Document 82nJ9z4LyBdr6LOeyK68mB65k

H^LancasterLaboratories ygr 2425 New Holland Pike Lancaster, PA 17601 AR226-2726 Analysis #0813FC - Revision 01 Supersedes Date: None "^ . Effective Date: Page 1 of 11 g3 ^ Extraction of Low Level FC-143 in Water and Wastewater Reference: Low Level Determination of FC-143 in Water, CH2M Hill, Inc., 0 -a Cross Reference: The following procedure is cross-referenced in SOP-OE-001, "Glassware Cleaning for Organ] Scope: SSBP . This method is designed to extrac^y^^^^nrrfoniupmerfluorooctanoate)from water. Basic Principles: FC-143 is extracted fp concentrated on a s| ethanol. Sulfuri^^i derivatize the with deio Impll^ta pH <1.5 into MTBE. The MTBE is gThe sample is then concentrated and exchanged to to the via! and then heated at 65C for 1 hour to ollowing this step, the sample is washed multiple times dfplaced into an autosampler vial for analysis. brage Conditions: ' w^gw" luld be extracted within 14 days of collection. prior to extraction. ' - ; All samples should be stored . COMPANY CONFIDENTIAL ft -ancaster Laboratories 2425 New Holland Rke Lancaster, PA 17601 Analysis #0813FC ' Revision 01 Supersedes Date: None Effective Date: a^p n u 5 q Page 2 of 11 "s il fc,!jy1. 14. Pipettes - Disposable 15. pH paper-Assorted ranges COMPANY CONFIDENTIAL _ancaster Laboratories 2d25 New Holland Pke Lancaster, PA 17601 Analysis #0813FC - Revision 01 Supersedes Date: None Effective Date: agKo ny 4s Page 3 of 1-1 "8 16. Solvent pumps 17. Automatic shaker-Capable of holding 2 L separator funnels 18. Beakers - Assorted sizes 19. Reacti therm vials 20. Screw cap GC vials 21. Glass wool 22. Amber crimp top GC vials 23. Balance - Capable of we| e grade or equivalent ide or equivalent fdegrade or equivalent esticide grade or equivalent sulfate - Reagent grade or equivalent. Bake at 400C for-4 hours in ' shallow pan to remove contaminants. Store in a glass jar for up to 1 year ""after baking. . 6. Sulfuric acid - ACS grade or equivalent (To prepare 1:1 solution, using graduated cylinders, add equal amount concentrated acid to deionized water in a volumetric flask. Never add-waterto add. Store for up to 1 year.) COMPANY CONFIDENTIAL ^I^LancasterLaboratories ^gr 2425 New Holland Pite Lancaster, PA 17601 ' Analysis #0813FC Revision 01 Supersedes Date: None Effective Date: Page 4 of 11 A, PR 0 3 2081 '^^ 7. Sodium hydroxide - ACS grade or equivalent - 10 N - Add 40 g NaRH to approximately 80 mL of deionized water in a volumetric flask. -" '" NaOH goes into solution. Using a wash bottle, dilute to 100 deionized water. Store at room temperature in a glass bot""" stable 1 year. If 1 N NaOH is needed a dilution of 10x 10 N solution. 8. Alumina N (neutral) super I activity-Use as 9. TeflonTM-boiling chips - Rinse thorough to remove contaminants- thyfene chloride prior to use Preparation of Glassware: See SOP-OE-001. Prior to use, th hexane to remove contaminants^rfiile" S^S9.h. appropriate rinse solvent. insed with either.ethyl ether or list of glassware and the Safety Precautions: Always add acid tc solutions get he ..s juce fuming. The sulfuric acid and sodium hydroxide ^ sd. Always wear gloves when handling these solutions. FC-143JS exposg| ^Jangerous i.n the neat form. The time weighted average mg/m3. Therefore, extreme care must be used when working jnd. Also, heating of the neat standard or any concentrated ie avoided. Any handling of the neat product must be done in a ^.. second analyst observing the process and acting as a safety spotter. The compounds used as surrogates standards are also dangerous. These compounds form hydrofluoric acid upon heating or breakdown. Therefore, the exposure of the neat material