Document dYoz52j59o8o8xkLbegy6pmmb

I RwuestorNanm Report Project / Study Archive Request 1 Shaded areas for Amhivist us8 only I I Phone I I R F C I Cabinet: Drawer: Summarv Group: ,E:sA AAJrqLqncnL GkOLP Group Project Number: Project Leadl Study Director: Contract - 3 OHA F L A H H 7 9 Laboratories: Contract Project # Client Organization: Client Contact: Client Project Number: 3 r/l L3/ LL,ArV, 1 &E46id f i u --7c4- g o 5 Analyte(s): Pa4 Test System (Sample Matrix): ,M I Project Type 0 Analysis R7iF-6. 0 Degradation E 0 Duct ResidueAnalysis 0 Ecotox FT%!AtuOL, ANA /&&- 7ohJE0 Method Validation z y s / a e m Propertses 0 ResearchlMethodDevelopment I Initiation Date: Completion Date: Electronic Media: / Archive Date Key Words: Project / Study Archive Request Scan Date OffSite Storage Date Distribution Point Date Study Title Characterization Study of PFOA: a.) Test Control Reference# TCR-99131-18 (lot #HU14401DU,Aldrich), b.) Test Control Reference# TCR-99131-37 (lot #332) PHASE:SOLUBILITYDETERMINATION Data Requirement 40 CFR 160.105(b) Author Mark E. Ellefson Phase Completion Date Date of Signing Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Environmental Laboratory Study # FACT-TCR-005 (LIMS #E00-1762) Centre Analytical Laboratories Study # 023-033 Total Number of Pages 28 3M Environmental Laboratory Report No. FACT-TCR-005 ~~ ~ ~~ ~ GLP COMPLIANCSETATEMENT Study Title: Characterization Study of PFOA: a.) Test Control Reference# TCR-99131-18 (lot #HU14401DU, Aldrich), b.) Test Control Reference# TCR-99131-37 (lot #332), Phase: Solubility Determination. Study Identification Number: FACT-TCR-005 (E00-1762), Centre Analytical Laboratories Study # 023-033 This phase of the study was conducted in compliance with Environmental ProtectionAgency (EPA) Good Laboratory Practice (GLP) Standards 40 CFR 160 with the exceptions in the bulleted list below. 0 Not all of the raw data generated during the course of this study is available or will be archived. Wllliam K. Reagen, Testing Facility Management Date LlMS# E00-1762, Page 2 Of 28 3M Environmental Laboratory Report No. FACT-TCR-005 QUALITYASSURANCSETATEMENT Study Title: C'haracterization Study of PFOA: a.) Test Control Reference# TCR-99131-18 (lot #HU1440'1DU, Aldrich), b.) Test Control Reference# TCR-99131-37 (lot #332), Phase: Solubiility Determination. Study Identification Number: FACT-TCR-005, Centre Analytical Laboratories Study # 023-033 This phase of the study has been inspected by the 3M Environmental Laboratory Quality Assurance Unit (QAU) as indicated in the following table. The findings were reported to the study director and laboratory management. I 07/17/00 I 09/08/00 I 04/09/01 I Inphase I Inphase I Data and Draft Report I 1 07/28/00 07/28/00 I 1 II 04/10/01 04/10/01 QAO Reprebentative Dbte ' LlMS # EOO-1762, Page 3 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 TABLEOF CONTENTS GLP Comp1ianc:e Statement............................................................................................................... 2 Quality Assurance Statement............................................................................................................. 3 Study Information............................................................................................................................... 6 Summary ............................................................................................................................................ 7 Purpose.............................................................................................................................................. 7 Test Substance .................................................................................................................................. 8 Test System ....................................................................................................................................... 8 Method Summaries ............................................................................................................................ 8 Preparatory Method............................................................................................................................ 9 Protocol Deviations ............................................................................................................................ 9 Analytical Results............................................................................................................................... 10 Data Summary ................................................................................................................................... 