Petroleum resins

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

05. Jul. 2018 to 13. Jul. 2018

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:

yes

Remarks:

See "Any other information" for details

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:

>= 0.35 - <= 0.81 mg/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

>= 6.22 - <= 7.42

Details on results:

The solubility of PETROLEUM RESINS (KENDEX 0897) in water was determined from the measured concentrations of DOC in the filtrated test solutions. The carbon content of the test item 86.54 % was used in the calculation of the test item concentration from the measured DOC concentration.
A dependency of the water solubility on the amount of the test item added was observed in the prelimi-nary test. Therefore, different loading rates (1 – 10 g/L) were used in the main test. Higher nominal load range was chosen as the solubility of the test item in the preliminary test was ≤ 1 mg/L. According to the guideline the flask method (slow-stirring) was used for the determination of the solubility of the test item in water.
As solubility was also dependent on nominal concentration in the main test, no exact value for the solubil-ity of the test item in water can be stated. The solubility range for the tested nominal concentration 1 – 10 g/L is 0.35 – 0.81 mg/L, corresponding to 0.04 – 0.01 % of the test item relating to the nominal concentration of the test item.
Dependency of pH value on amount of the test item (nominal load) was also perceived.
No observations arousing doubts concerning the accuracy of the results and the validity of the study were made.

Measurements during Equilibration

The data which was acquired during equilibration time (flask 1A-C, days 1 – 3, triplicate measurement) is presented in the following table:

 

Equilibration

Day	Flask #	Temperature [°C]	pH*	Measured Areas	Concentration DOC Mean [mg/L]	Conc. test item [mg/L]	Difference [%]
1	1A	20.0	6-7	1062 1120 1045	0.72	0.83	-
2	1B	20.0	6-7	1076 1109 1126	0.75	0.86	+3.6
3	1C	20.0	6-7	1026 1047 1035	0.68	0.79	-8.4
3 (blank)	-	19.5	6-7	170 278 303	< 0.1	-	-

*measured via pH paper

 

The carbon content of the test item 86.54 % was used in the calculation of the test item concentration from the measured DOC concentration.

After the analysis of the sample of day 3, the plateau was considered as reached.

 

Measurements at Plateau

The measured DOC concentrations in flasks 2 – 6 are presented in the following table:

 

Plateau

Flask	pH*	Temperature [°C]	Measured Areas	Concentration DOC Mean [mg/L]	Conc. test item [mg/L]
2	7.42	20.5	660 627 597	0.31	0.35
3	6.82	20.5	683 633 661	0.33	0.39
4	6.48	20.5	774 806 809	0.46	0.53
5	6.66	20.5	914 922 900	0.57	0.66
6	6.22	20.5	1026 1072 1068	0.70	0.81

*measured via calibrated pH meter

 

The results from the flasks 1A – 1C were used during the equilibration time only. All results in the flasks 2 – 6 are summarized in the following table:

 

Measurements used for Calculation of Solubility

Flask #	Measured Conc. Test Item [mg/L]	Nominal Conc. Test Item [g/L]	Dissolved Part [%]	pH
2	0.35	1.0	0.035	7.42
3	0.39	3.0	0.013	6.82
4	0.53	6.0	0.009	6.48
5	0.66	8.0	0.008	6.66
6	0.81	10.0	0.008	6.22

 

Dependency of solubility on amount of the test item (nominal load) was perceived in the main test.

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 1 – 10 g/L is 0.35 – 0.81 mg/L, corresponding to 0.04 – 0.01 % of the test item relating to the nominal concentration of the test item.

 

Dependency of pH value on amount of the test item (nominal load) was perceived, too.

Conclusions:

As solubility was dependent on nominal concentration, no exact value for the solubility of the test item in water can be stated:
0.35 – 0.81 mg/L at 20.0 ± 0.5 °C
0.35 – 0.81 * 10-3 kg/m3 (SI units)
for the following nominal concentration range of the test item in water: 1 – 10 g/L.

0.04 – 0.01 % of the test item relating to the nominal concentration of the test item was dissolved in wa-ter.

Executive summary:

Determination of the solubility in water of PETROLEUM RESINS (KENDEX 0897) according to OECD 105 resp. EU A.6

 

Findings and Results:

The solubility of the test item PETROLEUM RESINS (KENDEX 0897) 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 mg/L and 1000 mg/L were shaken at room temperature for 96.8 h and measured for DOC after membrane filtration (0.45 µm, PTFE). Undissolved particles were observed in the flasks. The measured DOC concentration lay at 0.2 mg/L and 1.0 mg/L in the flasks with the nominal concentrations 10 mg/L and 1000 mg/L, respectively. As dependency of the water solubility on the amount of the test item added was observed, different loading rates were used in the main test. According to the guideline the flask method (slow-stirring) was used for the determination of the solubility of the test item in water.

