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Diss Factsheets

Administrative data

Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2018-09-20 to 2018-12-14
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 guidelineopen allclose all
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
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7840 (Water Solubility)
Deviations:
no
GLP compliance:
no
Type of method:
flask method

Test material

Constituent 1
Chemical structure
Reference substance name:
ethyl 5-amino-1-[(2-fluorophenyl)methyl]-1H-pyrazole-3-carboxylate
EC Number:
805-733-7
Cas Number:
256504-39-9
Molecular formula:
C13H14FN3 O2
IUPAC Name:
ethyl 5-amino-1-[(2-fluorophenyl)methyl]-1H-pyrazole-3-carboxylate
Test material form:
solid

Results and discussion

Water solubilityopen allclose all
Key result
Water solubility:
140 mg/L
Conc. based on:
test mat.
Loading of aqueous phase:
2 g/L
Incubation duration:
144 h
Temp.:
20 °C
pH:
4
Key result
Water solubility:
> 140 mg/L
Conc. based on:
test mat.
Loading of aqueous phase:
2 g/L
Incubation duration:
144 h
Temp.:
20 °C
pH:
7
Remarks on result:
other: Equilibrium has not been reached; the given value must be seen as minimum.
Key result
Water solubility:
133 mg/L
Conc. based on:
test mat.
Loading of aqueous phase:
2 g/L
Incubation duration:
96 h
Temp.:
20 °C
pH:
9
Details on results:
The water solubility of the test item was determined using the shake flask method. The saturation mass concentrations of the test item were determined using UPLC / UV-VIS.
The results for the pH levels 4 and 9 showed no tendency to increase and met all validity criteria, therefore this part of the study is considered to be valid.
Corresponding to the analyses the water solubility was determined to be

pH 4: 140 mg/L
pH 7: > 140 mg/L (appraisal)
pH 9: 133 mg/L

at 20 °C.

The pH dependency seen in the preliminary test could not be reproduced.

pH 4:
During the first incubation timespans an increase in the concentrations from 132 mg/L to 150 mg/L has been seen. In a second approach, this increase could not be continued but a stable concentration at approx. 137 mg/L was established.
The relative standard deviation over all samplings of 15.4%. This does not meet the validity criteria of a deviation below 15%. The two elevated values from the 72 h incubation time were tested but were no outliers. Talking into account the increased incubation time with the continued sampling (n=12) and the small deviation of the validity criteria, the result is seen as valid.

pH 7:
For both first and second approach with continuously increased incubation time, an increase in concentration from about 115 mg/L to 140 mg/L has been observed.
It has been decided with the sponsor to not further increase the incubation time. A value of about 140 mg/L is given as appraisal. Equilibrium has not been reached; the given value must be seen as minimum.

pH 9:
No tendency of an increase over time has been seen during the normal incubation timespan between 24 and 96 hours, therefore no further experiment has been conducted.

Applicant's summary and conclusion

Conclusions:
The water solubility of the test item was determined using the shake flask method. The saturation mass concentrations of the test item were determined using UPLC / UV-VIS.
The results for the pH levels 4 and 9 showed no tendency to increase and met all validity criteria, therefore this part of the study is considered to be valid.
Corresponding to the analyses the water solubility was determined to be

pH 4: 140 mg/L
pH 7: > 140 mg/L (appraisal)
pH 9: 133 mg/L

at 20 °C.
Executive summary:

Title: Aminopyrazol: Determination of the Water Solubility at pH 4, 7 and 9 by the Shake Flask Method

Purpose: The purpose of this study was to evaluate the solubility of the test item in water which is specified by the saturation mass concentration of the test item in water at a specified temperature and defined pH-level.

Guidelines/Recommendations:

This study was based on the procedures indicated by the following internationally recognized documents:

OECD Guidelines for Testing of Chemicals, Guideline No.105, ”Water Solubility”; adopted July 27, 1995

Commission Regulation (EC) No 440/2008, Annex, Part A, Methods for the determination of physico-chemicals properties, A6 "Water Solubility", May 2008

Product Properties Test Guideline of the United States Environment Protection Agency (EPA), OPPTS 830.7840 Water Solubility: Column Elution Method; Shake Flask Method, March 1998

Results:The water solubility of the test item was determined using the shake flask method. The saturation mass concentrations of the test item were determined using UPLC / UV-VIS.

The results for the pH levels 4 and 9 showed no tendency to increase and met all validity criteria, therefore this part of the study is considered to be valid.

Corresponding to the analyses the water solubility was determined to be

 

pH 4: 140 mg/L

pH 7: > 140 mg/L (appraisal)

pH 9: 133 mg/L

 

at 20 °C.

This study is classified acceptable and satisfies the guideline requirements for water solubility studies.