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Environmental fate & pathways

Hydrolysis

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Reference
Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2015-11-26 to 2016-03-04
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study performed according to standard test guidelines (OECD, EC) and conform GLP requirements. The temperature variation (0.8°C) of the stove (19.8°C) fell outside the criterion (0.5°C) in the main study. Nevertheless, the data points in the plots of the logarithms of relative concentration against time at 20°C are all on a straight line. The results of the study can be considered reliable without restrictions.
Qualifier:
according to
Guideline:
OECD Guideline 111 (Hydrolysis as a Function of pH)
Deviations:
yes
Remarks:
in the main study, the temperature variation (0.8°C) of the stove (20°C) fell outside the criterion (0.5°C)
Qualifier:
according to
Guideline:
EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH)
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 835.2120 (Hydrolysis of Parent and Degradates as a Function of pH at 25°C)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source and lot/batch No. of test material: A14JB3442
- Expiration date of the lot/batch: 2016-09-30 (retest date)
- Purity test date: 2015-02-18

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: at room temperature
- Stability under test conditions: stable

Radiolabelling:
no
Analytical monitoring:
yes
Details on sampling:
- Sampling intervals for the parent/transformation products:
* Tier 1: at the beginning and after 120 hours
* Tier 2: at the beginning and at several sampling points after t=0
- Sampling method:
* Tier 1: Concentration of the test item in the test sample was determined immediately after preparation. The samples taken at t=5 days were cooled to room temperature using running tap water. The samples were diluted in a 3:1 (v:v) ratio with methanol and analysed.
* Tier 2: The sample not analysed on the sampling day were stored in the freezer. On the day of analysis, the frozen samples were defrosted at room temperature, treated and analysed.
- Sampling methods for the volatile compounds, if any: not applicable
- Sampling intervals/times for pH measurements: the pH of each test solutions was determined at least at the beginning and at the end of the test.
- Sampling intervals/times for sterility check: not applicable
- Sample storage conditions before analysis: not applicable
- Other observation, if any: no data
Buffers:
- pH:
* Tier 1: 4.0, 7.0, and 9.0
* Tier 2: 4.0, 7.0, and 9.0
- Type, final molarity and composition of buffer:
* buffer pH 4: solution of 16.7% 0.01 M sodium acetate in water and 83.3% 0.01 M acetic acid in water. The buffer contains 0.0009% (w/v) sodium azide
* buffer pH 7: solution of 0.01 M potassium di-hydrogenophosphate in water adjusted to pH 7 using 1 N sodium hydroxide. The buffer contains 0.0009% (w/v) sodium azide.
* buffer pH 9: solution of boric acid in water and 0.01 M potassium chloride in water adjusted to pH 9 using 1 N sodium hydroxide. The buffer contains 0.0009% (w/v) sodium azide.

Details on test conditions:
TEST SYSTEM
- Type, material and volume of test flasks, other equipment used: sterile vessel
- Sterilisation method: the buffer solutions were filter-sterilised through a 0.2 µm FP 30/0.2 CA-S filter (Wathman, Dassel, Germany) and transferred into a sterile vessel.
- Lighting: in the dark
- Measures taken to avoid photolytic effects: vessels placed in the dark
- Measures to exclude oxygen: Nitrogen was passed through the buffer solutions for about 5 minutes.
- Details on test procedure for unstable compounds: no data
- Details of traps for volatile, if any: not applicable
- If no traps were used, is the test system closed/open: under vacuum
- Is there any indication of the test material adsorbing to the walls of the test apparatus? no

TEST MEDIUM
- Volume used/treatment: 6 mL
- Kind and purity of water: Milli-Q
- Preparation of test medium: The test item was spiked to the solutions at a targetconcentration of 5 mg/L using a spiking solution in methanol.
- Renewal of test solution: not applicable
- Identity and concentration of co-solvent: not applicable

