Registration Dossier

Environmental fate & pathways

Hydrolysis

Currently viewing:

Administrative data

Link to relevant study record(s)

Reference
Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2010-10-04 to 2010-11-03
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results. The study report was conclusive, done to a valid guideline and the study was conducted under GLP conditions.
Qualifier:
according to guideline
Guideline:
EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Specific details on test material used for the study:
- Name as cited in study report: POPDa
- Color: clear, colorless
- Purity: 94%
- Lot/Batch number: LL100365
- Label: Jeffamine D-230 lot no.: LL 100365
- Date received: 2010-09-21
- Storage: in the dark
Radiolabelling:
no
Analytical monitoring:
yes
Details on sampling:

Preparation of samples: Sample solutions were prepared in stoppered glass flasks at a nominal concentration of 2 g/l in the three buffer solutions. The test solutions were split into individual vessels for each data point. The solutions were shielded from light whilst maintained at the test temperature.

Preliminary test/Tier 1: Sample solutions at pH 4 were maintained at 50.0 ± 0.5°C for a period of 147 hours. Sample solutions at pH 7 and 9 were maintained at 50.0 ± 0.5°C for a period of 121 hours.

Analysis of sample solutions: The sample solutions were taken from the water bath at various times and the pH of each solution recorded.
The concentration of the sample solution was determined by gas chromatography (GC).

Samples: To duplicate aliquots (A and B, 5 ml), 0.1 ml of diethylamine and approximately 0.5 g sodium chloride were added. The solutions were extracted with three portions (3 x 10 ml) of dichloromethane. The combined extracts were diluted to 50 ml using dichloromethane.

Standards: Duplicate standard solutions of test item were prepared in dichloromethane at a nominal concentration of 400 mg/l.

Matrix blanks: An aliquot (5 ml) of relevant buffer solution was treated as per a sample.
Buffers:
Specification of buffer solutions

Buffer Solution (pH) Components Concentration
(mol dm-3)
4 Potassium hydrogen phthalate 0.05
7 Disodium hydrogen orthophosphate (anhydrous) 0.03
Potassium dihydrogen orthophosphate 0.02
Sodium chloride 0.02
9 Disodium tetraborate 0.01
Sodium chloride 0.02
The buffer solutions were filtered through a 0.2 µm membrane filter to ensure they were sterile before commencement of the test. Also these solutions were subjected to ultrasonication and degassing with nitrogen to minimise dissolved oxygen content.
Details on test conditions:
Refer to details on sampling and analytical methods.
Duration:
121 h
pH:
4
Initial conc. measured:
ca. 2 g/L
Duration:
121 h
pH:
7
Initial conc. measured:
ca. 2 g/L
Duration:
121 h
pH:
9
Initial conc. measured:
ca. 2 g/L
Number of replicates:
Duplicate aliquots of sample were taken for analysis.
Positive controls:
no
Negative controls:
no
Preliminary study:
Preliminary test/Tier 1
The mean peak areas relating to the standard and sample solutions are shown in tables. (please see remarks on results including tables and figures section).
The test item concentrations at the given time points at pH 4, 7 and 9 are shown in tables: (please see remarks on results including tables and figures section).
Test performance:
Validation:
The linearity of the detector response with respect to concentration was assessed over the nominal concentration range of 0 to 1.6 x 103 mg/l. This was satisfactory with correlation coefficients of 1.000 being obtained for Peak No.1, 2 and 3, and 0.998 for Peak No.4.
Recovery of analysis of the sample procedure was assessed and proved adequate for the test. Recovery data is shown in the following table:( please see remarks on results including tables and figures section)
Transformation products:
not specified
Details on hydrolysis and appearance of transformation product(s):
Less than 10% hydrolysis after 121 hours at 50°C.
Key result
pH:
4
Temp.:
25 °C
DT50:
1 yr
Type:
not specified
Key result
pH:
7
Temp.:
25 °C
DT50:
1 yr
Type:
not specified
Key result
pH:
9
Temp.:
25 °C
DT50:
1 yr
Type:
not specified
Details on results:
At pH4, 7 and 9 there was less than 10% hydrolysis after 121 hours at 50°C, equivalent to a half-life greater than 1 year at 25°C.

