Document ppg1wYeBvXkevMn0J8XRrE3kd

Analytical Report Fluorochemical Characterization of Aqueous Samples Decatur Outfall 001 FC Monitoring (E03-0326) Exygen Research Laboratory Report No. L34657 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 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 L34657. 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 Perfluorohexanesulfonate Perfluorooctanesulfonate Perfluorobutvric Acid Perfluoropentanoic Acid Perfluorohexanoic Acid Perfluoroheptanoic Acid Perfluorooctanoic Acid Perfluorononanoic Acid Perfluorodecanoic Acid Perfluoroundecanoic Acid Perfluorododecanoic Acid Perfluorobutanesulfonamide Perfluorooctanesulfonamide 2-(N-methvlperfluorobutanesulfonamido)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. All samples were cooled to 4C from time of collection to receipt at the laboratory. Samples were stored at 4C from receipt until analysis. Eight individual containers were received. Field samples were collected on 5/28/03 and 5/29/03. Samples were received on 5/30/03. Chain-of-custody information is presented in Attachment C. PAGE 2 OF 5 3 Holding Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 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 portion of sample was diluted to forty-milliliters with Type I water. The dilution was performed prior to extraction in order to lessen the effects of matrix enhancement. This matrix enhancement was observed in earlier samples from this location and from screening runs performed on these samples. The diluted samples were 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 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 Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM) Samples were extracted on 6 /1 8 /0 3 . Initial analysis sh o w e d s o m e quality control failures, therefore re-extractions were performed for the C4 Acid, C7 Acid, C8 Acid, C4 Sulfonate, C6 Sulfonate, and C8 Sulfonate were performed on 6/25/03. Samples were analyzed between 6/18/03 and 6/25/03. Raw analytical data is provided in Attachment D. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 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. PAGE3 OF5 Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. 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. 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 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 th e sa m p le results in A ttach m en t 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 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 except the C4 Acid. The statement of accuracy is based on recoveries of field and laboratory spikes. Spike recoveries were within these ranges, except in cases where the spiking level was significantly lower than the indigenous sample concentration. The C4 Acid data is reported as non-quantitative screening data because of low (<50%) recovery of field and laboratory spikes. PAGE4 OF5 6 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 the C4 Acid and MeFBSE-OH. The limit of quantitation for these compounds is 4.0 ng/mL. 7 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. