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Analytical Report Fluorochemical Characterization of Aqueous Samples Decatur Outfall 001 FC Monitoring (E05-0543) Exygen Research Laboratory Report No. L0006004 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Gary , Hohenstein Environmental Manager, Special Projects, EHS Operations 3M Bldg, 42-2E-27 St. Paul, MN 55133 L.3058 Research D rive kState College, PA 16801, USA PAGE 800.281.3219 ,F: 814.272.1019 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 L0006004. Specific fluorochernical characterization by liquid chromatography / 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 PerfluoroDentanoic Acid Perfluorohexanoic Acid Perfluoroheotanoic Acid Perfluorooctanoic Acid Perfluorononanoic: Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide (PFB Amide) Perfluorooctanesulfonamide 2-(N-methvloerluorobutanesulfonamido)ethvl alcohol Acronym 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 8/23/05 and 8/24/05. Samples were received on 8/25/05. Chair-of-custody information is presented in Attachment C. PAGE 2 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 mg/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 treatment 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 on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. 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 miid temperature; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard H P 1100 HPLC system coupled to a PE Sciex API 4000 M S/M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 8/31/05. Samples were analyzed on 9/27/05. Raw analytical data is provided in Attachment 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 .9 8 5 (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. PAGE 3 OF5 Instrument 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 5.5 5.6 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 time 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 time of extraction. Each type of spike provides information needed to assess analyte stability, extraction efficiency, and matrix effects that may impact analytical results. Matrix spike recoveries are given in Attachment B. Please see Section 5.7 for additional discussion of matrix spike recoveries. Duplicates Field and laboratory duplicates were prepared for each field sample. Duplicate results are given along with the sample results in Attachment A. 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 Attachment 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 C6 Acid and C10 Acid are accurate to 40%. Results for C12 Acid, C4 Sulfonate, and FOSA are accurate to 50%. Results for the C5 Acid should be considered as screening quality because of high and variable field and laboratory matrix spike recoveries. 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 Attachment A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/mL). Please note that the limit of quantitation is 1.0 ng/mL for all compounds except MeFBSE-OH and C4 Acid, which have a quantitation limit of 4.0 ng/mL. PAGE 4 O F5 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. 7 Attachments 7.1 Attachment A: Results 7.2 Attachment B: Msitrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data 9 Signatures Other Lab Members Contributing to Data Karen Risha Amy Sheehan PAGE 5 O F5 Section A Analytical ^ Report L Summary of Fluorochemical Residues in Outfall 001 Effluent for E05-0115 C 4 A cid** S am p le ID Perfluorobutyric Acid Outfall 001 Effluent , 16.4 Outfall 001 Effluent* , 14.0 Outfall 001 Effluent Dup 19.4 Travel Blank , ND Equipment Blank , ND A nalyte Found (ng/m L) C 5 Acid C 6 Acid Perfluoropentanoic Acid Perfluorohexanoic Acid 2.53 2.68 2.49 2.75 2.36 2.54 ND ND ND ND C 7 Acid Perfluoroheptanoic Acid 1.35 1.32 1.27 ND ND S a m p le ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank C 8 Acid Perfluorooctanoic Acid 8.52 ,7.63 8.14 ND ND A nalyte Found (ng/m L) C 9 Acid Perfluorononanoic Acid C 10 Acid Perfluorodecanoic Acid ND ND ND ND ND ND ND ND ND ND C11 Acid Perfluoroundecanoic Acid ND ND ND ND ND S a m p le ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank C 12 Acid Perfluorododecanoic Acid ND ND ND ND ND A nalyte Found (ng/m L) C4 Sulfonate C6 Sulfonate Perfluorobutanesulfonate Perfluorohexanesulfonate 24.8 ND 24.9 26.8 ND ND ND ND ND ND C8 Sulfonate Perfluorooctanesulfonate 20.3 19.4 21.0 ND ND A nalyte Found (ng/m L) S a m p le ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank FBSA 9.23 8.43 8.66 ND ND FOSA 3.61 3.47 3.48 ND ND M e-FBSE-O H** ND ND ND ND ND ND = Not detected = Response between 0 and 1 ng/mL. **ND = Not detected = Response between 0 and 4 ng/mL. 