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Endpoint:
other: Amount of transformation substance extracted from a polymer
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2009
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Principles of method if other than guideline:
- Principle of test:
The method is in line with those used under Regulations for Food Contact approval. The amount of a transformation substance, perfluorohexanoic acid “PFHxA” extracted from a polymer produced from the monomer 6:2 FTA was investigated.

- Short description of test conditions
Test items
1) PFHxA - Suspension form (20% solids) of the polymer
2) Internal standard PFOA 13C4 labelled. Also called ‘surrogate compound’

0.5mL of the polymer in suspension form i.e. 20% solids and surrogate compound PFOA were added to methanol (8mL).

Target compounds were extracted by ultrasonic extraction. After centrifugation, upper phase was collected. i.e. the methanol does not dissolve the polymer but extracts the PFHxA and PFOA into the upper methanol phase.

The above extraction process was repeated on another sample of polymer suspension.

Both methanol extracts were combined.

4mL of the methanol extract solution was evaporated using N2 to concentrate it down to 1mL.

Then analysis by LC-MS/MS was carried out.

- Parameters analysed / observed:
• PFHxA quantification
• Method validation:
o Instrumental detection limit
o Method detection limit
o Recovery test
o Duplicate measurement
Specific details on test material used for the study:
"UNIDYNE TG- Polymer" is the trade name of the polymer referred to in the test reports as "S-2054"
Results:

1) Concentration of transformation substance PFHxA in sample
(From Expression 1)

Batch/sample: PFHxA (g/L):
Operation blank < 1
(1) S-2054L9601 54.4 (average of double measurement)
(2) S-2054L9602 62
(3) S-2054L9604 49

2) Instrument Detection Limit (IDL)
(From Expression 2)

IDL= 0.294 ug/L

3) Method Detection Limit (MDL)

MDL = 0.347 ug/L


4) Recovery test
Spiked amount (corresponding to a concentration in sample)
50 ug/L, Average recovery 108% (triplicate measurements)
100 ug/L, Average recovery 99.7% (triplicate measurements)

See attached full report for all raw data and tables

Conclusions:
The amounts of transformation substance PFHxA extracted from 3 batches of Polymer were: 54.4, 62 and 49 ug/L
Executive summary:

Polymer samples were extracted using methanol. The extracts were analysed by LC-MS/MS for substance PFHxA. The method was validated by standard solutions; Instrumental Detection Limit (IDL) and Method Detection limits were calculated.

Spiked samples demonstrated around 100% recovery; suggesting minimal losses from volatility.  The quantified amounts of PFHxA in the 3 batches of polymer suspension were 54.4, 62 and 49 ug/L.

 

 

For the purposes of this study’s inclusion in an updated REACH dossier under evaluation the author of the summary concludes on this method: that it will address the SEV Decision part 1.3 (ii) request in regard to the extractable amount of PFHxA from the polymers.

Endpoint:
other: amount of transformation substance in a polymer
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2009
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Principles of method if other than guideline:
-- Principle of test:
The method is in line with those used under Regulations for Food Contact approval. The amount of a transformation substance, 2-(Tridecafluorohexyl)ethanol “FTOH” present in a polymer produced from the monomer 6:2 FTA was investigated.

- Short description of test conditions:

1) Polymer was dissolved in acetone.
n-hexane used to precipitate out the polymer (“polymer was deposited”), centrifuged and the “extract solution” separated. [Sample 1]

2) FTOH reference standards made from a “master solution” of Standard reagent
[Sample 2]

3) “fortified sample for validation” from Standard reagent in acetone. Also referred to as "Spiked"
A polymer sample was added to the FTOH fortified solution to dissolve the polymer again.
n-hexane added to precipitate out the polymer again.
The sample was centrifuged and the clear extract removed [Sample 3].

4) Sample [1,2 and 3] were measured using GC-FID in triplicate


- Parameters analysed / observed:

FTOH analysed using GC-FID
Quantified and validated with standard reference substances
Specific details on test material used for the study:
"UNIDYNE TG- Polymer" is the trade name of the polymer referred to in the test reports as "S-2054"
Results:
Batch Average concentration (ug/g)
S-2054L9601A 25
S-2054L9602A 38
S-2054L9603A 42

FTOH quantitation

 

 

 

Concentration (ug/g)

RSD (%)

 

averaged

 

S-2054L9601A

 

1

25.0

25

3.2

2

26.3

3

24.8

S-2054L9602A

 

1

37.8

38

2.2

2

36.8

3

38.4

S-2054L9603A

 

1

42.1

42

0.6

2

42.4

3

41.9

 

 

 

Percent recoveries

 

 

 

Percent Recovery (%)

RSD (%)

 

averaged

 

S-2054L9601A

 

