Document QMMqe8azmByEpmbQYXrgDBaZv

BACK TO MAIN Study Title Characterization Study of PFOA (lot #332), Primary Standard - Test Control Reference #TCR-99030-030 Phase: Solubility Determination 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-006 (LIMS #E00-1763) Centre Analytical Laboratories Study # 023-034 Total Number of Pages 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 GLP Compliance Statement Study Title: Characterization Study of PFOA (lot #332), Primary Standard - Test Control Reference #TCR-99030-030, Ph ase: So lu bility Determ inatio n Study Identification Number: FACT-TCR-006, Centre Analytical Laboratories Study # 023-034 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. None Study # FACT-TCR-006, Page 2 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Quality Assurance Statement Study Title: Characterization Study of Ammonium Perfluorooctanoate (PFOA), Primary Standard # TCR-99030-030, PHASE: SOLUBILITY DETERMINATION Study Identification Number: FACT-TCR-006, Centre Analytical Laboratories Study # 023-034 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 m i too m i too 1 /1 5 -1 /1 6 /0 1 01/31/01-02/02/01 Phase Solubility Sample Preparation In Phase Sample Dilutions Data Audit Draft Report Date Reported to Management Study Director 7/17/00 7/17/00 7/17/00 7/17/00 01/19/01 01/19/01 2/02/01 2/02/01 S /so / ! Date Study # FACT-TCR-006, Page 3 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Table of Contents GLP Compliance Statement..................................................................................................................... 2 Quality Assurance Statement................................................................................................................... 3 Study Information...................................................................................................................................... 6 Summary.................................................................................................................................................... 7 Purpose...................................................................................................................................................... 7 Test Substance......................................................................................................................................... 8 Method Summaries................................................................................................................................... 8 Preparatory Methods........................................................................................................................... 9 Protocol Deviations............................................................................ ......................................................9 Data Summary, Analyses, and Results...................................................................................................10 Analytical Results................................................................................................................................ 10 Data Sum mary.....................................................................................................................................10 Statistical Methods and Calculations......................................................................................................10 Statement of Conclusion..........................................................................................................................10 References................................................................................................................................................ 11 List of Attachments................................................................................................................................... 11 Signature Page..........................................................................................................................................12 Study # FACT-TCR-006, Page 4 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 List of Tables Table 1. Summary Table of Solubility of PFOA TCR-99030-030 in Water, Methanol and Acetone. . 7 Table 2. Characterization of the Test Substance........................... ......................................................8 Table 3. Description of Test Systems Used in this S tudy.................................................................... 8 Table 4. Summary of Sample Preparation............................................................................................. 