'Laboratory Duplicate 0006 J ^ 3 0,3505f8 Research Drive State College, PA 16801, USA VT: 814.272.1039 F: 8 1 4 .2 3 1 .1 5 8 0 exygen.com Section B H Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E05-0115 Sample Description Outfall 001 Effluent Low Field Spike Outfall 001 Effluent High Field Spike Amount Spiked (ng/mL) C4 Acid*______________________ CS Acid_______________________ C6 Acid_______________________ C7Acld 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 Recovered Recovery (no/mL) (ng/mL) (%) (ng/mL) (no/mL) (%) (no/mL) (no/mL) (%) (ng/mL) (no/mL) (/.) 10 16.4, 28.3 119 2.53 43.6 436 2.68 8.79 61 1.35 14.9 136 250 16.4 , 298 113 2.53 780 312 2.68 144 57 1.35 329 131 Outfall 001 Effluent SpkC Low Lab Spike 1 16.4 18.6 " 2.53 9.24 671 2.68 6.00 332 1.35 3.87 252 Outfall 001 Effluent Spk D High Lab Spike 500 16.4 1260 249 2.53 2500 500 2.68 464 92 1.35 703 140 Field Blank Low Field Spike 10 ND 12.8 , 128 ND 10.0 100 ND 10.7 107 ND 11.0 110 Field Blank High Field Spike 250 ND 344 16 8 ND 209 84 ND 300 120 ND 305 122 Sample Description Outfall 001 Effluent Low Field Spike Outfall 001 Effluent High Field Spike Outfall 001 Effluent Spk C Low Lab Spike Outfall 001 Effluent Spk O High Lab Spike Field Blank Low Field Spike Field Blank High Field Spike C8 Acid C9 Acid C10 Acid C11 Acid Amount Amt Found Amount Amt Found Amount Amt Found Amount Amt Found Amount Spiked In Sample Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery In Sample Recovered Recovery (no/mL) (no/mL) (no/mL) (%) (no/mL) (ng/mL) (%) (ng/mL) (no/mL) (V.) (no/mL) (no/mL) (%) 10 8.52 16.9 84 ND 13.2 132 ND 13.6 136 ND 11.3 113 250 8.52 223 86 ND 307 123 ND 340 136 ND 265 106 1 8.52 9.31 ~ ND 1.45 145 ND 1.59 159 ND 1.43 143 500 8.52 514 101 ND 61, 122 ND 680 136 ND 704 141 10 ND 10.7 107 ND 9.43 94 ND 9.71 97 ND 10.1 101 250 ND 295 118 ND 276 fio ND 680 272 ND 213 85 ND = Not detected = Response between 0 and 1 ng/mL. *ND = Not detected = Response between 0 and 4 ng/ml.. 0007 J ^ 3 03055f8 Research Drive ^kStSatalte College, PA 16801, USA VT: 800.281.3219 F: 8 1 4 .2 7 2 .1 0 1 9 exygen.com P roven Results. Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E05-0115 Continued Sample Description Outfall 001 Effluent Low Fiald Spika Outfall 001 Effluent High Raid Spika Outfall 001 Effluant Spk C Low Lab Spika 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 Recovered Recovery (ng/mL) (ng/mL) (%) (ng/mL) infl/my____ (%) (ng/mL) (ng/mL) (%) (no/mL) (ng/mL) (V.) 10 ND 4.44 44 24.8 41.6 168 ND 11.7 117 20.3 32.2 119 250 ND 153 61 24.8 442 167 ND 295 118 20.3 322 121 1 ND C.875 86 24.8 28.7 ** ND 2.45 245 20.3 21.7 " Outfall 001 Effluant Spk D High Lab Spika Field Blank Low Fiald Spika 500 10 ND ND 825 125 24.8 3.92 89 ND 836 162 9.43 94 ND ND 524 105 20.3 640 124 10.9 109 ND 10.3 103 Field Blank High Fiald Spika 250 ND 198 79 ND 298 119 ND 318 127 ND 223 89 Sample Description Outfall 001 Effluent LowFiald Spika Outfall 001 Effluent High Fiald Spika Outfall 001 Effluant Spk C Low Lab Spika Outfall 001 Effluant Spk D High Lab Spika Field Blank Low Fiald Spika Field Blank High Fiald Spika Amount Spiked (ng/mL) Amt Found In Sample (ng/mL) FEiSA FOSA Me-FBSE-OH* Amount Amt.Found Amount Amt Found Amount Recovered Recovery in Sample Recovered Recovery In Sample Recovered Recovery (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) 10 9.23 18.7 95 3.61 19.6 160 ND 12.2 122 250 9.23 279 108 3.61 368 146 ND 149 60 1 9.23 10.1 ** 3.61 5.40 - ND 6.32 632 500 9.23 512 101 3.61 727 \ 145 ND 3920 784 10 ND 10.5 105 ND 9.93 99 ND 7.23 72 250 ND 296 118 ND 253 101 . ND 193 77 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. 