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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:
17 October 2017 to 20 October 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reference:
Composition 0
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.2 (Boiling Temperature)
Version / remarks:
2008
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
method according to Siwoloboff
Test material information:
Composition 1
Key result
Atm. press.:
97.8 kPa
Decomposition:
yes
Decomp. temp.:
>= 280 - <= 370 °C

Preliminary Tests

The following preliminary tests were performed:

- from 160 °C to about 370 °C at 10°C/min heating rate with two parallel samples: At about 280 °C the first bubbles appeared. At about 300 °C the test material started to turn brown. At about 310 °C continuous slow bubbles were formed. At about 370 °C the test material was dark brown and boiling-like bubbling was observed. The range of between the first and the boiling-like bubbles was very broad, furthermore signs of decomposition were apparently observed, therefore further preliminary tests were necessary within different temperature ranges with variant heating rates in order to obtain more accurate results to set the main study parameters.

- from 330 °C to about 335 °C at 0.5 °C/min heating rate with two parallel samples: At about 330 °C the first bubbles appeared. At about 335 °C a slow bubble-forming was observed. Within the examined temperature range using a 0.5 °C/min heating rate, continuous and steady slow bubble-formation was observed from the beginning with a change of colour, without increasing of velocity of bubble-formation.

- from 300 °C to about 385 °C at 3.0 °C/min heating rate with two parallel samples: At about 301 °C a slow bubbling started with small bubbles. The colour of test material changed continuously, at about 335 °C the test material was a dark brown colour. From about 354 °C faster bubble-formation was observed.

- from 370 °C to about 400 °C at 0.5 °C/min heating rate with two parallel samples: The test material started to turn brown then black immediately with quick bubble-formation.

- Based on the results of the previous preliminary tests, it seemed, that the boiling point of test material is close to 350 °C, therefore different capillaries filled with the test material were placed into the apparatus to various temperatures:

- at 360 °C: Intensive, boiling-like bubble-formation was observed.

- at 350 °C: Intensive, boiling-like bubble-formation was observed.

- at 340 °C: The bubble-formation was slower than at 350 °C.

 

Summary of the Preliminary Tests:

From about 280 °C, the formation of first bubbles were observed. The changing of the test material colour was seen continuously over the boiling range. Depending on the chosen initial temperature, bubble-formation was seen with different frequencies, but the accurate, standard boiling in an acceptable temperature range cannot be determined. Therefore, for the Main test, from 280 °C to 400 °C was the selected temperature range, with a 5 °C/min heating rate instead of the regular 0.5 °C/min rate.

 

Main Test

The observations were as follows in each main test:

At about 285 °C small bubbles appeared. From about 290 °C a change of colour was observed continuously. At about 350 °C a faster bubble formation was observed, but at this point the sample was black. Using a 5 °C/min heating rate, at about 370 °C boiling like bubble formation was observed.

The main tests were carried out at 97.8 kPa atmospheric pressure.

The observations demonstrate that the test material changes colour on heating, indicating decomposition occurs before boiling at normal atmospheric pressure. Hence the definite Boiling Point for the Test Material is not definable at normal atmospheric pressure, but it can be said that bubbling starts at about 285 °C and that the decomposing product boils at 280 – 370 °C, with further boiling of a very dark decomposition product at higher temperatures. Furthermore, using a slow heating rate, an acceptable boiling of test material cannot be seen, therefore the bubble formation cannot consider to represent real boiling. The test material decomposes but does not boil at normal atmospheric pressure.

Conclusions:
Under the conditions of this study, the test material decomposes but does not boil at normal atmospheric pressure.
Executive summary:

 The boiling point of the test material was determined in accordance with the standardised guidelines OECD 103 and EU Method A.2, under GLP conditions. The test was performed using the capillary method using a metal heating block.

The test material was assessed visually for any possible changes in its appearance, consistency and colour.

The observations demonstrate that the test material changes colour on heating from about 290 °C, indicating decomposition occurs before full boiling at normal atmospheric pressure. Bubbling of the liquid starts at about 285 °C, the decomposing product boils at 280 – 370 °C, with further boiling of a very dark decomposition product at higher temperatures.

Under the conditions of this study, the test material decomposes but does not boil at normal atmospheric pressure.

Description of key information

Under the conditions of this study, the test material decomposes but does not boil at normal atmospheric pressure.

Key value for chemical safety assessment

Additional information

The boiling point of the test material was determined in accordance with the standardised guidelines OECD 103 and EU Method A.2, under GLP conditions. The test was performed using the capillary method using a metal heating block. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The test material was assessed visually for any possible changes in its appearance, consistency and colour.

The observations demonstrate that the test material changes colour on heating from about 290 °C, indicating decomposition occurs before full boiling at normal atmospheric pressure. Bubbling of the liquid starts at about 285 °C, the decomposing product boils at 280 – 370 °C, with further boiling of a very dark decomposition product at higher temperatures.

Under the conditions of this study, the test material decomposes but does not boil at normal atmospheric pressure.