OTHER TEST CONDITIONS
- Adjustment of pH: no
- Dissolved oxygen: no data
Duration:
120 h
pH:
4
Temp.:
50 °C
Initial conc. measured:
5.03 - 5.04 mg/L
Duration:
120 h
pH:
7
Temp.:
50 °C
Initial conc. measured:
5.03 - 5.03 mg/L
Duration:
120 h
pH:
9
Temp.:
50 °C
Initial conc. measured:
5.02 - 5.05 mg/L
Duration:
725.5 h
pH:
4
Temp.:
20 °C
Initial conc. measured:
5.06 - 5.07 mg/L
Duration:
504.12 h
pH:
4
Temp.:
50 °C
Initial conc. measured:
5.05 - 5.06 mg/L
Duration:
165.62 h
pH:
4
Temp.:
60 °C
Initial conc. measured:
5.09 - 5.1 mg/L
Duration:
725.25 h
pH:
7
Temp.:
20 °C
Initial conc. measured:
5.03 - 5.04 mg/L
Duration:
503.78 h
pH:
7
Temp.:
50 °C
Initial conc. measured:
5.01 - 5.02 mg/L
Duration:
165.37 h
pH:
7
Temp.:
60 °C
Initial conc. measured:
4.97 - 4.99 mg/L
Duration:
725 h
pH:
9
Temp.:
20 °C
Initial conc. measured:
5.03 - 5.03 mg/L
Duration:
428.42 h
pH:
9
Temp.:
50 °C
Initial conc. measured:
5.06 - 5.06 mg/L
Duration:
165.12 h
pH:
9
Temp.:
60 °C
Initial conc. measured:
5.05 - 5.06 mg/L
Number of replicates:
2
Positive controls:
no
Negative controls:
no
Statistical methods:
no data
Preliminary study:
The preliminary hydrolysis tests were performed at 50°C at pH 4.0, pH 7.0 and pH 9.0. Aliquots of each test solution were analyzed at the beginning and after 120 hours. Further hydrolysis tests were performed at 20°C, 50°C and 60°C in the buffered test solution at pH 4.0, due to the instability of the test item found in the preliminary test at 50°C.
Transformation products:
not measured
% Recovery:
101
pH:
4
Temp.:
50.2 °C
Duration:
5 d
% Recovery:
101
pH:
7
Temp.:
50.2 °C
Duration:
5 d
% Recovery:
101
pH:
9
Temp.:
50.2 °C
Duration:
5 d
% Recovery:
101
pH:
4
Temp.:
20 °C
Duration:
725.5 h
% Recovery:
101
pH:
4
Temp.:
50 °C
Duration:
504.12 h
% Recovery:
102
pH:
4
Temp.:
60 °C
Duration:
165.62 h
% Recovery:
101
pH:
7
Temp.:
20 °C
Duration:
725.25 h
% Recovery:
100
pH:
7
Temp.:
50 °C
Duration:
503.78 h
% Recovery:
100
pH:
7
Temp.:
60 °C
Duration:
165.37 h
% Recovery:
101
pH:
9
Temp.:
20 °C
Duration:
725 h
% Recovery:
101
pH:
9
Temp.:
50 °C
Duration:
428.42 h
% Recovery:
101
pH:
9
Temp.:
60 °C
Duration:
165.12 h
pH:
4
Temp.:
20 °C
DT50:
343 d
Type:
(pseudo-)first order (= half-life)
pH:
4
Temp.:
25 °C
DT50:
165 d
Type:
(pseudo-)first order (= half-life)
pH:
4
Temp.:
50 °C
DT50:
144 h
Type:
(pseudo-)first order (= half-life)
pH:
7
Temp.:
20 °C
DT50:
575 d
Type:
(pseudo-)first order (= half-life)
pH:
4
Temp.:
60 °C
DT50:
40 h
Type:
(pseudo-)first order (= half-life)
pH:
7
Temp.:
25 °C
DT50:
251 d
Type:
(pseudo-)first order (= half-life)
pH:
7
Temp.:
50 °C
DT50:
142 h
Type:
(pseudo-)first order (= half-life)
pH:
7
Temp.:
60 °C
DT50:
40 h
Type:
(pseudo-)first order (= half-life)
pH:
9
Temp.:
20 °C
DT50:
494 d
Type:
(pseudo-)first order (= half-life)
pH:
9
Temp.:
25 °C
DT50:
217 d
Type:
(pseudo-)first order (= half-life)
pH:
9
Temp.:
50 °C
DT50:
125 h
Type:
(pseudo-)first order (= half-life)
pH:
9
Temp.:
60 °C
DT50:
34 h
Type:
(pseudo-)first order (= half-life)
Validity criteria fulfilled:
yes
Conclusions:
T001036 was found to be not hydrolytically stable at pH 4.0, pH 7.0 and pH 9.0, therefore further testing was performed. Additional testing determined a half-life time of 165 days at 25°C for pH 4.0, a half time of 251 days at 25°C for pH 7.0 and a half life of 217 days at 25°C for pH 9.0. The results of the test can be considered reliable without restriction.

Description of key information

One study (Brekelmans, 2016) was performed according to the OECD guideline 111 and regarded as a key study (Klimisch score of 1).    
A preliminary test was performed at 50°C at each pH of pH 4.0, 7.0 and 9.0. As the test item was found not to be stable according to the criteria given in the guideline, a main test was performed at pH 4, 7 and 9 at three different temperatures (20, 50 and 60 °C). The mean recoveries of the test item containing buffer solutions at t=0 fell within the criterion range of 90-110% at pH 4, 7 and 9. It demonstrated that the analytical method was adequate to support the hydrolysis study on the test item. A half-life time of 251 days at 25 °C and pH 7 was determined for T001036

Key value for chemical safety assessment

Half-life for hydrolysis:
251 d
at the temperature of:
25 °C

Additional information