Document gbaqJNwypxXEakGD0vj6qo9J3

Precise Research. Proven Results. A nalytical Report Fluorpchemical Characterization of Aqueous Samples DeCatur Outfall 001 FC Monitoring (E06-0694) Exygen Research Laboratory Report No. L0010333 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Gary A. Hohenstein Environmental Manager, Special Projects, EHS Operations 3M Bldg, 42-2E-27 St. Paul, MN 55133 .3058 Research Drive State College, PA 16801, USA J : 814.272.1039 ^F: 814.231.1580 exygen.com PAGE 1 0 F 5 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 L0010333. Specific fluorochemical 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 PerfluoroheDtanoic Acid Perfluorooctanoic Acid Perfluorononanoic Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide (PFB Amide) Perfluorooctanesulfonamide 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 12/12/06 and 12/13/06. Samples were received on 12/14/06. Chain-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 Water 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 C18 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 mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a PE Sciex API 4000 MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted and analyzed between 12/20/06 and 01/16/07. 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 >_0.985 (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. PAGE 3 OF5 Instalment 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 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. 5.5 Duplicates Field and laboratory duplicates were prepared for each field sample. Duplicate results are given along with the sample results in Attachment A. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliq water was spiked with all compounds of interest at 50 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 blank spikes and laboratory control spikes, the analytical method accuracy for all analytes is 30%. Based on the results of field matrix spike samples, the overall accuracy for all analytes except M eF B S E -O H is as follows: C4 Acid and C5 Acid screening quality because of high and variable spike recovery C12 Acid 40% All others 30% The analysis of the sample for the analyte MeFBSE-OH resulted in residue concentrations significantly above the level at which the sample was fortified at in the field spikes. In this case, a laboratory spike was used for the assessment of accuracy. Based on the results of the laboratory matrix spike, the overall accuracy for the analysis of MeFBSE-OH is as follows: MeFBSE-OH 50% All spike recovery data are reported in the data tables. PAGE 4 OF5 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. 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: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data 9 Signatures Christine E. Edwards, Lab Technician Other Lab Members Contributing to Data Krista Gallant Date PAGE 5 OF5 Section A RAenaplytoicarl t Summary of Fluorochemical Residues in Outfall 001 Effluent for E06-0694 Sample ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank \ C4 A cid*** Perfluorobutyric Acid 8.22 8.06 7.26 ND , ND Analyte Found (ng/mL) C5 A cid* C6 Acid* Perfluoropentarioic Acid Perfluorohexanoic Acid ND 1.16 ND 1.19 ND 1.18 ND ND ND ND C7 Acid* Parfluoroheptanoic Acid ND ND ND ND ND Sample ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank C8 Acid* Perfhiorooctanolc Acid . 