Decanoic acid, mixed esters with heptanoic acid, octanoic 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:

08 Dec. 2016 to 13 Oct. 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

OECD Guidelines for the Testing of Chemicals, Method No. 105, adopted 27. Jul. 1995: “Water Solubility “

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

Commission Regulation (EU) No 260/2014 amending Regulation (EC) No 440/2008: Method A.6: “Water solubility, adopted 24 January 2014.

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Specific details on test material used for the study:

No further details specified in the study report.

Key result

Water solubility:

< 0.14 mg/L

Conc. based on:

test mat.

Temp.:

20 °C

Remarks on result:

other: pH not specified

Details on results:

Main Test 1
Measurements during Equilibration
The TC content of the test item was determined under non-GLP conditions in the laboratory Mikroanalytisches Labor Pascher (D-53424 Remagen) with 69.17 % and the value was used in the calculation of the test item concentration from the measured DOC concentration.
The measured value in the blank flask lay below the LOQ of TOC (< 1.35 mg/L).
Temperature was measured with 20.0 ± 0.5°C.
Results
All measured values in the flasks 2 – 6 lay below the LOQ of TOC (< 1.35 mg/L) corresponding to the concentration of the test item in water < 1.95 mg/L.
As dependency of the water solubility on the amount of the test item added was always perceived for such complex substances as the test item, the solubility lower than 0.002 % of the test item was stated relating to the highest nominal concentration of the test item 100 g/L.

Main Test 2
Measurements during Equilibration
The carbon content of the test item 69.17 % was used in the calculation of the test item concentration from the measured DOC concentration. The measured value in the blank flask was subtracted from the measured value in the flasks 1A – 1C.
After the analysis of the sample of day 3, the plateau was considered as reached.
Measurements at Plateau
The measured value in the blank flask 0.15 mg/L was subtracted from the measured value in the flasks 2 – 6.
Temperature was measured with 20.0 °C.
Results
The measurements on day 3 (flasks 1A – 1C and 2 – 6) were included in the calculation of the solubility of the test item in water.
As solubility was dependent on nominal concentration, no exact value for the solubility of the test item in water can be stated. The solubility range for the tested nominal concentration 30 – 100 g/L is 0.67 – 1.72 mg/L (or ≤ 1.72 mg/L), corresponding to ≤ 0.0018 % of the test item relating to the nominal concentration of the test item.

Main Test 3
Measurements during Equilibration
The measured value in the blank flask lay also below the LOQ of TOC (< 0.1 mg/L).
Measurements at Plateau
The measured value in the blank flask lay also below the LOQ of TOC (< 0.1 mg/L).
Temperature was measured with 20.0 °C.
Results
The measured values in the flasks 1A – 1C and 3 – 5 lay below the LOQ of TOC (< 0.1mg/L) corresponding to the concentration of the test item in water < 0.14 mg/L (for nominal loadings range of 1 – 10 g/L).

Main Test 1

Equilibration

Day	Temperature [°C]	pH*	Concentration DOC [mg/L]	Concentration test item [mg/L]
1	20.0	6	< 1.35	< 1.95
2	20.0	6	< 1.35	< 1.95
3	19.5	6	< 1.35	< 1.95
4	20.5	6	< 1.35	< 1.95
5	20.5	6	< 1.35	< 1.95
6	20.0	6	< 1.35	< 1.95

*measured via pH paper

 

Plateau

Flask	pH*	Concentration DOC [mg/L]	Concentration test item [mg/L]
2	6.58	< 1.35	< 1.95
3	6.50	< 1.35	< 1.95
4	6.44	< 1.35	< 1.95
5	6.51	< 1.35	< 1.95
6	6.50	< 1.35	< 1.95

*measure via calibrated pH meter

 

Main Test 2

Equilibration

Day	Temperature [°C]	pH*	Measured Areas	Concentration DOC Mean [mg/L]	Conc. DOC – blank [mg/L]	Conc. test item [mg/L]	Difference [%]
1	20.0	6	1071 1193 1113	0.62	0.47	0.68	-
2	20.0	6	1195 1316 1170	0.71	0.56	0.82	+20.4
3	20.0	6	1162 1212 1172	0.67	0.52	0.76	-7.5
3 (blank)	20.0	6-7	625 677 583	0.15	-	-	-

