Document EqEDBvqBpGmj9G5kKL8wNyZ6g

1anraster Laboratories 2 4 2 5 N e w Holland Pike * Lancaster, PA 1 7 601 AR226-2726 Analysis #0813FC - Revision 01 Supersedes Date: None Effective Date: 0 3 2001 Page 1 of 11 Extraction of Low Level FC-143 in Water and Wastewater Reference: Low Level Determination of FC-143 in Water, CH2M Hill, Inc., Oc Cross Reference: The following procedure is cross-referenced in this docun enL SOP-OE-001, "Glassware Cleaning for O r g a n i Scope: This method is designed to extract bC -U o lamrffbnium perfluorooctanoate) from water. Basic Principles: FC-143 is extracted from th * ssnpie at a pH <1.5 into MTBE. The MTBE is concentrated on a s te a - bad The sample is then concentrated and exchanged to ethanol. Sulfuric acid ,s added to the vial and then heated at 65C for 1 hour to derivatize th e to n p o u rd s Following this step, the sample is washed multiple times with d e io n j.^ ^ a tfL |B d placed into an autosampler vial for analysis, .. - -- "`i s gngj gg!7 Holding T im e j||lb ra g e Conditions: |p s a i' aid be extracted within 14 days of collection. All samples should be stored afyBgjpjffC prior to extraction. ' COMPANY CONFIDENTIAL A l ancaster Laboratories 2 4 2 5 New H olland Pike Lancaster, PA 1 7 6 0 1 Analysis #0813FC Revision 01 Supersedes Date: None Effective Date: a; Page 2 of 11 ' ' Apparatus: 1. 2-L separatory funnel for extracting organic components frorrua^acf matrix ' 2. Kilderna-Danish (K-D) assembly with appropriate aip^ J ^ gr ei l a ctinq the solvent used during the extraction ~!"Saisr 3. Glass pipettes 4. ' N-evap with nitrogen supply ^ 5. Water bath or S-evap 6. Glass vials, various sizesy 7. Centrifuge 8. Graduated cyl^pFcs^^fips A, assorted sizes 9. Volumetrir ^lasl c " Class A, assorted sizes 10. Gla'is Pipettes --Class A, assorted sizes 14. Pipettes - Disposable 15. pH paper-Assorted ranges COMPANY CONFIDENTIAL 2 4 2 5 N e w Holland Pike Lancaster, PA 176 0 1 Analysis #0813FC - Revision 01 _ Supersedes Date: None Effective Date: 'PR g 3 2gg, Page 3 of 11 16. Solvent pumps ' 17. Automatic shaker --Capable of holding 2 L separator funnels 18. Beakers - Assorted sizes i 19. Reacti therm vials 20. Screw cap GC vials 21. Glass wool 22. Amber crimp top GC vials 23. Balance - Capable of we] GO! g Reagents: _#k"'Wr 1. Methylene chIpride =Tj% s ib k ie grade or equivalent 2. MTBE - Pestic degrade or equivalent 3. A cetone-Pesticide grade or equivalent 4' Hexarib - Besticide grade or equivalent f - ' 5. 'Sodium sulfate - Reagent grade or equivalent. Bake at 400C for 4 hours in j j f t 1shallow 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 water to acid. Store for up to 1 year.) COMPANY CONFIDENTIAL I anraster Laboratories 2 4 2 5 N e w H olland Pike Lancaster, PA 17601 Analysis #0813FC Revision 01 Supersedes Date: None Effective Date: Sodium hydroxide - ACS grade or equivalent - 10 N - Add 40 g NaOH to ^ approximately 80 ml_ of deionized water in a volumetric flask. S n t i l NaOH goes into solution. Using a wash bottle, dilute to 100 deionized water. Store at room temperature in a glass boif g./R caccnt ,si stable 1 year. If 1 N NaOH is needed a dilution of 10x can be jrpad& of the 10 N solution. 8. Alumina N (neutral) super I activity - Use as i=c-siv=-d.. 9. TeflonTM-boiling chips - Rinse thoroughlyJ^taCQethyflhe chloride prior to use to remove contaminants. . Preparation of Glassware: See SOP-OE-001. Prior to use the lllg g //* ' is prised with either.ethyl ether or hexane to remove contaminants S e ||lfith a list of glassware and the appropriate rinse solvent. Safety Precautions: . Always add acid to ^ te r jfe d u c e fuming. The sulfuric acid and sodium hydroxide solutions get ho' w ie n pj^|Bred. Always wear gloves when handling these solutions. FC-143 ppxtromqly dangerous in the neat form. The time weighted average e x p o s jffrim it is tiffm g/m l Therefore, extreme care must be used when working i/ith f^ fc n m |g i]n d . Also, heating of the neat standard or any concentrated avoided. Any handling