1.04 , ND 1..06 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* Perfluoroundacanolc Acid ND ND ND ND ND Sample ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank C12 Acid1 Perfluorododecanoic Acid ND ND ND ND ND Analyte Found (ng/mL) C4 Sulfonate* C6 Sulfonate* Perfluorobutanesulfonate Periluorohexanesulfonate 28.2 ND 26.4 27.6 ND ND ND ND ND ND C8 Sulfonate* Perfluorooctanesulfonate 2.38 2.31 2.53 ND ND Analyte Found (ng/mL) Sample ID Outfall 001 Effluent Outfall 001 Effluent* Outfall 001 Effluent Dup Travel Blank Equipment Blank FBSA* 20.8 20.6 20.6 ND ND FOSA* ND ND ND ND ND M e-FB S E -O H **1 444 438 525 ND ND ND = Not detected = Response between 0 and 1 ng/mL. **ND = Not detected = Response between 0 and 4 ng/mL. "Laboratory Duplicate ''Results to be used for screening due to high spike recoveries "Assessed accuracy is +/-30% 'Assessed accuracy is H -40% 2Assessed accuracy is +/-50% J ^ 3 03055i8 Research Drive jT ^ S tSatate College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com Section B CH Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E06-0694 Sample Description Outfall 001 Effluent Low FMd Spika Amount Spiked (na/mL) C4 Acid* Amt Found Amount Amt Found in Sample Recovered Recovery in Sample (ng/mL) (ng/mL) (%) (ng/mL) C5 Acid Amount Recovered Recovery (ng/mL) (%) Amt Found in Sample (ng/mL) C6 Acid Amount Recovered Recovery (ng/mL) (%) Amt Found In Sample (ng/mL) C7 Acid Amount Recovered Recovery (ng/mL) (%) 10 8.22 , 32.0 238 ND 17.4 174 1.16 11.6 104 NO 9.65 97 Outfall 001 Effluent High Flald Spika 100 8.22 . 293 285 ND 181 181 1.16 118 117 ND 117 117 Outfall 001 Effluant Spk C Low Lab Spiko 10 8.22 33.5 253 ND 18.5 185 1.16 12.9 117 ND 9.99 100 Outfall 001 Effluont Spk D High Lab Spiko Field Blank Low Fiold Spiko Field Blank High Fiold Spiko 100 10 100 8.22 ND ND 291 \ 283 11.1 ,111 115 115 ND ND ND 163 163 1.16 103 102 ND 9.80 98 ND 10.1 101 ND 93.2 93 ND 105 105 ND 112 112 11.5 115 119 119 Sample Description Outfall 001 Effluent Low Fiold Spiko Outfall 001 Effluent High Fiold Spiko Outfall 001 Effluont Spk C Low Lab Spiko Outfall 001 Effluont Spk O High Lab Spiko Field Blank Low Fiold Spiko Field Blank High Fiold Spiko Amount Spiked (na/mL) Amt Found in Sample (no/mL) C8 Acid Amount Amt Found Recovered Recovery in Sample (ng/mL) (%) (ng/mL) C9 Acid C 10 Acid C11 Acid 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 1.04 12.2 112 ND. 9.97 100 ND 9.03 90 ND 7.12 71 100 1.04 108 107 ND 114 114 ND 109 109 ND 101 101 10 1.04 11.6 106 ND 10.2 102 ND 8.08 81 ND 7.14 71 100 1.04 100 99 ND 113 , 113 ND 101 101 ND 97.2 97 10 ND 10.9 109 ND 10.8 108 ND 11.3 113 ND 10.9 109 100 ND 104 104 ND 110 110 ND 106 106 ND 110 110 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 3 times; therefore an accurate recovery cannot be calculated. M,^ L 3,03055f8 Research m sStatalte College, Drive PA 16801, USA V,T: 814.272.1039 F: 8 1 4 .2 3 1 .1 5 8 0 exygen.com CH Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E06-0694 Continued Sample Description Outfall 001 Effluent Low Fisld Spiks C12 Acid C4 Sulfonate C6 Sulfonate CS Sulfonate 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 (ng/mL) (ng/triL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) 10 ND 6.68 67 28.2 35.7 75 ND 10.3 103 2.38 11.6 92 Outfall 001 Effluent High Fisld Spiks 100 ND .93.5 94 28.2 136 108 ND 112 112 2.38 107 105 Outfall 001 Efflusnt Spk C Low Lab Spike 10 ND 6.95 70 28.2 38.8 106 ND 11.6 116 2.38 11.5 91 OutfefI 001 EfRusnt Spk O High Lab Spiks 100 ND 91.7 \ 92 28.2 132 104 ND 109 109 2.38 106 104 Field Blank Low Field Spiks 10 ND 10.5 105 ND 10.1 101 ND 10.6 106 