Reaction Products of Dimethyl hydrogen phosphite and Alcohols C14-18, Even, Linear

Water solubility

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Experimental starting date: 31 May 2016 Experimental completion date: 25 June 2016

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:

flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Other quality assurance:

other: The UK Good Laboratory Practice Regulations OECD Principles of Good Laboratory Practice EC Commission Directive 2004/10/EC of 11 February 2004

Type of method:

flask method

Key result

Water solubility:

< 0 g/L

Conc. based on:

other: loading rate

Incubation duration:

24 h

Temp.:

20 °C

pH:

>= 3.4 - <= 3.6

Details on results:

See next section for full details

PreliminaryTest

 

The preliminary estimate of water solubility at 20.0 ± 0.5 °C was determined to be less than

1.0 x 10-4g/L. The solution had a pH of 3.8.

Main Test

 

Typical chromatography is presented in the attached Appendix 1

 

The mean total peak areas relating to the standard and sample solutions are shown in the following tables:

 

Table 2

 

Solution	Mean Total Peak Area
Standard 0.025 mg/L	1.701 x 107
Standard 0.051 mg/L	2.094 x 107
Standard 0.076 mg/L	4.257 x 107
Standard 0.105 mg/L	3.941 x 107
Standard 0.253 mg/L	4.602 x 107
Standard 0.507 mg/L	6.887 x 107
Standard 0.760 mg/L	9.822 x 107
Standard 1.01 mg/L	1.013 x 108
Blank	1.209 x 107
Sample 1A	1.224 x 107
Sample 1B	1.222 x 107
Sample 2A	1.127 x 107
Sample 2B	1.124 x 107
Sample 3A	1.101 x 107
Sample 3B	1.080 x 107

 

The calibration curve from which the sample concentrations were interpolated is shown in the attached Figures (Figure 1).

  The concentration (g/L) of test item in the sample solutions at 20.0 ± 0.5 ºC are shown in the following table:

 

Table 3

 

Sample Number	Time Shaken at ~ 30 ºC (hours)	Time Equilibrated at 20 ºC (hours)	Concentration (g/L)	Solution pH
1	24	24	<2.53 x 10-5	3.6
2	48	24	<2.53 x 10-5	3.5
3	72	24	<2.53 x 10-5	3.4

Overall concentration:           less than 2.53 x 10-5g/L at 20.0 ± 0.5ºC

Conclusions:

The water solubility of the test item has been determined to be less than 2.53 x 10-5 g/L at 20.0 ± 0.5 °C.

Executive summary:

The water solubility of the test item has been determined to be less than 2.53 x 10-5 g/L of solution at 20.0 ± 0.5 °C, using the flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

Reference 2

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

09 February 2015 to 05 March 2015

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: Analysis conducted to GLP standards during investigation of aquatic toxicity.

Qualifier:

according to guideline

Guideline:

other: Method developed by Department of Analytical Services, Harlan Laboratories Ltd. Shardlow, UK

Deviations:

no

Principles of method if other than guideline:

The test item concentration in the test samples was determined by high performance liquid chromatography with mass spectrometry using an external standard. The test item gave a chromatographic profile consisting of a number of unresolved peaks.

GLP compliance:

yes

Type of method:

other: HPLC-MS-MS using an external standard

Water solubility:

0.636 mg/L

Temp.:

30 °C

Remarks on result:

other: pH not reported

Details on results:

- Results obtained for the concentration of the test item found in the test samples are presented in Table 4 (attached).
- Typical chromatograms are shown in Figures 2 to 4 (attached).

VALIDATION OF THE ANALYTICAL METHOD

Specificity

- Standard solutions contained a peak specific for the test item whose area changed according to known concentration.

- The specificity of the retention time method was thus confirmed.

Linearity

- Calibration data for the calibration standards of the test item is given in Table 2 and Figure 1 (attached).

- Data was found to have a quadratic correlation within the calibration range of 0 to 1.6 mg/L.

- The Rsquared fit of the calibration curve to the data was 0.9959 and was considered to be acceptable.

Accuracy (recovery) and precision

- A set of recovery samples accurately fortified at a relevant concentration of test item was prepared five-fold and analysed.

- Results obtained for the concentration of the test item in the recovery samples are presented in Table 3 (attached).

- The method was considered to be sufficiently accurate and precise for the purposes of the test.

- Test sample results were not corrected for recovery.

Limit of quantification

- The limit of quantification (LOQ) was determined by calculating the sample concentration that gave a peak equivalent to ten times the baseline noise.

- Using this method the LOQ was determined to be 0.11 mg/L.

Conclusions:

Interpretation of results (migrated information): slightly soluble (0.1-100 mg/L)
Concentration of test item in a sample of 100 mg/L nominal loading rate was determined to be 0.636 mg/L at zero hours.

Executive summary:

METHOD

The test item concentration in the test samples was determined by high performance liquid chromatography with mass spectrometry using an external standard. The test item gave a chromatographic profile consisting of a number of unresolved peaks.

RESULTS

The zero -hour concentration of test item in a sample with a nominal loading rate of 100 mg/L was determined to be 0.636 mg/L at 30 °C.

Description of key information

in the study Fox J M 2016 The water solubility of the test item has been determined to be less than 2.53 x 10-5 g/L of solution at 20.0 ± 0.5 °C, using the flask method, designed to be compatible with Method A.6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

 

In the test Harris, 2015 The zero -hour concentration of test item in a sample with a nominal loading rate of 100 mg/L was determined to be 0.636 mg/L at 30 °C (OECD 203 analytical method).

 

Key value for chemical safety assessment

Water solubility:

0.025 mg/L

at the temperature of:

20 °C