Document mmV1r3qVyMzGbr9jy5BKV3k1B

... . : . a.;. .:, ; ~- :.. . - :.... __ . q ~ceA a.. VV May 14, 204?:"<; Pace Ana0kal Services, Inc. } 700 Ekn St. SE, Suite 200 Minneapotist MN 56414 Phone; 61 2-607- 1700 Fex: 6 1 2-607-64 4 4 Mr. Ke~:r:i,;t:i.L;:i:,Cidstrom 3M ~ri:vlronmenta! Laboratory Build-Mg 260-5N-1 7 MN 5514 4 # k`RE : Lab Project Number : 1050968 Client Project ID: E07-0296 3M Guin Water Special Study Dear Mr. Lindstrom : Enclosed are the analytical results for sample(s) received by the laboratory on May 3 . 2007 . 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 Ande on diane .anderson@pacelabs .com Project Manage r enclosures ~ I ---, ... t~ . : _ 3 p. 2 PACE ANAl .YTlCAI. SERVICES, INC. ~ ceArrelreal3M www.peoefabs .oom Pace Project Manager : Diane Anderson Report Author. Brian Pike Analytical Team : Semivolatile Organics Dept At2**afRqjQt EPA $270 GUMS Pace Workorder 1650968 May 8, 2007 , ? Int:ro;. d< a... .e,:t<ti.a.n. , ;~ Gary Hohenstein of 3M submitted one sample for gas chromatography mass spectrometry (GC/MS) analysis . The sample was analyzed by GClMS 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 for the analysis for sample Distribution System Guin House yielded Diethylene Glycol Sutyt Ether at a concentration of 541 ug/L . The sample duplicate yielded results of 508 ug/L . ~, : ,, . : . ; ._, . .. ., . , :; .. .; .<.~~:.. .. . ' . . . ...... . .. . : : ._ , .; . .. ., : .: . . . The sample was received at Pace Analytical on May 3, 2007 . Please see attached documentation for the sample condition upon rece ipt. The sample was described as follows : Pace Analytical ID Client ID 405 096800 1 f3is#ribution System Guin House 3. Holding Tim-es The EPA 8270 method has a defined extraction holding time of 7 days from collection of sample with a subsequent 40 day analytical holding time . The sample was extracted and analyzed within this holding time . ~ ,: ,. ..Y .. . . , , . .: .. . Ah alyl ical and Preparatory ' . : >. The sample was analyzed under guidelines set forth in the EPA 8270 method for analysis of seml-votatile analyles. The sample and all associated quality control samples were extracted by EPA 3510 (separatory funnel extraction). The sample was measured for volume and the pH was taken . The sample and the quality assurance samples were fortified with surrogates and matrix spikes and laboratory control spikes were fortified with matrix 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 of 60 mL of methylene chloride for 2 minutes each shake . The sample and quality samples were then brought to a pH >11 with ION sodium hydroxide and extracted using 3 separate aliquots of 60 mL of methylene chlo ide for 2 minutes each shake, The extracts were dried by passing through baked and rinsed sodium sulfate prior to ooncentration . The sample and quality control samples were concentrated on a steam bath utilizing a KD/concentrator(snyder column set-up at 90 degrees C . The extract was concentrated to approximately 4-6 mL on the steam bath and then finally down to I mL by way of nitrogen blo+adown . The semivolatile analytes were fortified with 8270 internal standard and directly injected onto the GC/MS analytical system for analysis. The instrumentation used is listed below . Gas Chromatograph : Hewlett Packard 5890 Column : J&W Scientific DS-5MS (30 m x 0.25 mm x 0.5 m film thickness) PAGE 1 OF4 L5 p. 3 PACE ANALYTICAL SERVICES, INC. Detector: Hewlett Packard 5972 Mass Spectrometer Carder Gas : Helium 5- ArWlysis 5.1 Calibratio n A neat standard of 2-(2-Butoxyethoxy)ethanol (also known as Detttylene Glycol Butyl Ether) was purchased from Chem service and diluted into Methylene Chloride . The sample replicates were quantitated for Diethylene Glycol Butyl Ether using the average response factor generated from a six-point internal standard calibra tion curve per the EPA 8270 method . The analytes were calibrated from 10 to 200 ppb and the curve was not forced through ze ro . The quantita ti on was determined from the lowest standard level from the calibration curve . The 13mit of detection has not been statistically determined using a method detection limit study. The initial calibration was not verified by an external source . 