ND 11.0 110 Field Blank High Field Spiks 100 ND 102 102 ND 91.5 92 ND 107 107 ND 107 107 Sample Description Outfall 001 Effluent Low Fisld Spiks Outfall 001 Effluent High Fisld Spiks Outfall 001 Efflusnt Spk C Low Lab Spiks Outfall 001 Efflusnt Spk D High Lab Spiks Field Blank Low Fisld Spiks Field Blank High Fisld Spiks FBSA FOSA Me-FBSE-OH* Amount Amt Found Amount Anit Found Amount Amt Found Amount Spiked in Sample Recovered Recovery in Sample Recovered Recovery In Sample Recovered Recovery (ng/mL) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) 10 20.8 30.0 92 ND 11.3 113 444 498 " 100 20.8 138 117 ND 113 113 444 435 " 10 20.8 30.9 101 ND 10,2 102 444 523 * 100 20.8 131 110 ND 108 106 444 468 * 10 ND 10.3 103 ND 10.8 \1 0 8 ND 11.3 113 100 ND 112 112 ND 124 124 ND 122 122 ND h 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 3 times; therefore an accurate recovery cannot be calculated.. ,3058 Research Drive 4 * m s tSataite College, PA 16801, USA VJ: 814.272.1039 F: 8 1 4 .2 3 1 .1 5 8 0 exygen.com Proven Results. Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent for E06-0694 Sample Description \ Amount Spiked (ng/mL) Amt Found In Sample (ng/mL) Me-FBSE-OH* Amount Recovered (ng/mL) Recovery (%) Outfall 001 Effluent Spk C Lab Spike 500 453 1170 143 *ND = Not detected = Response between 0 and 4 ng/mL. NOTE: Sample was re-spiked at a higher level after the Initial analysis was performed. Initial analysis did not produce a matrix spike recovery because the analyte residue concentrations in the sample significantly exceeded the spike level. Initial analysis data for the sample results are confirmed with the re-analysis and will be reported. J ^ 3 .030558i Research Drive -# m s tSatatte College, PA 16801, USA VJ : 814.272.1039 F: 8 1 4 .2 3 1 .1 5 8 0 exygen.com Section C F pu 3058 Research Drive State College, PA 16801 R E S E A RRCCHH Phone: 814-272-1039 Fax: 814-231-1580 Loam Login Group: L0010333 Login #: Project: 10444 P0000522 Company Name: 3M Submitted By: Kent Lindstrom Login Type: Immediate Receipt of Samples Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Started: True Date Start: Due Date: 12/15/2006 12/25/2006 Login Initiated*: 12/15/2006 * Dates entered into "Login Initiated" field prior to 1/5/06 reflect dates of receipt. The field was formerly called "Received Date" Received By: Ammerman, Mark Spread Sample: Label: ^ Exygen SD/PI: Risha, Karen Project Title/Type: Outfall 001 Sampling, Decatur AL / ROUTINE Login Notes: Packaae m PK0012368 Carton Date / Condition Packages / Containers ShiDDer/ ID Received Date: 12/14/06 10:28 Package & Contents Uncompromised FEDEX 8578 5294 6923 TemD. Control/TemD. None 19.7 Direction / Handled Bv RECEIVED Ammerman, Mark Container # C0225943 C0225944 m C0225945 t f C0225946 C0225947 C0225948 C0225949 C0225950 Gross Weiaht dH Container TvDe 606.90 g 500 ml Clear Plastic Narrow 255.70 g 500 ml Clear Plastic Narrow 256.20 g 500 ml Clear Plastic Narrow 256.40 g 500 ml Clear Plastic Narrow 605.40 g 500 ml Clear Plastic Narrow 598.70 g 500 ml Clear Plastic Narrow 240.60 g 500 ml Clear Plastic Narrow 242.20 g 500 ml Clear Plastic Narrow Preservative NONE NONE NONE NONE NONE NONE NONE NONE Mfa. Lot Mfa. ID 12/15/2006 Login.rpt Report Version: Dec 13 2006 10:41PM Page 1 of 2 Instance: R0306547 R0306547 Sample ID L0010333-0001 Container C0225943 Matrix LIQUID L0010333-0002 C0225944 LIQUID L0010333-0003 C0225945 LIQUID L0010333-0004 C0225946 LIQUID L0010333-0005 C0225947 LIQUID L0010333-0006 C0225948 LIQUID