Document v0Z3vgJQRBjwLnK0VVja35jR

Project / Study Archive Request | Shaded anas for Archivist use only | Requestor Name /W a x k . Phone (% S i \ 7 7 Date Request fo r / 0 / Archival Retrieval Report FC Cabinet: LIMS number: r0 0 _ Drawer: Title/Summary: 5 r t / b y r r Pf=>A __ p H A r / Executive h r r /n > Summary Group: tAiV Q L ^ 'T'/CA Group Project Number: Project Lead/ Study Director: yj> O H*A rt& r y Contract Laboratories: Contract Project # r^ -^ /3 /-3 7 ________________ Client Organization: Client Contact: Client Project Number: Analytejs): 3 /m f t f c r - 72 ? /? - S Test System (Sample Matrix): j A r e * . Project Type Analysis ' Degradation Duct Residue Analysis Ecotox Regulatory Status: Initiation Date: Completion Date: Electronic Media: _|_' Non-GLP J2 GLP Other: *1[ /c & Q / n / ____________ /' . jv k Method Validation NA Phys/Chem Properties Research/Method Development Archive Date Key Words: Comments: Project / Study Archive Request Scan Date Off-Site Storage Date Distribution Point Date ** Study Title C haracterization Study of PFO A: a.) Test Control R eference# T C R -9 9 1 31 -1 8 (lot # H U 1 4 4 0 1 D U , Aldrich), b.) Test Control Reference# T C R -9 9 1 31-37 (lot #332) Phase: Solubility Determination Data Requirement 40 CFR 160.105(b) Author M ark 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 # FA C T-TC R -005 (LIM S #E 00-1762) Centre Analytical Laboratories Study # 023-033 Total Number of Pages 28 3M Environmental Laboratory Report No. FACT-TCR-005 GLP Compliance Statement Study Title: Characterization Study of PFOA: a.) Test Control R eference# T C R -9 9 1 3 1 -1 8 (lot #H U 1 4 4 0 1 D U , Aldrich), b.) Test Control R eference# T C R -9 9 1 31-37 (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 Protection Agency (EPA) Good Laboratory Practice (GLP) Standards 40 CFR 160 with the exceptions in the bulleted list below. Not all of the raw data generated during the course of this study is available or will be archived. William K. Reagen, Testing Facility Management Date LIMS # E00-1762, Page 2 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 Quality A ssurance Statement Study Title: Characterization Study of PFOA: a.) Test Control R eference# T C R -9 9 1 3 1 -1 8 (lot #H U 14401 DU, Aldrich), b.) Test Control R eference# T C R -9 9 1 3 1 -3 7 (lot # 3 3 2 ), Phase: Solubility 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. Inspection Dates 07/17/00 09/08/00 04/09/01 Phase In Phase In Phase Data and Draft Report Date Reported to M anagem ent Study Director 07/28/00 07/28/00 09/20/00 ' 09/20/00 04/10/01 04/10/01 LIMS # E00-1762, Page 3 of 28 Table of Contents GLP Compliance Statement............... Quality Assurance Statement............ Study Information................................ Summary..................... ......................... Purpose................................................. Test Substance.................................... Test System ......................................... Method Summaries............................. Preparatory Method............................. Protocol Deviations............................. Analytical Results............................... Data Sum m ary.................................... Statistical Methods and Calculations Statement of Conclusion................... R e fe r e n c e s .......................................... List of Attachments............................. Signature Page.................................... 3M Environmental Laboratory Report No. FACT-TCR-005 2 3 6 7 7 8 8 8 9 9 10 10 10 .10 .10 .11 .11 LIMS # E00-1762, Page 4 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 List of Taejles Table 1. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone.. 7 Table 2. Characterization of the Test Substance.................................................................................... 8 Table 3. Description of Test Systems Used in this Study...................................................................... 