Preliminary test/Tier 1

The mean peak areas relating to the standard and sample solutions are shown in the following table:

Solution

MeanArea

Peak No.1

Peak No.2

Peak No.3

Peak No.4

Standard 394 mg/l

5.201 x 105

4.048 x 105

1.384 x 105

3.047 x 104

Standard 398 mg/l

5.032 x 105

3.903 x 105

1.326 x 105

2.930 x 104

Initial Sample A, pH 4

1.203 x 105

1.586 x 105

5.933 x 104

1.233 x 104

Initial Sample B, pH 4

6.064 x 105

1.080 x 105

5.179 x 104

1.155 x 104

Initial Sample A, pH 7

1.562 x 105

1.677 x 105

5.612 x 104

1.016 x 104

Initial Sample B, pH 7

1.531 x 105

1.690 x 105

5.760 x 104

1.148 x 104

Initial Sample A, pH 9

1.583 x 105

1.727 x 105

5.780 x 104

1.173 x 104

Initial Sample B, pH 9

1.598 x 105

1.687 x 105

5.576 x 104

1.139 x 104

Standard 422 mg/l

5.259 x 105

4.097 x 105

1.395 x 105

3.052 x 104

Standard 488 mg/l

6.153 x 105

4.804 x 105

1.660 x 105

3.703 x 104

22-Hour Sample A, pH 4

1.419 x 105

1.635 x 105

5.756 x 104

1.141 x 104

22-Hour Sample B, pH 4

1.366 x 105

1.617 x 105

5.708 x 104

1.112 x 104

22-Hour Sample A, pH 7

1.647 x 105

1.678 x 105

5.556 x 104

1.072 x 104

22-Hour Sample B, pH 7

1.640 x 105

1.668 x 105

5.578 x 104

1.126 x 104

22-Hour Sample A, pH 9

1.547 x 105

1.608 x 105

5.421 x 104

1.119 x 104

22-Hour Sample B, pH 9

1.637 x 105

1.687 x 105

5.533 x 104

1.143 x 104

Standard 392 mg/l

4.719 x 105

3.697 x 105

1.247 x 105

2.624x 104

Standard 396 mg/l

4.680 x 105

3.661 x 105

1.241 x 105

2.712 x 104

96-Hour Sample A, pH 4

1.361 x 105

1.430 x 105

5.260 x 104

1.034 x 104

96-Hour Sample B, pH 4

1.335 x 105

1.429 x 105

5.514 x 104

1.063 x 104

96-Hour Sample A, pH 7

1.191 x 105

1.294 x 105

5.045 x 104

8.925 x 103

96-Hour Sample B, pH 7

1.471 x 105

1.383 x 105

5.198 x 104

8.847 x 103

96-Hour Sample A, pH 9

1.425 x 105

1.298 x 105

5.162 x 104

8.417 x 103

96-Hour Sample B, pH 9

1.533 x 105

1.410 x 105

5.302 x 104

9.269 x 103

 

Solution

MeanArea

Peak No.1

Peak No.2

Peak No.3

Peak No.4

Standard 392 mg/l

4.725 x 105

3.703 x 105

1.248 x 105

2.636 x 104

Standard 396 mg/l

4.681 x 105

3.655 x 105

1.234 x 105

2.690 x 104

121-Hour Sample A, pH 4

1.416 x 105

1.656 x 105

5.820 x 104

1.132 x 104

121-Hour Sample B, pH 4

1.400 x 105

1.666 x 105

5.807 x 104

1.100 x 104

121-Hour Sample A, pH 7

1.472 x 105

1.601 x 105

5.520 x 104

1.102 x 104

121-Hour Sample B, pH 7

1.475 x 105

1.650 x 105

5.409 x 104

1.043 x 104

121-Hour Sample A, pH 9

1.508 x 105

1.593 x 105

5.388 x 104

1.071 x 104

121-Hour Sample B, pH 9

1.450 x 105

1.621 x 105

5.529 x 104

1.104 x 104

Standard 481 mg/l

5.978 x 105

4.659 x 105

1.579 x 105

3.376 x 104

Standard 434 mg/l

5.507 x 105

4.300 x 105

1.469 x 105

3.158 x 104

147-Hour Sample A, pH 4

1.415 x 105

1.620 x 105

5.669 x 104

1.076 x 104

147-Hour Sample B, pH 4

1.295 x 105

1.574 x 105

5.891 x 104

1.142 x 104

 

 


The test item concentrations at the given time points at pH 4 are shown in the following tables:

pH 4 at 50.0 ± 0.5ºC ¿ Peak No.1

Time (Hours)

Mean Concentration (g/l)

