2-(methylnitroamino)ethyl nitrate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

18 October 2019 - 31 October 2019

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Specific details on test material used for the study:

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: the test substance was phlegmatized (15 mass% water addition) for the time of transportation. Before the study performance, the sample was dried at room temperature under vacuum conditions until a constant mass was obtained. The water content after drying process was determined using Karl Fischer method. The purity of test item after drying process was 99.88% ± 0.01%, and water content dropped to 0.391% ± 0.003%.

Key result

Water solubility:

6.81 g/L

Conc. based on:

test mat.

Incubation duration:

72 h

Temp.:

20 °C

pH:

>= 3.71 - <= 4.07

Table 1. Results of the preliminary test

0.1g in x ml of solution	0.1	0.5	1	2	10	100	> 100
Soluble (+/-)	-	-	-	-	-	+
Approximate solubility, g/l	> 1000	1000 to 200	200 to 100	100 to 50	50 to 10	10 to 1	<1

Table 2. Calibration solution

Day	Weight [mg]	Dilution [ml]	Cw [mg/ml]	Peak area		Average peak area Aw	f	Average  f
1	10.22	25-0.2-10	0.008176	437624	437859	437741.5	0.00001868	0.00001892
		25-0.5-10	0.020440	1067649	1065509	1066579.0	0.00001916
2		25-0.2-10	0.008176	437910	437990	437950.0	0.00001867	0.00001892
		25-0.5-10	0.020440	1066959	1065799	1066379.0	0.00001917
3		25-0.2-10	0.008176	434876	435153	435014.5	0.00001879	0.00001908
		25-0.5-10	0.020440	1055806	1055438	1055622.0	0.00001936

Table 3. Study solution in water

Sample mixing time/ flask		Weight of the sample [mg]	Dilution [ml]	Cp [mg/ml]	Peak area		Average peak area Ap	X [g/kg]
72h	1	200.21	10-1-10	2.0021	726427	726089	726258	6.8635
	2	200.67		2.0067	721439	719666	720552.5	6.7940
	3	198.76		1.9876	712710	711622	712166	6.7794
120h	1 (4)	201.17		2.0117	726628	726762	726695	6.8339
	2 (5)	200.69		2.0069	720894	719304	720099	6.7881
	3 (6)	200.66		2.0066	713271	717037	715154	6.7425
144h	1 (7)	200.97		2.0097	719209	718515	718862	6.8244
	2 (8)	200.76		2.0076	718058	718135	718096.5	6.8243
	3 (9)	203.07		2.0307	724413	724287	724350	6.8054

Table 4. Results of test item solubility in water

Mixing time at 20 ºC [h]	72			120			144
Samples	1	2	3	1 (4)	2 (5)	3 (6)	1 (7)	2 (8)	3 (9)
Temperature, ºC	20.4			20.1			19.8
pH	4.05	4.03	4.07	3.87	3.92	3.87	3.78	3.84	3.71
Concentration of Me-NENA (Methyl-2-nitratoethylnitramine), g/l	6.86	6.79	6.78	6.83	6.79	6.74	6.82	6.82	6.81
Average concentration Me-NENA (Methyl-2-nitratoethylnitramine), g/l	6.81			6.79			6.82
Average concentration Me-NENA (Methyl-2-nitratoethylnitramine), g/l	6.81

Saturation was achieved after 72 h of mixing at 20ºC. The density of this solution is about 1 kg/L (about water density). After recalculation: The solubility of Me-NENA (Methyl-2-nitratoethylnitramine) at pH 3.71 – 4.07  in water is 6.81 g/L.

Conclusions:

Solubility of the test item in water at 20 ± 0.5ºC and at pH ranging 3.71–4.07 is 6.81 g/L.

Executive summary:

The water solubility determination of the test item was performed in accordance with EU method A.6 and OECD TG 105. About 5 times the quantity necessary to saturate the desired volume of water, estimated in a preliminary test, was weighed into three glass vessels fitted with glass stoppers. These closed vessels were agitated in an incubator at 20ºC with magnetic stirrer. It was decided to execute the solubility test without pre-incubation at 30ºC due to the fact that the test item melting point is about 37ºC and thus the solubility test with preincubation at 30ºC could cause disturbances in the course of the study. In order to estimate the rate of establishment of the saturation equilibrium, samples were taken until the stirring time had no influence on the concentration measured. The samples taken during saturation were separated using a vial-centrifuge to give the clear liquid phase and the concentration of test substance in the clear solvent phase was determined by a validated HPLC method. The solubility of the test item in distilled water at pH 3.71 - 4.07 was determined to be 6.81 g/L at 20 ± 0.5 °C.

Description of key information

Key study: Test method EU A.6 and OECD 105. GLP study. The solubility of the test item in distilled water at pH 3.71 -4.07 was determined to be 6.81 g/l at 20 ± 0.5 °C.

Key value for chemical safety assessment

Water solubility:

6.81 g/L

at the temperature of:

20 °C