8 Table 4. Summary of Sample Preparation.................................................................................................9 Table 5. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone.. 10 LIMS # E00-1762, Page 5 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 Study Information Study Director John Flaherty Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 Analytical Chemistry Laboratories Solubility Testing Certificate o f Analysis 3M Environmental Technology and Safety Services (ET&SS) 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 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 Investigator 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 samples 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. LIMS # E00-1762, Page 6 of 28 3M Environmental Laboratory 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 TCR-99131-037 in Water, Methanol and Acetone. S olvent W ater M ethanol A ceto n e P F O A S o l u b il it y (m a s s /v o l u m e ) > 10% > 10% > 10% The solubility of TCR-99131-037 was determined to be greater than 10% (mass/volume) in water, methanol and acetone at 23"C. P urpose 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. UMS # E00-1762, Page 7 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 Test Substance PFOA, Test Control Reference #TCR-99131-037 Table 2. Characterization of the Test Substance T est Substance Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity PFOA 3M Specialty Materials, Bldg. 236-2A-01 12-15-2001 Frozen . TCR-99131-037 White powder 95.2% Test System Table 3. Description of Test Systems Used in this Study Source W ater I'" 1.. Millipore System Expiration Date NA Storage Conditions Ambient 3M Laboratory Identification Number Purity/Grade NA ASTM Type I M ethanol -- B & J Brand A cetone I EM Science '" 2005 2005 Ambient, Flammable Ambient, Flammable Cabinet Cabinet TN-A: 4466 TN-A: 4616 HPLC Grade HPLC Grade 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 Protection Agency 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. LIMS # 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. Incremental amounts 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. Preparatory Method ETS-8-170.0 "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. S tep S a m p l e P r e p a r a t io n 1 1 0 mg test substance is weighed into tared glass screw-capped vial. 2 0.1 mL of test solvent (water, methanol or acetone) is added to glass screw-capped vial. 3 Following the addition of test solvent, the vial is capped, shaken 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 solubility is determined to be greater than 10% (mass/volume) and no additional solubility testing is required. If a portion of the test substance remains undissolved, additional dilutions are performed using the appropriate solvent. D a t e (s ) P erform ed 9/8/00 9/8/00 9/8/00 9/8/00 Protocol Deviations There were no deviations from the original protocol for this phase. LIMS # E00-1762, Page 9 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 A nalytical Results Specificity (according to OPPTS 830.7840): The solubility determination as stated in the EPA Guidelines follows. This method should only be applied to: 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. Data S ummary Table 5. Summary Table of Solubility of PFOA TCR-99131-037 in Water, Methanol and Acetone. S olvent Water PFOA S o l u b il it y ( m a s s / v o l u m e ) > 10% Methanol Acetone >10% > 10% The solubility of PFOA TCR-99131-037 in water, methanol and acetone is greater than 10% (mass/volume) at 23"C. Attachment B contains solubility screening test sample preparation worksheets. Statistical Methods and Calculations No statistical methods or calculations were required. The data was reported as the solubility of PFOA being greater than 10% at 23"C (mass/volume) in water, methanol, and acetone as determined by the initial screening method. Statement of Conclusion Under the conditions of the present study, the solubility of PFOA TCR# 99131-037 in ASTM Type I water, methanol and acetone is greater than 10% (mass/volume) at 23"C. 