0008 J ^ 3 03055i8 Research Drive State College, PA 16 8 01 , USA YT. 800.281.3219 F; 8 1 4 .2 7 2 .1 0 1 9 exygen.com Section C 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 I Login Login Group: L0006004 Login #: 6115 Project: P0000522 Company Name: 3M Submitted By: Login Type: Kent Lindstrom Immediate Receipt of Samples Started: True Date Start: 08/25/2005 Due Date: 09/04/2005 Received Date: 08/25/2005 Received By: Ammerman, Mark Spread Sample: Label: Exygen SD/PI: Risha, Karen Project Title/Type: Groundwater Sampling, Decatur AL / ROUTINE Login Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Packaae PK0007020 Carton Date / Condition Packages / Containers ShiDDer/ ID Received Date: 8/25/05 10:40 Package & Contents Uncompromised FEDEX 8511 5371 4781 TemD. Control/TemD. None 23.3 Direction / Handled By RECEIVED Ammerman, Mark Container # C0088709 C0088710 C0088711 C0088712 C0088713 C0088714 C0088715 C0088716 Gross Weight dH Container Tvpe 240.50 g 500 ml Clear Plastic Narrow 244.50 g 500 ml Clear Plastic Narrow 245.40 g 500 ml Clear Plastic Narrow 258.00 g 500 ml Clear Plastic Narrow 243.10 g 500 ml Clear Plastic Narrow 247.40 g 500 ml Clear Plastic Narrow 243.30 g 500 ml Clear Plastic Narrow 615.00 g 500 ml Clear Plastic Narrow Preservative NONE NONE NONE NONE NONE NONE NONE NONE Mfa. Lot Mfg ID 8/25/2005 Login.rpt 0009 Report Version: Jun 6 2005 2:39PM Page 1 of 2 Instance: R0188272 IIH IIIIII Sample ID L0006004-0001 L0006004-0002 L0006004-0003 L0006004-0004 L0006004-0005 L0006004-0006 L0006004-0007 L0006004-0008 Container C0088709 C0088710 C0088711 C0088712 C0088713 C0088714 C0088715 C0088716 Matrix LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID LIQUID Login Fraction Water Samples Sample Outfall 001 Effluent Water Outfall 001 Effluent Dup Water Outfall 001 Effluent 10 ppb Spk Water Outfall 001 Effluent 250 ppb Spk Water Travel Blank Water Travel Blank 10 ppb Spk Water Travel Blank 250 ppb Spk Water Equipment Blank Date SamDled 08/24/2005 08/24/2005 08/24/2005 08/24/2005 08/23/2005 Date Due 09/04/2005 09/04/2005 09/04/2005 09/04/2005 09/04/2005 09/04/2005 09/04/2005 09/04/2005 Login Reviewed By: Date/Time: f c f h x j e r - M IS ' 8/25/2005 Login.rpt 0010 Report Version: Jun 6 2005 2:39PM Page 2of 2 Instance: R0188272 lUIHlllllllll CHAIN-OF-CUSTODY / Analytical Request Document aceA nalytical' /Section A ' Required Client Information: Company ^ O nl Address c v tu iv o v l. i-A b . The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Required Project Information: Rep0rtT0jV \r . Copy To: Section C Invoice Information: Attention: L in ifs fo v ry Company Name: NPDES UST fPage: ot / ___ 00 00 93(1 REGULATORY AGENCY GROUND WATER RCRA DRINKING WATER Other___________ Address: f ! ! _________ k r I m c U W n " W f i - ' m - S 3 i Fax Requested Due Date/TAT: Purchase Order No.: Pace Quote Reference: @ .w u n n /\.c fln 1 Project Name: Pace Project Manager . fW /i-W iv\ O uATa LL. 0 0 1 P c - fflo n . Q Tf . K ( c V > S w \ iH r ^ Project Number: g q Q _ 3 Pace Profile #: SITE LOCATION GA OH O IL DSC IN Wl Ml MN D N C THER A L A B A M A Section D Valid Matrix Codes Required Client Information matrix code DRINKING WATER DW S A M P L E ID One Character per box. /(Aa-7 u0 yQ// . )^ Samples IDs MUST BE UNIQUE WASTE WATER PRODUCT SOIL/SOUD OIL Wa,IrPE OTHER TISSUE WW P SL OL aWrP OT TS a. u>j-.o5Oil ujO o Qu E a ul. m \ i-P c ta r i Mi W W - M |3 VAv LvvV P sta Jl a%i PSS5%o" sV',"?<i/*U31.8 4/ of eST- er COLLECTED o COMPOSITE START COMPOSITE END/GRAB DATE 306, */a/oy >39? 