10 Statistical Methods and Calculations ................................................................................................. 10 Statement of C:onclusion .................................................................................................................... 10 References......................................................................................................................................... 10 List of Attachnlents............................................................................................................................. 11 Signature Page................................................................................................................................... 11 LlMS # E00.1762. Page 4 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 LISTOF TABLES Table 1. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone. .7 Table 2. Characterizationof the Test Substance.............................................................................. 8 Table 3. Descriptionof Test Systems Used in this Study ................................................................. 8 Table 4. Sumniaryof Sample Preparation........................................................................................ 9 Table 5. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone. . 10 LlMS # E00-1762, Page 5 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 STUDYINFORMATION Study Director John Flaherty Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 Analytical Chemistry Laboratories Solubility Tesfhg Certificate of Analysis 3M Environmental Technology and Safety Seivices (ET&SS) 3M EnvironmentalLaboratory Bldg. 2-3E-09 935 Bush Aveinue St. Paul, MN 56106 Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 John Flaherty, Study Director Dr. William K. Reagen, Laboratory Manager Mark E. Ellefson, Principal Analytical lnvesfigafor Kristin L. Terrell, Analytical Chemist Mark L. Anderson, Analytical Chemist Cindy M. Carlson, Analytical Chemist Sponsor 3M Environmental Laboratory 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55106 Dr. William K. Reagen Experimental Dates Sample Analysis Initiation: 08 September 2000 Sample Analysis Completion: 08 September 2000 Archives Reserve sarrrples of the reference standards will be maintained by the 3M Environmental Laboratory. All study data for this phase and a copy of the phase report are archived by the 3M Environmental Laboratory. LlMS # E00-1762,Page 6 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 SUMMARY Solubility of PFOA in water is a significant parameter because the spatial and temporal movement (mobility) of a substance through the environment is largely determined by its solubility in water. Water soluble substances readily gain access to humans and other living organisms; furthermore the knowledge of the solubility in water is a prerequisite for testing biological degradation, bioaccumulation, and other tests. Solubility of PFOA in methanol and acetone is a significant parameter for general laboratory knowledge in the preparation and analysis of PFOA. The approximate solubility of PFOA was determined by performing a solubility screen test (ETS-8170.0). PFOA was determined to be soluble at concentrations greater than 10% (mass/volume) in water, methanol, and acetone at 23'C. According to the screen test, if the substance is determined to be soluble at concentrations greater than 10% (mass/volume) then no additional solubility testing is required. Due to insufficient quantity of test substance, PFOA TCR-99131-018 was not tested. The small amount of remaining material was archived. Results are presented in table 1: Table 1. Summary Table of Solubility of PFOA TCR89131-037 inWater, Methanoland Acetone. __ Acetone 5 10% The solubility of TCR-99131-037 was determined to be greater than 10% (masslvolume) in water, methanol and acetone at 23'C. PURPOSE The purpose of this phase of the study was to determine the solubility of PFOA in water, methanol, and acetone as part of the characterization of this test substance. LlMS # E00-1762, Page 7 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 TESTSUBSTANCE PFOA, Test Control Reference #TCR-99131-037 Table 2. Characterizationof the Test Substance TESTSUBSTANCE PFOA Source 3M Specialty Materials, Bldg. 236-2A-01 I ExDiration Date I 12-152001 I I Storaae Conditions I Frozen I I 3M Laboratow Identification Number I TCR-99131437 I Physical Description white powder Purity 95.2% TESTSYSTEM Table 3. Descriptionof Test SystemsUsed in this Study Ideritification I Nurnber PuritylGrade I Millipore System NA NA I ASTM Type I [ B & J Brand 2005 Ambient, Flammable Cabinet I 2005 Ambient, Flammable Cabinet TN-A 4466 TN-A: 4616 I HPLCGrade I HPLCGrade I METHOD!SUMMARIES The solubility determination of PFOA TCR-99131-037 in water, methanol, and acetone was performed according to ETS-8-170.0, "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents," and is based off United States Environmental ProtectionAgency OPPTS 830.7840,"Water Solubility: Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility." ETS-8-170.0 was subsequently revised to more accurately account for what was done during the screening test, and to remove sensitive information. This revised version, ETS-8-170.1, may be found in Appendix A. LlMS# E00-1762,Page 8 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 The Solubility Screen Test Method was used to determine the solubility range of PFOA TCR-99131-037 in water, methanol, and acetone. Incrementalamounts of water, methanol, or acetone were added to PFOA neat material and a qualitative determination of the solubility was made. The screen test indicated the solubility of PFOA to be greater than 10% (mass/volume) in water, methanol, and acetone at 23.0 "C.A detailed description of the Solubility Screen Test method used in this study is located in Attachment A. PREPARATORMYETHOD 0 ETS-8-1701.0 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." This method is a pre-requisite to the shake flask and column elution methods and provides an estimate of the solubility of the test substance in the solvent of choice. If the test substance is determined to be soluble at concentrations greater than 10% (;mass/volume)then no additional testing is required. A preliminary screen test was performed on 17 July, 01. During this screen test, test solvent was continually added until a gel-like substance formed, and the PFOA never completely solubilized. The data and records for this preliminary test are not available, however the test was repeated on 08 September, 01 and the same results were observed and documented as follows. Approximately 10 mg PFOA was weighed into a glass vial, and 0.1 mL of the appropriate solvent was added. Following solvent addition, the vial was shaken, sonicated, and observed for particulates. The solubility screen test estimated the solubility of PFOA to be greater than 10% (mass/volume) in water, methanol and acetone at 23.0 "C.No additional solubility testing was necessary for any of the three solvents. Table 4. Summary of Sample Preparation. % I O mg test substance is weighed into tared glass screw-capped vial. 0.1 mL of test solvent (water, methanol or acetone) is added to glass screw-camed vial. 3 Followingthe addition of test solvent, the vial is capped, shaken 9/8/00 vigorously (or vortexed). and the mixture is sonicated. Record mixing and sonication times on the worksheet. 4 Following sonication, the sample is checked visually for undissolved particles of the test substance. If all of the test substance is dissolved, the solubilii is determined to be greater than 10%(rnasslvolurne) and no additional solubility testing is required. If a portion of the test substance remains undissolved, additional dilutions are performed using the appropriate solvent. PROTOCODLEVIATIONS There were no deviations from the original protocol for this phase. LlMS # E00-1762, Page 9 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 ANALYTICARL ESULTS 0 Specificity (accordingto OPPTS 830.7840): The solubility determination as stated in the EPA Guidelines follows. This method should only be applied to: 0 Pure substance. This study shows a purity of 95.2% Substances that are stable in water. Refer to "Hydrolytic Reactions of Perflurooctanesulfonate(PFOA)," 3M Laboratory Report Number E00-1851 for hydrolytic stability information. DATASUMMARY Table 5. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone. Water Methanol Acetone > 10% >lo% > 10% I Attachment 8;contains solubility screening test sample preparation worksheets. STATISTICAL METHODASND CALCULATIONS No statistical rnethods or calculations were required. The data was reported as the solubility of PFOA being greater than 10% at 23'C (masslvolume) in water, methanol, and acetone as determined by the initial screening method. STATEMENOTF CONCLUSION Under the conditions of the present study, the solubility of PFOA TCR# 99131-037 in ASTM Type Iwater, methanol and acetone is greater than 10% (mass/volume) at 23C. REFERENCES 1. Fate, Transport and Transformation Test Guidelines Office of Prevention, Pesticides and Toxic Substances (OPPTS) 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. EiPA 712-C-96-041, August 1996. 