Document 9yzng3vMLrBpXOjJQ9VwvRe5
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Study Title
Characterization Studyof 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 EnvironmentalLaboratory 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
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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, PHASE: SOLUBILITY DETERMINATION
Study Identification Number: FACT-TCR-006, Centre Analytical Laboratories Stud#y023-034
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 inbtuhleleted list below.
0 None
Date
Y#///?g/ -
/
WilliaG K. Reagen, Testing Facility Management
Date
Study # FACT-TCR-006, Page2 of 29
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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 IdentificationNumber: FACT-TCR-006, Centre Analytical Laboratories Study# 023-034 This phase of the study has been inspected by t3hMe Environmental Laboratory Quality Assurance Unit (QAU) as indicatedin the following table. The findings were reportetod the study director and laboratory management.
7117/00
SolubilSityampPlereparation
7117/00
PInhaSseampDleilutions
1115- 1/16/01 Audit Data
01/31101-02/02/01
Draft Report
I 7/17/00 I 7/17/00
I 01/19/01 I 2/02/01
I 7/17/00 1 7/17/00
~ 01/19/01 ~ 2/02/01
QAU
Date
Study # FACT-TCR-006, Page 3 of 29
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3M Environmental Laboratory
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TABLEOF CONTENTS
GLP Compliance Statemen.t.............................................................................................................. 2 Quality Assurance Statemen..t........................................................................................................... 3 Study Information............................................................................................................................... 6 Summary ............................................................................................................................................ 7 Purpose .............................................................................................................................................. 7 Test Substance.................................................................................................................................. 8 Method Summaries............................................................................................................................ 8
Preparatory Methods..................................................................................................................... 9 Protocol Deviations............................................................................................................................. 9 Data Summary. Analyses. and Resul.t.s............................................................................................ 10
Analytical Results.......................................................................................................................... 10 Data Summary .............................................................................................................................. 10 Statistical Methods and Calculations................................................................................................. 10 Statement of Conclusion .................................................................................................................... 10 References ......................................................................................................................................... 11 List of Attachment.s............................................................................................................................ 11 Signature Page................................................................................................................................... 12
Study # FACT.TCR.006. Page 4 of 29
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3M Environmental Laboratory Report No. FACT-TCR-006
LISTOF TABLES
Table Table
1. 2.
Summary Table of Solubility of PFOA TCR-99030-030
Characterization of the Test Substance..........................
.in Water, Methanol and Acetone.. 7 ................................................... 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-99030-030 in Water, Methanol and Acetone..10
Study # FACT-TCR-006, Page5 of 29
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3M Environmental Laboratory Report No. FACT-TCR-006
STUDYINFORMATION
Study Director
John Flaherty Centre Analytical Laboratory 3048 Research Drive State College, PA 16801
Analytical Chemistry Laboratories
Solubility Testing
Certificate of 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 by3tMheEnvironmental Laboratory. All study data for this phase anad copy of the phase reportare archived by the3M Environmental Laboratory.
Study # FACT-TCR-006, Page6 of 29
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3M Environmental Laboratory
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SUMMARY
Solubility ofPFOA in water isa significant parameter because the spatial and temporal movement (mobility) of asubstance through the environment is largely determined by its solubility in water. Water soluble substances readily gain accestso humans and other living organisms; furthermore the knowledgeof the solubility in water aisprerequisite for testing biological degradation, bioaccumulation, and other tests. Solubility oPfFOA in methanol and acetone isa significant parameter for general laboratory knowledge in the preparation and analysisPoFfOA. The approximate solubility ofPFOA was determined by performinga solubility screentest (ETS-8-170.1). PFOA was determinedto be solubleat concentrations greater than10% (massholume) in water, methanol and acetone at 2"3C. According to the screen test,if the test substance is determinedto be soluble at concentrations greater tha1n0% (massholume) then no additional testing is required.
Results are presented in table1:
Table 1. Summary Tableof Solubility of PFOA TCR-99030-030 in Water, Methanol andAcetone.
Water
> 10%
Methanol
I
Acetone
> 10% > 10%
The solubility ofPFOA TCR-99030-030 was determinedto be greater than 10%(massholume) in water, methanol and acetone a2t 3 "C.
PURPOSE
The purpose of this phase of the study wtoadsetermine the solubility oPf FOA in water, methanol, and acetone as part of the characterization of this test substance.