5.2 Blanks A method blank was analyzed along with the sample to determine system cleanGness . The method blank was prepared by adding 1000 mL of delonized water into a separato ry funnel . The method blank was extracted the same as the samples (pH adjusted, etc.) . Diethylene Glycol Butyl Ether was not dete cted in the method blank . 5 .3 Surrogate s Surrogates were added to the sample, sample replicates, and all quality control samples before the extraction process. This was done by adding 1 OOpL of 750-1000uglrnL surrogate standard . The recoveries for the surrogate standards may have been influenced by the concentration of target analytes and other non-target analytes present in the samples. The surrogate recoveries are summarized in a table later in this report . 5.4 Matrix Spikes A matrix spike (MS) at a higher concentration ( in upper range of the calibration) and matrix spike at a lower concentrati on ( in lower range of the calibration) were prepared by spiking 300 N1 and 50 pl of a 510 itg (mL solution respectively of Diethylene Glycol Butyl Ether. The laborato ry matri x spikes were attempted but were not used for the accuracy assessment because the endogenous levels in the sample greatly exceeded the fortified spike amounts. 5,5 Laboratory Control- Sample The LCS and LCSD's were extracted the same as the samples . A laboratory cont rol sample (LCS) and laboratory control sample duplicate (LCSD) at a higher concentrati on were prepared by spiking with 300 pL of 510 pg/mL of Diethylene Glycol Butyl Ether solution . The average recovery of Diethytene Glycol Butyl Ether wa s 77.4% . A laboratory control sample (LCS) and laboratory control sample duplicate (LCSD) at a lower concentration were prepared by spiking with 50 p L of 510 NgfmL of Diethylene Glycol Butyl Ether solution. The average recovery of Diethylene Glycol Butyl Ether was 57 .2I9 . 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 performed had a recovery for Diethylene Glycol Butyl Ether of 101 .6% . PAGE20F4 p. 4 PA CE ANAL VT/CAL SERVICES, INC. .6 Data Summary On-column Amount Fina l Sample ID value (ug/mL) Extracted (mL) Concentration Comments Result is over the calibration Distribution System range(Catibrated Guin House 496 .784 1 30 534 u/L to 200 u L Distribution System Guin House 5X dilution 100 .699 930 541 ug/L Result is over the calibration Distribution System range(Calibrated Guin House Duplicate 77 .071 930 913 u/L to 200 u L Distribution Syste m Guin House Duplicate 5X ditution 4.4645 930 508 ug/L Relative Percent Difference Sample to Sample Duplicate (diluted values) = 6 .3 percent On-column Amount Concentratio n value Extracted of Matrix Spike Percen t Sample ID (uglmL) (ml-) added u/mL recove No Peak Not Method Blank Present 1000 Not Applicable Applicable Comments LC S Low Conc 14 .5758 1000 25 .5 57 .16 LCSD Low Cone 14 .5966 1000 25 .5 57 .24 LOS High Cone 117.231 1000 153 76 .62 LCSD H 112h Cone 119.665 1000 153, 78 .21 orig sample Distribution System Guin amount not House MS Low Cone 500.152 930 25.5 1961 .38 subtracted out With sample subtracted is a negative value, detection too Distribution System Guin large in sample to House MS Low Cone 5X achieve accurate dilution 97.6686 930 25 .5 1915 .07 recove . orig sample Distribution System Guin amount not House MS Koh Conc 554 .643 960 153 362 .51 subtracted ou t Recovery with original sample subtracted (from 5X value) yields a 35 .9% recovery . Recovery is possibly bias du e Distribution System Guin to dilution and House MS High Cone 5X detection