[μ-(5-amino-1,3,3-trimethylcyclohexylamine-N:N')]hexafluorodiboron

Partition coefficient

Link to relevant study record(s)

Reference

Endpoint:

partition coefficient

Type of information:

experimental study

Adequacy of study:

key study

Study period:

This study was conducted between 23 September 2016 and 23 March 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: The study is considered to be a reliability 1 as it has been conducted according to OECD TG 117 (HPLC method) and in compliance with GLP.

Qualifier:

according to guideline

Guideline:

OECD Guideline 117 (Partition Coefficient (n-octanol / water), HPLC Method)

Version / remarks:

13 April 2004

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.8 (Partition Coefficient - HPLC Method)

Version / remarks:

EC 440/2008 of 30 May 2008

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Partition coefficient type:

octanol-water

Specific details on test material used for the study:

Identification : μ(5-amino-1,3,3-trimethylcyclohexylamine-N,N')hexafluorodiboron
Appearance/Physical state: Clear colorless liquid
Batch : AEF0009100
Purity : 51.8%
Expiry date : 29 August 2017
Storage conditions: Room temperature, in the dark.

Analytical method:

gas chromatography

Key result

Type:

log Pow

Partition coefficient:

< -2.34

Temp.:

21 °C

pH:

3.2

Type:

Pow

Partition coefficient:

< 0.004

Temp.:

21 °C

pH:

3.2

Details on results:

Preliminary Estimate

Approximate solubility in n-octanol: 2.7 x 10^-2 g/L
Approximate solubility in water: >119 g/L
Approximate Pow: <2.27 x 10^-4
Log10 Pow: <-3.65

 Definitive Test

The mean peakareasobtained for the standard, stock and sample solutions are shown in the following two tables:

Table 1            Organic Phase

Solution	Mean peakarea
Standard 173 mg/L	2.1940 x 10^6
Standard 165 mg/L	2.2583 x 10^6
Organic phase matrix blank	None detected
Sample 1	None detected
Sample 2	None detected
Sample 3	None detected
Sample 4	None detected
Sample 5	None detected
Sample 6	None detected

 

Table 2 Aqueous Phase

Solution	Mean peakarea
Standard 81.9 mg/L	7.2227 x 10^5
Standard 83.0 mg/L	7.3681 x 10^5
Aqueous phase matrix blank	None detected
Sample 1	1.9485 x 10^6
Sample 2	2.0936 x 10^6
Sample 3	2.2823 x 10^6
Sample 4	2.2263 x 10^6
Sample 5	2.3217 x 10^6
Sample 6	2.5078 x 10^6
Stock solution A	2.3670 x 10^6
Stock solution B	2.2846 x 10^6

The total weights (mg) and analyzed concentration (mg/L) of the respective phases are shown in the following table. As no test item peak was detected within the organic phase a limit value of the lowest detectable standard within the linearity was used (10 mg/L):

Table 3

Sample number	Total weight (mg)*	Organic phase		Aqueous phase			% recovery
		Analyzed concentration (mg/L)	Weight (mg)†	Analyzed concentration (mg/L)	Weight (mg)†	pH
1	105.1	<10	<0.400	2.20 x 10^3	88.1	3.21	~84.2
2	105.1	<10	<0.400	2.37 x 10^3	94.6	3.22	~90.4
3	141.9	<10	<0.270	2.58 x 10^3	139	3.20	~98.3
4	141.9	<10	<0.270	2.52 x 10^3	136	3.22	~95.9
5	70.96	<10	<0.540	2.62 x 10^3	70.8	3.26	~101
6	70.96	<10	<0.540	2.83 x 10^3	76.5	3.26	~109

pH of n-octanol saturated water:       6.7
pH of stock solution:                         3.2
Temperature:                                     21.0 ± 0.5°C

The partition coefficient determined for each sample is shown in the following table:

Table 4

Sample number	Organic/aqueous volume ratio	Partition coefficient	Log10Pow	Mean partition coefficient
1	1:1	<4.54 x 10^-3	<-2.34	<4.54 x 10^-3
2		<4.23 x 10^-3	<-2.37
3	1:2	<3.88 x 10^-3	<-2.41	<3.98 x 10^-3
4		<3.98 x 10^-3	<-2.40
5	2:1	<3.81 x 10^-3	<-2.42	<3.81 x 10^-3
6		<3.53 x 10^-3	<-2.45

Mean P_ow :<3.81x 10^-3                    log₁₀P_ow:<-2.34                  

 Validation

The aqueous linearity of the detector response with respect to concentration was assessed over the nominal concentration range of50to400mg/L. The results were satisfactory with a correlation coefficient (r) of 0.998 being obtained. Theorganiclinearity of the detector response with respect to concentration was assessed over the nominal concentration range of10to200mg/L. The results were satisfactory with a correlation coefficient (r) of0.998being obtained.

Discussion

The determination of partition coefficient was performed using the shake-flask method. This was due to the expected partition coefficient obtained in the preliminary assessment.

The stock solution was prepared in n-octanol saturated water in place of water saturated
n-octanol. This was due to the relative insolubility of the test item in the organic phase. This issue has been considered to have had a negligible impact on the overall result and has been considered to be more appropriate to obtain a more realistic partition coefficient value.

Analysis was carried out using unbuffered n-octanol saturated water. The pH of the stock solution decreased from pH 7 (n-octanol saturated water) to pH 3 (stock solution), this also occurred at lower concentrations (approximately 2.5 mg/L), suggesting that the pH change was due to the test item and not an impurity. The test item was still in its unionised form at pH 3, and therefore this had no impact on the test.

Multiple peaks were integrated during analysis, all peaks were processed as a group for quantification.

As no test item peak was detected within the organic phase a limit value of the lowest detectable standard within the linearity was used (10 mg/L)

* From analysis of the stock solution

† From analysis of therespective phase

Conclusions:

The partition coefficient of the test item has been determined to be less than 3.81 x 10^-3 at 21.0 ± 0.5 °C, log10 Pow< -2.34.

Executive summary:

The general physico-chemical properties of μ(5-amino-1,3,3-trimethylcyclohexylamine-N,N')hexafluorodiboron have been determined. 

Partition Coefficient (n-octanol/water). The partition coefficient(P_ow)of the test item has been determined to beless than 3.81 x 10^-3at21.0±0.5°C, log₁₀P_ow<-2.34, using the shakeflask method, designed to be compatible with Method A.8 Partition Coefficient of Commission Regulation (EC) No 440/2008 of 30 May 2008andMethod 107 of the OECD Guidelines for Testing of Chemicals, 27 July 1995. 

Key value for chemical safety assessment

Log Kow (Log Pow):

-2.34

at the temperature of:

21 °C