L0010333-0007 C0225949 LIQUID L0010333-0008 C0225950 LIQUID Fraction Water Samples SamDle Equipment Blank Water Field Control/ Travel Bk HI Spike (100 ppb) Water Field Control/ Travel Bk Low Spike (10 ppb) Water Field Control/ Travel Blank Water Outfall 001 Eff Comp. 100 ppb Water Outfall 001 Eff Comp. 10 ppb Water Outfall 001 Eff Composite Dup Water Outfall 001 Eff Composite Date SamDled 12/12/2006 Date Due 12/25/2006 12/11/2006 12/25/2006 12/11/2006 12/25/2006 12/11/2006 12/25/2006 12/13/2006 12/25/2006 12/13/2006 12/25/2006 12/13/2006 12/25/2006 12/13/2006 12/25/2006 Login Reviewed By: ^ Date/Tlme: / Z v Z - o g ' / / / O 12/15/2006 Login.rpt Report Version: Dec 13 2006 10:41PM Page 2 of 2 Instance: R0306547 R0306547 raceAnalytical /Section A ' Required Client Information: Company 3 ^ Address K t r /m J s ,f r e * r 7 @ m m m , c o H \ PL T | ' ^ 0 ' 5 3 S 3 l Fax Requested Due Date/TAT: HAlft-OF-tUstbDY?Ana^rticaTRequest document * The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Required Project Information: P k n -|- L ivid Screws, Copy To: Section C Invoice Information: Attention: Company Name: Address: Purchase Order No.: Pace Quote Reference: Project Name: . _ , Pace Project Manager: b e c ti-tu A . D ifr & k L L 0 01 P c (Don. Q T K . Project Number: ( C f^ Pace Profile #: Page: \ of | NPDES UST 1004186 REGULATORY AGENCY GROUNDWATER RCRA DRINKING WATER Other SITE LOCATION GA GIL GIN O H G SC n w i G Ml GM N GNC G OTHER _ A. Valid Matrix Codes Section D Required Client Information matrix code S . ilR1 _ . DRINKING WATER DW WATER WT A M P L E ID WASTEWATER WW PRODUCT P SOIL/SOLID SL One Character per box. oil ol i (A-Z, 0-9 /.-) WIPE AIR WP<AdfP AR Samples IDs MUST BE UNIQUE OTHER OT J b TISSUE TS m0V(-.O20II UJ COLLECTED 5 PH - LZU < t i COMPOSITE START COMPOSITE END/GRAB l H Oo Preservatives P roject Num ber LabI.D u p i v\evV 0 < )& w r6 ^p^3S* i-t> Cenan^o1 rnw h'J j* K iik h . F 1 & -0 h TAVi I k o v k 10T WT C hrxW I 17 "farti A n 0<S~ ^ < /t e t 2 # c . .8I _B_f oit'jL k/r c- 0 5 3 f3ff3bt. tO'f} O ulV T 4 u 0 0 IP ypbioty 0113 wr lalf*hi. to 5 3 ^hsloj to'Si Ou^la 00 E r t- I )v*u v $ t t ^ P 0 i 2 U/T" C- fP53 fy ,3 b i. \Q-*9 C tA^ f f * -V 0 0 I u - .... s it X'l fc /r /0 S 3 /g ' SJ Additional Comments: Ck(oAfl-L *Wj|L PAT- Tl*( /H i h * L 0 10 $ |^ /l|(r U U 3 c-g*p 0 ` 01 jlfnjoC r / ? f i n * t- 0 10 ^ / x l/y fa n o SEE REVERSE SIDE FOR INSTRUCTIONS O R IG iN A L RELINQUISHED BY / AFFILIATION DATE TIME ACCEPTED BY / AFFILIATION DATE TIME SAMPLE CONDITION I 1 y w jfc z -- , lo.'/r /Z-^% --------------------------------------- y~t---------------- zZ >> z > zZz >? > zz z >> > zz z >? > Temp in C Received on Ice Custody Sealed Cooler Samples Intact SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: '~7"* J I I . J . W u i/n m SIGNATURE of SAMPLER:*\ j i ) H DATE Signed /M M / DD / YY)| OC S-W-a/ot f / i ? / / j * /Oj, 1 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, tax, 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 o f 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 tor 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 (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 used. 7. Mark if the sample was filtered in the field by marking Y or N i n `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 o f the sampling event at the bottom o f the COC in the spaces designated for `SAMPLER NAME AND SIGNATURE'. 