Reaction mass of tetrasodium 5-{[4-chloro-6-(4-{[2-(sulfonatooxy)ethyl]sulfonyl}anilino)-1,3,5-triazin-2-yl]amino}-4-hydroxy-3-[(4-{[2-(sulfonatooxy)ethyl]sulfonyl}phenyl) diazenyl]naphthalene-2,7-disulfonate and trisodium 5-({4-chloro-6-[4-(vinylsulfonyl) anilino]-1,3,5-triazin-2-yl}amino)-4-hydroxy-3-[(4-{[2-(sulfonatooxy)ethyl]sulfonyl}phenyl)diazenyl]naphthalene-2,7-disulfonate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

29 October 1989 to 01 March 1990

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

84/449/EWG, appendix V

Deviations:

no

GLP compliance:

yes

Type of method:

flask method

Water solubility:

> 200 g/L

Temp.:

30 °C

pH:

1.9 - 2.4

Details on results:

- Quality of the water: after demineralisation the water was distilled
- Water volume added to the weighed amounts of the test substance: 50 ml
- Duration of equilibration at 20 °C after stirring different times at 30 °C: 24 h

After centrifugation of charges no 1 -3 no excess solid was existing. The “solutions” were very thick and viscous. From the weighed portions and the added water a water solubility of ≥ 700 g/L can be calculated.

Further experiments
Also amounts of 25.3 and 28.2 g of the test substance added to 25 ml water (stirring time: 20.5 h at 30 °C; 3 h at 20 °C) showed no sediments (solubility > 1000 g/L).

Further experiments with the following amounts were carried out:
4) 56.4 g test substance in 50 ml water
5) 56.7 g test substance in 50 ml water
6) 56.3 g test substance in 50 ml water
7) 60.4 g test substance in 50 ml water

Stirring time: 44 h at 30 °C, 3 h at 20 °C

After centrifugation undissolved particles could be recognized in the charges 5 and 7. It was impossible to stir these samples equally. The “solutions" were such high viscous that it was not possible to take aliquots using a pipette.

Due to the experiments described above the experiments for the determination of the water solubility were repeated with smaller amounts.

Water volume added to the weighed portions of the test substance: 50 ml
During of equilibration at 20 °C after stirring different times at 30 °C: 24 h


The results of the experiments 8-10 and 11-13 obtained by photometric determination are clearly below the results obtained from a direct calculation from the weighed portions, water volume and content of the main component even though there was no residue.

Due to the experimental difficulties (no residue in exp. 1-3, very thick and high viscous and dark solutions) as a final result a minimum water solubility > 200 g/L is given (refer exp. 11 - 13).

Table 1

Sample (no.)	Amount test substance [g]	Stirring time at 30°C [h]	pH-value	Test substance concentration (g/L) (photometric)
1	35.5	24	*)	*)
2	35.5	48	*)	*)
3	35.2	72	*)	*)

*) not determined

Table 2

Sample (no.)	Amount test substance [g]	Stirring time at 30 °C [h]	pH-value	Test substance concentration (g/L) (photometric)
8	26.7	24	2.2	429.2
9	26.9	48	2.1	431.3
10	27.6	72	1.9	434.0
			Mean value	431.5

 

Table 3

Experiment	Concentration calc. from weighed portion and added water volume (g/L)	Concentration converted under the premise of a content of 71.2% (g/L)
8	535.0	380.9
9	538.8	383.6
10	552.2	393.2
Mean:	542	386

 

Table 4

Sample (no.)	Amount test substance [g]	Stirring time at 30°C [h]	pH-value	Test substance concentration (g/L) (photometric)
11	20.1	24	2.4	345.8
12	20.1	48	2.3	345.8
13	20.1	72	2.2	344.5
			Mean value	345.4

 

Table 5

Experiment	Concentration calc. from weighed portion and added water volume (g/L)	Concentration converted under the premise of a content of 71.2% (g/L)
11	402.4	286.5
12	402.3	286.4
13	402.6	286.7
Mean	402	287

There was no sediment to recognise and no residue in the filter.

Table 6

Experiment	Concentration calc. from the weighed portion and volume H2O		Concentration calc. from photometry
	Directly calculated	Converted to 71.2%		Converted to 71.2%
	(g/L)	(g/L)	(g/L)	(g/L)
1 – 3	≥700	≥498	---	---
8 – 10	542	386	432	308
11 – 13	402	287	345	246

 

Conclusions:

The minimum water solubility of the test substance at 30 °C, applied to a content of 71.2 %, is > 200 g/L

Executive summary:

Study conducted to 84/449/EWG, appendix V, part A, in compliance with GLP using the "Flask Method" - determined following the preliminary visual experiments.

The minimum water solubility of the test substance at 30 °C, applied to a content of 71.2%, is > 200 g/L

Description of key information

Water solubility >200 g/L at 30°C

Additional information

The minimum water solubility cS of the test item at a temperature of 30 °C was determined (corrected for purity). The water solubility of the test substance was > 200 °C (cS > 200 g/L).