3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 1 of 9 

Final Report 

Water Solubility of 

Laboratory Project ID: 

Method or Regulatory Requirement: Non-GLP 

Testing Laboratory 

3M Environmental Health and Safety Operations 

3M Environmental Laboratory 

3M Environmental Laboratory 

Cleston Lange, Ph.D. 

3M Environmental Health and Safety Operations 

3M Environmental Laboratory 

3M Center, Bldg 260-5N-17 

St. Paul, MN 55144 

Phone: 651-733-9860 

clange@mmm.com

Client 

Jeff Stolte 

3M Materials Resource Division 

 3M Center, Bldg 236-1B-10 

St. Paul, MN 55144 

Phone: 651-575-0856 

jstolte@mmm.com
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 2 of 9 

1 Introduction/Summary 

The fluorinated polyurethane test substance 

 was received in February 19, 2015 from 3M Materials 

Resource Division (MRD) for evaluating its water solubility at ambient room 

temperature via limit testing using a modified shake flask procedure. The test 

substance properties are described in Table 1. 

The material was anticipated to be practically insoluble in water; therefore, 

solubility testing was performed as a limit test and conducted to evaluate 

whether a nominal 1 mg visible sample (actual 1.02 mg) would dissolve in 18 L 

of Mill-QTM water during > 24 hours at ambient temperature (22 + 1 °C) with 

gentle stirring. After the incubation, the glass vial was retrieved and the water 

decanted off and the recovered solids air dried. The air-dried sample was 

visibly examined for the presence non-solubilized test substance and 

photographed. Then the substance was dissolved into 0.5 mL acetone, 

transferred to a pre-weighed aluminum dish and acetone evaporated away 

and the sample air dried at ambient temperature, then accurate weight of 

recovered residue determined. 

Results showed that 1.02 mg of solid was recovered at 77% after a 

44 hour solubility test period in 18 L water. Visual results recorded via 

photography added a second level of confirmation that the test substance did 

not significantly dissolve in the water. The results demonstrate that the water 

solubility of is significantly less than nominal 0.057 mg/L (< 57 ppb). 

 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 3 of 9 

2 Experimental & Analytical 

2.1.1 Test Substance 

The test substance is the dried fluorinated polyurethane 

. The substance was referred to as dried solids and 

identified as dried solids. 

Table 1. Test Substance

Substance ID 

Alternative Name dried solids, 

urethane 

Source 3M 

Received Date 2/19/2015 

Expiration Date 2/25/2020 

Storage Frozen 

TCR No. 

Physical Description solid 

Purity 97.4% 

2.1.2 Laboratory Equipment 

Laboratory temperature was recorded as facility data using a REES 

temperature monitoring system and calibrated thermocouples. The 

temperature of the laboratory where water solubility testing was conducted 

was maintained at within 22 + 1 °C between March 24 and March 26, 2015. 

2.1.3 Balance 

Mettler Toledo 

SAG285 SemiMicro Balance 

SN: 1120370839 

3M Metrology ID: 148930 

LIMS ID: BAL ROBOT 

Functional Range 0.1 mg to 210 g 

Repeatability: 0.1 mg 

Linearity: + 0.2 mg 

Note: The balance was verified accurate to 1.0 mg using a 1.0 

mg calibrated weight, the smallest calibration verification weight 

available at the time. Readings below 1 mg were assumed 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 4 of 9 

accurate based on the accuracy of the 1 mg weight and a stable 

tare reading at 0.00 mg. Precision was demonstrated in the 

range of 0.5 to 1.0 mg by repeated measurements of a aluminum 

foil weight prepared at nominal 0.6 mg, as discussed herein. 

2.1.4 Calibration Verification Weight Set 

ID: 0222-8007 

Class F Weight Set (1.00 mg-100 g) 

Serial Number: 7937 

3M Metrology ID: 161204 

2.1.5 Milli-Q® Element DI Water System 

Millipore 

Provides ASTM type-1 water 

3M Metrology ID: 161236

2.1.6 Camera 

Fujifilm FinePixTM S9000 Digital Camera 

28-300 mm, 10.7X optical zoom 

Serial Number: 61A51564 

2.1.7 Solubility Test 

The test substance was provided as a solid substance in February 19, 

2015. The solubility testing was conducted in March 2015. Estimation of water 

solubility was conducted per a modification of the “Preliminary Test” procedure 

described in OECD-105. These modifications were performed to enhance the 

outcome of the evaluation by providing a water solubility value that is in the low 

part per billion (μg/L) concentration range. Due to the anticipated poor solubility of 

the test substance at less than nominal 1 mg/L (< 1 ppm) and lack of reliable 

analytical methods to quantify the polymers at low ppm or ppb levels, the following 

procedure was performed to provide a water solubility limit based on visual 

observation of significant non-solubilized material remaining after being placed in a 

large volume of water (18 liters) for > 24 hours. Below is a detailed description of 

the test, as performed: 

Step 1: An optically clear glass ~ 20 mL I-CHEM® vial had its weight 

determined and then was tared on a 5-place balance.

