Reaction mass of 1,4-bis(methylamino)anthraquinone and 1,4-bis[(2-ethylhexyl)amino]anthraquinone and 1-[(2-ethylhexyl)amino]-4-(methylamino)anthraquinone and 9,10-Anthracenedione, 1,4-bis(pentylamino)-, branched and linear and 9,10-Anthracenedione, 1-(methylamino)-4-(pentylamino)-, branched and linear and 9,10-Anthracenedione, 1-[(2-ethylhexyl)amino]-4-(pentylamino)-, branched and linear

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

February 20, 2017 to May 10, 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

GLP compliance:

no

Type of method:

flask method

Specific details on test material used for the study:

Identification: C.I. Solvent Blue 98
Appearance/Physical state: extremely dark blue solid block
Batch: ZA07212016
Purity: 98.0%
Expiry date: 18 July 2019
Storage conditions: room temperature in the dark

Key result

Water solubility:

0 g/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

6.18

Preliminary Test Results:

The preliminary estimate of the water solubility at 20.0 ± 0.5 °C was 1.43 x 10^-4g/L. The solution had a pH of 6.39.

Definitive Test Results:

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

Solution	Mean Peak Area
Standard 30.5 mg/L	9.8711 x 10^6
Standard 30.2 mg/L	9.6905 x 10^6
Sample 1A	*
Sample 1B	1.3990 x 10^7
Sample 2A	1.7323 x 10^7
Sample 2B	1.7487 x 10^7
Sample 3A	2.3821 x 10^7
Sample 3B	2.3590 x 10^7
Standard 30.1 mg/L	9.1475 x 10^6
Standard 30.2 mg/L	9.3716 x 10^6
Sample 4A	3.2036 x 10^6
Sample 4B	3.0509 x 10^6
Sample 5A	5.0637 x 10^6
Sample 5B	5.0261 x 10^6
Sample 6A	5.8471 x 10^6
Sample 6B	5.6522 x 10^6

*No result obtained.

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

Sample Number	Time Shaken at ~ 30°C (hours)	Concentration (g/L)	Solution pH
1	24	2.17 x 10^-4	6.74
2	48	2.70 x 10^-4	6.31
3	72	3.68 x 10^-4	6.04
4	24	5.08 x 10^-5	6.16
5	48	8.20 x 10^-5	6.42
6	72	9.35 x 10^-5	6.92

Mean concentration   :          3.19 x 10^-4 g/L at 20.0 ± 0.5 ºC (samples 2 to 3)
Range                         :          2.70 x 10^-4 to 3.68 x 10^-4 g/L
Standard Deviation    :          6.91 x 10^-5

Validation:

The linearity of the detector response with respect to concentration was assessed over the nominal concentration range of 10 to 50 mg/L. The results were satisfactory with a correlation coefficient (r) of 1.000 being obtained.

Assessment of the sample recovery procedure was performed and proved adequate for the test; at a nominal concentration of 0.15 mg/L, a mean percentage recovery of 101.2% was obtained (range 99.8 to 102.4%).

Test sample concentrations have not been corrected for the recovery of analysis.

Discussion:

On completion of the equilibration period, the samples were clear with excess test item present at the bottom of the test vessels. The solutions were decanted, avoiding excess test item prior to centrifugation. After centrifugation, the supernatant was taken for analysis. The supernatant was visually observed to be clear and free from un-dissolved test item.

The preliminary water solubility test indicated that the column elution method should have been performed as the solubility was less than 1x10^-2g/L. However, due to the large sample volume required for analysis, the column elution method was impractical. Therefore the flask method was used.

The test item consisted of several components therefore the impact of loading rate was assessed. A loading rate increase of 10 times produced approximately 3 times the analyzed result. It was therefore concluded that the higher loading rate was sufficient to saturate the more water soluble components. The results showed that the test item was not fully saturated after 24 hours shaking therefore the result reported is the mean of the higher loading rate, shaken for 48 and 72 hours.

The earlier eluting peaks of the test item had significantly higher water solubility than the later eluting components resulting in significant differences in the peak profile between

samples and standards. As the exact quantities of each component in the standards were unknown the results were calculated on the basis of total peak area.

Conclusions:

The water solubility of the test item has been determined to be 3.19 x 10^-4 g/L of solution at 20.0 ± 0.5 °C.

Executive summary:

Water Solubility. 3.19 x 10^-4g/L of solution at 20.0 ± 0.5 °C, using the flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

Description of key information

Water Solubility. 3.19 x 10^-4g/L of solution at 20.0 ± 0.5 °C, using the flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

Key value for chemical safety assessment

Water solubility:

0 g/L

at the temperature of:

20 °C

Additional information

3.19 x 10^-4g/L of solution at 20.0 ± 0.5 °C, using the flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.