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. EPA 712-C-96-041, August 1996. 2. OECD 105: Water Solubility. Adopted 27July, 1995. LIMS # E00-1762, Page 10 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 List of Attachments Attachment A: Solubility Screening Method ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents". Attachment B: Solubility Screening Test Sample Preparation Worksheets Signature Page W e certify that this report is a true and complete representation of the data for this phase of the study: Principal Analytical Investigator William K. Reagen Laboratory Manager Date LIMS # E00-1762, Page 11 of 28 3M Environmental Laboratory Report No. FA CT-TCR -005 Attachment A: Solubility Screening Method ETS-8-170.1 "Solubility Screen Test: A pproximate Solubility Determination o f a T est S ubstance in V arious 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.) LIMS # E00-1762, Page 12 of 28 3M Environmental Laboratory 3M Environmental Laboratory Report No. FACT-TCR-005 Solubility Screen T e s t : A pproxim ate Solubility Determ ination of a Test Substance in Various Solvents Method Number: ETS-8-170.1 Adoption Date: 09/08/00 Effective Date: 03/14/01 Approved By: William K. Reagen, Laboratory Manager A^ Marl Ef llefson, Project Le Q 3 /; /o / Date ' Date 1.0 Scope and Application_____________________ ;_______________________________ 1.1 Purpose. According to methods set forth by the United States Environmental Protection Agency (US EPA) 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 performing solubility testing via the Column Elution Method and Shake Flask Methods. The EPA and OECD solubility testing guidelines state that if the preliminary solubility determination test indicates a solubility of > 10'2g/L (10 ppm), the Shake Flask Method (ETS-8-172.0) 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 soluble in particular solvents, no further solubility determination will be necessary for compounds having solubility greater than 10% (mass/volume). 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. ETS-8-170.1 Page 1 of 9 Solubility Determination: Screen Test Method UNIS # E00-1762, Page 13 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 1.3 Acceptable Matrices. Aqueous (e.g. Milli-Q water, 0.01M CaCl2), 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, weigh 10 mg of test substance into a 100 mL 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 100 mL 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 cylinder/volumetric flask (concentration is approximately 10 ppm). The container should be sonicated and allowed to sit overnight to allow formaximal 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 1 L 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 CaCl2(aq)); and organic solvent matrices, including methanol, and acetone. 4.0 Warnings and Cautions______________________________________________ ;_____ 4.1 Health and Safety Warnings: 4.1.1 Wear 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 For 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 Detennination: Screen Test Method LIMS # E00-1762, Page 14 of 28 3M Environmental Laboratory Report No. F A C T-TC R -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 Supplies and Materials____________________________________________________ 7.1 Disposable glass graduated pipettes, 1 mL to 100 mL. 7.2 Disposable glass Pasteur pipettes and rubber bulbs. 7.3 Glass beakers, various sizes. 7.4 2.5 mL-4 mL glass screw-top vial. 7.5 Glass volumetric flasks, 10 mL to 1000 mL. 7.6 10 |oL-1000 p.L PipettemanTM 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, HPLC/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 CaCl2, A 0.01 M CaCl2stock solution is prepared by weighing 1.5 g CaCl2 Dihydrate in a weigh boat and transferring to a 1 L volumetric flask and diluting to the mark with Milli-QTM water. 8.6 Test substance of known purity. 