Document KR18a5onYxMJwpxMm2B26p9gX

RECYCLED 03 AR226-2681 3M Environmental Laboratory AR226-2681 Results from Analyses of Soil and Groundwater Samples From the E. I. DuPont de Nemours and Company Facility in Parkersburg, West Virginia STUDY COMPLETED: October 27,1997 FINAL REPORT COMPLETED: November 13,1997 Prepared by: . Susan A . Beach Senior Environm ental Biologist 3M Environmental Laboratory Building 2-3E -09 935 Bush Avenue S t Paul, MN 551 4 4 E ID 129573 ASHO10474 anil Environmental Laboratory Table of Contents Summary of Results: 3 Project Description: 6 POAA Analyses in Groundwater and Soil (5/97 Samples): 7 POAA Analyses in Groundwater (6/97 Samples): 15 POAA Analyses in Soil (6/97 Samples): 22 Volatiles and Semi-volatiles in Groundwater by Purge and Trap Concentration with GC/MS Analysis(6/97 Samples): 30 Volatiles by AED (5/97 Samples): 38 Volatiles by AED (6/97 Samples): 45 Total Fluoride in Soil (6/97 Samples) 55 Total, Organic and Adsorbable Fluoride in Groundwater (6/97 Samples) 64^sorDaoie Soil Properties and Nutrient Concentrations (6/97 Samples) 79 Copies of Chain of Custody, Shipping Papers, Lab Requests 105 m ASH010475 3L 4 ^ E ID 129574 3 M Environm ental Laboratory T ir Summary of Results . DuPont Washington Works Samples Sample Dates 5/8/97 (groundwater), 5/30/97 (soil) DuPont 3M LR No. Smpl. No. Matrix R2008-1 1 ground water R2008-2 2 ground water R2008-3 3 ground water R2008-4 4 ground water R2008-5 5 Dl blank R2008-6 none soil POAAi", PPb 52 49 52 53 n.d- 364 Voi. & Semi Vol. F, Cl, Br by AED, ppm <M QLW <M Q L <M Q L <M Q L <M Q L <M Q L (1) R O M = Perfluorooctanoic acid anion (2) limit o f detection/limit of quantitation = 650 ppt. (3) Minimum quantitation limits: Br -1 .1 7 6 ppm in w ater, 1 .1 8 7 ,1 .2 2 0 ppm in soil Cl = 1.408 ppm in water, 1.253,1.461 ppm in soil F 0.280 ppm in w ater, 0.282 ppm in soil . ASHO10476 vo f'O E ID 129575 iff c. V < 0li W**"* . n 'i DD** m Environmental Laboratory Summary of Results DuPont Washington Works Groundwater Samples ASHO10477 to J TP :r- E ID 129576 DuPont 3M LR No. Smpl. No. R2148-1 MW-1-1 R2148-2 MW-1-2 R2148-3 MW-2-1 R2148-4 MW-2-2 R2148-5 MW-3-1 R2148-6 MW-3-2 R2148-7 MW-4-1 R2148-8 MW-4-2 R2148-9 MW-5-1 R2148-10 MW-5-2 R2148-11 MW-6-1 R2148-12 MW-6-2 POAA mg/L 5.64 5.32 0.234 0.234 0.487 0.477 0.0842 0.0590 < PQL < PL~ < MDL < MDL Total Fluorine mg/L 8.0 16 3.3 3.5 4.2 3.3 4.0 4.2 3.0 2.8 2.3 4.2 Adsorb. Vol. & Semi- Trichlorotrl- Fluoride Ion Organic Organic F, Vol. F by fluoroethane mg/L F, mg/L mg/L AED, ppm pg/L 0.20 7.8 4.5 0.20 <[F]< 2.5 820 0.20 16 4.2 0.20 <[F]< 2.5 730 0.16 3.1 0.28 0.20 <IF]< 2.5 1600 0.16 3.3 0.46 0.20 <{F]< 2.5 1500 0.14 4.1 1.1 0.20 < fF]< 2.5 2300 0.14 3.2 0.76 0.20 <[F]< 2.5 2400 0.11 3.9 0.19 0.20 <[F]< 2.5 760 0.11 4.1 0.14 0.20 <[F]< 2.5 670 <0.10 2.9 0.11 IF] <0.05 130 <0.10 2.7 0.14 0.05 <[F]<0.20 140 0.10 2.2 <0.05 IF] <0.05 0.10 4.1 <0.05 IF] <0.05 .......... t-- Acetone pg/L . 10 __ _ 10 _ _ -- 1.1,1- tert-Butyl cis-1,2- trichloro- Trichloro- Tetrachloro- Trichlorofluoro- DuPont Alcohol Dichloroethene Chloroform ethane 3M LR No. Smpl. No. pg/L pg/L pg/L pg/L ethene pg/L ethene pg/L methane pg/L R2148-1 MW-1-1 59 mma ._ _ _. R2148-2 R2148-3 R2148-4 R2148-5 R2148-6 R2148-7 MW-1-2 MW-2-1 MW-2-2 MW-3-1 MW-3-2 MW-4-1 49 5.8 .. 140 150 5.5 14 520 5.9 14 570 37 6.3 81 _ _ _ 5 5.2 _ _ 16 18 26 26 5.9 R2148-8 MW-4-2 5.9 39 6.2 66 _ R2148-9 MW-5-1 13 R2148-10 MW-5-2 16 5.8 _ _ _,, R2148-11 MW-6-1 _ R2148-12 MW-6-2 _ _-- -- -- -- (1) POM Perfluoroootanoic add anion (2) Practical quant limit = 0.0510 m g /J ^ ^ , (3) Urnitof detect. - 0.0255 mg/L (4) Total Fluorine Fluoride ion - Organic Fluorine SM Environmental Laboratory Summary of Results DuPont Washington Works Soil Samples Sample Date 6/23/97 ASHO10478 DuPont 3M LR No. Sample No. R2382-1 SS-1 0-2' R2382-2 SS-1 4-6' R2382-3 SS-1 8-10' R2382-4 SS-1 12-14' R2382-5 SS-1 16-18' R2382-6 SS-1 20-22' R2382-7 SS-1 24-26' R2382-8 SS-1 28-30' R2382-9 SS-1 32-34' R2382-10 SS-1 36-68' R2382-11 SS-1 38-40' Total Fluoride, mg/kg 21,300 20,100 61,200 78,300 106,300 82,700 59,100 37,600 33,500 41,200 30,300 POAA"', mg/kg 0.119 0.17 614 207 219 39.8 24.6 29.3 13.1 6.78 2.11 Sulfate, mg/kg 98 99 73 54 43 70 220 150 100 63 46 Sulfite, mg/kg <2 <2 <2 <2 <2 <2 <2 <2 <2 <2 <2 Nitrite, mg/kg 0.41 0.41 .36 0.14 <0.10 <0.10 <0.10 0.11 <0.10 <0.10 <0.10 pH in water 7.7 7.7 7.3 6.7 5.7 6.0 5.8 6.8 5.8 6.1 6.8 pH in CEC, CaCI2 meq/100g 7.2 15.8 7.3 18.4 7.0 17.5 6.3 17.5 5.3 18.4 5.5 19.3 5.3 17.5 6.3 11.4 5.2 13.1 5.4 9.6 6.2 6.3 Moisture, % 12.3 12.7 15.5 18.9 18.3 19.2 20.0 18.1 , 13.6 17.9 22.2 (1) POAA = Perfluorooctanoic acid anion 5 "S* 10 E ID 129577 3M Environmental Laboratory Project Description Three coolers were received from E.I. DuPont de Nemours and Company ("DuPont"), each containing samples for analyses by the 3M Environmental Laboratory. Each cooler-group was assigned an unique project number (Lab Request Number). Each sample was also given an unique number which was a sub-set of the project number. The project numbers are as follows: R2008, samples 1-6 * Four groundwaters, one Dl water blank and one soil sample, with sample dates 5/8/97 (waters) and 5/30/97 (soil). R2148, samples 1-12 . *rp#w Twelve groundwater samples, with a sample date of 6/26/97f " R2382, samples 1-11 Eleven soil samples, with a sample date of 6/23/97 Samples were stored at 4C, in the dark, until analyzed. Different groups within the 3M Environmental laboratory were responsible for various analyses. Attached are the summary reports for analysesbf-iPCAA, e Total, free, organic and adsorbable fluoride, volatiles and serriMlatrlOSiihitratev sulfate, ahdrsulfide, and soil pH, percent moisture and cationsefdttlaftgliM capacity. ASHO10479 & EID 129578 3WI Environmental Laboratory POAA Analyses In Groundwater and Soil (5/97 Samples) t:>r 'llra t# 74 E ID 129579 ASH010480 3M Environmental Laboratory Date Received: Sponsor or Client: Representative Name CompanyName DuPont Company Address Phone Project Lead: Kris Hansen (8-6018) Group Leader. Jim Johnson (8-5294) Analyte(s) or T est Method #: POAA Sample Matrix: water and soil Analysis Dates: 9/97-11/97 Author, kjh reject Lead (or designee): James D . Johnson (or designee): Analyses): GML, JJ, kjh Data Reviewed by: Internai JDJ: QAU (Archives): ,IRN System: roject Manager: Sue Beach Others (ListRecipients/ Address/ Phone/ FAX) T. DiPasquale, 22-11E-03; 3-1891; 736-3257 mmf. aam raeel:-. Sent b y :/ Date lgh on 10/21/97 Sent b y :/D lgh on 11/10/97 /A ddress 36-325'-' 00 A copy of ifae report mcludingt&ii form and tlse dient eover page i*to he given ta QATJ, LERN and to the Group Leader. $H E ID 129580 \ ,4 , * 3MEi iVi u o mental Laboratory- Advanced Method Development Team Kris Hansen - Sr. Analytical Chemist Advanced Method DevelopmentTeam Building 2-3E-09 612-778-6018 Irjtiatiranffinmnm a im R eport - A nalytical Study Determ ination o f PO AA in Soil and W ater 1.0 Summary _ One soil sample and five water samples were submittedby DuPont for quantitative analysis o f ^s-/, perfluorooctanoic arid anion (POAA). The soil sample was assigned number R2008-6; the water samples ,6 a* sea** werepvennoinbeisKM 08-ldmnig^B2008-5. A n a l^ o ftlie san^les ly negative ion etec tan p i^ ; mass spectrometry (ES/MS) determined that perfluorooctanoaie acid anion is present in all samples except ? >; . , . R2008-5. Specific results are listed in Table 1. ' *> . ! Table 1. Concentration of POAA In R2008 aarngM , ft Sam ple# R2008-6 Dilution M atrix Factor E x tra c ta b a soil n a. na. C o rrected Average " T p b ) " ... Std. Bev. 0.364 mg/kg n a . n a . R2008-1-1 water R2008-1-2 water 2 2 1.3 1.3 R2008-2-1 water R2008-2-2 water 2 2 1.3 1.3 R2008-3-1 water 2 1.3 8 R2008-3-2 water 2 1.3 R2008-4-1 water 2 1.3 R2008-4-2 water 2 1.3 R2008-5-1 water 2 1.3 R2008-5-2 water 2 L3 * limit ofdetection/limit ofquantitation is650ppt '' 52 52 49 49 52 52 57 49 nd.* m<L* 52 0 49 0 1 #j rm agfen# -, i0 53 6 na. na. 2.0 TEST MATERIALS One soil and five water samples were received ftom DuPonton 06/10/97. The samples were stored at 4C until extraction; extracts were stored at 4C until analysis. -Am, 3.0 EXPERIMENTAL-OVERVIEW AND METHODS 3.1.1 Sample, soil - Because no uncontaminated soil was available for blank analysis, the method of standard HdirinTi ^35 4^.m iine the cnncentiarion ofPOAA in the soil received from DuPont An eight point standard curve was prepared by spiking 2gram samples ofthe soil with some amount ofPOAA solution between 500 ppt and 1.0 ppm. The soil was mixed with a^roxim ately 1 gram of diatonaaceous earth and loaded into a 10 mL stainless steel extraction cartridge. The spiked samples were extracted using high pressure solvent extraction (HPSE) with methanol; the extracts were dried with nitrogen and reconstituted with ACN/water (1:1). After analysis by negative ion ES/MS, the data was subjected to linrer regression and the resulting prediction equation was used to determine the concentration o f analyte fe . X g s Word Version 6.0 Lab Request #R2008 R2008DQC 1 1 4 '* s E ID 129581 in the unspiked material (see Figure 1, attached). Four unspiked soil samples were also extracted to confirm that the method reproducibility wasbetter than 10%. Th(method nfstandard addition assumes there are no interferences in the analysis and that the extraction efficiency of tlie analyte from the matrix is not dependentupon analyte concentration. The first assumption is addressed by the selectivity of the both the extraction and the analysis; the latter has been verified in another study that focuses on a similar matrix. 3.1.2 Sample, w ater For method development, two series ofsampleswere prepared for analysis by ES/MS. In series A, the target analyte was extracted from the samples with an ion pairing reagent and analyzed; in Series B, each sample was diluted (1:1) with acetonitrile (ACM). Both Series A and B consisted of 2 aliquots of water from two o fthe submitted samples (R2008-1 andR2008-3). The recovery ofPOAA resulting fiom Series A and Series B analysis were in close agreement ' All five water samples were prepared, in duplicate, for analysis using the Series B protocol. The samples were analyzed by ES/MS between two unextracted curves ofPOAA in ACN/H20. The reproducibility o f the curves was within 15%. 3.2 C alibration and controls, w ater A set of controls, including a miili-Q waterblank, milli-Q water spiked with POAA, and four samples of matrix spiked with POAA, was prepared along with each sample series. The controls were used to evaluate extraction efficiency ofthe POAA fiom water and subsequently determine an accurate extractability fector for final concentration calculations. A POAA standard curve firom 50 ppt to 1.0 ppm in ACN/H20 (1:1) was prepared; all extracts and prepared samples were analyzed by negative ion ES/MS and quantitated relative to a standard curve. The unextracted standard curve was plotted according to linear regression with a coefficient of determination (i2) equal to 0.999. Two-1 mL aliquots ofsample R2008-1 were spiked with POAA. These samples were designated the matrix giike (MS) and the matrix spike duplicate (MSB) and were prepared for analysis by the same procedure as the samples. The final concentration ofPOAA in the MS and MSDwasexpected to be 52 ppb. The concentration ofPOAA recovered from the samples was evaluatedirelifive.tethestandard curve. am -' < ' >: 3.3 Extraction specifics, soil The soil samples were extracted with the ISCO 3560 AcceleratedExtraction System, with ISCO 100DX high pressure syringe pumps according to the following conditions: Extraction solvent: methanol, HFLC grade Extraction pressure: 2500 psi Extraction tnnpcistuic* 70 C Restrictor temperature: 70 C Static extraction time-1: 40 minutes Dynamic extraction volume-1: 15 mL Static extraction time-2: 2 minutes 4.* Dynamic extraction time-2: 2 minutes Restrictor flow rate: 2.5 mTJmm Samples were reconstituted in glass autoviais with HPLC-grade ACN and milli-Q water. & g I w W ord Version 6.0 Lab Request #R2008 R2008.DOC 2 lO 4 IS' E ID 129582 3.4 ES/MS Analysis specifics, soil and w ater Negative ion ES/MS analysis was performed on a Micromass Platform E atmospheric pressure ionization mass spectrometer running Mass Lynx 2.1. A HewlettPackard 1100 was used for the autosampler and HPLC system. Mobile phase: ACN/H20 (1:1) How rate: 60 pL/min Injectionvolume: 15pL Cone Voltage=-20 Capillaryvoltage = -2.56 Source Temperature = 80C f AnalyzerVacuum Pressure=0.000079 mBar Quantitative results were based on the instrumental response generated by monitoring a single ion characteristic ofthe analyte. This type ofmonitoring minimizes interferenceby other ions in solution and increases system sensitivity to the target analyte. 4.0 DATA ANALYSIS 4.1 Sample, soli By the of^tarufani addition, the soil was determined to contain 0.364 mg POAA/kg. This value was calculated using the prediction equation resultingftom linear regression analysis erfthe eight point extracted curve. The coefficient of determination forthe curve is 0.990. Calculations used to determine the concentration ofPOAA in the soil are shown in AppendixA. 4.2 Samples, w ater - The concentration ofPOAA in each watersample was deternunedby comparisonipfdetected ncing the falhwring formula- C .= (P -I)/S ' i< ii M?9W5sfE fcSIStlfc (4) Where, C, = Concentration ofPOAA in sample (pg/mL) P = Peak area ofsample (response) I = Intercept of the calibration curve (response) S = Slope ofthe calibration curve (response / concentration) The concentration determined to be in the extract was convertedto tiie concentration in the water samples according to the following equation: C p= (C . * D )*E (5) Where, r , = Concentration ofPOAA in actual sample (pg/mL) C. = Concentration ofPOAA in prepared sample (pg/mL) D = Dilution Factor E = Extractability ` ASHO10484 W ord Version 6.0 Lab Request #R2008 B2008.DOC 3 /I 4 MS' E ID 129583 4.3 Determination ofpercent recovery and extractabiiity, w ater Matrix spike samples were analyzed to determine the recovery ofPOAAfrom the water. POAA recovery and the related extractabiiity value are calculated as follows: % R= [(Q - QO / Q|*100% (6) where, %R= Percent recovery ofPOAA Cf= Concentration ofPOAA found in MS/MSD (pg/mL) Q ,= Native concentration ofPOAA in samplebefore dilution adjustment (pg/mL) C ,= Concentration ofPOAA spiked in MS sample (p.g/mL). As an example, the percent recovery for the R2008-1-1, MS sample is calculated as follows: therefore, Cr= 0.057 ig/'mL; 0 = 0 .0 2 0 pg/mL; C, = 0.052 pg/mL; % R= (0.057-0.02J/0.052 x 100%=74% The extractabiiity is equal to 100% divided by %R- The percent recoveries ofPOAA in the MS and MSD samples and the corresponding extractabiiity fectors axe presented in Table 2. Table 2 % recovery ; Recovered S p ile d Concentration Concentration Sample (ue/mL) (h/mL) MS 0.057 0.052 MSD 0.059 0.052 Native (pgftnL) 0.02 0.02 Average % Recovery 74 75 75 Extractabiiity 1.3 1.3 L3 & uwuaxm& mi. - > r^.. re Sp;si . .ti jC <% . 5.0 CONCLUSION High pressure solvent extraction, ES/MS analysis and linear regression analysis were nsed to f s te e a m .: >> determine th at0.364 mg/kg ofPOAA is present in the soil sample received from DuPont W alersan^SK IA # R2008-1 through R2008-4 also contain about 50 ppb POAA. No POAA was detected in R2008-5. 6.0 MAINTENANCE OF SAW DATA AND RECORDS Hard copies of these data are filed in the AMDT archive. ' .m n ii . '*1I A1 ReportpcipoerfK^kjh go 2oo Lh W ord Version 6.0 Lab Request #R2008 R2008JDOC 4 4 E ID 129584 ' ` ,! III DATA TABLE 1.0 Spiked Standard Cone, of POAA In Extract (pg/mL) Blank 0.0005 0.005 0.050 0.100 0250 0.500 0.750 1.000 Cone, of POAA in Soil (pg/kg) 0.00 0.50 5.00 49.22 99.63 248.97 493.88 748.39 995.17 FIGURE 1.0 R-2008 DuPont Soil Data POAA Standard Curve and Data Table Volume of Extract (mL) 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Peak Area of Extract-a 1822272 2076435 1967476 2129047 2457197 3249144 5136166 5879632 .. 7704024 Spiked Amount of of POAA in Extract (pg) 0.00 0.001 0.01 0.10 0.20 0.50 1.00 1.50 2.00 Peak Area of Extract-b 141494 396700 475027 623624 225468 395568 666830 786883 842187 Mass of SoU (g) 2.0259 2.0032 2.0004 2.0319 2.0075 2.0083 2.0248 2.0043 2.0097 Total Peak Area (a +b) 1963766 2473135 2442503 2752671 2682665 3644712 5802996 6666515 8546211 Cone, of POAA in Soil (pg/kg) 0.00 0.50 5.00 49.22 99.63 248.97 493.88 748.39 995.17 i 9000000 soooooo 7000000 6000000 SOOOOOO A3. 4000000 3000000 2000000 1000000 0 0.00 Extracted POAA Standard Curve _______ Senesi -- Linear (Series!) 200.00 400.00 600.00 800.00 1000.00 Concentration ofPOAA in Soil (pg/bg) 1200.00 A SH 010486 3 4 US' EID 129585 R-20Q8 DuPont S oil Data POAA. Standard Curve and Data Table CALCULATIONS In order to plot the Total Peak Area versus die Concentration o fPOAA in Soil, die following conversion calculations were performed: Cone, o f POAA, 6om spiked standards, ixithe extract Volume Mass Convert X o f X o f X g to Extract Soil kg Cone, of S3 POAA in Soil pg X mT. X 1 X 1000 g - ......PS mL 1g kg kg To calculate total Peak Area, the area integrated for peak "a" for the initial extraction o fthe soil and the area integrated for peak "bn for the second extraction o fthe same soil are summed. Using the Method o f Standard Addition determine indigent analyte concentration by solving for for die x-intercept where y **0, and equation o fthe slope o f the line o fPeak Area vs. Cone, o fPOAA in Soil is: y = 6248 x + 2275109 x = -2275109 / 6248 x = -364 concentration of indigent analyte POAA in soil determined to be 364 pg/kg r>? ASH010487 f 4 IA S " *. E ID 129586 3M Environmental Laboratory POAA Analyses in Groundwater (6/97 Samples) Mill .F fc. IS i U S ' . E ID 129587 ASH010488 3M Environmental Laboratory, Date Received: Sponsor or Client: Representative Name CompanyName DuPont Company Address Phone Project Lead: Kris Hansen (8-6018) Group Leader: Jim Johnson (8-5294) Analyte(s) or Test Method #: POAA Sample Matrix: water Analysis Dates: 9/97-11/97 ' Analyses): LAC Author LAC, kjh Data Reviewed by: PAR reject Lead (or designee):kjh am esD . Johnson (or designee): <mm . 