13*5 fari / a s r P re s e rv a tiv e s N N dition al C om m ents: % ,,- H 'fir L C it f a n / I * * & ra le> & S c J tlfa n lL F i n a l , c ltie r-ifv e , REVERSE SIDE FOR INSTRUCTIONS T ln tL If RELINQUISHED BY / AFFILIATION I D A T E ! TIME ! ( ( * & ! m k i _____ ACCEPTED BY / AFFILIATIO N I DATE ! TIME SAMPLE CONDITION z ? o .o L 0 -^ O R I IN A L SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: /" l _ e r r v jjf'i/ia SIGNATURE of SA^PL^R: A 1 -- it (T tP f'i DATE Signed f (MM / DD / YY\ l s /w / ,, t 4 - ih lo s zz > >- gm I *8 oe co w ALLQ020rev.3,31 Mar05 Instructions for completing Chain of Custody (COC) 1. Section A and B: Complete all Client information at top o f sheet: company name, address, phone, fax, contact (the person to contact if there are questions, and who will receive the final report.), e-mail address (if available), PO#, Project Name and/or Project Number as you would like to see it appear on the report. _} ' . , . ,, 2. Section C: Invoice Information: Billing information is included in this section. This information should include the name and address of the person receiving the invoice. 3. Quote Reference should be completed if a quotation was provided by Pace Analytical. The Project Manager, and Profile No! will he completed by Pace Analytical Services. T . .:" : ' 4. Site Location: A separate COC must be filled out for each day of sample collection. Record the two letter postal code for the US state in which the , samples were collected. 5. Regulatory Agency: hist,the program that is guiding the work to ensure proper regulations are followed. 6. Section D: Complete Sample Description in the "SAMPLE ID' section as you would like it to appear on the laboratory report. The following information should also be included: the sample matrix, sample type (G (grab) or C (composite);," When collecting a composite, the start time and end time should be documented in the respective boxes. The collection time for a grab (G) sample should be entered in the boxes marked `Composite End/Grab'). Sample temp at collection (if required by state), the total number o f containers, and preservative qsed. ' . " ` - c. . 7. Mark if the sample was filtered in the field by marking Y or N in 'Filtered' row by the Analysis requested. : ; 8. Requested Analysis: List the required analysis and methods on the lines provided and place a check in the column for the samples requiring the analysis. Additional comments should be referenced in the bottom left hand comer or include attachments for extended lists of parameters. 9. The sampler should print their name in the space provided and sign their name followed by the date of the sampling event at the bottom of the COC in the spaces designated for `SAMPLER NAME AND SIGNATURE'. 10. When relinquishing custody of the samples to a representative of the laboratory or other organization, indicate the Item Numbers o f those samples being transferred: sign relinquished by, date and time, and include your affiliation. Important Note: Standard Turnaround Time is 2 Weeks/10 business days. Results will be delivered by end of business on. the date due unless other arrangements have been made with your project manager. Special Project Requirements such as Low Level Detection Limits or level of QC reported must be included on the chain of custody in the Additional Comments section. , CHAIN-OF-CUSTODY / Analytical Request Document m e A nalytical The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Page: / of } /Section A ' Required Client Information: Section B Required Project Information: Section C Invoice Information: -930848 Company Address S vtuirp/t. L-Ab. Report To: Copy To: Attention: Company Name: NPDES UST REGULATORY AGENCY GROUNDWATER RCRA DRINKING WATER Other___________ Email To __ k r lindsVon Fax e'Z s \ - m - K & Requested Due Date/TAT: Address: Purchase Order No.: Pace Quote Reference: Project Name: Pace Project Manager. ..................... Deca-Vuy OtAfALL 00| r~C- fllgB. QTg, KtcVr Project Number: g : q g _ 3 Pace Profile #: . , SITE LOCATION G A O IL IN Ml MN D N C O H D S C Wl other A l a b a m a D-- it S g C tiO n Valid Matrix Codes Required Client Information matrix code r DRINKING WATER DW ^ a ia n i f- - _ WATER WT S A M P L E ID WASTE WATER WW PRODUCT P SOIL/SOLID SL i One Character per box. o il ol , /(Aa -"Z7, n0q-9//.