Document 6bbzgZrrynJyp8m3O0wZVE6Rm

lPrecise Research. . Proven Results. Analytical Report Fliiprochemical Characterization of Aqueous Samples Decatur Outfall 001 FC Monitoring (E04-0548) Exygen Research Laboratory Report No. L0003445 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Project Lead Jess Eldridge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 St. Paul, MN 55133-3331 .3058 Research Drive State College, PA 16801, USA exygen.com 1 Introduction Results are reported for the analysis of aqueous samples received by Exygen Research (Exygen) from PACE Analytical. The Exygen study number assigned to the project is L0003445. Specific fluorochem ical characterization by liquid chrom atography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 8 samples (including field duplicates, blanks, and spikes) were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Compound Name Perfluorobutanesulfonate (PFBS) Perfluorohexanesulfonate (PFHS) Perfluorooctanesulfonate (PFOS) Perfluorobutvric Acid PerfiuoroDentanoic Acid Perfluorohexanoic Acid Perfluoroheotanoic Acid Perfluorooctanoic Acid Periluorononanoic Acid Perfluorodecanoic Acid Periluoroundecanoic Acid Periluorododecanoic Acid Perfluorobutanesulfonamide (PFB Amide) P eriluorooctanesulfonam ide 2-(N-methvlDerluorobutanesulfonamido)ethvl alcohol Acronvm C4 Sulfonate C6 Sulfonate C8 Sulfonate C4 Acid C5 Acid C6 Acid C7 Acid C8 Acid C9 Acid C10 Acid C11 Acid C12 Acid FBSA FOSA Me-FBSE-OH The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. Only the C8 Sulfonate, FOSA, and C8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis demonstrate the applicability of the method to the additional analytes. 2 Sample Receipt The water samples were submitted in plastic containers. Samples were received at ambient temperature. Samples were stored at 4C from receipt until analysis. Eight individual containers were received. Field samples were collected on 9/21/04 and 9/22/04. Samples were received on 9/23/04. Chain-of-custody information is presented in Attachm ent C. PAGE2 OF5 3 Holding times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 60 days of collection. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis W ater samples were initially treated with 200 uL of 250 m g/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A 40 mL portion of sample was transferred to a C i8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatm ent resulted in an eight-fold concentration of the diluted samples prior to analysis. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based oh the affinity of the analyte for the stationary phase in the colum n relative to the liquid m obile phase, the analyte is retained for a characteristic am ount of tim e. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochem icals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sam ple extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 9/27/04. Samples were analyzed on 9/27/04 and 9/28/04. Raw analytical data is provided in Attachm ent D. 5 Analysis 5.1 Calibration A 9-level calibration curve was analyzed at the beginning and throughout the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, 1000, 2500, and 5000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >0.985 (r2 > 0.970). Calibration standards are prepared using the same SPE procedure used for samples. All calibration criteria were met for this analysis. 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. PAGE3 OFS instrum ent blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical methods. 