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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:
26 November 2020 - 27 November 2020
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Well documented study performed according to OECD 103 guideline and EU method A.2, under GLP and without deviation
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to other study
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling Point)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
2018-11-15
Type of method:
differential scanning calorimetry
Boiling pt.:
ca. 203.9 °C
Atm. press.:
ca. 97.3 kPa
Decomposition:
no
Remarks on result:
other: First determination
Boiling pt.:
ca. 204.2 °C
Atm. press.:
ca. 97.3 kPa
Decomposition:
no
Remarks on result:
other: Second determination
Key result
Boiling pt.:
ca. 205.7 °C
Atm. press.:
ca. 101.3 kPa
Remarks on result:
other: Corrected value with the Sydney Young equation

Pre-study:


Peaks assigned to the boiling of the substance was observed and measurement was stopped at 250°C (Figure 1).


The initial boiling point of the substance was observed at 206.9°C.
A corresponding mass loss of 11.486 mg was observed between the beginning and the end of the boiling peak.


Temperature corresponding to this peak was used to create the following temperature program:


 


Temperature program:



























Step



Initial temperature (°C)



Final Temperature (°C)



Heating rate (°C/min)



Duration (min)



Furnace atmosphere



Rate* (mL/min)



Liquid nitrogen cooling



1



20



260



10



24



N2



60



NO




*Gas injection rate in the furnace. 


 


First Determination: 


Mass taken: 10.02 mg


Results: Initial boiling point was observed at 203.9°C (onset temperature of the peak) and a mass loss of 9.882 mg was observed between the beginning and the end of the boiling peak.
The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 97.3 kPa.


 


Second Determination: 


Mass taken: 12.14 mg


Results: Initial boiling point was observed at 204.2°C (onset temperature of the peak) and a mass loss of 11.979 mg was observed between the beginning and the end of the boiling peak.
The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 97.3 kPa.

Conclusions:
After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 205.7°C at 101.3 kPa (mean of 205.6°C for the first determination and 205.9°C for the second determination).
Executive summary:

 A study was performed to determine the boiling point of the test item (+)-CAMPHOLENIC ALDEHYDE using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.2. and OECD Test Guideline 103, "Boiling Point" (1995).


In this method, two crucibles were put in the apparatus furnace under inert atmosphere (nitrogen) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied.
The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram.


Two trials were conducted and corresponding thermograms were obtained, giving us the following results:


 






















Trial



Initial boiling point



Ambient pressure



1



203.9 °C



97.3 kPa



2



204.2 °C



97.3 kPa




The initial boiling point values respect validity criteria (less than 0.5°C of difference up to 326.85°C).
Moreover, the melting point of the Indium respects the checking cards limits (156.2°C for a reference value of 156.6°C) so as the enthalpy (30.32 J/g for a reference value of 28.6 J/g).


After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 205.7 °C at 101.3 kPa (mean of 205.6 °C for the first determination and 205.9 °C for the second determination).

Description of key information

After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 205.7°C at 101.3 kPa (mean of 205.6°C for the first determination and 205.9°C for the second determination).

Key value for chemical safety assessment

Boiling point at 101 325 Pa:
205.7 °C

Additional information

Key study conducted according to the OECD 103 Guideline and the EU A.2 method, under GLP without deviation and with certificate of analysis included. Therefore, a reliability of 1 is assigned and the result of this key study is proposed as the end point value.