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data 9 Signatures Other Lab Members Contributing to Data Emily Decker Karen Smith PAGE 5 OF 5 SECTION A P roven Results. Summary of Fluorochemical Residues in Outfall 001 Effluent Sample ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup Field Control/Travel Blank Equipment Blank C5 Acid Perfluoropentanolc Acid 2.26 2.18 2.05 ND ND Analyte Found (ng/mL) C6 Acid C7 Acid Perfluorohexanoic Acid Perfluoroheptanoic Acid 11.2 10.9 10.9 5.30 5.38 5.28 ND ND ND ND Sample ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup Field Control/Travel Blank Equipment Blank C8 Acid Perfluorooctanoic Acid 89.0 88.6 87.5 ND ND Analyte Found (ng/mL) 09 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 Sample ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup Field Control/Travel Blank Equipment Blank C12 Acid Perfluorododecanoic Acid ND ND ND ND ND Analyte Found (ng/mL) C4 Sulfonate C6 Sulfonate Perfluorobutanesulfonate Perfluorohexanesulfonate 12.4 6.44 12.3 5.79 12.1 6.21 ND ND ND ND C8 Sulfonate Perfluorooctanesulfonate 39.5 39.7 40.5 ND ND Analyte Found (ng/mL) Sample ID Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* Outfall 001 Effluent-Composite Dup Field Control/Travel Blank Equipment Blank FBSA 43.0 43.7 44.4 ND ND Fo sa 4.38 4.47 4.29 ND ND Me-FBSE-OH** 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 J ^ 3 03055f8 Research Drive < # ^ S tSatatte College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com SECTION B P roven Results. Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent Sample Description Outfall 001 Low Reid Spike Amount Spiked (ng/mL) C5 Acid_________________________ C6 Acid_________________________ C7 Acid 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/m U (%1 (ng/mL) (ng/mL) (%) 2.26 3.01 75 11.2 12.3 110 5.30 6.05 75 Outfall 001 High Field Spike 500 2.26 504 100 11.2 539 106 5.30 454 90 Outfall 001 Spk C Low Lab Spike 1 2.26 1.14 108 11.2 1.37 109 5.30 1.20 107 Outfall 001 Spk D High Lab Spike 500 2.26 488 98 11.2 501 100 5.30 505 101 Field Blank Low Field Spike 1 ND 1.17 117 ND 0.307 31 ND 0.992 99 Field Blank High Field Spike 500 ND 486 97 ND 574 115 ND 440 88 Sample Description Outfall 001 Low Field Spike Amount Spiked (ng /m L) C8 Acid Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) C9 Acid Amt Found Amount in Sample Recovered Recovery (ng/m t) (ng/mL) (%) C10 Acid Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) C11 Acid Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) 1 89.0 88.2 -80A ND , 0.726 73 ND 0.706 71 ND 0.594 59 Outfall 001 High Field Spike 500 89.0 586 99 ND 464 93 ND 471 94 ND 458 92 Outfall 001 Spk C Low Lab Spike 1 89.0 3.28 106 ND 1.01 101 ND 1.00 100 ND 0.989 99 Outfall 001 Spk D High Lab Spike 500 89.0 508 101 ND 527 . 105 ND 543 109 ND 565 113 Field Blank Low Field Spike 1 ND 0.931 93 ND 0.920 92 ND 0.827 83 ND 0.710 71 Field Blank High Field Spike 500 ND 498 100 ND 467 93 ND 426 85 ND 433 87 ND = Not detected = Response between 0 and 1 ng/ml. ASample residue exceeded the spiking level by more than 4 times; therefore an accurate recovery cannot be calculated. J & 3 30055f8 Research Drive State College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com P roven Results. Recovery Summary of Fluorochemical Residues in Outfall 001 Effluent Continued Sample Description Outfall 001 Low Field Spike Amount Spiked (ng/mL) C12 Acid Amt Found Amount in Sample Recovered Recovery (ng/mL) (ng/mL) (%) C4 Sulfonate Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) C6 Sulfonate C8 Sulfonate Amt Found Amount Amt Found Amount in Sample Recovered Recovery in Sample Recovered Recovery (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) ND 0.606 61 12.4 13.5 110 6.44 7.50 106 39.5 37.6 190a Outfall 001 High Field Spike 500 ND 455 91 12.4 473 92 6.44 576 114 39.5 556 103 Outfall 001 Spk C Low Lab Spike 1 ND 1.01. 