1,3-bis(hydroxymethyl)urea

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

from 201-03-23 to 2011-11-02

Reliability:

1 (reliable without restriction)

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Qualifier:

according to guideline

Version / remarks:

Homemade method to investigate complete miscibility: EM/00408/01 (chapter 4: visual method)

Principles of method if other than guideline:

A Pre-test according to OECD Guideline 105 was performed. In all ratios the test item was completely dissolved in the water. A complete miscibility of the test item in water was supposed. To performe the flask method described in the OECD Guideline 105, a saturated solution of the test item in water is required. Since this was not possible for this test item, a homemade method: visual method for investigation of the complete miscibility of substances, written by the test facility, was used to estimate the solubility of this test item.

GLP compliance:

yes (incl. QA statement)

Type of method:

other: visual method

Key result

Water solubility:

>= 12 - < 14 g/cm³

Conc. based on:

test mat.

Incubation duration:

> 12 - <= 72 h

Temp.:

20 °C

pH:

>= 6.8 - <= 7.8

Remarks on result:

completely miscible

Pre-testing:

Mixtures of the test item with water were prepared at different concentrations. After shortly shaking by hand at room temperature (23 °C), the preparations were visually checked:

Weight of test item	Amount of water added	Sample size	Observation
108.96 mg	10 mL	10.9 g/L	Completely dissolved
502.05 mg	10 mL	50.2 g/L	Completely dissolved
1.01 g	9.21 g	9.9 g / 100 g	Completely dissolved

Thus, a complete miscibility of the test item with water was supposed.

Analytical Method:

The test item and water were mixed in different ratios and shortly shaken by hand or agitated on a roller mixer at room temperature (T = 23 °C) to estimate the solubility / miscibility.
Mixtures no. 1, 4-7 and 9-10 were conditioned overnight and mixture no. 8 was conditioned over the weekend at 20.0 °C ± 0.5 °C. Mixtures no. 2 and 3 were not conditioned at 20.0 °C ± 0.5 °C. no changes were observed with exception of mixture no. 9 (1.4 : 8.6), where the solution was slightly turbid after conditioning.

Mixtures of the solubility test (mixtures no. 2 and 3) were analyzed applying liquid chromatography. The chromatograms showed changing ratios of the test item peaks depending on the amount of water in the mixture. This may be due to the moisture-sensitivity of the test item. Therefore it was not possible to determine the water solubility more precisely.

No.	Weight of test item [g]	Amount of water added [g]	Sample size [g/100g]	Ratio	Observations	pH
1	1.00	9.00	10.0	1 : 9	Clear, colorless and homogeneous solution / mixture, completely dissolved / mixed after shortly shaking by hand	6.8
2	5.03	5.05	49.9	1 : 1	Highviscous and homogeneous white mass, not completely dissolved / mixed after rolling overnight	^1)
3	1.98	7.98	19.9	2 : 8	Homogeneous white liquid, not completely dissolve / mixed after rolling overnight, after standing for about one hour homogeneous solution with white bottoms	^1)
4	3.12	7.12	30.5	3 : 7	Supernatant clear and colorless solution with amounts of the test item adhered to the walls and as white bottoms, not completely dissolved / mixed after rolling overnight and standing for further four days	7.7^2)
5	4.01	6.05	39.9	4 : 6		7.5^2)

¹⁾The measurement of the pH-value was not possible (suspension).

²⁾The pH of the filtrate (0.2 µm) was measured.

To determine the solubility / miscibility limits more detailed additional mixtures were prepared:

6	1.12	8.87	11.2	1.1 : 8.9	Clear, colorless and homogeneous solution / mixture, completely dissolved / mixed after shortly shaken by hand	7.8
7	1.20	8.86	11.9	1.2 : 8.8		7.8
8	1.30	8.71	13.0	1.3 : 8.7	Clear, colorless and homogeneous solution / mixture, completely dissolved / mixed after rolling overnight	7.5
9	1.42	8.64	14.1	1.4 : 8.6	Clear, colorless and homogeneous solution / mixture, completely dissolved / mixed after rolling overnight and additionally standing over the weekend	7.5
10	1.61	8.41	16.1	1.6 : 8.4	Clear, colorless and homogeneous supernatant with white bottoms, not completely dissolved / mixed after rolling overnight and standing for about one hour	7.5
Water used (no. 1 – 3)						6.1
Water used (no. 4 – 5)						6.3
Water used (no. 6 – 10)						6.2

 

Conclusions:

The solubility (miscibility) of the test item in water at 20.0 ± 0.5 °C is ≥ 13g/100g < 14g/100g (m test item / m mixture).

Executive summary:

Due to the impossibility of preparing a saturated solution of the test item, it was not possible to perform the test according to the OECD Guideline 105 - water solubility. A homemade method EM/00408/01, chapter 4: Visual method, was used to establish the complete miscibility of the test item. Ten mixtures with different ratios test item : water were prepared and the solubility was estimated by observations. Two of the mixtures were tested with liquid chromatography, but no certain results were observed. This may be due to the moisture-sensitivity of the test item. Therefore it was not possible to determine a more precise water solubility The water solubility based on the observations was estimated to be ≥ 13 g/ 100g < 14 g/ 100g (m_{test item}/ m_mixture).

Description of key information

The solubility (miscibility) of the test item in water at 20.0 ± 0.5 °C is ≥ 13g/100g < 14g/100g (m_{test item} / m_mixture).

Additional information

Due to the impossibility of preparing a saturated solution of the test item, it was not possible to perform the test according to the OECD Guideline 105 - water solubility (reference 4.8-1). A homemade method EM/00408/01, chapter 4: Visual method, was used to establish the complete miscibility of the test item. Ten mixtures with different ratios test item : water were prepared and the solubility was estimated by observations. Two of the mixtures were tested with liquid chromatography, but no certain results were observed. This may be due to the moisture-sensitivity of the test item. Therefore it was not possible to determine a more precise water solubility The water solubility based on the observations was estimated to be ≥ 13 g/ 100g < 14 g/ 100g (m_{test item}/ m_mixture).