2. OECD 1015:Water Solubility. Adopted 27July, 1995. LlMS # EOO-1762, Page 10 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 LISTOF ATTACHMENTS 0 Attachment A: Solubility Screening Method ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents". 0 Attachment B: Solubility Screening Test Sample PreparationWorksheets SIGNATURPEAGE We certify that this report is a true and complete representation of the data for this phase of the study: Principal Analytical lnvestigatoi ' Date William K. Reagen Laboratory Manager Date LlMS # E00-1762, Page 11 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 ATTACHMENAT: SOLUBILITSYCREENINMGETHODETS-8-170.1 "SOLUBILITSYCREENTEST:APPROXIMATSEOLUBILITDYETERMINATION OF A TESTSUBSTANCE IN VARIOUS SOLVENTS". (ETS-8-170.0, the method used in this study, is not included as an attachment. ETS-8-170.1, which is procedurally the same, will be included for confidentiality reasons.) LlMS # EOO-1762, Page 12 of 28 3M ENVIRONMENTLAALBORATORY 3M EnvironmentalLaboratory Report No. FACT-TCR-005 SOLUBILITSYCREENTEST:APPROXIMATSEOLUBILITDYETERMINATIONA'OF TESTSUBSTANCIEN VARIOUSOLVENTS Method Number: ETS-8-170.1 Adoption Date: 09/08/00 Effective Date: 03/14/01 Approved By: William K. Rea&, Laboratory Manager Date - 1.0 SCOPE AND APPLICATION 1.1 Purpose. According to methods set forth by the United States Environmental Protection Agency (USEPA) and the Organization for the Economic Cooperation and Development (OECD) a preliminary study, which will be outlined in this method, serves as a prerequisite to perfomling solubility testing via the Column Elution Method and Shake Flask Methods. The EPA and OECD solubility testing guidelines state that if the preliminary solubility determina.tiontest indicates a solubility of > 10" g/L (10 ppm), the Shake Flask Method (ETS-8-1'72.0) is to be used. If preliminary testing indicates a solubility of 10-2g/L,(10 ppm) the Column Elution Method (ETS-8-171.0) will be used to determine the solubility in the solvent of interest. Additionally, due to the tendency of certain compounds to be highly sohble in particular solvents, no hrther solubility determinationwill be necessary for compounds having solubility greater than 10% (madvolume). 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. ETS-8-170.1 Page 1 of 9 Sohbility Determination: Screen Test Method LlMS # E00-1762, Page 13 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 1.3 Acceptablle Matrices. Aqueous (e.g. Milli-Q water, 0.01M CaCl,), Acetone, Methanol, or other solvent(s) of interest. 2.0 SUMMARY OF METHOD 2.1 Preliminary Solubility Determination in solvent. Weigh approximately 10 mg of test substance into a 2.5 mL-4 mL glass screw-capped vial. Add test solvent in varying increments,to the vial. After each solvent addition, vortex mix for approximately 15 sec., and sonicate 2-5 minutes. Make observations of the solution and visually confirm whether or not particles are present; it may be necessary to allow the solution to sit for up to 5 minutes. Add test solvent in a stepwise fashion up to 2 mL. If the substance fully dissolves after the first solvent addition of 100 pL,the test substance shall be considered highly soluble, and no further testing is required. If there are still undissolved particles in the vial, wleigh 10mg of test substance into a 100mL glass stoppered volumetric flask or graduated cylinder. Add test solvent until visual confirmation of the substance dissolution has been achieved. Record all observations on a standardized preparation sheet or logbook. Once 100mL solvent has been reached, the approximate concentration is at 100 pg/mL. If the solubility limit has not yet been achieved, weigh approximately 10 mg of test substance and transfer to a 1 L graduated cylinderholumetric flask (concentration is approximaiely 10ppm). The container should be sonicated and allowed to sit overnight to allow for maximal dissolution. If the undissolved particles are still observed after sitting > 12 hours, the column elution method will be utilized (ETS-8-171.0). If the test substance dissolves in 1L or less of solvent, the shake flask method (ETS-8-172.0) will be used to determine the solubility. 3.0 DEFINITIONS 3.1 Test substance. A liquid or solid material for which the relative solubility in a specified solvent will be determined. 3.2 Test solvent. The matrix to which the test substance of interest is introduced. The test solvent may include but is not limited to aqueous matrices, including ASTM Type I Water and various salt matrices (e.g. 0.01M CaCl, and organic solvent matrices, including methanol,,and acetone. 