Document EKJv71ZvYv5nBZbawj43zMpV

BACK TO MAIN Study Title Solubility of Perfluoro-1-octanesulfonyl Fluoride (POSF) in Water Data Requirement 40 CFR 160.105(b) Author Mark E. Ellefson Performing Laboratory 3M EnvironmentalLaboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Environmental Laboratory Study # LlMS E01-0859 Total Number of Pages 19 BACK TO MAIN 3M Environmental Laboratory TABLEOF CONTENTS Study Information............................................................................................................................... 4 Summary............................................................................................................................................ 5 Purpose.............................................................................................................................................. 5 Test Substance .................................................................................................................................. 5 Test System ....................................................................................................................................... 6 Method Summaries ............................................................................................................................ 6 Preparatory Methods.......................................................................................................................... 6 Data Summary ................................................................................................................................... 7 Statistical Methods and Calculations ................................................................................................. 7 Statement of Conclusion.................................................................................................................... 7 References ......................................................................................................................................... 7 List of Attachments ............................................................................................................................. 8 Signature Page................................................................................................................................... 9 At Page 2 of 19 BACK TO MAIN 3M Environmental Laboratoly LIST OF TABLES Table 1. Summary Table of Solubility of POSF TN-A-2825 in Water................................................ 5 Table 2. Characterizationof the Test Substance .............................................................................. 5 Table 3. Description of test systems used in this study .................................................................... 6 Table 4. Summary of Sample Preparation........................................................................................ 7 Table 5. Summary Table of Solubility of POSF TN-A-2825 in Water................................................ 7 Page 3 of 19 STUDYINFORMATION Analytical Chemistry Laboratories Solubility Testing 3M EnvironmentalTechnology and Safety Services (ET&SS) 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Dr. William K. Reagen, Laboratory Manager Mark E. Ellefson, Principal Analytical lnvestigator Kristin L. Terrell, Analytical Chemist Mark L. Anderson, Analytical Chemist Experimental Dates ' Sample Analysis Initiation: 24 May 2001 Sample Analysis Completion: 01 Jun 2001 dl BACK TO MAIN 3M Environmental Laboratory Page 4 of 19 BACK TO MAIN 3M Environmental Laboratory SUMMARY Solubility of Perfluoro-1-octanesulfonylfluoride (POSF) 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. The approximate solubility of POSF was determined by performing a solubility screen test (ETS-8-170.1). POSF was determined to be soluble at concentrations less than 294 qg/mL in water at 22-24OC. Results are presented in table 1: Table 1. Summary Table of Solubility of POSF TN-A-2825 in Water. I Water I I ~~ The solubility of POSF was determined to be less than 294 qg/mL in water at 22-24'C. PURPOSE The purpose of this study was to determine the solubility of POSF in water. d ' TESTSUBSTANCE Perfluoro-1-octanesulfonyl fluoride (POSF), TN-A-2825 Table 2. Characterization