1 . -saem. Internal Sent b y./D ate JDJ: QAU (Archives): LIRN System: Project M anager Sue Beach __________________ .__________ _________________ ;_______ Others (ListRecipients/Address/Phone/FAX) Sent by: / Date T. DiPasquale, 22-11E-03; 3-1891; 736-3257 on 11/10/97 ASHO10489 A copy of the report including this form and the client cover page hi to be given to QAU, LIRN and to the Group Leader. . /& i n e E ID 129588 K 3M Environmental Laboratory - Advanced Method Developm ent Team C ontact: K ris H ansen - Senior A nalytical Chem ist B uilding 2-3E-09 778-6018 Final R eport - Lab R equest R2148 Electrospray M ass Spectrom etry A nalysis o f DuPont W ater Sam ples Prepared 8/26/97 1.0 SUMM ARY Twelve samples from DuPont were submitted to die 3M Environmental Laboratory for the analysis o f Surfactants. These samples were numbered R2148-1 through R2148-12 (MW-1 through M W -6) and analyzed with an Electrospray Mass Spectrometer. This analysis determined that perfluorooctanoic acid anion is present in samples 1 through 10. Results are listed in table 1. Table 1 Sam ple R esults Sample # R2148-1-1 (MW-1) v R2148-1-2 (MW-I) R2148-2-1 (MW-1) R2148-2-2 (MW-1) R2148-3-1 (MW-2) R2148-3-2 (MW-2) R2148-4-1 (MW-2) R2148-4-2 (MW-2) R2148-5-1 (MW-3) R2148-5-2 (MW-3) R2148-6-1 (MW-3) R2148-6-2 (MW-3) R2148-7-1 (MW-4) R2148-7-2 (MW-4) R2148-8-1 (MW-4) R2148-8-2 (MW-4) R2148-9-1 (MW-5) R2148-9-2 (MW-5) R2148-10-1 (MW-5) R2148-10-2 (MW-5) R2148-11-1 (MW-6) R2148-11-2 (MW-6) R2148-12- (MW-6) R2148-12-2 (MW-6) [on Count Dilution Area Factor 160473 157432 148341 153530 79430 75610 80126 74915 135558 143990 135283 139707 43324 37814 35756 32916 24116 23264 21873 26025 11696 11932 9132 10595 20 20 20 20 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 Concentration pg/mL (ppm ) 5.71 5.58 5.21 5.42 0.242 0.226 0245 0.224 0.469 0.504 0.468 0.486 0.0954 0.0731 0.0647 0.0532 <PQL <PQL <PQL <PQL <MDL <MDL <MDL <MDL Average 5.64 $32 $ 0234 0234 0.487 0.477 0.0842 0.0590 <PQL <PQL <MDL <MDL Std. Dev. 0.0872 .vf M-) 0.14% / V*>S-**M-r0*li-)*. 0.0110 0.0149 0.0242 0.0127 0.0158 0.00814 <PQL <PQL <MDL <MDL ASHO10490 i s if ; 1 Word Version 6.0 R2148.DOC Page 1 o f 5 17 M S ' E ID 129589 2.0 TEST M ATERIALS Tw elve water samples were received from DuPont on 07/02/97 (M W -l-l, M W -1- 2, M W -2-1, M W -2-2, MW-3-1, MW-3-2, M W -4-1, MW-4-2, M W -5-1, M W -5-2, M W -61, and M W -6-2). These samples were checked-in as R2148-1 through 12 and were analyzed for surfactants. The samples were stored at 4C until preparation and analysis. 3.0 EXPERIM ENTAL-OVERVIEW AND M ETHODS 3.1 Investigative Sam ples One h alf mL was removed from each sample and diluted with 0.5 mL o f acetonitrile (ACN, TN-A-1504) for a final sample solvent com position o f 1:1 ACN:Water. These samples were vortex mixed and ready for analysis by electrospray m ass spectrometry (ES/MS). 3.2 M atrix Spike Samples Matrix spike (MS) and matrix spike duplicate (MSD) samples were each prepared diluting 0.5 mL from sample R2148-12-1 with 0.5 mL o f ACN. The M S and M SD samples were each spiked with 0.005 mL o f a 101.1 pg/mL (ppm) ammonium perfluorooctanoate standard solution (W 397-741) for final concentrations ofQ .503pg/m L. 3.3 C alibration Ammonium Perfluorooctanoate calibration standards, ranging in concentration ..iooeuu^-. . from 0.0500-1.01 pg/mL, were analyzed bracketing the samples. The calibration curve irfj>"m? was developed by plotting die mean o f two standard peak areas o f ammonium tag ths asm o f w perfluorooctanoate versus the concentration o f ammonium perfluorooctanoate standardstfceoaaemtraiii: using linear regression. 3.4 Instrum entation The following instrumental conditions were used to analyze these samples: Micromass Platform Electrospray Mass Spectrometer Hewlett Packard 1100 Pump and Autosampler MassLynx 2.1 software Cone Voltage = -14 Skimmer Lens Offset = 3 Source Temperature = 80C Analyzer Vacuum Pressure = 0.000079 mBar Injection/sample: 1 Injection size: 10 pL Flow Rate: 0.080 mL/min 3.5 C ontinuing Calibration Standards Continuing calibration standards at 0.253 ppm ammonium perfluoroctanoate were analyzed bracketing every ten samples during sample analysis. oIS-- V2O Word Version 6.0 R2148.DOC Page 2 o f 5 a 4 E ID 129590 3 .6 D etection Lim its The method detection lim it (MDL) is equal to approximately 3 tim es the baseline noise and h alfthe practical quantitation lim it (PQL). The PQL corresponds to the low est point on the calibration curve. The PQL is 0.0510 pg/mL; the method detection lim it is 0.0255 pg/mL. 4.0 DATA ANALYSIS 4.1 C alibration Curve Average peak areas from the initial curve were plotted against the concentration o f ammonium perfluorooctanoate in the calibration standards. The standard curve w as linear (R2> 0.99). 4.2 C ontinuing Calibration Standard Continuing calibration standards were analyzed before and after every 10 sam ples, The continuing calibration standards remained within 20% o f the initial standard This m eets the criteria used to determine if the calibration curve has maintained linearity. The relative percent difference is calculated using the follow ing equation: s1 *es e u 1:6 E quation 1 %D = -- xl00% where, '. new %D = relative percent difference ' Rj = area 0.253 ppm calibration standard from the initial calibration R* = area 0.253 ppm calibration standard from the continuing calibration "#em tee 4.3 Investigative Sam ples 4.3.1 C alculations Concentrations o f ammonium perfluorooctanoate were determined by comparison o f detected peak areas to the calibration curve using the follow ing formula: etfltiS rvg E quation 2 S W here, Ce = Concentration o f ammonium perfluorooctanoate in extract (pg/m L) P = Peak area o f sample I = Intercept o f the calibration curve oH-* g to Word Version 6.0' R248.DOC Page 3 o f5 /? 4 U S E ID 129591 S = Slope o f the calibration curve (mL/pg) The concentration o f ammonium perfluorooctanoate in the extract was converted to tire concentration in the water samples by using the following equation: Equation 3 Cp = CexD W here, Cp= Concentration o f ammonium perfluorooctanoate in water sample (pg/m L) Ce = Concentration o f ammonium perfluorooctanoate in extract (pg/m L) D = Dilution Factor A s an exam ple, ammonium perfluorooctanoate anion was detected in sample R 2148-1, where P = 160473, S = 493135 m L/pg, I = 19797; therefore, using Equation (2), Ce = ((160473-19797)/493135) = 0.285 pg/mL. To determine the concentration in water, using Equation (3), Ce = 0.285 pg/mL and D = 20; thus Cf= 0.285 pg/mL x 20 = 5.71 pg/m L (ppm). 4.4 M atrix Spike Sam ples Matrix spike samples were analyzed to determine the recovery o f ammonium perfluorooctanoate. Recovery was calculated using the following equation: E quation 4 %R = C" ~ - - xlQ0% Caw where, %R Percent recovery o f ammonium perfluorooctanoate Cn = Detected concentration o f ammonium perfluorooctanoate in MS sample (pg/m L) I- wt e rSfi mAverage background concentration o f ammonium perfluorooctanoate in saipple^ig/m L ) p k fu e/r Cmc= Expected concentration o f ammonium perfluorooctanoate in M S sample (pg/m L). A s an example, the percent recovery for the R2148-12-1, MS sample is calculated as follow s: C,,, = 0.404 pg/mL; Cb= 0 .0 0 pg/mL; Cme= 0.503 pg/mL; therefore, %R - (0.404-0.00)/0.503 x 100% - 80%. A SH 010493 Word Version 6.0 R2148.DOC Page 4 o f 5 0 4 U S' E ID 129592 The percent recoveries o f ammonium perfluorooctanoate in the MS and MSD samples are presented in Table 2. T able 2 M atrix Spilt Results Recovered Expected Sam ple Type Sam ple ED Concentration Concentration1 (jig/m L) (jrg/mL) % Recovery DuPont Water R2148-12-1, MS R2148-12-1, MSD 0.404 0.401 0.503 0.503 80 ^ 80 Notes: Average 80 1 Recovered concentration is equal to the concentration detected in the spiked sample minus the average concentration detected in associated unspiked samples. 5.0 CONCLUSION The results o f ES/M S analysis determined that the ammonium perfluorooctanoate anion is present in DuPont water samples R2148-1 through R2148-10 at average concentrations o f 5.64 ppm, 5.32 ppm, 0.234 ppm, 0.234 ppm, 0.487 ppm, 0.477 ppm, 0.0842 ppm, and 0.0590 ppm respectively. The results have been presented in table 1. 6.0 M AINTENANCE O F RAW DATA AND RECORDS Hard copies o f these data are filed in the AMDT archive. " ' ,ii! 7.0 APPENDICES The appendices are not included with these data. They are filed in the AM DT archive. 7.1 Extraction Logbook -------- 7*2Instrument Runlog----------------- --------------------' .............. - 7 3 Curve and Chromatograms 7.4 Results ASHO10494 LAC 8/29/97 Word Version 6.0 R2148.DOC Page 5 o f 5 1 \3L$~ E ID 129593 3M Environmental Laboratory POAA Analyses in Soil (6/97 Samples) <2* 4 M S ' E ID 129594 ASHO10495 3M Environmental Laboratory Data Transmittal Summary Final copy of the report including this fona and the client cover page is to be given to QAU, U R N and to toe Group Leader. A3 4 M S' E ID 129595 ASHO10496 TMKris Hpa-n"svenl-rSMr. A..n.a..ly..t.ic..a.l.c..n..e.n..u..s.i AdvancedMethod DevelopmentTeam Building 2-3E-9 612-778-6018 {ghansen@miam.com 1.0 Summary Eleven soil sampleswere : listed intaible 1. ' >*~ * * * * Sam ple# aag POAA/kg soiiJ R2382-1 0.119 R2382-2 0.170 R2382-3 748 R2382-4^ 272 R2382-S 80 2382-6 52.8 B2382-7 373 2382-8 39.7 R2382-9 18.0 R2382-l<r 12.7 2382-11 2.27 of dfitecrionAimit ofquantitation is 0.100 mg (100 ppb). 'limit until extraction; extracts were stored at 4 C until analysis. J3 8 M ,r i n n s ! -f" *WMU The samples were stored at 4c ASHO10497 WordVersion 6.0 Lab Bequest #R2382 K2382.DOC 2H 4 ! * ? E ID 129596 with nitrogen and reconstituted with acetonitrile (ACN), filtered, and diluted with water (1:1). After ^ analysis by negative ion ES/MS, the data from the spiked samples was subjected to linear regression and the resulting prediction equation was used to determine the concentration of analyte in the unspiked sample R2382-1 (see Figure 1, attached). The remaining soils were evaluated relative to this curve. Soil from samples R2382-2 through -11 was prepared in the same way. For most samples, dilutions o f the extracts in `a' and `b' vials were necessary. It was also necessary to dilute and reanalyze four samples on 11/04/97. The POAA rnncentratinns ofthese samples were determined by the same method, using a standard curve generated that day (see Figure 2, attached). The method of standard addition assumes there are no interferences in die analysis and that the extraction efficiency ofdie analyte from the matrix is not dependent upon analyte concentration. The first aggnmptfnn is addressed by die selectivity o fboth the extraction and die analysis; die latter has been verified in another study that focuses on a similar matrix. 3.1 Extraction specifics .. The soil samples were extracted with the ISCO 3560 Accelerated Extraction System equipped with ISCO 100DX high pressure syringe pumps according to die following conditions: Extraction solvent: Extraction pressure: Extraction temperature: Restrictor temperature: Static extraction time-1: Dynamic extraction volume-1: Static extraction time-2: Dynamic extraction time-2: Restrictor flow-rate: methanol, HPLC grade 2500 psi 70 C 70 C 40 minutes 15 mL 2 minutes 2 minutes 2.5 mL/min Samples were reconstituted in glass autovials with HPLC-grade ACN and milli-Q water. 3.4 ES/MS Analysis specifics ' <ncs Negative ion ES/MS analysis was performed on a Micromass Platform II atmospheric pres]ire , ionization mass spectrometer running Mass Lynx 2.1 operating system. A HewlettPackard.)IftO ^ ^ u s e d for the autosampler and HPLC system. Mobile phase: ACN/H20 (1:1) Flow rate: 60 pL/min Injection volume: 15pL Cone Voltage = -20 Capillary voltage" -2.56 Source Temperature= 80C Analyzer Vacuum Pressure = 0.000079 mBar Quantitative results were based on the instrumental response generated by monitoring a single ion ^.ptprigtic of die analyte. This type of monitoring minimizes interference by other ions in die extract and increases system sensitivity to the target analyte. 4.0 DATA ANALYSIS By the method ofstandard addition, sample B2382-1 was determined to contain 0.119mg/kg of POAA This value was calculated using die prediction equation resulting from linear regression analysis o f the five-point extracted curve. The coefficient o f determination for the curve is 0.999. Calculations used to determine the concentration of POAA in the soil are shown in Appendix A. The pur"*"" of POAA in samples R2382-2 through R2382-11 wasidetermined by evaluation of ES/MS response relative to die curve generated for sample R2382-1. Calculations are detailed in Appendix A. Word Version 6.0 Lab Request #R2382 R2382.DOC 2 zs 4 A SH 010498 E ID 129597 5.0 CONCLUSION High pressure solvent extraction, ES/MS analysis, and linearregression analysis were used to determine that between 0.119 and 614 mg/kg of POAA is present in the eleven soil samples received from DuPont 6.0 MAINTENANCE OF RAW DATA AND RECORDS Hard copies o fthese data are filed in the AMDT archive. Sample preparation : GML/JJ Analysis: GMMMgh Report preparation: kjh/JJ ASH010499 Word Version 6.0 Lab Request 0R2382 R2382.DOC % 3 4 MS' E ID 129598 R-2382- DuPont Soil Data Appendix A R-2382 POAA Determination Calculations ForDetenninationofindigent" amount inStandardAdditionsCuryeibrR2182cl Step I: From Plot o f Peak Area vs Spiked POAA Standard Concentration determine equation of the linear regression by least squares analysis, for y = mx+ b Example: y = 126000 x +15000 Step 2: Solve linear equation forx, where y = 0, for tire x-intercept ofthe line. Example: 0 = 126000 x +15000 x = -15000/126000 x = -.119 Step 3: indigent amount will equal absolute value ofx. For Soil R-2382 Soils 2-11 Step 1: (Peak Area - Y intercept)/ Response = Diluted Cone, of POAA (ug/ml) PeakArea, intercept, andresponse fiomstd.additions curve calculatedin ugftnl Example: (31000 - 15000yi26000 = 0.127 ug/ml >e Step 2: (Diluted Cone, ofPOAA ug/ml * Dilution Factor) + Indigent Cone. ug/mL= Adjusted Cone, of POAA ug/ml Example: (0.127 ug/ml * 50) +.119 ug/ml = 6.47 ug/ml Step 3: Adjusted Cone, (ug/ml) * 2ml extract/mass (g) * 1000 g/kg * 1mg/1000 ug = Total Cone, ofPOAA (mg/kg) Fvample- 6.47 ug/ml * 2ml extract/1.9999 g * 1000 g/kg * lm g /1000 ug =>6.47 mg/kg POAA Step 4: Add Total Cone, o f POAA determined forPeaks "a* and "b" - Total determined POAA (mg/kg) Example: 6.47 mg/kg+0.43 mg/kg=6.90 mg/kg me A SH 010500 Calculations R2382J03097 8:59 PM11/4/97 *7 $ /*5" E ID 129599 R-2382- DuPont Soil Data Figure-L R-2382-1 Soil- Standard Addition Curve fug/ml extract! Cone, o f POAA Spiked into Soil (ug/ml) 0.05 0.10 0.25 0.50 0.75 File D1Q2897B Peak Area o f Extracts-a 20000 25000 40000 71000 96000 File D1Q2897B File D102897B Peak Area of Total Peak ArealTotal Peak Area Extracts-b (*b) 1000 21000 3000 28000 4000 44000 9000 80000 14000 110000 FileD102897D FileDlQ2897D Peak-a Peak-b 0.05 20000 1000 0.10 27000 3000 0.25 44000 4000 0.50 71000 9000 0.75 94000 14000 21000 30000 48000 80000 108000 Extracted POAA Standard Curve Y-intereept___________________Slope (m) Curve Equation: 15000 126000 X-intercept -0.119 Indigent POAA analyte (Absolute value of X-intercept): 0.119 ug/ml ASH010501 Soil 1 Curve ugml R2382103097 9:00 PM11/4/97 41 E ID 129600 R-2382- DuPont Soil Data Figure.2 R-2382-1 Soil- Standard Addition Curve Analyzed bv ESMS on 11/04/97 Cone, o f POAA Spiked into Soil (ug/ml) 0.05 0.10 0.25 0.50 0.75 FileD110497B Peak Areaof Extracts-a 21000 26000 41000 ...... 67000 94000 FileDll0497B File D l I0497B Peak Area o f Total Peak Area Extracts-b (a+b) 1700 22700 3200 29200 4400 45400 8200 752 13700 107700 Extracted POAA Standard C arve Y-intercept Curve Equation: 16000 Slope (m) 120000 Indigent POAA analyte (Absolute value ofX-intercept): X-intercept -0.133 0.133 ASH010502 11.04 Curve ugrni R2382J03097 8:58 PM11/4/97 E ID 129601 3M Environmental Laboratory Volatiles and Semi-volatiles in Groundwater by Purge aMbit-vo*** Trap Concentration with GC/MS Analyses (6/97 Samplets)t r ' ? 