Bicyclo[2.2.1]heptanebis(methylamine)

Hydrolysis

Link to relevant study record(s)

Reference

Endpoint:

hydrolysis

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 February 2016 to 21 April 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 111 (Hydrolysis as a Function of pH)

Deviations:

no

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)

Radiolabelling:

no

Analytical monitoring:

yes

Buffers:

Buffer solutions were prepared as follows:

pH 4:
0.2M aqueous glacial acetic acid (102.5 mL) was mixed with 0.2M aqueous sodium acetate (22.5 mL) and diluted to volume (250 mL) with purified water. The pH was measured and confirmed to be 4.0 ± 0.05.

pH 7:
0.1M aqueous tris(hydroxymethyl)aminomethane (125 mL) was mixed with 0.1M hydrochloric acid (116.5 mL). The pH was measured and confirmed to be 7.0 ± 0.05.

pH 9:
0.1M aqueous tris(hydroxymethyl)aminomethane (250 mL) was mixed with 0.1M hydrochloric acid (28.5 mL). The pH was adjusted to 9.0 ± 0.05 with further 0.1M hydrochloric acid.

Details on test conditions:

PRELIMINARY TEST
The following procedure was carried out at each of pH 4, 7 and 9:
Aliquots (1 mL) of a stock solution of test material in purified water (15 g/L) were added to separate Wheaton vials containing buffer solution (9 mL), which had been purged with nitrogen and pre-equilibrated at test temperature (50 ± 0.5 °C). It was necessary to add increments of hydrochloric acid solution to the samples to maintain nominal test pH. An aliquot (20 μL) of 10M acid was added to each test solution, while an additional aliquot (15 μL) of 1M acid was added to the pH 4 and pH 9 samples only.
The samples, of nominal concentration 1.5 g/L, were placed in a 50 °C waterbath in the dark until sampling was required (immediately, and then after 2.4 and 120 hours).
At each sampling time, two samples were removed from the bath and an aliquot (1 mL) of each was diluted to volume (20 mL) with acetonitrile for analysis by gas chromatography (GC). As it became apparent that there was suppression of the response of pH 7 samples due to a matrix effect, these samples were further diluted (1 mL to 2 mL with acetonitrile) to minimize this.
Sample pH and incubation temperature were monitored over the period of the test.

Number of replicates:

Not specified

Positive controls:

not specified

Negative controls:

not specified

Preliminary study:

The preliminary study showed that at each of pH 4, 7 and 9 and 50 ± 0.5 ºC, less than 10 % hydrolysis had occurred after 120 hours (5 days), equivalent to a half-life of greater than 1 year under environmental conditions (25 °C). No further testing was considered necessary.

The results show that there were no significant changes in pH and temperature with time.

Transformation products:

not measured

pH:

4

Temp.:

50 °C

DT50:

> 365 d

Type:

not specified

Remarks on result:

hydrolytically stable based on preliminary test

pH:

7

Temp.:

50 °C

DT50:

> 365 d

Type:

not specified

Remarks on result:

hydrolytically stable based on preliminary test

pH:

9

Temp.:

50 °C

DT50:

> 365 d

Type:

not specified

Remarks on result:

hydrolytically stable based on preliminary test

Details on results:

Linearity
Under the conditions described, the calibration of the test material was found to be linear over the range 0 to 100 mg/L with a regression coefficient of 0.9997.
It was considered that the analytical method was sufficiently sensitive to quantify test item concentrations down to 10 % or less of the initial concentration.

Validity criteria fulfilled:

yes

Conclusions:

The test material was determined to be hydrolytically stable under acidic, neutral and basic conditions.

Executive summary:

A study was performed to determine the rate of hydrolysis of the test material as a function of pH. The test was conducted under GLP conditions and in accordance with the preliminary test as described in Commission Regulation (EC) No. 440/2008 (Method C.7) and the OECD Guidelines for Testing of Chemicals (Method 111).

The preliminary study showed that at each of pH 4, 7 and 9 and 50 ± 0.5 ºC, less than 10 % hydrolysis had occurred after 5 days, equivalent to a half-life of greater than 1 year under environmental conditions (25 °C). No further testing was considered necessary.

Under the conditions of the study, the test material was determined to be hydrolytically stable under acidic, neutral and basic conditions.

Description of key information

The test material was determined to be hydrolytically stable under acidic, neutral and basic conditions, OECD 111, EU Method C.7, C Pointer (2017)

Additional information

A study was performed to determine the rate of hydrolysis of the test material as a function of pH. The test was conducted under GLP conditions and in accordance with the preliminary test as described in Commission Regulation (EC) No. 440/2008 (Method C.7) and the OECD Guidelines for Testing of Chemicals (Method 111).

The preliminary study showed that at each of pH 4, 7 and 9 and 50 ± 0.5 ºC, less than 10 % hydrolysis had occurred after 5 days, equivalent to a half-life of greater than 1 year under environmental conditions (25 °C). No further testing was considered necessary.

Under the conditions of the study, the test material was determined to be hydrolytically stable under acidic, neutral and basic conditions.