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Boiling point

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Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
05-12 February 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP. The test substance is adequately characterised. Therefore full validation applies.
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Version / remarks:
2008
Deviations:
no
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 8 April 2015
Type of method:
method according to Siwoloboff
Key result
Boiling pt.:
167.4 °C
Atm. press.:
>= 99 477 - <= 99 721 Pa
Decomposition:
yes
Decomp. temp.:
>= 140 °C

Pre-test:

The test tube with test item was set into the aluminium block at 24.2 °C. The aluminium block was heated with gas burner.

The following observations were noted:

Observations

Temperatures

At the bottom slightly shrivelled together

Since 50 °C

Completely melted to a yellow clear sticky mass

82.3 °C

Lots of fine foam / bubbles

(on the bottom clear and on top foam)

Since 130 °C

Foam rose up

Since 150 °C

Bubble chain with lots of foam,

gas burner switched off

175 °C

Bubble chain broke

174.6 °C

Main test:

Observations

Temperatures

First

Determination

atmospheric pressure

99477 Pa

Second

Determination

atmospheric pressure

99721 Pa

Test start:

Test item melted immediately to a clear yellow sticky mass with lots of fine foam. The foam vanish slowly and rose up, the sample became a liquid.

140.0 °C

136.0 °C

Some bubbles and sample getting slightly darker

142 °C

140 °C

No foam anymore

145 °C

Boiling chain, gas burner switched off

173.7 °C

178.1 °C

Boiling chain broke

168.6 °C

166.2 °C

After cooling down the test item appeared as a yellow-brown clear solid.

No calculation following Sydney-Young was carried out as decomposition (change of colour) is considered.

Results of boiling point:

 

Boiling point

under decomposition

Pressure in Pa

First determination

168.6 °C (441.8 K)

99477 Pa

Second determination

166.2 °C (439.4 K)

99721 Pa

Mean

167.4 °C (440.6 K)

 

Mean ± standard deviation (without correction following Sydney Young)= 167.4 ± 1.7 °C (440.6 ± 1.7 K)

Conclusions:
The determination of the boiling point of test item was performed following the Siwoloboff Method.
First signs of possibly decomposition indicated by colour change were observed since 140°C (lowest value).
Therefore the boiling point of test item should be stated as: 167.4 ± 1.7 °C (440.6 ± 1.7 K) under decomposition of the test item.
These values are the mean of two independent determinations without Sydney-Young correction.
Executive summary:

The study was performed in order to determine the boiling point of test item according to OECD 103, resp. EU A.2, guideline, using the Siwoloboff method.

The boiling point of test item should be stated as: 167.4 ± 1.7 °C (440.6 ± 1.7 K) under decomposition of the test item.

Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
6-14 February 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP. The test substance is adequately characterised. Therefore full validation applies.
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Version / remarks:
2008
Deviations:
no
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 8 April 2015
Type of method:
method according to Siwoloboff
Key result
Boiling pt.:
179.2 °C
Atm. press.:
>= 99 350 - <= 99 910 Pa
Decomposition:
yes
Decomp. temp.:
>= 120 °C

Pre-test:

The test tube with test item was set into the aluminium block at 18.1 °C. The aluminium block was heated with gas burner.

The following observations were noted:

Observations

Temperatures

Shrivelled together

44.1 °C

Completely melted to a yellow clear sticky mass

65 °C

On surface small bubbles with colourless condensate, lots of fine foam. The foam vanishes slowly.

Since 100 °C

Individual bubble

Since 120 °C

No foam anymore

Since 125 °C

Getting slightly turbid

Since 135 °C

Bubble chain, gas burner switched off

195 °C

No bubbles anymore

179.1 °C

After cooling down the test item appeared as a yellow-brown clear solid.

Main test:

Observations and measured values are presented in the following table.

Observations

Temperatures

First

Determination

atmospheric pressure

99350 Pa

Second

Determination

atmospheric pressure

99910 Pa

Test start:

Test item melted to a clear yellow viscous liquid with lots of fine foam.The foam vanishes slowly. Colourless condensate visible.

120.0 °C

Some bubbles in large interval.Sample slightly turbid.

Since 126 °C

No foam anymore.

Since 126 °C

Since 129 °C

Boiling chain, gas burner switched off

202.7 °C

198.5 °C

Boiling chain broke

179.7 °C

178.7 °C

After cooling down the test item appeared as a yellow-brown clear solid.

No calculation following Sydney-Young was carried out as a sign of possibly decomposition (colourless condensate) is considered.

Results:

 

Boiling point

under decomposition

Pressure in Pa

First determination

179.7 °C (452.9 K)

99350 Pa

Second determination

178.7 °C (451.9 K)

99910 Pa

Mean

179.2 °C (452.4 K)

 

Mean ± standard deviation (without correction following Sydney Young)= 179.2 ± 0.7 °C (452.4 ± 0.7 K).

Conclusions:
The determination of the boiling point of test item was performed following the Siwoloboff Method.
First signs of possibly decomposition indicated by a colourless condensate was observed since 120°C.
Therefore the boiling point of test item should be stated as: 179.2 ± 0.7 °C (452.4 ± 0.7 K) under decomposition of the test item.
This value is the mean of two independent determinations without Sydney-Young correction.
No observations were made which might cause doubts on the validity of the study outcome. Therefore, the result of the study is considered valid.
Executive summary:

The study was performed in order to determine the boiling point of test item according to OECD 103, resp. EU A.2, guideline, using the Siwoloboff method.

The boiling point of test item should be stated as: 179.2 ± 0.7 °C (452.4 ± 0.7 K) under decomposition of the test item.

Description of key information

The boiling point under decomposition of test item was determined to be 167.4°C or 179.2°C depending the composition tested.

Key value for chemical safety assessment

Additional information

Two fully reliable experimental studies, conducted according to OECD 103/ EU A2 guideline are available.

Both are considered as a key study, and the result is retained as key data.