30 4 E ID 129602 ASHO10503 ANALYTICAL SUMMARY Department: 3048 Lab Request: R2148 Project Description: DuPont Water Summary Prepared by: Dennis Seeger, Pace-I Contract Lab: Pace-I Project Lead: Dennis R. Seeger Sample Matrix: Water Date: 10/7/97 Analytical Tests Requested *auesteo Twelve water samples were submitted for identification and quantitation of volatile organic sample components by purge and trap sample concentration with gas chromatography/mass spectrometry (GC/MS) analysis. wceatration ' Analytical Results The results of foe GC/MS analyses are reported in Appendix A. After an- initial analysis of foe undiluted jjwwea m / samples, appropriate dilutions were analyzed for quantitative determinations of trichlorotrifiuoroefoane iaaip& S for q i and trichloroefoene. Where foe calculated concentrations were below foe practical quantitation limit (I suissed cancaat- footnote), foe reported values should be considered as estimates. *be consider! Analytical Summary -^ Gas Chromatography Methods Sum m ary The samples were analyzed using foe GC/MS instrument and sample concentrator conditions listed below. Procedure GC/MSParameters (InstrumentID *Alphie") Samnle Concentrator; Tekmar model 2000 sample concentrator and model 2050 vial autosampler. Trap: Purge time: Purge gas flow: Desorb time: Desorb temp.: Desorb flow: CarbopackB/Carboxen 1000 & 1001 (VocarbSOOO) 11 min. 40 mL/min. 0.5 min. - 270"C 30 mL/min GC column: Restek RTx-624,60 m x 032 mm I D., 1.8 pm film thickness. aO o Ut 2 3\ 4 US' E ID 129603 GC conditions and oven tem perature program: Initial temp.: Oven temp, ramp: Injection port temp.: Interface temp.: Purge B: Head pressure: Split flow: Mass spectrometer: Solvent delay: Electron multiplier: Scan range: Scans per second: Scan threshold: 40C; 2.0 min. hold 12C/min. to 220C; 1.0 min. hold 250C 250C Initial value ON 19.6 psig 30 mL/min. 2.2 min. 2033 volts 35 to 260 amu 2.17 100 Instrument Calibration *' Prior to sample analyses, the analysis o f 30 ng of bromofluorobenzene (BFB) demonstrated die accuracy and resolution of the mass spectrometer. A calibration check standard containing each o f the target analytes at the midpoint concentration o f the most recent five level calibration curve was analyzed to demonstrate acceptable instrument response for target analyte quantitation. A blank water sample water sample was analyzed to demonstrate analytical system cleanliness. All quality control analyses satisfied the criteria specified for analyzing samples by EPA method 8260. C lo s in g This analytical summary and associated analytical results have been reviewed andsafeiapproved for release. Dennis R. Seeger, Project Manager (612) 778-6093 ASH010505 2 3* i M S' E ID 129604 I Appendix A: Report o f Laboratory Analysis I- ) 'l 3 3 5 ^ US' E ID 129605 ASH010506 Method 8260 Results for R2148 Com pound D ichlorodifluorom ethane Chiorom ethane Vinyl Chloride B rom om ethane C h lo ro e th a n e Trichiorofluorom ethane Ethyl Ether Trichlorotrifluoroethane Acrolein 1,1 -D ic h !o ro e th e n e A cetone Isopropyl Alcohol Carbon Disulfide Allyl Chloride M ethylene Chloride tert-Butyl Alcohol tert-M ethyl Butyl Ether tra n s -1 ,2 -D ic h lo ro e th e n e A crylo n itrile Isopropyl E ther 1 ,1 -D ic h lo ro e th a n e 2 ,2 -D ic h lo ro p ro p a n e Ethyl Acetate c is -1 ,2 -D ic h lo ro e th e n e 2 -B u ta n o n e 2-B u ta n o l B rom ochlorom ethane Tetrahydrofuran Chloroform 1 ,1 ,1 -T ric h lo ro e th a n e Carbon Tetrachloride 1,1 -Dichloropropene Isobutanol Benzene 1 ,2 -D ic h lo ro e th a n e n-Butanol Trichloroethene 1 ,2 -D ich lo ro p ro p an e D ibrom om ethane B rom odichlorom ethane 2-Chloroethyl Vinyl Ether 2 -N itro p ro p a n e c is -1 ,3-D ich lo ro p ro p ene 4-M ethyl-2-pentanone T o lu e n e 4-M ethyl-2-Pentanol PRL ! (u g /L )! R2148-1 10 i 10 } io ; 10 10 ! 10 j 5i 5i 40 1 5! 10 i 60 ! 5' 5i 5! 20 ! 5; 5i 40 J 5! 5i 5! 10 ' 5i 10 ! 60 ~ ! 5' 10 i 5! 5! 5i 5! 100 ! 5i 5i 100 J 5J 5i 5! 5| 10 i 10 i 5} 10 \ 5i 60 ! 820 2 .7 J 59 *- - 1.8 J - - - S a m p le C o n c e n tra tio n s (u g /L ) R 2148-2 R 2148-3 R 2148-4 R 2148-5 - 730 - 10 2 .9 J 49 - - - 1.5 J - ,- - - 16 1600 - - 140 .- - - 18 1500 - 3 .7 J - . 150 - '- 26 2300 7 .8 J 2 .3 J 2.9*0 3 .3 J 5 .5 14 520 - R 2148-6 26 2400 - 8.0 J - 2 .7 J - 3 .0 J - 3 .5 J - 5 .9 14 570 - - ASHO10507 PR L - Practical Quantitation Limit J - T h e concentration is below the practical quantitation lim it Page 4 3V ^ U S E ID 129606 Method 8260Results for R2148 PRL ! Com pound (ugfL)l R2148-1 tran s-1 ,3 -D ic h lo ro p ro p e n e 1 ,1 ,2 -T ric h lo ro e th a n e Tetrachloroethene 1 ,3 -D ic h lo ro p ro p a n e 2 -H e x a n o n e D ibrom ochlorom ethane 1,2-Dibrom oethane C h lo ro b en zen e E th y lb e n z e n e 1 ,1 ,1 ,2 -T e tra c h lo ro e th a n e m & p-Xylene o -X y le n e S ty re n e Bromoform isopropyl benzene C y c lo h e x a n o n e 1 ,1 ,2 ,2 -T e tra c h lo ro e th a n e 5i 5J 5* 5l 10 ; 5* 5i 5! 5| 5; 5! 5! 5J 5i 5! 60 J 5i 3.6 J - B rom obenzene n-Propyl benzene 1,2 ,3 -T ric h lo ro p ro p a n e 5i 5i 5| - 2 -C h lo ro to lu e n e 1,3,5-Trim elhylbenzene 4 -C h lo ro to lu e n e tert-Butyl benzene 1,2,4-Trim ethyIbenzene s e c -B u ty lb e n ze n e p-lsopropyltofuene 1,3 -D ic h lo ro b e n ze n e 1,4 -D ic h lo ro b e n ze n e n-Butyl benzene 1,2 -D ic h lo ro b e n ze n e 1,2-Dibrom o-3-Chloropropane 1,2 ,4 -T n c h lo ro b e n z e n e H e xach lo ro b u tad ien e N a p h th a le n e 1 ,2 ,3 -T n c h lo ro b e n z e n e 5 5! 5! 5; 5i 5! 5! 5i 5\ 5| 5J 5i 5! 5* 5i 5! - S a m p le C o n c e n tra tio n s (u g /L ) R 2148-2 R 2148-3 R 2148-4 R2148-S 1.7 J - - " -. - - - 1.1 J 1.8 J - - -. * - 5 '" - " - " R 2 1 4 8 -S 5 .2 " " - " " " - -- .- ASHO10508 PRL - Practical Quantitation Limit J - T he concentration is below the practical quantitation lim it Page 5 354 E ID 129607 Method 8260 Results fo r R2148 Com pound Dichlorodifluorom ethane Chlorom ethane Vinyl Chloride Brom om ethane C h lo ro e th a n e Trichlorafiuorom ethane Ethyl Ether T richlorotrifluoroethane Acrolein 1 ,1 -D ic h lo ro e th e n e A cetone Isopropyl Alcohol Carbon Disulfide Allyl C hloride M ethylene Chloride tert-Butyl Alcohol tert-M ethyl Butyl Ether trans-1,2-D ichloroethene A crylo n itrile Isopropyl Ether 1 ,1 -D ic h to ro e th a n e 2 ,2 -D ic h lo ro p ro p a n e Ethyl A cetate cis-1,2-D ichloroethene 2 -B u ta n o n e 2-B u ta n o l B rom ochtorom ethane Tetrahydrofuran C hloroform 1 ,1 ,1 -T ric h lo ro e th a n e Carbon Tetrachloride 1,1 -Dichloropropene Isobutanol Benzene 1 ,2 -D ic h lo ro e th a n e n -B u ta n o l Trichloroethene 1 ,2 -D ic h lo ro p ro p a n e Dibrom om ethane B rom odichlorom ethane 2-Chloroethyl Vinyl E ther 2 -N itro p ro p a n e c is -1 ,3 -D ic h fo ro p ro p e n e 4-M ethyl-2-pentanone T o lu e n e 4-M ethyl-2-Pentanol PRL ! (u g /L )! R 2148-7 10 i 10 ! 10 J 10 i 10 ! 10 * 5 5i 40 ! 5{ 10 i 60 [ 5J 5 5! 20 ! 5' 5! 40 \ 5! 5i s! 10 ; 5i 10 ! 60 ! 5! 10 i 5! 5! 5i 5! 100 ' 5! 5i 100 ! 5! 5i 5! 5i 10 i 10 ! 5i 10 ; 5i 60 j 5 .9 - 760 . 6.7 J - . . - - -' - 5 .8 . 37 6 .3 - - 81 - - - - - S a m p le C o n c e n tra tio n s (u g /L ) R 2148-8 R 2148-9 R2148-1Q R2148-11 R 2148-12 - * m. .. . 670 _ 10 . - - 5 .9 39 6 .2 . - - m - m- 130 140 3 .2 J -. 2* - " " ' . ;r .- .- -- -- - 2.7 J 2.6 ir o - _ mranone _- 13 16 . 5.8 . - . - _ 1.8 J * 5.6 J . _ _ _'_ _ . - .. _ 66 . --- _. -. _ - - '- . --- -- . ---- _ ---- - PRL - Practical Quantitation Limit J - The concentration is below the practical quantitation lim it Page 6 ASH010509 34 ^ U S E ID 129608 Method 8260 Results for R2148 PRL ! Com pound (u g /L )l R 2148-7 tran s-1,3 -D ic h lo ro p ro p e n e 1,1 ,2 -T richloroethane Tetrachloroethene 1 ,3 -D ic h lo ro p ro p a n e 2-H exanone D ibrom ochlorom ethane 1,2-Dibrom oethane C h lo ro b en zen e E th y lb e n ze n e 1 ,1 ,1 ,2 -T e tra c h lo ro e th a n e m & p-Xylene o -X y le n e S ty re n e Bromoform Isopropyl benzene C y c lo h exan o n e 1 ,1 ,2 ,2 -T e tra c h Io ro e th a n e B ro m o ben zen e n-Propyl benzene 1 ,2,3-Trichloropropane 2 -C h lo ro to lu e n e 1,3,5-Trim ethylbenzene 4 -C h lo ro to lu e n e tert-Butyl benzene 1,2,4-Trim ethy (benzene s e c -B u tylb en zen e p-lsopropyltoluene 1 ,3 -D ic h lo ro b e n ze n e 1 ,4 -D ic h lo ro b e n ze n e n-Butyl benzene 1 ,2 -D ic h lo ro b e n ze n e 1,2-Dibrom o-3-Chloropropane 1 ,2 ,4 -T ric h lo ro b e n z e n e H e xach lo ro b u tad ien e N a p h th alen e 1,2,3-Trichlorobenzene 5! - 5J - 5 ' 4 .8 J 5i - 10 J - 5j - 5i - 5! - 5! - 5i - 5! 51 - 5! 5i 5! 60 J 5i - - 5! 5{ 5J 5i 5! 6! - 5! 5i 5| 5J 5i 5! 5{ 5J - 5i 5{ 5' 5i 5j - Sample Concentrations (ug/L) R2148-8 R 2148-9 R2148-10 R2148-11 R 2148-12 5 .8 ASH010510 PRL - Practical Quantitation Limit J - The concentration is below the practical quantitation lim it Page 7 37 4 US' E ID 129609 3M Environmental Laboratory Volatiles by AED (5/97 Samples) 32 i n s E ID 129610 ASH010511 3M Environmental Laboratory Data Transm il Summary Preliminary (F i (circle one) Lab Request#; Date Received: 3M Study #: `Z 'W t e S S n L n t / i v Contract LaboraioryW Sponsor or Client: Representative Name Company Name p(A fo A 't Company Address Phone Project Lead: Nam e /Phone K |4#/vl ^6vi / Group Leader: Nam e / Phone JDJohnson/85294 Analyte(s) or Test Method #: PO A A Sample Matrix: \})ca ( So 1 1 Analysis Dates: T- 0 Analyst(s): $ Ml ! U#" Author: SM> IlV" ' Data Reviewed by: Project Lead (or designee): James D . Johnson (or designee): JDJ: QAU (Archives): LIKN System: Project Manager: (ug. S e\.cV\ Others (List Recipients /A d d re ss / Phone lF A X ) Sent by: / Date ASHQ10512 A copy of the report including this form and the client cover page is to be given to QAU, U RN and to the Group Leader. 3, J E ID 129611 h r* e i 3M Environm ental Laboratory - Advanced Method Development Team Contact: K ris H ansen B uilding 02-3E-09 612-778-6018 kjhansen@ m m ra.com Final R eport - Lab R equest R2008 D uP ont W ater and S oil Sam ples 07 November 1997 1.0 SUM M ARY Five water samples and eight soil samples from DuPont w |t|e analyzed fejA e ? ..;.: i. -J'. . presence o f fluorine, chlorine, bromine, carbon, and hydrogen using headspace sampling ' and gas chromatography coupled with an atomic emission detector (GC/AED). The o mtb m a sam ples were analyzed on two different columns, a DB-5 and a DB-624. Standard curves w e st colon were generated during each analysis. Very little was seen in the samples and the <. compounds that were detected existed at levels below the lowest standard. si? 2.0 INTRODUCTION Five w # e r samples and eight soil^samples were received flom ^DuPont under request #2008. The samples were to be analyzed for the presence o f perfluorooctanoic acid anion (POAA). However, since it is not volatile, POAA was not detected using GC/AED. A headspace sampler was used to introduce any volatile or sem i-volatile components o f the samples into the GC/AED. The samples were monitored for fluorine (F690), bromine (Br478), chlorine (C1479), hydrogen (H486), and carbon (C496). eight" I s w^ , fa 3.0 TEST M ATERIALS The five water samples were labeled on large amber glass bottles as follows: Lab Request # R 2008-1 R20Q8-2 R2Q08-3 R 2008-4 R 2008-5 # o f Bottles 1 1 1 1 1 __________________ Sample Description_________________ DuPont Wash. W orks Ranney W ell FC143 1:48 pm DuPont Wash. Works Ranney W ell FC143 1:48 pm DuPont Wash. Works <D Ranney W ell FC143 1:50 pm DuPont Wash. W tirks RanneyW ell FC 143 1:50 pm D I Water UIoU--)*i 3M Environmental Laboratory, Lab Request R20Q8 Page 1 o f5 YO ^ E ID 129612 The eight soil samples were labeled on. 1L plastic containers as follows: Lab Request # # ofContainers __________________ Sample Description ______________ R2008-6 8 DuPont Washington Dirt 5/30/97 11:00 A ll samples were refrigerated at approximately 4C until sample preparation and analysis. 4.0 EXPERIM ENTAL-OVERVIEW Sample Preparation The water samples were prepared by pipetting lOmL o f each sample into 20mL glass headspace vials. Each sample was "salted" by adding approximately 2 to 3 grams o f sodium chloride (this was done to increase the ionic strength o f the solution). The soil samples were prepared by transferring 10 0.5 grams o f soil (weight* recorded) into headspace vials. The soil samples were not salted. The standard curves were prepared using two differenflstandards, para- bromofluorobenzene (p-BFB) and ortho-dichlorobenzene (o-DCB). The p-BFB was prepared in acetone and the o-DCB was prepared in methanol. The standards were spiked into lOmL Milli-Q water at levels o f 25pl, 5Gpl, and lOOpl. Acetone and methanol spikes (lOOpl each) in lOmL Milli-Q as well as a lOmL Milli-Q blank were also analyzed. Since all eight containers o f soil were the same, three o f the eight samples were used to make a standard curve. These were spiked exactly as the waters-were. One soil t sample was spiked with acetone and methanol, leaving four icpntainei^ pfisoil to be treated as "samples." "* * ' Because two different columns were used and all five elements could not be monitored simultaneously, the water and soil samples were prepared four separate times. Each time a standard curve was generated. When just F690 was monitored, the standard curve was generated based on p-BFB. When all other elements were monitored, two standard curves were generated, using p-BFB and o-DCB. ASH010514 Headspace Sampler. Hewlett Packard 19395A Settings: Bath Temperature 85C Valve/Loop Temperature 140C Probe in, t = l second Vial Pressurized, t = 3 seconds to 13 seconds Vent/Fill Loop, t = 14 seconds to 19 seconds Inject into GC, t = 20 seconds to 50 seconds Probe out, t= 51 seconds Packed column on vent 3M Environmental Laboratory, Lab Request R2008 ''i; Page 2 of 5 V/ 4 /% 6~ E ID 129613 Gas Chromatograph: Hewlett Packard 5890 Series II Column: DB-5 (J&W Scientific) 30 x .25 x .25, serial # 2633586 Oven Program: 1 min @ 60, lQ/min to 300 for 5 min (F690) 1 min @ 40, 107min to 300 for 5 min Column: DB-624 (J&W Scientific) 30 x .32 x 1.8, serial # 5812142 Oven Program: 1 min @ 40, lQ7min to 200 for 5 min Injection Port: 225C, split Atomic Emission Detector: Hewlett Packard 5921A "Flo" GC Block/Transfer Line Temp 275 Cavity Block Temp 275 5.0 DATA ANALYSIS SAMPLERESULTS: Lab Request # Column_______Element__________________ Results*.. R2008-1 DB-5 F no peaks detected R208-2 DB-5 F no peaks detected R2008-3 DB-5 F no peaks detected R2008-4 DB-5 F no peaks detected R2008-5 DB-5 F no peaks detected R2008-6 DB-5 F no peaks detected 'minimum quantitation limit: 0.280 ppm F in water, 0.282 ppm F in soil Lab Request # Column Elements Results' R2008-1 DB-5 H, C, Br, Cl no peaks detected R2008-2 DB-5 H, C, Br, Cl no peaks detected R2008-3 DB-5 H, C, Br, Cl no peaks detected R2008-4 DB-5 H, C, Br, Cl no peaks detected R2008-5 DB-5 H,C,Br,Cl no peaks detected R2008-6 DB-5 H, C, Br, Cl no peaks detected 'minimum quantitation limits: 1.176 ppm Br in water, 1.220 ppm Br in soil . linuss- 1.408 ppm Cl in water, 1.461 ppm Cl in soil Lab Request # Column Element Results* R2Q08-1 DB-624 F no peaks detected R2008-2 DB-624 F no peaks detected R2008-3 DB-624 F no peaks detected R2008-4 DB-624 F no peaks detected R2008-5 DB-624 F no peaks detected R2008-6 DB-624 F. no peaks detected 'minimum quantitation limit: 0.280 ppm F in water, 0.282 ppm F in soil ASH010515 3M Environmental Laboratory, Lab Request R2008 Page 3 of 5 VA 4 MS' EID129614 Lab Request# Column Elements Results* R2008-1 DB-624 H, C, Br, Cl peaks detected on Cl channel (below mql), no peaks on other channels R2008-2 DB-624 H, C, Br, Cl peaks detected on Cl channel (below mql), no peaks on otherchannels R2008-3 DB-624 H, C, Br, 1 peaks detected on Cl channel (below mql), no peaks on other channels R2008-4 DB-624 H, C, Br, Cl peaks detected on Cl channel (below mql), no peaks on other channels R2008-5 DB-624 H, C, Br, Cl no peaks detected R2008-6 DB-624 H, C, Br, Cl no peaks detected minimum quantitation limits: 1.176 ppm Br in water, 1.187 ppm Br in soil 1.408 ppm Cl in water, 1.253 ppm Cl in soil STANDARD CURVES: The following are examples o f standard curves taken from die analyses: F Curve for DuPont Soil (DB-5) Cl Curve for DuPont W ater (DB-824) ASH010516 3M Environmental Laboratory, Lab Request R2008 Page 4 of 5 H3 4 o r EID129615 6.0 CONCLUSION Qualitative analysis of DuPont o r and E S ta tue oamnles. Cl-contaimng compounds were found using tne u o -o s , S fiS w S i **>*, *-- n oam itS jocan se they were present in levels W ow the lowest standard. " n0` 7.0 MAINTENANCE OF RAW DATA H ard copies o f the data are filed in th e A M DT archive. SE M iller 110797 ASH010517 3M Environmental Laboratory, Lab Request R2008 Page 5 o f5 wi EID 129616 3 M E nviro n m en tal Laboratory Volatiles by AED (6/97 Samples) H S '4 1 2 S~ EID 129617 ASH010518 3M Environmental Laboratory D ata T ransm ittal Sum m ary Prelim inary A finaly(cfrc/e one) Lab Request#: P O .I4S Date Received: 3M Study#: Contract Laboratory # Sponsor or Client: RepresentativeName CompanyName Pu-Powir Company Address Phone Project Lead: Name/Phone (-1-1c*jv\& sy\J Group Leader: Name / Phone JDJohnson/85294 l a l y S o S s t M ^ d S ^ u ^ ? C ^ K ^ 4 ^ i ^ ,' iuSamp.le Mw atrix: vva.+, ev' ` Analysis Dates: (fa c/tT')'}- Analyst(s): SFMjHev 7?. (i/olA-bltS +fe*yii-w lattile Author: SEMiItev' Data Reviewed by: PA fttH'lW l tl 1 v T c\~} Project Lead (or designee): ; James D. Johnson (or designee): JDJ: QAU (Archives): LIRN System: Project Manager: S iaL%IAc4o___________________ ___ Others (List R ecipients / A ddress / P hone / FAX) ASH010519 A copy of the report including this form and the client cover page is to be given to QAU, LIRN and to the Gronp Leader. 