9 Table 5. Summary Table of Solubility of PFOA TCR-99030-030 in Water, Methanol and Acetone. . 10 Study # FACT-TCR-006, Page 5 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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, Analytical Investigator 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 Dr. William K. Reagen 3M Environmental Technology and Safety Services (ET&SS) 3M Environmental Laboratory 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Experimental Dates Sample Analysis Initiation: 17 July 2000 Sample Analysis Completion: 12 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. Study # FACT-TCR-006, Page 6 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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-8-170.1). 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 test substance is determined to be soluble at concentrations greater than 10% (mass/volume) then no additional testing is required. Results are presented in table 1: Table 1. Summary Table of Solubility of PFOA TCR-99030-030 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-99030-030 was determined to be greater than 10% (mass/volume) 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. Study # FACT-TCR-006, Page 7 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Test Substance PFOA, Test Control Reference #TCR-99030-030 Table 2. Characterization of the Test Substance T est S ubstance PFOA Source 3M Specialty Materials, Bldg. 236-1B-10 Expiration Date Storage Conditions 01-01-2010 Frozen 3M Laboratory Identification Number Physical Description TCR-99030-030 White Powder Purity * 95.0% * The purity of the PFOA usedin this study was determinedto be 95.0%. The same bt/soume of compound was used throughout the entire study. Test System Table 3. Description of Test Systems Used in this Study W ater S o u rce Expiration Date Storage C onditions Millipore System NA Ambient 3M Laboratory Id e n tific a tio n N um ber Purity/G rade NA ASTM Type I Methanol B & J Brand 2005 Ambient, Flammable Cabinet A cetone EM Science 2005 Ambient, Flammable Cabinet TN-A: 4466 TN-A: 4616 HPLC Grade HPLC Grade Method Summaries The solubility determination of PFOA TCR-99030-030 in water, methanol, and acetone was performed according to United States Environmental Protection Agency OPPTS 830.7840, "Water Solubility: Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility" Guidelines as implemented by 3M Laboratory ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents". The Solubility Screen Test Method was used to determine the solubility range of PFOA TCR-99030-030 in water, methanol, and acetone. Incremental amounts of water, methanol, or Study # FACT-TCR-006, Page 8 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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 C. A detailed description of the Solubility Screen Test method used in this study is located in Attachment A. Preparatory Methods ETS-8-170.1 " S olubility Screen Test: Approxim ate S olubility Determination o f 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. 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 C. The solubility screening information was used to determine that no additional solubility testing was necessary. Table 4. Summary of Sample Preparation. S tep 1 2 3 4 S a m p l e P r e p a r a t io n 10 mg test substance is weighed into tared 2.5 mL - 4.0 mL glass screw-capped vial. 0.1 mL of test solvent (water, methanol or acetone) is added to glass screw-capped vial. 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. . Following sonication, the sample is checked visually for undissolved particles o f the test substance. If all o f 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 erfo rm ed 9/08/00 9/08/00 9/08/00 9/08/00 Protocol Deviations There were no deviations from the original protocol for this phase. Study # FACT-TCR-006, Page 9 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Data Summary, A nalyses, and Results A nalytical Results S pecificity (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 95.0% Substances that are stable in water. Hydrolytic studies have been conducted at the 3M Environmental Laboratory according to the United States Environmental Protection Agency Guidelines, OPPTS 830.2110 "Hydrolysis as a Function of pH." Refer to 3M Environmental Laboratory Report No. W1878 (currently in submittal) for study conclusions and results. Data S ummary Table 5. Summary Table of Solubility of PFOA TCR-99030-030 in Water, Methanol and Acetone. S olvent PFOA S o l u b il it y (m a s s / v o l u m e ) Water > 10% Methanol > 10 % Acetone > 10% The solubility of PFOA TCR-99030-030 in water, methanol and acetone is greater than 10% (mass/volume) at 23 C. Attachment B contains solubility screening test sample preparation worksheets. S t a t is t ic a l M e t h o d s a n d C a l c u l a t io n s No statistical methods or calculations were required. The data was reported as the solubility of PFOA being greater than 10% (mass/volume) at 23 C 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# 99030-030 in ASTM Type I water, methanol and acetone is greater than 10% (mass/volume) at 23 C. Study # FACT-TCR-006, Page 10 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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. 