101 12.4 1.39 108 6.44 1.33 117 39.5 2.15 116 Outfall 001 Spk D High Lab Spike 500 ND 534 107 12.4 445 89 6.44 495 99 39.5 517 103 Field Blank Low Field Spike 1 ND 0.742 74 ND 1.04 104 ND 1.06 106 ND 1.30 130 Field Blank High Field Spike 500 ND 472 94 ND 455 91 ND 568 114 ND 512 102 Sample Description Outfall 001 Low Field Spike Amount Spiked (ng/mL) FBSA Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) FOSA Amt Found Amount in Sample Recovered Recovery (ng/mL) (ng/mL) (%) Nle-FBSE-OH* Amt Found Amount In Sample Recovered Recovery (ng/mL) (ng/mL) (%) 43.0 45.0 200a 4.38 4.85 47A ND ND - Outfall 001 High Field Spike 500 43.0 543 100 4.38 527 105 ND 482 96 Outfall 001 Spk C Low Lab Spike O u tfa ll 001 S pk D High Lab Spike 1 500 43.0 43.0 2.08 529 101 106 4.38 4.38 1.15 104 520 , 104 ND ND * 410 82 Field Blank Low Field Spike ND 0.952 95 ND 0.726 73 ND ND - Field Blank High Field Spike 500 ND 504 101 ND 456 91 ND 535 107 ND = Not detected = Response between 0 and 1 ng/mL. *ND = Not detected = Response between 0 and 4 ng/mL. ASample residue exceeded the spiking level by more than 4 times; therefore an accurate recovery cannot be calculated. 'Response was below the detection limit of 4 ng/mL 1J ^ 3 03055i8 Research Drive - # m s tSatate College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com Proven Results. Summary of C4 Acid in Outfall 001 Effluent Analyte Found (ng/mL) C4 Acid A _________ Sample ID______________ Perfluorobutyric Acid Outfall 001 Effluent-Composite Outfall 001 Effluent-Composite* 25.5 2 5 .3 Outfall 001 Effluent-Composite Dup 24.2 Field Control/Travel Blank ND Equipm ent Blank ND ND = Not detected = Response between 0 and 4 ng/mL. ` Laboratory Duplicate AC4 Acid data is reported as non-quantitative screening data because of low recovery (<50% ) of field and laboratory spikes J ^ 3 03055f8 Research Drive > # ^ S taSt1ate College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com P roven Results. Recovery Summary of C4 Acid in Outfall 001 Effluent Sample Description Outfall 001 Low Field Spike Outfall 001 High Field Spike Amount Spiked (ng/mL) C4 Acid AA Amt Found Amount in Sample Recovered Recovery (ng/mL) (ng/mL) (%) 1 25.5 24.0 -150A 500 25.5 116 18 Outfall 001 Spk C Low Lab Spike 1 25.5 ** - Outfall 001 Spk D High Lab Spike Field Blank Low Field Spike Field Blank High Field Spike 500 1 500 25.5 ND ND 232 46 ND 114 23 ND = Not detected = Response between 0 and 4 ng/mL. ASample residue exceeded the spiking level by more than 4 times; therefore an accurate recovery cannot be calculated. "Response was below the detection limit of 4 ng/mL aa C4 Acid data is reported as non-quantitative screening data because of low recovery (<50%) of field and laboratory spikes J & 3 30055t8 Research Drive .# W 5 taSt1ate College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com SECTION C CHAIN-OF-CUSTODY/Analytical Request Document face A n a lytica l" The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. www.pacelabs.com R equired Client Information: Section A R equired Client Information: Section B Report To: P r D j r c F Ltud ___________________ Page: | of ( 639386 To Be Completed by Pace Analytical and Client SGCtiOtl C Company ^ m EvVi'/aM<vict&U TietX Copy To: t4.-k| S c-Vi 00b^fc-Vn Client Information (Check quote/contract): Address Invoice To: Requested Due Date: ftsT Svxw'.VetO. ^ U.t\c(iiy\<L . 0 . fto jt ' ir. P ^ l , Phone 2. 