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Physical & Chemical properties

Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
15 April 1999 to 23 June 1999
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
GLP compliance:
yes (incl. QA statement)
Type of method:
capillary method
Key result
Melting / freezing pt.:
>= 93 - <= 95 °C

Results of the Study

Melting Stage*

Temperature (°C)

Sample I

Sample II

A

93.0

93.0

B

94.0

94.0

C

94.0

94.5

D

94.5

94.5

E

95.0

95.0

*as referenced in OECD 102

Conclusions:
Under the conditions of the study, the melting range of the test material was found to be 93.0 to 95.0 °C.
Executive summary:

The melting point of the test material was investigated in accordance with the standardised guideline OECD 105, under GLP conditions.

The test material was tightly packed into a capillary tube to a height of 3 mm. Following an initial estimation of melting point, the melting point apparatus was set at approximately 10 °C below the expected melting temperature. The capillary tube was placed in the apparatus and heated at 1 °C/ minute until melting was complete. The procedure was performed in duplicate using a fresh sample on each occasion.

Under the conditions of the study, the melting range of the test material was found to be 93.0 to 95.0 °C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
24 January 1991 to 29 April 1991
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:
yes (incl. QA statement)
Type of method:
capillary method
Melting / freezing pt.:
> 85.9 - < 90.4 °C

Test Material Results

Melting Stage

Temperature (°C)

Run I

Run II

A

85.9

85.9

B

86.4

86.9

C

87.4

87.4

D

89.9

88.9

E

90.9

89.9

 

The melting stages A to E are defined thus:

Stage A (Wet point): Fine droplets adhere uniformly on the inside wall of the capillary tube.

Stage B (Shrinkage point): A clearance appears between the sample and the inside wall due to shrinkage of the melt.

Stage C (Collapse point): The shrunken sample begins to collapse downwards and liquifies.

Stage D (Liquifying point): A complete meniscus is formed at the surface, but an appreciable amount of the sample remains solid.

Stage E (Final stage of melting): There are no solid particles.

 

Thus the melting range of the test material was 85.9 - 90.4 °C (358.9 - 363.4 K) (mean of 85.9 - 90.9 °C and 85.9 - 89.9 °C).

Conclusions:
Under the conditions of this study, the melting point range determined by the capillary method was 85.9 - 90.4 °C.
Executive summary:

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A1, under GLP conditions.

The melting point determination was carried out by a capillary tube method using a Buchi 530 melting/boiling point apparatus to provide the heating. The melting points of certified reference materials were determined to calibrate the apparatus and provide a correction to the measured melting temperatures by inserting the measured values into the linear regression.

Under the conditions of this study, the melting point range determined by the capillary method was 85.9 - 90.4 °C.

Description of key information

Key Study: Comb (2000)

Under the conditions of this study, the melting range of the test material was found to be 93.0 to 95.0 °C.

Supporting Study: Cowlyn (1993)

Under the conditions of this study, the melting point range determined by the capillary method was 85.9 - 90.4 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
93 °C

Additional information

Key Study: Comb (2000)

The melting point of the test material was investigated in accordance with the standardised guideline OECD 105, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The test material was tightly packed into a capillary tube to a height of 3 mm. Following an initial estimation of melting point, the melting point apparatus was set at approximately 10 °C below the expected melting temperature. The capillary tube was placed in the apparatus and heated at 1 °C/ minute until melting was complete. The procedure was performed in duplicate using a fresh sample on each occasion.

Under the conditions of the study, the melting range of the test material was found to be 93.0 to 95.0 °C.

 

Supporting Study: Cowlyn (1993)

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A1, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The melting point determination was carried out by a capillary tube method using a Buchi 530 melting/ boiling point apparatus to provide the heating. The melting points of certified reference materials were determined to calibrate the apparatus and provide a correction to the measured melting temperatures by inserting the measured values into the linear regression.

Under the conditions of the study, the melting point range determined by the capillary method was 85.9 - 90.4 °C.