of the Test Substance Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity 01-01-2010 Ambient TN-A-2825 Clear liquid, density = 1.824g/mL 98% Page 5 of 19 BACK TO MAIN 3M Environmental Laboratory TESTSYSTEM Table 3. Description of test systems used in this study Source Millipore System Expiration Date I I Stora-ge Conditions I I 3M Laboratory Identification Number I I Purity/Grade I, NA Ambient INA ASTMTypeI METHODSUMMARIES The solubility determination of POSF TN-A-2825 in water was performed according to 3M Laboratory Method ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents". I' The Solubility Screen Test Method was used to determine the solubility range of POSF TN-A2825 in water. Incremental amounts of water were added to POSF neat material and a qualitative determination of the solubility was made. The screen test indicated the solubility of POSF to be less than 294 qg/mL in water at 22-24'C. A detailed description of the Solubility Screen Test method used in this study is located in Attachment A. PREPARATOMRYETHODS 0 ETS-8-170.0"Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." This method is a pre-requisiteto the shake flask and column elution methods and provides an estimate of the solubility of the test substance in the solvent of choice. Microliter amounts of sample were added to varying amounts of water. Following sample addition, the volumetric flasks were shaken and observed for POSF droplets on the bottom. The solubility screen test estimated the solubility of POSF to be less than 294 qg/mL in water at 22-24'C. Page 6 of 19 BACK TO MAIN 3M Environmental Laboratory Table 4. Summary of Sample Preparation. volumetric flask. 2 The volumetticflask is sealed, shakenand then allowedto sit over night for 24 hours. 3 The volumetricflask isvisually checkedfor the test substance,which would be in the form of oily droplets on the bottom. 4 This sametest was donewith 5uL in6.205L (1.47ugmL) and 1ULin 5/25/01 to 6/01/01 6.205L (294ngmL)ina 6 Lvolumetricflask. The 294ng/mL solution was allowedto sit for 5 days. The samplewas stillvisibleinthe flask after 5 days. I DATASUMMARY Table 5. Summary Table of Solubility of POSF TNA-2825 in Water. I Water < 294 qg/rnL STATISTICAL METHODASND CALCULATIONS No statistical methods or calculations were required. The data was reported as the solubility of POSF being less than 294 qglmL at 22-24'C in water as determined by the initial screening method. STATEMENT OF CONCLUSION Under the conditions of the present study, the solubility of POSF TN-A-2825 in ASTM Type I water is less than 294 qg/mL at 22-24 '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. Page 7 of 19 BACK TO MAIN 3M Environmental Laboratory LISTOF ATTACHMENTS 0 Attachment A: Solubility Screening Method ETS-8-170 "SolubilityScreen Test: Approximate Solubility Determination of a Test Substance in Various Solvents",including the sample preparation worksheets. Page 8 of 19 BACK TO MAIN 3M Environmental Laboratory SIGNATUREPAGE We certify that this report is a true and complete representationof the data for this phase of the study: Mark E. Ellefson Principal Analytical Investigator Date I William K. Reagen Laboratory Manager Date Page 9 of 19 ~ ~ ~ ~ ~ A ~ A C H M E NAT BACK TO MAIN 3M EnvironmentalLaboratory I' Page 10 of 19 3M ENVIRONMENTLAALBORATORY ~~ ~~ BACK TO MAIN 3M Environmental Laboratory SOLUBILITSYCREENTEST:APPROXIMATSOELUBILITDYETERMINATIOONF A TESTSUBSTANCE IN VARIOUS SOLVENTS Method Number: ETS-8-170.1 Adoption Date: 09/08/00 Effective Date: 03/14/01 Approved By: Wil6arn K. Reaggn, Laboratory Manager Date I' Marcd Ellefson, Projgt Le+ 1.0 SCOPE AND APPLICATION 1.1 Purpose. According to methods set forth by the United States Environmental Protection Agency ( U S 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/I, (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/volurne). 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. ETS-8-170.1 Soliibility Determination: Screen Test Method Page 1 o f 9 Page 11 of 19 BACK TO MAIN 3M Environmental Laboratory 1.3 Acceptable Matrices. Aqueous (e.g. Milli-Q water, 0.0 1M CaCl,), Acetone, Methanol, or other solvent(s) of interest. 