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 Study # FACT-TCR-006, Page 11 of 29 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Signature Page We 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 Study # FACT-TCR-006, Page 12 of 29 BACK TO MAIN 3MinviF@nmntl Li&efgtefy Attachment A: Solubility Screening Method Study # FACT-TCR-006, Page 13 of 29 3M Environmental laboratory BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Solubility Screen Test: Approximate Solubility D etermination 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 V 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). E x a e F B o p y ^ f aQbl^ nalytes* Test substance and degradation products for solubility testing. ETS-8-170.1 Solubility Determination $ f $ j t _ ^ $ ! t f $ page u of 29 Page 1 of 9 BACK TO 3M Environmental Laboratory Report No. FACT-TCR-006 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 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 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 Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 15 of 29 Page 2 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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 p,L-1000 \iL 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 A cetone, 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 Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 16 of 29 Page 3 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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 Solvent addition 2 0.5 Solvent Solvent addition 3 addition 4 12 1OOOQ0__ 1:2-- 1---- 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 all 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 Study # FACT-TCR-006, Page 17 of 29 Page 4 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 100 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 of 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 Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 18 of 29 Page 5 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 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 A ffe c te d D o c u m en ts_____________________________________________________________ 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 Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 19 of 29 Page 6 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 20.0 Revisions___________________________________________________________ _ Revision Number Reason For Revision Revision Date 1 It was desirable to make the method more universally applicable by removing references to specific test substances. 03/13/01 ETS-8-170.1 Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 20 of 29 Page 7 of 9 Attachment A: Example Preparation Worksheet, page 1 o f 2 BACK TO MAIN 3M Fnvirnnmentai Laboratory SOLUBILITY SCREEN GLP Study N um ber:________________ ________ Sample preparation worksheet Test Substance:__________________ ID*-------------- Date:_________________ S o u rc e :_____________ Solvent:________________________ [Dft____________ Step S o u rc e :_____________ 1 Weigh approximately 10m g1 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 optional.;_______________ mg Thermometer ID:___________ . 2 Add test solvent according to the table below. Following each addition of solvent, shake vlgorously/vortex, and sonicate the mixture and visually check for undissolved particles._________________________________________________ A n a ly s t A n a ly s t A n a ly s t A n a ly s t volum e added (m L)/ approx cone, after addition (ug/m L) Sample Prep D ate/Tim e--------------L---------------- S tep 2-1 T o ta l volu m e so lve n t added (m L) Q.1 Approxim ate Solubility (ug/mL) 100,000 OBSERVATIONS/NOTES r Is there solute still presentTTes-continue to step 2-2 N O - The solution is at 10%, and Is considered "infinitely soluble." N fu rth e r solubility testing is required. D ate/Tim e-------------- 1---------------- S tep 2-2 T o ta l volu m e so lve n t added (m