*measured via pH paper

 

Plateau

Flask	pH*	Measured Areas	Concentration DOC Mean [mg/L]	Conc. DOC – blank [mg/L]	Conc. test item [mg/L]
2	5.89	1872 1629 1740	1.20	1.06	1.53
3	5.49	1103 1155 1093	0.61	0.46	0.67
4	5.80	1234 1341 1303	0.78	0.63	0.91
5	5.78	1878 1925 1856	1.34	1.19	1.72
6	5.96	1706 1818 1659	1.19	1.04	1.50

*measured via calibrated pH meter

 

Measurements used for Calculation of Solubility

Flask	Measured Conc. Test Item [mg/L]	Nominal Conc. Test Item [mg/L]	Dissolved Part [%]
2	1.53	10	0.0153*
3	0.67	30	0.0022
1**	0.75	50	0.0015
4	0.91	60	0.0015
5	1.72	80	0.0021
6	1.50	100	0.0015

*the value was stated as an outlier (Grubbs test) and was not used in the evaluation

**mean value of flask 1A – 1C

 

Main Test 3

Equilibration

Day	Temperature [°C]	pH*	Measured Areas	Concentration DOC Mean [mg/L]	Conc. test item [mg/L]
1	20.0	6-7	333 443 402	< 0.1	< 0.14
2	20.0	6-7	381 467 477	< 0.1	< 0.14
3	20.0	6-7	359 461 424	< 0.1	< 0.14
5	20.0	6-7	440 596 580	< 0.1	< 0.14
6	20.0	6-7	519 498 510	< 0.1	< 0.14
7	20.0	6-7	531 593 544	< 0.1	< 0.14

*measured via pH paper

 

Plateau

Flask	pH*	Measured Areas	Concentration DOC Mean [mg/L]	Conc. test item [mg/L]
2	6.04	670 776 745	0.25**	0.35**
3	5.96	446 456 428	< 0.1	< 0.14
4	6.02	423 461 462	< 0.1	< 0.14
5	5.78	515 570 613	< 0.1	< 0.14
6	5.96	664 813 845	0.29**	0.41**

*measured via calibrated pH meter

**the values were stated as outlier, as in all other flasks 1A – 1C and 3 – 5 values lay below the LOQ of TOC 0.1 mg/L

Conclusions:

Therefore, the concentration of the test item in water in the main test 1 was stated as
< 1.95 mg/L at 20.0 ± 0.5 °C
< 1.95 * 10-3 kg/m3 (SI units)
As dependency of the water solubility on the amount of the test item added was always perceived for such complex substances as the test item, the solubility was also stated as < 0.002 % (relating to the highest nominal concentration of the test item 100 g/L).
As the measured values from the main test 1 lay below the LOQ of TOC (< 1.35 mg/L), the test was repeated (main test 2) using the vario TOC cube as the analytical instrument with the LOQ of TOC 0.1 mg/L as described above. Because of a difference of less than 15 % in the concentrations on days 2 and 3 and no upward tendency, the test was finished on day 3. The concentration of the test item in water was measured in the range of 0.67 – 1.72 mg/L as the solubility was dependent on nominal concentration.
Therefore, the solubility in the main test 2 was stated as
≤ 1.72 mg/L at 20.0 °C
≤ 1.72 * 10-3 kg/m3 (SI units)
for the following nominal concentration range of the test item in water: 30 – 100 g/L.
As dependency of the water solubility on the amount of the test item added was perceived the solubility was also stated as ≤ 0.0018 %.
In order to confirm a dependency of the water solubility on the amount of the test item added, the test was repeated with lower range of the nominal load (1 – 10 g/L) again (main test 3). Because of the measured values lay below the LOQ of TOC on days 1 – 3 and 5 – 7, the test was finished.
Therefore, the concentration of the test item in water in the main test 3 was stated as
< 0.14 mg/L at 20.0 °C
< 0.14 * 10-3 kg/m3 (SI units)
for the following nominal concentration range of the test item in water: 1 – 10 g/L.