to any concentrated solutions must be avoided. COMPANY CONFIDENTIAL -ancaster Laboratories 2^25 New Holland Pike Lancaster, PA 17601 Analysis #0813FC - Revision 01 Supersedes Date: None Effective Date: . Page 5 of 11 APR 0 3 2081 The toxicity or carcinogenicity of each reagent used in this method has not been precisely defined; however, each chemical compound should be treated as^^'"' health 'hazard. From this viewpoint, exposure to these chemicals must he^redl fume^''"'"'5'31"5*'" the lowest possible level by whatever means available, such as safety glasses, and gloves. Always wear gloves when handling any samples or standar safety equipment must be utilized (lab coat, safety glasse: Since the extracts are concentrated on a steam working around this apparatus. All solvent wast be collected for recycling (if applicable) or mus containers. These will then be transferred waste material (disposable pipettes, bro in the normal solid waste collection m'flffbe exercised while rpm this preparation must tif in the designated disposal facility. Any solid C"pHpaper) may be disposed of Personnel Training and Qualifil All personnel performing t ^w yielded acceptable recgj working with an exD_gS|gn ^SS^siSi-. proficiency of th fes should have performed a quad study that '143. Personnel should spend several days paration technician who has demonstrated their Also, seve observa^ capabifnde r .,!i- vS-ss-a-. - Herbicide water samples should be performed under the direct experienced preparation technician to assure the trainee is ident preparation. COMPANY CONFIDENTIAL 4l^ Lancaster Laboratories T(F 2425 New Holland Pike lancasler; PA 17601 Analysis #0813FC ' Revision 01 Supersedes Date: None -^ EPfafgeceti6veofD1a1te: ArN ,,u . m Procedure: 1. Set up a 2-L separatory funnel for each sample and QC sam)J;S extracted. For field samples which are using 1 full bottle, the bottle with a scriber at the meniscus of the sample volu'B bottle vigorously and then pour the contents into a 2-^^garl [funnel. Fill the bottle to the marked level with water and transf^fl^^^^lo a graduated cylinder to determine the initial volu^^^teml^ply, weigh the empty bottle and tare the balance. Fill the be^^^^^arked level with water and place the bottle on the tared bal^gg, This^tight rounded to a whole number is the initial sample volu^g^tf^^asamplesusing a specified volume, shake each bottle vigorou cylinder to measure the desired s graduated cylinder. Record a clean graduated .sfer the sample to a 1-L any comments about the samples in the extraction In; 2-L separatory funnel. 2. Using pipettes, adj sample in the aqueo andards and spiking solutions to the aqueous ie!. Be certain the standard drips directly into it touching the glass side of the separatory funnel or poor iay result. Add 1 mL FC-143 surrogate (perflubrononanoic acid) to all tanks, and spikes. iiking solutions - Add 1 mL FC-143 spiking solution to the laboratory _ lontrol sample (LCS), LCSD if applicable, matrix spike, and matrix spike duplicate samples. Using a disposable pipette, adjust the pH of the sample to >12 with 10 N NaOH, Check the pH using pH paper to ensure it is >12. COMPANY CONFIDENTIAL ^i^LancasterLaboratories , ^g(r 2425 New Holland Pike . Lancaster, PA 1760) .^^ Al"ial, ySlS #081 3FC - Revision 01 Supersedes Date: None Effective Date: Page 7 of 11 W^"^ pp 0 ^ ^m 4. Using asolvent pump, add,100 mL of methylene chloride to the se,aRifia^_ratory funnel, cap the funnel, invert it, and vent immediately. Place the -"'" the automatic shaker and shake at the designated speed for; . the stopcocks closed. NOTE: Shaker speeds vary greatly between instru setting is marked on each. j| 5. Allow the phases to separate for at.least 10^^ffteS^^fin the stopcock and drain the methylene chloride (bottom layer^^^gi wasWcontainer and 6. Using a disposable pipette, adju^yeg^jftV^e samples to <1.5 with 1:1 sulfuric acid. Check the pl^^^yy^iper to ensure it is <1.5. 