Study # FACT-TCR-006, Page7 of 29
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3M Environmental Laboratory
Report No. FACT-TCR-006
TESTSUBSTANCE
PFOA, Test Control Reference #TCR-99030-030
Table 2. Characterization of the Test Substance
I I I TESTSUBSTANCE
PFOA
Source
I 3MSpecialtyMaterialsB, ldg2.36-1B-10
I
I n x p i r a t i o nDate
I 01-01-2010
I
I StoraCgoenditions
1 Frozen
I
TCR-99030-030
I
t I I DescripPthioynsical
~~~
~
Powder White
Purity
* 95.0%
I *Thepuritv of Ute PFOA usedin this &K& was determined to be 95.0% . ThesameWmmof compound was used
thmghouttheentk st@.
TEST SYSTEM
Table 3. Description of Test Systems Used in this Study
I Source
I MiSlliDvsoterem
Expiration Date NA
Storage Conditions Ambient
3M Laboratory Identification Number
Purity/Grade
NA
ASTM Type I
I B & J Brand
SIciEenMce
I
2005
2005
Ambient, Flammable Ambient, Flammable
Cabinet
Cabinet
TN-A: 4466
TN-A: 4616
HPLC Grade HPLC Grade
METHOD SUMMARIES
The solubility determinationof 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 OEC1D05, "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 amounotsf water, methanol, or
Study # FACT-TCR-006, Page 8 of 29
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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 tha1n0% (massholume) in water, methanol, and acetone a2t 3 "C. A detailed description of the Solubility Screen Test method used in this study is located in Attachment A.
PREPARATOMRYETHODS
0 ETSB-170.1 "Solubility Screen Test: Approximate Solubility Determinationof 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 substanthce in 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. Approximately10 mg PFOA was weighed into a glass vial, and0.1 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 PFOAbteo greater than10% (massholume) in water, methanol and acetone at23 "C. The solubility screening information was used to determine that no additional solubility testing was necessary.
Table 4. Summary of Sample Preparation.
I I
I screw-cawed vial.
9/08/00
2
0.1 mL oftest solvent (water, methanolor acetone) is added to glass
9/08/00
screw-capped vial.
3
Followingthe addition of test solvent, the vial is capped, shaken
9lO8lOO
vigorously (or vortexed), and the mixture is sonicated. Record mixing
I and sonicationtimes on the worksheet. I
4
Following sonication,the sample is checked visually for undissolved
particles of the test substance. If all of the test substance is dissolved,
the solubilityis determined tobe greater than10% (masslvolume)and
no additional solubility testing isrequired. If a portion of the test
substance remains undissolved,additionaldilutions are performed using
the appropriate solvent.
PROTOCODLEVIATIONS
There were no deviations from the original protocol for this phase.
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3M Environmental Laboratory Report No. FACT-TCR-006
DATASUMMARY, ANALYSESA,ND RESULTS
ANALYTICARLESULTS
0 Specificity (according to OPPTS 830.7840): The solubility determination as stated in the EPA Guidelines follows. This method should only be applied to:
0 Pure substance. This study shows a purity of 95.0%
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 830.21 10 "Hydrolysis as a Function of pH." Refer to 3M Environmental Laboratory ReportNo. W1878 (currently in submittal) for study conclusions and results.
DATASUMMARY
Table 5. Summary Table of Solubility of PFOA TCR-99030-030 in Water, Methanol and Acetone.
I
Water
I
> 10%
I
Methanol
>IO%
~
~~~
~
Acetone
> 10%
The solubility of PFOA TCR-99030-030 in water, methanol and acetone is greater 1th0a%n (mass/volume) at 23"C.
Attachment B contains solubility screening test sample preparation worksheets.
~~~~
~
~~
STATISTICAL METHODASND CALCULATIONS
No statistical methods or calculations were required. The data was reported as the solubility of PFOA being greater than 10% (massholume) 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 PFOTCAR# 99030-030 in ASTMType I water, methanol and acetone is greater tha1n0% (massholume) at 23 'C.
Study # FACT-TCR-006, Page 10 of 29
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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.
LISTOF ATTACHMENTS
0 Attachment A: Solubility Screening Method ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents".
0 Attachment 9:Solubility Screening Test Sample Preparation Worksheets
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3M Environmental Laboratory Report No. FACT-TCR-006
SIGNATURPEAGE
We certify that this report is a true and complete representaotifotnhe data for thisphase of the study:
Principal Analytical Investigator
Date
William K. Reagen Laboratory Manager
Date
Study # FACT-TCR-006, Page 12 of 29
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Attachment A: Solubilitv Screenina Method
Study # FACT-TCR-006, Page 13 of 29
3M ENVIRONMENTLAALBORATORY
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3M Environmental Laboratory Report No. FACT-TCR-006
SOLUBILITY SCREEN TEST: APPROXIMATE SDOELTEURBMILIINTAYTIONOF A
TESTSUBSTANCEIN VARIOUS SOLVENTS
Method Number: ETS-8-170.1
DaAted: option
09/08/00
Effective Date: 03/14/01
Approved By: WMilacnaLamagbeKor r.aRtoerayggn,
033/,$/&
Date
1.0 SCOPE AND APPLICATION
1.1 Purpose. According to methods set forth by the United States Environmental Protection
Agency (US EPA) andthe Organizationfor the Economic Cooperation andDevelopment
(OECD) a preliminary study, which will be outlined in this methods,erves as a prerequisite
to performing solubility testing via the Column Elution Method anSdhake Flask Methods.