4 / s' EID 129618 3M E nvironm ental L aboratory-A dvanced M ethod D evelopm ent T eam Contact: K ris Hansen Building 2-3E-89 612-778-6018 kjhansen@ nunm .com Final Report - Lab Request R2148 DuPont W ater Samples 07 November 1997 1.0 SUMMARY Twelve water samples were received from DuPont on July 2,1997. The samp|siS , were analyzed for:the presence of fluorine, chlorine, bromine, carlK)n, :an^;ihydj:qgepi . ,,,, , ^sing headspara sampling and gas chromatography coupled wi& a n - *' - detector (GC/AED). The samples were analyzed on two different colunmsiiaiDB-5 u DB-624. Standard curves ofno less than R2=0.99 were generated during each analysis , - Column Samples DB-5 1-8 Results Description halogenated organics Levefe&Bie* .setts 0.23-1.3 ppmF, 0.29-0.86 ppm C, 0.39-2.5 ppm Cl DB-5 9-10 low levelsofhalogenated organics 0.32-0.35 ppm C, F andl areas les?. iaym mUt than low standard response DB-5 11-12 C only detected C area less than low standard response DB-624 1-8 halogenated organics 0.23-1.1 ppm F, 0.24-0.50 ppm C, 0.45-3.6 ppm Cl DB-624 9-10 low levels ofhalogenated organics 0.082 ppm F (#10), F, C, and Cl areas less than low standard response .. mt, I j DB-624 11-12 C and F only detected Cand F areas less than low standard response reported as total ppmper sample Bromine was not detected in any of die samples on either column. Hydrogen was detected in four samples on the DB-5 and in one sample on the DB-624. ASHO10520 3M Environmental Laboratory, Lab RequestR2148 Page l of 8 V7 4 U S ' EID 129619 1.y a r s s s o STSM , !>-o und ft! i W , i i5 apm ) a 2.0 INTRODUCTION Twelve monitoring well water samples were received from DuPont under lab request R2148. The samples were to be analyzed for die presence of organofluorines. A headspace samplerwas used to introduce any volatile or semi-volatile components of the samples into a GC/AED. The samples were monitored for fluorine (F690), bromine (Br478), chlorine (0479), carbon (C496), andhydrogen (H486). 3.0 TEST MATERIALS The water samples were received in amber glass bottles and labeled as follows: 3M Lab Request# Sample Description R2148-1 MW-1 1 o f 2 R2148-2 MW-1 2 o f 2 R2148-3 MW-2 1 of 2 R2148-4 MW-2 2 of 2 R2148-5 MW-3 1 of 2 5 R2148-6 MW-3 2 o f 2 R2148-7 MW-4 1 o f 2 R2148-8 MW-4 2 of 2 R2148-9 ' MW-5 1 o f 2 R2148-10 MW-5 2 o f 2 R2148-11 MW-6 1 o f2 R248-12 MW-6 2 of 2 i All samples were refrigerated at approximately 4C until sample preparation and analysis. 4.0 EXPERIMENTAL-OVERVIEW Sam ple Preparation The water samples were prepared by transferring approximately lOmL o f each sample into tared headspace vials containing approximately 4 0.1 grams of sodium chloride. The vials were rewieghed to get the weight o f die water. Tins was done instead of pipetting an exact volume so that exposure to air was kept to a minimum, and the possibility of losing volatile components reduced. Standard curves were prepared using two different standards, para- bromofluorobenzene (p-BFB) and ortho-dichlorobenzene (o-DCB). Two standard curves were necessary so calibration curves could be generated for all elements o f interest: fluorine, carbon, hydrogen, and bromine from p-BFB; carbon, hydrogen, and chlorine from o-DCB. The p-BFB was prepared in acetone and the o-DCB was prepared in methanol. The standards were spiked into lOmL Milli-Q water (salted) at levels o f 5pL, 3M Environmental Laboratory, Lab Request R2148 Page 2 o f 8 H8 M S' ASHO10521 EID 129620 2SjxL, 50pL, 75pL, and lOQpL. Acetone and methanol spikes (100pL each) in lOmL Milli-Q as well as a lOmL Milli-Q blank were also analyzed. The combination o f two columns (die DB-5 is good for late eluting compounds and the DB-624 is used to separate compounds that elute relatively quickly) yielded a thorough analysis for each sample. Because two different columns were used and all five elements could not be monitored simultaneously, the samples were prepared four separate times. When just F690 was monitored, the standard curve was generated based on pBFB. When all other elements were monitored, two standard curves were generated, using both p-BFB and o-DCB. The final results for fluorine, carbon, hydrogen, and bormine were based on p-BFB. The chlorine curve was based on o-DCB. Instrumentation and Operating Conditions Headspace Sampler: Hewlett Packard 1939SA Settings: Bath Temperature 85C Valve/Loop Temperature 140C Probe in ,t= 1 second Vial Pressurized, t = 3 seconds to 13 seconds Vent/Fill Loop, t = 14 seconds to 19 seconds Inject into GC, t = 20 seconds to SOseconds Probe out, t = 51 seconds Packed column on vent Gas Chromatograph: Hewlett Packard 5890 Series II Column: DB-5 (J&W Scientific) 30m x .25mm x .25pm, serial #2633586 Oven Program: 1 min @ 40, 10/min to 300 for 3 min Column: DB-624 (J&W Scientific) 30m x .32mm x 1.8pm, serial #5812142 Oven Program: 1 min @ 40, I0/minto 240 for 5 min Injection Port: 225C, split Atomic Emission Detector: Hewlett Packard 5921A "Flo" jasjw M iM tail rscsasa ir.ieaiific) 30in , :V WfVjttM 3M Environmental Laboratory, Lab Request R2148 > CO Wo toOo) Page 3 o f8 11 i U S' EID 129621 5.0 DATA ANALYSIS SAMPLEANALYSIS: Column: D B -5 L a b R equest# R 2148-1 R 2 1 4 8 -2 R 2148-3 R 2148-4 R 2 1 4 8 -5 R 2 148-6 R 21 4 8 -7 R 2148-8 R 21 4 8 -9 R 2 1 4 8 -1 0 R 2 1 48-11 R 2 148-12 *low standard concentration: 0.0S6 ppm F F690* 023 ppm, 1peak < low std. response 0.23 ppm, 1peak < low std. response 0.079ppm, 0.55ppm 0.34ppm, 1peak < low std. response 0.26ppm, 0.57ppm 0.39ppm, 0.90ppm 0.066ppm, 0.21ppm 0.075ppm, 022ppm 2 peaks < low std. response 2 peaks < low std. response none detected none detected C olum n: DB-624 Lab R e q u e st# R 2 1 4 8 -1 R 2 1 4 8 -2 R 2 1 4 8 -3 R 21 4 8 -4 R 2148-5 R 21 4 8 -6 R 2 1 4 8 -7 R 2 1 4 8 -8 R 2 1 4 8 -9 R 2148-10 R 2148-11 F69Q* 026 ppm F, 3peaks < low std. response *'-# 0.23ppm F, 3peaks < low std. response * 0.075 ppm, 0.44ppm F,2 peaks < low std. response 0.074ppm, 0.42ppm F, 2peaks < low std. response 0.086 ppm, 0.27ppm, 0.70 ppm F,3peaks <low std. response 0.080 ppm, 0.23 ppm, 0.59 ppm F,3peaks <low std. response 0.087ppm, 020ppm F,2peaks<low std response 0.083ppm, 0.16ppm F, 2peaks <low std. response 5peaks <low std.response 0.082ppm F,4 peaks <low std response 1 peak < low std. response R 2 1 4 8 -1 2 none detected *same lowstandardconcentration as above ASH010523 3M Environmental Laboratory, Lab Request R2148 Page 4 of 8 So e 5~ EID 129622 Column: DB-5 Lab Request # R2148-1 C496* 1peak < low std. response H486* none detected 0479* 0.39 ppm R2148-2 R2148-3 R2148-4 R2148-5 l peak < low std. response 0.43 ppm none detected none detected 0.39 ppm, 3 peaks < low std. response 0.32 ppm, 0.42 ppm, 2 peaks < low std. response 1peak < low std. response 0.13 ppm, 2 peaks < low std. response 0.46 ppm 12 ppm, 2 peaks < low std. response 1.0 ppm,2 peaks < low std. response 0.43 ppm, 1.2 ppm, 031 ppm R2148-6 0.36 ppm, 0.50 ppm, 2 peaks < low std. response 0.078 ppm, 2 pedes < low std. response 0.54 ppm, 1.6 ppm, 0.40 ppm R2148-7 0.29 ppm, 2 peaks < low 1 peak < low std. response std. response 0.46 ppm, 2 peaks < low std. response R2148-8 2 peaks < low std. response none detected 0.46 ppm, 2 peaks < low std response R2148-9 0.32 ppm, 2 peaks < low none detected 2 peaks < low std. std. response response R2148-10 0.35 ppm,2 peaks < low none detected 2 peaks < low std. std. response response R2148-11 1peak < low std. response none detected none detected R2148-12 l peak < low std. response none detected none detected low standard concentrations: 0.21 ppm C, 0.060 ppm H, 0.28 ppm Cl, 0.24 ppm Br Br478* none detected none detected none detected none detected none detected none detected none detected none detected none detected none detected ' none dettteUiiifV! none detected ASHO10524 3M Environmental Laboratory, Lab Request R2148 4 Page 5 o f8 Si i U S ' EID 129623 nomme;. Column: DB-624 Lab R equest# R2148-1 C496* peak < tow std. response R2148-2 l peak< low std. response R2148-3 0.24 ppm, 1peak < low std. response R2148-4 1peak <low std. response R2148-5 0.34 ppm, 3 peaks < low std. response R2148-6 0.S0 ppm, 3 peaks < low std. response R2148-7 2 peaks < low std. response R2148-8 2 peaks< low std. response R2148-9 1peak < low std. response R2148-10 1peak < low std. response R2148-11 1peak< low std. response R2148-12 1peak< low std. response same low standard concentrations as above H486* none detected none detected none detected nonedetected none detected 1peak < low std. response none detected none detected none detected none detected none detected none detected CI479* 0.57 ppm B r4 7 8 * none detected 0.45 ppm none detected 12 ppm none detected 1.0 ppm none detected 0.40 ppm, 1.6 ppm, 0.42 ppm 0.57 ppm, 2.4 ppm, 0.58 ppm, 1 peak < low std. response 0.45 ppm, 1peak < low std. response 0.66 ppm, 2 peaks < lowstd. response 3 peaks < low std. response 3 peaks < low std. response none detected none detected none detected none detected none detected none detected none detected none detected none detected none detected Sif, .nr-iMtwm m All results were normalized, assuming the density of water = Ig/mL. ASHO10525 3M Environmental Laboratory, Lab Request R2148 Page 6 o f8 SZ 4 MST EID 129624 STANDARD CURVES: Example o f a standard curve from the analysis (all standard curves had R2 of 0.99 or greater): 6.0 CONCLUSIONS . Twelve water samples were analyzed on two different columns with a GC/AED. More fluorine was detected using the DB-624 than the DB-5; in the DB-5 analysis, more carbon, hydrogen, and chlorine were detected. All o f the samples evidence o f at least one oeseoiea of the elements targeted. Many peaks were detected but not quantitated because the peak o peaks f dais; areawas less than the low standard response for that element. reasonse fo - 7.0 MAINTENANCE OF RAW DATA * * ATA Copies of all datawill be filed in the AMDT archive. " M: 8.0 APPENDICES . Appendix A: Chromatogram of sample 6 (MW-3 2 of 2) F690 DB-624 SEMiUer 110797 3M Environmental Laboratory, Lab Request R2I48 Page 7 o f 8 >cz> fot--f*i o 0to\ S3 <=t U S EID 129625 Appendix A: Chromatogram o f sample 6 (MW-3 2 o f2) F690 1 DB-624 3M Environmental Laboratory, Lab RequestR2148 Page 8 of 8 > CO oa a tUooi f i 4 us EXD129626 m Environmental Laboratory Total Fluoride In Soil (6/97 Samples) S F H MS' EID 129627 ASH010528 3M Environmental Laboratory Data Transmittal Summary Preliminary / Final (circle one) Lab Request#: R2382 Date Received: 06/06/97 ^ ^ ^ 3 M S tu d y # ^ ^ ^ Contract Laboratory # Sponsor or Client: Roger Zipfel Dupont Washington Works Plant Project Lead: Name / Phone Kris Hansen / (612) 778-6018 Analyte(s) or Test Method #: Total Fluoride Sample Matrix: Soil Analysis Dates: 9/29/97 through 10/01/97 Analyst(s): Daniel Howman Author: Daniel Howman Data Reviewed by: Kris Hansen rouan Reviewer: James D. Johnson QAU (Archives): Rich Youngblom LIRN System: Denise Appleton Project Manager: Sue Beach Others (List R ecip ien ts / A d d ress / P h o n e /F A X ) Project Lead: Kris Hansen . DRH / 11-07-97 Sent by: / Date DRH /11-07-97 ASHO10529 A copy of the report including this form and the client cover page is to be given to QAU, LIRN and to the Group Leader. SI 12 EID 129628 3M Environmental Laboratory - Advanced Method Development Team Kris Hansen - Sr. Analytical Chemist Advanced Method Development Team Building 2-3E-09 612-778-6018 kjhansen@mmm.com Final Report Determination o f Total Fluoride in Soil Laboratory Request R23S2 1.0 SUMMARY Eleven soil samples from Dupont, Washington Works Plant were submitted to the Environmental Laboratory for analysis of total fluoride. The samples were submitted under Lab Request No. R2382, samples 1 through 11. EE nalysis The samples were analyzed using an Orion EA 940 Expandable Ion Analyzer after combustion using a Dohrmann DX2000 Organic Halide Analyzer modified for fluoride analysis. The following table contains a summary of the results. The Total Fluoride values are the average o fthree replicates of the same sample, and are given in the table along with the standard deviation ofthe three replicates. Total fluoride is defined as file concentration of F- measured following complete combustion of thesample. i * : 'me aiawes. ..-tv. 07*. , i' a ; * w: / Date 2.0 TEST MATERIALS The soil samples were sent from Dupont, Washington Works Plant, andreceived at file Environmental Laboratory in St. Paul on 6/6/97. The samples were logged in under Lab Request R2382, samples l through 11. Samples were refrigerated at 4C until analysis. A nalyst/D ate Daniel Howman /10-1-97 Page 1of7 S? > CO fo--f*i oVu>i o EID 129629 3.0 INSTRUMENTATION A. Dohrmann DX2000 Organic Halide Analyzer modified for fluoride analysis OPERATING CONDITIONS Combustiontube temperature= 950 C Oxygen and Helium flow=50 cc/minute Vaporization/Drying time = 240 seconds Bake time = 300 seconds Collection fluid = 3.0 mL of 1:1 TISAB/Milli-Q H20 B. Orion EA940 Expandable Ion Analyzer with Orion 9609BN Combination Fluoride Electrode 4.0 EXPERIMENTAL OVERVIEW: Total Fluoride Determination 4.1 Standards A standard curve was prepared from Amonium Perfluorooctanoate (POAA) stock solution (S397-420) at the following concentrations: 25,50, 250,500,1000 ppm POAA in MeOH. For each sample, 0.2mL of soil was extracted thermally with the Dohrmann DX2000 Organic Halide Analyzer. The EOX-Liquids computerprogramwas used for the standard extraction. Standards were prepared and analyzed in triplicate. The extraction products ofthe standards were collected in 3 mL of 1:1 TISAB n/H20 . The collection vial was placed so that the tip of the combustion tube was in the collection fluid. Gases released during pyrolysis bubble through tire collection fluid; the F- partitions into the collection fluid. . The concentration of fluoride in the collection vial was determined by direct measurement with the Orion EA940 Expandable Ion Analyzer with 4 Orion 9609BN Combination Fluoride Electrode. The Orion EA94Q was calibrated by direct measurement with no blank correction, using standards with a concentration of 0.1,0.5,1.0,1.5,5.0 ppmF. Standards were , prepared using Coming Sodium Fluoride (TN-A-Q572) and diluted in 1:1 TISAB li/H20 . ..` * ASH010531 4.2 Blanks Prior to analysis of the samples and standards, O.lmL of Milli-Q was extracted on the DohrmannDX2000 Halide Analyzer in the same way as the standards to insure the system was free of any fluoride contamination. Total fluoride was then measured on the Orion EA940. A n alyst/D ate Daniel Howman / 10-1-97 Page 2of7 8 $ MS' EID 129630 4.3 Samples For cample analysis, 0.02 gramsamples ofsoil were extracted in triplicate on the DohrmannDX-20Q0 in the same way as die standards. The EOXSolids rnm pnter programwas used for sample extraction. The ornrintratinn of fluoride extractedwas determinedby direct measurement with die Orion EA940. 5.0 DATA ANALYSIS: Total Fluoride determination 5.1 Standards A standard curve was developed using the POAA standard solutions (see appendix). The fluoride content of POAAis 66.10%, thus, the concentration of fluoride in die standards was determined by multiplying the concentration of POAA by 66.10%. Concentration of F- = (Standard concentration) * (0.661) Concentration of F- = (25ppm POAA) * (0.661) Concentration of F- in 25ppm POAA = 16.5ppm These calculated values were plotted and a standard curve calculated using linearregression. The equation ofthe regression is y = 0.0Q67x - 0.1061. A linear correlation coefficient o f0.9962 was obtained for the standard range o f25 -1000 ppm APO. 5.2 Blanks No further analysis was done on the blanks. nmm n 5.3 Samples The Total Fluoride in the samples is reported as the average of triplicate sample analysis using the linear regression equationto correct for extraction efficiency (see appendix). CalculatedF- (mg/L) = (Meter Reading+ Intercept) / Slope Calculated F- (mg/L) = (Meter Reading ofR2382-1-1 + 0.1061) / (0.0067) CalculatedF- (mg/L) --(0.8047 + 0.1061) / (0.0067) Calculated F- of R2382-1-1 = 136mg/L Calculated F- (mg/Kg) = (Calculated F- (mg/L)) * (Collection Volume) / (Sample Weight) Calculated F- (mg/Kg) = (136mg/L) * (3ml)/(0.0203grams) Calculated F- (mg/Kg) = 2Q10Qmg/Kg Analysis blanks and calibrationcheck standards were analyzed periodically to verify that the system continued to operate properly. Analyst / Date Daniel Howman/10-1-97 Page 3of7 SI ASH010532 EID 129631 6.0 CONCLUSIONS Triplicate analysis o f the pyrolysis products o fR2382-1 to R2382-11 determined that fluorine is present in all samples. Total fluoride concentrationvaries from 20100ppm to 106,300ppm; data are summarized in the Summary Table (section 1.0). The highest levels of fluoride were found in R2382-5 andR2382-6 andthe lowest levels in samples R2382-1 and R2382-2. ASHO10533 Analyst / Date Daniel Howman/10-1-97 Page 4 of7 LO 4 IA $EID 129632 Standard Curve POAA ASHO10534 ''O Meter Reading EID 129633 A nalyst / Date D aniel Howman /1 0 -1 -9 7 Page 5 of 7 Project: R2382 Dupont Washington Soil Samples C alculations for Standard Curve C alculated F - (mg/L) = M eter Reading * CotecScn Volume / Sam ple Volume Sam ple ID c a u tio n Sam ple 2 BLANK-1 BcuLANK-2 1 0.Q1 1 0.01 1 0.01 2SPPM W 397-919 25PPM W 397-919 1 0.01 1 0.01 29SSPPPPMMWW 33Q977--991199____ 1 1 0.Q1 0.01 nr. 4 OPPM HgCK______ 1 0.01 SOPPM W 397-820 SOPPM W 397-920 SflPPMW397-92Q____ 1 1 1 0.01 0.01 aoi 25GPPM W 397-921 1 0.01 1 0.01 1 BLANK-1 BLANK-2 1 0.02 1 0.02 1 0.02 . 25PPM W 397-S19 25PPM W 397-919 95PPM W 397.919 1 0.02 1 002 1 002 50PPM W 397-920 50PPM W 397-920 fiflPPM W 197-92Q 1 0.02 1 002 1 0.02 1 250PPM W 397-921 250PPM W 397-921 1 0.02 1 0.02 1 0.02 50QPPM W 397-922 1 0.02 5Q0PPM W 387-922 1 002 1 0.02 1000PPM W 397-923 10QOPPM W 397-923 1 0.02 1 0.02 1 0.02 Q C 1.0PPM CHECK 1 N otebook R eference: Cariton-SA-2. P.20'21 Collection 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 3 .0 F -fm sft.) 10.3 16.5 128 13.9 3 0 .5 2 6 .2 2 1 .7 111.7 128.4 13.7 17.2 16.0 2 6 .5 2 8 .6 26.S 130.6 146.5 144.1 301.0 3 0 0 .6 3 1 4 .4 645.2 6721 8S0.5 S tandard F- I M eter 1 % 1 m m e ru s 16.5 1 6 .5 10.5 16.5 33.1 33.1 33.1 165.3 185.3 ia s 16.5 16.5 33.1 33.1 33.1 165.3 . 