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Boiling point

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Reference
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
May 22 to July 16, 2014
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP.
Restrictions apply considering the difficulty to interprete the result obtained for such complex substance and to determine the initial boiling point & temperature of decomposition of the substance. The substance is considered to be adequately characterised. Therefore a validation with restrictions applies.
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling point/boiling range)
Version / remarks:
dated 27 July 2015
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:
Regulation (EC) n°761/2009, dated 23. Jul.2009
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 29 and 30 November 2010 / signed on 11 April 2011
Type of method:
dynamic method
Key result
Decomposition:
ambiguous
Remarks on result:
other: No defined boiling point of the test item could be determined using the dynamic method.

Two experiments were performed using the dynamic method and the following observations were made:

Table 4.3/1: Observations

Observation

First determination

Second determination

Thermometer

Cottrell Pump

Thermometer

Sample

Thermometer

Cottrell Pump

Thermometer

Sample

Cottrell pump pumps

224.4 °C

346 °C

No pumping up

to 318.1 °C

No pumping

up to 375 °C

Atmospheric pressure

99888 Pa

99526 Pa

 

In both determinations, a white damp formed when the test item was boiling under strong foaming. The white damp sublimated in the cooler as a yellow residue.

After cooling down following observations were made:

The colour of the residue on the thermometer of the Cottrell pump appeared brown like rust. The colour of the residue on the sample thermometer appeared olive green. The sample in the vessel appeared brown-black. The mass sublimated in the cooler was yellow on top and white under the surface.

The odour resembled frankincense.

 

Because of the high difference between the first and the second determination, two additional experiments were performed with slow heating.

The following observations were made:

 

Table 4.3/2: Observations

Observation

First determination

Second determination

Thermometer

Cottrell Pump

Thermometer

Sample

Thermometer

Cottrell Pump

Thermometer

Sample

Damp visible

in the vessel

34.4 °C

Approx. 50 °C

34.0 °C

Approx. 50 °C

Clear, colourless

condensate visible

44.6 °C

90 °C

43.9 °C

Approx. 93 °C

First rising into the

Cottrell Pump

66.0 °C

140 °C

67.8 °C

Approx. 145 °C

Boiling in the test

vessel under foaming

109.3 °C

225 °C

110 °C

Approx. 210 °C

Cottrell pump pumps

256.1 – 282.4 °C

298 -339 °C

No pumping

up to 203.6 °C

No pumping

up to 375 °C

Atmospheric pressure

99626 Pa

100386 Pa

 

After cooling down, the same observations were made as in experiments 1 and 2.

 

Finally, four experiments were performed using the dynamic method. Only in two experiments, boiling, indicated by pumping of the Cottrell pump, was observed.

The change of the appearance and the odour of the test item after cooling down are clear signs for decomposition of the test item during the experiment. The observed damp, the colourless condensate, the sublimated mass in the cooler may be due to the decomposition of the substance or to the higher volatile constituents of the substance.

In addition the thermometer in the Cottrell pump showed a much lower temperature than the temperature in the sample, which may be a sign of decomposition too.

Therefore, no initial boiling point of the test item could be determined using the dynamic method and the temperature of initial decomposition of the test item cannot be clearly stated using this method.

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 clear initial boiling point of the test item could be determined using the dynamic method. In addition, signs of decomposition were observed when the substance is heated up to 375°C.
Executive summary:

A study was conduted to determine the initial boiling point of the test substance under GLP according to EU Method A.2 and OECD 103 following the dynamic method.

Four experiments were conducted but no clear initial boiling point of the test item could be determined using this method and considering the complex nature of the substance. In addition, signs of decomposition were observed when the substance is heated up to 375°C : Indeed, the change of the appearance and the odour of the test item after cooling down are clear signs of decomposition of the test item during the experiment. The observed damp, the colourless condensate, the sublimated mass in the cooler may be due to the decomposition of the substance or to the higher volatile constituents of the substance.

In addition the thermometer in the Cottrell pump showed a much lower temperature than the temperature in the sample, which may be a sign of decomposition too.

Therefore, no clear initial boiling point or initial temperature of decomposition of the test item could be determined using the dynamic method.

Description of key information

No clear initial boiling point of the test item could be determined using the dynamic method. In addition, signs of decomposition were observed when the substance is heated up to 375°C.

Key value for chemical safety assessment

Additional information

A reliable experimental study, conducted according to a recognized OECD/EC, following the dynamic method and under GLP, is available. It is considered as a key study. However, no clear initial boiling point or initial decomposition temperature could be determined using the dynamic method. Considering the complex nature of the substance, no key value is retained for this endpoint.

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