Benzenamine, reaction products with aniline hydrochloride and nitrobenzene

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2 August 2006 to 8 December 2006

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted to GLP 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.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

yes

Remarks:

See the comments in Principle of method if other than guideline.

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

yes

Remarks:

See the comments in Principle of method if other than guideline.

Principles of method if other than guideline:

Due to a blockage of the column elution apparatus resulting in a significant loss in solution volume for determination B, only 4 samples were obtained, not the minimum of 5 samples on the saturation plateau as recommended by the method guidelines. This was concluded not to impact on the validity of the test, as determination A was demonstrated to have reached saturation equilibrium over the same time period. Since determination B was the faster flowing apparatus, it would have achieved saturation equilibrium before determination A, and therefore it can be concluded that determination B was at equilibrium at the time of sampling, as supported by the common limit value obtained for all 4 determination B samples. In addition, sufficient data was generated to demonstrate that the test material solubility was not significantly flow rate dependent, the reason that two individual determinations are required for the column elution method.

GLP compliance:

yes (incl. QA statement)

Type of method:

column elution method

Water solubility:

< 0.1 mg/L

Temp.:

20 °C

Remarks on result:

other: pH values not reported

Details on results:

Preliminary test
The preliminary estimate of water solubility was 3.28 x 10^-4 g/l.

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

Table 1.

Solution	Mean Peak Area
Standard 10.0 mg/l	2.009 x 10^3
Standard 10.2 mg/l	2.079 x 10^3
Standard Blank	32.854
Sample Blank	147.658
Determination A, Sample 2	186.263
Determination B, Sample 2	209.971
Determination A, Sample 3	141.815
Determination B, Sample 3	149.438
Determination A, Sample 4	158.457
Determination B, Sample 4	194.56
Determination A, Sample 5	192.857
Standard 10.0 mg/l	2.195 x 10^3
Standard 10.2 mg/l	2.197 x 10^3
Standard Blank	none detected
Sample Blank	26.86
Determination A, Sample 6	25.568

The concentration (g/l) of test material in the sample solutions is shown in the following table:

Table 2.

Sample Number	Sampling time (hour)		Concentration (g/l)		Solution pH
	Determination A	Determination B	Determination A	Determination B	Determination A	Determination B
1	192.5	193	<1.0 x 10^-4	<1.0 x 10^-4	6.4	6.6
2	312	312	<1.0 x 10^-4	<1.0 x 10^-4	6.5	6.7
3	337.5	338	<1.0 x 10^-4	<1.0 x 10^-4	6.5	6.2
4	357.5	358	<1.0 x 10^-4	<1.0 x 10^-4	6.4	6.5
5	383	-	<1.0 x 10^-4	-	6.2	-
6	454.5	-	<1.0 x 10^-4	-	6.5	-

The overall results are shown in the following table:

Table 3.

Determination	Overall Concentration (g/l)
A	<1.0 x 10^-4
B	<1.0 x 10^-4
Overall	<1.0 x 10^-4

 

Validation

The linearity of the detector response with respect to concentration was assessed over the nominal concentration range of 0 to 250 mg/l. This was satisfactory with a correlation coefficient of 0.999 being obtained.

Recovery of analysis of the sample procedure was assessed and proved adequate for the test. Recovery data is shown in the following table:

Table 4.

Nominal concentration (mg/l)	Recovery range (%)	Mean recovery (%)
0.50	64.1 to 64.9	64.5
0.10	66.7 to 68.7	67.6

 

Discussion

On the analysis of all sample solutions from both determination A and determination B, the instrument responses were approximately equal to that of the respective sample blank, such that a theoretical concentration range of -1.2 x 10^-6 to 4.3 x 10^-5 g/l was obtained, with no time or flow rate dependent trends; i.e, the test material was shown to be essentially insoluble in water. An overall limit value of less than 1.0 x 10^-4 g/l has been reported for the water solubility of the test material, originating from the lowest nominal concentration at which the analytical method extraction procedure was successfully validated.

Due to a blockage of the column elution apparatus resulting in a significant loss in solution volume for determination B, only 4 samples were obtained, not the minimum of 5 samples on the saturation plateau as recommended by the method guidelines. This was concluded not to impact on the validity of the test, as determination A was demonstrated to have reached saturation equilibrium over the same time period. Since determination B was the faster flowing apparatus, it would have achieved saturation equilibrium before determination A, and therefore it can be concluded that determination B was at equilibrium at the time of sampling, as supported by the common limit value obtained for all 4 determination B samples. In addition, sufficient data was generated to demonstrate that the test material solubility was not significantly flow rate dependent, the reason that two individual determinations are required for the column elution method.

Conclusions:

The water solubility of the test material has been determined to be less than 0.1 mg/l of solution at 20.0 ± 0.5°C.

Executive summary:

In a general physico-chemical properties study (0370/0351), the water solubility of the test material was determined to be less than 0.1 mg/l of solution at 20.0 ± 0.5°C, according to OECD Test Method 105.

Description of key information

The water solubility of the test material has been determined to be less than 0.1 mg/L of solution at 20.0 ± 0.5 °C.

Key value for chemical safety assessment

Water solubility:

0.1 mg/L

at the temperature of:

20 °C

Additional information

In a general physico-chemical properties study (0370/0351), the water solubility of the test material was determined to be less than 0.1 mg/L of solution at 20.0 ± 0.5 °C, according to OECD Test Method 105. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).