2,4-Pyrimidinediamine, 6-chloro-, 3-oxide

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

30/11/2017 to 11/12/2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Test material

Test material information

Constituent 1

Reference substance name:

2,4-Diamino-6-chloropyrimidine-3-oxide

EC Number:

609-076-5

Cas Number:

35139-67-4

Molecular formula:

C4H5ClN4O

IUPAC Name:

2,4-Diamino-6-chloropyrimidine-3-oxide

Test material form:

solid

Remarks:

white/beige solid

Specific details on test material used for the study:

- Analytical purity: > 99% - Lot/batch No.: 0160405 - Expiration date of the lot/batch: 21/02/2018

Results and discussion

Water solubility

Key result

Water solubility:

ca. 1 786.31 mg/L

Conc. based on:

test mat.

Loading of aqueous phase:

12 g/L

Incubation duration:

> 0 - <= 72 h

Temp.:

20 °C

pH:

>= 7.55 - <= 8.84

Any other information on results incl. tables

All measurements of flasks 2 - 6 were included in the calculation of the mean.

Table8.3‑a     Measurements used for Calculation of Solubility

Day	Flask	Concentration [mg/L]	TotalMean[mg/L]	Total StandardDeviation[mg/L] (RSD* [%])
6	2	1811.39	1786.31	16.34 (0.9)
6	3	1772.42
6	4	1784.01
6	5	1791.91
6	6	1771.83

*RSD = relative standard deviation

 

Mean at the plateau is 1786.31 ± 16.34 mg/L.

The solubility of the test itemin water was determined from the measured concentrations of the test item in the filtrated test solutions.

Equilibration time can be considered as approx. 2 days, as the values which were measured were within ± 15 % of the measurements on previous days and no rising tendency was observed.

The concentration was measured in the flasks 2 – 6 after 6 days of shaking. The solubility ofthe test itemin water at 20 ± 0.3 °C was 1786.31 mg/L (mean from two measurements each in five individual flasks). All replicates showed good correspondence. The standard deviation of the samples which were used for the calculation of water solubility at the plateau was 16.34 mg/L, corresponding to a relative standard deviation of 0.9 %.

No observations arousing doubts concerning the accuracy of the results and the validity of the study were made.

 

 

Applicant's summary and conclusion

Conclusions:

At the plateau, the concentration of the test item in water had reached 1786.31 ± 16.34 mg/L at 20.0 ± 0.3 °C (mean value ± standard deviation of five individual vessels).

Executive summary:

The solubility of the test item in water was determined in GLP compliance according to the OECD TG 105 with the shake flask method, and measured in the filtrated test solutions using HPLC.

In the pre-test, no concentration dependency was observed. According to the guideline, the flask method was used for the determination of the solubility of the test item in water.

In the main test, five identical loading rates of the test item were chosen: 12 g/L (nominal), corresponding to at least 5fold excess of the test item were chosen for the main test. Three flasks 1A - C with the same loading rate (12 g/L) were used during equilibration. Seven vessels (flasks blank, 1C (for the sampling point 72 h) and 2 – 6) were set onto the shaking apparatus immediately. After 24 ± 2 hours, flask 1B (for the sampling point 48 h) and after 48 ± 2 hours, flask 1A (for the sampling point 24 h) were set on the shaker and all flasks were shaken for further 24 ± 2 hours at room temperature (20.0 ± 0.5 °C). Then, flasks 1A - 1C were taken from the shaker, samples were taken, membrane filtered and analysed. No rising tendency in the test item concentration of the solutions were observed. Equilibrium was considered as reached at latest after 3 d after test start.

No Tyndall effect (i.e. a laser beam was scattered when transmitted through the liquid) could be observed indicating that colloidal dispersed particles or micelles are present.

At the plateau, the concentration of MEXORYL SAG/10 lyophilisé in water had reached

1786.31 ± 16.34 mg/L at 20.0 ± 0.3 °C

= 1.7863 ± 0.0163 kg/m3 (SI units)

(mean value ± standard deviation of five individual vessels)