5.4 Matrix Spikes Field and laboratory spikes were prepared using all compounds of interest. Field spikes were prepared by adding a measured volume of field sample to a container spiked with the target analytes by the laboratory prior to shipping containers for sample collection. Laboratory spikes consisted of aliquots of un-spiked field samples that were fortified at the laboratory at the tim e of extraction. Field blank spikes consisted of laboratory water fortified at the laboratory and shipped with the sample containers to the field and back to the laboratory for analysis. Laboratory control spikes (see section 5.6) are samples of laboratory water spiked at the tim e of extraction. Each type of spike provides information needed to assess analyte stability, extraction efficiency, and matrix effects that may impact analytical results. M atrix spike recoveries are given in Attachment B. Please see Section 5.7 for additional discussion of m atrix spike recoveries. 5.5 Duplicates Field and laboratory duplicates were prepared for each field sample. Duplicate results are given along with the sample results in Attachm ent A. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliq water was spiked with all compounds of interest at 100 and 500 ng/mL during each extraction set. All recoveries for all compounds were between 70 130% in each LCS. Results are given along with the raw data in Attachm ent D. 5.7 Statement of Accuracy Based on results of field spikes, laboratory fortified field samples, field blank spikes, and laboratory control spikes, the analytical accuracy of all analytes is 30% for all compounds with the following exceptions. Results for the C12 acid and FBSA are accurate to 50%. Results for C5 Acid, C4 Sulfonate, and MeFBSE-OH should be considered as screening quality data. The statements of accuracy are based on an overall evaluation of recoveries of field and laboratory spikes, field blank spikes and laboratory control spikes. 5.8 Data Summary Please see Attachm ent A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/mL). Please note that the lim it of quantitation is 1.0 ng/mL for all compounds except MeFBSE-OH and C4 Acid, which have a quantitation lim it of 4.0 ng/mL. 6 Data/Sample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. PAGE4 OF5 7 Attachments 7.1 Attachment A: Results 7 2 Attachment B: Matrix Spike Recoveries 8.3 Attachm ent C: Chain of Custody 8.4 Attachm ent D: Raw Analytical Data 9 Signatures O ther Lab Members Contributing to Data Karen R lsha Date Date PAGE5 OF5 SECTION A L Report1 Analytical 1 Proven Resulte. Summary of Fluorochem ical Residues in Outfall 001 Effluent for E04-0548 Sam ple ID Sample Outfall 001 Sample Outfall 001* Sample Outfall 001 Dup Equipment Blank Field Blank C4 Acid** Perfluorobutyric Acid 35.6 39.6 38.2 ND , ND Analyte Found (ng/mL) C5 Acid C6 Acid Perfluoropentanoic Acid Perfluorohexanoic Acid 8.93 11.1 9.52 11.6 10.4 11.2 ND ND ND ND C7 Acid Perfluoroheptanoic Acid 5.71 5.89 5.76 ND ND Sam ple ID Sample Outfall 001 Sample Outfall 001* Sample Outfall 001 Dup Equipment Blank Field Blank Sample ID Sample Outfall 001 Sample Outfall 001* Sample Outfall 001 Dup Equipment Blank Field Blank Sample ID Sample Outfall 001 Sample Outfall 001* Sample Outfall 001 Dup Equipment Blank Field Blank C8 Acid Perflurooctanolc Acid 22.3 22.8 22:6 ND . ND Analyte Found (ng/mL) C9 Acid C10 Acid Perfluorononanoic Acid Perfluorodecanoic Acid ND ND ND ND ND ND ND ND ND ND C11 Acid Perfluoroundecanoic Acid ND ND ND ND ND C12 Acid Perfluorododecanoic Acid ND ND ND ND ND Analyte Found (ng/mL) C4 Sulfonate C6 Sulfonate Perfluorobutanesulfonate Perfluorohexanesulfonate 149 4.48 168 4.61 ' 149 4.82 ND ND ND ND C8 Sulfonate Perfluorooctanesulionate 22.7 23.5 22.8 ND ND Analyte Found (ng/mL) FBSA 12.8 13.3 12.8 ND ND FSA 2.23 2.28 2.26 . ND ND Me-FBSE-OH** 4.38 4.28 4.28 ND ND ND = Not detected = Response between 0 and 1 ng/mL. **ND = Not detected * Response between 0 and 4 ng/mL. Laboratory Duplicate .