Executive summary:

The solubility of the test item Hatcol 3178 in water was determined by measurement of DOC concentration in the filtrated test solutions using TOC analyser.

In the pre-test, flasks with nominal concentrations 10.4 mg/L and 1003 mg/L were shaken at room temperature for 90 h and measured for DOC after membrane filtration (0.45 μm, PTFE). Undissolved particles were observed in the flasks. The measured DOC concentration lay below the LOQ of TOC (< 1.35 mg/L) in both flasks. As dependency of the water solubility on the amount of the test item added was perceived for such complex substances as the test item, different loading rates were used in the main test.

In the main test 1, six different loading rates of the test item were chosen to study the effect of the loading rate on the measured water solubility: 10.02, 30.01, 50.01, 60.01, 80.02 and 100.00 g/L. Three flasks 1A - C with the same loading rate (50.00 – 50.01 g/L) were used during equilibration. Seven vessels (flasks blank, 1C (for the sampling point 72 h) and 2 – 6) were set onto the shaking apparatus immediately. After 24 ± 2 hours, flask 1B (for the sampling point 48 h) and after 48 ± 2 hours, flask 1A (for the sampling point 24 h) were set on the shaker and all flasks were shaken for further 24 ± 2 hours at room temperature (20.0 ± 0.5 °C). Then, flasks 1A - 1C were removed from the shaker, samples were taken, membrane filtered and analysed for DOC via TOC analyser. As the measured values lay below the LOQ of TOC (< 1.35 mg/L), the test was prolonged and the flasks 1AC were measured on days 4 – 6. Because the measured values lay below the LOQ of TOC on days 5 and 6, the test was finished. The final measurement was performed as determination from flasks 2 – 6.

No Tyndall effect (i.e. a laser beam was not scattered when transmitted through the liquid) could be observed indicating that no colloidal dispersed particles were present.

All measured values in the flasks 2 – 6 lay below the LOQ (limit of quantification) of TOC (< 1.35 mg/L). The TC content of the test item 69.17 % was used in the calculation of the test item concentration from the measured DOC concentration.

 

Therefore, the concentration of the test item in water in the main test 1 was stated as

< 1.95 mg/L at 20.0 ± 0.5 °C

< 1.95 * 10-3 kg/m3 (SI units)

As dependency of the water solubility on the amount of the test item added was always perceived for such complex substances as the test item, the solubility was also stated as

< 0.002 %

(relating to the highest nominal concentration of the test item 100 g/L).

 

As the measured values from the main test 1 lay below the LOQ of TOC (< 1.35 mg/L), the test was repeated (main test 2) using the vario TOC cube as the analytical instrument with the LOQ of TOC 0.1 mg/L as described above. Because of a difference of less than 15 % in the concentrations on days 2 and 3 and no upward tendency, the test was finished on day 3. The concentration of the test item in water was measured in the range of 0.67 – 1.72 mg/L as the solubility was dependent on nominal concentration.

 

Therefore, the solubility in the main test 2 was stated as

≤ 1.72 mg/L at 20.0 °C

≤ 1.72 * 10-3 kg/m3 (SI units)

for the following nominal concentration range of the test item in water: 30 – 100 g/L.

As dependency of the water solubility on the amount of the test item added was perceived the solubility was also stated as ≤ 0.0018 %.

 

In order to confirm a dependency of the water solubility on the amount of the test item added, the test was repeated with lower range of the nominal load (1 – 10 g/L) again (main test 3). Because of the measured values lay below the LOQ of TOC on days 1 – 3 and 5 – 7, the test was finished.

 

Therefore, the concentration of the test item in water in the main test 3 was stated as

< 0.14 mg/L at 20.0 °C

< 0.14 * 10-3 kg/m3 (SI units)

for the following nominal concentration range of the test item in water: 1 – 10 g/L.