1

101

103

2.0

2

102

3

105

S-2054L9602A

 

1

97

91

6.0

2

91

3

86

S-2054L9603A

 

1

95

93

4.9

2

96

3

88

 

Conclusions:
The amounts of transformation substance FTOH in the 3 batches of Polymer were 25, 38 and 42 µg/g
Executive summary:

Polymer samples were dissolved in acetone. Following re-precipitation of the polymer the remaining solution was analysed by GC-FID for substances FTOH. The method was validated by standard solutions. Spiked samples demonstrated around 100% recovery; suggesting minimal losses from volatility.  A limit of detection for the method was not included. For the original study purpose only a target of below 50 ppm was necessary.  The quantified amounts of FTOH in the 3 batches of polymer were 25, 38 and 42 µg/g.

 

For the purposes of this study’s inclusion in an updated REACH dossier under evaluation the author of the summary concludes on this method: that it will address the SEV Decision part 1.3 (i) request in regard to the FTOH content of the polymers

Endpoint:
other: Residual monomer in a polymer
Type of information:
experimental study
Adequacy of study:
key study
Study period:
August 2006
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Principles of method if other than guideline:
- Principle of test:
The method is in line with those used under Regulations for Food Contact approval. A number of substances were analysed and measured including the amount of residual monomer of interest under this REACH evaluation, within a polymer intended for Food Contact use. The monomer is perfluorohexylethyl acrylate (6:2 FTA)

- Short description of test conditions:
Triplicate measurements
Solid polymer received on Al trays. Dissolved by acetone. Around 1g was weighed and noted and made up to 100 ml of acetone for the test solution.

- Parameters analysed / observed:
6:2 FTA analysed by GC-MS
Quantified and validated with standard reference substances
Specific details on test material used for the study:
"UNIDYNE TG- Polymer" is the trade name of the polymer referred to in the test reports as "S-2054"
Results:
Residual monomer was not detected above 100 ppm in any of the triplicate samples

Perfluorohexylethylacrylate monomer quantitation

Sample (Lab ID)

Concentration (ppm)

Target Level Provided by Client (ppm)

AD99516

Not detected

100

AD99517

Not detected

100

AD99518

Not detected

100

 

Validation/Recoveries from spiked samples

Concentration added (ug/g)

Concentration Detected (ug/g)

Recovery (%)

97.1

103

106

97.1

99.6

103

97.1

110

113

 

 

Average 107

Conclusions:
The study did not detect any residual perfluorohexylethylacrylate monomer in polymer samples at levels greater than 100 ppm
Executive summary:

Polymer samples were dissolved in acetone and analysed by GC-MS for substances including residual monomer.  The method was validated by standard solutions. Spiked samples demonstrated around 100% recovery.  A formal limit of detection method was not included but for the original study a target amount of less than 100 ppm was of interest and the method was designed such that the results can concluded that there was no monomer detected at >100 ppm.  

 

For the purposes of this study’s inclusion in an updated REACH dossier under evaluation the author of the summary concludes on this method: that it will address the SEV Decision part 1.3 (i) request in regard to the 6:2 FTA monomer content of the polymers.

Description of key information

Three existing studies were available on the amounts of 6:2 FTA monomer and transformation substances FTOH and PFHxA there were either present or extracted from polymers.  The existing studies had been conducted for use in Food Contact Approvals for the polymer in 2009.

 

The studies are relevant for use in response to SEV final decision 11 February 2019 parts 1.3 (i and ii).  Although they were not conducted to any international standard the methodology is sound and they report ‘sufficient experimental details’.  The concern of volatility of some of the substances has been addressed by including recovery tests in all three studies; they are all around 100%.

 

For  6:2 FTA monomer and transformation substance FTOH the studies quantify the amount in the polymer (ref. 1.3 (i)) and for transformation substance PFHxA, the amount extracted from the polymer (ref. 1.3 (ii)).  The results of these studies are also relevant to SEV Decision part 1.3 (iii) determining if a risk assessment is required.  See summary table below.

 

Substance

Amount in Polymer

Implication on 1.3 part (iii)

Monomer 6:2 FTA

 

None detected at

> 100ug/g.

Since releases cannot be confirmed or otherwise at lower than 100ug/g, a Tier 1 risk assessment will be carried out

Transformation substance FTOH

 

25 ug/g

38 ug/g

42 ug/g

A risk assessment based on  worst case value obtained in (i) will be used as the release

Transformation substance PFHxA

54.4 ug/L

62 ug/L

49 ug/L

A risk assessment will be carried out using value obtained under (ii)

 

Additional information

Please see file attachment point in end point record "monomer 6:2 FTA in polymer (NFL 2009)" for a Presentation file summary of the registrant's approach in response to the SEV part 1.3 requests.