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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:
11-03-2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Guideline study performed under GLP. All relevant validity criteria were met.
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
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7220 (Boiling Point / Boiling Range)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
inspected: January 2013; signature: March 2013
Type of method:
differential scanning calorimetry
Boiling pt.:
>= 250 - <= 255 °C
Atm. press.:
1 013 hPa
Decomposition:
yes
Decomp. temp.:
> 180 °C
Remarks on result:
other: The measured boiling range is considered to be indicative of that of partially degraded test item; the decomposition reported is indicative of oxidation/rearrangement reactions occuring prior to boiling at > 180 °C.

Table 1. Results of the DSC analysis:

Run Number

Sample Weight / mg

Onset of effect / °C

Range of Effect / °C

Air Pressure / hPa

Remarks

1

12.94

-29.74

-35 – -29 (exo)

1016.4

Cooling run (- 0.25 K/min)

 

 

-11.15

-15 – 0 (endo)

1016.4

Heating run (+10 K/min)

 

 

186.05

180 – 230 (exo)

 

 

 

 

249.79

230 – 310 (endo)

 

 

 

 

 

 

 

 

2

13.43

-33.36

-35 – -30 (exo)

1016.8

Cooling run (- 0.25 K/min)

 

 

-11.15

-15 – 0 (endo)

1016.8

Heating run (+10 K/min)

 

 

184.39

180 – 230 (exo)

 

 

 

 

254.79

230 – 310 (endo)

 

 

 

 

 

 

 

 

 

The test item showed a small exothermic effect in the temperature range of 180 – 230 °C which was directly followed by an endothermic signal in the temperature range of 230 - 310°C that can be associated with the boiling of the test item. For the correction of the boiling temperature to standard pressure the test item was assigned to chemical group 2 (e.g.Hydrocarbons, Camphor). A correction value φ = 5.05 was used for the temperature range from 250°C to 260 °C. The lowest measured onset temperature is corrected to the normal pressure to be 249.65 °C and the highest onset temperature to be 254.63 °C. As the corrected onset temperatures in both tests deviate by more than 0.5 K from their mean value of 252.14 °C, the test item has a boiling range from 250 °C to 255 °C. No further thermal effects were observed up to the test end temperature of 500 °C

Measurements by the capillary method:

To verify the results of the DSC-measurement, an additional measurement with the capillary method was performed in the temperature range 180 – 300 °C with a heating rate of 10 K/min. The observations during the test with the capillary method is provided in table 2.

Table 2: Observations during the test with the capillary method (Heatingrate:10 K/min from 180 °C to 300 °C)

 

Sample

Start (180°C)

Colourless liquid

205°C

Change in colour to yellowish

210°C

Bubble formation

280°C

Change in colour to brownish, test item is boiling out of the capillary

295°C

Capillary almost empty

 

The measurement with the capillary method within the temperature range of 180 °C to 300 °C confirmed the results of the DSC-measurements. The exothermic effect in the temperature range of 180 – 230 °C can be associated with a change in colour of the test item at about 205 °C. The endothermic signal in the temperature range of 230 – 310 °C was confirmed as the boiling range of the test item.

Conclusions:
The test item was observed to decompose at > 180 °C. The test item boiling temperature range was determined to be 250 °C to 255 °C at 1013.25 hPa atmospheric pressure.
Executive summary:

The boiling temperature was determined using OECD TG 103 and EU Method A.2: Differential Scanning Calorimetry (DSC) method. The test substance was tested in duplicate. The test item was observed to decompose at > 180 °C in duplicate and this was confirmed by further capillary method testing, observed colour changes. The test item boiling temperature range was determined to be 250 °C to 255 °C at 1013.25 hPa atmospheric pressure.

Description of key information

Decomposes at > 180 °C. Bp Range: 250 °C to 255 °C at 1013.25 hPa atmospheric pressure, OECD TG 103 - DSC method, 2014

Key value for chemical safety assessment

Additional information

The boiling temperature was determined using OECD TG 103 and EU Method A.2: Differential Scanning Calorimetry (DSC) method. The test substance was tested in duplicate. The test item was observed to decompose at > 180 °C in duplicate and this was confirmed by further capillary method testing, observed colour changes. The test item boiling temperature range was determined to be 250 °C to 255 °C at 1013.25 hPa atmospheric pressure.