10. When relinquishing custody o f the samples to a representative o f 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: I' 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. !aceAnalytical /Section A ' R equired Client Information: Company ^ /r / fr Address , < S3 Email To:*. . . . p iW in a s T rp ry ? g m m ni c o m Phone _ _ Fax .S -|-? 7 - -S 3 3 L Requested Due Date/TAT: ^ A & Q s f^ ^ n l^ ic J R e q ^ s t The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Required Project Information: P Copy To: l-tv ld s 4 r W \ Section C Invoice Information: Attention: Company Name: Address: Purchase Order No.: Pace Quote Reference: Project Name: __ Pace Project Manager: e c a - k iA OufrtALt. ool Pc rD o n . OTTC. Project Number: Q Pace Profile #: NPDES UST Page: ^ of | 1004186 REGULATORY AGENCY GROUND WATER RCRA DRINKING WATER Other SITE LOCATION GA n iL DIN noH nsc nw i DMI MN NC n other Section D RequiredClient Information S' AM PLE * ID _ * One Character per box. (A-Z, 0-9 /.- ) Samples IDs MUST BE UNIQUE Valid Matrix Codes MATRIX code DRINKING WATER DW WATER WT WASTE WATER PRODUCT WW P SOIL/SOLID SL o il ol , wAIRip e OTHER TISSUE WATOSRTP5- MW ^JI Sg COLLECTED COMPOSITE START COMPOSITE END/GRAB TIME cn ULLzU < Oo Preservatives P roject Number Lab I.D M i rn *n V O & A / f i q k c OC'T- W T Cq ia ^:]b1 A j : k\r& 'tt 6 . ^ ik 0O (o WT oc 5" iv r OC>t Ic tf Cpnp 11Op| B Ip LJ T mi i 7% Q 2_ wr Q/ fai L 0 0 f l ( U n teli* 2 u /r Oq 1 Coj k fi:s r t i oc 1 t / r io -3 y H 11lo lo /05 3 O S 3 f*h 3/0^ >053 'V /3 ^ U fO '.5 ^ 'JcXo /O S3 'drzla. \ o f K Additional Comments: cM ft/ifi-t /fir h * L Oi o - C - Q ^ P 0 >oi 0 OH SEE REVERSE SIDE FOR INSTRUCTIONS PAT- Tfirf. p /t >|o(r / | i 3 j*|n K /x/tylof, /oc 2 RELINQUISHED BY / AFFILIATION DATE TIME ACCEPTED BY / AFFILIATION DATE ? f$ SAMPLER NAME AND SIGNATURE PRINT Name o f SAMPLER: SIGNATURE of SAM PLER:^ O '-r-- 1 // J . t y ija ff lr n / ) Af DATE S ig n e d /(M M / DD / YY); C ? C w i i f e / ---- / -VYJ/ t;6 f / - 2 / / J / 0 & , TIME SAMPLE CONDITION zz ?? zz >? zz >? zz ?? z ? z > z ? z ? Temp in C Received on Ice Custody Sealed Cooler Samples Intact 1 ALLQ020rev.3,31 Mar05 Instructions for completing Chain of Custody (COC) tj 0 ^ ct*on 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 qucstjonm-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 appearorrthe report. .; ,'w y 2. Section C: Invoice Information: Billing information is included in this section. This information should include the name and address o f 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.1 5. Regulatory Agency: Li.st the program that is guiding the work to ensure proper regulations are followed. y- i ~ ; .-r 'W 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 Minx, sample type (G (grab), or C (composite.),., When fcolleeting a composite, fire staijlti^ne apd end time should be documented in .the respective boxes. The collection time for a grab (G) sample should bt| entered in the boxes marked "Composite find/Girab'). Sample temp at collection (if required By state), the total number o f containers, and 'pieservdtive used. ' .\C T - > .. ' i , a ' ' - A ' t >. 7. Mark if the sample was filtered in the field by marking Y or N in Loitered'.row by the Analysis reqycstejd. ' o v o ' j - ' ,* i- v~ ' .i . . ... __ , . . ' . ,\ , X. Requested Analysis' List the required analysis and methods on the lines provided and place a check in the columtt'fbr.the SctniplesTetjuiriiig the analy sis:. Additional comments should be referenced .in the bottom left hand corner or include attaehmer ts for extended lists, of jjarameters : %*' 9. The sampler should print their narne in the space provided and sign their name followed bv the date o f M;e sampling' event at the'bottom ofithe COC in the spaces designated for "SAMPLER NAME AND SIGNATURE'. \ ,_ 10. When relinquishing custody of the samples to a representative o f the laboratory or other organization, in lieate 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 W eeks/! 