Extract obtained from defatted powder of Theobroma cacao (Malvaceae) by extraction with ethanol

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

24 Oct. 2017 - 06. Dec. 2017

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Version / remarks:

1995

Deviations:

yes

Remarks:

A Cottrell vessel with three openings and an additional thermometer in the sample was used instead of a vessel with two openings. It allows to detect the temperature of the substance in the Cottrell vessel.

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

2008

Deviations:

yes

Remarks:

A Cottrell vessel with three openings and an additional thermometer in the sample was used instead of a vessel with two openings. It allows to detect the temperature of the substance in the Cottrell vessel.

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected on 13 and 14 October 2014 / signed on 08 April 2015

Type of method:

dynamic method

Remarks:

and DSC method

Decomposition:

ambiguous

Remarks on result:

not determinable

Pre-test following Siwoloboff method

Observations Pre-test following Siwoloboff method

Observations	Temperatures
Melting start	Since 40 °C
Melted with a solid part	90 °C
Completely melted	100 °C
Some bubbles on surface	120 °C
Lots of foam, looks like boiling, especially in ground zone, the upper part rose up in the capillary. Tube slightly dropped. Foam vanished test item is liquid with bubbles on the surface.	130 °C
Burner switched off	155 °C
No bubbles visible anymore	150 °C

After cooling down the test item appeared as a black-red- brown solid, more homogeneous as before the determination.

Some of this material was ground and looked like the original state.

DSC measurements:

The DSC measurements yield no reliable results which indicate a boiling of the test item (no clear endothermic event was observed) . However, after testing, the following observations were reported:

	weight loss of crucible after measurement	Observations
First measurement	75.7%	The crucible was visual unchanged and opened the test item was carbonized.
Second measurement	77.7%	The test item had left the crucible through the perforation.

The ambient pressure was recorded with 100258 Pa.

Results following the dynamic method:

Two experiments were performed using the dynamic method to determine the initial boiling point of the substance.

Beginning boiling was observed in the vessel at 100°C (first determination ) and 95 °C (second determination). At a temperature of

130°C (first determination ) and 120 °C (second determination) the test item boiled with foam and a colourless condensate was visible. At 155°C (first determination) 145°C (second determination), there ise more foam and the test item began to rise up. No mixture of vapour and liquid were produced. The temperature was stable at 170°C (first determination) and 164 °C (second determination) whereas the temperature of the Cottrell pump was measured with 62.2 °C and 61.3°C respectively. Due to the difference of temperatures between the Cottrell pump and the test item, no clear initial boiling point can be determined using dynamic method. After cooling down the test item had become to a black –brown solid with a bit of an oily liquid. The difference of temperatures may indicate a decomposition of the test item and the changed appearance after cooling down may confirm this.

Considering that the DSC didn’t allow detecting a potential decomposition or a phase transition of the substance (such as boiling point), no initial boiling point of the test could be determined using the standard methods reported in this report.

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:

No boiling point can be determined using standard methods conducted in this study (DSC method and dynamic method) and signs of potential decomposition of the substance were observed during the tests.

Executive summary:

A reliable GLP experimental study, conducted according to a recognized OECD/EC guidelines is available. It is considered as a key study.

The DSC method and the dynamic method with Cottrell apparatus were performed to determine the initial boiling point of the substance.

Using the dynamic method, a significant difference of temperatures between Cottrell pump and test item was observed during the study, which may be the sign of decomposition of the substance. The change of appearance of the test item after measurement would confirm this.

In addition no endo/exothermic events were detected using the DSC method, which may indicate the boiling or a potential decomposition of the substance.

Therefore no temperature of initial boiling point or initial decomposition of the test item can be determined using the dynamic method or DSC method used in this report.

Description of key information

No boiling point can be determined using standard methods (DSC and Dynamic methods) and signs of decomposition of the test item were observed during the tests.

Additional information

A reliable GLP experimental study, conducted according to a recognized OECD/EC guidelines is available.

It is considered as a key study.