9.0 Sample Handling__________________________________________________________ 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 of 9 Solubility Determination: Screen Test Method UNIS # E00-1762, Page 15 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 10.0 Quality Control_________________________________________________________ 10.1 Not applicable. 11.0 Calibration and 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 Procedures______________________________________________________________ 12.1 Solubility screen. 12.1.1 Weigh 10 mg 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 (pg/mL)... Solvent addition 1 0.1 100000 Solvent addition 2 0.5 20000 Solvent Solvent addition 3 addition 4 12 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 allow the solution to settle for up to 5 minutes before making observations. Record observations on the standardized prep sheet. 12.1.4 If till particles dissolve, then estimate the approximate solubility and document the concentration. Because the concentration is >10 pg/mL, the shake flask method (ETS-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 >10% (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 allow 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 LIMS # E00-1762, Page 16 of 28 3M Environmental Laboratory Report No. FACT-TCR-005 100 mL volumetric Solvent addition 1 Solvent addition 2 Solvent addition 3 flask or equivalent Total volume solvent 10 50 100 added (mL)... Approximate Solubility (pg/mL)... 1000 200 100 12.1.7 If the solubility point 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 o f test substance, weigh out 10 mg 1 mg test substance and transfer to a 1 L volumetric flask, graduated cylinder, or equivalent. Dilute to 1 L 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-8171.0) . If no visible particulates are observed, the shake flask method (ETS-8172.0) shall be used to determine the solubility. 13.0 Data Analysis and 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 = a/b 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 Method Performance_________________________ ;_________ _________________ 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 and 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 of 9 Solubility Determination: Screen Test Method LIMS it E00-1762, Page 17 of 28 3M Environmental Laboratory 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 of 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 Sample Preparation Sheet: Solubility Screen Prep Sheet. 18.0 References_______________________________________ _ 18.1 Organization for Economic Cooperation and Development. OECD Guideline for Testing of Chemicals. Water Solubility -OECD 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 Environmental Laboratory Method ETS-8-171.0, "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 Determination of Test Substance in Various Solvents." 19.0 Affected Documents______________________________ ____________________ 19.1 ETS-8-171.0, "Column Elution Method: Solubility Determination of Test Substance in Various Solvents." 19.2 ETS-8-172.0, "Shake Flask Method: Solubility Determination of Test Substance in Various Solvents." ETS-8-170.1 Page 6 of 9 Solubility Determination: Screen Test Method LIMS # 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 03/13/01 ETS-8-170.1 Page 7 of 9 Solubility Determination: Screen Test Method LIMS # E00-1762, Page 19 of 28 Attachment A: Example Preparation Worksheet, page 1 o f 2 3M Environmental I ahoratory SOLUBILITY SCREEN GLP Study Number: _______________________ Sample preparation worksheet Test Substance: IDS:____ ------- Date: Source: Solvent: ID#: Step Source: 1 Weigh approximately 10 mg 1 mg of test substance into a 2.5 mL-4 mL glass screw-top vial. Weight of test substance: __________ mg Balance ID:-------------------- Date/lnitials: 2nd replicate optlonal:_ _mg Thermometer ID: 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorously/vortex, and sonicate the mixture and visually check