The EPA and OECDsolubility testing guidelines state that if the preliminary solubility
determinationtest indicates a solubility of > lo'* g L (10 ppm), the Shake Flask Method
(ETS-8-172.0) is to be used. If preliminary testing indicates a solubility of
g/L (10
ppm) the Column Elution Method (ETS-8-171.0) will be used tdoetermine the solubility
in the solvent of interest. Additionally, due to the tendencyof certain compounds to be
highly soluble in particular solvents, no further solubility determinationwill be necessary
for compounds havingsolubility greater than 10% (massholume).
-1
atible Analytes. Test substance and degradation products fosrolubility testing.
E x a e W & OF=@::7?7
dA%/&- I .
L
$1
7&:.%&).- -1
ETS-8-170.1
Page 1 of 9
Solubility D e t e ~ ~ t i l t a t i o n SPa~ge~,4 ~of ~29~ ~ ~ ~ ! ~ ~ ,
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3M Environmental Laboratory
Report No. FACT-TCR-006
1.3 Acceptable Matrices. Aqueous (e.g. Milli-Q water, 0.01M CaCl,), Acetone, Methanol, or other solvent(s) of interest.
2.0 SUMMARY OF METHOD
2.1 Preliminary Solubility Determination in solvent. Weigh approximately 10 mg of test substance into a 2.5 mL-4 mL glass screw-capped vial. Add testsolvent in varying increments to the vial. After each solvent addition, vortex mix for approximately 15 sec., and sonicate 2-5 minutes. Make observationsof the solution and visually confirm whether or not particles are present;it may be necessary to allow thesolution 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 testsubstance shall be considered
highly soluble, and no further testing is required. If there are still undissolved particles in the vial, weigh 10mg oftest substance intoa 100mL glass stopperedvolumetric flask or graduated cylinder. Add test solvent until visual confirmation of the substance dissolution has been achieved. Record a l f observations on a standardized preparation sheet or logbook. Once 100mL solvent has been reached, the approximateconcentrationis at 100 pg/mL. If the solubility limit has not yet been achieved, weigahpproximately 10 mg of test substance and transfer to a 1 L graduated cylinder/volumetricflask (concentrationis approximately 10ppm). The container shouldbe sonicated and allowed tosit overnight to allow for maximal dissolution. If the undissolvedparticles are still observed after sitting > 12 hours, thecolumn elution method willbe utilized (ETS-8-171.0). If the test substance dissolves in 1 L or less of solvent, the shake flask method (ETS-8-172.0w) ill be used to determine the solubility.
3.0 DEFINITIONS 3.1 Test substance. A liquid or solid material for which therelative 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 matriceisn,cluding ASTM Type I Water
and various salt matrices (e.g. 0.01M CaC1, (aq)); and organicsolvent matrices, including
methanol, and acetone.
4.0 WARNINGSAND CAUTIONS 4.1 HealthandSafetyWarnings:
4.1.1 Wear the proper lab attire for all parts of these procedures. Weargloves and eye protection at all times.
4.1.2 Handle all solvents in a hood for all parts of the describedsample preparation procedure.
4.1.3 For potential hazards of each chemical used, refer to materiaslafety data sheets, packing materials, and3M Environmental Laboratory's Chemical Hazard Review.
4.1.4 No mouth pipetting is allowed.
ETS-8-170.1 Solubility Determination: ScreenTest Method
Study # FACT-TCR-006, Page15 of 29
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3M Environmental Laboratory Report No. FACT-TCR-006
4.2 Cautions: 4.2.1 Glassware in which standards are prepared should betriple 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 tsotarting the screeningprocedure.
6.0 EQUIPMENT 6.1 Analytical balance sensitive to 0.1mg. 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-topvial.
7.5 Glass volumetric flasks, 10 mL to 1000mL.
7.6 10 pL-1000 pL Pipettemanm manual pipettor and plastic pipette tips, or equivalent.
8.0 REAGENTS AND STANDARDS 8.1 Methanol (MeOH), HPLC/SPEC/GC grade fiom 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 CaCl,
Dihydrate in a weigh boat and transferring to a L1volumetric flask and diluting to the mark with Milli-QTM water. 8.6 Test substance ofknown purity.