\ <J#^m3 0s.3t5S0a5tat8teRCeoselleagrceh, Drive PA 16801, USA VJ: 814.272.1039 F: 814.231.1580 exygen.com. SECTION B CH Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E04-0548 Sample Description Outfall 001 Low Flaid Spiks Amount Spiked (ng/mL) C4 Acid* AmtFound Amount Amt Found In Sample Recovered Recovery in Sample (ng/mL) (ng/mL) (%) (ng/mL) C5 Acid CSAcid Amount Amt Found Amount Amt Found Recovered Recovery in Sample Recovered Recovery in Sample (n g /m L ) (/.) (ng/mL) (ng/mL) (%) (ng/mL) C7 Acid Amount Recovered Recovery (ng/mL) <%> 10 35.6 47.9 123 8.93 37.2 372 11.1 21.3 102 5.71 12.3 66 Outfall 001 High Flald Spiks 250 35.6 .224 75 8.93 856 342 11.1 263 101 5.71 202 79 Outfall 001 Spk C Low Lab Spika 1 35.6 3 9 .2 * 8.93 20.3 * 11.1 12.6 ** 5.71 6.97 * Outfall 001 Spk D High Lab Spiks 500 35.6 1970 387 8.93 3990 798 11.1 816 161 5.71 731 145 Field Blank Low Flald Spiks 10 ND 12.2 122 ND 11.2 112 ND 9.13 91 ND 11.5 115 Field Blank High Flsld Spiks 250 ND 246 98 \ ND 222 89 ND 240 96 ND 246 98 Sample Description Outfall 001 Low Flald Spika Amount Spiked (ng/mL) Amt Found in Sample (ng /m L) C Acid Amount AmtFound Recovered Recovery in Sample (ng/mL) (%) (ng/mL) C9 Acid C10 Acid C11 Acid Amount Amt Found Amount Amt Found Amount Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery (nfl/mL)_____ (%1,, .. (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%> 10 22.3 28.5 62 0.0421 6.44 64 0.0128 6.99 70 ND 6.98 70 Outfall 001 High Flald Spika 250 22.3 236 86 0.0421 264 106 0.0128 267 107 ND 281 112 Outfall 001 Spk C Low Lab Spika Outfall 001 Spk D High Lab Spika 1 500 22.3 22.3 23.5 697 * 0.0421 135 0.0421 1.33 129 711 . 142 0.0128 0.0128 1.23 782 122 156 ND ND 1.25 880 125 176 Field Blank Low Flald Spika 10 ND 11.3 113 ND 11.2 112 ND 10.9 109 ND 12.3 123 Field Blank High Flald Spika 250 ND 247 99 ND 251 100 , ND 250 100 ND 241 96 ND = Not detected Response between 0 and 1 ng/mL. *ND N ot detected = Response between 0 and 4 ng/mL. J ^ 3 035058 Research Drive iT m s tSatatte College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com CH Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E04-0548 Continued Sample Description Outfall 601 Low Flald Splka Amount Spiked (ng/mL) C12 Acid______________________ C4 Sulfonate____________________ C6 Sulfonate____________________ C8 Sulfonate Amt Found Amount Amt Found Amount Amt Found Amount Amt Found Amount in Sample Recovered Recovery In Sample Recovered Recovery in Sample Recovered Recovery in Sample R ecovered R ecovery Ino/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) 10 ND , 4.31 43 149 178 ** 4.48 14.7 102 22.7 32.1 94 Outfall 001 High Flald Splks 250 ND 216 86 149 1010 344 4.48 311 123 22.7 341 127 Outfall 001 Spk C Low Lab Splka 1 ND 1.11 \ 111 149 159 " 4.48 5.74 " 22.7 24.7 ** Outfall 001 Spk D High Lab Splka 500 ND 874 \ 175 149 1890 348 4.48 614 122 22.7 665 128 Field Blank Low Fiold Spiko 10 ND 10.3 13 ND 10.2 102 ND 11.0 110 ND 10.8 108 Field Blank High Flald Splka 250 ND 177 71 ND 256 102 ND 252 101 ND 248 99 Sample Description Outfall 0 0 i Low Flald Splka Amount Spiked (ng/mL) FBSA FOSA Me-FBSE-OH* Amt Found Amount Amt Found Amount Amt Found Amount in Sample Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery (ng/mL) (ng/mL) {%) (ng/mL) (ng/mL)_____ (%)___ (ng/mL) (ng/mL) (/.) 10 12.8 23.9 111 2.23 12.4 102 4.38 17.3 129 Outfall 001 High Flald Splka 250 12.8 389 150 2.23 338 134 4.38 0 0 Outfall 001 S pkC Low Lab Splka Outfall 001 Spk D High Lab Splka 1 500 12.8 12.8 14.3 964 " 190 2.23 2.23 3.48 763 125 152 4.38 4.38 4.07 496 " 98 Field Blank Low Flald Splka 10 ND 10.7 107 ND 12.2 122 ND 8.35 84 Field Blank High Flald Splka 250 ND 242 97 ND 256 102 , ND 320 128 ND = Not detected = Response between 0 and 1 ng/mL. \ *ND = Not detected = Response between 0 and 4 ng/mL. . " Sample residue exceeded the spiking level by more than 4 times; therefore an accurate recovery cannot be calculated. J ^ 3 03055f8 Research Drive x r m s tSataite College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com SECTION C 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 i p i i f i f s p r e r e n p T Login #: P ro je c t: 3555 P0000689 Company