3 F - 0 3333/ KV7/V Eax ? S~g<33-33J/ p o (2epf (f= ^1 Project Name:/ P r o f i t Deca-ku^ QufLU<pO/ Project Number: *Turn around times less than 14 days subject to laboratory and contractual obligations and may result in a , Rush Turnaround Surcharge. Fc X0o ^ Turn Around Time (TAT) in calendar days. ( (S ') 7 ? P -5 n 2 3 3 l(fc 5 r/) y^??-V 0 0 0 2 ( ? W Quote Reference: Project Manager: Project #: , 3/*i M a l2ioues< Profile0f W , / A -I--------o f f 9 /9 Requested Analysis: /T O ? - 03~?& "PA(G Frtff SA^plirH. fi* DATE COLLECT ITEM # SAMPLE ID One character per box. (A-Z, 0 - 9 / .- ) Sample IDs MUST BE UNIQUE WATER SOIL OIL WIPE AIR TISSUE OTHER WT SL OL V WP AR TS 5 . 1 OT tso MATRIX CODE 3 1 ^ < m^ 2 UJ *=d CtnV^ , Un: mm a/p # Containers Unpreserved Methanol CO 0 Ococv 0z XX 0 X X 0 CO z CO z<0* .C O / / / / / / / / / / Remarks / Lab ID 1 0 u + Z a u t * c>0 1 f A . f c r X i m fl Q ii L rj6 i 1 2 f t U S t U - 1>o r U X J QVM00 6 A K p f m f K/ s t o * % 1 * / _ J - 1"t U _ c o n i r 0 1 Z j lT L L J / A n 1<L V tiz h 1 \-- 7 fflj P i a / 4 5 r*V L _ [_ / d iv . 1 r ^ *T d L / -- n/ 6 * / k i -- j; o k CO / / Q _ 4 /V (J _ <>;k _ F r- TV sr7 ^ 8 L _ / > 1*/<i t j , yg T/T/^ 7 /c 7e 9 y ; C /a / o 1 r & Li *, / x i rr--/* --t---o-----/- l r -- t r i x / x / 10 i~ jy c r 7 - t ___ c 3 * (.r7 -j L 3 H<* r i - H C vc, X 7 - f c C, 6 J 9 (0 3 - 7 - 7 c - ...... 11 i 12 SHIPMENT METHOD SAMPLE CONDITION Temp in C Received on Ice Y/N Sealed Cooler Y/N Samples Intact Y/N Additional Comments: AIRBILL NO. i SHIPPING DATE NO. OF COOLERS SOAHMIVPlrLLEt NI3OWTI ECSO 0.1D C G s ry p o S ^tjL &PS ' c L~ < 0 ' otb AfoTt O Vfr 5 fi Ps( -I _ it . l t-q RELINQUISHED BY /AFFILIATION DATE IS TIME ACCEPTED BY / AFFILIATION 11:00 it r - --------- 7 ^ DATE TIME 7m SAMPLER NAME AND SIGNATURE PRINTNameofSAMtLfe: * l w - < T L V v a a I'VvX^^ SIGNATUREQf^ftlPLER: DATESigned. (MfVfc/DD/YY) 1 --------------- ____________ in s tru c tio n s fo r co m p le tin g Chain of C usto dy (COC) 1; Complete all Client Information at top of sheet: name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if different from client, POQ 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 hied 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. ' 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 made prior to samples being submitted to the laboratory. Contact your project manager. Special Project Requirements such as Low level Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) CHAIN-OF-CUSTODY / Analytical Request Document race A nalytica l www.pacelabs.com R equired Client Information: Section A Company 3^^ Address 1 jy*.--f-L. I Ci H Q F a s t r~>-roiA f] t ' v - U / n A i P f f , l~ A ^ . R equired Client Information: Report To: f * t ad P\ d Copy To: The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Page: j of Client Information (Check quote/contract): Requested Due Date: 639389 To Be Completed by Pace Analytical and Client Quote Reference: Section C Project Manager: b u .l/L , 2.-T-Q7 O' 6* o * ST f i r v - ' i 3 "5 s / 'V7 /V> r ja 7 ? P - 5^33 P.o. i Z f p p ! 30 7 /! * Turn around times less than 14 days subject to laboratory and contractual obligations and may result in a Project Name:{Yro i ' ' * Rush Turnaround Surcharge. 5 3 - 3 37/ LPrsyifi. r-,.,<f-dlL mOl F t l/Vffir, I Turn Around Time (TAT) in calendar days. Project Number: -2.24, O Q CO <-.7 y9 Project JJ/v? #: U/5 3 Profile #: r'* \, ijf\ b0* o s ' / - / / Poo * F 03 ~ Vfl Section D R equired Client Information: S A M P L E ID One character per box. (A-Z, 0-9 / .