-\) WIPE AIR WP AR Samples IDs MUST BE UNIQUE OTHER OT TISSUE TS E 05 - 05^3 u0j.S0 PmOii DATE Q l u t ha E i lu [__ l i A-fe CVfi w PS- 0^13 % of 6 c T- O - 'S V T - ter Additional Comments: " % c h ftx in ^ - G ra b _ ....... - C o W ifO S ife f e c ltlto n L P h a l cltipt'itv. SEE REVERSE SIDE FOR INSTRUCTIONS . T | L SU RELINQUISHED BY / AFFILIATION DATE I TIME ! ACCEPTED BY / AFFILIATION U. ( ( M i f f r ;______ I DATE ; TIME / / / / * V f o .dL o SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: ~ CT L / ug SIGNATURE of SA^PL^fe: ( \ \ --------- wn DATE Signed (MM / DD / YY 1 S /W U 5 4 W P * SAMPLE CONDITION zz > zz ?? z z ? z zz ? 8 >. u ALLQ020rev.3,31 Mar05 es . Instructions for completing Chain of Custody (COC) p IVp 1 p Section A and B: Complete all Client information at top of sheet: -company name, address, phone, fax, contact (the person to contact if there are V whn.ywall report.), e-mail address (if available), PO#. Project Name and/or Project Number as you would like to see it " -appearon thereport - / 2. Section C: Invoice bifonnation; Billing information is included in this seetion. This information should include the name and address of the person receiving the invoice. ; 3. Quote Reference should be completed if a quotation was provided by Pace Analytical. The Project Manager, and'Profile No. will be completed by t v Pace Analytical Services. " ' ; " : 1 ' ; c .. - 'v, -- ' ^ I .* .> ,' ' - M. . . S r ; - l ' v' 4. Site Location: A separate CQC must be filled out for each day of sample collection. Record the two letter postal code for the US state in which the , samples were collected. 5. Regulatory Agency: .List the program that is guiding the work to ensure proper regulations are followed. 6. Section D: Complete ^Sam ple'Description in the ' SAMPLE ID' section as you would like it to appear on the laboratory report. The following information should also be included: the sample matrix*sample type (G (grab) or C f composftqijr When. Collecting a*composite* the, start time, i ^ e h t l ' ime should be documented ip the respective boxes.* T he collection time for a grab (G) sample, shog|d be e'nitered in the boxes marked `Composite . Enn ;d! /j GV: ra1b'), SC -aimin ipUlie. ttei -mmpn a-itt c/ o. .l1lei ctio. inti (i !iff rr.e-jq1u11iirte. -drl bn yv sta'Ittei ):, tthli.e- tMotta'.lli nn ulmi bmeri o- f! c.o'n)ta-in, eMrs,n a/nfd prese-rrvv :aUt)iv\ e1' lasted , , 1 ! j . ' - 1 ' ' J 7. Marie if the sample was filtered in the field by marking Y or N in 'Filtered' row by the Analysis request;' w * 8. Requested Analysis: List the required analy sis and methods on the lines provided and place a check in the column for the samples requiring the analy sis. Additional comments should be referenced in the bottom left hand comer or include attachments for extended lists o f parameters. ._ %` ., : ; ! , 9. The sampler should print their name in the space provided and sign their name followed by the date of the sampling event at the bottom of the COC in the spaces designated for `SAMPLER NAME AND SIGNATURE'. ' i$ ; ; t '. |- ' :, 10. When relinquishing custody o f the sinpples to a representative o f the laboratory or other organization, indicate the Item Numbers of those samples beirfg transferred; sign relinquished by, date and time, and include your affiliation. : ; ! , '* ' ^Important Note: ;! | Standard Turnaround Time is 2 Weeks/10 business days. Results will Tie delivered by chef-of business opthe date,,due unless other arrangements have been made with your project manager: -- _ _ ' - :C , -: , Special Project Requirements such as Low Level Detection l imits or level of QC re Comments section. must Le included on the chain of custody in the Additional . . - . . . Vi ' "\ 1 ' * CHAIN-OF-CUSTODY / Analytical Request Document m e Analytical* /Section A ' Required Client Information: Section B Required Project Information: The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section C Invoice Information: Page: / of / -930848 " " in Address e ,,, . U ib . Copy To: Attention: Company Name: NPDES UST iLATORY AGENCY GROUND WATER DRINKING WATER RCRA Other___________ Address: E m a n k r t in iiS W n Purchase Order No.: > TM ssi m -5 3 s t:" Project Name: D ic a k tA . O tA f A L L Requested Due Date/TAT: Project Number: g f q i j ------ 1-----$f-------------------------------------------------------------- Section D Valid Matrix Codes Required Client Information MATRIX CODE DRINKING WATER DW SAMPLE ID WATER WASTE WATER PRODUCT SOIL/SOLID L One Character per box. OIL * (A-Z, 0-9 /.