L) Q.5 Approxim ate Solubility (ua/mLI 20.000 D ate/Tim e--------------L_________ SteD 2-3 Total volum e solvent added (mL) Approxim ate Solubility (uo/mLl 10.000 D ate/Tim e-------------- L---------------- Step 2-4 Total volum e solvent added (mL) Approxim ate Solubility (ua/mLI 5.000 Flask vortex-m ixed? Y es/N o R oom Tem p_____!C Is th e re so lu te still present? Y e s/N o Flask so nica te d? Y es/N o Tim e--------------- -- min Flask allow ed to settle? Y es/N o Tim e--------- min Flask vortex-m ixed? Y es/N o R oom Te m p -- _ ! C IS th e re so lu te still present? Y e s/N o Flask sonicated? Y es/N o Tim e_________ -- min Flask vortex-m ixed? Y es/N o R oom Tem p-- -- !C Is th e re solute still present? Y e s/N o Flask so nica te d? Y es/N o Tim e___________ min Cnnrliisinns' 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-006 Study # FACT-TCR-006, Page 21 of 29 ETS-8-170.1 Solubility Determination: Screen Test Method Page 8 of 9 BACK TO MAIN Attachment A Cont: Example Preparation Worksheet, page 2 o f 2 3M E nvironm ental L a b o ra to ry SOLUBILITY SCREEN G L P S tu d y N u m b e r : _______________________________ Sam ple prepa ra tio n w orksheet T e s t S u b s ta n c e :_________________________ ijm:_______________ Source:____________ _ D a te :_______________________ S o lve n t: ID#: Source:____________ S tep (continued from page 1) ***D id th e te s t s u b s ta n c e d is s o lv e in 2 m L ? Y es/N o If Y ES, th e te st is co m p le te , and th e re is n o need to c o n tin u e w ith th e screen te s t. If NO, c o n tin u e to ste p 3 to dete rm in e th e a pp ro xim a te s o lu b ility o f th e substance. 3 Weigh approxim ately 1 0 m g 1 mg o f test substance into a 100 mL graduated stoppered cylinder/volum etric flask. W eiqht o f test substance: ma B alance ID: . D ate/lnitials: 2 n d re p lica te o ptional: ma T herm om eter ID: . 4 Add test solvent according to the table below. Following each addition o f solvent, shake vigorously/vortex, and sonicate the m ixture and visually check for undlssolved particles.______________________________________________________ _______ v o lu m e a d d e d (mL)/ a p p ro x c o n e , after S o lu b ilit y d a ta addition (ug/mL) Sam ple P rep O B SER VATIO N S/N O TES A n a ly s t D a te/T im e / S te p 4-1 Total volume solvent added fm Ll... 10 Approximate Solubility (ug/mL)... 1,000 Flask vortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Tim e C min min Is there solute still present? Yes/No Analyst D a te/T im e / Step 4-2 Total volume solvent added (m U ... 50 Approximate Solubility (ug/mL)... 200 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 min A n a lyst D a te /T im e / Step 4-3 Total volume solvent added im U ... 100 Approximate Solubility (ug/mL)... 100 Flask vortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Tim e C Is there solute still present? Yes/No min min 5 Weigh approxim ately 10 mg 0 .5 mg o f test substance into a 1 L graduated stoppered cylinder/volum etric flask/or equivalent. W e ig h t o f te s t s u b sta n ce :_______ m a ____________________B a la n c e ID: . ______________________D a te /ln itia ls : A n a ly s t Date/Time / Step 5-1 1000 Approximate Solubility (ug/mL)... 10 Flask vortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Tim e Flask allowed to settle? Yes/No Tim e C Is there solute still present? Yes/No min min C o n clu sion s: D id th e s u b s ta n c e d is s o lv e in 1000 m L o r le ss o f solvent? Y e s -ADDroxim ate concentration a t w hich the te st substance is soluble in solvent: u a/m l The solubility o f the te s t substance is to be determ ined via the shake flask m ethod. or N o -The solubility o f the te st substance is to be determ ined via the colum n elution m ethod. N otes/ a d d itio n a l co m m en ts: 3M Environmental Laboratory Report No. FACT-TCR-006 Study # FACT-TCR-006, Page 22 of 29 ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 of 9 BACK TO MAIN 3M Environmental Laboratory Report No. FACT-TCR-006 Attachment B: Solubility Screening Test Sample Preparation Worksheets Study # FACT-TCR-006, Page 23 of 29 BACK TO MAIN Study # FACT-TCR-006, Page 24 of 29 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-006 Sample preparation w orksheet Test Substance: PFOA_______________ id#: TCR-99030-30 Source: 3M Internal Date: C D C jC TC - Solvent: W ater 'D*= M/A Source: -Q ^ Step tt oo o 1 Weigh approximately 10 mg 0.5 mg of test substance into a 2.5 mL-4 mL glass screw-top vial. Weight o f test substance: iO -2 3 ma Balance ID: / 7 ______ ._ 2nd replicate optional: --------- ma Thermometer ID: T-hp.