2.0 SUMMARY OF METHOD 2.1 Preliminary Solubility Determination in solvent. Weigh approximately 10 mg of test substance into a 2.5 mL-4 mL glass screw-capped vial. Add test solvent in varying increments to the vial. After each solvent addition, vortex mix for approximately 15 sec., and sonicate 2-5 minutes. Make observations of the solution and visually confirm whether or not particles are present; it may be necessary to allow the solution to sit for up to 5 minutes. Add test solvent in a stepwise fashion up to 2 mL. If the substance fully dissolves after the first solvent addition of 100 pL,the test substance shall be considered highly soluble, and no further testing is required. If there are still undissolved particles in the vial, 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 observationson a standardizedpreparation 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/volumetricflask (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.O). 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 CaCI, (ad); 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 Page 2 of9 Page 12 of 19 BACK TO MAIN 3M Environmental Laboratory 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. dt 7.5 Glass volumetric flasks, 10 mL to 1000 mL. 7.6 10 pL-1000 pL Pipettemanm manual pipettor and plastic pipette tips, or equivalent. 8.0 REAGENTASND 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 CaCl,, A 0.01 M CaCl, stock solution is prepared by weighing 1.5 g CaC1, Dihydrate in a weigh boat and transferring to a 1 L volumetric flask and diluting to the mark with Milli-Qm water. 8.6 Test substance of known purity. 9.0 SAMPLHEANDLING 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 Page 3 of 9 Page 13 of 19 BACK TO MAIN 3M Environmental Laboratory 10.0 QUALITCYONTROL 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 k 1 mg of test substance into a 4 mL glass screw-top vial or equivalent. Record the weight (refer to attachment A for an example of a standardized prep sheet). 12.1.2 Add solvent (e.g. water, methanol, acetone) according to the table below to the test substance. 4 mL vial or equivalent Solvent addition 1 Total volume solvent 0.1 I' added (mL). .. Approximate Solubility 100000 (Pd~)... Solvent addition 2 0.5 20000 ~~ ~~ solvent ~ Solvent addition 3 addition 4 1 2 10000 5000 12.1.3 Following addition of solvent, vortex mix approximately 15 seconds, sonicate 2-5 minutes. Visually check for undissolved particles. If undissolved test substance remains, continue adding solvent according to the above chart. It may be necessary to 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 >lo 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 >lo% (mass/volume). The test substance shall be regarded as "highly soluble," and no further testing is required. 12.1.5 If the test substance did not dissolve in the 2 mL of solvent, weigh 10 mg f 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 Page 14 of 19 BACK TO MAIN 3M Environmental Laboratory 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 1000 200 100 (Clg/mL). - 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 k 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 concentrationof 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.O). If no visible particulates are observed, the shake flask method (ETS-8172.0) shall be used to determine the solubility. I' 13.0 DATAANALYSIASND CALCULATIONS 13.1 The.solubility determination in this method is qualitative/semi-quantitative.. 13.2 The point to which the substance dissolves in solvent is confirmed visually. The solubility point is therefore a qualitative determination. 13.3 The concentration estimation is semi-quantitativein that the approximate concentration is calculated by the following equation: c=a/b Where: c= the semi-quantitativeconcentration pg/mL, a= amount of substanceweighed out (vg), and b= the approximate amount of solvent added (mL). 