4.0 WARNINGASND CAUTIONS 4.1 Health and Safety Warnings: 4.1.1 Wiear the proper lab attire for all parts of these procedures. Wear gloves and eye protection at all times. 4.1.2 Handle all solvents in a hood for all parts of the described sample preparation procedure. 4.1.3 Folr potential hazards of each chemical used, refer to material safety data sheets, packing materials, and 3M Environmental Laboratory's Chemical Hazard Review. 4.1.4 No mouth pipetting is allowed. ETS-8-170.1 Page 2 of 9 Solubility Deteimiiintion: Screen Test Method LlMS # E00-1762. Page 14 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 4.2 Cautions: 4.2.1 Glassware in which standards are prepared should be triple rinsed with acetone and methanol to reduce the possibility of accidental contamination. 5.0 INTERFERENCES 5.1 Impurities may significantly affect the solubility of the test substance. The purity of the test substance should be known and documented prior to starting the screening procedure. 6.0 EQUIPMENT 6.1 Analytical balance sensitive to 0.1 mg. 6.2 Vortex mixer. 6.3 Sonicating device. 7.0 SUPPLIEASND MATERIALS 7.1 Disposable glass graduated pipettes, 1mL to 100 mL. 7.2 Disposable glass Pasteur pipettes and rubber bulbs. 7.3 Glass beakers, various sizes. 7.4 2.5 niL-4 mL glass screw-top vial. 7.5 Glass volumetric flasks, 10 mL to 1000 mL. 7.6 10 pL-10010 pL Pipettemanm manual pipettor and plastic pipette tips, or equivalent. 8.0 REAGENTS AND STANDARDS 8.1 Methanol (MeOH), HPLC/SPEC/GC grade from EM Science, or equivalent. 8.2 Acetone, lHPLC/SPEC/GC grade from EM Science or equivalent. , 8.3 Water, ASTM Type I, or equivalent. 8.4 Calcium Chloride Dihydrate, Approximately 99%or better, from Sigma or equivalent. 8.5 0.01 M CiaCl,, A 0.01 M CaC1, stock solution is prepared by weighing 1.5 g CaCl, Dihydrate in a weigh boat and transferring to a 1L volumetric flask and diluting to the mark with Milli-Q"" water. 8.6 Test substance of known purity. 9.0 SAMPLHE ANDLING 9.1 Record times of initial preparation and dilution on a sample preparation sheet or logbook. 9.2 Once the preliminary testing has been completed and the appropriate information is extracted, the screen test samples should be disposed into the proper waste stream. ETS-8-170.1 Page 3 of9 Soltrbility Determination: Screen Test Method LlMS # E00-1762, Page 15 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 10.0 QUALITYCONTROL 10.1 Not applicable. 11.0 CALIBRATIOANND STANDARDIZATION 11.1 The compounds of interest must be of known characterization according to laboratory specifications. 11.2 All equipment used, such as the analytical balance, should be calibrated daily prior to use. 12.0 PROCEDUKES 12.1 Solubility screen. 12.1.1 Weigh 10 mg k 1 mg of test substance into a 4 mL glass screw-top vial or equivalent. Record the weight (refer to attachment A for an example of a standardized prep sheet). 12.1.2 Add solvent (e.g. water, methanol, acetone) according to the table below to the test substance. 4 mL vial or equivalent Total volume solvent added (mL). .. Approximate Solubility (CLg/mL). * * Solvent addition 1 0.1 100000 Solvent addition 2 0.5 20000 Solvent Solvent addition 3 addition 4 1 2 10000 5000 12.1.3 Following addition of solvent, vortex mix approximately 15 seconds, sonicate 2-5 minutes. Visually check for undissolved particles. If undissolved test substance remains, continue adding solvent according to the above chart. It may be necessary to idlow the solution to settle for up to 5 minutes before making observations. Record observations on the standardized prep sheet. 12.1.4 If all particles dissolve, then estimate the approximate solubility and document the concentration. Because the concentration is >10 pg/mL, the shake flask method (E'TS-8-172.0) will be used to determine the accurate solubility point. However, if the test substance dissolves after thefirst solvent addition of 100 pL the solubility is determined to be >lo% (mass/volume). The test substance shall be regarded as "highly soluble,'' and no further testing is required. 12.1.5 If the test substance did not dissolve in the 2 mL of solvent, weigh 10 mg & 1 mg of test substance into a 100 mL glass volumetric flask or equivalent. Record the weight (refer to attachment A for an example of a standardized prep sheet). 