Document 9L16X7qrkd23wymvkpyppq16V

M iZ Z ir 2727 Pace Analytical Services, Inc. 1700 Elm St. SE, Suite 200 Minneapolis, MN $5414 Phone: 612-607-1700 Fax: 612-607-6444 May 14, 20Q;A Mr. Kerrtt-indstrom 3M EnvirwonVment.al ILaboratory Building 260-5N-17 S^FTaul, MN 55144 Mm* ' `RE: m r' J5!**r Lab Project Number: Client Project ID: Dear Mr. Lindstrom: 1050968 E07-0296 3M Guin W ater Special Study Enclosed are the analytical results for sample(s) received by the laboratory on May 3 .2 0 0 7 . Results reported herein conform to the most current NELAC standards, where applicable, unless otherwise narrated in the body of the report. If you have any questions concerning this report, please feel free to contact me. Sincerely, diane.anderson@pacelabs.com Project Manager enclosures P-2 PACE ANALYTICAL SERVICES, INC. Pace Project Manager: Diane Anderson Report Author: Brian Pike Analytical Team: Sem ivolatile Organics Dept AnalyticalReport EPA 8270 GC/MS Pace W orkorder 1050966 May 8,2007 1 : Introduetion ./ 7 Gary Hohenstdn o f 3M submitted one sam ple fo r gas chromatography mass spectrom etry (GC/MS) analysis. The sample was analyzed by GC/MS to verify the concentration of Diethylene Glycol Butyl Ether (CAS 112-34 5) using Method 3510C for the extraction and Method 8270 for the analysis. The results fo r the analysis fo r sample Distribution System Guin House yielded Diethylene Glycol Butyl Ether at a concentration o f 541 u g /L The sample duplicate yielded resufts of 508 ug/L. Sample*Repefot V.'. The sample was received at Pace Analytical on M ay 3, 2007. Please see attached documentation fo r the sample condition upon receipt The sample was described as follows: Pace A n a lytica l ID 1050968001 C lie n t ID Distribution System Guin House 3 Hofding Times The EPA 8270 method has a defined extraction holding tim e of 7 days from collection of sample with a subsequent 40 day analytical holding tim e. The sample was extracted and analyzed within this holding tim e. 4 M e tlm d s k A ^ s i^ ip s I e n d P rep arato ry ; . y - v .V - The sample was analyzed under guidelines set forth in the EPA 8270 method fo r analysis of sem l-voiatile analytes. The sample and all associated quality control samples were extracted by EPA 3510 (separatory funnel extraction). The sample was measured for volum e and the pH was taken. The sample and the quality assurance samples were fortified with surrogates and m atrix spikes and laboratory control spikes were fortified with m atrix spike. The sample and quality samples were first acidified to a pH of <2 with 1:1 sulfuric acid and extracted using 3 separate aliquots o f 60 mL o f methylene chloride fo r 2 minutes each shake. The sample and quality sam ples were then brought to a pH >11 with 10N sodium hydroxide and extracted using 3 separate aliquots o f 60 mL of methylene chloride fo r 2 minutes each shake. The extracts were dried by passing through baked and rinsed sodium sulfate prior to concentration. The sample and quality oontrol samples were concentrated on a steam bath utilizing a KQfooncentrator/snyder column set-up at 90 degrees C. The extract was concentrated to approxim ately 4-6 mL on the steam bath and then finally down to 1 m L by way o f nitrogen blowdown. The sem ivolatiie analytes were fortified w ith 8270 internal standard and directly injected onto the GC/MS analytical system fo r analysis. The instrum entation used is listed below. Gas Chromatograph: Hewlett Packard 5890 Column: J&W Scientific DB-5MS (30 m x 0.25 mm x 0.5 pm film thickness) PAGE 1 OF 4 P -3 PACE ANALYTICAL SERVICES, INC. Detector: Hewlett Packard 5972 Mass Spectrom eter C arrier G as: Helium 5 Analysis 5.1 Calibration A neat standard o f 2-(2-Butoxyethoxy)ethanol (also known as Dlethylene Glycol Butyl Ether) was purchased from Chem service and diluted into Methylene Chloride. The sam ple replicates were quantitated fo r Diethylene G lycol Butyl Ether using the average response factor generated from a six-point internal standard calibration curve per the EPA 8270 method. The analytes were calibrated from 10 to 200 ppb arid the curve was not forced through zero. The quantitation was determined from the lowest standard level from the calibration curve. The lim it o f detection has not been statistically determined using a method detection lim it study. The initial calibration w as not ve rified by an external source. 