of the neat product must be done in a |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 ies 2 4 2 5 N ew H olland Pike * Lancaster, PA 176 0 1 Analysis #0813FC - - Revision 01 Supersedes Date: None Effective Date: - Page 5 of 11 APR 0 3 2001 The toxicity or carcinogenicity of each reagent used in this method has not bej precisely defined; however, each chemical compound should be treated ashealth hazard. From this viewpoint, exposure to these chemicals must the lowest possible level by whatever means available, such as fu m e i safety glasses, and gloves. Always wear gloves when handling any samples or standari safety equipment must be utilized (lab coat, safety glasse Wife laboratory Since the extracts are concentrated bn a steam bath caution molffbe exercised while working around this apparatus. All solvent waste genemned irpm this preparation must be collected for recycling (if applicable) or mi ist ce disposed "of in the designated containers. These will then be transferred t ^ ^ b - w i d e disposal facility. Any solid waste materia! (disposable pipettes, b r o k ^ ^ ^ # v / ^ , pH paper) may be disposed of in the normal solid waste collection CQitilsJlrs, ' Personnel Training and Qualifications: All personnel performing those IWB ilb u bs should have performed a quad study that yielded acceptable recoveries for F ^ f4 3 . Personnel should spend several days working with an expose need preparation technician who has demonstrated their proficiency of the -extraction. , Also, several^^ckls-pPfierbicide water samples should be performed under the direct observaiiOii of an otfterexperienced preparation technician to assure the trainee is c a p a b liS k id ^ p s id e n t preparation. l5^;r.~=3iW COMPANY CONFIDENTIAL I anraster Laboratories 2 4 2 5 N e w Holland Pike Lancaster; RA 17601 Analysis #0813FC ' Revision 01 . Supersedes Date; None Effective Date: Page 6 of 11 -APR0 3 200! Procedure: Set up a 2-L separatory funnel for each sample and QC sampleJo be - - extracted. For field samples which are using 1 full bottle, jcn pis o u i^ fe of the bottle with a scriber at the meniscus of the sample v o lu r ^ ^ ^ d f e the bottle vigorously and then pour the contents into a 2-^aparai<jry funnel. Fill the bottle to the marked level with water and tr a n s ^ p iip s t ^ r io a graduated cylinder to determine the initial v o lu ro |J e m la p iy , weigh the empty bottle and tare the balance. Fill the fe jifta ja rk e d level with water and place the bottle on the tared balatjfc. ThiSipeight rounded to a whole number is the initial sample volurv-i F -r a'l samples using a specified volume, shake each bottle vigorouj.lv, nno then use a clean graduated cylinder to measure the desired^y|-irne -1 .ansfer the sample to a 1-L graduated cylinder. Record th ^ja fflp e ^o ju m e and any comments about the samples in the e x t r a c t i o n t r a n s f e r to the 2-L separatory funnel ' 2. Using pipettes, add;Brrc^e%tandards and spiking solutions to the aqueous sample in the s ^ s ra ip p lJ jrfte l. Be certain the standard drips directly into the agi hamisijiS n ^S w ifM siit touching the glass side of the separatory funnel * -v*- roci rlf Add 1 mL FC-143 surrogate (perfluorononanoic acid) to all ifep^liy b la n k s . and spikes. = iking solutions --Add 1 mL FC-143 spiking solution to the laboratory iontroi 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 2 4 2 5 N e w H olland Pike Lancaster, PA 17501 Analysis #0813FCRevision 01 Supersedes Date: None Effective Date: Page 7 o f 11 4. Using a solvent pump, add 100 ml_ of methylene chloride to the segaratory funnel, cap the funnel, invert it, and vent immediately. Place the o r a ?. the automatic shaker and shake at the designated speed for 2 mnu cs `in the stopcocks closed. , ' "I*"T - "/ NOTE: Shaker speeds vary greatly between instrum #ft|^o ro p e r setting is marked on each. 4 I - , 3rr 5. Allow the phases to separate for at.least 1Q jjlp te s Open the stopcock and ' drain the methylene chloride (bottom laye rifh lopajPwwaa i f container and discard. ' 6. Using a disposable pipette, a d ju ^ f.e pH o ' the samples to <1.5 with 1:1 sulfuric acid. Check the pH us *-g pH paper to ensure it is <1.5. 