9.0 SAMPLE HANDLING
9.1 Record times of initial preparation and dilution on a sample preparationsheet or logbook. 9.2 Once the preliminary testing has been completed and the appropriate information is
extracted, the screen test samples should be disposed intothe proper waste stream.
ETS-8-170.1
Solubility Determination: Screen Test Method Study # FACT-TCR-006, Page 16of 29
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3M Environmental Laboratory Report No. FACT-TCR-006
10.0 OUALITYCONTROL 10.1 Not applicable.
11.0 CALIBRATION AND STANDARDIZATION 11.1 The compounds of interest must beof known characterizationaccording tolaboratory
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 f 1 mg of test substance into a 4 mL glass screw-top vial or equivalent. Record the weight (refer to attachment A for an exampleof a standardized prep sheet).
12.1.2 Add solvent (e.g. water, methanol, acetone) according to the table belowthetotest substance.
4 mL vial or equivalent Total volume solvent
added (mL)...
Solvent addition 1
0.1
Solvent addition 2
0.5
Solvent Solvent
addition 3 addition 4
1
2
5000 O0O0
ywbr'c 12.1.3 Following addition of solvent, vortemxi pproximately 15seconds, sonicate 2-5 minutes. Visually check for undissolved particlesIf. undissolved test substance remains, continue adding solventaccording to the above chart. It may be necessary to allow the solution to settle for upto 5 minutes before makingobservations. Record observations on the standardized prepsheet.
12.1.4 If all particles dissolve, thenestimate the approximate solubility and document the concentration. Because the concentrationis >10 pg/mL, the shake flaskmethod (ETS-8-172.0) willbe used to determinethe accurate solubilitypoint. However, if the test substance dissolves afterthefirst solvent addition of100 pL the solubility is determined tobe >lo% (mass/volume). The test substance shallbe regarded as "highly soluble," and no furthertesting is required.
12.1.5 If the test substance did notdissolve in the 2 mL of solvent,weigh 10 mgf 1 mg of test substanceinto a 100mL glass volumetric flaskor equivalent. Record the weight (refer to attachmentA for an example of a standardized prepsheet).
12.1.6 Add solvent according to thteable below to the test substance todeliver 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 procedureson the preparation sheet.
ETS-8-170.1 Solubility Determination: Screeit Test Metlzod
Study # FACT-TCR-006, Page17 of 29
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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
1000
200
100
(Yg/mL)* - -
12.1.7 If the solubilitypoint is reached ator prior to the complete addition of 100 mL,the
concentrationestimation at whichthe substance is soluble should be documented and shall be usedas a starting pointfor the shake flask method (ETS-8-172.0).
12.1.8
If the 100 mL solvent levelhas been reachedwithout complete dissolution of test
substance, weigh out 10mg k 1 mg testsubstance and transfer to a 1L volumetric flask, graduated cylinder,or equivalent. Dilute to 1 L with test solvent. The
approximate concentration of test substanceis at 10 pg/mL. The flask should be allowed tosit 12-24 hours to allow for maximadl issolution. If the undissolved particles are still observed, the column elution methodwill be utilized (ETS-8171.O). If no visible particulates are observedt,he shake flask method (ETS-8172.0) shall be used to determinethe solubility.
13.0 DATAANALYSIASND CALCULATIONS 13.1 The solubility determinationin this methodis qualitativelsemi-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 concentrationpg/mL, a= amount of substanceweighed out(pg), and b= the approximate amountof solvent added (mL).
14.0 METHODPERFORMANCE 14.1 Limitation of data. The accuracy to which the solubilityis determined is subject to a
large margin of error due to the way in which the solvent is added thoe solute. Since large and varyingincrementsof solvent are being added tohe solute, this error margin must be considered when reportintghe concentration estimation.
14.2 The data obtained throughthis study is an estimation only and shoulbde treated as a qualitative estimation of the solubility of test substance in a givesnolvent.
ETS-8- 170.1 Sohlbility Deteimination: Screen Test Method
Study # FACT-TCR-006, Page18 of 29
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3M Environmental Laboratory Report No. FACT-TCR-006
14.3 For an accurate measurementof 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 placingin high or low BTU containers as appropriate. Use
broken glass containers to dispose ogflass pipettes.
16.0 RECORDS 16.1 Sign and date all observations and calculations.
17.0 ATTACHMENTS 17.1 Attachment'A-Exampleof a StandardizedSample Preparation Sheet:Solubility Screen
Prep Sheet.