5.2 Blanks A method blank was analyzed along w ith the sample to determine system cleanliness. The method blank was prepared by adding 1000 mL o f deionized w ater into a separatory funnel. The method blank was extracted the sam e as the samples (pH adjusted, etc.). Drethylene Glycol Butyl Ether was not detected in the method blank. 5.3 Surrogates Surrogates were added to the sample, sam ple replicates, and all quality control samples before the extraction process. This was done by adding 100pL o f 750-1000ug/mL surrogate standard. The recoveries fo r the surrogate standards m ay have been influenced by the concentration o f target analytes and other non-target analytes present in the samples. The surrogate recoveries are sum m arized in a table later in this report. 5.4 Matrix Spikes A m atrix spike (M S) at a higher concentration (in upper range o f the calibration) and matrix spike at a lower concentration (in lower range of the calibration) were prepared by spiking 300 pi and 50 pi of a 510 pg/mL solulion respectively of Diethylene Glycol Butyl Ether. The laboratory m atrix spikes were attem pted but w ere not used fo r the accuracy assessm ent because the endogenous le vels in the sam ple g reatly exceeded the fo rtifie d spike am ounts. 5.5 Laboratory Control Sample The LCS and LCSD's were extracted the same as the samples. A laboratory control sam ple (LCS) and laboratory control sam ple duplicate (LCSD) at a higher concentration were prepared by spiking with 300 pL of 510 pg/m L o f Diethylene Glycol Butyl Ether solution. The average recovery o f Diethylene Glycol Butyl Ether was 77.4%. A laboratory control sample (LCS) and laboratory control sam ple duplicate (LCSD) at a lower concentration were prepared by spiking w ith 50 pL o f 510 pg'roL o f Diethylene Glycol Butyl Ether solution. The average recovery o f Dlethylene Glycol Butyl Ether was 57.2%. 5.6 Continuing Calibration Verification Continuing calibration verification standards (CCV's) were analyzed during the analytical sequence to verify consistent system operation. The opening CCV for the dilutions perform ed had a recovery fo r Diethylene Glycol Butyl Ether of 101.6%. PAGE2 0F4 P-4 PACE ANALYTICAL SERVICES; INC. 6 Data Summary S am ple ID D istri bution System G uin House D istribution System Guin house 5X dilution D istribution System G uin House D uplicate D istribution System Guin House D uplicate 5X d ilu tio n O n-colum n va lu e (u g /m L ) 496784 Am ount F in a l E xtra cte d (m L) C o n ce n tra tio n C om m ents R esult is over the calibration range(C alibrated 930 534 ug/L to 200 ug/L) 100.699 930 477.071 930 541 ug/L 513 ug/L R esult is over the calibration range(C alibrated to 200 ug/L) 94.4645 930 508 ug/L R elative P ercent D ifference Sam ple to Sam ple D uplicate (diluted values) = 6.3 percent S am ple ID Method Blank LCS Low Gone LCSD Low Cone LCS H igh Cone LCSD High Cone D istribution System Guin House MS Low Cone D istribution System Guin House MS Low Cone 5X d ilu tio n D istribution System Guin House MS High Cone D istribution System Guin House MS High Cone 5X d ilu tio n O n -co lu m n va lu e (ug/m L) No Peak P re s e n t 14.5758 14.5966 117.231 119.665 500.152 97.6686 554.643 111.676 A m ount E xtra cte d (m L) 1000 1000 1000 1000 1000 930 930 960 960 C o n ce n tra tio n o f M a trix S p ike added (ug/m L) N ot A pplicable 25.5 2 5 .5 153 153 2 5 .5 2 5 .5 153 153 P ercent re c o v e ry C om m ents Not A pplicable 57.16 57.24 76.62 78.21 orig sam ple amount not 1961.38 subtracted out 1915.07 362.51 W ith sam ple subtracted is a negative value, detection too large in sam ple to achieve accurate recovery. orig