12.1.6 Add solvent according to the table below to the test substance to deliver the appropriate amount of solvent. As described in 12.1.3, vortex mix, sonicate, and alllow the test solution to settle. Record all observations and procedures on the preparation sheet. ETS-8- 170.1 Solubility Determination: Screen Test Method Page 4 of 9 LlMS # E00-1762, Page 16 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 100 mL volumetric Solvent addition 1 Solvent addition 2 Solvent addition 3 $!ask or equivalent Total volume solvent 10 50 100 added (mL). .. Approximate Solubility 1000 200 100 (Pg/mL)* - * 12.1.7 If'the solubilitypoint is reached at or prior to the complete addition of 100 mL, the concentration estimation at which the substance is soluble should be documented and shall be used as a starting point for the shake flask method (ETS-8-172.0). 12.1.8 If the 100 mL solvent level has been reached without complete dissolution of test substance, weigh out 10mg k 1mg test substance and transfer to a 1L volumetric flask,graduated cylinder, or equivalent. Dilute to 1L with test solvent. The approximate concentration of test substance is at 10 pg/mL. The flask should be allowed to sit 12-24 hours to allow for maximal dissolution. If the undissolved particles are still observed, the column elution method will be utilized (ETS-8- 171.O). If no visible particulates are observed, the shake flaskmethod (ETS-8- 172.0) shall be used to determine the solubility. 13.0 DATAANALYSIASND CALCULATIONS 13.1 The solubility determination in this method is qualitative/semi-quantitative. 13.2 The point to which the substance dissolves in solvent is confirmed visually. The solubility point is therefore a qualitative determination. 13.3 The concentration estimation is semi-quantitative in that the approximate concentration is calculated by the following equation: c=db Where: c= the semi-quantitative concentration pg/mL, a= amount of substance weighed out (pg), and b= the approximate amount of solvent added (mL). 14.0 METHODPERFORMANCE 14.1 Limitation of data. The accuracy to which the solubility is determined is subject to a large margin of error due to the way in which the solvent is added to the solute. Since large andl varying increments of solvent are being added to the solute, this error margin must be considered when reporting the concentration estimation. 14.2 The data obtained through this study is an estimation only and should be treated as a qualitative estimation of the solubility of test substance in a given solvent. ETS-8-170.1 Page 5 o f 9 Solubility Determination: Screen Test Method LlMS # E00-1762, Page 17 of 28 3M EnvironmentalLaboratory Report No. FACT-TCR-005 14.3 For an accurate measurement of the substance solubility concentration, the shake flask method, or column elution method will be used. 15.0 POLLUTION PREVENTION AND WASTE MANAGEMENT 15.1 Dispose o f sample waste by placing in high or low BTU containers as appropriate. Use broken glass containers to dispose of glass pipettes. 16.0 RECORDS 16.1 Sign and date all observations and calculations. 17.0 ATTACHMENTS 17.1 Attachment`A-Example of a Standardized SamplePreparation Sheet: Solubility Screen Prep Sheet. 18.0 REFERENCES 18.1 Organization for Economic Cooperation and Development. OECD Guideline for Testing of Chemical:;. Water Solubility -0ECD Guideline 105: pp. 1-7, Adopted 1995 18.2 United States Environmental Protection Agency. OPPTS 830.7860 Water Solubility (Generator Column Method). Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-96-042: pp. 1-17,1996 18.3 United States Environmental Protection Agency. OPPTS 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-96-041: pp. 1-12,1996 18.4 3M Envirionmental Laboratory Method ETS-8-17 1.O, "Column Elution Method: Solubility Determination of Test Substance in Various Solvents." 18.5 3M Environmental Laboratory Method ETS-8-172.0, "Shake Flask Method: Solubility Determini3tion of Test Substance in Various Solvents." 19.0 AFFECTED DOCUMENTS 19.1 ETS-8-17 1.O, "Column Elution Method: Solubility Determination of Test Substance in Various Slolvents." 19.2 ETS-8-17'2.0, "Shake Flask Method: Solubility Determination of Test Substance in Various Solvents." ETS-8-170.1 Page 6 of9 Solubility Deteimination: Screen Test Method LlMS # E00-1762, Page 18 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 20.0 REVISIONS Revision Number Reason For Revision 1 It was desirable to make the method more universally applicable by removing references to specific test substances. Revision - Date 03113/01 ETS-8-170.1 Page 7 of 9 Solubility Detelmination: Screen Tesr Method LlMS # E00-1762, Page 19 of 28 I Attachment A: Example Preparation Worksheet,page 1 of 2 I GLP Study Number: Test Substance: w IN.