-) WIPE AIR Samples IDs MUST BE UNIQUE OTHER TISSUE 061 PO _ flip p . ^ Pace Quote Reference: Pace Project Manage^ QT R ch Pace Profile #: . SITE LOCATION GA O IL OH DSC G IN Wl Ml MN G N C BOTHER A L A B A - Additional Comments: P A re . -alt. T | . % P w A t- G rab t h i h f f e C b l& tn t W V *' O .o L fe fa b l \ >' 0 > / SEE REVERSE SIDE FOR INSTRUCTIONS o i'JNQ UISHED B Y /A F F IL IA T IO N : DATE I TIME i -{P ACCEPTED BY / AFFILIATION i DATE TIME / . ,, SAMPLE CONDITION - ?z z > z zz SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: 1 ,f _____- G~. SIGNATURRE of SAMPLER: f l l ____ A * ----- - DATE Signed * (MM / DD / YY) t t f a it 5 4 fe/o o-- t4r) co A l I O n ^ flrA v 3 31 M a rflfi T: ' a fl 5sc;tv*r.fA \ Vt'JC ; o J O - lC - r .: `- . \ 0 - '!A ,'i/- Instructions for completing Chain of Custody (COC) A; | \ p fVt Section A and B: Complete all Client information at top of sheet: company name, address, phone, faxfcontact (the person to contact if there are ^asiions^aadqyho ^ ll^ e e iy g .the final report.), e-mail address (if available), PO#. Project Name and/or Project Number as you would like to see it appear on the report ~ Ct/A* . , _ < ,'C -t 2. Section C: Invoice Information: Billing information is included in this section. This information should include the name and address of the person receiving the invoice. .... xf 3. Quote Reference should be completed if a quotation was provided by Pace Analytical. The Project Manager, and 'Profile fsToi will be completed by * f Pace Analytical yrvices. v r ^ > .'J - ` J ' i A ' .' "' ' - - * i - '. 4. vSite Location: A separate COC must be,filled out for each day ot sample collection. Record the two letter postal Code for the US state in which the , . samples were collected. : ' ' ; i . ') .f , ! .i ' 5. Regulatory Agency: List tire program that is guiding the work to ensure proper regulations are followed. ." v' ' 1 ' ,4 6. Section D: Complete a-Samjile Description in the `"SAMPLE ID' section as you would like it to appear on the laboratory report. 'The following information should also be included: the sample matrix,sample type (Q- (grab) orC (cblrnposilejy When -collecting a composite,- the,stafi tirpc and end time should be documented in the respective boxes. The collection time for a grab (G) sample should be entered *n d*e boxc marked'`t'omposite End/tbrab'), Sample temp at collection (if required by state), the total number of containers, and preservative used . ' * " A - ' ' . i ' . f *. : c " ' c ,: 7. Mark |t the sample was filtered in the field by marking Y or N in Filtered' row by the Analysis requested., .. ; v >)i "\ . A >(' . : -,~j . ' - '; > . f. . := ' ' 'i : 8. Requested Analysis: List thd required analysis and methods on the lines provided and place a chick in the column for the samples requiring the 1 analy sis. Additional comments should be reference^! in the bottom left hand comer or include attachments for extended lists o f parameters. I 1 4. '4 1. '. . 9. fhe sampler should print their name in the space provided and sign their name followed by the ddte of the sampling event at the bottom of the COC in the |pqces designated f o r `SAMPLER NAME AND SIGNATURE'. : J!j ,. ; i ; ! ' ; : ;: ' i: : i ( !. ; ; ' : : ; . : ' 10. When relinquishing custody of the samples to a repfesentative of the laboratory' or other organization, indicate the Item Numbers o f those samples : beirjg transferred; sign relinqhished by, date and tiihe, and include your affiliation. !; 1 : ! Ii ?: . 