Description of key information

The concentration of the test item in water in the main test 3 was stated as

< 0.14 mg/L at 20.0 °C

< 0.14 * 10-3 kg/m3 (SI units)

for the following nominal concentration range of the test item in water: 1 – 10 g/L.

Key value for chemical safety assessment

Water solubility:

0.14 mg/L

at the temperature of:

20 °C

Additional information

The solubility of the test item Hatcol 3178 in water was determined by measurement of DOC concentration in the filtrated test solutions using TOC analyser.

In the pre-test, flasks with nominal concentrations 10.4 mg/L and 1003 mg/L were shaken at room temperature for 90 h and measured for DOC after membrane filtration (0.45 μm, PTFE). Undissolved particles were observed in the flasks. The measured DOC concentration lay below the LOQ of TOC (< 1.35 mg/L) in both flasks. As dependency of the water solubility on the amount of the test item added was perceived for such complex substances as the test item, different loading rates were used in the main test.

In the main test 1, six different loading rates of the test item were chosen to study the effect of the loading rate on the measured water solubility: 10.02, 30.01, 50.01, 60.01, 80.02 and 100.00 g/L. Three flasks 1A - C with the same loading rate (50.00 – 50.01 g/L) were used during equilibration. Seven vessels (flasks blank, 1C (for the sampling point 72 h) and 2 – 6) were set onto the shaking apparatus immediately. After 24 ± 2 hours, flask 1B (for the sampling point 48 h) and after 48 ± 2 hours, flask 1A (for the sampling point 24 h) were set on the shaker and all flasks were shaken for further 24 ± 2 hours at room temperature (20.0 ± 0.5 °C). Then, flasks 1A - 1C were removed from the shaker, samples were taken, membrane filtered and analysed for DOC via TOC analyser. As the measured values lay below the LOQ of TOC (< 1.35 mg/L), the test was prolonged and the flasks 1AC were measured on days 4 – 6. Because the measured values lay below the LOQ of TOC on days 5 and 6, the test was finished. The final measurement was performed as determination from flasks 2 – 6.

No Tyndall effect (i.e. a laser beam was not scattered when transmitted through the liquid) could be observed indicating that no colloidal dispersed particles were present.

All measured values in the flasks 2 – 6 lay below the LOQ (limit of quantification) of TOC (< 1.35 mg/L). The TC content of the test item 69.17 % was used in the calculation of the test item concentration from the measured DOC concentration.

 

Therefore, the concentration of the test item in water in the main test 1 was stated as

< 1.95 mg/L at 20.0 ± 0.5 °C

< 1.95 * 10-3 kg/m3 (SI units)

As dependency of the water solubility on the amount of the test item added was always perceived for such complex substances as the test item, the solubility was also stated as

< 0.002 %

(relating to the highest nominal concentration of the test item 100 g/L).

 

As the measured values from the main test 1 lay below the LOQ of TOC (< 1.35 mg/L), the test was repeated (main test 2) using the vario TOC cube as the analytical instrument with the LOQ of TOC 0.1 mg/L as described above. Because of a difference of less than 15 % in the concentrations on days 2 and 3 and no upward tendency, the test was finished on day 3. The concentration of the test item in water was measured in the range of 0.67 – 1.72 mg/L as the solubility was dependent on nominal concentration.

 

Therefore, the solubility in the main test 2 was stated as

≤ 1.72 mg/L at 20.0 °C

≤ 1.72 * 10-3 kg/m3 (SI units)

for the following nominal concentration range of the test item in water: 30 – 100 g/L.

As dependency of the water solubility on the amount of the test item added was perceived the solubility was also stated as ≤ 0.0018 %.

 

In order to confirm a dependency of the water solubility on the amount of the test item added, the test was repeated with lower range of the nominal load (1 – 10 g/L) again (main test 3). Because of the measured values lay below the LOQ of TOC on days 1 – 3 and 5 – 7, the test was finished.

 

Therefore, the concentration of the test item in water in the main test 3 was stated as

< 0.14 mg/L at 20.0 °C

< 0.14 * 10-3 kg/m3 (SI units)

for the following nominal concentration range of the test item in water: 1 – 10 g/L.