18.0 REFERENCES 18.1 Organization for Economic Cooperation and Development. OECD Guidelinfeor Testing of
Chemicals. Water Solubility -0ECD Guideline 105: pp. 1-7, Adopted 1995 18.2 United States Environmental Protection Agency. OPPTS 830.7860 WaterSolubility
(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 WaterSolubility: Column Elution Method; Shake Flask Method. Prevention,Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-96-041p:p. 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, "ShakeFlask Method: Solubility Determination of Test Substancein Various Solvents."
19.0 AFFECTEDDOCUMENTS 19.1 ETS-8-171.0, "Column Elution Method: SolubilityDetermination of Test Substance in
Various Solvents." 19.2 ETS-8-172.0, "ShakeFlask Method: Solubility Determination of Test Substance in
Various Solvents."
ETS-8- 170.1 Solubility Determinntion: Screen Test Method
Study # FACT-TCR-006, Page 19 of 29
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3M Environmental Laboratory Report NO.FACT-TCR-006
Revision Number
Reason ForRevision
1 It was desirable to make the methodmore universally applicableby removing references to specific testsubstances.
Revision Date
03/13/01
ETS-8-170.1
Solubility Determination: Screen Test Method
Study # FACT-TCR-006, Page 20 of 29
Page 7 of 9
I Attachment A: Example Preparation Worksheet,page 1 of 2 I
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GLP Study Number: Test Substance:
Io1L:
Source:
I N-.
Sample preparation worksheet Date:
Solvent:
ID#
Source:
Step
1 Weigh approximately 10 mg f 1 mg of test substance into a 2.5 m L 4 mL glass screw-top vial.
subWstaenigchet:of test
c
n
g
Balance ID:
Date/lnitials:
2nd replicateoptional:
mg
Thermometer ID:
2 Add test solvent accordingto the table below. Following each addition of solvent, shake vigorouslyhortex,and sonicate
the mixture.and visually checkfor undissolved padicles.
DAatnflatmly-st
-
Analyst
-
Analyst
-
Analyst
-
volume added (mL)/
.. approx conc. after addition (uglmL)
Sample prep
OBSERVATIONWNOTES
Total volumseolvenatdded
Step 2-1 (mL) a.1
Approximate Solubility(ug/mL) 100,000
Flask vortex-mixed?Y ~ ~ R/~~N~ T~~ & Flassoknicated? Yes/No Flaskallowed to settle?YeslNo T-i
ISthere solutestill present7escontinue tostep 2-2
NO-The solution is at 10%. and is considered"infinitelysoluble." P further solubility testing is required.
D a t e T I m P ,Step 2-2 Total volumseolvenatdded (mL) 0.5
ADproximate Solubility (uq/mL) 20.000
DateITim-
Step 2-3
Total volumseolvenatdded (mL) I
Approximate Solubilitv(uq/mL) 1.0.000
Datdim-
Step 2 4
Total volumseolvenatdded (mL) 2
Approximate Solubility (uq/mL) 5,000
Flask vortex-mixed?YedNo Room T e
Flasksonicated?YeslNo
T- i
Flaskallowedtosettle?YeslNo T -i
d Is there solutestill present? YedNo
Flask vortex-mixed? YeslNoRoom T e t n p - - Z
Flasksonicated?Yes/No
T - i
Flaskallowedtosettle?YeslNo T-i
Is there solute still present? YeslNo
Flask vortex-mixed? Yes/NoRoom T e m p 2 1s there solutestill present?
Flasksonicated?Yes/No
T - i
Flaskallowed to settle?YeslNo T-i
Did thesubstance dissolvein 2 mL or less of solvent?
Yes-Approximateconcentrationatwhichthetestsubstanceissolubleinsolvent:
II~M
The solubilityof the test substanceis to be determined via the shake flask method.
or No Continuetopage two forfurthertesting.
Notes/ additional comments:
ETS-8-170.1 Solubility Determination: Screen Test Method
Page 8 o f 9
1 Attachment ACont.: Example Preparation Worksheet,page 2 of 2
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at ratiSonample NumbGerL: P Study
Substance:
Test
3M Environmental Laboratow SOLUBILITYSCREEN
ID& Sn,,rra.
Date:
Solvent:
ID#:
Source:
Step
(continued from page I)
"Did the test substance dissolve i n 2 mL? YeslNo If YES, the testIs complete, and thereIs no need to continue with the screen
test. If NO, continue to step3 to determine the approximate solubiliotyf the substance.
3 Weigh approximately 10 rng f 1 mg of test substanceinto a 100 mL graduated stoppered cylinderholumetrifclask.
substancWee: ight of test
mq
Balance ID:
optionaml:pticate 2nd
mg
Thermometer I D
Datdlnitials:
4 Add test solvent accordintgo the table below.Followingeach addition of solvent, shake vigorouslyhortex, and sonicate
the mixture andvisually check for undissolved particles.
