyf)-3-roethyt

MtaioliteF QbullPT C=Ce 1b bull Nl3221

Qerrid Ncrre= S-Triazine-24-1H3HclCte Jcltj~1relhyi-

CS ~N middot rcne

MaxliteG QbulleatCCNmiddot N-T4916

Qerric Narre=STriazine--24-1H3H-Glcre JclaquoclEgt~yenaffioo

cs csr c middot rxne

DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292

FIGURE 1(CONTlNUED) CHEMICAL STRUCTURES AND NAMES

Welttxiite H middot p er ccre h bull JN-A-0111

Omira Nam S-Triazire-241H2hOcre 3

~= (AC ~estcy fb ~

-~iteG3170 o eyt Cap Nimiddot IN-G3170

Qerid Ncrre STriaitine-~4-(1H2h acre1-rrah)l~ anro

~rcre

Mtadite G31i0 n-gtucsiCeD poundTr ore Na JN-NCS33

Omira S-Tria2ire-241H2h]-Ccre 1~rrenlariroOil=de

DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547

Modifications to Duoont-2549 to confinn bv LCMSMS

If sample splitting is needed to allow confirmation by LCMSMS the 16xOO mm silanized glass tube used in step 445 must be calibrated at 10 mL as well as 20 mL

Follow the method (Met-JOI revision 2) through step 451 At step 451 insert at end Adjust to 20 mL with methanol vortex to mix sonicate 5 minutes Readjust to 20 mL with methanol ind vortex Remove I mL for LCMSMS if required

Evaporate to dryness Continue with method DuPont-2292 (soil and water LCMSMS method) final preparation step 429 Cl8 Bond Elut CleanupFinal Preparation step 8

Standards for LCIMSMS analysis inaybe prepared from standard solutions used for GCNPD analysis by evaporairig the organic solvent and redissolving the residue inmiddot water with mixing and sonication

- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION

Deviation Number 1 Date of Occurrence 050699

CAL Study Number 008-036 Sponsor Study Number DuPont-2547

DESCRIPTION OF DEVIATION

Step 429a Cl8 Step 9 ofDuPonr-2292 located in Protocol Appendix 2 states that exactly 20 mL ofHPLC water should be added to the tube containing the evaporated C18 eluate Instead for the reagent blank sample controls and spikes A-E the volume to be added to the tube was calculated as described in step 454 ofDuPont-2549 (Protocol Appendix 1 ) so that the concentration of the sample in the final extract was 25 gmL

-middot ACTIONS TAKEN

ie amendment issued SOP revision etc

Deviation issued

Recorded ByDate lad )vi-d 5 -17-i)

IMP ACT ON THE STUDY

No negative impact on the study

~ di-eNtnJ s -17-1l Study Director Signae Date

CAL QAU Review Gw tj 19 lqq February 12 19982

126

DuPont-2547

~ _

C-middotmiddotmiddot

(

~middot

~middot-- bull

Ceitrifuge

Ceitrifuge Tubes

Evaporators

Evaporator tubes

Filter Pap-

EDP Electronic Pipets witi suitable tips

Reservoirs (75 mL 25 mL or 15 mL) and adapters for use witi SPE cimidges

Solid Phase Extraction Apparatus

Solid Phase Extraction Columns

DuPont-2547

SOP Metlt-101 Page2

[EC clinical cemrifuge (lnrenational Equipment Co Needham Hts MA)

50 mL polyehyleie or poiypropyleie c-itrifuge tubes Widi scew-cip closures

N-Evap Models 112 and 115 attached to a nitrogen source (Organomation Associates Souti Berlin MA)

Turbo-Yap 200 mL unit (Zymarlc Corp~ Hopkinton MA)

Zymark 200 mL tnbes (Zymarlc Corp Hopkinton MA)

Wbatman541

VortexGenie 2 VWR Scientific Bridgeport NJ)

Rainin Ridaefieri NJ

Varian Analytictl Instruments Sunnyvale CA

Vac Elut Mode SPS 24 (Varian Analytical Instrwiients Sunnyvale CA) or

Y-tsiprepnlt Solid-Phase Extraction Vacuum Manifold (Supelco Inc Bellefonte PA) middot

SupelcI=nlt Envftrade-Carb SPE Tubes Custom 12 mL Polypropylene Tubes with Teflon Frits packed with 15 grim ofENVI-CARB (Supleco Inc Bellefonte PA)

C13 Mega Bond Elut 6 cdl grun (Varian Part1225shy600 I) (Varian Inc Harbor City CA)