7. Using a solvent pump, nnse earn sample bottle or graduated cylinder with 100 mL of MTBE separatory funnel. 8. Shake the sepgl^bi^4iBfteL for 2 minutes on the automatic shaker. 9. Allow the phases ie separate for 5-10 minutes before draining the aqueous (lower) layer back into a 2-L beaker. 10. 4 jii5 tk |lM T B E extract through approximately 10 cm of sodium sulfate into a K-0 Apparatus containing a TefIonTM-boiling chip. 11 - petLrn the aqueous sample to its respective separatory funnel. Using a Jtesnh/pnt pump, rinse the sample bottle or graduate with 60 mL of fresh, MTBE le fo re adding the MTBE to the separatory funnel. . . 12. Repeat steps 8 through 11. 13. Repeat steps 8 through TO. COMPANY CONFIDENTIAL Analysis #0813FC ' Revision 01 Supersedes Date: None EffeoUv, Date: - , !? 14. Attach a 3-bali Snyder column to the K-D, wet with MTBE, and concentrate at 80 to 85C to less than 4 mL. 4 15. Using a piptte, add 5 mL of ethanol to the ampule and N - ^ p J |& B N ir fc t at 35 2C to 1 mL. 16. Place 10 drops from a disposable pipette of react! therm vial, then transfer the extract to | lb add into a and swirl. 17. ' Place the sample on a rack into an o\rer^atM%ytoj57'& for 1 hour to . derivatize the compounds of interest t f t i ^ ^ l ^ ^ ^ t i v e ethyl esters. 18. Remove the samples from thejffc h j p d moped lately place the reactor vials in the freezer until cold, a p p r d x iip ^ ^ . ^ ^ inutes. Remove the cap and using pipettes, add 1.0 m L cf m e tft^S "c h lo rid e and 1.0 mL of deionized water. Recap and s h | | jf ig d % i| y f o r several seconds. Allow the phases to separate and u s i n a y e , P i p e t t e remove the methylene chloride (lower) layer. Place the fchldride layer into a screw cap GC via! containing 1.0 mL o" d secor js (loiiij^B y r.ass wog =|yater. Cap the vial and shake vigorously for several phases to separate. Remove the methylene chloride Bn the extract through a disposable pipette containing a plug md sodium sulfate. Bring the extract to exactly 1.0 mL with .4 - meti'^eiWchloride. 9A iftlb e the extract in an amber crimp top GC vial. Cap the GC vial securely lSllk j g n d store in the freezer. Record the final volume in the extraction log. Calculations: See analysis method. COMPANY CONFIDENTIAL Analysis #0813FC ' Revision 01 Supersedes Date: None . Effective Date: Page 9 of 11 APR 0 o Statistical Information: See analysis method. Quality Assurance: ISSSgsS- Each day samples are extracted, a blank, laboratory c o n t r o I j g p p l e " e i o n i z e d water blank spiked with all compounds of interest carried and LCSD if applicable must be prepared. In addition^ |he e ftire procedure), j|j|s and matrix spike duplicate must be extracted. If there is limited sampjej"" i presents the preparation of the MS/MSD, the LCSD must be prepared ins*ead the batch contains only field or equipment blank samples, the LCC/L should be 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 ii fjfy j l ay an additional batch must be prepared. If any client, agency, or QC or batch requirements, these must be followed instead. Revision Log: Initiated Date: 03/22/Qs! . '' Effect-ve Daici si w - Jt4. _4w4/ k 081JFC ' COMPANY CONFIDENTIAL # I ancaster Laboratories2425 N ew Holland Pike Lancaster, PA 17601 Analysis #0813FC ' ' Revision 01 Supersedes Date: None Effective Date: - ^ ^ Page 10 of 11 PH Ud 20i Date: - A f7z Da-e: V - z - * / Approved by: J X 7 Y Y ~) Quality Assuratee ----- -- ^ a*e` -- ^ f ^ l .^J- COMPANY CONFIDENTIAL Analysis #0813FC - Revision 01 Supersedes Date: None Effective Date: . _ Page 11 of 11 APR U`3 Table FC-143 Prep Rinsing List Rinse 2x with acetone and then 2x with MTBE 2-L separatory funnels . K-Ds . Ampules . Sodium sulfate columns . ,;u Snyder columns 2-L beakers TeflonTM stoppers 250 mL beakeis' Reacti-vial^caps/frnS's COMPANY CONFIDENTIAL