in the dilution 111 .676 960 153 364 .95 original sample . PAGE3OF4 ~ p. 5 PACE ANALYTrCAL SERVICES, INC. Surrogate Recoveries ( Percent Recovery ) : LCS LCSD LCS Method Low Low High Blank Cone Cone Cone Distribution Distribution system Distribution Dist ribution system Guin House System system Guirl LCSD Guei House MS Low Guln House House M6 Example High MS Low Conc 5X MS High high Cone Reravery Conc Cone dilution Cone SXdilution Limits, 2-Ftuorphenc3 41 .4 35.5 34.3 35 .1 36 .1 28.0 23.2 29.3 24 .5 19-100 Phenol-d6 24 .2 21 .0 19.9 21 .0 22 .9 0 0 0 0 11-100 Nltrobenzene-d5 77 .1 74.3 74.3 77 .4 73 .7 78.5 76 .8 79.6 76 .9 51-100 2-Flucrobl hen 64 .4 59.3 59.4 64 .4 63 .6 2,4,6Tribrornaphenoi 75 .6 74.8 77.7 70 .1 75 .8 75.3 69.2 91 .7 73 .1 60 .5 89 .2 83 .2 49-100 73 .1 23-109 T hen -d14 77 .7 74.6 78 .0 76 .2 83 .6 82 .5 85 .3 84 .2 84 .2 35-142 Diethyiene Glycol Butyl Ether ND 57 .2 57 .2 76 .6 78.2 1961,4 1915 .1 NOW. Accuracy limits for Diethylene Glycol Bt q Ether could not be detem 4ned due to ladt or data points. 382.5 365 ' Recwery limits for seperetay funnel eztrsefians deriNad from a combination of Paco Ansly8cal Green Bay and Indianapolis recovery Gmits for EPA 8270 Distribution Distribution Distribution System Distribution System System Guln System Guin Example Guin Guin House House House Oup Recovery House 5X Duplicate 5X Limits 2-Fluor henol 31 .7 Phenol- d6 0 28.5 i 0 29 .6 27.1 19-100 0 .5 0 11-1 00 Nitrobenzene-d5 62 .0 81 .7 75 .0 74 .9 51-100 2-Fluoroblphen 74 .5 93.3 62 .8 84 .8 49-100 2,4,6-Tribromo enol 71 .7 77.9 71 .9 73 .8 23-109 Te hen -d14 83 .0 88.4 81 .3 82 .4 35-142 7 Observafiotalt?iscus slon MDL studies and initial demonstrations of capability were not performed for Diethylene Glycol Butyl Ether. 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Receipt Client Name: 3!` I Project # 10.5_01(o 8, Courier : u Fed Ex u UPS u USPS Xclient uCommercia u Pace Other Tracking # : Custody Seal on CooierlBox Present : u yes no Seals intact : u yes no Packing Material: ~Bubble Wrap Bubble gags u None u O1he r Thermometer Used 230194010 Type of Ice :~ Blue None Samples on ice, cooling process has begun Temperature Bioo4gica Tissue Is F rozen : Yes Cooler Ternp should be above freezing to 8'C Comments : [late and Inlttals of person examining No contents : C:L..~'~ "Cf~f Chain of Custod Present : u Yes *o u ruA 1, Chain of Custody Filled Out : u Yes u No nuA 2 . Chain of Custody Relinquished : u Y.s u No v}A 3. Sampler Name & Signature on COC: DYes u rao N/A 4. Samples Arrived within Hold Time : cs QNo u N rA ;, Short Hold Time Analysis < 72hr : Rush Turn Around Time Requested, Dyes No UNIA 6. u Yes u No u H/A 7 . Sufficient Volume: v6s ONO Correct Containers Used : Yes CNo u N/A 8 . u NrA 9 . -Pace Containers Used, Yes u No QNIA Containers Intact : u Yes A0 nN/A t 0 . G-i ~ c~,~ Filtered volume received for Dissolved tests u Yes u No K NIA 1 .1 . Sample Labels match COC : DYes A . u N/A 12 . ^J-0 1 D"~ e, 5 ~ .~: ~~~' -Includes date/time/[D/Analysis Matrix : All c ur:tainers rteedutg preservation have been checked- Oyes u No C1A 13, All containers needing preservation are found to be in compliance with EPA recommendation. exception . OA, oliform, TOC, O&G, WI-DRO (water) u Yes u Na ~%/A Initial when Lot # of added Yes u No completed prese rv ative Sample ecked for dechorination : Heads ace in VOA Vials >6mrn : uYes u vo uruA 14 . uYes u No OwA 1 5 . Trip Blank Present : OYas El t,o ON/A 16, Trip Blank Custody Seals Present u Yes u No u NiA Pace Trip Blank Lot N (if purchased : Client Notification/ Resolution : Field Data Required? Person Contacted : Comments/ Resolution : Date/Time: e- ~ i u 1~lil ~'j' C1v~ C3~~ ~2 D RI Y/ N Project Manager Review: Date: Note: Whenever there is a discrepancy affecting North Carolina compliance 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, 11September2006 13