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Boiling point

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Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2013-09-13
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Remarks:
The study was conducted in accordance with a relevant test method and in compliance with a known quality system (ISO 9001:2008)
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling point/boiling range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
GLP compliance:
no
Other quality assurance:
other: ISO 9001:2008
Type of method:
dynamic method
Key result
Atm. press.:
1 013 hPa
Decomposition:
yes
Decomp. temp.:
216.7 - 274.8 °C
Remarks on result:
other: The colour of the test substance changes from slightly yellow to yellow-brown

Results:

Method 1: Dynamic method

Table 1: Results of Method 1 – Dynamic method

Test

Measured boiling temperature

Measured pressure (kPa)

Boiling temperature corrected to normal pressure

 

°C

K

 

°C

K

1

273

546.2

97.2

274.9

548.1

2

215

488.2

97.2

216.7

489.9

Approximate accuracy of the instrument: ± 0.5 K (up to 600 K)

 

With method 1 (dynamic method) it was not possible to achieve a constant boiling temperature. When repeating the measurement the boiling temperature falls to finally 215°C. During this test the colour of the test substance changes from slightly yellow to yellow-brown.

Conclusions:
Decomposition temperature of 216.7 - 274.9°C was obtained for the substance using a relevant test method and in compliance with a known quality system. During the study colour of the test substance changes from slightly yellow to yellow-brown. The result is considered to be reliable.
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2013-10-25
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Remarks:
The study was conducted in accordance with a relevant test method and in compliance with a known quality system (ISO 9001:2008)
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling point/boiling range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
GLP compliance:
no
Other quality assurance:
other: ISO 9001:2008
Type of method:
photocell detection
Key result
Boiling pt.:
210 - 287 °C
Atm. press.:
1 013 hPa

Method 2: Capillary tube method

Visual observation:

- Begin of bubbling at about 208°C (1-2 bubbles / min)

- Constant bubbling at about 285°C (1 bubble / 5-1 0 s)

- Constant bubbling at about 292°C (1 bubble / 2-3 s)

- Instrument stops the measurement at 300°C (upper limit) without photocell detection

Atmospheric pressure: 96.9 kPa

Corrected temperature: 210 – 287°C (483 – 560 K) at 101.32 kPa

The temperatures were corrected to normal atmospheric pressure (101.32 kPa).

Conclusions:
A boiling range of 210-287°C at 1013 hPa was determined for the substance using a relevant test method and in compliance with a known quality system. The result is considered to be reliable.
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2013-07-30 to 2013-10-24
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Remarks:
The study was conducted in accordance with a relevant test method and in compliance with a known quality system (ISO 9001:2008)
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling point/boiling range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
GLP compliance:
no
Remarks:
ISO 9001:2008
Type of method:
differential thermal analysis
Remarks:
Differential Scanning Calorimetry (DSC) combined with thermogravimetrie (TGA)
Key result
Atm. press.:
97 kPa
Decomposition:
yes
Decomp. temp.:
210
Remarks on result:
other: A small mass loss of about 3% at 210°C was observed in a TGA thermogram. This was followed by a 78% mass loss with onset temperature of about 269°C

Method 3: DSC/TGA method

With exclusive application of the DSC method it was not possible to detect a boiling temperature (no endothermic peak). See enclosure 1 (attached DSC diagram).

The TGA-diagram shows a small loss of mass (ca. 3%) at about 210°C. At this temperature, a clear decline of the mass curve begins. This sharp decline had an onset temperature of about 269°C. At the end of the measurement (400°C) about 78 % of the test substance had evaporated. See enclosure 2 (attached TGA diagram).

Conclusions:
An onset decomposition temperature of about 208°C was obtained for the substance using a relevant test method and in compliance with a known quality system. The result is considered to be reliable.

Description of key information

Boiling temperature: The substance was observed to undergo thermal decomposition from about 210°C (EU Method A.2)

Key value for chemical safety assessment

Additional information

The boiling point of the substance has been determined using three different methods (Haas 2013); 1) dynamic method, 2) capillary tube method / photocell detection method and 3) Differential Scanning Calorimetry (DSC) combined with thermogravimetric analysis (TGA) method in accordance with EU Test Method A.2 and in compliance with a known quality system (ISO 9001:2008).

In the dynamic method, it was not possible to obtain a constant boiling temperature for the substance but a decomposition temperature of 216.7 - 274.9°C at 1013 hPa was obtained. During the study, a colour change from slight yellow to yellow-brown was observed. To further evaluate the boiling point of the substance accurately, a capillary tube/photocell detection method was used. The results of visual observation indicate an onset of boiling temperature from about 210 - 287°C. Also, in the DSC/TGA method, onset of decomposition temperature was observed at about 208°C with initial mass loss of about 3%. This was followed by sharp decline with an onset temperature of about 269°C. At the end of the study (400°C), about 78% of the test substance has been lost.

Based on the findings in the above studies, the submission substance is considered to undergoes thermal decomposition from about 210°C. The results are considered to be reliable and are used as weight of evidence.

In available secondary sources to which reliability could not be assigned, boiling point values of 237 - 247°C at 35 hPa and >250°C at 0.13 hPa, 236°C were reported for the substance.