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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:
02 February 1999 to 22 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
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes
Type of method:
capillary method
Key result
Melting / freezing pt.:
>= 93.5 - <= 97.5 °C
Decomposition:
no
Sublimation:
no
Remarks on result:
other: Atmosphric pressure was not specified.

The results of duplicate melting point determinations on the test material (pure grade) were as follows:

Melting Stage*

Temperature

(°C)

Sample 1

Sample 2

A

93.5

93.0

B

94.5

94.5

C

96.0

96.0

D

96.5

96.5

E

97.0

97.5

*As referenced in OECD Method 102.

Conclusions:
Under the conditions of the study the melting range of the test material was found to be 93.5 to 97.5 °C.
Executive summary:

The melting point of the test material was assessed according to OECD Test Guideline 102 and EU Method A.1. and in compliance with GLP using a capillary method.

Dried test material was pulverised to a fine powder and a small amount 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 (pure grade) was found to be 93.5 to 97.5 °C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
11 April 1990 to 20 August 1990
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
Qualifier:
according to guideline
Guideline:
other: EPA FIFRA Subdivision D § 63-5
Deviations:
no
GLP compliance:
yes
Type of method:
capillary method
Key result
Melting / freezing pt.:
>= 81.5 - <= 92 °C
Remarks on result:
other: Atmospheric pressure not specified.

Melting Point of Reference Materials

 

Melting Point (°C)

Reference Material

 

Measured Value

Certified Value

4-Nitrotoluene

50

52.30

Naphthalene

80

80.81

Acetanilide

115

114.58

Diphenyl acetic acid

151

147.57

2 -Chloroanthraquinone

213

210.75

Carbazole

250

246.70

Linear regression:

y = 2.746 + 0.973x

Where:

y = Certified value

x = Measured value

Results of Duplicate Melting Point Determinations on the Test Material

 

Tempertaure (°C)

Melting Stage 

Run I

Run II

A

81.5

81.5

B

82.0

82.0

C

87.0

87.0

D

89.5

88.5

E

91.5

92.0

Thus the melting range of the test material is 81.5 - 92.0 °C (354.5 - 365.0 K) (the mean of 81.5 - 91.5 °C and 81.5 - 92.0 °C).

Conclusions:
Under the conditions of the study the melting range of the test material is 81.5 to 92.0 °C (354.5 - 365.0 K) (the mean of 81.5 - 91.5 °C and 81.5 - 92.0 °C).
Executive summary:

The melting range was assessed according to OECD Method 102, EEC Method A1, EPA FIFRA Subdivision D § 63-5 and in compliance with GLP using the capillary method.

The melting point determination was carried outby 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 method 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 range of the test material is 81.5 to 92.0 °C (354.5 - 365.0 K) (the mean of 81.5 - 91.5 °C and 81.5 - 92.0 °C).

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
October-November 1994
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
Key result
Melting / freezing pt.:
>= 94.6 - <= 96.2 °C
Remarks on result:
other: Atmospheric pressure not specified.

Usinge the capillary method the melting point of the reference substance, benzile, was determined to be 93.5 - 95.0 °C.

The melting point of the test material was determined to be:

Determination 1: 94.7 - 96.2 °C

Determination 2: 94.6 - 95.9 °C

From these results for the pure active test material the melting range is: 94.6 - 96.2 °C.

Using DSC a melting curve was registered from 60 to 360 °C with a heating rate of 10 K/min (sample weight 3.48 mg). The melting curve shows an endothermic melting peak at about 100 °C, which agrees with the capillary method.

Conclusions:
Under the conditions of the study the melting range of the pure active test material is 94.6 - 96.2 °C.
Executive summary:

The melting range was assessed according to OECD Method 102 and in compliance with GLP using the capillary method.

The test material was also investigated for exothermic/endothermic effects by differential scanning calorimetry (DSC).

