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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:
03 July 2019 to 04 July 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
capillary method
Specific details on test material used for the study:
No further details specified in the study report
Key result
Melting / freezing pt.:
> 45.3 - < 45.9 °C
Atm. press.:
> 98.1 - < 98.3 kPa
Decomposition:
yes
Decomp. temp.:
50 °C

TEST PARAMETERS AND CONDITIONS

The tests were carried out at air atmospheric pressure (98.1 – 98.3 kPa) and room temperature (approximately 20°C) using a digital melting point device (Büchi B540 Melting Point Unit, calibrated) with a temperature range up to 400°C (673 K).

CHECKING OF THE MELTING POINT TESTER

Before the test item analysis, the proper performance of the instrument was checked by measuring the melting point of Vanillin, Phenacetin and Caffeine. The block was heated at a rate of 0.5°C/minute from a pre-set temperature 5°C lower than the certified melting point values.

Measured reference substances on 03 July 2019

Chemical name

Supplier

Batch No.

Expiry date

Certified melting point value [°C]

Mean of the measured melting point* [°C]

Vanillin

VWR

170115

30 April 2022

82.5 ± 0.3

82.4 ± 0.0

Phenacetin

VWR

180145

31 May 2023

135.8± 0.3

135.5 ± 0.0

Caffeine

VWR

180164

30 June 2023

236.8± 0.3

236.7 ± 0.3

*Mean of three parallel measurements with their 95% confidence interval

The measured values of the reference substances were determined to be in the required range.

Measured temperatures at the beginning of the melting of the test item (three experiments (I, II, III) with three parallel samples each (1, 2, 3) 

Measured temperatures at the final stage of the melting [°C]

I / 1

I / 2

I / 3

II / 1

II / 2

II / 3

III / 1

III / 2

III / 3

Mean

St. Dev

45.5

45.5

45.5

45.9

45.8

45.8

45.3

45.3

45.3

45.5

0.24

 

 

Measured temperatures at the final stage of the melting of the test item (three experiments (I, II, III) with three parallel samples each (1, 2, 3)

Measured temperatures at the final stage of the melting [°C] *

I / 1

I / 2

I / 3

II / 1

II / 2

II / 3

III / 1

III / 2

III / 3

Mean

St. Dev

63.5

63.5

63.5

66.2

65.5

65.5

64.0

63.9

63.9

64.4

1.05

 

*Please note that the final stage of the melting was only apparent, due to colour change was occurred from about 50°C, before the test item was completely melted. It may indicate decomposition, therefore, these measured temperatures were reported, but they were not considered in the evaluation.

Conclusions:
The temperature at the beginning of the melting of CAS 577978-76-8 was found to be approximately 45.5 °C, i.e. 318.7 K. From about 50°C the colour of the test item became darker, then the test item apparently melted.
Due to the observed changes during the melting, no exact melting (softening) range was identified.
Executive summary:

For the determination of the melting point or melting (softening) range, the capillary method using a metal block was applied.

Using a linear heating rate of 0.5°C/minute, the temperature at the beginning of the melting of CAS 577978-76-8 was found to be approximately 45.5 °C, i.e. 318.7 K. From about 50°C the colour of the test item became darker, then the test item apparently melted.

Due to the observed changes during the melting, no exact melting (softening) range was identified.

Description of key information

The temperature at the beginning of the melting of CAS 577978-76-8 was found to be approximately 45.5 °C, i.e. 318.7 K. From about 50°C the colour of the test item became darker, then the test item apparently melted.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
45.5 °C

Additional information

Due to the observed changes during the melting, no exact melting (softening) range was identified.