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Physical & Chemical properties

Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Study period December, 12, 2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
no
Other quality assurance:
other: ISO 9001
Type of method:
differential scanning calorimetry
Remarks:
A glass tube method was also used
Specific details on test material used for the study:
Trade name: Trigonox D-C50
Batch number: 1211442406
Description: Colourless clear liquid
Storage temperature: 5°C, based on information Certificate of Analysis
Expiration date: December 1, 2022
Key result
Melting / freezing pt.:
-15 °C
Atm. press.:
1 atm

Calibration check

Measured values for Indium:

- Onset temperature : 156.6°C

- Enthalpy of melting : 28.8 J/g

The measured values are within the acceptance limits

Test method 1: Thermal analysis method:

The DSC curve of the measurement is shown below. An endothermic peak was obtained.

This is the melting traject of di-tert-butyl sec-butylidenediperoxide, 50% solution in isododecane. The endpoint of the melting traject is -15.8°C, rounded -16°C. At this temperature all the crystals are dissolved.

Test method 2: The glass tube method

First the reaction mixture, seeded with glass splinters was cooled to -25°C, to crystallize the reaction mixture. After spontaneous crystallization, the mixture was heated stepwise.

The temperature steps and appearance of the sample at each sample temperature is mentioned below.

  • 11 days at -25°C : spontaneous crystallization
  • 1 day at -24°C : approximately 60% solids, 40% liquid
  • 1 day at -22°C : approximately 60% solids, 40% liquid
  • 3 days at -20°C : approximately 50% solids, 50% liquid
  • 1 day at -19°C : approximately 50% solids, 50% liquid
  • ½ day at -18°C : approximately 50% solids, 50% liquid
  • ½ day at -17°C : approximately 50% solids, 50% liquid
  • ½ day at -16°C : approximately 40% solids, 60% liquid
  • 1 day at -15°C : completely dissolved
Conclusions:
The melting/freezing point of this substance is -15°C.
Executive summary:

The melting point of di-tert-butyl sec-butylidene diperoxide, 50% solution in ìsododecane was determined according to EC Regulation No 440/2008, Guideline A.1 and according to OECD Guideline 102, and in accordance with European Chemicals Agency (ECHA), Guidance on information requirements and chemical safety assessment, Chapter R.7a, Endpoint specific guidance, May 2008.

The melting point was determined using two methods, a thermal analysis method and a method a glass tube method, which is equivalent to the capillary method of the guidelines EC A.1 and OECD 102.

The melting point of the test substance is -15°C.

Description of key information

The measured mp of the substance is -15 oC.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-15 °C

Additional information