Name: 3M Subm itted By: Jess Eldridge Login Type: Im m ediate Receipt o f Sam ples S ta rte d : True Date Start: 09/23/2004 Due Date: 10/23/2004 Received Date: 09/23/2004 Received By: Am m erm an, M ark Spread Sam ple: Label: Exygen SD/PI: Risha, Karen Project Title/Type: D ecatur O utfall 001 FC M onitoring / ROUTINE Login Notes: Conform Notes: ;ontorm am pie: Conform COC: Conform Sam ple: Conform Request: rue True True True Package PK0004220 C a rto n Packages / Containers Mail Date / C ondition S h ip p e r/ ID 9/23/2004 2:08:11PM Package & Contents Uncompromised FEDEX 8479 6709 6571 Temp. Control/Tem p. None 23.4 D irection / Handled By RECEIVED Ammerman, Mark Container # C0045991 C0045992 C0045993 C0045994 C0045995 C0045996 C0045997 C0045998 Gross Weight pH Container Type 615.70 g 500 ml Clear Plastic Narrow 612.20 g 500 ml Clear Plastic Narrow 595.50 g 247.40 g 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 255.00 g 261.30 g 257.90 g 258.10 g 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow Preservative NONE NONE NONE NONE NONE NONE NONE NONE Mfg. Lot Mfg. ID 9/23/2004 Login.rpt Report Version: Sep 3 2004 9:36AM Page 1 of 2 Instance: R0121893 ^ Sample ID L0003445-0001 L0003445-0002 L0003445-0003 L0003445-0004 L0003445-0005 L0003445-0006 L0003445-0007 L0003445-0008 Container C0045991 C0045992 C0045993 C0045994 C0045995 C0045996 C0045997 C0045998 Matrix LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID Fraction Water Samples Sample Equipment Blank Water Sample Outfall 001 Water Sample Outfall 001 Dup Water Outfall 001 Low Spk (10 ppb) Water Outfall 001 High Spk (250 ppb) Water Field Blank Water Field Blank Low Spk (10 ppb) W ater Field Blank High Spk (250 ppb) Date Sampled Date Received Date Due 09/21/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 09/22/2004 09/23/2004 10/23/2004 9/23/2004 Login.rpt Report Version: Sep 3 2004 9:36AM Page 2 of 2 Instance: R0121893 raceAnalytical* CHAIN-OF-CUSTODY / Analytical Request Document The Chain-of-Custody Is a LEGAL DOCUMENT. A ll relevant fields m ust be com pleted accurately. , R e q u ire d C lie n t In fo rm a tio n : Section A Address e ri s s 9 T j n ) m - n a f" Required Client Information: Kep> - CopyTo: ^ Invoice To: r ^ s s. Section B eu ren t. ' _____________ Page: 4 of J Client Information (Check quote/contract): Requested Due Date: *TAT: P.O. Project Name: {JCCq T w ^ i K o uhne , P C fflcrtiJdnrt*, 3 f r i t Project Number: OUrfitM-L OO! 'Turn around time less than 14 days subject to laboratory and contractual obligations and may result in a Rush Turnaround Surcharge. Turn Around Time (TAT) in calendar days. 857010 To Be Com pleted by Pace Analytical and C lient Quote Reference: Project Manager: o < f-o z t8eProject #: Profile #: Section C Section D Required Client Information: SAMPLE ID One character per box. (A-Z, 0-9 /.- ) Sample IDs MUST BE UNIQUE Valid M atrix Codes MATRIX DRINKING WATER GROUNDWATER SURFACE WATER WASTE WATER PRODUCT SOIL O IL WIPE AIR OTHER CODE DW GW SW WW P SL OL WP AR OT ORIGINAL (0 0 ^ < U n ri^ Instructions for completing Chain of Custody (COC) -Y. Complete all Client Information at top of sheefoname, address, phone,.contact (person to whom report will be sent and contact can be made if questions^arise),- billing information $ different from client, PO#, Project Name and/or Project Number as it will appear on the report. 2. Quote Reference, Project Manager, Project No. and Profile No. will be completed by Pace. 3. - A separate COC must be filled out for each day of sample collection. 4. Sampler should print their name ib % sp ap f RtQvsidpd and sign their namfeifollowed by the date of the sampling event. , I ~y: . c ' .. ; "*.> "v;j - * H V a> W 1- .