- ) Sample IDs MUST BE UNIQUE MATRIX CODE # Containers Unpreserved NaOH 1 Methanol | Other | Valid Matrix Codes < MATRIX CODE WATER WT SOIL SL i t OIL OL M WIPE WP AIR TISSUE AR TS e - OTHER OT QQ LU LU <0 d^ O O s2E 0LU P d0 re mm/ dd/ yy hahm:m(m? a/p Preservatives t OCO 0 z 0 XXX CD 0COCM cq1 z / l ~ H `-ip / $ 7 y '/* ^ " u` ^ ** ^ / / / / / / / / / / R em arks / Lab ID _o u t - t C>Q 1 - r\- f i d "A V- -- /^ t, n - .- j 1 L -r 7 ; r / / - 0 - U L 1 L -- X;-, < - T > dir t i /* 0 iT\ j r 0 1 Z : Vs vr - ( OKtNp r si t _ a 3 / io a ftf p z iv' 0 i ' ! - F 1 ___J ' ; / 0 1 / i : -y. O ' ; 7 1 lJ 2 .m L- t i tj ai ft. ! /I / ^ A. - */ t j '/ , --,, A*: < , Aa i !/ / y m . Q s i/o 2 j/ ./a ft /i / -./ . r 1 1 ; X 4 O r '{ L ' `Vi- ` '' / r/;_ / : / - //. ^ FI L rU ! / 4 /o / T i r/ !^ .JoA /: 1 (' ^ i SHIPMENT METHOD SAMPLE CONDITION Temp in C Received on Ice Y/N Sealed Cooler Y/N Sam ples Intact Y/N Additional Comments: 1J SAMPLE NOTES V . tkT". V, `7 4v' / fV ` ^ L. j; d SHIPPING DATE NO. OF COOLERS ITEM NUMBER RELINQUISHED BY / AFFILIATION DATE -o*- 0 .1 0 tv / l - H \ \ N._/ < _____ ^ /o > TIME I t to ACCEPTED BY / AFFILIATION J __ ______ _ T T " -------- ff irr ---------------------------/7-------y- 7+---------- DATE .j j. C c r~*^pc>r / f j ,t v, r -fi. [ )?>. ' C 1--- - ' O T c O vJ u -V , ] \ i c cP 0 O *--* ht 1 u SAMPLER NAME AND SIGNATURE PRINT Name^of SAMPLER: , - ______O Kk VA-\ -f ( \ SIGNATURE qf^M^LER: ' yv-- DATE Signed, ( M M /D D /Y Y ) _______ TIME /, * in s tru c tio n s fo r completing Chain of C usto dy (COC) 1 Complete ail Client "information at top of sheet; name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if different from ceni, PC#, Project Name and/or Project Number as it will appear on the report. Quote Reference.. Project Manager, Project No. and Pa No, will be comple'ed by Pace, COC m u jo coil o ' enoh ucty of sum 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. ` 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 made prior to samples being submitted to the laboratory. Contact your project manager. ii . ; Special.Project Requirements such as Low l evel Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) CHAIN-OF-CUSTODY/Analytical Request Document *aceA n a lytica l' 77e Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. www.pacelabs.com Required Client Information: Company p y y \ r r, U ; f c ,1 w L Address PtsT SGCtiOD A T < * cln c<--( /> , i-A r: R equired Client Information: Report To: O , > L - ft f T > -- s Copy To; (\ f'J A Invoice To: Section B Page: i of | Client Information (Check quote/contract): Requested Due Date: 63938* To Be Completed by Pace Analytical and Client Quote Reference: Section C Project Manager: b u ,V ! 4-- J - 0 7 m ; L i* ' 3 ? 3 V / A vi O'? V Phone Fax . 6>S' ) 7 ? H - T- 3 3 (t S 7 ) 7 7 b - V P.0 .Ctopl tr 50 7 /1 Project Name:/pi'o r '' 1 n s lu * , O if* fcfl I L lO Q f Project Number: D O 0 7 ( ^ 7 p<4 9 -Y Turn around times less than 14 days subject to laboratory and contractual obligations and may result In a Rush Turnaround Surcharge. f < </*0n f Turn Around-Time (TAT) in calendar days. Project #: ,, j/V 7 A 3 . r . ** Profile It: ",F'* ' i f t T OS't -7 / SOP Requested Analysis: / / 0 3 -- OZS Q, x y r - ' r . r<J 5^1 /////// i- f '7 ' Section D R equired Client Information: S A M P L E ID One character per box. (A-Z, 0-9 / .- ) Sample IDs MUST BE UNIQUE Valid Matrix Codes MATRIX CODE WATER WT - SOIL SL : ^ OIL OL w ip e w p ;. AIR TISSUE OTHER A R j! ^ ^ TS i (VS '* OT < ` > LU [ o 5 LU Q =1 o o o LU m 2 LU = d r-n -iflo * 1 mm / dd / yy hh:mm a/p Preservatives / / /s r / c / / y n y 7 K K r y ^ 4 / r 'A y j r y J - o 3 J io Remarks / Lab ID /0 .