Step 2: On 3/24/2015 a visible and measurable quantity of 

dried solids was accurately weighed into the bottom of a tared clear 

glass vial and recorded as 1.02 mg. A photograph was taken as a 

record of the visibility of the material before dissolution testing. A 

laboratory control sample was similarly prepared with 1.05 mg of test 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO.

Water Solubility of 

Page 5 of 9 

substance, but not exposed to water solubility testing and was retained 

for later stages of the testing. For each, the test substance was gently 

heated to adhere it to the bottom of the vial. 

Step 3: The vial with 1.02 mg of test substance was then filled with MilliQTM water and carefully submerged into the final test volume of water 

(18L) contained in a 5 gallon HDPE pail. A magnetic stir bar was 

placed in the bottom and used for gentle stirring during the incubation 

using a magnetic stir plate. 

Step 4: The solubility test was conducted from 2:45 PM on March 24, 

2015 until 10:45AM on March 26, 2015 (44hrs,). The temperature of 

the ambient room air was recorded at 22°C+ 1°C during the water 

solubility experiment and assumed equal to the water temperature at 

the end of the experiment. 

Step 5: After the incubation period. The vial was carefully recovered 

and inspected for any visible, non-solubilized test substance. The test 

substance was visibly present as a disintegrated powder in the vial. 

The water phase was then carefully decanted off and the recovered 

solids air dried at ambient temperature and photographed. 

Step 6: The air-dried solids of the test sample and control sample were 

then dissolved into 0.5 mL acetone and transferred to a pre-weighed 

aluminum weigh boat. The acetone was evaporated away and the final 

recovered mass of accurately determined and recorded on 

4/2/2015. 

A maximal solubility value was determined based the initial weight divided by 

the volume of water tested. For example, visible remaining material after 

dissolution testing for a 1.02 mg weight of test substance tested in 18 L water 

would result in a reported water solubility of less than 1.02 mg÷18 L (i.e. < 

0.057 mg/L; < 57 ppb). Because solid non-dissolved material was recovered, 

the actual water solubility is confidently expected to be significantly less than 

this value. 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO.

Water Solubility of 

Page 6 of 9 

2.1.8 Quality Controls 

2.1.9 Laboratory Control Samples 

A 1.05 mg aliquot of the test substance was accurately weighed into a clean clear 

I-CHEM® vial. The material was then air dried similar to the water solubility 

sample at ambient temperature. The results of LCSs were used to demonstrate 

no loss of test substance due to the drying process and to demonstrate accurate 

recovery of the substance via the drying procedures. The results of the LCS are 

shown in Table 3. 

2.1.10 Precision Evaluations 

A small piece of aluminum foil (nominal mass 0.6 mg) was prepared as a 

precision evaluation weight. This precision weight was weighed 10 times prior 

to each balance use to validate the balance precision between 1 mg and 0.5 

mg. The results determined for two different days of weight determination are 

shown in Table 4. 

3 Results 

3.1.1 Balance Calibration Verification Results 

Calibration verification of the balance was performed following ETS-9-006 “Use of 

Analytical Balances” using a 1 mg verification weight and demonstrated at within 

100% + 5% accuracy. 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 7 of 9 

3.1.2 Solubility Test Sample Results 

Recovery of Test Substance from the solubility test samples is shown in Table 2. 

3.1.3 Photographic (Visual) Results 

Photographs of the test substance were taken before and after the solubility 

test and are shown in Figure 1. The loss of the test substance was not 

observed. Slight changes in the color from yellow-tinted to white were 

observed, indicating potential loss of colored impurities during the solubility 

testing. The substance also appeared to disintegrate during the incubation 

period, originally starting as a single flake of material and ending as 

several small pieces and powdered substance after solubility testing.

Figure 1. before (left) and after (right) the solubility test. 