*4 .j ? ' ^w ' 5. Complete Sample Description asnhwill appar,on\the -laboratory/report; jpolude tirfre of-sapipllqg, sample matrix, no. of containers and preservative-used. 6. Analysis Requested: Complete analysis on the lines provided and place a check in the column for the samples requiring the analysis. It may be necessary to use the space provided for additional comments or include attachments for extended lists of parameters. 7. Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation. * IMPORTANT NOTE: Standard Turnaround Time is 2 weeks. If this does not satisfy your requirements, arrangements must be rhade prior to samples being submittedbiathe laboratory. Contact your project manager. ' Special Project Requirements such as Low Levdl Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) ., ' / * 2 faceA nalyticqr ' S.CM Required Client Information: Section A Company 3m e rf ss Address CHAIN-OF-CUSTODY / Analytical Request Document The Chain-of-Custody is a LEGAL DOCUMENT. A ll relevant fields m ust be com pleted accurately. Required Client Information: Report To: c o p y'T o : Section B ' Page: / of , 857010 # To Be Com pleted by Pace A nalytical and C lient Quote Reference: ClienHntormation (Check quote/contract): Invoice To; Requested Due Date: ` TAT: Project Manager: m PrtiectNam e: 0 t C d h * r >^* AL-A ^ K o u h d Z P<L fflOrfrknAtj 3 oTK\ Project Number: OUTfiftt-L- Q Qt ` Turn around time less than 14 days subject to laboratory and contractual obligations and may result in a Rush Turnaround Surcharge. Turn Around Time (TAT) in calendar days. M ____ Project #: P rofile #: Section C NC SC GA I Other NPDES GROUNDWATER DRINKING WATER UST RCRA Other:__________ SAMPLE CONDITION SAMPLE NOTES Temp in C Received on Ice Y/N Sealed Cooler Y/N Samples Intact Y/N Additional Comments: ^ Ij ,0 / 'fr it ~r O / fe """ 1 - - -------* _ f0o<7 _____________ ` Q`O l ^ ( 0 - c itfa rin g ________ * 2 (0 0 ^ t Z b T ^ \ : ^ - J k 9 = r -- -- 7 f * 4 y --1p----/--------- ^/ - =^ ------------- // r J f 9--__------- r/c/o SAMPLER NAME AND SIGNATURE * I PRINT Name of SAMPLEST (L U ( o f - f a 's t SIGNATURE, LR DATE Signed: (MM / DD / Y Y ). 9 / >/ - * * / c y in e m u c o O ta R u p sfl IoitylcnA X Y O O T 8 U O -1 0 -H IA H 3 V .W'-.. a iviuic. fc-V,5! *'A TV3 MAJO0 0 KD?. J a a ^-uO ^o-m srt^ ' I Y ^ ii S xM 0 noi*"o3 ?o -sgs*! u-jvugefl \6 o \ty \e n A 9 o e fl -3 h- rjSD.WWW A nO i)"`:S3 bv^O b -ptiR - . ^ , .;rnr-5| Instructions for comptetrn^iMiain of Custody (COC) 1. Corhplete all Client Information hwufHioirnuT address, phone,, contact, (pefson to whom report will be sent and contact cart^ benmadeiiiluquestions arise), billing information if different from client, P O IL Project Name and/or Project Number as it will appear oh the re p o rt." i o'r;! ]:;3110 0 n o il:.:3 8 Qqote Reference, Project Manager, Project No. and Profile No.jwill.be c o m p lie d by Pace. . '* ` \ | ; ; ; ; !- ; :j j , J j ! //w !j . Q I 3 Ji "1 '1 %S 3 r A separate COC must be filled out for each day of sample collection. ;.e: ?.:o>dd i,ri-'<i] .e!.'. enO 4. j Sampler should print their! pamd in the space pm vidpd and s ig n th e irn a n ie followed by thq date; of; j the sampling event. ! ! L , 1 j> ! i : ' i ; : . 1| : i ; ' l| L !' i ! : ;< ! '-! 4'- ; 1 b ' v ' m o * 5. jComplete Sample description ps it will appear on ,the laboratory report; include tin # o f.s iip ? liijg , sample matrjxj no; pf ppntainerS and preservative used. ; . ,, j , j |r ! t V .. , ,4 ; ^-J0' . \ ( 6. Analysis Requested! Complete analysis on ttje lines provided ahd pljace a chepk in the column for the samples requiring the analysis. It may be necessary to us the spade provided for additional comments or include attachments for extended lists of parameters, j ; j \j iiWt, *'^1; 3* m 7. Submission b f| spm plesitq laboratory:;Indicate Item Number of those sajmple$ being transferred;! sign relinquished by, and include your affiliation. . ' ' ! i ; ' i M i ' * IMPORTANT NOTE: M i !1 must be mcfiT prior to sainples being s u b iriiiB S ib in e iaboiaAuiy. ^u itra r b i 'P'i'Ojebl 11IUIId^l 13&O