for undlssolved particles. Analyst Analyst Analyst Analyst volume added (mL)/ approx cone, after addition (ug/mL) Sample Prep OBSERVATIONS/NOTES Date/Time- Step 2-1 Total volume solvent added (mL) Q.1 Approximate Solubility (ug/mL) 100,000 Flask vortex-mixed? Yes/No Room Temp------!C Is there solute still presentYes-contlnue to step 2-2 Flask sonicated? Yes/No Time-----------------rain NO- The solution Is at 10%, and is considered "infinitely soluble." bfs Flask allowed to settle? Yes/No Time--------- rain further solubility testing Is required. Date/Time- Step 2-2 asTotal volume solvent added (mL) Approximate Solubility (ug/mL) 20,000 Date/Time- -L. Steo 2-3 1Total volume solvent added (mL) Approximate Solubility fuo/mL) 1.0,000 Date/Time- J- Step 2-4 2Total volume solvent added (mL) Approximate Solubility (ug/mL) 5.000 Flask vortex-mixed? Yes/No Room Temp--------!C Is there solute still present? Yes/No Flask sonicated? Yes/No Time----------------- min Flask allowed to settle? Yes/No Time----------pain Flask vortex-mixed? Yes/No Room Temp--------!C Is there solute still present? Yes/No Flask sonicated? Yes/No Time---------.--------min Flask allowed to settle? Yes/No Time----------min Flask vortex-mixed? Yes/No Room Tem pFlask sonicated? Yes/No Time-----------Flask allowed to settle? Yes/No Time-- -1C Is there solute still present? Yes/No O n n n ln s in n s : Did the substance dissolve in 2 mL or less of solvent? Yes -Approximate concentration at which the test substance is soluble in solvent:_______ ug/ml The solubility of the test substance is to be determined via the shake flask method. or No Continue to page two for further testing. Notes/ additional comments: 3M Environmental Laboratory Report No. FACT-TCR-005 LIMS # EOO-1762, Page 20 of 28 ETS-8-170.1 Solubility Determination: Screen Test Method Page 8 of 9 Attachment A Coni.: Example Preparation Worksheet, page 2 o f 2 i GLP Study Number: 3M Environmental Laboratory SOLUBILITY SCREEN _________________________ Sample preparation worksheet T est Substance:_______________________US;______________ Source: Date:_____________________ Solvent: ID#: Source:___________ Step (continued from page 1) " D id th e test substance dissolve in 2 mL? Yes/No If Y ES , th e test is com plete, and there Is no need to co ntinue w ith th e screen test. If NO, continue to step 3 to determine the approximate solubility o f the substance. 3 Weigh approximately 10 mg 1 mg of test substance into a 100 mL graduated stoppered cylinder/volumetric flask. Weight of test substance: ______ mo Balance ID:________________t Date/lnitials:. 2nd replicateoptional:_____________mg Thermometer ID:____________t 4 Add test solvent according to the table below. Following each addition o f solvent, shake vigorously/vortex, and sonicate the mixture and visually check for undlssolved particles. volume added (mLy approx cone, after S olubilitv data addition (ug/mL) Sample Prep O B S E R V A T IO N S /N O T E S Analyst Date/Time / Step 4-1 Total volume solvent added (mL)... 10 Approximate Solubility (ug/mL)... 1,000 Flaskvortex-mixed? Yes/No Room Temp Flasksonicated? Yes/No Time Flaskallowed to settle? Yes/No Time ___ ! is there solute still present? Yes/No min min Analyst Date/Time / Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL)... 200 Flaskvortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Time Flaskallowed to settle? Yes/No Time ___ !C Is there solute still present? Yes/No min min Analyst Date/Time / Step 4-3 Total volume solvent added (mL)... 100 Approximate Solubility(ug/mL)... 100 Flaskvortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Time Flaskallowed to settle? Yes/No Time ___ !G Is there solute still present? Yes/No min min 5 Weigh approximately 10 mg 0.5 mg o f test substance into a 1 L graduated stoppered cylinder/volumetric flask/or equivalent. Analyst Weight of test substance: mo__________________ Balance ID: -____________________ Date/lnitials:. Date/Time / Step 5-1 Total volume solvent added (mL)... 