^r-n O '-! Date/lnitials'.S .S ^p 0 0 Q H C < 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorous/y/vortex, and sonicate the mixture arid visually check for undissolved particles.__________________________ , f r( ao o CO 3 Analyst ( Analyst Analyst volume added (mL)/ approx cone, after S olubility data addition (ugfmL) Date/Timrg V f / < f l / - f l ? f > (D Step 2-1 Total volume solvent added (mL)... 0.1 100,000Approximate Solubility (ug/mL)... Sample Prep OBSERVATIONS/NOTES Flask vortex-m ixedZ^^/N o Room TempJ S . Flask sonicated?<2ewNo T im e_ Flask allowed to settle? ^ j ^ / N o Time /C . m in Is there solute still present? Yes-contlnue to step 2-2 lO j/T h e solution Is at 10%, and is considered "Infinitely soluble." No rther solubility testing is required. Date/Time Step 2-2 Total volume solvent added (mL)... 0.5 Approximate Solubility (ug/mL)... 20,000 Date/Time_ Total volume solvent added (mL).. Approximate Solubility (ug/mL).. Step 2-3 1 10,000 Date/Tii Total volume'aelyent added (mL).. Approximate Solubiifj Flask vortex-mixed? Yes/N p-R oom Tem p________fC Flask sonicated? Yes/No Tim e____________ min Flask allowed to settle? Yes/No Time________ min Is there solute Yes/No Flaskp/drtex-mlxed? Yes/No Room Temp________ ik sonicated? Yes/No Time_____________ rniQ Flask allowed to settle? Yes/No Time________ min Is there solute still present? Yer 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 C o n clu sio n s: Did the substance dissolve in 2 mL o r less o f solvent? Yes -Approximate concentration at which the test substance is soluble In solvent:^ ' /Q%?uq/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: Solubility Screen Test Page 1 of 2 G>I',o H l^rxk (jgg)c/ne SStf* O b 3M ETS Laboratory on r"\ Study # FACT-TCR-006, Page 25 of 29 BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-006 Sample preparation worksheet T est S ubstance: PFOA_______________id#: TCR-99Q30-30 Date: Source: 3M Internal S olvent: Water ID#: Source: Step (continued from page 1) ***D id the te s t sub stan ce d iss o lv e in 2 m L? Yes/No If YES, the te st is com plete, and there is no need to co n tinu e w ith the screen te s t. If NO, c o n tin u e to ste p 3 to d e te rm in e th e approxim ate s o lu b ility o f the substance. 3 Weigh approximately 10 mg 0.5 mg o f test substance into a 100 mL graduated stoppered cylinderArolumetric flask W eight of test substance: ____________mg Balance ID:_______________ . Da0/Initials: 2ndreplicate optional:____________ mg Thermometer ID:____________, 4 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 volume added (mL)/ approx cone, after S o lu b ility data addition (ug/mL) Date/Time Step 4-1 Total volume solvent added (mL)... 10 Approximate Solubility (ug/mL),,. 1,000 Sam ple Prep lOBSERVATIONS/NOTES Flask vortex-mixed? Yes/No Room Tem p_ IS Flask sonicated? Yes/No Time___________ min Flask allowed to settle? Yes/No Time_______ min Is there solute still present? Yes/No Analyst Date/Time_ Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL)... 200 Flask vortex-mixed? Yes/No RoomTemp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time i Is there solute stm 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 Room Temp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time min min 5 Weigh approximately 10 mg 0 .5 mg o f test substance into a 1 L graduated stoppered cylinder/volumeftic flask/or equivalent. Balance ID: Analyst Date/Time / Step 5-1 mnn Approximate Solubility (ug/mL)... 10 Flask vortex-mixed? Yes/No Room Temp Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Time C Is there solute still present? Yes/No m in / roifi C o n c lu s io n s : D id th e su b sta n ce d is s o lv e in 1000 m L o r less o f so lv e n t? Yes -Approximate concentration at which the test su{)atnce is soluble in solvent: ___ ua/ml The solubility of the test substance is to b-ddfermined via the shake flask method. V or No -The solubility of the test substancgjs'tS be determined via the column elution method. N ofesfadditional comm ents: Solubility Screen Test Page 2 of 2 3M ETS Laboratory to 73 S om3a- 5u<m' P3 or Q> H oa>>f3 BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-006 Sample preparation worksheet Test Substance: PFOA id #; TCR-99030-30 Date: CD CfTC Source: 3M Internal Solvent: M ethanol IDttTN//) Source: M rt IT J3 . Step < tP c*T )c S sept- OD 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: ' O - 5 3 mg Balance ID: i-lQi T______ 1 Date/lnitials^S p p ^ C O 2nd replicate optional: --------------------- mg Thermometer ID: "T h (L rm C H 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.__________________________ ^ .