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Diss Factsheets

Administrative data

Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
1999-01-29 until 1999-03-02
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: Guideline-conform study under GLP. Minor restrictions, such as no validity criteria for the study are given, and no details on transformation products reported.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
1999
Report date:
1999

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH)
Deviations:
no
GLP compliance:
yes

Test material

Constituent 1
Chemical structure
Reference substance name:
-
EC Number:
431-060-1
EC Name:
-
Cas Number:
153719-38-1
Molecular formula:
Hill formula: C4H8N4O3 CAS formula: C4H8N4O3
IUPAC Name:
3-methyl-N-nitro-3,6-dihydro-2H-1,3,5-oxadiazin-4-amine
Details on test material:
- Name of test material (as cited in study report): CA 2343
- Substance type: organic mono-constituent substance
- Physical state: solid
- Analytical purity: 99.7%
- Impurities (identity and concentrations): no data
- Composition of test material, percentage of components: no data
- Purity test date: no data
- Lot/batch No.: AMS 790/1
- Expiration date of the lot/batch: no data
- Stability under test conditions: no data
- Storage condition of test material: no data
- Other:
Specific details on test material used for the study:
Details on properties of test surrogate or analogue material (migrated information):
not applicable
Radiolabelling:
no

Study design

Analytical monitoring:
yes
Details on sampling:
- Sampling intervals for the parent/transformation products:
Test 1: pH4, 50 °C: sampling on 0 h, 2-4 h, 2 d, 5 d
Test 1: ph 9, 50 °C:: sampling on hours 0, 2, 4,5, 7, 24, 26, 28, 30
Test 2: pH 7, 50 °C: sampling on days 0, 0.1, 2, 5, 7, 9, 12, 13
Test 3: pH 7, 70 °C: sampling on hours 0, 3, 20, 27, 44, 50
Test 3: pH 7, 80 °C: sampling on hours 0, 18, 20, 23
Test 3: pH 9, 40 °C: sampling on hours 0, 2, 5, 7, 24, 31, 48, 54

- Sampling method: not specified
- Sampling methods for the volatile compounds, if any: not applicable
- Sampling intervals/times for pH measurements: see above
- Sampling intervals/times for sterility check: The buffer solutions were prepared under clean room conditions, filtered through a 0.2 µm membrane filter and were sterile.
- Sample storage conditions before analysis: not applicable
- Other observation, if any (e.g.: precipitation, color change etc.):
Buffers:
- pH:
- Type and final molarity of buffer:
citrate buffer (pHI 4.0): 20 mM sodium citrate
phosphate buffer (pH 7.0): 20 mM sodium phosphate
borax buffer (pH 9.0): 20 mM sodium tetraborate
- Composition of buffer: see above
Estimation method (if used):
The results from the preliminary test using the pH 4.0 buffer solution indicated that less than 10 % of the test substance had hydrolysed after five days at 50 °C. In accordance with the EEC method C.7, when less than 10 % of the test substance has hydrolysed after five days at 5O °C then no further testing is required.
Details on test conditions:
TEST SYSTEM
- Type, material and volume of test flasks, other equipment used: Approximately 50 mg of the test substance were added to amber, 100 ml volumetric flasks. Then 100.0 ml of the appropriate, srerile buffer solution were added to the flasks. The flasks were placed in a thermosratically controlled water bath, where the contents were thereafter stirred continuously for the duration of the experiment. After about one hour an aliquot was removed and the concentration of CA 2343 determined by high performance liquid chromatography (HPLC).
- Sterilisation method: filtered through a 0.2 µm membrane filter
- Lighting: To exclude light from the hydrolysis system the water bath was covered in aluminum foil. As a further precautionary measure, amber volumetric flasks were used. This gave protection during the times that tlasks were exposed to light, for example, for the purpose of removing the aliquors.
- Measures taken to avoid photolytic effects: To exclude light from the hydrolysis system the water bath was covered in aluminum foil. As a further precautionary measure, amber volumetric flasks were used. This gave protection during the times that tlasks were exposed to light, for example, for the purpose of removing the aliquors.
- Measures to exclude oxygen: Any dissolved oxygen was removed by bubbling a stream of nitrogen gas through the solutions for about 5 minutes.
- Details on test procedure for unstable compounds: not applicable
- Details of traps for volatile, if any not applicable
- If no traps were used, is the test system closed/open not reported
- Is there any indication of the test material adsorbing to the walls of the test apparatus? not reproted

TEST MEDIUM
- Volume used/treatment 100 ml
- Kind and purity of water: not reported
- Preparation of test medium:
The buffer solutions were prepared under clean room conditions, filtered through 0.2 µm membrane filter and were sterile. The hydrolysis solutions were stirred initially for a period of about one hour to ensure that the test substance completely dissolved in the buffer solution and that the solutions were at test temperature before the removal of the initial aliquot. The pH values of all the hydrolysis solutions at the end of the respective tests were determined (at test temperature). The concentration of CA 2343 in all six hydrolysis solutions was less than half the solubility in water and less than 0.01 M.
For each of the three buffer solutions investigated two hydrolysis solutions were prepared as follows: Approximately 50 mg of the test substance were added to amber, 100 ml volumetric flasks. Then 100.0 ml of the appropriate, srerile buffer solution were added to the flasks. Any dissolved oxygen was removed by bubbling a stream of nitrogen gas through the solutions for about 5 minutes. Subsequently, the flasks were placed in a thermosratically controlled water bath.
- Renewal of test solution: not reported
- Identity and concentration of co-solvent: not applicable