1000 Approximate Solubility (ug/mL)... 10 Flaskvortex-mixed? Yes/No RoomTemp Flasksonicated? Yes/No Time Flaskallowed to settle? Yes/No Time #Q Is there solute still present? Yes/No miq min Conclusions: Did the substance dissolve In 1000 mL o r less o f solvent? Yes -AoDroximate concentration at which the test substance is soluble in solvent: ua/ml The solubility of the test substance is to be determined via the shake flask method. or No -The solubility of the test substance is to be determined via the column elution method. Notes/ additional comments: 3M Environmental Laboratory Report No. FACT-TCR-005 LIMS # E00-1762, Page 21 of 28 ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 of9 3M Environmental Laboratory Report No. FACT-TCR-005 Attachment B: Solubility Screening T est Sample Preparation W orksheets LIMS # E00-1762, Page 22 of 28 LIMS # EOO-1762, Page 23 of 28 3M Environm ental Laboratory SOLUBILITY SCREEN G LP S tudy Num ber: TCR-005 Sample preparation worksheet Test Substance: P F O A ________________ id#: T C R -9 91 31 -0 37 Source: 3M Internal D ate:^ ^ ~/ OCJ Solvent: A ce to n e Source: f 'i A n CJL step 1 Weigh approximately 10 mg 0.5 mg of test substance into a 2.5 mL-4 mL glass screw-top vial. Weight of test substance: i O - l l mg Balance ID:____ Llr^/ Il <'_____ .t , Date/lnitials:8<<' p f' D O 2nd replicate optional: _mg Thermometer ID:r34j%D T K Y f inO M 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorousiy/vortex, and sonicate the mixture end visually check for undissolved particles. Tip Q f \C Analyst r. ir'c Analyst Analyst volume added (mL)/ approx cone, after Solubility data addition (ug/mL) Date/Time 2 ^pj-oCi i'-^ r lp * * . Step 2-1 Total volume solvent added (mL)... 0.1 Approximate Solubility (ug/mL)... 100,000 Date/Time Step 2-2 Total volume solvent added (mL).. 0.5 Approximate Solubility (ug/mL).. 20,000 Date/Time_ Step 2; Total volume solvent added (mL).. Approximate Solubility (ug/mL).. ',000 Date/Time / Step 2-4 Jotal volume salxewfScJded (mL)... 2 Approximate Solubility (ug/mL)... 5,000 Sample Prep OBSERVATIONS/NOTES Flask vortex-mixedTSsS/No Room Temp C Flask sonicated?igs/Klo Time _______ min Flask allowed to settle? /fesl/No Time min Is there solute still present? Yes-continue to step 2-2 N M T h e solution is at 10%, and is considered "infinitely soluble." No rther solubility testing is required. Flask voitafamixeU? us/Nu UoanaTemp, :sonicated? Yes/No Time ^ min Flask allowed to settle? Yes/No Time ^ \ m i n Is there solute still present? Yes/No Rask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time__ Rask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time__ solute still present? Yes/No Is there solute still preesseennl P/Sfeg/No^ Conclusions; Did the substance dissolve in 2 mL or less of solvent? \ .& Yes -Approximate concentration at which the test substance is soluble in solvents 'Ynug/m l Timi sulubility af the teat aubataiilb is LuLib (M auilined VIU Uie shaKa TH3L.Kniellim i or No Continue to page two for further testing. . v>-------J S u b stan ces Notes/additional comments: -lO % r e ^ U 'V e . T o _ i <_ ! f U . Solubility Screen Test Page 1 of 2 Exact Copy of Original t r ____ tfy ii Initial D ate 3M ETS Laboratory Ca) TD 3m O< |P3 o5 "l Ijsr o7g3r 8oi>5 LIMS # EOO-1762, Page 24 of 28 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparation worksheet Test Substance: PFOA id#: TCR-99131-037 Source: 3MInternal Date: Solubility Screen Test Page 2 of 2 "Exact Copy of Original w -iw Initial . j u . Date ~ 3M ETS Laboratoiy & w T<7p33 3mS O< PP 3 0n " UST *1?0) o01>|< 3M Environm ental Laboratory SOLUBILITY SCREEN G LP Study Num ber: TCR-005 Sample preparation worksheet Test Substance: P F O A id#: TC R -99131-037 Source: 3M Internal D a t e ^ C irj r J w Solvent: M eth an o l Source: Q*T Or-rlr-V 1 Weigh approximately 10 mg 0. 