- r UU. o T( -v- V f L <- r t- Di jt V 530-TM 5 *$ Mr O ! \fr r , u :o m o,n P f \.o^ t r\ tC. a/ &$Bbp, f ] V/ / // // /iy SAMPLE CONDITION Temp i|i C R ecei\^d on Ice Y/N Sealed Cooler Y/N Samples Intact Y/N _ _________ Additional Comments: AIRBILL NO. SAMPLE NOTES t\P 7 , ^ T1 ''' \ / v- " - - SHIPPING DATE NO. OF COOLERS ITEM NUMBER RELINQUISHED BY / AFFILIATION DATE v -<cv 0 . / 0 A -, > \ ( L. \ ! ------------------ TIME ACCEPTED BY / AFFILIATION DATE 1 1-o o T/"1-----------------------------------------------fA-----v----", ----------- TIME C c'-V 'p o zrti %>.i ' C l-- 0. Tf iZ r-- r I , o -!it ' Noie o vt< {,|!<j jp-M-'i !I ---------------------------------- -- --- --- ----------------- i SAMPLER NAME AND SIGNATURE PRINT Namejpf SAPJPL^p: O v..:v ' O1 SIGNATURE of S A IL E R : DATE Sigrjec (M IJ/DD/YY) 1,^ 3 Instructions fo r completing Chain of C usto dy (COC) 1, Complete all Client Information at top of sheet: name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if different from client, PC#, Project Name and/or Project Number as it will appear on the report. 2. Quote Reference, P;eject Manager, Project Mo. and PwQe No, will be completed by Pace. . A sepa>-ate cO o must no iilieu out tor each usy of saucae collection. 4. Sampler should print their name in the space provided and sign their name followed by the date of the sampling event. 1 5, Complete Sample Description as it will appear on the laboratory report; include time of sampling, sample matrix, no. of containers and preservative used. ' , 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 made prior to samples being subrniiteddo the laboratory. Contact your project manager. " i r, Special.Project Requirements such as Low Level Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) . CHAIN-OF-CUSTODY / Analytical Request Document Pace A nalytical www.pacelabs.com Required Client Information: Company Section A Required Client Information: Report To: Copy To: \M The Chain-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Section B Page: of 63938R To Be C om pleted by Pace Analytical and Client Quote Reference Section C -m ' Address T ac C ' t A ft ' no /o f . LA p. 0 ,,, >' A ; Phone 6S 0 ' JT - o 7 3 s 3 ?/ ^V7 'V s ` . >'*'> m / Fax 3 3 f6s-< ) 7 7 ; - 7 y j f c i. ; Invoice To: P.O. '/ Project N a m e y r' p f q ^ * i O 'X > rt Project Number: fpiL coI "> > . t T -V' 1 c/- y r ( ah,. Client Inform ation (Check quote/contract): Requested Due Date: l'TAT: 1 Turn around tim es less than 14 days subject to laboratory and contractual obligations and may result in a Rush Turnaround Surcharge. J Turn Around-Time (TAT) in calendar days. Project Manager: Project #: J /i- i t - t ~ ^ Profile #: l ''> . i f i v > f! ' n _____ ---------------------------7------- 7 ~ -- 7-------7------- 7-------; r r - y ., 7 . 7------- 7-------7-------7------ Section D Required Client Information: SAMPLE ID One character per box. (A-Z, 0-9 /.- ) Sample IDs MUST BE UNIQUE Valid Matrix Codes --------- MATRIX CODE WATER WT SOIL SL OIL OL WIPE WP AIR AR ^ TISSUE OTHER TOST : f-AJ ^ mm / dd / yy *V'- , \ rj / a u u- c 7 i h .i j" Ili t [ u - -1Ap nr 1 ! - - f V- L_/ ' 4? - / !c _i_r -1-1.; O i.-.' / / L ( , ^ / . L / - -/ - Yj ( -J .7 J y- i j - ! :I I; '/ ! SAMPLE CONDITION Temp in C Received on Ice Y/N Sealed Cooler Y/N Sam ples Intact Y/N Additional Comments: / !j i1 AIRBILL NO. SAMPLE NOTES /V ' , ii :j { 'i i --- j T _ i . ..... - -- i s /SHIPPING DATE NO. OF COOLERS ITEM NUMBER RELINQUISHED BY AFFILIATION DATE < \ .J,,,.V__----M ~ ;v r# C TIME /ACCEPTED BY AFFILIATION II I' : // //_ DATE TIME C r . , p c -."L f -n i - 7 7 7 ^ ..