OTHER TEST CONDITIONS
- Adjustment of pH: not reported
- Dissolved oxygen: Any dissolved oxygen was removed by bubbling a stream of nitrogen gas through the solutions for about 5 minutes.
Duration of testopen allclose all
Duration:
13 d
pH:
7
Temp.:
50 °C
Initial conc. measured:
510.324 mg/L
Duration:
13 d
pH:
7.01
Temp.:
50 °C
Initial conc. measured:
477.543 mg/L
Duration:
50 h
pH:
7.03
Temp.:
70 °C
Initial conc. measured:
548.926 mg/L
Duration:
50 h
pH:
7.02
Temp.:
70 °C
Initial conc. measured:
554.47 mg/L
Duration:
23 h
pH:
7
Temp.:
80 °C
Initial conc. measured:
532.482 mg/L
Duration:
23 h
pH:
7.02
Temp.:
80 °C
Initial conc. measured:
527.655 mg/L
Duration:
30 h
pH:
9.04
Temp.:
50 °C
Initial conc. measured:
544.573 mg/L
Duration:
30 h
pH:
9
Temp.:
50 °C
Initial conc. measured:
506.314 mg/L
Duration:
54 h
pH:
9
Temp.:
40 °C
Initial conc. measured:
536.876 mg/L
Duration:
54 h
pH:
9.04
Temp.:
40 °C
Initial conc. measured:
502.03 mg/L
Number of replicates:
2
Positive controls:
no
Negative controls:
no
Statistical methods:
no statistics applied

Results and discussion

Preliminary study:
Based on the preliminiary study at 50°C and pH 4, the half-life time of CA 2343 in the buffer solution pH 4 is estimated to be greater than one year at 25 °C (which means also greater than one year at 20 °C).
Test performance:
not reported
Transformation products:
not measured
Details on hydrolysis and appearance of transformation product(s):
- Formation and decline of each transformation product during test: not measured
- Pathways for transformation: not measured
- Other:
Total recovery of test substance (in %)open allclose all
% Recovery:
>= 68 - <= 68.8
St. dev.:
0.56
pH:
7
Temp.:
50 °C
Duration:
13 d
% Recovery:
33.2
St. dev.:
0
pH:
7
Temp.:
70 °C
Duration:
50 h
% Recovery:
14.2
St. dev.:
0
pH:
7
Temp.:
80 °C
Duration:
23 h
% Recovery:
>= 19.5 - <= 20
St. dev.:
0.35
pH:
9
Temp.:
50 °C
Duration:
30 h
% Recovery:
>= 45.6 - <= 46
St. dev.:
0.28
pH:
9
Temp.:
40 °C
Duration:
54 h
% Recovery:
ca. 100
St. dev.:
0
pH:
4
Temp.:
50 °C
Duration:
5 d
Dissipation DT50 of parent compoundopen allclose all
pH:
7
Temp.:
20 °C
Hydrolysis rate constant:
0 h-1
DT50:
3 756 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: no r² given in the study report, however the graph indicates a very good correleation
pH:
7
Temp.:
25 °C
Hydrolysis rate constant:
0 h-1
DT50:
1 500 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: no r² given in the study report, however the graph indicates a very good correleation
pH:
9
Temp.:
20 °C
Hydrolysis rate constant:
0 h-1
DT50:
> 36.2 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: no r² given in the study report, however the graph indicates a very good correleation
pH:
9
Temp.:
25 °C
Hydrolysis rate constant:
0 h-1
DT50:
16.9 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: no r² given in the study report, however the graph indicates a very good correleation
pH:
3.8
Temp.:
20 °C
DT50:
> 1 yr
pH:
3.8
Temp.:
25 °C
DT50:
> 1 yr
Details on results:
TEST CONDITIONS
- pH, sterility, temperature, and other experimental conditions maintained throughout the study: Yes
- Anomalies or problems encountered (if yes): none reported


MAJOR TRANSFORMATION PRODUCTS : none reported


MINOR TRANSFORMATION PRODUCTS : none reported


MINERALISATION (distinguish between dark and irradiated samples): not applicable
- % of applied radioactivity present as CO2 at end of study:


INDICATION OF UNSTABLE TRANSFORMATION PRODUCTS: not applicable


VOLATILIZATION (at end of study) : not applicable


UNIDENTIFIED RADIOACTIVITY (at end of study) : not applicable



PATHWAYS OF HYDROLYSIS : not reported



SUPPLEMENTARY EXPERIMENT (if any): RESULTS: not applicable

Applicant's summary and conclusion

Validity criteria fulfilled:
not specified
Conclusions:
The half-life times (t1/2) of the test substance were determined either by extrapolation of the experimental values (pH 7.0 and pH 9.0) or by estimation from the preliminary test (pH 3.8). The following results for the half-life times of the test substance were obtained by this study.
20 °C: pH 3.8 < 1 a, pH 7 = 3800 d, pH 9 = 1500 d; 25 °C: pH 3.8 < 1 a, pH 7 = 1500 d, pH 9 = 17 d.
Executive summary:

The purpose of this study was to evaluate the hydrolysis as a function of pH for the test substance CA 2343, oxadiazinamine. The study was performed in accordance with the EEC method C.7., OfficiaI Journal of the European Commnunities 92/69/EEC, 1992. The half-life times (t1/2) of the test substance were determined either by extrapolation of the experimental values (pH 7.0 and pH 9.0) or by estimation from the preliminary test (pH 3.8). All experiments were performed using buffer solutions. The following results for the half-life times of the test substance were obtained by this study.

Half-life times (t1/2):

Buffer solution

at 20 °C

 

at 25 °C

 
 pH 3.8  < 1 year < 1 year 
 pH 7.0 3800 d  1500 d 
 pH 9.0 36 d   17 d