^ ritp ld l/ o i Cf & t m Analyst QtrC- Analyst CO *t< Analyst > Q O Analyst 73 o0 o> 010 to CD o> aro to volum e added (mL)/ approx cone, after S olubilltv data addition (ug/mL) Date/Timif s Y W c O / `'I S g ~ / w > Step 2-1 Total volum e solvent added (mL)... 0.1 Approximate Solubility (ug/mL)... 100,000 Date/Time_ / Step 2-2 Total volum e solvent added (mL)... 0.5 Approximate Solubility (ug/m L)... 20,000 D ate/T im e Step 2-3 Total volume solvent added (mL)... 1 Approximate Solubility (ug/mL).,, 10,000 Step 2-4^ solvent added (mL).. i,000Approxima~Selubility (ug/m LLrf Sample Prep OBSERVATIONS/NOTES Flask vortex-mixed? ^ lo Room Temp Flask s o n ic a te d ? ^ e ^ N o Tim e__A_n_t____________ Flask allowed to settle? c S S /N o Tim e / C * min Is there solute still present? Yes-continue to step 2-2 tig s The solution is at 10%, and is considered "infinitely soluble." No irther solubility testing is required. Flask vortex-mixed? Y e s /N o g o e rtri emp_ Flask sonicated? YejiWo nm e_ Flask allowed s there solute still present? Yes/No ask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time C m in min Rask vortex-mixed? Yes/No Room Temp C Flask sonicated? Yes/No Tim e . .______ min Flask allowed to settle? Yes/No Time________ min Is there solute still present? Yes/I C on clusion s: Did the substance dissolve in 2 mL o r less o f solvent? Yes -Approximate concentration at which the test substance is soluble in solvent: C w ua/m l 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: <D Solubility Screen Test Page 1 of 2 m o c J [M e r-fe rd U ,T tX C M C i en ^ y 'cr o^jm /o\ c : ^ , 7 c c a Tta C^ M ^ E T s S io S r ^ ^ 3 ^ a ora ory UAs tmdaUM ^ U [o ^ ~ w 31s *oflo> =Z<mTJ 23 p3 on " z3?j s3r oo CD i # Ov BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-006 ' Sample preparation worksheet T est S ubstance: PFOA id#: TCR-99030-30 Date:________________ Source: 3M Internal Solvent: Methanol*34 ID#: Source: Step (continued from page 1) ***D id th e te s t s u b sta n ce d is s o lv e in 2 m L ? Yes/No IfvESl, th e te s t is com plete, and there is no need to co n tin u e w ith th e screen te st. If NO, co n tin u e to s te p 3 to d e te rm in e the approxim ate s o lu b ility o f th e substance. 3 Weigh approximately 10 mg 0 .5 mg o f test substance into a 100 mL graduated stoppered cylinder/volumetric flask. Weight of test substance: __ _________mg Balance ID:_______________ . Date/lnitials: 2ndreplicate optional:____________ mg Thermometer ID:____________L 4 Add test solvent according to the table below. Following each addition of solvent, shake vigorously/vortex, and son/cafe ________ the mixture and visually check for undlssolved particles.__________________________________ Analyst Analyst Analyst Analyst volume added (mL)/ approx cone, after S o lu b ility data addition (ug/mL) Sample Prep OBSERVATIONS/NOTES Date/Time Step 4-1 Total volume solvent added (mL)... 10 Approximate Solubility (ug/mL)... 1,000 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 min Date/Time Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL)... 200 Flask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time_______ Flask allowed to settle? Yes/No Time Is there soltite still present? Yes/No 3d, Date/Time_______ /_________ Step 4-3 Flask vortex-mixed? Yes/No RoomTemp ^ "C Is there solute still present? Yes/No _Tot.a.l vo.lume so.lv..e..n...t.a...d..d..e..d...(..m...L..)... ~100 Flas,k sonicat.e. d? Yes/No ,, Time T. X -----------m---inr , _ . . . . . . . __ Flask allowed to settle? Yes/No Titfie_______ mm Approximate Solubility (ug/mL)... 100________________ __________ ____________ ___________________________________ W eigh approxim ately 10 m g 0 . 5 m g o f te s t substance in to a 1 L graduatpd'stoppered cylinderA /olum etric fla sk/or equivalent. Weight of test substance:______ ma ____________ ^B a la n c e ID: _.___________________ DDaattee//lnitials: Date/Time_______ /_________ Step 5-1 Total volume solvent added (mL)... 1000 Approximate Solubility (ug/mL)... 12________________ < Conclusions: Flask vo[ie5<-mixed? Yes/No Room Temp Flaskionlcated? Yes/No Time F fis k allowed to settle? Yes/No Time C Is there solute still present? Yes/No min min Did the substance disso lve in 1000 m ie s s o f solvent? Yes -Approx! s concentration at which the test substance is soluble in solvent: ua/ml solubility of the test substance is to be determined via the shake flask method. ^The solubility of the test substance is to be determined via the column elution method. Notes/ additional 3M Environmental Laboratory Report No. FACT-TCR-006 Study # FACT-TCR-006, Page 27 of 29 Solubility Screen Test Page 2 of 2 3M ETS Laboratori' BACK TO MAIN ix o S -T) 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: TCR-006 Sample preparation worksheet !fi?) Test Substance: PFOA Solvent: Acetone id: TCR-99030-30 Source: 3M Internal Date: g S p - f C O C 'h n C - Oo Step o O Source: 5 E i* g /lC L 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: >> mg Balance ID: 1. Date/lnitialsv R S ^ p ^ r ^ O 2nd replicate optional: ---- mg Thermometer ID: ~TV~) . 