5 mg of test substance Into a 2.5 mL-4 mL glass screw-top vial. Weight of test substance: /Q . fcJ 2nd reptate optional: mg _mg Balance ID: V 9 '/* 7 Thermometer ID: ChnOL/. Date/lnitialsS ^ ? ^ - CO C 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorously/vortex, and sonicate the mixture and visually check for undissolved particles._______________________________ Analyst Cvnr Analyst volume added (mL)/ approx cone, after Solubility data addition (ug/mL) Date/Tlmefrt y t c o I / \ & ^ Step 2-1 Total volume solvent added (mL)... 0.1 Approximate Solubility (ug/mL)... 100,000 Date/Time / Total volume solvent added! 0.5 _Agg^mate_So^Mto^g/my^ 20,000 Date/Time_ Step 2-3 Total volume soient added (mL).. 1 Approximate Solubility (ug/mL).. 10,000 Date/Time / Step 2-4 ToJaTvolume solvent added (mL)... 2 Approximate Solubility (ug/mL)... 5,000 Sample Prep OBSERVATIONS/NOTES Flask vortex-mixedT^'sSTNo Room Tempo? .-^ C Is there solute still present? Yes-oontinue to step 2-2 Flask sonicated'fYiVNo Time Flask allowed to settle? Q & N o Tim e 3 Q min ( N O ^ /h e solution Is at 10%, and is considered "infinitely soluble " No min further solubility testing is required. Flask voltexjmixed? Yes/No Room Temp_______ IC Flask sonicaietKLYes/No Time____________min Flask allowed to settle? Yes/No Time_______ min Is there solute still present? Yes/No Flask vortex-mixed? Yes/No Roam Temp_ Flask sonicated? Yes/No Time\ 3 1Flask allowed to settle? Yes/No Timfe>- Flask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time_ Flask allowed to settle? Yes/No Time Is there solute still present? Yes/No min Conclusions: Did die substance dlssolyejn 2 mL or less of solvent? ^ Y e s )-Approximate concentration at which the test substance is soluble in solvent:^?/O f p ua/ml The solubility sf the toot eubotanoo io to be determined via Uib 1iak.u flabh. i i wthoU. VJLf 0U - t o - 0 1 or No Continue to page two for further testing. S u b S ls n C S hatA n/J & S b lt/b ,//l7 tJ Notes/additional comments: fecriJUl''^ ' H O 'fu K h & ir" 3M Environmental Laboratory Report No. FACT-TCR-005 LIMS # EOO-1762, Page 25 of 28 Solubility Screen Test Page 1 of 2 Exact Copy of Original j 7 ____ Initial o H -tm Date 3M ETS Laboratory \\\ Ox'S 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparation worksheet Test Substance: PFOA id#: TCR-99131-037 Date: Source: 3M Internal Solvent: Methanol Step (continued from page 1) ID#: Source: test. If NO, continue to step 3 to determine the approximate solubility of the substance. 3 Weigh approximately 10 mg 0. 5 mg of test substance into a 100 m l graduated stoppered cylinder/volumetric flask. Weight of test substance: ___________mg Balance ID:______________ . Date/lniti; 2nd replicate optional:____________ mg Thermometer ID:___________. A Add test solvent according to the table below. Following each addition of solvent, shake vigorouslyAortex, and sonicate _______ the mixture and visually check for undlssolved particles._________________________ volume added (mLV approx cone, after addition (ug/mL) Sample Prep OBSERVATIONS/NOTES Analyst Date/Tlme_ Step 4-1 Total volume solvent added (mL).. 10 Approximate Solubility (ug/mL).. 1,000 Flask vortex-mixed? Yes/No RoomTemp_ Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Time ^ / Is there solute still present? Yes/No min min Analyst Date/Time Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL)... 200 Flask vortex-mixed? Yes/No Roorj Flask sonicated? Yes/No Tirfie_ Flask allowed to settle? Yis/No Time Is there solute still present? Yes/No min Analyst Date/Tlme_ Step 4-3 Total volume solvent added (mL)... 100 Approximate Solubility (ug/mL)... 100 Flask vortex-mbjed? Yes/No Room Temp______ Is there solute still present? Yes/No Flask sonieptio? Yes/No Time__________ min Flask allowed to settle? Yes/No Time_______mjfl 5 Weigh approximately 10 mg 0. 5 mg of test substanc&lnto a 1 L graduated stoppered cylinder/volumetric flask/or equivalent. Weight of test substance: ___________mgr ______________ Balance ID: .