T3U Li Special Project Requirements such as Low Le v|l Detection Limits or level of QC reported#-rtbM be indicated ion the chair! of custody. (Use Additional Comments Section.) ., ' -OiTiC/.OO 3 ? M A S U!W !f ac1no ,,.J /f\/ .7 O O J nb i/L ' j .Mb'M ' "T* y-:S raceAnalytical* wawjMetiafe* Required Client Information: 3 m e r f s sCompany Section A Address CHAIN-OF-CUSTODY / Analytical Request Document The Chaln-of-Custody Is a LEGAL DOCUMENT. A ll relevant fields must be completed accurately. Required Client Information: Section B ___________________ 857010 for.Report To: CopyI TTao*: s. fldr, eke. * Page: / of j To Be Com pleted by Pace Analytical and C lient Quote Reference: Client Information (Check quote/contract): Invoice To: Requested Due Date: TAT: Project Manager: Section C P.O. *Tum around time less than 14 days subject to Project Name: ->e-e*-"er-' " ~ j l A . laboratory and contractual obligations and may result in a Rush Turnaround Surcharge. Ko{J P C l r ir h r tflt) 3 n i A. Turn Around Time (TAT) in calendar days. Fax h>)7W - 2& Project Number: -- OUT f a n OOt ~ ________L___ . ._ S e ctio n D Required Client Informatio i: Valid Matrix Codes MATRIX CODE DRINKING WATER DW GROUNDWATER GW SAMPLE ID SURFACE WATER SW WASTE WATER WW One character per box. (A-Z, 0-9 /.-) Sample IDs MUST BE UNIQUE PRODUCT SOIL O IL WIPE AIR OTHER P SL OL WP AR OT COLLECTED START ^ --------- DATE TIME END DATE TIME Preservatives 1C<ICO5M 01zCOoX XozCOzCj [ p \s 4 t M L j 2?f " i fi\ k V c r Ate u O k / / a btm OtJ t r .r S Mill ft KZ t aiM D nrot 7 1 l u r*\ d L Wc 1 1JiigSfc 0 7; b 2 ^ fs> 2 i ' ' % V o r G Zr Ifrf C 1 U '-, 3 l/W c e r Sy--T : r . /0C> /o o S \ */-4 y o ? & - 1 ^ ief I y k 3 0 $ t i c 1 fl2 j(o < i i o 5 L < 1 t ------- V -- 3 n |>v-. 111 t-r. ' t. M ATRIX CODE SAMPLE TYPE G=GRAB C=COMP. SAMPLE TEMP AT COLLECTION Unpreserved WT i Project #: to y -o s tS Profile #. / q Tr f Hf y / // // / / / / / > i > ---- 1 U f, /Remaries Lab ID IS - IS !f 1__ 1 ,, _ SITE LOCATION REGULATORY AGENCY NC SC GA Qther NPDES GROUND WATER DRINKING WATER UST RCRA Other_________ SAMPPLUE CONDITION SAMPLE NOTES Temp in C R eceived on Ice Y/N U ife y . . ' )> / s j , 7-fO i - "> 7A i_ tv 0- - /"6 ^ / L c i* f 6,,o < L Sealed C ooler Y/N S am ples Intact Y/N Additional Comments: fa /b i ` Oos 0 0 1 rvjC- V^ 3 ( 0 0 ^ d r Pb Vis/ i RELINQUISHED B Y /AFFILIATIO N JLDATE i TIM E I ACC EPTED BY / AFFILIATION DATE TIME SAMPLER NAME AND SIGNATURE ~fPRINT Name of SAMPLER^ q C jZ fo l b 'S i DATE Signed: (M M /D D /Y Y ). 9/ jn d m u o o G la su p o fl !o ily!sn A \ Y q 0 T 3 U 0 -1 Q ~ K B 0 _Vy* TWr* DC .jO-IO- 0 notloeS .-.srO Q : vT jiTi a ncitooS I om le ir ' r 51l. >fi .1 .vA \ oT .oc:'. .oi o:i'voi H. >0**092 . . -. - r,,: q.qiB nuT* i . '; X 1. Complete al Client lnfrmation''at:td ^ li^ .M ||^ ^ |g L m o , address, pinone, contact (person to whom report will be sent and contact can be m ade ifufijyfistians arise), billing information if different from \ . . client, 3roject Name and/or Project Number as it will a'ppear oh the report. " \ \ ' r v \ v-,\ x2 . uote Reference, Project Manager, Project No. and ProfilCNQ-iwill b dprriplifed by Pace. v - A ' ." . i \ .: i : !' /-31i Gl 3 J R M A 8 '-ni .03 :.; : C nO?.r.>,AiKp 4\ J V Sc \\\ \ \ ' t;o ', o : e bplfectiob. v-W .rod \ (l-i) **o an S-A; -a 3 u c ; / u 8 V3UM -.ai *lqrp&3 . jSampler should print their ipam initmspaqq `pn^dfed ^d, sign;theif nan^, fqlipwpd by thq date of | , C l thesam pling event, i ; , ! N i ! j ^ " ; 1 J ;* l ;: ' ' 1 v" ' ' ' ' 1 ` ' A 1 4 ' i Lt 5.;Complete!simple Description as.it.will appeanon.the laboratoiiy jsample matrix, no^ of cqnfainers^and presery^tive used. | J report; .:> include j . thfoi jj of s`^lu1m.'p,.ing, ' ' ^^ 4. "y ; -v -v y IL* : !6. jAnalysis Requested; Complete analysis on the fines provided ahd place a chepk jn tjhe column for, j the samples requiring the analysis, it may be necessary to use the.space provided for additional: 1 1comments of ; 7, Submission of samples to laboratory: Indicate Itenrj Number of those samples beirig transferred; sign relinquished by, and include your affiliation. ; 1i ! ' i ; ! IMPORTANT NOTE: m*P, If this does not satisfy your requirements, arrangements c, iO rau Special Project Requirements such as Low Detection Limits or level of QC repOif^f-iffiMs! be indicated on th4 chain of custody. (Use Additional Comments Section.) npirrirwi`'twwt - - ; ; -j.; [_ ___ __ -Ittitp G MOITiUviCO 'jJv.JU2_ ' 0 " ni qneT /1G ! 