165.3 165.3 3 3 0 .5 3 3 0 .5 330.5 661.0 661.Q 661.0 2062 0 .0 5 8 5 3 0.03891 0.02618 0.Q 6097 0.05506 0 .0 4 2 5 6 0.04638 0 .9 6 8 5 0.1016 0.08735 0 .0 7 2 3 9 0 .3 7 2 4 0.4279 0.9845 0 .0 7 9 8 4 0.02783 0 .0 2 6 9 4 0.09136 0 .1 1 4 9 0 .1 0 6 7 0 .1 7 6 4 0.1906 0 .1 7 6 4 0.9725 0.6710 0 .9 7 6 5 0 .9 6 0 7 .v 201 2 * 2004 2096 4.301 4.481 4.390 0.9646 95.25 110.69 99.96 77.26 84.20 96.85 92.22 7929 65.71 87.61 77.68 98.45 Due to low m eter readings and kw recw eiv. d ed d e d to rerun using 20uL a s sam ple vnlumesIH 8293 104.25 96.85 80.04 86.50 BQ.G4 97.25 79.06 88.64 67.20 .91.32 90.95 95.13 97.61 101.68 99.63 96.46 A n a lyst / Date Daniel Howman /10*1*97 Pag6 o f7 & Sh-* O UuLT>| UX iX S EID 129634 Project: R2382 Soil Sam ples from Dupont Washington ' C a lcu latio n s fo r T o ta l F lu o rid e in S o il C alculated F - (mgA.) 3 (M eier R eading+ Intercept) /S lo p e C alculated F - (mg/Kg) = C alculated F - (mgA.) * C ollodion Volume / S am ple W eight S am ple ID Dilution Sam ple C ollection M eter C alculated W eight (g) V olum e (mL) R eading F - (mqlL) A nalysis: DRH 3-30-37 QC 433P PM ERA CHECK BLANK-1 BLANK-2 BLANK-3 R 2382-1-1 R 2382-1-2 R 2382-1-3 R 2382-2-1 R 2382-2-2 R 2382-2-3 Q C 15PP M CHECK R 2 3 8 2 -3 -1 R 2382-3-2 R 2382-3-3 R 2382-4-1 R 2382-4-2 R 2382-445 R 2382-4-4 w /10uL spike of 2 1 1 1 1 0.0203 0.0231 0.023 03236 (U 15 03219 0.0204 0.0225 0.0202 0.0235 0.0227 0.0225 0.023 2.079 . 3.0 0.07713 3.0 0.05811 3.0 005166 3 .0 0.8047 136 3 .0 0.8870 148 3.0 1.155 188 3 .0 0 .8 0 8 0 136 33 0 .9 1 6 3 153 3 .0 05542 158 0.9698 33 2 .4 8 5 387 3 .0 2383 461 3 .0 2.841 440 3 .0 3.668 563 3 .0 3 .8 9 8 598 3 .0 4.109 629 30 6 .1 8 9 940 10.000oBm POAA R 2382-5-1 R 2382-5-2 R 2 3 8 2 -S -3 Q C 1.0PPM CHECK R 23S 2-6-1 R 2382-6-2 R 2382-6-3 R 2 3 8 2-7-1 R 2382-7-2 R 2382-7-3 R 2382-8-1 R 2382-8-2 R 2382-8i3 > Q C 1.0PPM CHECK R 2382-9-1 R 2382-9-2 R 2382-9-3 QC 1.0PPM CHECK 0.0228 0.023 0.D226 1 0021 0.021 0.0214 0.0218 0.0201 0.021 0.022 0.0216 0.0215 1 0.0209 0.021 0.0203 1 3 .0 5.349 814 33 5 .4 3 6 827 3 .0 5 .1 3 6 782 0.9856 3 .0 3 .8 3 5 588 33 3 .7 8 9 581 3.0 3.774 579 3 .0 2 .9 8 3 461 3 .0 2 .5 8 8 402- 3 .0 2 .4 1 5 376 3 .0 1.811 286 3 .0 1.841 291 3 .0 1.503 240 0.9777 3 .0 1.485 237 3 .0 1.509 241 3 .0 1.342 216 05737 A nalysis: DRH 10-1-87 QC 433P PM ERA CHECK 2 BLANK-1 t BLANK-2 1 BLANK-3 1 R 2382-10-1 R 2382-10-2 0.0203 0.0201 R 2382-10-3 0.0208 R 2 3 8 2 -1 1 -1 0.0218 R 2382-11-2 0.0223 R 2382-11-3 0.022 Q C 1.0PPM CHECK 1 N otebook R eference: C artton-SA-2. p 21-23 2.019 3.0 0.1319 3.0 0.06430 3.0 0.05910 3 .0 1.665 264 3 .0 1.741 276 3 .0 1.909 301 3 .0 1288 208 3 .0 1.471 235 3 .0 1.402 2 0 .9 4 2 0 C alculated S`tatisU cs % =- {mg/Kn) ' mgiKg) Recovery 963 20,100 19500 24.500 17,300 21,300 21.700 56,900 61,500 65.300 71500 79,000 83.900 122,600 AVE 21300 STD 2800 cv 13 AVE 20100 STD 2400 CV 12 & AVE 61200 STD 4200 cv 7 AVE 78300 STD 6000 CV 8 107,100 AVE 106300 107500 STD 2100 103,900 CV 2 84,000 AVE 82700 83,000 STD 1400 81200 cv 2 63,400 AVE 59100 60,000 STD 4900 53.800 CV 8 39,000 AVb 37600 40,400 STD 3600 33.500-.rv CV 10 iOFPaCHteCK 34,100" AVE .3 3 5 0 0 34,400 STD 1400 31500 CV 4 97.0 51.4 98.6 97.8 97.4 933 39,100 41.100 43.400 28,600 31.700 30.7QQ AVE STD CV AVb STD CV 41200 2200 5 30300 1600 5 942 Com m ents .... ........ -.........- >CO So3 H-* oV* G\ Analyst / Date Daniel Bowman/10-1-97 Page 7 of 7 ,3 J EID129635 3 M E n viro n m en tal L ab o rato ry, Total. Organic and Adsorbable Fluoride in Groundwater (6/97 Samples) LH $ M S' EID129636 ASHO10537 3M Environm ental Laboratory Data Transmittal Summary Preliminary / Final (circle one) Lab Request #: R-2148 Date Received: 3M Study#: BigenenVir Contract Laboratory # Sponsor or Client: Representative Name Dale Bacon/Robert Howell CompanyName 3M Company Address 935 Bush A ve., St Paul, MN Phone 778-4736 / 778-7540 Project Lead: Name / Phone Kris Hansen Group Leader: Name /Phone 612-778-6018 __________________ Analyte(s) or Test Method #: Total Fluorine, Fluoride Ion, Adsorbable Organic Fluonde ' Sample Matrix: Dupont Waters Analysis Dates: 8/15/97-8/25/97 Analyst(s): Jan Schutz, Nancy Bergman Author: Jan Schutz Data Reviewed by: Project Lead (or designee): PatRethwill 10/03/97 James D. Johnson (or designee): Internal JDJ: Kris Hansen QAU (Archives): Rich Youngblom LIRN System: Denise Appleton Project Managen Sue Beach Sent by: / Date JGS/11/07/97 JG S /11/07/97 JG S /11/07/97 JG S /11/07/97 m HI .-.:Mr A copy o f the report Including this form and the client cover page b to be given to QAU, LIRN and to the Group Leader. 4 5" EID129637 3M Environm ental L aboratory - A dvanced Methjod Developm ent Team Contact: K ris Hansen - Sr. Analytical Chemist Building 02-3E-09 778-6018 kjhansen@ m m m .com Final Report - Lab Request R2148 Total Fluoride Analysis - DuPont 30 September 1997 1.0 SUMMARY Twelve water samples from DuPont were submitted to the 3M Environmental Laboratory for organic fluorine analysis. The samples were submitted under Lab Request R2148, samples 1 through 12. Samples were tested for fluoride ions, total fluorine, and adsorbable organic fluorine (AOF). A modified version of DIN method 38 402 H29 was used to measure the AOF. The following table contains a summary o f the results. Sample ID Sample Request MW-1-1 MW-1-2 MW-2-1 MW-2-2 MW-3-1 MW-3-2 MW-4-1 MW-4-2 MW-3-1 MW-5-2 MW-6-1 MW-6-2 R2148-1 R2148-2 R 2 148-3 R2148-4 R2148-5 R2148-6 R2148-7 R2148-S R2148-9 R248-10 R2148-11 R 2 148-12 2.0 INTRODUCTION Fluoride Ion (pg/inLF-) Total Fluorine (pg/mLF-) Total Fluorine Fluoride Ion (pg/mL) Adsorbable Organic Fluorine (pg/mL F-) 020 0.20 '...... 0.16 0.16 0.14 0.14 0.11 0.11 <0.10 <0.10 0.10 0.10 8.0 16 ...... 71.68 * 3.3 3.1 3.5 3.3 4.2 4.1 3 J 3.2 4.0 3.9 42 4.1 3.0 2.9 2.8 2.7 2.3 2 2 42 4.1 4.5 42 028 0.46 1.1 0.76 0.19 0.14 0.11 0.14 <0.05 <0.05 A request was made o f the 3M Environmental Laboratory to determine the amount o f fluoride andorganic fluorine in twelve monitoring well water samples, using a modified Dohnnann Organic Halide Analyzer and the OrionEA940 Meter with a fluoride specific electrode. 3.0 TEST MATERIALS Twelve monitoring well water samples were received from DuPont. The samples were labeled as having been collected on 6/26/97. The samples were logged in as Lab 3M Environmental Laboratory, Lab Request R2148 Uo ^ ^ ASH010539 EID129638 Request R2148, samples 1 through 12. Samples were kept refrigerated until they were analyzed. A standard curve was prepared, from an ammonium perfluorooctanoate (POAA) standard (S397-386) for total fluoride plus organic fluorine analysis and from an ammonium perfluorooctanoate (POAA) standard (S397-383) for adsorbable organic fluorine. The Orion meter was calibrated daily with standards prepared from a Coming fluoride stock standardin 50%TISAB fl/50% Milli-Q water 4.0 EXPERIMENTAL-OVERVIEW 4.1 Fluoride Ion Analysis This analysis measured the amount of fluoride ion in die sample without combusting the sample. For measurement of fluoride ion, an Orion EA940 meter was calibrated daily, using Coming standards over die range o f 0.05 - 1.5 ppm fluoride. One milliliter o f unfiltered sample was diluted with one m illiliter of TISAB II and analyzed on the Orion meter. A mid-range calibration standard was analyzed periodically to verify that the system continued to operate properly. 4.2 Adsorbable Organic Fluorine (AOF) This analysis measures the amount o f adsorbable organic fluorine as fluoride in the sample by passing the filtered sample through two carbon columns and then combusting the carbon. For measurement of AOF, a modified version of die German wastewater analysis method, DIN method 38 402 H29 (column method), was followed. The POAA standard curve and samples were prepared by running 100.0 mL of standard or sample (or an aliquot of sample3diluted to 100 mL) through two carbon columns using a Dohrmann AD-2000 Adsorption Module. The carbon columns were burned in a modified Dohrmann DX2000 Organic Halide Analyzer, collecting the off-gases in 3.0 mL of 1:1 TISAB II/Milli-Q water and analyzing on an Orion EA940 meter with a fluoride specific electrode. The Orionmeter calibrated from 0.5 - 25.0 ppm fluoride. 4 3 Total Fluorine Analysis This analysis measured the amount o f total fluorine by combusting an aliquot o f unfiltered sample, collecting the off-gasses, and analyzing the collection solution for fluoride. For this measurement a modified Dohrmann Organic Halide Analyzer andan Orion EA940 meter (calibrated from 0.1 - 5.0 ppm F-) were used. An POAA standard curve was generated by burning 0.10 mL standard and collecting the off-gasses in 3.0 mL 1:1 TISAB n/Milli-Q water for analysis on the Orion EA940 meter. The water samples were analyzed following tire same method as the standards. INSTRUMENTATION Dohrmann DX2000Organic Halide Analyzermodified forfluoride analysis Dohrmann AdsorptionModule AD2000 3M Environmental Laboratory, Lab Request R2148 6-7 # )ZS ASH010540 EXD129639 INSTRUMENTATION Orion EA940 Expandable Ion Analyzer with Orion 9609BN Combination Fluoride Electrode DX2000 software, version 1.00, modified for fluoride extraction DX2000 software, version 2.00, modified for fluoride extraction (AOF analysis) Microsoft Excel OPERATING CONDITIONS Combustion tube temperature = 950 C Oxygen and Helium flow = 50 cc/minute VPOAArization/Drying tim e=240 seconds Bake time = 300 seconds Collection fluid=3.0 mL 1:1 TISAB II/Milli-Q water REAGENTS Fluoride Standard 100 ppm, purchased from Corning (part #478170, lot #1113022) Total Ionic Strength Adjustment Buffer (TISAB II), Orion (part #940909, lot AR1) 5.0 DATA ANALYSIS The Orion Meter, serial # 4202, was calibrated each morning prior to any samples being run. Calibration was based on direct measurement of calibration standards made from Coming fluoride stock standard. An acceptable correlation coefficient is = 0.9950. date 18 - 21 August 1997 18 August 1997 15-25 August 1997 analysis done Total Fluorine Analysis / POAA standard curve Fluoride ion analysis AOF Analysis / POAA standard curve correlation coefficient (Rz) >0.9993 >0.9998 >0.9999 A standard curve for total fluorine was generated by combusting 0.1 mL aliquots of 2.0, 5.0, 20, 50, and 100 ig/mL POAA standard (POAA is 66.1% fluoride) in the Dohrmann DX2000 Modified Organic Halide Analyzer. The off-gasses were collected in 3 mL of 1:1TISAB W Milli-Q water and analyzed with the Orion meter. Using least squares linear regression, plotting the fluoride concentration ofthe standardon the x-axis, and the Orion meter response on the y-axis, the following curve was generated: Y = 0.034lx 0.0157 and R2= 0.9988. A standard curve for adsorbable organic fluorine (AOF) was generated by pushing 100 mLs each o f 5 standards containing 4.9,14.4,23.6,33.5, and 43.1 pg/mL fluorine as POAA through two carbon columns. The carbon columns were combusted in the Modified Dohrmann DX2000 Organic Halide Analyzer. The effluent was collected in 3 mL of 1:1 TISAB II / Milli-Q water and analyzed with foe Orion meter. Using least squares linear regression, plotting the fluoride concentration of foe standard on foe x axis, and the Orion meter response on the y axis, foe following curve was generated: Y =0.2894x + 0.0196 andR1= 0.9949. ASH010541 3M Environmental Laboratory, Lab Request R2148 , 4 i M S' EID129640 SAMPLE ANALYSIS: Fluoride Ion Analysis Meter Sample# Reading Dilution Factor Quantity of Sample (mL) Fluoride Ion in Sample (pg/mL) R2148-1 0.1005 2 1.0 0.20 R2148-2 0.1017 2 1.0 0.20 R2148-3 0.0813 2 1.0 0.16 R2148-4 0.0801 2 1.0 0.16 R2148-5 0.0701 2 1.0 0.14 R2148-6 0.0696 2 1.0 0.14 R2148-7 0.0567 2 1.0 0.11 R2148-8 0.0556 2 1.0 0.11 R2148-9 R2148-10 0.0465 0.0463 2 2 1.0 0 .1 0 * 1.0 0 .1 0 * R2148-11 0.0491 2 1.0 0 .1 0 * R2148-12 0.0497 2 1.0 0 .1 0 * ` Method detection limit (MDL) = 0.100 ppm (lowest calibration standard x dilution factor) AOF Standard Curve Total Ammonium Perfluorooctanoate Standard in Columns (top + bottom) * ' < Sample ID * POAA Standard 1 0.072 ppm POAA Standard2 0.217 ppm POAA Standard 3 0.362 ppm POAA Standard4 0.507 ppm POAA Standard 5 0.652 ppm *POAA Standardis 66.1%Fluoride Quantity Combined Spiked Sample Orion Meter fig/mL F- (mL) Reading in Sample (pg/mL F-) Dr 100 1.62 0.05 100 4.18 0.14 100 6.75 024 100 9.31 0.34 100 129 0.43 Y = 0.2894X+0.0196 Rz = 949 ' AOF Sample Analysis Sample ID Combined Quantity ofSample Adsorbable Organic Fluorine Meter Reading (mL) in Sample (pg/mL) R2148-1 (top+ bottom) R2148-2 (top + bottom) R2148-3 (top +bottom) R2148-4 (top+bottom) R2148-5 (top+bottom) R2148-6 (top+ bottom) R2148-7 (top+ bottom) R2148-8 (top -t-bottom) R2148-9 (top+bottom) R2148-10 (top+bottom) R2148-11 (top+bottom) R2148-12 (top +bottom) *MDL =0.05 pgftnL. 6.544 6.063 6.776 11.30 3235 2229 2.696 2.024 1.556 1.937 0.537 0.536 3M Environmental Laboratory,Lab Request R2148 5.0 5.0 85.0 85.0 10.0 10.0 50.0 50.0 50.0 50.0 100.0 100.0 4.5 4.2 028 0.46 1.1 0.76 0.19 0.14 0.11 0.13 <0.05* <0.05* ^i ASHO10542 5- EID129641 Total Fluorine Standard Curve Ammonium Perfluorooctanoate in Milli-Q water Sample ID POAAstandard l -2.00 ppm POAA standard 2 - S.OOppm POAA standard 3 - 20.0 ppm POAA standard 4 - 50.0 ppm POAA standard 5 - 100ppm Quantity Sample (mL) 0.100 0.100 0.100 0.100 0.100 Orion Meter Reading G ig taL F -)' 0.048 0.100 0.421 1.089 2.248 Spiked pg/mL F-in Sample * 1.32 3.31 13.2 33.1 66.1 'Based on the average oftoce replicates. Y = 0.0341x - 0.0157 RJ=0.9988 ` ammonium perfluorooctanoatestandard is 66.1 % Fluoride Total Fluorine Sample Analysis Sample ID M eter* Quantity of Total pg/mL Reading Sample (mL) F-in Sample MW-1-1 R2148-1 02568 MW-1-2 R2148-2 MW-2-1 R2148-3 0.5217 0.0964 MW-2-2 MW-3-1 MW-3-2 MW-4-1 MW-4-2 R2I48-4 R248-5 R2148-6 R2148-7 R248-8 0.1051 0.1279 0.0963 0.1199 0.1260 MW-5-1 R2148-9 0.0960 MW-5-2 R2148-10 MW-6-1 R2148-11 0.0802 0.0636 MW-6-2 R2148-12 0.1286 * Based on average ofthree replicates. 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 8.0 16 3.3 3.5 4.2 33 4.0 42 3.0 2.8 23 42 6.0 CONCLUSION Fluoride ion concentrations range from <0.10 to 0.20 pg/mL, <0.05 to 4.5 jig/mL F- for adsorbble organic fluorine analysis, and 2.3 to 16 pg/mL F- for total fluorine analysis. The large difference in concentration o f total fluorine for samples, R2148-1 and R2148-2 (duplicate samples) may have been caused by differences in the amount o f solid particulate matter in the sample aliquots. The results for the adsorbable organic fluorine analysis may be lower than expected, due to die fact that die solid particulate matter was filtered from the AOF samples, and some polymers may not adsorb on to the charcoal columns. 7,0 MAINTENANCE OF RAW DATA Hard copies of the data are filed in the AMDT archive. JG Schtz 09-30-97 ASHO10543 coneoaraon 3M Environmental Laboratory, Lab Request R2148 70 EID129642 F- Cono, in Standard 4.9 14.4 23.9 33.5 43.1 Meter Reading 1.6156 4.1827 6.7477 9.3122 12.8872 Curve Perfluorooetanoate AOP Curve ASHO10544 E ID 129643 E ID 129644 Orion Data ASHO10545 DATA FOR AMMONIUM PERFLUOROOCTANOATE AOF STANDARD CURVE ^ F- Cone. fDamPle Meter Collect Dilution Sample CalcAOF reading Vol(mL) Factor Volume of ,, (ppm F-) ______ column top&bottom TM alof Ononread TOTAL AOF (Top& In Standard % Recovery __ Bottom) rmL^ blankbottom Std#1 bottom Std#2 bottom Std# 3bottom Std#4 bottom Std#5 bottom blank top Std* Hop Std#2 top Std#3 top Std#4 top Std#5 top QC check 5.0 0.1522 0.4536 0.3701 0.3643 0.1815 0.1232 0.0544 1.1620 3.8126 6.3834 9.1307 12.764 5.098 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 1.0 1 1 1 100 100 100 100 100 100 100 100 100 100 100 F L U O R ID E IO N A N A L Y S IS Sample ID MeterReal TISABVol Dilution SampleVoi QC check 0 .5 0 1 R2148-1 R2148-2 82148-3 R2148-4 R2148-S R2148-6 R2148-7 R2148-8 R2148-9 R2148-10 R2148-11 R2148-12 0.5018 0.1005 0.1017 0.0813 0.0801 0.0701 0.0696 0.0567 0.0556 0.0465 0.0463 0.0491 0.0497 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1 1.0 1.0 .1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 0,4565 0.0136,1 0.01110 0.0109296 0.00544 0.00370 0.00163 0.03486 0.1144 0.1915 0.2739 0.3829 5.098 Total Fluoride (ufl/mL) 0.502 0.201 0.203 0.163 0.160 0.140 0.139 0.113 0.111 0.093 0.093 0.098 0.099 0.504 1.616 4.183 6.748 9.312 12.887 0.048 0.125 0.202 0.279 0.387 0.049 0.144 0.239 0.335 0.431 100% 87% 85% 83% 90% 101% b Pagel R2148.xls Orion Data ASHO10546 E ID 129645 s Orion Data ASHO10547 AOF ANALYSIS Sample IU AOF Calc. (ug/mL) = ((total m eter reading - intercept)/ slope) / sample volume Calc. Adsorbable Meter Collect Dilution Sample Meter Reading Organic Fluorine V V I \IIIU / y=0.2894+0.0196 Comments % Recovery RP14R.9bottom R214S-10 bottom R2148-11 bottom o bottom R 914&& tOS R2148-10top R2148-11 top R2148-12 top R2148-7MS Bottom R2148-7 MSTop QC calcheck4.33 ppm R2148-11 bottom R2148-12 bottom R2148-11 Top R 2148-12 Top QC check 0.080 ppm 0.2705 0.2784 0.1188 0.0713 1.2856 1.6588 0.3520 0.2683 0.1134 3.0297 2.228 0.0760 0.0839 0.4608 0.4518 0.4988 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 1.0 3.0 3.0 3.0 3.0 1.0 1 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 50 50 50 50 50 50 50 50 100 100 1 100 100 100 100 1 1.5561 1.9372 0.4707 0.3396 3.143 05368 0.5357 0.1062 0.1325 0.0312 0.0221 0.1079 4.456 read below lowstd, re-run read belowlowetcI, re-run 103% 0.0176 0.0175 98% N Page 3 R2148.XIS measured electrde responce (ppm F-) 2.50000 2.00000 1.50000 1.00000 0.50000 0.00000 POM CURVE ASHO10548 Thermally Extracted Perfluorooctanoate Curve 20 30 40 50 STANDARD CONCENTRATION (PPM F-) P ager EID 129648 DUP0NT1.xls 11/7/97 3:30 PM rem uoroocuiiiuaw omii*mim vw VV 1-- ' 1 factor!I sample] COLLECT CALC. POAA lim ili iPB illiWM 1 QC 1.0PPM STDCHECK BLK-1 BLK-2 BLK-3 POM 1.0 PPMW397-795 POM 1.0 PPMW397-795 POM 1.0 PPMW397-795 ERA4.33PPMSTD 0.1 3 w 0.1 3 1.02 0.1 3 0.48 ASHO10549 Actual %REC COMMENTS 2.0 ' 0.9652 0.0491 0.0340 0.0161 1<)1.6 ' BELOWDETECTION LEVEL USE2.0PPMSTD DATA NOTINCLUDEDINCURVE 99.86 r* POM 100PPMW397-799 POM 100PPMW397-799 POM 100PPMW397-799 QC 1.0 PPMCHECK Pagel D U PO N Tlxls 11/7/97 3:17 PM TABLE : R2148 F- DETERMINATION: SAMPLES DUPONT INC. CALCULATED(PPMF-) = (meter reading *J?