Glycerides, tall-oil mono-

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

04. Jun. 2018 to 19. Jun 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

OECD Guideline No. 103 “Boiling Point“, dated 27. Jul. 1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

EU-Method A.2 dated 30. May 2008 published on 31. May. 2008, “Boiling Temperature“

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

No futher details specified in the study report.

Key result

Boiling pt.:

418.78 °C

Decomposition:

yes

Decomp. temp.:

> 328.46 - < 429.26 °C

Pre-test following Siwoloboff

All observations of the Pre-test following Siwoloboff are presented in the following table.

 

Pre-test following Siwoloboff

Observations	Temperatures in °C
The test item was getting clearer	50
The bubbles from the inside of the test item rose up	64
White streaks inside the test item like white flakes	138
Condensate visible	141
Single bubbles	330
More single bubbles	350
The test item boiled – boiling chain, gas burner turned off	405
Boiling chain broke up	398

 

After cooling down the test item was visually like the original test item.

 

Security Pre-test for the DSC instrument

The crucible was found visual changed after reaching a temperature of 450 °C. The top colour of the crucible was completely grey-brown coloured. Therefore, a second crucible with less test item was heated to 450 °C. This crucible was just brown at the perforation. The weight was recorded with 46.06 mg for the first crucible and 49.41 mg for the second.

 

Calibration

After calibration with indium and zinc the measurement of indium yielded the following values:

 

Values DSC Indium

Expected Melting point	Measured Melting point	Expected Energy	Measured Energy	Assessment
156.6 ± 1.0 °C	156.51 °C (onset)	28.45 ± 1.0 J/g	28.53 J/g	OK

 

The measurement of indium after calibration met the validity criteria.

 

DSC Measurement of the Test Item

Values DSC Test Item first determination

	Temperature [°C] Event marker	Heat flow [mW]
Beginning of the first Event	334.94	18.7712
Beginning of the second Event	406.26	18.1040

 

The temperature program of the further determinations was adapted (25 °C to 445 °C) as not all expected event was measured.

 

Values DSC Test Item second determination

	Temperature [°C] Event marker	Heat flow [mW]
Beginning of the decomposition	332.01	17.9685
Beginning of the endotherm peak	405.49	17.4326
Highest Point of the Peak	426.26	18.6813
Boiling point under decomposition	418.63	18.1849

 

Values DSC Test Item third determination

	Temperature [°C] Event marker	Heat flow [mW]
Beginning of the decomposition	328.46	18.6516
Beginning of the endotherm peak	409.49	17.7795
Highest Point of the Peak	427.60	19.1046
Boiling point under decomposition	418.92	18.5506

 

Observations

Values Observations

	Mass test item	Mass crucible (before measurement):	Mass crucible (after measurement):	Observations
First Crucible	2.81 mg	49.24 mg	47.78 mg	After the test the crucible was visually unchanged
Second Crucible	2.61 mg	47.95 mg	45.93 mg	After the test the crucible was visually unchanged. The crucible was opened after performance and the test item was darker (yellow) as before
Third Crucible	2.91 mg	48.38 mg	46.12 mg	After the test the crucible was visually unchanged

 

 

Interpretation of the measurements

In every measurement, a lowered baseline was detected, which could be a sign for decomposition of the test item. The beginning of decomposition was evaluated with the event marker function. Based on the observations of the pre-test and the visually change of the test item inside the crucible, the endotherm peak can be interpreted as boiling. As the left tangent of the left peak was detected the onset equates the event marker set there. As where the left half tangent of the peak meets the baseline correspond to intercept point the temperature of the onset value is calculable. The beginning and the peak maximum were evaluated with event marker, too.

 

Presentation of Results

All results are presented in the following table.

 

Results

Beginning of lowering of Baseline	in °C (event mark)	in K
1 Determination	334.94	608.09
2 Determination	332.01	605.16
3 Determination	328.46	601.61
Min	328.46	601.61

 

Beginning of event	in °C (event mark)	in K
1 Determination	406.26	679.41
2 Determination	405.49	678.64
3 Determination	409.49	682.62
Min	405.49	678.64

 

Peak max	in °C (event mark)	in K
1 Determination	Not completely detected
2 Determination	429.26	702.41
3 Determination	427.60	700.75

 

Boiling under decomposition	in °C (event mark)	in K
1 Determination	Not completely detected
2 Determination	418.63	691.78
3 Determination	418.92	692.07
Min	418.78	691.93

 

DISCUSSION

The boiling point was determined via DSC (differential scanning calorimetry).

Because of the specificity of the DSC 4000 (445°C is the highest measure temperature); no complete Peak could be detected.

The test item showed possible signs of decomposition beginning at 328.46 °C (601.61 K) indicated by lowering of the baseline.

The followed detected endothermic event with a maximum of 429.26 °C (702.41 K) (highest value) can be interpret as the boiling point.

Therefore the boiling point of the test item under decomposition can be stated with 418.78 °C (691.93 K) under the given test conditions.

This value is the mean of two independent determinations.

No observations were made which might cause doubts on the validity of the study outcome.

Therefore, the result of the study is considered valid.

Conclusions:

The boiling point of the test item under decomposition can be stated with 418.78 °C (691.93 K) under the given test conditions.

Executive summary:

Determination of the boiling point of LUMULSE GMT-K according to OECD 103 resp. EU A.2

Findings and Results:

The boiling point was determined via DSC (differential scanning calorimetry).

Because of the specificity of the DSC 4000 (445 °C is the highest measure temperature); no complete Peak could be detected.

The test item showed possible signs of decomposition beginning at 328.46 °C (601.61 K) indicated by lowering of the baseline.

The followed detected endothermic event with a maximum of 429.26 °C (702.41 K) (highest value) can be interpret as the boiling point.

Therefore the boiling point of the test item under decomposition can be stated with 418.78 °C (691.93 K) under the given test conditions.

This value is the mean of two independent determinations.

Description of key information

The boiling point of the test item under decomposition can be stated with 418.78 °C (691.93 K).

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

328.46 °C

Additional information

The boiling point was determined via DSC (differential scanning calorimetry).

Because of the specificity of the DSC 4000 (445 °C is the highest measure temperature); no complete Peak could be detected.

The test item showed possible signs of decomposition beginning at 328.46 °C (601.61 K) indicated by lowering of the baseline.

The followed detected endothermic event with a maximum of 429.26 °C (702.41 K) (highest value) can be interpret as the boiling point.

Therefore the boiling point of the test item under decomposition can be stated with 418.78 °C (691.93 K) under the given test conditions.