90i no ; .. >`.H 1/1'X' 1 A _li, jI, . . . f~\ ... J f^:Sbb4 'aceAnalytical* R e tir e d Client Information: Company 3 /7 7 e Address SGCtiOF) A rf ss CH/UN-OF-CUSTODY / Analytical Request Document The Chaln-of-Custody is a LEGAL DOCUMENT. A ll relevant fields m ust be com pleted accurately. Required Client Information: Section B _____ ______ 857010 Report To: oe ? r. J ? S 5 S . f i d r . clrf e Copy To: Page: t of A To Be Completed by Pace A nalytical and C lient Quote Reference: Client Information (Check quote/contract): Invoice To: Requested Due Date: Project Manager: Section C Phpne Fax P.O. Pn ^ u i iNluaiMmve.: [)C -- q fu /V -- Je- Ofj F C G/fi Project Number: o u > Ta l l o d i *Tum around time less than 14 days subject to laboratory and contractual obligations and may result in a iRiuu- sa hii Tl uuiri Knauruouunnud gSuuiruchi aairygce.. , Turn Around Time (TAT) in calendar days. S e ctio n D Required Client Information: S A M P L E ID One character per box. (A-Z, 0-9 /.-) Sample IDs MUST BE UNIQUE Valid M atrix Codes MATRIX DRINKING WATER GROUNDWATER SURFACE WATER WASTE WATER PRODUCT SOIL O IL WIPE AIR OTHER CODE DW GW SW WW P SL OL WP AR OT i4 ? -- JOl '*rr k 2 * 0 ' i U Q /v7 l i . O O-L ? E O l i > /1 t o r 1r IJZ r 2\ uT j n. , 7r IS ile -MJ IL 0 l 1 ,/4 h ft 2 u H i of G llll e c 1 Preservatives COLLECTED START END DATE ^ TIME DATE TIME 0CO 0 CO 1w 0zCO 0 XX X Od CO <z3 9 z /i, - i| /$'- j 'I: ^ lc ? o 5 1 %c i tOM'S f.W it>s j o 5 I a ......... v ; V ^ ....... -- * MATRIX CODE SAMPLE TYPE G=GRAB C=COMP. SAMPLE TEMP AT COLLECTION Unpreserved Methanol Project #: Profile #. Analysis: <D .C O r- *Prg;-; . 1 S:! * . Ill l-Vr; |G - -* ... j SITE LOCATION REGULATORY AGENCY NC SC - GA ] OQtlher________ NPDES GROUND WATER DRINKING WATER UST RCRA Other_________ SAMPLE CONDITION Temp in C SAMPLE NOTES ri1 ^ y RELINQUISHED BY /AFFILIATIO N j DATE | TIME I ACCEPTED BY / AFFILIATION DATE I TIME V ^ - U e r ---------------- p /l ----- ' / ------------ f /------, f-:i ----------- R eceived on Ice Y/N Sealed C ooler Y/N Sam ples Intact Y/N Additional Comments: 4 0 ' / ^ / _ uO*-,, ..... " ~7P~ f i AH- G OI (C. !} \ O HiM K o I i 1 r< I ' f ,;J T :/. t ^ v * - ^ J- SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER*. ___________ SIG NYU R EjJ SAMPLER: DATE Signed: (MM / D D / YY)> 9 / -> / - * A / 0 y  I0V ? 8 's-'A ' Y - TBW .. **\ ' - a/:- * V' >1 ,,a H Instructions for completing Chain of Custody (COC) 1. Complete-all' Client In fd fffl^ fltf laMisg' address, phone, contact (person to whom report will be sent and contact can be m ade ^questions arise), billing information if different from client, P O # /Project Name and/or Project Number as it will appear on the report. | \ .. - V 5. - -.1 2. Quote Reference, Project M e a g e r, Project No. and Profile No. will be completed by Pace. ; : i! J -1 ; ' '} 3. A separate COC must be filled out for each day of sample collection. >, 4. Sampler should print their name in the space provided and sign their name followed by the date of the sampling event. \ ; 5. Complete Sample Description as it will appear on the laboratory report; include time of sampling, sample matrix, no. of containers and preservative used. V 6. Analysis Requested: Complete analysts-ofvthe lines provided and place a check in the column for the samples rquiring the analysis. It may be necessary to use the space provided for additional comments or include attachments for extended lists of parameters. 