I
I
volume added(d)l
approx conc. after
Solubilitv dataaddition(ua/mL)
Sample Prep
OBSERVATlONSlNOTES
DalefAlimnaelyst
-
I
Step 4-1
Total volume solvent added (m..L.)10
Approximate Solubility (uglm.L..) 1,000
FlaJtvortexmixed? YeslNo Room T ~
soFnlYiacseakstelNd?o
Time
Flaaskllowsetoedttle?
Y M oTimmein
P O Is tChere solutestill present? YerMo mi4
DaterlAimnealyst
I
Step 4-2
$ -
Total volume solvent added (m...L5)0
Q Approximate Solubility (uq/m.L..) 200
Y
Flaskv o ~ ~ ~ i xYeesdlN7o Roan Temp ' somFnilYTinaciseamksteelNd?o
FlaaslklowseteodttleY?eslNToimmein
O C Is there solutestill present? Y e a 0
DateflAimnealyst
I
Step 4-3
Flaskvoltexmixed?Y e a 0 RoToemmp
'C Is theresolute still present? YeslNo
T -
Total volume solvent added (.m..L1)00
0
Approximate Solubility (uglm.L..) 100
soFrnlaiYTcnsaiemktdeeNd?o FlaaslklowseteodttleY?eslNToimmein
z?J 5 Weigh approximately 10 mg f 0.5 mg of test substanceinto e 1 L graduated stoppered cylinder/volumetric flasWor equivalent.
0
0
substancWee: ight of test
0
mu
Balance ID:
Datehitials:
cs)
DaterAlimnaelyst
I
Step 5-1
Flaskvortex-mixed? YeslNo RoomT e m p 2 Is there solute still presentY? d o
- Total volume solvent added (m.L..)1OW
soFnlYTiacsieamksteelNd?o
min
Approximate Solubility (u@m..L.)10
FlaaallowseteodttleY?eslNToimmein
N
N
Conclusions:
4
Did the substance dissolvien 1000 rnL or lessof solvent?
N
u)
Yes -Approximateconcentrationat which thetestsubstance is soluble in solvent:
uu/ml
The solubility of the test substance is tobe determined via the shakfelask method.
or No -The solubility of the test substance is to be determined via the column elution method.
Notes1 additional comments:
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 TestSample Preparation Worksheets
Study # FACT-TCR-006, Page23 of 29
BACK TO MAIN
3M EnvironmentalLaboratory SOLUBILIN SCREEN
GLP Study Number: TCR-006 Test Substance: PFOA
IWI: TCR-99030-30
Source: 3M Internal
a m f l Samplepreparation worksheet
Date: r&~h
d
Solvent: Water
2 Step
, u/fl ID#:
Source: Pii\\<.-Q
\
5
.
&
M
A
n c 0
- &-/ i
P
* ' I
1 Weigh approximately10 mg f 0.5 mg of test subsfence into a 2.5 mL-4 mLglass screw-top vial.
Weight of test substance: 10.33
2nd replicate optional:
mg mg
Balance ID: 49 /
Thermometer ID: W : Q , - ~
2 Add test solvent accordingtothetablebelow.
Followingeachaddition of solvents,hakevigorously/vortexa,ndsonicate
D a t e l l n i t i a l s . : ~ . ~ ~0r ! -0 Ct
Flask sonicated
considered "infinitely soluble." No
added
DatefTime solvent
8 Q
Y
3*0 . .
-I
4
0
?J
0
-%
-0 P
Ip
ID
s N
P
N
(D
Analyst volume
\.
I Total
ApproximaSteolubil(iutyglmL)
I (mLa) ddseodlveonlutmTeotal
(uglmL) SoluAbpiliptyroximate
Step 2-2 0.5
... 20,000
Step 2-3
... I ... 10.000
Temp
OC sth here sol min min
Psol
L Is there
rnin rnin
I
Step 2-4
vortesxo-FFmnlaliaicxssaekktde?d?
Y eYaW0No RTiomoemYTeps/rNesoenmt?stipltmisn2olutIeSthere
Flask allowed to settle? YedNo Time
min
i
Conclusions:
Did the Substance dissolvein 2 mL or less of solvent?
Yes -Approximate concentration at whichthe test substance is soluble in solvent:& iO;7/3ua/ml
The solubilii of the test substance is to be determined via the shakfleask method. or No Continuetopage two for further testing.