1 ; t ] 1' ' ' 1 : ! : ! |; : I . :;! `Im portant Npte: r 1 r' *' Standard T urnaround Time is 2 Weeks/10 business days. Results will be delivered b y 'em! ofjbus'mess on the date due unless other arrangements have been made with your project manager. '. r, ' " " Special Project Requirements such as Low Level Detection Limits or level of QC reported must be included on the chain of custody in the Additional Comments section. i, si# ace A nalytical /Section A ' Required Client Information: Company O Ml Address C flg U b. Emarl To ^ r j ( ^ ^ s | < 0 t V \ ^ Phr d - ? ? f i - 5 3 s / ax Requested Due Date/TAT: CHAIN-OF-CUSTODY / Analytical Request Document The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Required Project Information: ' ReportTo| ^ r Copy To: Lt Section C Invoice Information: Attention: Company Name: Address: Purchase Order No.: Pace Quote Reference: \ Project Name: Pace Project Manager: . , D fr/i W O u *# A tU 00 | r O ff W . G7f bS * \ i H s Project Number: g r q g _ Q g t J 3 Pace Profile #: NPDES UST Page: / of j -930848 REGULATORY AGENCY GROUNDWATER RCRA DRINKING WATER Other___________ SITE LOCATION G A miL OH DSC IN Wl Ml MN D N C iTHER A L A S # * >/? Additional Comments: a L Cif %. e Grai> I { Com posite f e r* ' f i UAL \ G>(* b I SEE REVERSE SIDE FOR INSTRUCTIONS SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: SA L 1 k \ J r 1/ A SIGNATURE of SA^PL^R: a >____ * T P (\ DATE Signed, (M M / D D /Y Y ) . *________________ t b v l o * s / o s ALLQ020rev.3,31 Mar05 Instructions for completing Chain of Custody (COC) -L, Section A and B: Complete all Client information at top o f sheet: company name, address, phone, fax, contact (the person to contact if there are - questions, and who will receive the final report.), e-mail address (if available), PO#. Project Name and/or Project Number as you would like to see it appear on the report. 2 Section C: Invoice Information: Billing information is included in this section. This information should include the name and address of the person receiving the invoice. 3. Quote Reference should be completed if a quotation was provided by Pace Analytical. The Project Manager, and Profile No. will be completed by Pace Analytical Services. 4. Site Location: A separate COC must be filled out for each day o f sample collection. Record the two letter postal code for the US state in which the samples were collected. 5. Regulatory Agency: List the program that is guiding the work to ensure proper regulations are followed. 6. Section D: Complete a Sample Description in the "SAMPLE ID' section as you would like it to appear on the laboratory report. The following information should also be included: the sample matrix, sample type (Ci (grab) or C (composite), When collecting a composite, the start time and end time should be documented in the respective boxes. The collection time for a grab (G) saniple should be entered in the boxes marked `Composite End/Grab'), Sample temp at collection (if required by state), the total number o f containers, and preservative used. 7. Marti if the sample was filtered in the field by marking Y or N in `Filtered' row by the Analysis requested. 8. Requested Analysis: List the required analysis and methods on the lines provided and place a check in the column for the samples requiring the analysis. Additional comments should be referenced in the bottom left hand comer or include attachments for extended lists of parameters. 9. The sampler should print their name in the space provided and sign their name followed by the date of the sampling event at the bottom o f the COC in the spaces designated for `SAMPLER NAME AND SIGNATURE'. 10. When relinquishing custody of the samples to a representative of the laboratory or other organization, indicate the Item Numbers o f those samples being transferred; sign relinquished by, date and time, and include your affiliation. Important Note: Standard Turnaround Time is 2 Weeks/10 business days. Results will be delivered by end o f business on the date due unless other arrangements have been made with your project manager. Special Project Requirements such as Low Level Detection Limits or level of QC reported must be included on the chain of custody in the Additional Comments section. 08-22-'05 18:20 FROM-PACE ANALYTICAL 7048759091 T-047 P002/005 F-793 8/2/2005 Project: EQ5-0543 3M ENVIRONM ENTAL LABORATORY Prelim inary/U nauthorizcd R eport Page I of 2 Requester: Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number: 0022674449 Date Received: 8/2/2005 Project Description: Decatur Outfall 001 FC Monitoring Quarterly Comments: Completion Date: Project Lead: Kent Lindstrom Phone Number: 651-778-5352 Email Address: krlindslrom@mmm.com Statement o f Accuracy: .