__________________ Date/lnitials: Analyst Date/TIme / Step 5-1 1000 S Approximate Solubility (ug/mL)... i g X Flask vortax-mixed? Yes/No RoomTemD Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Time C Is there solute still present? Yes/No fnin min Conclusions: / Did the substance dissolve in 1000 mL or less of solvent? / Yes -Approximate concentration at which the test substance is soluble in solvent: ua/ml y ' The solubility of the test substance is to be determined via the shake flask method. / or No -The solubility of the test substance is to be determined via the column elution method. NotesTadditional comments: 3M Environmental Laboratory Report No. FACT-TCR-005 LIMS # EOO-1762, Page 26 of 28 Solubility Screen Test Page 2 of 2 Exact Copy of Original 3M ETS Laboratory LIMS # EOO-1762, Page 27 of 28 3M Environm ental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparation worksheet Test Substance: PFOA________________ id #: TCR-99131-037 Source: 3M Internal Date: 8 " Srp-f- c Q Solvent: Water ID#: AJ/fl Source: M f | !' ~ f 2 . _ . " = / & - Step 1 Weigh approximately 10 mg 0.5 mg of test substance into a 2.5 m i-4 mL glass screw-top vial. Weight of test substance: fO -i* mg Balance ID: ~ j i / *7 Pate/lnitials:<R 3 ^ ^ 2nd replicate optional: -- mg Thermometer ID: T~Ai D^- 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorously/vortex, and sonicate the mixture and visually check for undissolved particles. 0^ C /V \ _ 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-005 Sample preparation worksheet Test Substance: PFOA id#: TCR-99131-037 Date: Source: 3M Internal Solvent: Water ID#: Source: Step (continued from page 1) ***Dld the test substance dissolve in 2 mL? Yes/No If YES, the test Is complete, and there is no need to test. If NO, continue to step 3 to determine the approximate solubility of the substance. tinue with the screen 3 W eigh approximately 10 m g 0 .5 m g o f test substance into a 100 m L graduated stoppered cyffnderA/olumetric flask. Weight of test substance: ___________mg Balance ID:_______ Date/lnitials: 2nd replicate optional:____________ mg Thermometer ID: / 4 A dd test solvent according to the table below. Following each addition o f solvent, sht fe vlgorouslyArortex, and sonicate the mixture an d visually check for undlssolved particles.______________________ ' Analyst volume added (mL)/ approx cone, after Solubility data addition (ug/mL) Sample Prep Date/Time Step 4-1 Total volume solvent added (mL)... 10 Approximate Solubility (ug/mL)... 1,000 Flask vortex-mixed? YepfNo I loFlask sonicated?Ye: Flask allowed to settlfer? Yes/No Time OBSERVATIONS/NOTES Isthere solute still present? Yes/No Analyst Date/Time Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL),,, 200 Flask vortex-mixdd? Yes/No Room Temp______ Flask sonicate/i? Yes/No Time__________ rnin Flask allowedlo settle? Yes/No Time______ min Is there solute still present? Yes/No Analyst Date/Time Step 4-3 Total volume solvent added (mL)... 100 Approximate Solubility (ug/mL),,. 100 Flask vortex-mixed? Yes/No RoomTemp_ Flask sonicated? Yes/No Time______ Flask a)(owed to settle? Yes/No Time__ Is there solute still present? Yes/No 5 W eigh approximately 10 m g 0 .5 m g o f test substance Mto a 1 L graduated stoppered cylinderAolumetric flask/or equivalent. Analyst Weight of test substance: ma ___/ Balance ID:______________ . Date/lnitlals:_ Date/Time / Step 5-1 Total volume solvent added (mL)... 1000 Approximate Solubility (ug/mL),,, 10 /Flask vortex-mixed? Yes/No RoomTemD / Flask sonicated? Yes/No Time / Flask allowed to settle? Yes/No Time "C Isthere solute still present? Yes/No min min Conclusions: Did the substance dissolve in 1000 mL or Idss of solvent? Yes -Approximatorconcentration at which the test substance is soluble In solvent:____ ua/ml The solubjHry of the test substance is to be determined via the shake flask method. or No -The sojdbility of the test substance Is to be determined via the column elution method. Notes/ additional comments: 3M Environmental Laboratory Report No. FACT-TCR-005 LIMS # EOO-1762, Page 28 of 28 Solubility Screen Test Page 2 of 2 Exact Copy o f Orgi initial _ D ata 3M ETS Laboratory