0 business days. Results will be delivered"by end o f business on the date duq unless other arrangements hav e 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. ID ID 3 ID ID ID l ^ s f o b ^ n J fy iic fR e ^ s t 6o>cuS?nt=> 'aceAnalytical /Section A >R equired Client Information: Company ^ Drrl r Address $.<> Section B R equired Project Information: Report To: (S e n t- Copy To: .. i-tv ia S T ro v w . The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section C Invoice Information: Attention: Company Name: NPDES UST Page: | of J 1004186 REGULATORY AGENCY GROUNDWATER RCRA DRINKING WATER n Other Email To: i , . . . 1\vi inasrrorn @ i w i n i n . c o m Phone _ Fax Requested Due Date/TAT: Address: Purchase Order No.: Pace Quote Reference: Project Name: t e c a - k c A OiSXaU. OOi F c rtO on. Q H t . Project Number: Pace Project Manager: Pace Profile #: SITE LOCATION G A DIL G IN o h nsc n w i G M I MN n other GNC Secti.on D Required Client Information SAMPLE ID One Character per box. (A-Z, 0 -9 / .-) Samples IDs MUST BE UNIQUE Valid Matrix Codes m atr ix code DRINKING WATER DW WATER WT WASTE WATER WW PRODUCT P SOIL/SOLID SL OIL OL WIPE WP. AIR AR OTHER OT TISSUE TS Sp COLLECTED COMPOSITE START COMPOSITE END/GRAB (ctu0r - Z < o o Preservatives P roject Num ber L ab l.D M il Ml p V o& |o 3jT j. LEJ^ C o 1AlN roi k -I'ASll L i k kC >rr\rp| '1 & % WT t+ij Sfiiki ooQ> w r O tS U /r -Oil O tH ' CoY>p Mop B fp1 1 XXjt I Fta m 00 Cud a Q O T i - Gh it t i ( j3 w r Ml oca i/v f*fa lot. /'lit'qU te/'J/c'0(p 0 5 3 ( 0$> ,fiho /o u / > S 3 /o S 3 Ufaip(o lo^X 'lrjleu, io 3 Additional Comments : i-MArt-t m , i- O'-'<o PAr. Tfr,e fjliojoU u>3 co<*p , 0 / . n b ' r" / ? 0 OH ' - h 1* ' //cc- SEE REVERSE SIDE FOR INSTRUCTIONS REUNOUISHED BY / AFFILIATION TIME S ACCEPTED BY / AFFILIATION DATE | TIME p { '4huJ2JX 3P t D * rA V /V SAMPLE CONDITION SAMPLER NAME AND SIGNATURE PRINT Name o f SAMPLER: SIGNATURE o f SAMPLER:. J ( J u ^ /r r fr / t l A * fc W 'q / / 3 /o 85 c ALLQ020rev.3t31 Mar05 . v m _ _ * __ _ -B ___* .. _# <-- .----- ' -- m '-- JP -----* - -m >___ ........... Instructions for completing Chain of Custody (COC) P f* j\ Q f l e c t io n 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 (G (grab) or C (composite). When collecting a composite, the start tjntc and end time should be documented in the respective boxes. The collection tune for a grab (G) sample should be entered in the boxes marked "Composite Lnd/Grab'). Sample temp at cbllection (if required by'state), the total number o f containers, andpreservative used. 1` 1. V 7. Mark if the sample was filtered in the field by maridng Y orN in 'Filtered' row by the Analysis requested. 1 8 . Requested Analysis: l ast the required analysis and methods on the lines provided and place a check in the column-for the samplesrequiring the analysis. 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 spdee provided and sign their name followed by the date o f the sampling event af the bottom o f the COC in the spaces designated for 'SAMPLER NAMH'AND SIGNATURE'. \. , . " _; . 