- : Jr'> C ' ^ L - ' ' ol r r j .. fr i/ , Ui r - r n i i SAMPLER NAME AND SIGNATURE PRINT Name of SAMPLER: - i , \ SIGNATURE of SAMPLER: .; ) .- .-- -- DATE Signed : ( M M /D D /Y Y ) 14 i I.7> Instructions for completing Chain of Custody (COC) 1. Complete all Client Information at top of sheet: name, address, phone, contact (person to whom report will be sent and contact can be made if questions arise), billing information if 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 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. 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 made prior to samples being submitted to the laboratory. Contact your project manager. Special Project Requirements such as Low Level Detection Limits or level of QC reported must be indicated on the chain of custody. (Use Additional Comments Section.) John Quartieri - 3M Decatur Lab Request From: To: Date: Subject: <rasm ith@ m m m .com > <John.Q ualtieri@ pacelabs.com > 5/23/03 12:54PM 3M Decatur Lab Request I have attached the 3M Lab Request form for the Decatur FC project. You will also have a number of bottles that are not listed on this Lab Request. They are for QC samples that will not be reported in this format, only on the Exygen report. (See attached file: Decatur FC - May LR.pdf) Thanks, Rich Richard Smith Pace Analytical Services, Inc. Field Services Division Servicing on-site: 3M Environmental Laboratory, Building 2-3E-09 Phone: 651-778-6913, FAX: 651-778-4226 Email: rasmith@ mmm.com CONFIDENTIAL This communication is intended only for the addressee(s) named above. It contains confidential information. Unauthorized use, disclosure, dissemination or copying of this communication, or any part thereof, is strictly prohibited. If the reader of this message is not the intended recipient please notify us immediately by telephone or electronic mail and delete or destroy this message and all copies thereof, including attachments. CC: <Felicia.Grogan@pacelabs.com>, <jseldridge@ mmm.com>, "Brad Jacobson" < bjacobso n@ p acelabs.com > Page 1 John Q u iltiri - Decatur FC - May LR.pdf Page 1 5/23/2003 Project: E03-0326 3M ENVIRONMENTAL LABORATORY P relim in a ry /U n a u th o rizec R ep o rt Requester: Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number: 0022674449 Date Received: 5/22/2003 Project Description: Decatur Outfall 001 FC Monitoring Comments: Completion Date: Project Lead: Jess S. Eldridge Phone Number: 651-778-5233 Email Address: jseldridge@mmm.com Project Results/Activity Pace Field Sampling Event 3M SampleNum ber E03-0326-48837 S a m p le d D a te 5/28/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN EXYGEN A nalytical M ethod PFOS by ESMS PFHS PFBS by ESMS FOSA PFOA E 03-0326-48861 5/28/2003 LAB EXYGEN EXYGEN Analytical M ethod PFOS by ESMS PFHS EXYGEN EXYGEN EXYGEN PFBS by ESMS FOSA PFOA E 03-0326-48862 5/28/2003 LAB EXYGEN Analytical M ethod PFOS by ESMS EXYGEN PFHS EXYGEN PFBS by ESMS EXYGEN FOSA EXYGEN PFOA E 03-0326-48863 5/28/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN EXYGEN Analytical M ethod PFOS by ESMS PFHS PFBS by ESMS FOSA PFOA Sample Description Outfall 001 Effluent - Composite Com ponents PFOS PFHS PFBS FOSA PFOA Result O u tfa ll 001 E fflu e n t - C o m p o s ite D u p lic a te Com ponents PFOS PFHS PFBS FOSA PFOA Field C o n tro l/T ra v e l B lank Result Com ponents PFOS PFHS PFBS FOSA PFOA E q u ip m e n t B lank Result Com ponents