% of mean 22-Hour concentration

A

B

A

B

0

0.932

0.470

-

-

22

1.13

1.09

-

-

96

1.14

1.12

103

101

121

1.19

1.17

107

106

147

1.13

1.03

101

92.9

pH 4 at 50.0 ± 0.5ºC ¿ Peak No.2

Time (Hours)

Mean Concentration (g/l)

% of mean 22-Hour concentration

A

B

A

B

0

1.58

1.08

-

-

22

1.67

1.65

-

-

96

1.53

1.53

92.1

92.1

121

1.78

1.79

107

107

147

1.65

1.61

99.4

96.6

pH 4 at 50.0 ± 0.5ºC ¿ Peak No.3

Time (Hours)

Mean Concentration (g/l)

% of mean initial concentration

A

B

A

B

0

1.75

1.52

-

-

22

1.72

1.70

106

105

96

1.67

1.75

103

108

121

1.85

1.85

114

114

147

1.70

1.77

105

109

pH 4 at 50.0 ± 0.5ºC ¿ Peak No.4

Time (Hours)

Mean Concentration (g/l)

% of mean initial concentration

A

B

A

B

0

1.64

1.53

-

-

22

1.54

1.50

97.3

94.8

96

1.53

1.57

96.5

99.2

121

1.68

1.63

106

103

147

1.51

1.60

95.1

101

Result:         Less than 10% hydrolysis after at least 125 hours at 50°C, equivalent to a half-life greater than 1 year at 25°C.

The test item concentrations at the given time points at pH 7 are shown in the following tables:

pH 7 at 50.0 ± 0.5ºC ¿ Peak No.1

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.21

1.19

-

-

22

1.31

1.31

110

109

96

0.999

1.23

83.4

103

121

1.23

1.24

103

103

pH 7 at 50.0 ± 0.5ºC ¿ Peak No.2

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.67

1.69

-

-

22

1.72

1.71

102

102

96

1.39

1.48

82.6

88.3

121

1.72

1.77

102

105

pH 7 at 50.0 ± 0.5ºC ¿ Peak No.3

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.64

1.69

-

-

22

1.66

1.66

99.6

100

96

1.60

1.65

96.2

99.1

121

1.75

1.72

105

103

pH 7 at 50.0 ± 0.5ºC ¿ Peak No.4

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.47

1.52

-

-

22

1.45

1.52

96.8

102

96

1.32

1.31

88.3

87.5

121

1.63

1.54

109

103

Result:         Less than 10% hydrolysis after 121 hours at 50°C, equivalent to a half-life greater than 1 year at 25°C.


The test item concentrations at the given time points at pH 9 are shown in the following tables:

pH 9 at 50.0 ± 0.5ºC ¿ Peak No.1

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.23

1.24

-

-

22

1.23

1.31

100

106

96

1.20

1.29

97.1

104

121

1.26

1.22

103

98.7

 pH 9 at 50.0 ± 0.5ºC ¿ Peak No.2

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.72

1.68

-

-

22

1.64

1.73

96.6

101

96

1.39

1.51

81.8

88.8

121

1.71

1.74

100

102

pH 9 at 50.0 ± 0.5ºC ¿ Peak No.3

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.69

1.63

-

-

22

1.62

1.65

97.3

99.3

96

1.64

1.68

98.5

101

121

1.71

1.76

103

106

pH 9 at 50.0 ± 0.5ºC ¿ Peak No.4

Time (Hours)

MeanArea

% of mean initial peak area

A

B

A

B

0

1.56

1.51

-

-

22

1.51

1.54

98.5

101

96

1.24

1.37

81.2

89.4

121

1.59

1.64

103

107

Result:         Less than 10% hydrolysis after 121 hours at 50°C, equivalent to a half-life greater than 1 year at 25°C.

Validity criteria fulfilled:
yes
Remarks:
See test performance - remarks
Conclusions:
The test item was determined to be hydrolytically stable at pH 4, 7 and 9, with estimated half-lives of greater than 1 year at 25°C.
Executive summary:

Assessment of hydrolytic stability was carried out using a procedure designed to be compatible with Method C7 Abiotic Degradation, Hydrolysis as a Function of pH of Commission Regulation (EC) No 440/2008 of 30 May 2008.

The test item was determined to be hydrolytically stable at pH 4, 7 and 9, with estimated half-lives of greater than 1 year at 25°C. 

Description of key information

A test was conducted following EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH; Butler & White, 2010). The substance is hydrolytically stable at all pH's.

Key value for chemical safety assessment

Half-life for hydrolysis:
1 yr
at the temperature of:
25 °C

Additional information