||Brcept) / slope) SEE STANDARDCURVEFOR EQUATION: Y= 0.0341X - 0.0157 ASH010550 ------------------------- 1 SAMPLE ! COLLET Actual MSI CALC. | ERA4.33PPM STD QC 1.0PPMSTDCHECK BLK-1 BLK-2 BLK-3 QC1.0PPM CHECK R2148-11-1 R2148-11-2 R2148-11-3 R2148-12-1 R2148-12-2 R2148-12-3 R2148-10-1 R2148-10-2 R2148-10-3 QC 1.0 PPMCHECK R2148-9-1 R2148-9-2 R2148-9-3 R2148-8-1 R2148-8-2 R2148-8-3 QC 1.0PPMSTDCHECK 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 2.162 0.9864 3 0.01599 3 0.01455 3 0.01491 . `0.9743 3 0.05555 2.09 3 0.06031 2.23 3 0.07499 2.66 3 0.1699 5.44 3 0.1233 4.08 3 0.09247 3.17 3 0.08379 2.92 3 0.06284 2.30 3 0.09400 3.22 0.9663 3 0.1042 3.52 3 0.07910 2.78 3 0.07286 2.60 3 0.1361 4.45 3 0.1279 4.21 3 0.1131 3.78 0.9624 STATS AVE 2.33 STD 0.30 CV 12.8 AVE 4.23 STD 1.14 CV 27.0 AVE 2.81 STD 0.47 CV 16.6 AVE 2.96 STD 0.49 CV 16.4 AVE 4.15 STO 0.34 CV 8.24 %REC 99.86 98.64 97.43 96.63 96.24 5* N IN E ID 129649 DUPONTlxls 11/7/97 3:17 PM Ift >P ASH010551 I EID 129650 3NS Environmental Laboratory Soil Properties and Nutrient Concentration Analyses (6/97 Samples) 7<\ <i 135 E ID 129651 ASH010552 3 M E cotoxico lo g y a n d E n v iro n m e n ta l F a te L ab o rato ry Soil Properties and Nutrient Concentration Analyses of Samples Received From the E. I. DuPont de Nemours and Company Facility in Parkersburg, West Virginia ; s S T U D Y C O M P L E T E D : August 2 7 ,1 9 9 7 F IN A L R E P O R T C O M P L E T E D : O cto b er 3 1 ,1 9 9 7 Lab Request No. R2382 Prepared by: Se usan Aa . DBeachh y Senior Environmental Biologist 3MEnvironmental Laboratory Building 2-3E-09 935 Bush A v e n u e St Paul, MN55144 ' go EID129652 3 M E cotoxicology a n d E n v iro n m e n ta l F a te L a b o ra to ry 1.0 Introduction Eleven soil samples were received from E.l. DuPont de Nemours and Company for preparation and analyses by the Ecotoxicology and Environmental Fate Testing Group of the 3M Environmental Laboratory. These samples were assigned a Lab Request number (LR No.) of R2382. The sample date was 6/23/97. Samples were numbered R2382-1 through R2382-11 as follows: 3M LR No. R 2382-1 R 2 3 8 2-2 R 2 382-3 R 2 3 8 2-4 R 2382-5 R 2382-6 R 2 3 8 2-7 R 2 3 8 2-8 R 2382-9 R 2382-10 R 2 3 8 2-1 1 n n P o n t C O C D escrio tio n S S -1 0 -2 ' S S -1 4 -6 ' S S -1 8 -1 0 ' S S -1 1 2 -1 4 * S S -1 1 6 -1 8 ' S S - 1 2 0 -2 2 ' S S - 1 2 4 -2 6 ' S S -1 2 8 -3 0 ' S S -1 3 2 -3 4 ' S S -1 3 6 -3 8 ' S S -1 3 8 -4 0 ' 2.0 Results A summary of the results obtained is presented below. Copies of methods, raw data sheets, and contract laboratory reports are attached to this summary report. DuPont Sulfate, Sulfite, Sample No. tng/kg mg/L R2382-1 SS-1 o-z R2382-2 SS-1 4-6' R2382-3 SS-1 8-1O' R2382-4 SS-1 12-14' R2382-5 SS-1 16-18' R2382-6 SS-1 20-22' R2382-7 SS-1 24-26' R2382-8 SS-1 28-30' R2382-9 SS-1 32-34' R2382-10 SS-1 36-38' R2382-11 SS-1 38-40' 98 99 73 54 43 70 220 150 100 63 46 <2 <2 <2 <2 <2 <2 <2 <2 <2 <2 <2 Nitrite Nitrogen, mq/kq 0.41 0.41 0.36 0.14 <0.10 <0.10 <0.10 0.11 <0.10 <0.10 <0.10 pHin CaC!2 7.2 7.3 7.0 6.3 5.3 5.5 5.3 6.3 5.2 5 .4 6.2 pHin water CEC, meq/100g 7.7 7.7 7.3 6.7 5.7 6.0 5.8 . 6.8 5.8 6.1 6.8 *.* 15.8 18.4 17.5 17.5 18.4 19.3 17.5 11.4 13.1 9.6 6.3 % Moisture, (as-rec'd) 12.3 12.7 15.5 18.9 18.3 19.2 20.0 18.1 13.6 17.9 22.2 ASH010554 2 SI t I EID129653 3R1 E cotoxicology a n d E n v iro n m e n ta l F a te L a b o ra to ry 3.0 Initial Observations 3 .1 S a m p le R 2 3 8 2-1 H a lf o f th e tw o fo o t co lu m n not fille d . O n ly o n e fo o t o f s o il p re s e n t. 3 .2 S a m p le s R 2 3 8 2 -2 th ro u g h R 2 3 8 2 -1 1 H a d a n u n u s u a l o d o r, p ossib ly h ydrocarbo n s. 3 .3 S a m p le s R 2 3 8 2-1 th ro u g h R 2 3 8 2 -6 A p p e a r to b e c la y /s ilt. 3 .4 S a m p le s R 2 3 8 2 -7 a n d R 2 3 8 2 -8 A p p e a r to b e e la y /s ilt/s a n d , m o re silt/san d . 3 .5 S a m p le R 2 3 8 2 -9 A p p e a rs to b e s an d /siit. 3 .6 S a m p le R 2 3 8 2 -1 0 A p p e a rs to b e s a n d /s iit w ith fre e -flo w in g w a te r in co lu m n . 3 .7 S a m p le R 2 3 8 2-1 1 A pp ears to be coarse sand. t ^ * 4.0 Sub sampling A o n e -fo o t c o re from th e to p o f e a c h colum n th ro u gh th e c e n te r w a s re m o v e d . T h e s a m p le w a s thoroughly m ix e d th en sp lit fo r in o rg a n ic an d o rg a n ic a n a ly s e s . T h e rem ain in g in ta c t co res w e re re frig e ra ted a t 4 C in th e d a rk . 5.0 Sample Preparation A liq u o ts o f w e ll-m ix e d w e t so il (a s re c e iv e d ) w e re p re p a re d a s n e c e s s a ry fo r so il p ro p e rtie s te s tin g , n u trien t a n a ly s e s , C E C , a n d to ta l flu o rid e a n a ly s e s . A fte r p re p a ra tio n , a liq u o ts w e re p ro vid ed to th e p ro p e r lab o ra to ry p e rs o n n e l fo r te s tin g . 5 .1 A ir-D rie d S o il - 2 .0 0 m m . S o il s a m p le s w e re air-d ried a t a m b ie n t room tem p e ra tu re to c o n s ta n t w e ig h t. S o il w a s c ru s h e d , a s n ecessary w ith a m o rtar an d p e s tle , and p a s s e d th ro u g h a 2 .0 0 m m s ta in le s s s te e l s ie v e . S oil p rep ared th is w a y w a s u sed fo r p H a n a ly s e s . ASHO10555 82. 4 3 EID129654 3 M E cotoxicology a n d E n v iro n m e n ta l F a te L a b o ra to ry 5 .2 A ir-D rie d S o il - 0 .5 0 0 m m A liq u o ts o f a ir-d rie d 2 .0 0 m m so il w e re c ru s h e d w ith a m o rta r a n d p e s tle u n til th e e n tire sa m p le p assed th ro u gh a 0 .5 0 0 m m s ta in le s s s te e l s ie v e . S oil p re p a re d th is w a y w as u sed fo r C E C a n d n u trie n t an aly s e s . 5 .3 O v e n -D rie d S o il - 0 .0 6 3 m m A liq u o ts o f th e 2 .0 0 m m a ir-d rie d so il w e re fin e ly g ro u n d w ith a m o rta r an d p e s tle u n til th e en tire sam p le p a s s e d th ro u g h a 0 .0 6 3 m m s ta in le s s s te e l s ie v e . T h e s a m p le s w e re then o v e n -d rie d (1 0 5 C ) to c o n s ta n t w eig h t. S o il p re p a re d th is w a y w a s u sed fo r to ta l flu o rid e a n a ly s e s (re s u lts p re s e n te d in a s e p a ra te report by 3 M A M D T L ab o rato ry). 6.0 Analytical Methodology 6 .1 S o il W a te r C o n te n t A lu m in u m p a n s w ere o v e n -d rie d to c o n s ta n t w e ig h t. T w e n ty -th re e to th irty -fiv e g ra m a liq u o ts o f w ell-m ixed w e t s o il (a s -re c e iv e d ) w e re w e ig h e d in th e alu m in um p an s. T h e pans an d so il w e re th e n o v e n -d rie d a t 1 0 5 C to co n s ta n t w e ig h t. T h e so il w a te r c o n te n t w a s d e te rm in e d b y th e fo llo w ing e q u a tio n : W eig h t o f W e t S oil - W e ig h t o f D ry S o il W e ig h t o f D ry S o il X 100 6 .2 S o il p H . 6 .2 .1 p H in W a te r T e n g ram s of 2 .0 0 m m -sieved so il a n d 1 0 m L M iili-Q w a te r w e re p la c e d into 5 0 m L co nical c e n trifu g e tu b e s . T h e tu b e s w e re th e n c a p p e d a n d s h aken fo r one hour. A fte r sh a k in g , th e tu b e s w e re a llo w ed to stan d fo r o n e h ou r. A C o le -P a rm e r M o d e l 5 9 9 2 -6 0 so il e le c tro d e w a s u s e d to m easu re th e pH. 6 .2 .2 p H in 0 .0 1 M C a C l2 A fte r p H in w a te r w a s d e te rm in e d , 0 .1 0 m L o f 1 .0 M C a C l2 w a s a d d e d to e a c h tu b e . T h e tu b es w ere s h aken fo r 3 0 -m in u te s th en allo w ed to sta n d fo r 3 0 -m in u te s . A C o le -P a rm e r M o d e l 5 9 9 2 -6 0 so il e le c tro d e w a s u s e d to m easure th e pH . . . 6 .3 C a tio n E x c h a n g e C a p a c ity (C E C ) b y S o d iu m S a tu ra tio n 6 .3 .1 A d s o rp tio n S te p F iv e g ram s o f 0 .5 0 0 m m -sieved so il a n d 1 3 2 m L o f 1 .0 N pH 8 .2 N a O A C w e re p la c e d into 2 5 0 m L c o n ic a l p o ly p ro p y le n e c e n trifu g e tu b e s . T h e veo w g --OUi*Sll ^ 23 4 MS' EID129655 3 N I E cotoxicotogy a n d E n v iro n m e n ta l F a te L ab o rato ry tu b e s w e re th e n ca p p e d a n d sh aken o v ern ig h t a t 3 0 0 -4 0 0 rpm . A fte r s h a k in g , th e tu b e s w e re ce n trifu g e d fo r 1 0 m inutes a t 3 0 0 0 rp m . T h e s u p e rn a ta n t w a s th e n d e c a n te d a n d d is c a rd e d . 6 .3 .2 W a s h in g S te p F ifty m L o f 2-p ro p a n o l w a s th e n a d d e d to e ach s o il. T u b e s w e re cap p ed a n d s h a k e n fo r 3 0 -m in u te s . A fte r s h a k in g , th e y w e re c e n trifu g e d a s in 6 .3 .1 a n d th e s u p e rn a ta n t d is c a rd e d . T h is step w a s th e n re p e a te d w ith a n o th e r 5 0 m L a liq u o t o f 2 -p ro p a n o l. 6 .3 .3 D e s o rp tio n S te p O n e hun d red m L o f 1 .0 N , p H 7 .0 N H 4O A C w a s a d d ed to e a c h sam p le. T h e tu b e s w e re sto p pered an d s h aken o ver-n ig h t. A fte r sh akin g , th ey w e re cen trifu g ed fo r 10 -m in u te s a t 3 0 0 0 rpm . T h e su p ern atan ts w ere d e c a n te d fo r so diu m a n a ly s e s . T h e s u p e rn a ta n ts w e re th e n su b m itted to th e In o rg a n ic A n alysis G ro u p o f th e 3 M E n viro n m en tal L ab o rato ry fo r a n a ly s is o f sodium b y IC P (S W -8 4 6 , M e th o d 6 0 1 0 ). 6 .3 .4 C a lc u la tio n o f C a tio n E x c h a n g e C a p a c ity Q.1 x (pong. of, N .a,_m giL )/23 o ven -d ried w eig ht o f s o il, g * x 100 - m eq / 100 g soil S u b -s a m p le s o f 0 .5 0 0 m m a ir-d rie d soil w e re o v e n -d rie d to c o n s ta n t w e ig h t a n d th e m o isture c o n te n t w a s d e te rm in e d . T h e v a lu e s o b ta in e d w e re u sed to c a lc u la te th e fin a l C E C v a lu e o f so il on an o v e n - d rie d w e ig h t b asis. 6 .4 N u trie n t A n a ly s e s A liq u o ts o f th e 0 .5 0 0 m m -s ie v e d so il w e re s u b m itte d to M in n e s o ta V a lle y T e s tin g L a b o ra to rie s , In c. (M V T L ) fo r a n a ly s is o f n itrite, s u lfa te and s u lfite . T h e fo llo w in g m eth o d s w e re em p lo y e d : 6 .4 .1 N itrite N itro g e n M eth o d s o f S o il A n alysis, 2 n d E d itio n , 3 3 -8 . 6 .4 .2 S u lfa te S W -8 4 6 , M ethod 9 0 8 8 . . 6 .4 .3 S u lfite E P A M ethod 3 7 7 .1 . ASH010557 5 EXD129656 3 N I E cotoxico lo g y a n d E n v iro n m e n ta l F a te L a b o ra to ry Copies of Raw Data and Contract Laboratory Reports ** . `r S5~ot M S ' EID129657 ASH010558 ENVIRONMENTALLABORATORY WORKSHEET LR PAGE / OF / DATE 8 / 5 / f / A N /5S ^^*3 ^^ / w , TM y * v f . < /* & ]& jc ^ + m // "ks M U silflSiWf ------------- A fl*w fa hr fiA td fa /'f- -- ----------------------------------- >r r ^ b , ` gu f f i / f - t t u w t f t r f ' m i l K f fitS S J A - W " * * - a ^ S # r f t 6 f W <% < Y f r W r f 8 b ef M S ' EID129658 ENVIRONMENTAL LABORATORY SOILWATER CONTENT PERCENTAGEOF WATER IN THE SAMPLE ON A DRY-MASS BASIS Gardner, Walter. 1986. WaterContent, p. 493-544. In Arnold Klute (Ed.). Methodsof Soil^tysis Part 1. Physical and Mineralogical Methods. Agronomy Monograph No. 9 (2nd Edition). %WaterContent = WeightofWeSoil - Weightof PfY-SfiSl Weightof DiySoil 100 D A T & ,) 87 4 MS' EID129659 * ENVIRONMENTALLABORATORY ! SOILpH and LIMEREQUIREMENT^} It ? jsijr McLean, E. 0 .1982. Soil pHand Lime Requirement, p. 199-224. InA. L. Page, R. H. Miller&D. R. Keeney (Eds.) Methods ofSoil Analysis, Part 2. Chemical and Microbiological Properties, AgronomyMonograph No. 9 (2nd Edition). 2.00 mm air-dried soil used. Soil - to - Miilipore Milfi-QTMWater Ratio 1:1,10 g plus 10 mL For LR. SMP single-buffermethodused, Soil - to - SMP Buffer Ratio 1:2.10 g plus 20 mL SAMPLE DESCRIPTION ? X 4 R u 1 < q in it pHw (pH in water) ... 7 .* / 7.*> f*rf serf An ee.* L .t pHs (pH in 0.01M CaCI2) Soil-Buffer pH 1-7j___________ i , n ________ La ' K .X %&>____________ 7> ,2> *e .7 . 3 , - f ____________ ff. 7- J LR (T/A) anai5?s T Z = S ^ 5 D A T E :_ 5 ^ ^ I . --------- ----------- > CO K oUl On S3 4 MS' EID129660 EXD129661 ENVIRONMENTAL LABORATORY SOIL WATER CONTENT PERCEN TAG E O F WATER IN THE SAM PLE ON A DRY-MASS BASIS Gardner, Walter. 1986. Water Content, p. 493-544. In Arnold Khite (Ed.). Methods of Soil Analysis, Part 1. Physical and Mineratogfcal Methods. Agronomy Monograph No. 9 (2nd Edition). % W ater Content = Weight of Wet Soil - Weight of Dry Soil x 100 Weight of Dry Soil For SAM PLE DESCRIPTION Z. -4 .<7 la 'i < *1 in it Wet Soli g (air-dried) i. *14 I d 7ef h .X id U J ,< f lO 'Z f, U .1< 4 b .U fs .M f) .. Dry Soil g (oven-dried) ` NET LOSS g % __________ O .O U L ______ 0 . 7 3 , . q . o g j - __________ 0 ,0 2 5 --------- O A l ....... 0 , 0.11---------- - O S L ______ '"i.O Z J __________ o . o g f f i _____ J L B 2L ____ U . 4 5 2 -________ Q . a ^ ______ J L M ______ U . Ia02- 0 .0 3 3 -____ _ 0 , 7 3 ._______ ^ C H O - Q . - & S C _____ 0 .1 8 _______ m .o t X . _______ 6 , Q & i ___ __ J 2& L ______ u> nzjl. ... o . o n ______ u r n _______ ........... 0 , 0 .2 1 ______ 0 , 5 2 ~ .... t ^ o t s : _______ d J u S .______ 0 `1 2 5 -______ ---------- > sJ 10 4 ^ EID129662 ENVIRONMENTAL LABORATORY CATION EXCHANGE CAPACITY (CEC) BYSODIUMSATURATION Rhoades, J. D. 1982. Cation Exchange Capacity, p. 149-157. in A. L Page, R. H. Miller& D. R. Keeney (Eds.) Methods of Son Analysis, Part 2. Chemical and Microbiological Properties. Agronomy Monograph No. 9 (2nd Edition). Extracts prepared using 0.500 mmair-dried soil. Cation Exchange Capacity by Sodium Saturation; modificationof method is as follows: _ 'ADSORPTION Batch equilibrium method (over-night) with 1.0 N NaOAc pH 8.2 as saturation solution. WASHED Two washings with 2-Propanol. 'DESORPTION Batch equilibrium method (over-night) with 1.ON NH40Ac pH 7.0 as extraction solution. CEC EQUATION: (0.1 Na ppm/2 3 / oven-driedwt.ofsoilg ) x 100 = meq/100gsoil *7) 1%~ EID129663 LABORATORIES, Inc. P.O. BOX 249, 1126 N. FRONT STREET NEW ULM, MN 56073-0249 PHONE (507) 354-8517 WATS (800) 782-3557 FAX (507) 359-2890 WE ARE A N EQUAL OPPORTUNITY EMPLOYER AOL Report To: R ochelle Rotrideau 3M Eavironm talLab 935 Bush Ave., Bldg. 20 S t Paul, MN 55106 Date: W ork Order: Date Received: 27 August 1997 10-0447 Md 25 August 1997 Page 1 o f4 In orgaaicsL ab N o...................... Soil la b N o ................................ Sample ID ................................. S4352 S4353 W-547 W-548 R2382-1 R2382-2 S4354 S4355 S4336 S4357 W-549 W-550 W-551 W-552 R2382-3 R2382-4 R2382-5 R2382-6 Analyte NitriteNitrogen (mg/KgN) . . 0.41 0.41 036 0.14 < 0.1 0.1 j41 Sulfate (mg/Kg).................... 98.4 98.6 73.3 53.9 43.4 70.4 Sulfite (mg/L)......................... < 2 < 2 < 2 < 2 < 2 < 2 Repeat approved by: 7 A nthony R -K ocfcele By and fo r M innesota V a ik y Testin g Laboratories, lh c . ASH010565 M .'fM Jalw iaiclarfltoiteauaacB B irolhir $1 * 1 i EID129664 LABORATORIES, Inc. P.O. BOX 249, 1126 N. FRONT STREET NEW ULM, MN 660734)249 PHONE 1507) 354-8517 WATS (800) 782-3557 FAX(507) 359-2890 WE ARE A N EQUAL OPPORTUNITYEMPLOYER ACH Report Te: RochelleRobideau SMEoviroamenalLab 935 Bush Ave., BMg. 20 S t Paid,MN 55106 Date: W ork Order: Date Received: 27 August 1997 10-0447 25 August 1997 * Page 2 o f4 -1 i Inorganics Lab N o ................... S4358 S4359 S4360 S4361 S4362 Sod Lab N o .............................. W-553 W-554 W-555 W-556 W-557 Sample ID . ........................... 82382-7 R2382-8 R2382-9 82382-10 82382-11 Analyte Nitrite Nitrogen (mg/KgN) . . <0.1 0.11 <0.1 4tntadiM <0.1 Stiliate (m g/K g).................... 217 153 102 63.3 46.2 SulSte (m g/L)........................ <2 <2 <2 <2 <2 ASHO10566 Report approved by: AnthoayR. Koebele a By and for MinnesotaValley Testing Laboratories, foe. MVTLg u a rto te* tiba aecura^of the aaabiia done seapla w bettte fcr teelto Il b a rt peadbl6 r M V IH geanetee UwU t * eaapteaaUM allcooditioluafliKtiagtheeM BpUuetheaK-- ,fodng M paBgby5CVTL.Aaagtttalpiolrttoe teB*at m he paldlfteod< o fctenla, and airthpriaatten fccpublication ofitat aaiinfs. nonHwsfcwea r S a rta frate e r lagartagourreporta to raascvi d panillnfoar written >pteitffl be tha samoon any other r*a,nUreporta xeaubmUWdaethe coeddeatilproperty 93 4 U S' EID129665 LABORATORIES, Inc. P.O. BOX 249, 1126 N. FRONT STREET NEW ULM, MN 56073-0249 PHONE (507) 354-8517 WATS (800) 782-3557 FAX (507) 359-2890 WE A S E A N EQUAL OPPORTUNITYEMPLOYER Analyte Nitrite Nitrogen Analysis of 3M Samples Page 1 o f 1 0.1 mgKgN Methods o f Soil Analysis, 2nd Edition, 33-8 Sulfate 40m g/K goaa5 g SW-846, Method 9038 S u lfite 2.00 mg/L EPA Method377.1 ASH010567 EID129666 DATE: 0 8 /2 1 /1 9 9 7 .' ' '3 3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY PARAMETER LAB REQUEST NO. R 2 3 3 2 CCNTPACT LAB : HVTL PROJECT NIMBER : BIGENSNVIR SHTP BATE : S "7n J^T 7 C om puter Cade T e s t Naine PROJECT LEAD: RD HOUiELL TELEPHONE FAX : : 612-778-6176 Sam ple N umbers Sam ple A v ailab le D ate R esu lt Due D ate N 02-N 03 SC t N ITR ITE NITROGEN - a s N 1 , 2 , 3 , A , 5 , 6 , 7 , 8 , 9 , 10, 11 SULFITE 1 2 , 3 , A , - , 6 , 7 , 8 , 9 , 10, 11 SULFATE - a s SQ4 1., 2 , 3 , A , S , 6 , 7 , 8 , 9 , 10, il 0 3 /1 3 /1 ??? 