 

In the main test, six different loading rates of the test item were chosen to study the effect of the loading rate on the measured water solubility: 1, 3, 5, 6, 8 and 10 g/L. Three flasks 1A - C with the same loading rate (5 g/L) were used during equilibration only. Seven vessels (flasks blank, 1C (for the sampling point 72 h) and 2 – 6) were set onto the shaking apparatus immediately and shaking (vertical) without agitator at 100 rpm was started. 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). Due to a difference of less than 15 % in the concentrations on days 2 and 3 and no upward tendency in the three values, the test was finished. The final measurement was performed as determination from flasks 2 – 6 and the values were used for evaluation. 

 

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.

The following results were observed in the flasks 2 – 6:

 

Measurements used for Calculation of Solubility

Flask #	Measured Conc. Test Item [mg/L]	Nominal Conc. Test Item [g/L]	Dissolved Part [%]	pH
2	0.35	1.0	0.035	7.42
3	0.39	3.0	0.013	6.82
4	0.53	6.0	0.009	6.48
5	0.66	8.0	0.008	6.66
6	0.81	10.0	0.008	6.22

 

Dependency of solubility on amount of the test item (nominal load) was perceived in the main test.

Dependency of pH value on amount of the test item (nominal load) was also perceived.

 

As solubility was dependent on nominal concentration, no exact value for the solubility of the test item in water can be stated:

 

0.35 – 0.81 mg/L at 20.0 ± 0.5 °C

0.35 – 0.81 * 10-3 kg/m³(SI units)

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

 

0.04 – 0.01 % of the test item relating to the nominal concentration of the test item was dissolved in water.

Description of key information

As solubility was dependent on nominal concentration, no exact value for the solubility of the test item in water can be stated:

 

0.35 – 0.81 mg/L at 20.0 ± 0.5 °C

0.35 – 0.81 * 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:

0.81 mg/L

at the temperature of:

20 °C

Additional information

The solubility of the test item PETROLEUM RESINS (KENDEX 0897) 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 mg/L and 1000 mg/L were shaken at room temperature for 96.8 h and measured for DOC after membrane filtration (0.45 µm, PTFE). Undissolved particles were observed in the flasks. The measured DOC concentration lay at 0.2 mg/L and 1.0 mg/L in the flasks with the nominal concentrations 10 mg/L and 1000 mg/L, respectively. As dependency of the water solubility on the amount of the test item added was observed, different loading rates were used in the main test. According to the guideline the flask method (slow-stirring) was used for the determination of the solubility of the test item in water.

 

In the main test, six different loading rates of the test item were chosen to study the effect of the loading rate on the measured water solubility: 1, 3, 5, 6, 8 and 10 g/L. Three flasks 1A - C with the same loading rate (5 g/L) were used during equilibration only. Seven vessels (flasks blank, 1C (for the sampling point 72 h) and 2 – 6) were set onto the shaking apparatus immediately and shaking (vertical) without agitator at 100 rpm was started. 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). Due to a difference of less than 15 % in the concentrations on days 2 and 3 and no upward tendency in the three values, the test was finished. The final measurement was performed as determination from flasks 2 – 6 and the values were used for evaluation. 

 

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.

The following results were observed in the flasks 2 – 6: 

Measurements used for Calculation of Solubility

Flask #	Measured Conc. Test Item [mg/L]	Nominal Conc. Test Item [g/L]	Dissolved Part [%]	pH
2	0.35	1.0	0.035	7.42
3	0.39	3.0	0.013	6.82
4	0.53	6.0	0.009	6.48
5	0.66	8.0	0.008	6.66
6	0.81	10.0	0.008	6.22

 

Dependency of solubility on amount of the test item (nominal load) was perceived in the main test.

Dependency of pH value on amount of the test item (nominal load) was also perceived.

 

As solubility was dependent on nominal concentration, no exact value for the solubility of the test item in water can be stated:

 

0.35 – 0.81 mg/L at 20.0 ± 0.5 °C

0.35 – 0.81 * 10-3 kg/m³(SI units)

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

 

0.04 – 0.01 % of the test item relating to the nominal concentration of the test item was dissolved in water.