A melting curve was registered from 60 to 360 °C with a heating rate of 10 K/min (sample weight 3.48 mg). The melting curve shows an endothermic melting peak at about 100 °C, which agrees with the capillary method.

Under the conditions of the study the melting range of the pure active test material is 94.6 - 96.2 °C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
15 March 1994
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study without detailed documentation
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.:
>= 95.5 - <= 96.8 °C
Remarks on result:
other: Atmospheric pressure not specified.

The following melting points have been observed.

Test material determination 1: 95.5 - 96.1 °C

Test material determination 2: 95.7 - 96.8 °C

Reference substance, Benzile: 92.5 - 94.5 °C.

Reference substance, Benzoic acid: 122.7 - 125.0 °C.

From these results for the pure active test material the melting range is: 95.5 - 96.8 °C.

Conclusions:
Under the conditions of the study the melting range of the test material is 95.5 to 96.8 °C.
Executive summary:

The melting point of the test material was assessed according to OECD Test Guideline 102 and in compliance with GLP using the capillary method.

Under the conditions of the study the melting range of the test material is 95.5 to 96.8 °C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
14 December 1994
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study without detailed documentation
Qualifier:
according to guideline
Guideline:
other: CIPAC MT 2
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
other: Not specified.
Key result
Melting / freezing pt.:
>= 84 - <= 91 °C
Remarks on result:
other: Atmospheric pressure not specified.
Conclusions:
Under the conditions of the study the melting range of the test material is 84 to 91 °C.
Executive summary:

The melting range of the test material was assessed according to CIPAC MT2 and in compliance with GLP.

Under the conditions of the study the melting range of the test material is 84 to 91 °C.

Description of key information

Comb (2000b)

Under the conditions of the study the melting range of the test material is 93.5 to 97.5 °C.

O'Connor (1990)

Under the conditions of the study the melting range of the test material is 81.5 to 92.0 °C (354.5 - 365.0 K) (the mean of 81.5 - 91.5 °C and 81.5 - 92.0 °C).

Türk (1994)

Under the conditions of the study the melting range of the test material is 94.6 to 96.2 °C.

Supporting Study: Türk (1994b)

Under the conditions of the study the melting range of the test material is 95.5 to 96.8 °C.

Supporting Study: Kästel (1994)

Under the conditions of the study the melting range of the test material is 84 to 91 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
93.5 °C

Additional information

Comb (2000b)

The melting point of the test material was assessed according to OECD Test Guideline 102 and EU Method A.1. and in compliance with GLP using a capillary method. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Dried test material was pulverised to a fine powder and a small amount 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 (pure grade) was found to be 93.5 to 97.5 °C.

O'Connor (1990)

The melting range was assessed according to OECD Method 102, EEC Method A1, EPA FIFRASubdivision D § 63-5 and in compliance with GLP using the capillary method. 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 method 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 range of the test material is 81.5 to 92.0 °C (354.5 - 365.0 K) (the mean of 81.5 - 91.5 °C and 81.5 - 92.0 °C).

Türk (1994)

The melting range was assessed according to OECD Method 102 and in compliance with GLP using the capillary method. 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 also investigated for exothermic/endothermic effects by differential scanning calorimetry (DSC).

A melting curve was registered from 60 to 360 °C with a heating rate of 10 K/min (sample weight 3.48 mg). The melting curve shows an endothermic melting peak at about 100 °C, which agrees with the capillary method.

Under the conditions of the study the melting range of the pure active test material is 94.6 to 96.2 °C.

Supporting Study: Türk (1994b)

The melting point of the test material was assessed according to OECD Test Guideline 102 and in compliance with GLP using the capillary method. The study was awarded a reliability score of 2 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of the study the melting range of the test material is 95.5 to 96.8 °C.

Supporting Study: Kästel (1994)

The melting range of the test material was assessed according to CIPAC MT2 and in compliance with GLP. The study was awarded a reliability score of 2 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of the study the melting range of the test material is 84 to 91 °C.