10. When relinquishing custody o f 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. ! I ^Important Note: * Standard Turnaround Time is 2 W eeks/10 business days. Results will he 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 l ow Level Detection Limits or level of QC reported must be included on the chain of custody in the Additional Comments section. m ~) c d raceAnalytical /Section A ! R equired Client Information: Company ^ ^ z> r r l f r Address 55, Email To: IsviindsfrorjT (woim.Cjm Phone Fax L.<Ti - ? * f t - 53S/3L Requested Due Date/TAT: ^ A i ^ F ^ s f b b ^ n JiR icIR ecjK st S ^ u lQ it The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B R equired Project Information: Report To: , n P v tf Copy To: ,. L ivA a s t y o w v Section C Invoice Information: Attention: Company Name: Address: Purchase Order No.: Pace Quote Reference: Project Name: ViecAk c A Ou^^AlL OOl F c W . O T t . Project Number: ,, n,t Pace Project Manager: Pace Profile #: NPDES UST Page: ^ of | 1004186 REGULATORY AGENCY GROUND WATER RCRA DRINKING WATER Other SITE LOCATION G A D IL D IN noH nsc nw i D M I MN n other DNC Secti.on D Required Client Information SAMPLE ID One Character per box. (A-Z, 0-9 /.- ) Samples IDs MUST BE UNIQUE Valid Matrix Codes m atr ix CODE WTDRINKING WATER DW WATER WASTE WATER WW PRODUCT P SOIL/SOLID SL OIL WIPE AIR OTHER OT TISSUE TS COLLECTED S t--o -<Z COMPOSITE START COMPOSITE END/GRAB oO Preservatives P roject Num ber Lab I.D y r 'Q(p WT h lD ie wr teli o{ Uff tnk>o(. n>r b i l lvU o S 3 . to ML ^i'i loU t o S i Ol, io LI U tol, to 5 3 hhsbi4> fr ' UT 4j l(Q f o ^ i teirilou ! - /> Additional Comments: M < /-a UC f /A U O C>3 5 ' 3W SEE REVERSE SIDE FOR INSTRUCTIONS Ti^r. it '3 / io i' ; ' ' 4 RELINQUISHED BY / AFFILIATION DATE TIME ACCEPTED BY / AFFILIATION y -J .J h r * .-,,-- s/ jfir f t - . i : r > : . ; /- . /'V . , , DATE TIME SAMPLE CONDITION --------------- 1 zz ?? zz V? zz ?? zz >? z ? z ? z ? z > Temp in C Received on Ice Custody Sealed Cooler Samples Intact SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: --' J ) f/ . SIGNATURE of SAM PLER :-, J , l j/ltr t / V ' V ,\ 4i C ^ * . < . t h / - x .----------- f DAT^ Signed ,{MM / DD / YY) } / ~ / i , / i / U / / y / o 5-, ' 1 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 o f 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 tor 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 (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 used. 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 o f parameters. 9. The sampler should print their name in the space provided and sign their name followed by the date o f the sampling event at the bottom o f the COC in the spaces designated for 'SAMPLER NAME AND SIGNATURE'. ' 10. When relinquishing custody o f the samples to a representative o f 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 W eeks/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. 11/29/2006 Project: E06-0694 3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report Page 1 o f 4 Requester: Schnobrich, Dana M (223-1N -08) Department: 530711 Project Number: 0022674449 Date Received: 11/29/2006 Project Description: Decatur Outfall 001 FC Monitoring Quarterly Comments: Completion Date: Project Lead: Kent Lindstrom Phone Number: 651-778-5352 Email Address: krlindstrom@mmm.com Statement o f Accuracy: __________________________________________________ Project Results/Activitv Pace Field Sampling Event 3M Sam ple N um ber______ Sam pled D ate_______Sam ple D escription____________________________________ E06-0694-001 12/12/2006 Outfall 001 Effluent - Composite LAB EXYGEN Analytical Method LCMS Components PFOS Result RL PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid ____________________________________C 12 a c id ____________________________________________________________________ E06-0694-002 12/12/2006 Outfall 001 Effluent - Composite Duplicate LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid Result RL Qualifier Qualifier 11/29/2006 3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report Project: E06-0694 (cont.) 3M S am ple N um ber_______S am pled D ate______ Sam ple D escription E06-0694-003 12/12/2006 Outfall 001 Effluent Comp -1 0 PPB Low Spike LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid Result E06-0694-004 12/12/2006 Outfall 001 Effluent Comp -1 0 0 PPB High Spike LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid Result E 0 6 -0694-005 12/12/2006 Field Control/Travel Blank LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA Result RL RL RL Page 2 o f 4 Qualifier Qualifier Qualifier Il 11/29/2006 3M ENVIRONMENTAL LABORATORY Prelim inary/Unauthorized Report Project: E06-0694 (cont.) 3M Sam ple N um ber_______Sam pled D ate Sample Description E06-0694-005 (cont.) 12/ 12/2006 Field Control/Travel Blank i LAB Analytical Method EXYGEN LCMS (cont.) Components C9 acid CIO acid C ll acid C12 acid Result E06-0694-006 12/ 12/2006 Field C ontrol/Travel Blank Low Spike LAB EXYGEN Analytical Method LCMS Components PFOS PFHS PFBS FOSA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid Result E06-0694-007 12/ 12/2006 Field C ontrol/Travel Blank High Spike f LAB Analytical Method EXYGEN LCMS Components PFOS Result PFHS PFBS FO SA PFBAmide MeFBSE-OH C4 acid C5 acid C6 acid illit C7 acid PFOA C9 acid Ml CIO acid C ll acid C12 acid E06-0694-008 12/ 12/2006 Equipment Blank LAB Analytical Method i EXYGEN LCMS Components PFOS PFHS PFBS FOSA PFBAmide Result Page 3 o f 4 RL Qualifier RL Qualifier RL Qualifier RL Qualifier 11/29/2006 i 3M ENVIRONMENTAL LABORATORY Preliminary/Unauthorized Report Page 4 o f 4 Project: E06-0694 (cont.) 3M Sam ple N um ber______ Sam pled D ate______ Sam ple D escription___________________________________ E06-0694-008 (cont.) 12/12/2006 Equipment Blank m LAB EXYGEN Analytical Method LCMS (cont.) i i Components MeFBSE-OH C4 acid C5 acid C6 acid C7 acid PFOA C9 acid CIO acid C ll acid C12 acid Result RL, Qualifier i i it i Itf 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231 -1580 TEMPORARY SAMPLE STORAGE FORM To be completed during ExyLIMS Login Project # :__________ f f Login # :_________ L / &?] ]_________ In itia ls / D a te:______ (/lh n jr lu . One form to be completed for each package Date / Tim e Received: / 2 -Z ^ /- o C / O Z V Received By: _____________ Shipper: __________________________ Shipper Package ID: Q S 7* S Z. *9 Z. S ' Tem perature (deg C )/ Therm om eter ID: /fy . ~7 Tem perature Control Method: /ty<oAJL^ - /( /* i A ', e .ri> l Tem porary Storage Location: u k / i ; *n Condition of sample(s): i^ G_Gooiod - Package and contents uncompromised ___ Fair - Package damaged / contents uncompromised ___ Poor - Package and contents compromised Notes: LIBRARY ID: V0001402-3 LABORATORY FORM fedax.com 1.800.GaFedEx L800.463.3339 US A irb ill Express 57 52=14 b=123 Recipient's Copy 1 From . I, Data I 9 - 1 1 3> 1? g f J . Q iz d k ^ i Company Pa <C Phone 7 o 4 S 7 - O ^ S D ------- 1 *0 0 K v ^ c e y . A u o i ^ -- rey U u ^ t ? 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