__________________________________ Project Resalts/Actlvitv Pace Field Sampling Event 3M S am ple N u m b er_____ S am p led D ate 05-0543-86889 8/23/2005 LAB EXYGEN Analytical Method LCMS E05-0543-86890 8/23/2005 tA B , EXYGEN Analytical Method LCMS Sam ple Description O utfall 001 Effluent - Com posite (Vunnnnenn PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid Cfi acid C7 acid PFOA C9 aoid CIO acid Cl 1 acid 0 2 acid Result Outrait 001 E ffluent - C om posite D uplicate Component PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid CUacid CI2 acid Remit RL, Qualifier RL. Qualifier 0012 08-22-'05 18:20 FROM-PACE ANALYTICAL 7048759091 T-047 P003/005 F-793 8/2/2005 :>M E N V IR O N M E N T A L L A B O R A T O R Y Prelim inary/Unauthorized Report Project: E05 0543 (cont.) 3M Sample Num ber Sam pled P ate EOS-0543-86891 8/23/2005 Sam ple Deecription Field C ontrol/Travel Blank LAB EXYOEN Analytical M ethod LCMS E09-0543-86892 8/23/2005 LAB EXYGEN Analytical Method LCMS Component R em it RL PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid______________________'____________________________ Equipm ent Blank C o m p o n en t,. PFOS PFHS PFBS FOSA PFBAmide McFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA CP acid CIO acid Cl I acid CI2 acid R etail Bk Page 2 o f 2 Qualifier Q u a lifie r 0013 08-22-'05 18:20 FROM-PACE ANNALYTICAL 7048759091 T-047 P004/005 F-793 Sampla.SaTest.Test_ Test.Replic Test.Analy.1ResuItNan ResultRes Result.Entr ResultAttri Result.Unit 86689 969412 1 LCMS WV PFOS N NG/ML 86889 969412 1 LCMS WV PFHS N NG/ML 86889 969412 1 LCMS WVPFBS N NG/ML 86889 969412 1 LCMS WVFOSA N NG/ML 86889 969412 1 LCMS_WV PFBAmide N NG/ML 86889 969412 1 LCMS^WV MeFBSE-C N NG/ML 86889 969412 1 LCMS WV C4 acid N NG/ML 86889 969412 1 LCMS~WV C5 acid N NG/ML 86889 969412 1 LCMS_WV C6 acid N NG/ML 86889 969412 1 LCMS WV C7 acid N NG/ML 86889 969412 1 LCMS_WV PFOA N NG/ML 86889 969412 1 LCMS_WV C9 acid N NG/ML 66889 969412 1 LCMS WVC10 acid N NG/ML 86889 969412 1 LCMS WVC11 acid N NG/ML 86889 969412 1 LCMS WVC12 acid N NG/ML 86890 969413 1 LCMS WV PFOS N NG/ML 86890 969413 1 LCMS_WV PFHS N NG/ML 86890 969413 1 LCMS~WV PFBS N NG/ML 86890 969413 1 LCMS WVFOSA N NG/ML 86890 969413 1 LCMS WV PFBAmide N NG/ML 86890 969413 1 LCMS WVMeFBSE-CN NG/ML 66890 969413 1 LCMS WV C4 acid N NG/ML 86890 969413 1 LCMS WV C5 acid N NG/ML 86890 969413 1 LCMS WV C6 acid N NG/ML 86890 969413 1 LCMS_WV C7 acid N NG/ML 86890 969413 1 LCMS_WV PFOA N NG/ML 86890 969413 1 LCMS_WVC9acld N NG/ML 86890 969413 1 LCMS~WVC10 acid N NG/ML 86890 969413 1 LCMS WVC11 acid N NG/ML 88890 969413 86891 969414 1 LCMS WVC12 acid N 1 LCMS_WV PFOS N NG/ML NG/ML 86891 969414 1 LCMS~WV PFHS N NG/ML 86891 969414 1 LCMS_WV PFBS N NG/ML 86891 969414 1 LCMS WVFOSA N NG/ML 86891 969414 1 LCMSJ/W PFBAmide N NG/ML 86891 669414 1 LCMS~WV MeFBSE-C N NG/ML 86891 969414 1 LCM$_WV C4 acid N NG/ML 86891 969414 1 LCMS VWC5 acid N NG/ML 86691 969414 1 LCMS_WV C6 acid N NG/ML 86891 969414 1 LCMS WV C7 acid N NG/ML 86891 969414 1 LCMS_WV PFOA N NG/ML 86891 969414 1 LCMS WV C9 acid N NG/ML 86891 969414 1 LCMS WVC10 acid N NG/ML 86891 969414 1 LCMS WVC11 acid N NG/ML 86891 969414 1 LCMS WVC12 acid N NG/ML 86892 969416 1 LCMS WV PFOS N NG/ML 86892 969415 1 LCMSJ/WPFHS N NG/ML 86862 969415 1 LCMS_WV PFBS N NG/ML 88692 969415 86892 969415 1 LCMS' WVFOSA N 1 LCMS WV PFBAmide N NG/ML NG/ML 86892 969415 1 LCMS_WV MeFBSE-C N NG/ML 0014 -22-'05 18:20 FROM-PACE ANALYTICAL 7048759091 66892 66692 86892 86892 86892 86892 88892 88892 86892 96941S 969415 969415 969415 969415 969415 969415 969415 969415 1 LCMSJ/WC4 acid 1 LCMS_WV C5 acid 1 LCMS_VW C6 acid 1 LCMS WV C7 acid 1 LCMS VWPFOA 1 LCMS VW C9 acid 1 LCMS WVCIOacid 1 LCMS WVC11 acid 1 LCMS WVC12 acid N N N N N N N N N T-047 P005/005 NG/ML NG/ML NG/ML NG/ML NG/ML NG/ML NG/ML NG/ML NG/ML 0015  USAirbill Express 1 From Data c 651153714701FedEx Tracking Sendai's Name 3. 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