Decanoic acid, mixed esters with heptanoic acid, octanoic acid and pentaerythritol

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

20 Feb. 2017 to 28 Feb. 2017

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 further details specified in the study report.

Key result

Boiling pt.:

> 350 °C

Decomposition:

yes

Decomp. temp.:

420 °C

Remarks on result:

other: DSC measurements were performed under inert gas

Observations of the Pre-test following Siwoloboff

Observations	Temperature
Intermittent bubbling	Since 55 °C
The bubbles were away	Since 260 °C
One bubble	276 °C
One small bubble	300 °C
One small bubble	320 °C
Intermittent bubbling	Since 330 °C
Continuous bubbling, colour slightly yellowish and getting continuously yellow	Since 350 °C
Bubble chain, the gas burner was turned down	445 °C
The chain broke	364 °C
After cooling down the colour of the test item was yellow-brown, the test item decomposed

 

Security Pre-test for the DSC instrument

The lid of the first crucible was found to be bloated. Discoloration occurred on the side, and at the perforated hole. The findings are indicative of the test item overflowing from the hole after reaching a temperature of 420 °C. After cooling down the weight was recorded as 64.95 mg.

In successive repetition tests the crucible was found visually unchanged after reaching a temperature of 420 °C but discoloration was noted on the side. The weight was recorded as 46.29 mg. After further heating to 600 °C and cooling down the crucible was visually unchanged, and the discoloration on the side had disappeared. The weight was recorded as 45.85 mg.

 

Values DSC Indium

Expected Melting point	Measured Melting point	Expected Heat flow	Measure Heat flow	Assessment
156.6 ± 1.0 °C	156.73 °C	28.45 ± 1.0 J/g	28.24 nJ/g	OK

The measurement of indium after calibration met the validity criteria.

 

Values DSC Test item first determination

	Temperature [°C]	Energy
Event	Not found	Not found

No event was detected in the first determination therefore the determinations from 15 °C to 420 °C were performed.

 

Values DSC Test Item second determination

Event	Temperature [°C]	Energy	Delta Y [mW]
1	85.44	-18.05 [mW]	0.1325
2	399.19	-79.09 [mW]	0.1194
3	409.44	-81.11 [mW]	0.3671
4	412.69	-81.64 [mW]	0.1873
5	414.49	-81.96 [mW]	0.2711

 

Values DSC Test Item third determination

Event	Temperature [°C]	Energy	Delta Y [mW]
1	202.82	-36.34[mW]	0.1618
2	212.67	-38.19 [mW]	0.1141
3	312.51	-58.92 [mW]	0.7381
4	335.41	-63.95 [mW]	0.6632
5	354.98	-68.31 [mW]	0.0957

 

As the deviation between the values of the second and third determinations were >0.5 °C a fourth determination was performed.

 

Values DSC Test Item fourth determination

Event	Temperature [°C]	Energy	Delta Y [mW]
1	100.87	-27.23 [mW]	0.5395
2	105.81	-28.14 [mW]	1.0988
3	165.60	-40.47 [mW]	0.5869
4	380.14	-102.87 [mW]	0.1667
5	390.51	-106.28 [mW]	0.2773
6	399.99	-109.27 [mW]	0.1323

 

Values Observations

	Mass test item	Mass crucible (before measurement)	Mass crucible (after measurement)	Observations
First Measurement	1.06 mg	47.09 mg	46.87 mg	After the test the crucible was visually unchanged
Second Measurement	1.10 mg	46.64 mg	46.17 mg	After the test the crucible was visually unchanged
Third Measurement	1.06 mg	47.69 mg	47.62 mg	After the test the crucible was visually unchanged
Fourth Measurement	1.12 mg	47.10 mg	46.67 mg	After the test the crucible was visually unchanged

 

Conclusions:

The determination of the boiling point was determined via DSC (differential scanning calorimetry)
Four determinations were performed resulting in different chromatograms, with very small events.
Observations of decomposition of the substance, were noted during the performance of the Pre-test following SIWOLOBOFF indicated by colour change.
DSC measurements were performed under inert gas; therefore the test item was protected from the environment and may explain why no feasible event occurred.
Therefore including all data the boiling point of Hatcol 3178 can be stated as > 350 °C.

Executive summary:

The determination of the boiling point was determined via DSC (differential scanning calorimetry)

Four determinations were performed resulting in different chromatograms, with very small events.

Throughout the test no boiling point as indicated by a clear endotherm event could be observed.

The detected events cover a range from 0.0957 to 1.0988 mW. The signal noise of the instrument was measured with approx. 3.5 μW (routine maintenance of 08. Dec. 2016). In accordance with the manufacturer, only events which are 3 times bigger than the signal noise are significant. In this case some events are above this limit.

 

For a better differentiation of the artefacts, a blank measurement (empty aluminium crucible as sample) performed on 12. Jan. 2017 (routine inspection) was taken into account.

Events from 0.0076 to 0.0242 mW were detected.

By comparing the test item measurements with the blank measurement it is apparent that some reaction took place. This is supported by the fact that after three of the four performed measurements the crucible was lighter, which is surely caused through evaporation of the test item.

Observations, which may be the proof of decomposition of the substance, were observed during the performance of the Pre-test following SIWOLOBOFF indicated by colour change.

DSC measurements were performed under inert gas; therefore the test item was protected from the environment this might explain why no feasible event occurred.

 

Therefore including all data the boiling point of Hatcol 3178 can be stated as > 350 °C.

 

No observations were made which might cause doubts on the validity of the study outcome. Therefore, the result of the study is considered valid.

Description of key information

The boiling point of Hatcol 3178 can be stated as > 350 °C.

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

350 °C

Additional information

The determination of the boiling point was determined via DSC (differential scanning calorimetry)

Observations, which may be the proof of decomposition of the substance, were observed during the performance of the Pre-test following SIWOLOBOFF indicated by colour change.

DSC measurements were performed under inert gas; therefore the test item was protected from the environment this might explain why no feasible event occurred.

 

Therefore including all data the boiling point of Hatcol 3178 can be stated as > 350 °C.