trans-1-butyl-4-[trans-4-[(E)-prop-1-enyl]cyclohexyl]cyclohexane

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

June 22, 2018 - June 28, 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

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

GLP compliance:

no

Type of method:

column elution method

Key result

Water solubility:

< 0.03 mg/L

Conc. based on:

test mat.

Incubation duration:

48 h

Temp.:

20 °C

pH:

>= 6.5 - <= 7

Table 1: Recovery

All recovery values are calculated from the measured and unrounded concentration values and not from the rounded values given in Table 1. The recovery of the standards indicated a sufficient accuracy of the analytical method.

Standard	Measured concentration /mg/L	% Recovery (mean values)
A2 (c = 3.360 mg/L)	3.891 /3.776	114.1
B1 (c= 12.56 mg/L)	13.78/13.69	109.3
C1 (c= 13.20 mg/L)	13.70/13.59	103.4
A1 (c = 33.60 mg/L)	39.96 / 37.86	115.8

Table 2: Repeatability

The repeatability was checked by measuring standard H2 six-fold. The resulting area was used to calculate the standard deviation and the variation coefficient.

Measurement No.	Area / mAU*s
1	107.165
2	106.862
3	106.360
4	105.317
5	109.549
6	106.272
Mean value	106.9
Standard deviation	1.4
Variation coefficient / %	1.3

The accuracy of the analytical method was evaluated as sufficient as the variation coefficient of the repeatability measurements was < 2.

Three preliminary tests were carried out with specified amounts of the test item and 100 mL and 500 mL demineralized water, respectively. After each addition of an amount of water, the mixture was stirred for at least 24 hours, and visually checked for any undissolved particles.

Table 3: Results of the preliminary test

Amount of test item / mg	Total volume of demineralized water / mL	Appearance of mixture
12.1	100	not dissolved
23.1	500	not dissolved
4.3	500	not dissolved

The preliminary test showed that the water solubility of the test item is < 10 mg/L. According to the preliminary test the water solubility was determined by the column elution method in the main test.

Table 4: Column elution method, column 1 (approximately 12.5 mL/h)

Fraction No.	V/mL	pH	water solubility /µg/L
12-14	57.0	6.5-6.8	<28
15-17	57.0	6.5-6.8	<28
18-20	57.0	6.5-6.8	<28
21-23	57.0	6.5-6.8	<28
24-26	57.0	6.5-6.8	<28

Column 1: Rotation period of the fraction collector: 90 min per fraction Duration of sampling: about 48 h (32 fractions)

The water solubility was found to be below the quantification limit of 28 µg/L.

Table 5: Column elution method, column 2 (approximately 25 mL/h)

Fraction No.	V/mL	pH	water solubility /µg/L
43-45	55.5	6.6-7.0	<28
46-48	54.5	6.6-6.7	<28
49-51	54.0	6.7-6.9	<28
52-54	54.0	6.8-6.9	<28
55-57	54.0	6.7-7.0	<28

Column 1: Rotation period of the fraction collector: 45 min per fraction Duration of sampling: about 48 h (64 fractions)

The water solubility was found to be below the quantification limit of 28 µg/L.

In both columns the concentration of five consecutive fractions was constant within ± 30 %. No increasing or decreasing tendency was observed.

Table 6: Coating check

	Amount of test item used for coating /mg	Measured concentration of test item in eluate /mg/L	Amount of test item eluted / mg
Column 12.5 mL/h	25	15.864/15.511	15.7
Column 25 mL/h		21.828/21.553	21.7

The coating check was successful. Enough test item remained on the columns. The water solubility cs of the test item was below the quantification limit of 28 µg/L (mean value of the columns).

Conclusions:

The water solubility of the test item at a temperature of 20°C was determined according to the column elution method. It was found to be below the quantification limit: < 0.03 mg/L

Executive summary:

 The water solubility of the test item was determined according to OECD 105 and Regulation (EC) No. 440/2008 method A.6 using the column elution method with HPLC analysis. About 100.1 mg of the test item were dissolved in 100 mL acetone. For charging the columns in each case 25 mL of the test item solution was added to about 3 g of sea sand and the mixtures were shaken. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, approx. 10mbar). The dry residues were placed into the columns of the test apparatus, which have afterwards been filled with water (test temperature: 20 °C; water pH at 23 °C: 6.0). After a swelling time of 2 h pumps were started to rinse the test item coated sand with demineralized water. At the end of the study it was confirmed that residual test item remained on the columns. The residual test item was eluted with 50 mL acetone. The concentration of test item was determined by means of HPLC. The pH of each sample was recorded. The water solubility of the test item at a temperature of 20°C was found to be below the quantification limit: < 0.03 mg/L.

Description of key information

The water solubility of the test item at a temperature of 20°C was determined using the column elution method. It was found to be below the quantification limit: < 0.03 mg/L

Additional information

The water solubility of the test item was determined according to OECD 105 and Regulation (EC) No. 440/2008 method A.6 using the column elution method with HPLC analysis (reference 4.8-1). About 100.1 mg of the test item were dissolved in 100 mL acetone. For charging the columns in each case 25 mL of the test item solution was added to about 3 g of sea sand and the mixtures were shaken. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, approx. 10mbar). The dry residues were placed into the columns of the test apparatus, which have afterwards been filled with water (test temperature: 20 °C; water pH at 23 °C: 6.0). After a swelling time of 2 h pumps were started to rinse the test item coated sand with demineralized water. At the end of the study it was confirmed that residual test item remained on the columns. The residual test item was eluted with 50 mL acetone. The concentration of test item was determined by means of HPLC. The pH of each sample was recorded. The water solubility of the test item at a temperature of 20°C was found to be below the quantification limit: < 0.03 mg/L.