- Samplepreparation worksheet Date: Source: Solvent: ID#: Step Source: 1 Weigh approximately 70 mg f 7 mg of test substance into a 2.5mL4 mL glass screw-top vial. Weight of test substance: m n Balance ID: Datellnitials: 2nd repllcateoplional: mg Thermometer ID: 2 Add test solvent according to the table below. Followingeach addition of solvent, shake vigorousiyhortex,and sonicate - Total volume solvent added (mL) Flask sonicated? Yes/No Flask allowed to settle? Ye NO- The solutlon Is at lo%, and Is consldered "infinitelysoluble." I Analyst Daterrim- Is there solute still present? YedNo 2v) ?t ? Did the substance dissolve in 2 mL or less o f solvent? A 2 Yes -Approximate concentrationat which the test substance is soluble In solvent: ~ l m l N The solubility of the test substance is to be determined via the shake flask method. or No Continue to page two for further testing. N 0 Notes/ additional comments: 0, N 0) ETS-8-170.1 Solubility Determination: Screen Test Method Page 8 of 9 Attachment A Cont.: Example Preparation Worksheet,page 2 o f 2 L GLP Study Number: Test Substance: Solvent: 3M Environmental Laboratory SOLUBILITY SCREEN Sample preparation worksheet p#: Date: StXWC.. IW. Source: - A ~ l p l A~lp.1 - A~lpt - volume added (mL)/ appmx cone. after Solubilltv data addlUon(ug/W Dalellime I Step44 ... Total volumesdve~Vadded(mL)... 10 Appmximale Solubilily (ug/mL) 1,000 Dalflime I Step4 4 ... TdaJ volumesdvent added (mL) 50 ... Approximate Solubllily (ug/mL) 200 DatelTime I Step44 ... Tolal volume sdvent added (mL) 100 ApproximaleSdubllily (ug/mL)... 100 Sample Prep Flaskvortexdxed? YeslNo Rwm Temp Flasksonicaled?YeslNo Time Flaskallowedlo settle? YedNo Tlme flaskvorlexmixed? Y W o Room Temp Flasksonlcated?YeslNo Time Flaskallowedto setUe? YeslNo Time Flaskvortexmlxed? YesiNo Room Temp Flask sonicated? YedNo Time flask allowedlo selUe? Ye040 Time OBSERVATIONSINOTES G' Isthere sdute sull presenl?YeslNo min 'C Is there solute still pcesant? Y e a 0 nun min "G Is there solute stlll present? YedNo nun mi0 ~nalysl Dale/Tme I Step 5-1 f - ... Total volumesdvenl added (mL) loo0 ... Approxlmale Sdubilily (uglmL) 10 rn 0 ? 3 In (0 N 0, N Q) Flaskvortexmlxed?YeslNo RoMnTemp Flasksonicated?YedNo Time Flaskallowedlo SeIUe? Y W o Time 'C Isthere solute ~1111present? YeslNo rmn rn ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 of 9 3M Environmental Laboratory Report No. FACT-TCR-005 ATTACHMENBT: SOLUBILITSYCREENINTGESTSAMPLPEREPARATION WORKSHEETS LlMS # E00-1762, Page 22 of 28 3M Environmental Laboratorv SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparatlon worksheet Test Substance: PFOA ID#: TCR-99131-037 Date:< @ . f O O c*vtc Source: 3M Internal Step 1 Weigh approXimately 10 mg f Weight of test substance: 2nd replicate optional: - 0.5iom.g 1o1f test substance rng mg into a 2.5 mL-4 mL glass screw-to Balance ID: L I q J Thermometer ID:&@ vial. Thf-W d D a t e / l n i t i a l s : & ~ ~ cd.n( Analyst 0% btmm Totalv volume added (mLy approx conc. after Flask vortex-rn Flask sonicated Analyst Datemme at volume solvent added Flask sonicated?Yes/No Time Flask allowed to settle? YeSMo Tlme re solute still present? Yes-continue to step 2-2 Is there solute still present? Y&No Conclusions: Did the substance dissolve In 2 mL or lessof solvent? c(17 olsc-/o-o~ Yes -Approxim.a.teconcentration at which the test substance is soluble in siolven$ /%ua/ml f l @ or No Continue to page two for further testing. Notes/ additional comments: Solubility Screen Test Page 1 of 2 - & Exact copy et QrO$lnaU !Faast!d %kOdl Date 3M ETS Laboratory 3M EnvironmentalLaboratow SOLUBILITY SCREEN GLP Study Number: TCR-OOJ Samplepreparation worksheet Test Substance: PFOA IDR TCR-99131-037 Date: Source: 3M Internal Solvent: Acetone Step (continued from paae 1) IW. Source: 2ndrep/icefe@one/: mg Thermometer ID: the mixture and visually check for undissolvedpart/cles. Ivolume added (mLV aoDrox cone. after /I Analyst - Daterrime I Step 4-1 Total volume solvent added (mL) ... 10 Approximate Solubility (uglmL)... 1.000 Flaskvortex-mixed7 YesMo Room Temp Flask sonicated?Yes/No Time Flaskallowed to settle7 YedNo Time / 'C I mij / mi j 15there solutestilt present? Y~SMO Analyst - ... Datflime I Step 4-2 Total volume solvent added (mL) 50 ApproximateSolubility (uglmL)... 200 Flask vortex-mixed7 YeslNo Room Temp , Flask sonicated7YeSMo Time Flask allowed to seffle? YesMo Time / I "C 1s there mlr\ miq still presenn y e a 0 I- ... Totalvolume solventadded (mL) 100 ApproximateSolubility (uglmL)... 100 Flask wnlcated?YeslNo Time I mlQ Flaskallowed to settle7 YeslNo Tim mlQ 5 Weigh approximately 10 mg f 0.5 mg of test substance into a I L d cylinder.olumetric flask/or equivalent. aalyst - Weight of test substance: n19 Datflime I Total volume solvent added (mL)... lo00 Approximate Solubility (uglml)... 