- 13 shy

76

l

DuPont-2547

middotmiddot

Shake

Test Tubes

ultrasonic Bath

pHmeer

Actcne


Ethyl Acetaie


middotHexane

Metianol


Sodium Chloride

Toluene

Water


DuPont-2547

SOP Me-Ji-1O1 Page 3








Reigem grade



Reagent grade

Reigent grade


HPLC grade

- 14 shy

77

DuPont-2547

DuPont-2547

SOP Meth-Ot Pige 4

33


Analvte











MLx



- 15 shy

78

DuPont-2547

DuPont-2547
















- 16 shy

79

DuPont-2547

DuPont-2547






41 Princiole












- 17 shy

80

DuPont-2547

DuPont-2547















- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

l

DuPont-2547

middotmiddot

Shake

Test Tubes

ultrasonic Bath

pHmeer

Actcne


Ethyl Acetaie


middotHexane

Metianol


Sodium Chloride

Toluene

Water


DuPont-2547

SOP Me-Ji-1O1








Reigem grade



Reagent grade

Reigent grade


HPLC grade

- 14 shy

77

DuPont-2547

DuPont-2547

SOP Meth-Ot Pige 4

33


Analvte











MLx



- 15 shy

78

DuPont-2547

DuPont-2547
















- 16 shy

79

DuPont-2547

DuPont-2547






41 Princiole












- 17 shy

80

DuPont-2547

DuPont-2547















- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Meth-Ot Pige 4

33


Analvte











MLx



- 15 shy

78

DuPont-2547

DuPont-2547
















- 16 shy

79

DuPont-2547

DuPont-2547






41 Princiole












- 17 shy

80

DuPont-2547

DuPont-2547















- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Meth-10 l















- 16 shy

79

DuPont-2547

DuPont-2547






41 Princiole












- 17 shy

80

DuPont-2547

DuPont-2547















- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547






41 Princiole












- 17 shy

80

DuPont-2547

DuPont-2547















- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Meth~OI middot (














- 18 shy

DuPont-2547

DuPont-2547

SOP Meh-Ql Page 8
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Meh-Ql
















- 19 shy

82

DuPont-2547

DuPont-2547

SOP Meth-to Page 9














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Meth-to














- 20 shy

83

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101 Page 10







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

( 46 GC Anilvsis

SOP Mem-101







Carrier Gas Helium

Flow Column Makeup



Detector 285 C


Rale2 Final


462 Sample Analvsis


- 21 -

84

DuPont-2547

DuPont-2547


46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP Me11-101

46J Calculations



y=mx+b

where



( m=siope

b = y-intercept


L ppb analyte =


where




- 22 shy

85

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547








ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

mL solvent =

mL aliquot =

mL final volume =

GC dil fuct- =

DuPont-2547

middotso Metli-10







ppo addd -x 100

50 REFERENCES




r--middot

- 23 shy

86

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547



Purnqse




Procedure


h=e shy





- 28 shy

91

DuPont-2547

DuPont-2547

SOP MedJ-lO





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

SOP MedJ-lO Page 13





(


Kevin Clarl

rmiddot

- 29 shy

92

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547









To~ cortrpeted




To ~ a1mpleted


LJ poundquipme1Jt

Sundlrds Pr~2ririon

DRAIT 3

- 33 shy

95

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

DuPont Lort lo1292





















DRAFT 4

- 34 shy

96

11

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547












40 METHODS






4 I 3 lOMS Anavs-is


DRFf 5

- 35 shy

97

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

Duoot Rrort ia 1292














DRAFT 6

- 36 shy

98

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547












DRAFT 7

- 37 shy

99

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

CuPon Reorr ~a 192



anal~is set



41










DRAIT

- 33 shy

100

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

















DRAFT 9

- 39 shy

101

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547



















DRFT 10

- 40shy

102

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

















DRAFT 11

- 41 shy

103

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547












fJ InruumeruariJJn

JJ I DecriDrion






DRU

- 42 shy

104

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

Mobile~ Prosnm










DuPont-2547

Duoni Reon ~o 292

A B

0 100 0 90 10

10 50 50 LO 25 75 151 5 95 200 5 95 201 0 100 300 0 100




Set is shown below







DRAFJ

- 43 shy

105

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547
















DRu-f

- 44 shy

106

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547



4 J middot ferhods











DRAFT 15

- 45 shy

107

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547












DRAFf

- 52 shy

114

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

Duot teort ~o 2292



OB

~r-(- t JI

o~N1iCR3I ell


I C3

lOQ~X aN~o

I ex

Q~ o~ll

I shyex



CS PeSQr middotrcoe







CS ~N middot rcne




DRAFf 23

- 53 shy

bull

115

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547

OuPoct Rort No 2292




~= (AC ~estcy fb ~



~rcre



DRAFT 24

- 54 shy

116

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

DuPont-2547






- 63 shy

125

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

DuPont-2547

l

Page 1 of 1

PROTOCOL DEVIATION







Deviation issued






126

45132802 Hexazinone ECM Soil - US EPA...Assorted laboratotY g1.,;sware including: gradlla!ed...

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Transcript of 45132802 Hexazinone ECM Soil - US EPA...Assorted laboratotY g1.,;sware including: gradlla!ed...