PFOS PFHS PFBS FOSA PFOA Result RL RL RL RL I of I Q ualifier Q ualifier Q ualifier Q ualifier RESEARCH 3058 Research Drive State College, PA 16801 Phone: 800-281-3219 Fax: 814-272-1019 Laboratory Sample Log-in Sheet (Environmental) Complete upon sample receipt: Client and/or Project Name Method of Delivery Walk-in Tracking#: Pick-up 01 J I'd UPS /* / Ji^FedEx Air Borne Other (explain! Chain of Custody Temperature Preservation Custody Seals: ^B'present, & Jtfntact / broken (explain) absent Thermometer ID: 0 ^ 2) i Cooler ID: {xoeoO O / "/ Cooler ID: Cooler ID: Cooler ID: Cooler temp: Cooler temD: Cooler temD: Cooler temD: . ? C C C C Chain of Custody Record: present absent Samples Receiyed: .R tip ic e ice meit with ice pack none Explanation Completed by Slanature: * Complete durlna sample log-ln: LIMS Log-in # Physical Condition Samples intact? Chain of Custody Samples received agree with COC record? Analysis Request Analysis request clear? r Preservation Sample containers appropriate? Chemical preservation appropriate? Samples received within holding time? Sample volume/mass adequate? Date fTimel: * f / ?0/ cM en JZ ides No (explain) / Y e s No (explain) O^Ves No (explain) Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain) Explanation Completed by Slanature: / Date: h0 Complete following resolution of anv nonconformances: Client Contacted Yes Client: No Resolution Date (Timet: Completed by Signature: Lab Sx Log-in Sheet -Ex Date: 11-5-01/0 LOGIN CHAIN OF CUSTODY REPORT (InOl) Jun 02 2003, 07:58 am Login Number: L34657 Account: 2046 3M ENVIRONMENTAL LABORATORY L3 4657-1 :; '% ...OUTFALL 001 EFFLUE N T - C O MP O S I T E 2 8 -MAY-03 3 0 -MAY- 03 L34657-2 I; . ::; OUTFALL 001 E F FLUENT-COMPOS ITE 2 8 - M A Y - 03 3 0 - M A Y - 03 COMPLETE ID READS OUTFALL 001 EFFLUENT-COMPOSITE DUP. L34657-3 : 'J ; FIELD CONT R OL/TRAVEL B L A N K 2 9 -MAY- 03 30 -MAY- 03 : L34657-4 ;/"-"C;r". EQUIPMENT BIANK I I S - M A Y - 03 3 0 - M A Y - 03: ; : L34657-5 SAMPLE #1 L OW S PK 1 PPB 2 9 -MAY-03 30-MAY-03 L34657-6 J! SAMPLE #1 HIGH SPK 500 PPB 29-MAY-03 30-MAY-03 L34657-7 F . .;C:; FIELD B L A N K 1 PPB SP K 30-MAY-03 V L34657-8 ; : ::C. H I G H .FIELD B L A N K 500 PPB SPK 30-MAY-03 Page 1 Signature : Date : USA Airbill Express 1 From s.__ U -lh i fl4D7SEflaTi70FedEx Tracking Number Nanner S v j " / j ) ^ Companv - E a C P L f j l f i y \ ____________ / rlaltf {-c a I Phqho 7 0 V \ S ervice. ~JyyC. Address ____ 9 _ B _ q o Iw k ic A / ^T A A je j u . e_____ S h A t io D ^ Dept/Floor/Suite/Room l^UVA'VlfSU4-lLe A/ C- 07 9____City ________ State z ip _____ 2 Your Internal Billing Reference 3 To 3oh / o hHr.Recipient's!! Name F fir Ty____ _ Phone fioo - 3 3 )1 Company E / y ^ m _______________ ------ 'T Address To'HOLD* at FedEx location, print FedEx address. , We cannot deliver to P.0, boxes or P.0. ZIP codes. Address 3 0 ^ 0 ___ PS, e n / c \ D n ) (EL. Oept/Floor/Suite/Rooni City A A ^ C -____ C o l / e d b .____ State ? A \(>ZIP_____ <00 [ A4Q7 SEfi 1*170 a- r ' L ______ ___ 4a Express Package Service Packagesup to 150lbs. DeWery commitment may be later in some erees. r FedEx Priority Overnight k Next business morning r i FedExStandard Overnight 1-- J Next business afternoon * I I FedEx First Overnight 1-- 1 Earliest next business mommg delivery to select locsbons I I FedEx 2Day ( Second business day [ Fex Express Saver TlfrfJsn'Mxay FedEx Envelope rate not available Minimum charge, une pound rete 4b Express Freight Service [ ~ ] FedEx 1Day Freight* '-- * Next butmoss day Cell for Confirmebon t ^