Noted addltional comments:
TesStScroeluebnility Page 1 of 2
0 .r : 5i'./p,n @ cmc BW 00
3M ETS Laboratory
BACK TO MAIN
GNLuPmSbteurd:y SubstaTnecset :
3M Environmental Laboratory SOLUBILITY SCREEN
TCR-006
prSwepaoamrkrpasltheloenet
PFOA
1 ~ 1 1 :TCR-99030-30
Date:
Source: 3M Internal
Solvent: Water
IWI:
Source:
Ste(pcontinuefrdopmage
1)
"Did the test substance dissolve in 2 mL? YeslNo If YES, the testis complete, and thereis no needto continue with the scree
test. If NO, continue to step 3 to determine the approximatesolubility of the substance.
3 Weigh approximatelyIO mgf 0.5 mg of testsubstanceinto a100 m i graduated stoppered cylinderholumetric flask
BalanscueWbsetaignhcteo:f test
ID:
2nd replicate optional:
Thermometer ID:
4t
d ?J
0 0 OY
n-ul In
(0
N VI
5,
N u)
1
Solubility Screen Test Page 2 of 2
Yes -Approximate concentrat
ke flask method. umn elution method.
3M ETS Laboratory
BACK TO MAIN
3
3M Environmental Laboratow SOLUBILITY SCREEN
GLP Study Number: TCR-006
Sample preparation worksheet
Test Substance: PFOA
ID#: TCR-99030-30
Date: tq
00 C m
Source: 3M Internal
Solvent: Methanol
rcc)
ID#:thl# ClJlPc
Source: w e 3
ts
m c Q2ptOO
0
1
.'1Q9
-- 1 Weigh approximately10 mg f 0.5 mg of test substance into d 2.5 mi-4 m i glass screw-top vial.
Weight o f test substance:
op2tinmdar/e: plicate
t'L? 3 3 mg
mg
Balance ID: L/qI 7
Thermometer ID: ' f i e r r n d
Date/lnitials&d= a c rrc
2 Add test solvent according to the table bdow. Following each additionof solvent, shake vigorously/vortex, and sonicate
the mixture and visually check for undissolvedparticles.
t l t3/07/0r
volume added (mL)/
approx cone. after
Solubility data addltlon (UglmL)
CI
AnalyDsat teITim&#&/
'! 5 5 0 ~Step 2-1
Totavol lumesobenatdded (mL),.. 0.1
s0T nJi3m im tede 7ge SamplePrep I
OBSERVATlONSlNOTES
Flasvkoaex-mked? e Room Tern
0 IS thesroelustteilt
presenn Yescontinue to step 2-2
Flask
$The solution is at IO%, ancisdonsidere"dinfiniteslyoluble."
No
Approximate Solubility (ug/mL)... 100,000
Flask allowedto settle? &No lime
rther solubility testing is required.
Anaiyst
Date/Time
Total volume solvent adde(dmL)...
re solute still present? YeslNo
sksonicated? Y e a 0 Time
3 Flaskallowedto settle? Y d N oTime
0
9
4
0 A
-0
0)
Conclusions:
n lIn
Did the substance dissolveIn2 mL or less of solvent?
N m
Yes -Approximate concentrationat which thetest substance is soluble in solvent: >/O%ug/ml
4N The solubilityof the test substance is to be determined viathe shake flask method.
(D
or No Continue to page two for furthertesting.
Notedaddltlonal comments:
BACK TO MAIN
NumSbteurd: yGLP SuTbsetsatnce:
3M Environmental Laboratory SOLUBILITY SCREEN
TCR-006
prweSpoaarmkrsaphtlieeoenl
PFOA
IM TCR-9903030
Date:
Source: 3M Internal
Solvent: Methanol
IDR
Source:
Q Ste(cpontinuefrdopmage
1)
"Did the test substancedissolve in 2 mL? Yes/No I E , the test is complete, and thereis no needto continue with the screen
test. If NO, continue to step 3 to determine the approxim esolubility of the substance.
3 Weigh approximately10 mgf 0.5 mgof testsubstanceinto aI00 mL graduated stoppered cylinderholumetric flask.
Wseuigbhstaonfctes: t
rng
ID: Balance
op2ntidonreapl licate
mg
Thermometer ID:
2 a
DateA/Tnimalyest
Y
- Approximate Solubility(ug/mL)... 100
substance:
1
DatefrimAenalyst
-
I
I
Weight of test
I
Step M
Total volume solvent added(tnL).., I000
Approximate Solubility(ughL)... 10
Conclusions:
II present? YesMo
P " scolute Is there min
mi4
YesMtillopresent?