03/27/1997 08/13/1997 0 8 /2 7 /1 9 9 7 08/13/1997 0 3 /2 7 /1 9 9 7 ASH010568 < s H> EID 129667 a w E cotoxico lo g y a n d E n v iro n m e n ta l F a te L ab o rato ry Copis of Soil Methods U 4 M S' i EID 129668 ASH010569 3 M E N V IR O N M E N T A L L A B O R A T O R Y P R E L IM IN A R Y P R E P A R A T IO N O F S O IL S A M P L E S FO R L A B O R A TO R Y A N A L Y S IS 2.00 mm Air-Dry Soil . Air-dty (ambient room temperature) so samples on flat Bays for24 to 48 hours or unfithoroughly dry (constant weight). It desired, samples can be oven-dried at 35C overnight (1 8*4 hours).* . P ass air-dried soil (crashed and mixed via mortarand pestle) Btrou^t a 2.00 mm (10 mesh) s i n l e s s steel sieve. This removes large pieces of foreign material such as stones, gravel and Mugs. . Partition the sample by me -quarter* system or by passing through a riffle sampler (sample splitter). If desired, quarters can be further divided into smaller portions. soluble salts analysis or store in a cool, dark room. snil RFACTION TESTS pH lime Requirement Gypsum Requirement ^ IIIR IF SAITS ANALYSIS Electrical Conductivity a-.so ABcairiy PHYSICALCHARACTERISTICS So* texture and dassiBcatkm "i ' 0.500 mm Air-Dry Soil . obtain about 20 to 40 g of a representative portion of the 2.00 mm soil and grindin an agate mortar and pestle until the entire sample passes through a 0.500 mm (35 mesh) sieve. . . Use this soil for exchange activity tests (Cation Exchange Capacity. Base Saturation. SAR. ESP) and for nutrient analysis (N, P, S). 0.063 mm Oven-Dry Soil . Obtain about 10 to 20 g of a representative portion of the 2.00 mm soil and finelygrind in an agate ball mill until the entire sample passes though a 0.063 mm (250 mash) sieve. . Oven-dry (105-110C) the above sample (placed inatared aluminum weighing dish) overnight and report the loss in weight . Use this finely ground (bail milled) oven-diy son for total elemental analysis (1CP.AA).total fluoride and TOC analysis. SPECIAL NOTE . All dried so* samples are placed in impermeable, polypropylene bottles.They are stored in ihe soil cabinet(dark and a t ambient room temperature) for one year after testing. . Disposal for aH soils and Iheir extracts is by incineration. REFERENCES Page. A. L.. MQierR.H. &Keeney D.R.(Eds.) 1932. Methodsof Soii Analysis. Part 2. Chemical and Microbiological Properties, Agronomy Monograph No.9 (2nd Edition). Sk, K. and R. H. Geiderman.1988. Soil Sample Preparation. ^ .Ire R a a x n m e n d a d Chemical Son Test Procedures lor the North Central Region. North Central Regional Publication No. 221 (Revised). NOTE. If nitrate analyses are to be determined, the soil should be dried within twelve hours of sampting to preventchanges in the nitrate content. (Revised 12/94 RRR) ' o o m 4 M S' t i EID 129669 3M ENVIRONMENTAL LABORATORY SO IL WATER CONTENT PERCENTAGE OF WATER IN THE SAMPLE ON A DRY-MASS B A SIS PRINCIPLE OF THE SOIL WATER CONTENT METHOD The amount of water in a soil affects directly the growth of crops, microbes, and insects. The strength of the soil, which determines root penetration and the energy requirements for tillage are dependent onthe water content, however, die amount of plant available water in the soil is dependent on the sou water potential- Since the water potential is more difficult to determine, the water content is used as ^ at9 of water in the soil (In laboratory terms, practically every type of soil analysis requires that the results be reported on a dry mass basis.) Traditionally, the water content has been expressed as the ratio of the mass of ^ ter,p fa sep t ip?tha sample to the mass of the sample after it has been dried at 105 C to a constant mass. Thus, usually used in soil studies is a dimensionless ratio of two masses or is expressed as a percentage resulting from multiplying the dimensionless ratio by 100. The laboratory procedure employed here is water content measurements by the grawmetric method. It involves weighing the wet sample, removing the water, and reweighing the sample to determine tne anwunt of water removed. Water content is determined by dividing the difference between wet and dry masses by the mass of the dry sample to obtain the ratio of the water mass to the mass of the dry soil, then multiplied by 100. This is now the percentage of the water in the sample on a dry-mass or dry-weight basis. RANGE AND SENSITIVITY The range and sensitivity will depend on the time necessary to reach constant weigfjt apd.the analytical balance used. used IN TER FER EN C ES Factors that may influence the results include: Failure of temperature control. The drying oven used must maintain a temperature in toe range of 105 to I 100. . Sample matrix. Organic soils may have mass losses arising from oxidation and volatilization of organic components, also stony and gravelly soils, both on a mass and volume b ass, can be grossly misleading. PRECISION AND ACCURACY Accuracy and reproducibility of water content measurements, assuming that theweighingprecsicn is consistent with the desired precision of the water content measurements, depend upon the drying technique and how used (whether 24 hours is adequate in obtaining a constant weight). Z iiMtSWU 1.*x' 1 to ' f' filr |!h ASH010571 ejg ej U S ' 1 I EID 129670 EQUIPMENT AND REAGENTS 1 ). Analytical balance accurate to 0.001 g. 2). Oven-dried aluminumweighing dishes. 3). Drying oven with temperature control device that will maintain a temperature betw een1K -110 c . Forced -air circulatingovens will dry samples more rapidly, but convection ovens are sufficient 4) D.esiccators containing active desiccant 5) No reagents are required. WATER CONTENT PROCEDURE 1). Obtain at a minimum 10 to 40 g representative portion of either a ball milled (air-dried),spnple or as received (wet) sample. ! 2). Place in oven-dried aluminum weighing dish. 3) W. eigh the sample to the nearest 0.001 g a s soon as possible. , 4) P.lace the sample in the drying oven and dry it to a constant weight (at a minimum 2 4 hours). 5). Remove the sample from the oven and place it in a desiccator until cooled to ambient room temperature. 6). Reweigh the sample to the nearest 0.001 g. t tw* mmm 7). the water content as percentage of water in the sample on a dry-magjggfif^ W8ter^ %Water Content - iWainht of Wet Sn * Pan - Weinht of Dry Soil * Eao) * 10 ' Weight of Dry Soil -m m s REFERENCES Gardner, W. 1986. Water Content, p. 493-544. In: Arnold Klute (Ed.). Methods of Soil Analysis, Part 1. Physical and MineraJogical Methods. Agronomy Monograph No. 9 (2nd Edition). ASH010572 ^ 135" E X D 129671 3M ENVIRONMENTAL LABORATORY SOIL pH METHOD PRINCIPLE OF THE SOIL pH METHOD Son pH is one of the most indicative measurements of die chemical properties of a soil. W h e th e r j acidic, neutral, or basic has much to do with the solubility of various compounds, the relative bonding of ions to exchange sites, and the activity of various microorganisms. Three soil pH ranges we partlttiraiiy informative: a pH < 4 indicates the presence of free acute generally from oxidationof Mlfries. a pH <5.5 suggests the likely occurrence of exchangeable Al; and a pH from 7.8 to B.2 indicates the presence of CaC03> Soil pH is a measure of tire activity of H+ in the soil solution. Ionized H b in equilibriumwith the adsorbed nonionized H but usually is a small fraction of it Much of the nonioitized acidity is exchangeable only at higher pH. Although other criteria are sometimes used as indices of time needs of and> . requirement is generally a measure of the base (time) required to neutralize that fraction of the total aeidny that must be neutralized to attain a desired soil pH that is favorable for crop groyrth. Hence the activity of in the sod solutions is the intensity factor (index), whereas exchange acidity and lime requirement are the capacity factors of sod acidity. -'* RANGE AND SENSITIVITY The range and sensitivity of the method will depend on the pH meter used. In routine soil testing, it is only necessary to read the pH to 0.1 units. INTERFERENCES Factors that may influence the measured pH include: if >-*>- r The nature and type of inorganic and organic constituents that contribute to soil acitfrty^ wn,, Qi mnywi'c ant*., ( Hydrogen ions may Associate from the exchange sites or maybe displaced by h y q rp v jl.tey fase ;in from The soil/sotution ratio (1:1 is the most commonly used). uiiar-aifeiv ;> mas- The salt or electrolyte content (H+ are displaced by the cations of salts contained in the soils, in addition, the salts also displace exchangeable Al, which upon hydrolysis increases the H+ in solution. , The CO2 content (CO2 irom the atmosphere or soil air) dissolves in water forming caibonic acid (H2CO3) which can lower the pH. In the actual measurement of soil pH, the soil and water are shaken so they come to equilibriumwith the CO2 <nthe air, there is no effect on the pH measurement Only in sods of very low [H+] where the pH is considerably above 7.0 and particularly in soils containing free CaC0 3 does the CO2 concentration of the air has any appreciable measurement effect on pH. Errors associated with equipment standardization and liquid junction potential. The use of 0.01 M CaCfe is recommended to minimize differences caused by some of the above factors. This dilute salt solution masks small differences in salt contents without displacing a large fraction of the H+ or Al3*. in addition, errors due to the liquid junction potential are decreased. PRECISION AND ACCURACY Random variation of 0.1 to 02. pH units is allowable in replicate determinations and can be expected from one laboratory to another. Dehydrated and scratched electrodes will give erratic values. ASH0I0573 1 loo ^ /35~ ' EID 129672 .S-iH'K? if? opmmr- *- ' "f ' i"; ':-<> S wrge tnasnon EQUIPMENT AND REAGENTS 1). pH meterequippedwitha combinationelectrode( orsoilpHelectrode. Cote-ParmerModel #5992-60} and automatictemperature compensation (ATC)probe. 2). Standardbuffets, pH 7.0 andpH 4.0. 3) 50. mLconical, polypropylenecentrifuge tubes. 4 ) A.utomatic pipets. 5 ) G.yratory shaker. 6) M.ilCporeM M TM water. 7 ) . Calciumchloride (CaCig) solution. 1 M or 0.01 M. . pHw AND pHs PROCEDURES 1>- Calibrate pH meterwith commercially preparedbuffersolutionsof pH 7.0 and 4.0 accordingtothe instrument instruction manual 2). Weigh 10.000 g of2.00 mmair-dried soilintoa 50 mLconicalcentrifuge tube. 3 ) W. ithautomaticpipe!, add 10 mL of Mffli-QTMwaterto eachtube. 4 ). Mixthoroughly for 5 minutes, preferably on a gyratory shaker. (Option: mixfor onehour.) 5 ) Le. t stand for 10 minutes. (Option: let standfor one hour.) 6) in.sertthe electrodes into the container. Note; the test mixture after settlingwill have an uPP ^ . , rdte-QTM ** <w , .... 7). 8). 9 ). 10}. while leaving the reference contact inthe supernatant layer. sccontact the wto*t Allowtime fortheelectrode to reach equilibrium(-1 to 3 min.) and record assoil pH in water, pHw- "**.**< s To determinethesoilpH in0.01 M CaCI2. add0.10 mLof 1M Cad2 solutionto tits soilwater suspension. M ix intermittently for 30 m inutes. (Option: mix 30 minutes, let stand30 minutes.) Insert electrodes, andrecordas soi pH in 0.01 M CaCfe. pHa- Alternatively, the soil pH in 0.01M CaCl2 may be determined directly by substituting0.01 M CaCSgforthe water in step 2. 11) If the Timerequirementis tobe determinedonthe samples(pH < 6.9), savethemforthispurpose after reactingthepHworpHs. REFERENCES 9 (2nd Edition). o iol 4 M S ' 1 I EID 129673 3 M E N V IR O N M E N T A L L A B O R A T O R Y CATION - C H A N O ^ C A P A C ,^ (CEC, B V ^ U M SATURATIOH PRINCIPLE OF THE CEC METHOD S o possess an etactiosiatfc chars as a racuH cf ih s k s k e `J S - n .-- . 1-- MPnnlav mddas. ---- O K U tt RANGE AND SENSITIVITY The ransa and sensitivity of rha m alhod are dependant on lh a compBcating interacrions batweaa saturating. 2 l S J M S nm lin^soluiicns and rh. so cnnsMuents. INTERFERENCES Potential errors mdst in W t o S S t "I ' W; Saturation Step. Exchange sites ,f V S Z l o r adsorption sties or mapbrndue to the saturating exchangeable aluminum and its hydro!qr ^ ^ ^ g J L l o n s 1 T h is effect c a u sa s a n undarestim ata readltyexchanged a h ^ " ^ . ^ ^ ^ ^ S l S ^ m s a m a o l o t h a d r d i o n s i n , . O f th e C E C . A n o th e r problem f ^ ' ^ ^ r^ na,e g yp su m and silicate m inerals), saturating solution (dissokilion < oua so f errors. The adsorbed cation m ay be " S ^ . S K T a h ^ c g a n inn. ft m a y h - c-m ns hmu d i f o S s andorginic matter may be lost during d e ^ n g ^ e s o toe n m ^ so!ution may S a a rm c ^ ^ he sLlt is retained. The majority fthesa hks^ b e^ e en interlayers by contraction of expandable sss . replacement during extraction. The e n d ^ aah|a a ations may ^ extracted from zeolites, feldspathoid, axMarfng srrhnion. Thn error givas high CEC cabras. -psaor -TSP'Ppri; . .sm on v t> uis'i , rampfcw ..eating lor *ti .. 8i*ew PRECISION AND ACCURACY sssssss s ss-- ------------------------ I -oU^3i iosl $ /a ~ EID 129674 EQUIPMENT AND REAGENTS ' } 250 mL conical, polypropylene centrifuge tabes. Automatic pipeis. Gyratory shaker. Programmable centrifuge. . 1.0 N, pH 7.0 NH4OAc (Ammonium acetate), identified as Reagert#2: For each liter of solution, add 58 mL of glacial acetic add (CH3COOH) to mL of Milli-QTMwater and then add 70 mL of concentrated ammonium hydroxide (NH4OH, specnic aravity 0.90). It is best to add the NH4OH under a fume hood through a tong-stemmed glasstannel lo that ft is introduced into the bottom of the acid ^ u tto a C o o l the lutionto ^ mtemperatare (-20 to 25 *C) and adjust the pH to 7.0 with either CH3COOH or NH4OH. Dilutethe solution to volume, mix it and store until ready for use. Recheck the pH prior to using the solution. Reagent grade. 2 -propanol (99% isopropyl alcohol). PROCEDURE for cec by sodium saturation Weigh 5 .0 0 0 g of a 0.500 mm air-dried soft sample and transfer the sample to a 250 mL conical, polypropylene centrifuge tube. Add 132 mL of 1.0 N. pH 8.2 NaOAC solution (Reagent # 1 ) ^ ? * ' " gyratory shaker over-night (M8 hours) at 300 to 400 rpm. This is the saturation step. Remove the sample from the shaker and place it in the centrifuge. Centrifuge l 0 rm ^ e 3 dt 3000 ro rH h is W m le n d e d time and speed will be sufficient; a clear supernatant w,ll be Rbtamed. Decant the supernatant and discard the liquid. Particles of soil tost during the decanting steps will effert the final CEC resuft, a tower CEC value is the end result of this which leads to a false interpretation: poor soil quality. Washing the sample is the next step. This eliminates the ^ ^ L dminutes more. Shaker speed should be the same as used in the saturation step. (Total wash time 60 minutes using 100 mL of 2 -propanol.) Add 100 mL of 1.0 N. pH 7.0 NH4OAC (Reagent #2) to the sample, stopperthetabe and shake it on tthhee gyratory shakarover-night (-18 houre). This is ih e m p ^ m e n t step. NOTE: Make sure the identical shaker speed and time are used as in the saturation step. Remove the sample from the shaker and place it ^ n ^ u g a Centrifuga 10 minutes at 3000 rpm and decant the supernatant into a 125 mLpolypropylene bottle. Determine the sodium (Na) content by available methods. e.g. 1CP. ASH010576 2 loi 4 4 1 EID 129675 C ALCU LATIO N CEC EQUATION: , 0.1Nawmfi3- . x 100 - meqrtOOg soil ovetMfeiedweightof soUfe)* *% soil moisture was previously determined. REFERENCES 9 (2nd Edition). Brown. J. R. and D. Warncka. 1988. Recommended M io n Teste and Maasur^crf Cstton Capacity p. 15-16. In; Recommended Chemical SoBTest Procedures for the North Central R e g H M S * * ^ w r Central Regional Publication No.221 (Revised). * * * # * . No ' " ASHO10577 f 1.*ii 3 M t EID 129676 3 M E n viro n m en tal L abo ratory Copies of Chain of Custody, Shipping Papers, Lab Requests \o S -4 sEXD129677 ASHO10578 lm4m lmSHIPPING MEMQRANDUMOm (FOR NO-CHARGE SHIPMENTS ONLY) S h ip t o 4 a 3M E n v ir o n m e n ta l T e c h n o lo g y & 4m S e r v ic e L a b o r a to r y , B -2 -3 E -0 9 4m 935 B u sh A venue 4m S t . P a u l, M in n e s o ta 5 5 1 4 4 -1 0 0 0 4m A ttn : R o b e r t H o w e ll (D ate I |R ou tin g i IF .0.B . | D ate |S h ip p ed I IBA 0 5/08/97 4m Q u a n t i t P roduct Code / D e sc r ip tio n 4m 1 C on tain er o f V ater Sam ples 4m 4m 4m 4m 4m 4m 4m 4m 4m S p e c i a l I n s t 4 m A b so lu te ly m u st a r r i v e F r id a y AM/Time r e s t r a i n t s . F r e i g h t C la s s 4m No. 38-972' W eight 48 lb s 4m 4 m 0 r i g in a t o r VERA L WIGAL Phone 304-863-4895 4mCharge (C ost Code) 8309019511001280 |MSDS S h e e t s R e q u ir e d ? 4mPurchase Order No. (H azardous M a teria l? N 4mValue f o r Customs S h ip From 4 m S to res, B ld g . 4 | MATERIAL CLASSIFICATION 1 |C o rro siv e T oxic |Flam m able O ther 4m 4m| * * AUTHORIZATION * * 0m | 0m I 4m I J0m I 4m I I | 0m ! 4m I jOm & SH-* o -4 lOi> *6 IA S~ VO EID 129678 E ID 129679 Purcheee Ord*r# ______^ u J U J U J L J .L J L J .L J L J l Project Name n ,,0n *Si (J aS $ v S " S r!