Reaction product of 3,5,5-trimethyl-hexanoic acid and 2-methylpropanoic acid and pentaerythritol

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 July 2011 - 09 February 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Study was conducted in accordance with International guidelines and GLP. All guideline validity criteria were met.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

27 July 1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

Commission Regulation (EC) No 440/2008 laying down test methods pursuant to Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH).

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Specific details on test material used for the study:

RADIOLABELLING INFORMATION (if applicable)
- Radiochemical purity: N/A
- Specific activity: N/A
- Locations of the label: N/A
- Expiration date of radiochemical substance: N/A

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: Room temperature in the dark and under nitrogen.
- Stability under test conditions: Assumed stable.
- Solubility and stability of the test substance in the solvent/vehicle: N/A, applied as supplied.
- Reactivity of the test substance with the solvent/vehicle of the cell culture medium: N/A

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: N/A
- Preliminary purification step (if any): N/A
- Final dilution of a dissolved solid, stock liquid or gel: N/A
- Final preparation of a solid: N/A

FORM AS APPLIED IN THE TEST (if different from that of starting material): Applied as supplied.

TYPE OF BIOCIDE/PESTICIDE FORMULATION (if applicable): N/A

OTHER SPECIFICS: No

Key result

Water solubility:

<= 2.5 mg/L

Conc. based on:

test mat.

Loading of aqueous phase:

1 g/L

Incubation duration:

>= 3 - <= 7 d

Temp.:

20 °C

pH:

>= 6.9 - <= 7.1

Details on results:

The detector calibration was found to be linear for each component over the approximate range 0 to 5 mg/L of standard solutions in acetonitrile:water (1:1 v/v).

A measured value of approximately 2.5 mg/L was determined for the lowest molecular weight component at 4.8 minutes, whilst other significant components were below the limit of quantification (approximately 1 mg/l). Computer modelling (WSKOWWIN, Version 1.41, U.S. Environmental Protection Agency) indicated that the values for these components would fall significantly below this order of magnitude.

An acceptable mean recovery of approximately 106 % of Tetraesters of pentaerythritol with 2- methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid from fortified samples was achieved and considered to be acceptable.

Table 1       Measurement of solubility at 20 ºC

Retention time of component (mins)	Replicate	Sampling time (days)	Concentration (mg/L)	Mean concentration (mg/L)	Sample pH
4.8	A	3	2.72	2.26	7.0
	B		1.80		6.9
	C	4	2.71	2.69	7.0
	D		2.68		7.1
	E	7	2.88	2.67	7.0
	F		2.47		7.0
6.1	A	3	<LOQ	<LOQ	7.0
	B		<LOQ		6.9
	C	4	<LOQ	<LOQ	7.0
	D		<LOQ		7.1
	E	7	<LOQ	<LOQ	7.0
	F		<LOQ		7.0
7.9	A	3	<LOQ	<LOQ	7.0
	B		<LOQ		6.9
	C	4	<LOQ	<LOQ	7.0
	D		<LOQ		7.1
	E	7	<LOQ	<LOQ	7.0
	F		<LOQ		7.0
10.5	A	3	<LOQ	<LOQ	7.0
	B		<LOQ		6.9
	C	4	<LOQ	<LOQ	7.0
	D		<LOQ		7.1
	E	7	<LOQ	<LOQ	7.0
	F		<LOQ		7.0

LOQ = 1 mg/L

Conclusions:

The lowest molecular weight component of Tetraesters of pentaerythritol with 2- methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid was found to have a water solubility of 2.5 mg/L at 20 °C, whilst other significant components had solubilities below 1 mg/L.

Executive summary:

OECD 105 (2012) - A modified flask method employing slow stirring was used, this being deemed most appropriate for the oily test substance. This involved sampling the saturated aqueous solution from the bottom of the test sample, thus eliminating potential contamination (the test substance floats on water) and precluding the need for filtration or centrifugation.

 

A 2 L glass aspirator bottle containing approximately 2 g of test substance and 2000 mL of purified water was sealed and placed on a magnetic stirrer in a temperature controlled room at 20 °C. Stirring was started, the glass stir bar speed being adjusted to a very slow speed resulting in a minimal vortex. At 3, 4 and 7 days, stirring was stopped in the sample and duplicate portions removed for analysis. An aliquot (5 mL) of each was diluted to volume (10 mL) with acetonitrile for analysis by high performance liquid chromatography (HPLC). The pH of each sample was also recorded.

 

A control system was similarly set up, but without test substance. Portions of this were similarly analysed on each sampling occasion. The efficiency of sample processing was also investigated by fortifying portions (10 mL) of purified water with an aliquot (80 μL) of a solution of the test substance in acetonitrile (approximately 1 g/L) and then processing as for the samples as detailed above.

 

The detector calibration was found to be linear for each component over the approximate range 0 to 5 mg/L of standard solutions in acetonitrile:water (1:1 v/v).

 

A measured value of approximately 2.5 mg/L was determined for the lowest molecular weight component at 4.8 minutes, whilst other significant components were below the limit of quantification (approximately 1 mg/L).

An acceptable mean recovery of approximately 106 % of Tetraesters of pentaerythritol with 2-methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid from fortified samples was achieved and considered to be acceptable.

 

In conclusion, the lowest molecular weight component of Tetraesters of pentaerythritol with 2-methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid was found to have a water solubility of 2.5 mg/L at 20 °C, whilst other significant components had solubilities below 1 mg/L.

Description of key information

Water solubility = ≤ 2.5 mg/L at 20 ºC; OECD 105; Sydney, P. (2012)

Key value for chemical safety assessment

Water solubility:

2.5 mg/L

at the temperature of:

20 °C

Additional information

OECD 105 (2012) - A modified flask method employing slow stirring was used, this being deemed most appropriate for the oily test substance. This involved sampling the saturated aqueous solution from the bottom of the test sample, thus eliminating potential contamination (the test substance floats on water) and precluding the need for filtration or centrifugation.

 

A 2 L glass aspirator bottle containing approximately 2 g of test substance and 2000 mL of purified water was sealed and placed on a magnetic stirrer in a temperature controlled room at 20 °C. Stirring was started, the glass stir bar speed being adjusted to a very slow speed resulting in a minimal vortex. At 3, 4 and 7 days, stirring was stopped in the sample and duplicate portions removed for analysis. An aliquot (5 mL) of each was diluted to volume (10 mL) with acetonitrile for analysis by high performance liquid chromatography (HPLC). The pH of each sample was also recorded.

 

A control system was similarly set up, but without test substance. Portions of this were similarly analysed on each sampling occasion. The efficiency of sample processing was also investigated by fortifying portions (10 mL) of purified water with an aliquot (80 μL) of a solution of the test substance in acetonitrile (approximately 1 g/L) and then processing as for the samples as detailed above.

 

The detector calibration was found to be linear for each component over the approximate range 0 to 5 mg/L of standard solutions in acetonitrile:water (1:1 v/v).

 

A measured value of approximately 2.5 mg/L was determined for the lowest molecular weight component at 4.8 minutes, whilst other significant components were below the limit of quantification (approximately 1 mg/L).

An acceptable mean recovery of approximately 106 % of Tetraesters of pentaerythritol with 2- methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid from fortified samples was achieved and considered to be acceptable.

 

In conclusion, the lowest molecular weight component of Tetraesters of pentaerythritol with 2- methylpropanoic acid and 3,5,5-trimethyl-hexanoic acid was found to have a water solubility of 2.5 mg/L at 20 °C, whilst other significant components had solubilities below 1 mg/L.