sam ple amount not subtracted out R ecovery w ith original sam ple subtracted (from 5X value) yields a 35.9% recovery. R ecovery is possibly bias due to dilution and detection in the 364.95 original sam ple. PAGE 3 OF 4 1 PACE ANALYTICAL SERVICES, INC. Surrogate Recoveries (Percent Recovery): 2-Fluorphenol Phsnohd Nltrobenzene-d5 2-Fluroblphenyl 2.4.8Tribromophenoi Terohenyl-d14 Method Blank 41.4 24.2 77.1 64.4 LCS LOW Cone 35.5 21.0 74.3 59.3 LCSD Low Cone 34.3 19.9 74.3 59.4 LCS High Cone 35.1 21.0 77.4 84.4 LCSD High Cone 38.1 22.9 78.7 63.6 Distribution System Gum House MS Low Cone 28.0 0 78.5 75.3 Distribution System G tin House M S Low Conc5X dilution 23.2 0 76.8 91.7 Distribulion System Guin House M S High Cone 29.3 0 79.6 60.5 Distribution System Guin House MS High Cone SX dilution 24.5 0 76.9 83.2 Example Recovery Limits1 19-100 11-100 51-100 49-100 75.8 77.7 74.8 74.6 77.7 78.0 70.1 76.2 75.8 83.6 69.2 82.5 73.1 85.3 68.2 842 73.1 84.2 23-109 35-142 Diethylene Glycol Butyl Ether ND 57.2 57.2 76.6 78.2 1861.4 *Note: Accuracy limits for Diethylene Glycol Butyl Ether could not be determined due to leek of data points. 1915.1 362.5 365 1 Recovery limits for separatory funnel extractions derived from a combination <rf Paco Analytical Green Bay end Indianapolis recovery limits for EPA 8270 2-FIUo;phenol Phenol-d6 Nitrobenzene-dS 2-Fluoroblphenyl 2,4,6-Tribromophenol Terphenyt-di4 Distribution System Guin House 31.7 0 82.0 74.5 71.7 83.0 Distribution System Guin House 5X 28.5 0 81.7 93.3 77.9 86.4 Distribution System Guin House Duplicate 29.6 0.5 75.0 62.8 71.9 81.3 Distribution System Guin House Dup 5X 27.1 0 74.9 84.6 73.6 82.4 Example Recovery Limits 19-100 11-100 51-100 49-100 23-109 35-142 7 Observaiioh/Discussion MDL studies and initial dem onstrations o f capability were not performed fo r Diethylene Glycol Butyl Ether. The process outlined in this report is based on Pace Analytical's standard operating procedure fo r EPA 8270. 8 Data / Sample Retention Hardcopies and electronic copies of the data are kept on file at the Pace Analytical. PAGE 4 OP 4 Surrogate Recoveries 2-Fluorphenol Phenol-d6 N'rtrobenzene-d5 2-Fluorobiphenyl 2,4,6-Tribromophenol Terphenyl-d14 Distribution Distribution Distribution Distribution System Guin System Guin System Guin System Guin Example Method LCSLow LCSD Low LCS High LCSD High House MS House MS Low House MS House MS High Recovery Blank Cone Cone Cone Cone Low Cone Cone 5X dilution High Cone Cone 5X dilution Limits 41.4 35.5 34.3 35.1 38.1 28 23,2 29.3 24.5 19-100 24.2 77.1 21 74.3 19.9 74.3 21 77.4 22.9 78.7 0 76.5 0 76.8 0 79.6 0 11-100 76.9 51-100 64.4 59.3 59.4 64.4 63.6 75.3 91.7 60.5 83.2 49-100 75.8 74.8 77.7 70.1 75.8 69.2 73.1 69.2 73.1 23-109 77.7 74.6 78 76.2 83.6 82.5 85.3 84.2 84.2 35-142 Diethylene Glycol Butyl E ND 57.2 57.2 76.6 78.2 1961.4 1915.1 362.5 365 2-Fluorphenoi Phenol-d6 Nitrobenzene-d5 2-Fluorobiphenyl 2 ,4 ,6-T ribromophenol Terphenyl-d14 Distribution Distribution Distribution Distribution System System System Example System Guin House Guin House Guin House Recovery Guin House 5X Duplicate Dup 5X Limits 31.7 28.5 29.6 27.1 19-100 0 0 0.5 0 11-100 82 81.7 75 74.9 51-100 74.5 93.3 62.8 84.8 49-100 71.7 77.9 71.9 73.6 23-109 83 88.4 81.3 82.4 35-142 Results for 3M sample for Diethylene Glycol Butvi Ether CAS#H 2-34-5 Sam ple ID distribution System Guin House Distribution System Guin House 5 X dilution Distribution System Guin House Duplicate Distribution System Guin House Duplicate 5X dilution On-colum n value (uq/m L) 496.784 100.699 477.071 94.4645 A m ount Extracted <mU 930 930 930 930 Final Concentration 534 ufl/L 541 uq/L 513 ug/L 506 ug/L C om m ents R esult Is over the calibration ranqefCalibrated to 200 uc/L R esult is over the calibration ranqefCalibrated to 200 uofL Relative Percent Difference Sample to Sample Duplicate (diluted values) = 6.3 percent Quality Control Sam ples Sam ple ID Method Blank LCS Low Cone LCSD Low Cone LCS High Cone LC SD High Cone Distribution System Guin House