- J ^ T Prajact Manager &Phene# H p La J 6 ^ ~ Report Copy to: SH 7 .,r F & ~ j l t 7 ^ P fC 'J - RaquaaledComplailon Data: Sampling Requirement* 8DWA MPOES RCRA QTIffiR D O JL- Sample Dlapoaal: Dlaooaa Return Sr 1` eoVrv': ASH010580 LAB TE8T CODES li> * * ANALYSES REQUESTED U b i# Lab 2# to*. Quote# /;** KIIRequeet# Project # .< v: >r . A___ i'_____________ -- N c o f Semple* . tlr .'-i1- Pa* , Of *; " \ . *,* ` U1.*-? v*<. r. *. C O O JIw P .UMSYaT X' `V, jfe iiif {> .V"S8Mi v /tfa l -, * ; YJS M. REMARKS S l* ifc y -,1 0 ^ //V 2 /= Z 7 ,f> 1 WorkAlilhoriied By Instructions and A greem ent P rovisions on R everse s id e Lm4m lmSHIPPING MEMORANDUMOm (FOR NO-CHARGE SHIPMENTS ONLY) Om S h ip t o 4m 3M E n v ir o n m e n t a l T e c h n o lo g y & [Date 06/02/97 No. 38-9732010m 4m S e r v i c e L a b o r a t o r y , B -2 -3 E -0 9 [Routing Ora 4m 9 3 5 B ush A venue 4m S t P a u l , M in e s o t a 5 5 1 4 4 -1 0 0 0 [F.O.B. Date 1Shipped Ora Om 4m A t t n : R o b e r t H o w e ll I 4m Q u a n t it y | 4m 1 I I C o n ta in e r /S o il sam ple I 4m I 4m [B/L >tion 4m 4m 4m 4m 4m 4m I 4m S p ecia l In st 4m Ship O v e r n ig h t 6 / 2 - -M u st b e d e l i v e r e d T u e s . AM 1 1 Weight 1 30 lbs 1 1 1 1 1 1 1 1 1 ! 1 1 l 1 1 1 Ora Om Om Om Om Om Om Om Om Ora Om Om .sh ip u v e m i g h t Om F r e i g h t C l a s s 4m Om Om 4m Om 4m 4 m 0 r i g in a t o r VERA L W1GAL Phone 304-863-4895 Om 4mCharge (C o st Code) 8309019511001280 . ^ jMSDS S h e e t s R e q u ir e d ? , ,. 0 4mPurchase Order No. ^ [H azardous M a teria l? N Om 4mValue f o r C ustom s ' 1 MATERIAL CLASSIFICATION Om S h ip From 4 m S to r e s, B ld g . 4 4m 4m 4m[ I 4m | I 4m | I 4m | [C orrosive I IFlam mable * * AUTHORIZATION * * T oxic O ther 0m [0m | 0m 0m [0m Ora Om ASH010581 10S oL 13. EID 129680 1 RS'/ ` * ENGINEERING CgjTPORP COMPUTATIONSHEET ' * ----------- Ti7i.Z*P^CJ CP3~-C^ SUB- SCT--------------------- n u P a r^T u ^ s / ^ t - lA S & T & fp s-- c -- PHCJ. CH Study NO _______ ______ >o n. i<r-^< /3v*~j i a j \ / ________________ ---------woBKs----------------- -------------- . 12 S3 4 ---------- -------- ---------_ _ _ _ C O ^ T B . - u | S - | 6 1 7 , a 1 9 - g -- a ? * TC2 2 2 3 Z 4 ZS 2 6 Z ? '" 2 8 8 9 3C t N.V t> 2 J A / t s a P C - d S rO)0 Y g> A /^fiLA fi 7 / f - a o S ' Ie ? d l < / 3 ~ r /3A***fi*fi o*s 5* j 3 ^ / f 7 yw%- &**-> 9 10 11 12 13 !4 15 5 .7 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 ^4 35 36 37 (S=/-^ o><= / 3 r S Z O /Z & t-T 3 ^*T. ' 3& H -~ $ ~ .'- f - i l S ' ASHO10582 U S E STANDARDS FOR MINIMUM ESSENTIAL INSTALLATIONS / o ^ /* ( EID 129681 E ID 129682 Form 10620 P -P W O White Environmental Lab Archives PWc* Contractor CanaryDisbursements r lm4m ImSHIPPING MEMORANDUMOm (FOR NO-CHARGE SHIPMENTS ONLY) 1 , ' 0m S h ip t o 4m 3M E n v ir o n m e n t a l T e c h n o lo g y & D ate 1 0 6 /26/97 No. 38-9737950m 4m S e r v i c e L a b o r a to r y , B -2 -3 E -0 9 1R o u tin g 1 0m 4m 9 33 B ush A venue 4m S t . P a u l, M in n e so ta 5 5 1 4 4 -1 0 0 0 JF.O .B . 1 D ate 1S h ip p e d 1 0m 0m 4m A t t n : R o b e r t H o w e ll |B /L 11 4m Q u a n t it y | P roduct Code / D e sc r ip tio n i1 4m 7 I C oolers co n ta in in g w ater sam ples/w ater & ic e 1 4m I1 1 4m 1 1 4m 1 1 4m 1 4m 4m 4m 4m 4m .. 1 1 1 1 1 1 1 1 1 - ^ | W eight | | 40 each * 1. 3 / __ I 11 1 1 1 11 1 1 1 1! 1 i i I1 i i 0m 0m 0m 0m 0m 0m 0m 0m 0m 0m Om Om S p e c iljl I n s t 4mNeed 7 la b e l s , O vern igh t A ir , D e liv e r 6 /2 7 b eforeu n o o n it F r e i g h t C l a s s 4m Om Om 4m Om 4m Om 4 m O r ig in a to r VERA L WIGAL 4mCharge (C o st C ode) 8309066742001280 Phone 304-863-4895 1 |MSDS S h e e t s R e q u ir e d ? Om Om 4mPurchase Order No. o r Custom s Ship From 4raS tores, B ld g . 4 H azardous M a teria l? I N | MATERIAL CLASSIFICATION 1 1 C orrosive T oxic Om Om Om 4m 4m 41m | I 4m 1 I 4m 1 II 4m 1 JF lam m ab le * * AUTHORIZATION * * O ther 0m |0m 1 |0m I1 |0m 1I (0m Ora ASHO10584 1 flj 1 IH 1 i X i T EID 129683 E ID 129684 GH2MHILL Analytical Services LHQ8667 Falriane Drive Montgomery, AL36118-1622 (334)1271-1444 FAX(334)271-3428 LRDSOSOCaterpilar Road Heddlng.CA96003-1412 ,, (916)244-5227 FAX(916) 244-4109 (S1B>74MS7S FfSt (B19) 7474SG0 CVO2300 NWWalnut Boulevard Cwvalia,Oregon 97330-35 (541)762-4271 FAX(514) 762-0278 Project# Purchase Order# RequeuedAnalytical Method# Project Name O u fd A J T Company Hame v J A fifo /J L T O A / It tS h J A J T Report Copytot T 0 T A L # 0 F A /J M fiJ U M J j e M Requested CompletionDate: SiteID Sampling Dale Type Matrix c a iV S A 0Rt0 1 MA 1 R pB L 1 ,H L SampleDisposal; Dhpoee Baum e c LJ CLIENTSAMPLEID (9 CHARACTERS) LAB QC C 0 N T A 1 N E R S rwAM af ij nt . j t / ttA h i Z <3fc 1 VJ i o - \ u \d i . r f4 k | - i. : 5t * 1 Preservative xXx X \o u, A s COC#_ THISAREAFOR LABUSEONLY Lab# Page ol c< Lab PM Custody Review PH Custody Seale Y N lee QC LIVM 1 2 9 OBIr Cooler Temperature Alternate Description YN Lab ID ASH01058 Sem^ByiTOi >A-> M R i f r SpacUlnstmctloMi tasbuetiMis andAgreementP m b h tm an Reverse SMe m a* RellAqulehdBy V ShippedVia UPS Fad-Ex Other. tfz t DaMfrlme Shippinga I L qol OBimUTlO N: Original-LAB, Yatew -LinA*BA,imPMac-*CHant E ID 129685 CH2MHILL Analytical Servies LMQ2667 Patitane Driva Montgomery, AL3(1116-1622 (334)271-1444 FAX(334)271-3426 O LRD5090Caterpilar Road Redding, CA90003-1412 (916) 244-6227 FAX(916)244-41 Projet# Purchase Otti## Projtd Nam* Q f a f l f r v Jt^M ih Ju T A J ( J & - s CompanyName J l f M T ___________ Report Copyte: r A a JiP'p l ) b m L T T E ) ______ Requested CsmpMlnData: Sitalo Sampling lypa Matrix Data Tima Sample Disposal: H*pm Rdum T sr CLIENTSAMPLE ID (9 CHARACTERS) LAB QC JH M t $o LKWCernirAnalyticalLaboratories, Inc. SOBathurst, Un) 12,Waterloo, Ontario, Canada N2V2CS (519)747-2675 FAX(519)747-3606 a CVO2300 NWWWnut Bwdevatd Cavalle, Oregon 97330-3538 (541)762-4271 FAX(514) 762-0276 COC# RequestedAnalytical Method# THISAREAFORLABUSEONLY Lab# Paga Of TP f*"i Uj t- \i> f V\ C u: Preservative H Lab PM Custody Review PH Custody Saala Y N lea QC Laval 1 2 3 Other Cooler Temperatura Alternata Description YN Lab ID ASH010586 a to* Spadai Instructions: (RMMaipffdpUmH) mm| Mudtomind^gvMMlRuiMmoftffMntSHe DataTTIm* DaleTTm* Shipped Via UPS Fad-Ex MtfTIm* 0*#ipandgrinmat) ' D atam i Other. Shipping# (G<s>a DISTRIBUTION; O rigin^-LAB, Y M m -L A B , PMc-CH*tA it E ID 129686 CH2MHILL Analytical Services LMQ 2567 FaMane Drive Montgomery.ALM118-1I822 (334)271-1444 FAX(334)271-3428 UtD 5090 CaterpUar Road Redding, CA96003-1412 (616) 244-5227 FAX(916)244-4108 Project# Purehtee Order* (5,S)7*7-2575 FA*(51)7*7-3 CVO2900 NWwwnui BtNMVara Cavalla, Oregon 973303638 (541)752-1271 FAX(514) 762-0276 Raqusalsd Anriytkal Method Project Name O v & A JT Company Nnw U S A W f W r o A ) W & IC ^ S - u fb /jr_ Project Itanagefcpr Contact APhen# # Report Copy lo: CSScjf W t r * 9 & AaSM.&JHMl17W_ RequestedCompMIenData: StteID Smmpla fflip o til* gr " Sampling TVP Matrix CLIENTSAMPLED (9 CHARACTERS) LAB OC QO & II sj O Preeervallve \J <Sw <1 IA & m * * wfx , 2 *1P coct_ THISAREAFOR LAB USE ONLY Lab* Page of Lab PM Custody Review PH Custody Seals Y N Ice QC Level 1 2 3 O ther. Cooler Temperature Alternata Description YN Lab ID ASHO10587 ----------- IBy f k w ripari )M mm| /nainirttone and AoneamentPlmdatene on Reverse SWe Datsmms RellnquMied By Shipped Via UPS Fed-Ex liftiRf mM r |n*MHUlripWllMt T T z c /r: DewTIms ' Other. i tip Shipping# IL Q C l DtSTmBfJTONiOrlgkmt-LAB, Ytow~LAB, P fn k -G k n t SttSa E ID 129687 CH2MHIU. Analytteal Services LMQ2567 Fabiana Drive Project# (91^244-5227 FAX(916)244-4109 PwvhiaeOtder* g,L S ^ S ^ N 2 V 2 C 5 (516)747-2575 FAX(519) 747-3808 CVO2300NWWalnutBotJsvanl CoivaMa, Oregon 97330-3638 (541) 762-4271 FAX(514) 752-0275 Lab* Project ame & ^P?>a s T Company Kami I A U S U A 7 tn W I r ^ t C S C k jh v T ( M S * ! H M r m ) __ a. m UIm Mai fittaIB RaportCopyto: O F CO f f ' \ Samoli dapoed: V/N 5 LabPM PH coca Pag* of Cuatody Revtew Cuetody Seal* Y N le* Y N itivcaofam^*gntmnlPrBvitomon^mm9*3l<S* E ID 129688 CH2MHILL Analytical Services PLMCI2667 Fabiane Drive Montgomery,AL96116-1622 (334) 271-1444 FAX(334)271-3428 LRD 5090Caterpilar Road Redding, CA86009-1412 (816)244-5227 FAX(916) 244-4109 IT>-O-jf-fCK Purchase Order# Project N*ne LKWCernirAnalyticalLaboratories, Ine. 50 Battant, Uni 12,Waterloo, Ontario,Canada N2V2CS (519)747-2575 FAX(519) 747-3806 CVO2300 NWWalnut Boulevard Covali, Oregon97330-3638 (541)752-4271 FAX(514) 752-0276 coc* RequestedAnalytical Methodf THIS AREA FOR LAB USE ONLY Lab# Page Of -S Dj t b f * r U J M f r i A t a W ConipenyNnne _____ u _________________________________ &Phone# Report Copyto; " n s s y ' R S t0 Z - fy jp e c u H ai RequestedCompletionData: She ID Sampf*Gtipoul; StapON flvton iff Type Matite Sampling Date Unie CLIENTSAMPLE ID (9 CHARACTERS) LAB QC Vj a ix Preservative \b (JL -i Lab PM Custody Review PH Custody Seals Y N Ice QC Level 1 2 3 Other Cooler Timperature Alternate Description YN Lab ID W l X>< zK ASHO10589 ByATHe f k m j hwI>iWm i| 'e ssa i A* flMMlFd|*IIWl4 fWHNnariiMMm) Spadaikratruribna.' IriatruttiOtw aixJA greernerttftptdatoieonR avereaSbte Maxime RelinguishedBy, m hi mnqaMwdBf Dali & ShippedVia UPS Fad-Ex 91m m lifn ri prMMM4 ^ piMMliftripMMM) Datarilme . .. ptarrime ' O ther. Shippinga .L A O .. DISTRIBUTION:Origin!-LAB, Y tB m -L A B . Ptok-Cltonl E ID 129689 CH2MHILL Analytical Services LMQ2607 Fatitene Drive Montgomery, AL38116-1022 (334)271-1444 FAX(334)271-3428 LRD5090Caterpliar Road Redding. CA96003-1412 (916) 244-6227 FAX(916) 24+4109 LKWCaminoAnalytical Laboratori*, Inc. SOBathurst, Uni 12,Waterloo, Ontario, Canada N2V2CS (519)747-2576 FAX(619)747-3606 CVO2300 NWWalnut BoUevaid Cotvalls,Oregon 97330-3538 (541) 752-4271 FAX(514)752-0276 coc#_ 3 Propel* Purchase Olderf Project Name Oufrr/T bJoete Company Name ___ Dv PiMT_____________________ Report Copy to: AMletH H*LTmJ RsquetiedCompieHoti Date: SiteID Sampling iype Matrix Date Time Samp! Diapoul: Q- ttapOM Rtfum CLIENTSAMPLE ID (8 CHARACTERS) LAB QC Requested Analytical Method* CO I V 5 fc & V fe I< Cl ' i Va Preeaivatlve THAREAFOR LABUSEONLY Lab* Page of Lab PM Custody Review PH Custody Seels Y N lee OC Levai 1 2 3 Other Cooler Temperature Alternate Deecriptlon YN Lab ID jy ijS - u s k x * Mm Xx y 2z< ASH010590 SamphABy ATHIt . FtaMitoandpMmM ' w m u zL -jL ? ~ p%midpsBdpHmM piMHaletaiaaMnMl Spedaihtetracnena: JnatrudtoneandAgnement Pmvtotonaon Reveraeria Retiti tim i pH mm* RaHnquMied By 4 ^ 6 EP mmsip andpH mm) DfWTIm . ^A f Shipped Vie UPS Fed-Ex Other. Shipping* i DISTRIBUTION!Origbtl-LAB, Yttow -LA B , Pink-C lbnt E ID 129690 E ID 129691 Environmental Laboratory Request Form - Continued ftimtwao-M-C-PWO SaMy Coneoms/Spodai Handling Comminili ____ 3M Environmental Laboratory Building 2-3E-09 935 Bush Ave. ^ St. Paul, MN55106 Lab Request No. 2 Date Received Page oi A ASHO10592 XT Sample No. Sample Code Sample Dale Sample Description (Range 0-999) -- (12 Character Max)--* 1 M W - 3 - % (MM/DD/YY) -- C / x L / f y (12 Character Max) --# ~3 f K V J - "2. C f n /* \ 4 / z t f n t o f t A \u J - V W j /O 4 / fa y /Jlfe/'C / o / i m u j - s > 2 * /a tf? 7 I ! I I j White Environmental Lao Archives Pink Contractor Canary-Requester Environmental Laboratory Request Form - Continued Forni IOKO-14.C-PWO S&StS iS bS5!H?T53S!b Comments 3MEnvironmental Laboratory Building 2-3E-09 935 Bush Ave. St. Paul, MN55106 T __ TasURaqtirad Sample No. (Range 0-999) -- U- Sample Code (12 Character Max) ft\W - 6 - Sample Date (MM/DD/YY) -+ / > V > 7 Sample Description (12 Character Max) -* / K U J ~ (> l o f * - 3M I.D. (11 Character Stock No.) --# ComputarCoda Clab AVDaia DOate ---.-.-v----i-V---- -------- ----.. * * * < ? . ''. & sm f 2~~ 2*?2. r.w C ?.: -.V - .. '-<. *,,/ *.` .* VVhRo*Environmental Lab rchbss Pink Contractor Canary-Roqwstor U b Rtquail No. RZI46 Dale Received Page ______ 3 of 3 ASHO10593 1 % 5 ~ sr n ts lm4m ImSHIPPING MEMORANDUM)] (FOR NO-CHARGE SHIPMENTS ONLY) 0m S h ip t o 4m 3M E n v ir o n m e n ta l T e c h n o lo g y & ID ate 0 6 /2 4 /9 7 No. 3 8 -9 7 3 7 4 0 . 4m S e r v i c e L a b o r a t o r y , B - 2 - 3 E - 0 9 (R outing 4m 9 3 5 B u sh A ven u e (F.O.B. D ate 4m S t . P a u l, M in n e s o ta 5 5 1 4 4 -1 0 0 0 IS h ip p e d 4m A t t n : R o b e r t H o w e ll I IBA 4m Q u a n t it y P rod u ct Code / D e sc r ip tio n s W eight 0m Om 0m 0m Om 4m 1 4m 4m 4m C ooler o f s o i l s a m p le s/so il & ic e 100 lb s 0m 0m 0m 0m 4m 0m 4m 0m 4m 0m 4ra 0m 4m 0m 4m S p e c i a l I n s t 4m 0vernight-E A G L E USA AIR# wr-i 0m 0m F r e i g h t C la s s 4m ' Om 4m Om 4m Om 4 m 0 r ig in a t o r VERA L WIGAL Phone 304-863-4895 Om 4mCharge (C o st Code) 8309066742001280 ^ (MSDS S h e e t s R e q u ir e d ? Om 4mPurchase O rder No. (H azardous M a teria l? N Om 4mValue f o r C ustom s S h ip From i p s t o r e ,B l d g . 4 ' I MATERIAL CLASSIFICATION i (C orrosive T oxic Om Om 4m 4m 4m| I 4m | 1 4m | I 4m | IFlam m able. * * AUTHORIZATION * * O ther Om | 0m (Om (Om | 0m Om ASHO10594 Ul 4 U S' E ID 129693 EXD129694 CH2M HIU Analytical Services MoLnMtgQom26e6ry7.APLel3it6e1n1e6D-1r6iv2e2 (334J271-1444 FAX(334)271-3428 LR05090 CaleipHar Road Redding, CA96003-1412 ,, (816)244-6227 FAX(916)244-4106 s s a & T S s e x a ttL t.m > ** P1SJ747-267B FAX,19)7,7-3.7 D CVO2300 NWWalnut Boulevard RWpi^re24J276 coc# Project Pureha Older Raquaatad Analytical Method THISAREAFOR LABUSE Of*IV Lab* Page Of Project Name O .J rf- u fic a n iU M J u J fitte Company Name t ' & STOP'S / I *I 28 Lab PM Custody Review /?u A w r v7VmL & 4 ). Project H ^ ^ C o q t ^ h o g . ^ Report Copy lor 4a/M eh/ metXT&O Dei! SttaIDB m u m Im I CA m ntoH flf) tee u tfM X f V l ^ l Type Matrix SampleDisposal: nagae ttriwn |p i t \<30 d- fJf 4 g if t -ii 5*3 Preservative \a * PH Custody Seal V N lee QC Level 1 2 3 Other VN Sampling CLIENTSAMPLEID (9 CHARACTERS) LAB QC Cooler Temperature 3 3 F Alternate Description / g l Lab ID Data Tima fiso X X ^ ><x X X A CUT m n e n V isa \ r 16 ip * 6 ic v ' \L70 y 11 * tC r mm % v ' IC S y V tm * ik 20 - 22 24 zc & k: N/ v M sjj SampledBya Title fa /M -l ReeilvedEy ' Spadai Instruction; fT S tein ptweeindeMnaS DettRlme drtefflme RethiquMiee By U ShippedVia UPS Fed-Ex Other. lip antpHm m ) ripHmm) Dttafflntt/ Date/TIma Shipping* hubvetkm andAgreementPiwMant onRevere Stfe m m B U V O H tO rig M -U m , Y W ew -L A ft HWr-CSeert EID129695 ! CH2MHIU. Analytical Services (334)271-1444 FAX(334)271-3428 LRD5090CatsroHar Road Redding, CA96003-1412 (916) 244-5227 FAX(916) 244-4109 H1kimUlJeVtrUl fff Purchase Order# (5S19) 747-2575 F/aO5C( (519)747-3805 CVO2300NWWalnut Boulevard Corvallis, Oregon97330-3538____ (541)752-4271 FAX(514) 752-0278 RequestedAnelytlcel Method Project Name ^ w m r i J i T v J J tJ K . o a P d f J T r C ~ % S r * i _______ Company Nam ( a / T ^ ajs/ aJ / ^ m l fp e e g lt f Report Copy to; 0 F b J tH S U H M iT & lS RequestedCompMhxi M e : SiteID ,( g & > h tx $ * cC fAW -\ Simple Uepoeil: Hepeee Relea er n IP ol c+* r S i is V's 1 h 'j Prwarvitlva Vs coc#_ THISAREAFOR LABUSEONLY Lab* Pag* Of VO re V rA c* Lab PM Custody Review PH Custody Seals Y N Ice OC Laval 1 2 3 Other YN s- tft 1 1 1 l HmlnrttomBndAgrttmMPtwfohmoriRwwSh I uLnArnBp,MM v*n- O- I* t iima JA4 4 M S ' Environmental Laboratory 3M E n v iro n m e n ta l L a b o ra to ry 935 B u sh A ve. B u ild in g 2 -3 E -0 9 NOT, ........ r \i W S l O T ^ W i l o 'f c h . n i f l . t . Mate) Lab Request No. ** R equest Location . PnonaNo. -------------------------------------------------------------- Date Received K5T ] . . . -- ;----------` " " * . R * '8 n Plant Code ' -1 Environmental Lab .K D r if tf e - f j m h Planning Slates * Quaffly Review S t. P a u l, M N 5 5 1 0 6 i S r i P n r r U /A * siilk U T 7 * J U . a r k s . DpCNo.*(MaihJ Sub. Acci. ' _________________ ciassMoiyproiect no. _ J i _________ Class/Ptfcrlty Date Shaped A ttn : S a m p le C u s to d ia n P h o n e (6 1 2 ) 7 7 8 -6 7 5 0 MUST BE CHECKED Q Yes JS .N o ? > Q g p > I V f f N B M B B _____________ i Safety C oncem s/Special Handling C o n rn tn l ASHO10597 TestiRoquuad SampleNo. (Range0-999) * 1 . ______________ , . . i 2 pc*4------ ----------- Sample Date &Time (MM/DD/YY, HHiMM)....... -- /Z ^ k l 1 6 5 0 Sample Description (12CharacterMax)-------- 0 - 2 / 3Ml.D. (11 CharacterSlockNo.) Computer Code cub I f f c Z f r l IS S I \tl22k ] Uoio 4 ~ (/ e -io ' ........................ _ j S ________________ ------------------------? aJ& Jw w U f ik -is ' ruy,^cr-5YA A &L .PikiA Vare.T? t / f * - La 1 K n,-kC V ia 8 fa /il Form10620*F-PWO SCkL fyl^ B iD P 'rN Sk. 4 U l-VUL-d- *U -P aFU T i t/ %ht f jf a <kiin f/^ rt % fu tfA?> erfja IT <g//f# If If.r 1 White Environmental Lab Archives 'Canary - Disbursements l00ftI-*. s v t Psrt Environmental Laboratory Request Form - Continued Forni 10620* M-C-PW O S55^S5S3!S!^5ST!33B^ 3M Environmental Laboratory Building 2-3E-09 935 Bush Ave. St. Paul, MN55106 Lab Raqua No. K 2582. Dale Received Page _________ 2 - ' of^-1 ASHO10598 Tests Required Sam ple No. L(R ange 0-999) -- __________ ___________ *1 - ft - <\ IO | Sam ple C ode (12 C h a ra c te r Max) " + ti Sam ple Date (MM/DD/YY) -* Sam ple Description (12 C h a ra c te r Max) -- 3 M I.D. (11 C h a ra c te r S to ck No.) -- #> to - 22/ z t f - S f r i !U fO If-# ' tt/& fc 7 H 0 3 -s < / tie fa n fc -S S ' 3 5 -1 0 / Computer Code Clab AVDate DData u ^ 3<s e r \ ............... ___________ - -* f While *Environmental U b Archives Pink Contractor Canary* Requester