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. v* CVCCL volum e added (mL)/ 3 approx cone, after fi) Solubility data addition (ug/mL) Sample Prep OBSERVATIONS/NOTES Analyst r ivy Pate/Time0 / /'. 5 Step 2-1 Total volum e solvent added (mL)... 0.1 Approximate Solubility (ug/mL)... 100,000 Flask vortex-mixed? Room Temp r - ^ 3 c Flask s o nicatedljJe^N o rTime S m in Flask allowed to settle? (yg s/N o T im e I S m in Isjh e re solute still present? Yes-continue to step 2-2 N O ^ T h e solution Is at 10%, and is considered "infinitely soluble." No Trmer solubility testing Is required. Analyst Date/Time / Step 2-2 Total volum e solvent added (mL)... 0.5 Approximate Solubility (ug/mL)... 20,000 Date/Time I Step 2-3 Total volume solvent added (mL)... 1 Approximate Solubility (ug/mL)... 10,000 Flask vortex-mixed? Yes/No Room Tj Flask sonicated? Yes/No Flask allowed to settle? bred? Yes/No R oo m T e m p _ lioated? Yes/No Time________ allowed to settle? Yes/No Tim e Is there solute it? Yes/No C m in m in Is there solute still present? Yes/No Analyst Approximate R ask vortex-mixed? Yes/No Room Temp_ Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Tim e___ Is there solute still present? Yes/No m in C on clusion s: Did the substance dissolve in 2 m L o r less o f solvent? -y Yes -Approximate concentration at which the test substance is soluble in solvent: ' ' / O f cug/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: Study # FACT-TCR-006, Page 28 of 29 Solubility Screen Test Page 1 of 2 K tec vu> - WUf c C5^e\..(Xj \xjO O , vxtf uoas Q \ 4-Vv . -A oprcLdfisri u 3M ETS Laboratory m ov^\ ^ oz[cn-/o\ Vtcfc Study # FACT-TCR-006, Page 29 of 29 BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Number: T C R -0 0 6 Sample preparation worksheet Test S ubstance: PFOA_______________ID#: TCR-99Q30-30 D a te :_______________ Source: 3M Internal S olvent: Acetone*34 ID#: Source: Step (continued from page 1) ***D id th e te s t s u b sta n ce d is s o lv e In 2 m L? Yes/No If YES, th e te s t is com plete, and th e re is no need to co n tin u e w itl t e s t If NO, c o n tin u e to ste p 3 to d e term in e th e approxim ate s o lu b ility o f th e substance. 3 Weigh approximately 10 mg 0 .5 mg o f test substance into a 100 mL graduated stoppered cylinder/volumt ic flask. W eight of test substance: ___________ mg Balance ID: Date/ln'rtials: 2ndreplicate optional:_____________mg Thermometer ID: 4 Add test solvent according to the table below. Following each addition of solvent, shake vigorousjyfvortex, and sonicate ____ ____ the mixture and visually check for undissolved particles.____________ _____ Analyst Analyst Analyst Analyst volume added (mLV approx cone, after S o lu b ility data addition (ug/mL) Sam ple Prep OBSERVATIONS/NOTES Date/Time Step 4-1 Total volume solvent added (mL)... 10 Approximate Solubility (ug/mL)... 1,000 Flask vortex-mixed? Yes/Njv'Room Temp_ Flask sonicated? YeslU e Time_______ Flask allowed to sejdd? Yes/No Time__ Is there solute still present? Yes/No Date/Time_ Step 4-2 Total volume solvent added (mL)... 50 Approximate Solubility (ug/mL)... 200 Is there solute still present? Yes/No 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 allowed to settle? Yes/No Time___ Is there solute still present? Yes/No min 5 Weigh approximately 10 mg 0 .5 rmy6f test substance into a 1 L graduated stoppered cyllnder/volumetric flask/or equivalent. Date/lnitials: Date/Time / / Step 5-1 Total volume solvent addd (mL)... 1000 Approximate SolyBraty (ug/mL)... 10 Flask vortex-mixed? Yes/No RoomTemo Flask sonicated? Yes/No Time Flask allowed to settle? Yes/No Time C Is there solute still present? Yes/No min min Conclusions: / Did the substance d iss o lv e in 1000 m L o r less o f s o lve n t? Yes -Approximate concentration at which the test substance is soluble in solvent:. uo/ml The solubility of the test substance is to be determined via the shake flask method. No -The solubility of the test substance is to be determined via the column elution method. Notes/ additional comm ents: Solubility Screen Test Page 2 of 2 3M ETS Laboratory * w n> m -OO <=3 U P3 o3 1a ZjST 73 oco 3<