MS Low Cone Distribution System Guin House MS Low C o re 5 X dilution Distribution System Guin House MS Hiqh Cone Distribution System Guin House MS Hiqh Cone 5X dilution Concentration of Percent On-colum n value A m ount Extracted (mLl M atrix Spike added recovery Com ments No Peak Present 1000 None Non-detec 14.5758 1000 25.5 57. t6 14.5966 1000 25.5 57.24 117.231 1000 153 76.62 119.665 1000 153 78.21 500.152 orig sam ple am ount not subtracted out 930 25.5 1961.38 (pending dilutions for oriqinal sample) w ith sam ple subtracted is a negative value, 97.6686 detection too large in sam ple to achieve 930 25.5 1915.07 accurate recovery. 554.643 orig sam ple am ount not subtracted out 960 153 362.51 (pending dilutions fo r original sample) Recovery with original sam ple subtracted (from 5X value) yields a 3 5.9 % recovery. 111.676 Recovery is possibly bias due to dilution am 960 153 364.95 detection in the original sample. **Calibration range for Diethylene Glycol Butyl Ether 10 ppb (ug/mL) to 200 ppb (ugAnL) 3W Environmental Laboratory Shipping Address: M- Bldg. 2-3E-0S 935 Bush Avenue S i Paul, UN 55106 Totylhrte; Sample Receiving: (551) 778-6753 Alternate: (65l)77&-4946 FAX: (651) 778-6176 C hain o f C ustody / R equest fo r Laboratory A n a lytica l S ervices Project 1p/ProJct Name 3M Guin Volatiles Analysis Template # Sample Condition Upon Receip!: Temperature: `C um er Associateci uous: 0 Acceptable O O ther 0 Received on Ice Copies to: Page___ O t_____ Original - Accompanying Samples i! 1 comments. This chain of custody prepared at 3M Environmental Lap. AC ibe 574/37. (Lcf<L jy jL e x f Vi ''fcu. S fa to n . S to . o^j -3 . Last Page - Originator P t y iV ii/V v . j 'r^AuAj^' ...................................... See Reverse Side for Instructions 3 z U *ih b,___ _ ------ f & c t S fa 0 1 p 00 P-9 p. 10 Sample Condition Upon Receipt 2aceAnalytical Client Name: 3>jA t I Courier: Q Fed Ex D UPS Q U S PS J^j^lient Ocommercial LJ Pace Other Tracking #: Custody Seal on Cooler/Box Present: D y e s /i ^ n o Seals intact: yes Project # / S Z > 3 O f a gM a te Packing Material: ^ ^ B u b b ie Wrap ^ B u b b le Bags Q None Other ____ 2301.94010 Cooler Temperature l\ L .f f Temp should be above freezing to 6'C / Blue None Biological Tissue is Frozen: y8a no Comments: ~ Date and initials of person examining contenta: C s L -' Chain of Custody Present: f Chain of Custody Filled Out: 1 Chain of Custody Relinquished: G yss G n/a 1. ' . Gyes G no x n /a 2. \ O ybs D no J(wa 3, Sampler Name & Signature on COC: GYas Gr-to JTn/a 4. Samples Arrived within Hoid Time: Short Hold Time Analysis (<72hr): Rush Turn Around Time Requested: O no G n/a 5. UYes ^ T no G n/a 6. GYes G no D n/a 7, Sufficient Volume: ySi^es G no G n/a 8. Correct Containers Used: -Pace Containers Used: / ^ V es * - No 9, x jv e s G no O n/a Containers Intact: H yss G n/a 10. < b y \ JL-- Filtered volume received for Dissolved tests Dyes D no J ^ n/a 1-1. Sample Labels match COC: Gyes G n/a 12. 5 -Includes date/dme/ID/Analysis Matrix: i . T"T All containers needing preservation have been cheeked. Qyss GNo C ^ A 13. All containera needing preservation are found to be in compliance with EPA recommendation. exception/roA./oliform, TOC, O&G, WI-DRO (water) |-|y9s b%te^ ' ) ^ i s ^ No Initial when completed _ot ff of added jreservative SampleVcfiecked for dechlorination: Gves G no O n/a 14. Headspace in VOA Vials ( >6mm}: GYes G no G nia 15. Trip Blank Present: Gves G no G n/a 16. T rip Blank Custody Seats Present GYes G no G n/a Pace Trip Blank Lot it (if purchased): . Client Notification/ Resolution: Person Contacted: Comments/ Resolution: _ p A Date/Time: ufa. Field Data Required? slyIn ~ fctfi Y/ N Project Manager Review: Date: < S " h A rj Note: Whenever there is a discrepancy affecting North CaroIinsTcompliance samples, a copy of this form will be sent to the North Carolina DEHNR Certification Office ( i.e out of hold, incorrect preservative, out of temp, incorrect containers) F-ALLC003rev.3, 11Seplember2006 3