Solubility Scree6Test Page 2 of 2
3M ETS Laboratory
BACK TO MAIN
' GNLuPmSbteurd:y Test Substance:
3M Environmental Laboratory SOLUBlLlN SCREEN
TCR-006
Sample prwepoarkrashtieoent
PFOA
IMC:TCR-99030-30
Source: 3M Internal
Date: E rSni u
+Jb IDt#:y$Jfl
Source: f - ~ F t i ~ r n C e
ri-q'lc-
Io,- a!&[$c -()c 1 Weigh approximately 10 rng f 0.5 rng of test substance into a 2.5 rnL-4 rnL glass screw-top vial.
Weight of test substance:
2nd replicate options/:
rng Themrmg ometer
Balance ID: Ycl I 7
ID: t-hurn&/
Datellnitials$?
2 Add test solvent according to the table below, Following each addition of solvent, shake vigorouslylvortex, and sonicate
the mixture and visually check for undissolved particles.
ol..33-Q'
-P.,D
Analyst
r*.w.
data
Solubility
volume added (mLy approx conc. after addition (UslmL)
D a t f l i m e d C bI 1;55
Step 2 4
vosTaoloudltvmadelendt
(mL)... 0.1
Approximate Solubility(uglmL)... 100,000
Flask s o n i c a t e d m o Time
solution
Falamswked to settle7 @No luTtbeimislitiyng
OBSERVATiONSlNOTES
solute sYtiellsp-creosnetinntu?e
to step 2-2
e solubleIs."at IO"%in,finaintedlyis considered Is required.
\
No
DatemimAenalyst
I
\.
I
step 2-2
Totvaollume solvent added (mL)... 0.5
ApproximSaotelubility (ughL)... 20,000
Total vdume solvent added (mL)... 1
Approximate Solubility(uglmL)... 10,000
Flask sonicated?Y e a 0
0
flask vortex-mixed? YesMoRoom Temp Flasksonicated? YeslNo Time Flask allowed to settle? YeslNo Time
2 Is theresolute still present? Y e a 0 miq
min
"CsoluItsethere min
mlq
stYillepsrleNsoent?
-~
/
Conclusions:
7 Did the substance dissolvein 2 mL or less of solvent? Yes -Approximate concentrationat which the test substance is soluble insolvent: //flaaIrnl The solubility of the testsubstance is to be determined via the shake flask method. or No Continue to page two for further testing.
Notes/ additionalcomments:
BACK TO MAIN
3M Environmental Laboratory SOLUBILITYSCREEN
GLP Study Number: TCR-006
Sample preparation worksheet
SubTsetsatnce:
PFOA
ID&T C R - 9 9 0 3 0 3 0
Source: 3M Internal
Date:
Solvent: Acetone
ID&
source:
Ste(pcontinuefrdopmage
1)
-Did the test substancedissolve In 2 mL? YeslNo If YES, the test is complete, and t
test If NO, continue to step 3 to determine the approximatesolubility of the substance.
3 Weighapproximately 10 mg f 0.5 mg of test substance intoa I00 mL graduated
test
of
Weight
Datellnitiamlsg:
ID:
Balance
2nd replicateoptional:
mg
Thermometer ID:
4 Add test solvent according to the table below. Following each additioonf solvent,
the mixture and visually chefcokr undissolved patficles.
I
I
I
/
i
.- DateAlTniamlyest
-
volume added (mLy
approx cone. athr
Solubilitv data addition(WlmL) PrSepample
I
1 7 Totalvolume solvenatdded (mL)... 10 Approximate Solubility (ug/ml'
1 FiFi;;;;~~~;'YedNoTimemin Time
Total volume solvenatdded (mL)... 50
OBSERVATlONSlNOTES
- DatelTAimnaelyst
I
Step 4 3
Total volume solvent adde(mdL)... 100
Approximate Solubility(uglmL)... 100
/ Flavsokrtex-mixeYde?dRNoooTmemp
soFnlaiYcsaektseMd?o
Time
Flaskallanred to settle? Y&NToimmei9
OC 1sthere solute still present? y e a 0 mirl
5 Weigh approximate/y 10 mg f 0.5 m y f test substance into aI L graduated stoppered cylinderholumetric flasklor equivalent.
TveomrRtDeFpoYxaloa-temndssaTkiMxliymeosdet?
-
soFnlaicsakted?
Y e a 0 mTinime
Flasakllowed to settleY?edNToimmeiQ
'C 1s there soluteall p-nn y a o
L or less of solvent?
mateconcentrationatwhichthetestsubstanceissoluble
in solvent:ua/ml
The solubilityof the test substanceis to be determined via the shake flask method.
or No -The solubilityof the test substanceis to be determined viathe column elution method.
Notes/ additional comments:
Solubility Screen Test Page 2 of 2
3M ETS Laboratory