7. Submission of samples to laboratory: Indicate Item Number of those samples being transferred; sign relinquished by, and include your affiliation. * IMPORTANT NOTE: Standard Turnaround.Time is 2 weeks. If this does not satisfy your requirements, arrangements must be made prior to samples being subm ittM bM the laboratory. Contact your project manager. Special Project Requirements such as Low Levtfl Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) 9/22/2004 Project: E04-0548 3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report Page 1 o f2 R equester: Schnobrich, D ana M (223-1N -08) D epartm ent: 530711 Project N um ber 0022674449 D ate R eceived: 8/4/2004 P roject D escription: D ecatur O utfall 001 FC M onitoring Q uarterly Com m ents: C om pletion D ate: Project Lead: Jess S. E ldridge Phone N um ber 651-778-5233 E m ail A ddress: jseldridge@ m m m .com Project Results/Activitv P ace F ield Sam pling E vent 3M Sample Number Sampled Date Sample Description E04-0548-72462 9 /2 1 /2 0 0 4 Outfall 001 Effluent - Composite LAB EXYGEN Analytical Method LCMS E04-0548-72463 9 /2 1 /2 0 0 4 Components PFOS Result PFHS PFBS FOSA PFBAmide MeFBSE-OH C 4acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid Outfall 001 Effluent - Composite Duplicate LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C 6 acid C7 acid PFOA C 9 acid CIO acid C ll acid Result RL RL Qualifier Qualifier 9/22/2004 3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report Project: E04-0548 (coot.) 3M Sample Number Sampled Date Sample Description E04-0548-72463 (cont.) 9/21/2004 Outfall 001 Effluent - Composite Duplicate LAB EXYGEN Analvtical Method LCMS (cont) Cooinonentx C12 acid Result E04-0548-72464 9/21/2004 Field Control/Travel Blank LAB EXYGEN Analvtical Method LCMS Comoonents PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C 4 acid CS acid C 6 acid C7 acid PFOA C 9 acid CIO acid C l I acid C12 acid Result E04-0548-72465 9 /2 1 /2 0 0 4 Equipment Blank LAB EXYGEN Analvtical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C 5 acid C 6 acid C7 acid PFOA C 9 acid CIO acid C ll acid C12 acid Rwult Page 2 o f 2 L Qualifier RL Qualifier RL Qualifier . USAirbill Express a r- J hy (.Ou* 47% 70U 571 Recipient's Copy 7<3y s89~^sn 4a ExpressPackageSanies 1X T * * Priority Overnight fj ^ \ N a a b u M M morning* ' I- ] FedExStandard Overnight t-- I N t t b u i a w i abamuun* naftss. Q MExExpressSever fMg _____ I I FedExFirst Overnight '-- ' M M m tfe w iM W 'M f it in t fW n ry n li.H iitiw r _P/kCompany _Am iif 'kfj S e r v i e B< ____ T 2 f ff l _ K i t ^ y 4 u * - k s v iiii /lu e . > t/c J c T t r )O Q 4b b^MaaHwgNtSaivica FedExTOeyfreight Q ME3QyFreight 5 M 6t M b tP a k* FedEx Tmakea ^ b th e r M r John - II fZ yytjfM Recipient's Address We cannot defiverto P.0, boxes or P.0. ZIP codes. Address " 3 S 'f i R s h ^ -8 J g |-3 3 < 7 K ? P S , r a r c l i __________________ Oept/Roia/Suitafftoom E V t\/ - Handling I^ I A0*ww*W*ftKte.MfflfEtcY^2WOx2^&M0faEioyxrity H # t b H i u Z i p codas lf--~)1EESSESmS*Zm* ...... - *** h h r 1 ^ I 5 >* jr ' * _ _ . f..c..*... Shipper's Declaration notreqiiired Dangerousgoodsfmckjdwyg Dry !ce| cannotbe stuped in FedExpackaging. ri (fcyfc* I-- I DryIlcea,99,,Ut N t845 _ I I Cargo Aircraft Only Payment BXito: V:A \to tfe ii E tfw FedExA c c i No. or C retfitCard No.below. - Recipient Third Party Credit Card ObtainRecip.j 1 Acci No. I-- I Cashffihack * " ' r i ' :f r k -\ y v jd x h>- .. . 1; v j'M ^ Cto S ' f a ' f e . C $ ) ) p ^ Q _ ama ap * / % # } m Jr h w g d t e S W u n l ^ ^ o ^ d B ^ r e j J ^ w value. See beck fe r datai. u . . ...... _ . t a s t e deliver this shipment w ithout obtaining a signature m i aeneto indemnifyandhold us harmless from any resulting claims. [HfcTl