Table 2. Test Substance Recovery from Solubility Testing

Substance ID Original Mass (mg) [a] Recovered Mass (mg) Percent 

Recovery [a]

 1.02 0.79 77% 

[a] Values shown at 2 significant figures due to variability at the 0.01 mg position, however 

recoveries were determined using full precision 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 8 of 9 

3.1.4 Laboratory Control Sample Results 

A laboratory control sample was prepared by weighing 1.05 mg into a 

clean I-CHEM® vial, but not exposed to the water solubility testing. The control 

sample was dried in parallel to the water solubility test sample. Percent recovery 

of the dried laboratory control samples are reported in Table 3. 

To evaluate the precision of the balance in the mass range used, a sliver of 

aluminum foil was cut and weighed 10 times prior to weight determination on 

3/24/2015 (initial weight determinations) and prior to weight determinations on 

4/2/2015 (final recovered weight determinations). The average (+std. dev.) 

determined mass was 0.582 + 0.084 mg (RSD 14%), on 3/24/2015 and 0.63 

+0.048 mg (RSD 7.6%) on 4/2/2014. Results are shown in Table 4.

Table 3. Laboratory Control Sample Recovery

Substance ID Original Mass (mg) Recovered Mass (mg) Percent 

Recovery [a]

control 1.05 0.980 93% 

[a] Values shown at 2 significant figures due to variability at the 0.01 mg position, however 

recoveries were determined using full precision 

Table 4. Balance Precision (1.0 to 0.5 mg mass range)

Substance ID Determined Masses on 

3/24/2015 (mg) 

Determined Masses 

on 4/2/2015 (mg) 

Measurement 1 0.56 0.56 

Measurement 2 0.54 0.67 

Measurement 3 0.57 0.68 

Measurement 4 0.74 0.57 

Measurement 5 0.48 0.58 

Measurement 6 0.54 0.59 

Measurement 7 0.55 0.64 

Measurement 8 0.50 0.65 

Measurement 9 0.68 0.66 

Measurement 10 0.66 0.68 

AVERAGE 0.58 0.63 

STD. DEVIATION 0.084 0.048 

RSD 14% 7.6% 
3M ENVIRONMENTAL LABORATORY 

PROJECT NO. 

Water Solubility of 

Page 9 of 9 

4 Conclusion 

The solubility of the test substance 

was investigated through limit testing using a modified shake flask 

procedure. These results were determined empirically through weighing of 

sample before and after solubility testing as well as visually recording via 

photographs. 

The water solubility of was determined to be negligible and less than 

0.057 mg/L (< 57 ppb) at 22°C + 1°C. The percent recovery of test material 

during dissolution testing was 77% by mass. The recovery of the laboratory 

control sample was 93%. Precision of the analytical method was good based 

on repeat measurement of a control weight at between 1 mg and 0.5 mg, with 

an RSD of < 15% (n = 10). 

5 Data/Sample Retention 

Data and samples will be retained according the 3M Environmental Laboratory 

SOPs. Data will be maintained and archived within a study file identified as 

study . It is anticipated that the raw samples and the data files will 

be retained indefinitely. 

6 Approval Signatures 

The following persons have reviewed and approved this report: 

Cleston C. Lange, Ph.D. Project Lead Date 

William K. Reagen, Ph.D., Technical Director Date

The 3M Environmental Laboratory’s Quality Assurance Unit has audited the data 

and report for this project. 

Quality Assurance Unit Representative Date 

Digitally signed by Cleston C. Lange 

DN: c=US, st=MN, l=St. Paul, ou=3M Environmental Laboratory - authenticated 

by LRA, email=clange@mmm.com, o=3M, cn=Cleston C. Lange 

Reason: I am the author of this document 

Date: 2015.04.30 08:28:33 -05'00'

Digitally signed by William K. Reagen 

DN: c=US, st=MN, l=St. Paul, ou=Laboratory Director, ou=3M Environmental Laboratory - 

authenticated by LRA, email=wkreagen@mmm.com, o=3M, cn=William K. Reagen 

Reason: I am approving this document 

Date: 2015.04.30 08:48:24 -05'00'

Digitally signed by Daryl K. Peterson 

DN: c=US, st=MN, l=St. Paul, ou=3M Environmental Laboratory - authenticated by LRA, 

email=dpeterson2@mmm.com, o=3M, cn=Daryl K. Peterson 

Reason: I have reviewed this document 

Date: 2015.04.30 09:22:27 -05'00'