Dodecanoic acid, ester with 1,2-propanediol

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 Jun - 10 Dec 2018

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2019

Report date:

2019

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

yes

Remarks:

adaptation to flask method and slow-stirring method; see "Any other information on materials and methods incl. tables".

GLP compliance:

yes

Type of method:

other: Slow-stirring method

Test material

Test material information

Constituent 1

Reference substance name:

Dodecanoic acid, ester with 1,2-propanediol

EC Number:

253-462-2

EC Name:

Dodecanoic acid, ester with 1,2-propanediol

Cas Number:

37321-62-3

Molecular formula:

C15H30O3 C27H52O4

IUPAC Name:

Dodecanoic acid, ester with 1,2-propanediol

Results and discussion

Water solubility

Water solubility:

<= 1.28 mg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: The solubility was measured considering the two major constituents separately: <0.24 mg/L (below LoQ) for the diester constituent, 1.28 mg/L for the monoester constituent. The solubility of the monoester is taken as a conservative upper limit.

Any other information on results incl. tables

Preliminary test results

Test item quantity (mg)	106.9	106.9	106.9	106.9	106.9	113.6
Volume of water added (mL)	0.1	0.5	1	2	10	100
Time of shake (h)	0.1	0.1	0.1	0.1	0.1	48
Observation	Not dissolved. Presence of an oil	Not dissolved. Presence of an oil	Not dissolved. Presence of an oil	Not dissolved. Presence of an oil	Not dissolved. Presence of an oil	Not dissolved. Presence of an oil
Solubility observed (g/L)	1069	213.8	106.9	53.45	10.69	1.136

 

Conclusion of the preliminary test: Due to the presence of lots of suspended particles at the tested solubility 1 g/L, the solubility was estimated to be < 10 mg/L.

The behaviour of the test item like an oil permitted to anticipate that the loading of the column was a critical phase. Therefore, an amendment was signed to realise a slow-stirring method.

An adaptation of the shake flask method was also realised (non-GLP) to observe the consequence of vigorous agitation on the kinetic of the solubility.

 

 

Adapted flask method results

Only one phase was observed so the flasks were centrifuged at 20 °C and 4500 rpm during 2h

The centrifugation did not permit to separate the phases. Only one white phase was observed. So the sampling could not be realised.

The solubility could not be measured because only one white phase was observed.

 

 

Slow-stirring method results

 

Quantification results

 

Description	Sampling n#	Concentration [mg/L]
		Monoester 1	Diester 1
R01	1	2.37	< LOQ*
	2	2.87	< LOQ*
	3	2.45	< LOQ*
	4	2.26	< LOQ*
	5	2.09	< LOQ*
	6	2.30	< LOQ*
R02	1	2.57	< LOQ*
	2	3.01	< LOQ*
	3	2.74	< LOQ*
	4	2.92	< LOQ*
	5	2.48	< LOQ*
	6	2.63	< LOQ*
R03	1	2.34	< LOQ*
	2	3.56	< LOQ*
	3	2.77	< LOQ*
	4	3.00	< LOQ*
	5	2.47	< LOQ*
	6	2.54	< LOQ*
	* LOQ:	0.10	0.50

* LOQ = Limit of quantification (available in the last row of the table).

 

Water solubility calculation

Using results of the certificate of analysis provided by the sponsor, equivalent to each substance quantified was calculated:

 

	Peak of Monoester 1	Peak of Diester 1
Area Sum % of the test tiem	51.4 %	48.3 %

 

Description	Sampling n#	Equivalent concentration in test item [mg/L]
		Monoester 1	Diester 1
R01	1	1.22	< LOQ*
	2	1.48	< LOQ*
	3	1.26	< LOQ*
	4	1.16	< LOQ*
	5	1.07	< LOQ*
	6	1.18	< LOQ*
R02	1	1.32	< LOQ*
	2	1.55	< LOQ*
	3	1.41	< LOQ*
	4	1.50	< LOQ*
	5	1.27	< LOQ*
	6	1.35	< LOQ*
R03	1	1.20	< LOQ*
	2	1.83	< LOQ*
	3	1.42	< LOQ*
	4	1.54	< LOQ*
	5	1.27	< LOQ*
	6	1.31	< LOQ*
	* LOQ:	0.05	0.24

* LOQ = Limit of quantification (available in the last row of the table).

 

The solubility at 20 °C of the test item was measured with the slow-stirring method after 10 days at 1.28 mg/L with the monoester quantification and < 0.24 mg/L with the diester quantification.

 

 

Validity criteria

The sampling difference ((S2-S1/S1) of the at least two last sampling would not differ by more than the analytical method MBA (30 %). This criterion was verifed for all flasks.

 

Description	Sampling n#	Equivalent concentration in test item [mg/L]		Sampling difference [%]		Validity criteria
		Monoester 1	Diester 1	Monoester 1	Diester 1	Monoester 1	Diester 1
R01	5	1.07	< LOQ*	10%	N/A**	< 30%	< 30%
	6	1.18	< LOQ*
R02	5	1.27	< LOQ*	6%	N/A**	< 30%	< 30%
	6	1.35	< LOQ*
R03	5	1.27	< LOQ*	3%	N/A**	< 30%	< 30%
	6	1.31	< LOQ*
	* LOQ:	0.05	0.24

* LOQ = Limit of quantification (available in the last row of the table).

** N/A: Not Applicable calculation because the quantification was < LOQ.

 

 

The relative standard deviation (RSD) between the sampling will not be upper than the analytical method MBA (30%). This criterion was verified.

 

Description	Sampling n#	Equivalent concentration in test item [mg/L]
		Monoester 1	Diester 1
R01	6	1.18	< LOQ
R02	6	1.35	< LOQ
R03	6	1.31	< LOQ
Average [mg/L]		1.28	< LOQ
RSD [%]		7 %	N/A*
RSD Validity Criteria		< 30 %	< 30%

* N/A: Not Applicable calculation because the quantification was < LOQ.

 

 

 

General conclusion

Using the flask method, the solubility at 20 °C of the test item could not be measured because only one phase was observed after centrifugation (4500 rpm ; 2 h ; 20 °C).

 

By applying the slow-stirring method, the solubility at 20 °C of the test item was measured after 10 days between < 0.24 mg/L to 1.28 mg/L in function of the ester measured.