10 Concluslons: Did the substance dissolve in 1000 mL or less of solvent? Date/lnltials:p Notes1additional comments: Solubility Screen Test Page 2 of 2 leaMia!_, Date 3M ETS Laboratory 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparation worksheet Test Substance: PFOA ID#: TCR-99131-037 Source: 3M Internal D a t e P 2 , j 00 f r l*y, Solvent: Methanol 1~#:-j-afi-+/6(4 Source: 15 I J ~.&-cxnc\ s t p rn 1 Weigh approximately 10 mg f 0.5 mg of test substance into a 2.5 mL-4 mL glass screwtop vial. Weight of test substance: !0.I d mg Balance ID: 49'1'I L Analyst CkWr volume added (mL)/ approx cone. after Solubility data addition (WmL) D a t e / T i m e 3 5 t ~ + ~2l /8~ - Step 2-1 Total volume solvent added (mL)... 0.1 Approximate Solubility (uglml)... 100,000 Sample Prep 0 6 s ERVATlONSlNOTES a-3 (p Flaskvortexmked-0 Room Tern Flask Flask allowed to settle7 @No Time OC IS there Solute Still preSent7 Yer-continue to step 2-2 solution Is at I O % , and is considered"infinitely soluble." No rther solubility testing is required. I Step 2 4 solvent added (mL)... 2 e Solubility (uglmL)... 5,000 Flask vortex-mixed7 Yes/No Room Temp Flask sonicated? YedNo Time Flask allowed to settle7 Y e 4 0 Time \ * ~ ~~ ~~ Conclusions: Did the substance dlssol n 2 m l or less of solvent? & - A p p r o x i m a t e concentrationat which the test substance is soluble in soIvent:\2/fl7~ualml f l @ 04-10-01 or No Continueto page two for further testing. Subs*- )wn'nq 8 mIddih Notes/ additional comments: Solubili Screen Test Page I Of2 Exact copy of QrigiRan IfV 3M ETS Laboratory 3M EnvironmentalLaboratow SOLUBlLlNSCREEN GLP Study Number: TCR-005 Sample preparatlpn worksheet Test Substance: PFOA ID# TCR-99131437 Source: 3M Internal Date: Solvent: Methanol ID#: source: .^^.^.. . .. ---- Step (continued from page 1) m nA. *Ur *L,l l ~L=SL suLu-s*miiLe u-Ii s a u*i .v.-e I- a 111 .L r.anLr resiiu'o if YES, the test is compieie, ana inere is no need to continue with the screen test. If NO, continue to step 3 to determine the approximate solubility of the substance. 3 Weigh approximately I O mgf 0.5 mg of test substanceinto a 100 mL graduatedstopperedcylinderholumetricflask. Weight of test substance: mq Balance ID: 2ndreplicateoptronal: mg Thermometer ID: 4 Add test solventaccordingto the table below. Followingeach addition of solvent, shake vigorouslyhortex, endsonic the mixtureand visually check for undissolvedparticles. Analyst DateJrim volume added(mLy approx conc. after Solubilitv data addieon ( U g h 4 Sample Prep Flask vortex-mixed? YeSMo Room Tern Flask sonicated? YedNo Tim Flask allowed to settle? YeSMo , ere solute still present? YesMo Flask sonicated? YeSMo Flask allowed to settle? Total volume solvent add settle? YedNo Flask allowed to settle? Y&No e concentrationat which the test substanceis soluble in solvent: ua/ml The solubility of the test substance is to be determinedvia the shake flask method. or No -The solubility of the test substance is to be determined via the column elution method. nal comments: Solubility Screen Test Page 2 of 2 3M Environmental Laboratory SOLUBILIN SCREEN c GLP Study Number: TCR-005 Test Substance: PFOA Sample preparation worksheet IMI: TCR-99131-037 Source: 3M Internal Solvent: Water Step N / S IMI: Source: M;II; - Q -18. a M a 1 Weigh approximately 70 mg f 0.5 mg of test substance into a 2.5 mL-4 mL glass screwtop vial. a Weight of test substance: t'c) I 6 rng Balance ID: 3 4 17 Datellnitials: - ,-mnL/ 2nd replicateoptional: mg Thermometer ID: T h p 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorouslyhortex, and sonicate the mixture and visually check for undissolved particles. Conclusions: Did the substance or NO Continueto page two for further testing. Notes1additional comments: N -4 s. N P) Solubili Screen Test Page 1 of 2 ,LJ OL(-(lLko~ wmLL..- Date 3M ETS Laboratory TA 6\ sa `i a. %+anCes ualrnl @ w 04-10-0 aoq0 ~w/\r)~ b ~ ~ t ~ i - f y 3M EnvironmentalLaboratow SOLUBILITY SCREEN GLP Study Number: TCR-005 Samplepreparation worksheet Test Substance: PFOA IMI: TCR-99131437 Source: 3M Internal Date: Solvent: Water IW Source: olumetric flask, Datdlnitials: ex, end sonicate - Analyst DaWTime Totalvolume solvent added (mL)... 50 - Analyst ~ Datalime I step 4-3 Total volume solvent added (mL)... 100 Approximate Solubility (uglmL)... 100 settle? Y e a 0 Time solute still present? YeslNo min 1s there solute still present? y m o or No -The Notes/ additional comments: centration at which the test substance is soluble in solvent: the test substance Is to be determined via the shake flask method. f the test substance is to be determined via the column elution method. 'W Solubility Screen Test Page 2 of 2