14.0 METHODPERFORMANCE 14.1 Limitation of data. The accuracy to which the solubility is determined is subject to a large margin of error due to the way in which the solvent is added to the solute. Since large 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 Solubiliv Determination: Screen Test Method Page 5 o f 9 Page 15 of 19 BACK TO MAIN 3M Environmental Laboratory 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 -0ECD Guideline 105: pp. 1-7, Adopted 1995 18.2 United States Environmental Protection Agency. OPPTS 830.7860 Water Solubility (Generator Column Method). Prevention, Pesticides and Toxic Substances: Fate, Transport ,and Transformation Test Guidelines. EPA 712-C-96-042: pp. 1-1 7, 1996 18.3 United States Environmental Protection Agency. OPPTS 830.7840 Water Solubility: Coliunn 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.O,"Column Elution Method: Solubility Determination of Test Substance in Various Solvents.'' 18.5 3M Environmental Laboratory Method ETS-8-172.0, "Shake Flask Method: Solubility Determination of Test Substance in Various Solvents." 19.0 AFFECTEDDOCUMENTS 19.1 ETS-8- 171.O, "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 Page 6 of 9 Page 16 of 19 BACK TO MAIN 3M Environmental Laboratory 20.0 REVISIONS Revision Number Reason For Revision 1 It was desirable to make the method more universally applicable by removing references to specific test substances. Revision Date 03113/0 1 J! ETS-8- 170.1 Solubiliw Determination: Screen Test Method Page 7 of 9 Page 17 of 19 I Attachment A: Example Preparation Worksheet,page I of 2 I BACK TO MAIN the mixture and visually check forundissolvedparticles. Analyst - volume added (mLy .. aapdpdritoioxnco(Wncm. aLft)er Sample Prep OBSERVATlONSlNOTES Datflim- Step 2-1 Total volume solvent added (mL) 0.1 Approximate Solubility (uglmL) 100,000 Flask vortex-mixed? Y ~ J NR~~~ iem oc Is there P solute still present'Kescontinue to step 2-2 Flask - Ti Flask allowed to settle? Yes/No T-i NO- The solution is at lo%, and is considered"infinitely soluble." h 2 further solubility testing is required, Analyst - D a t m i m a SteD 2-2 Total volume solvent added (mL) 0.5 Approximate Solubility (ualmU 20,000 Flask vortex-mixed?YeslNo RoomT e d IS there solute still present? YedNo Flask sonicated?YeslNo T-i Flask allowed to settle? YeslNo-Ti Analyst __ D a t e l T i m p Step 2-3 Total volume solvent added (mL) 1 Approximate Solubility (uqlmL) 10.000 Flask vortex-mixed? Yes/No Room T e U Is there solute still present? Yes/No Flask sonicated? YeslNo T-i Flask allowed to settle? YeslNo-Ti Analyst Datemim- SteD 2-4 Flask vortex-mixed? Y e s " Room T e d Is there solute stili present? Yes/No __ b Total volume solvent added (mL) 2 Approximate Solubility (udrnL) 5,000 Flask sonicated? YedNo -Ti Flask allowed to settle? YeslNoT i U w 5 Did the substance dissolve in 2 mL or less of solvent? Yes -Approximate concentration at which the test substance is soluble in solvent: ~ g h l TJ The solubility of the test substance is to be determined via the shake flask method. P a(P or No Continue to page two for further testing.' Notes/ additional comments: W ETS-8-170.1 SolubiliQ Determination: Screen Test Method ~~ ~ Page 8 of9 I Attachment A Cont.: Example Preparation Worksheet,page 2 of 2 GLP Study Number: Test Substance: Solvent: 3M Environmental Laboratory SOLUBILITY SCREEN Samplepreparation worksheet ID#: Date: L Source: I IW BACK TO MAIN ~naiyst - Analyst - Analyst - volum added (mly approx conc. after Solubilitv data .ddMon I u d W Dalefriune I Step 4-1 Total volwne solvent added (mL) . 10 Approximale Solubility(uglmL)... 1,ooO DalelTime / step 4-2 Total volwne solvent added (mL) 50 npproximateSolublity (uglmL)... 200 Dalefriie / Step 4-3 Total volune solvent added (mL) . 100 Approximate Solubility(uglmL)... 100 Sample Prep Flask voctexmixed? YeslNo Room Temp Flask sonicated? YeslNo Time Flask allowed lo settle? Yes/No Time Flask vorlexmixed? YedNo Room Temp Flask sonicated?YedNo Time Flask allowed to sellle? YedNo Time Flask vorlexmixed? YesMo Room Temp Flask sonicated? YeslNo Time Flask allowed to settle? Yes/No Time OBSERVATlONSlNOTES "C Is there solute still present? YeslNo min min 'c Is there solute still present? YeSMo min min O C Is there solute still present? YeslNo min min Analyst __ Datefrime / Step 5-1 Total volume solvent added (mi) . 1ooO nppoximate Solubility(uglmL)... 10 Flask vorlexmixed? Y e s " RoomTemp ~ Flask sonicated?YedNo Time Fbsk allowed to settle? YesMo Time O C Is there solute still present? Y e a 0 min rnin ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 of9