7. Using a solvent pump, 100 mL of MTBE bottle or graduated cylinder with separatory funnel. 8. Shake the seDg^bj^^^^lfbr 2 minutes on the automatic shaker. separate for 5-10 minutes before draining the aqueous b a 2-L beaker. extract through approximately 10 cm of sodium sulfate into a us containing a TeflonTM-boiling chip. h the aqueous sample to its respective separatory funnel. Using a Ivent pump, rinse the sample bottle or graduate with 60 mL of fresh, MTBE 'efore adding the MTBE to the separatory funnel. 12. Repeat steps 8 through 11. 13. Repeat steps 8 through 1'0. COMPANY CONFIDENTIAL ^i^LancasterLaboratories Ugr 2425 New Holland Pike Lancester, PA 17601 . A l i a l,y S . I S #, 081 3FC Revision 01 Supersedes Date: None Effective Date: Page 8 of 11 .A.,P,, R 0, 3 2QQ1 14. Attach a 3-ball Snyder column to the K-D, wet with MTBE, and concentrate at 80 to 85C to less than 4 mL. 15. Using a pipette, add 5 mL ofethanol to the ampule and N-j 35 2C to 1 mL. ^ 16. Place 10 drops from a disposable pipette of conq^^rte^^^iBc acid into a reacti therm vial, then transfer the extract to ffllTtlyand swiri. 17. ' Place the sample on a rack into an overL_a^^i 67'''Cffor 1 hour to derivatize the compounds of interest^^^^^^^^tiveethyj esters. . 18. Remove the samples from the tft^diately place the reactor vials in the freezer until cold, apprd^^^^^Kiinutes. Remove the cap and using pipettes, add 1.0 my^^a^^^ychloride and 1.0 mL of deionized water. Recap and sha^^lg'Q^^sly'tor several seconds. Allow the phases to separate and using .gJS^^^j^B^ipette remove the methylene chloride (lower)- layer. ,,' -S5g! chloride layer into a screw cap GC vial containing jyater. Cap the vial and shake vigorously for several phases to separate. Remove the methylene chloride h the extract through a disposable pipette containing a plug nd sodium sulfate. Bring the extract to exactly 1.0 mL with v the extract in an amber crimp top GC vial. Cap the GC vial securely nd store in the freezer. Record the final volume in the extraction log, Calculations: See analysis method. COMPANY CONFIDENTIAL I^LancasterLaboratories W 2425 New Holland Pike Lancastai; PA -17601 Analysis #0813FC - Revision 01 Supersedes Date: None Effective Date: 'Page 9 of 11 . APR 0 3 2QQ1 Statistical Information: See analysis method. Quality Assurance: Each day samples are extracted, a blank, laboratory control water blank spiked with all compounds of interest carried and LCSD if applicable must be prepared. In addition^ le^^^l^eionized Ahe enlTreprocedure), and matrix spike duplicate must be extracted. If there is limited sarn^j^ 5 prevents the preparation of the MS/MSD, the LCSD must be prepared ins|gjr' field or equipment blank samples, the LCC/L^^^ batch contains only Fshouldbe used. A batch is defined as the samples to be extracted ', but not to exceed 20 field samples. If more than 20 samples are p ly an additional batch must be prepared. If any client, agency, or ringent QC or batch requirements, these must be followed instead. Revision Log: Initiated Date: 03/22/1 .SiS-, COMPANY CONFIDENTIAL Analysis #0813 FC - Revision 01 Supersedes Date: None Effective Date: Page 10 of 11 A, _P_R 0. . ^ 29S1 COMPANY CONFIDENTIAL .ancaster Laboratories 21Z5 New Holland Pike Lancaster, PA 17601 Analysis #0813FC .. Revision 01 Supersedes Date: None Effective Date: . Page 11 of 11 APRQ-3 2801 COMPANY CONFIDENTIAL ' v. & . & &