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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:
February 07th, 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted July 27, 1995
Qualifier:
according to
Guideline:
other: OECD Guideline 113 (Screening Test for Thermal Stability and Stability in Air)
Version / remarks:
adopted May 12, 1981
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
The test item was used in its initial form.
Melting / freezing pt.:
96 - 127 °C
Atm. press.:
1 atm
Decomposition:
yes
Decomp. temp.:
252 - 344 °C

Before the test the appearance of test item was red, clay; after the experiments the test item became black melts with bubbles in the melt.

During the heating two consecutive endotherm peaks were observed in the temperature range of approx. 96 ˗ 127 °C, which can be associated with the melting of the test item. Afterwards, in the temperature range of approx. 252 ˗ 344 °C two contiguous exothermic decomposition reaction peaks were observed.

Summary of the DSC Test of Test Item

Peak 1 Onset of effect (°C) Endset of effect (°C) Left Limit (°C) Right Limit (°C) Area (mJ)

 Test itemΔH (g/J)

Sample 1

94.86

112.69

32.57

117.93

-9062.81

910.84

Sample 2

98.08

113.71

50.49

118.87

-7564.37

750.43

Mean

96.47

113.2

41.53

118.4

-

-

Peak 2

Sample 1

121.44

127.44

118.05

129.67

-229.72

23.09

Sample 2

120.16

126.44

118.91

128.34

-166.39

16.51

Mean

120.8

126.94

118.48

129.01

-

-

Peak 3

Sample 1

288.29

307.76

252.58

343.93

2979.97

-299.49

Sample 2

280.43

303.94

251.82

343.82

3488.71

-346.1

Mean

284.36

305.85

252.2

343.88

-

-

Data of weight and weight loss of the DSC run in the first experiment

Sample weight [mg]

Total loss of Mass of the Sample (%)

9.95

72.7

Values of the DSC run in the first experiment

Onset of effect (°C) Endset of effect (°C) Left Limit (°C) Right Limit (°C) Area (mJ)

 Test itemΔH(J/g)

Peak 1

94.86

112.69

32.57

117.93

-9062.81

910.84 (endothermic)

Peak 2

121.44

127.44

118.05

129.67

-229.72

23.09 (endothermic)

Peak 3

288.29

307.76

252.58

343.93

2979.97

 -299.49 (exothermic)

Data of weight and weight loss of the DSC run in the second experiment

Sample weight [mg]

Total loss of Mass of the Sample (%)

10.08

69.6

Values of the DSC run in the second experiment

Onset of effect (°C)

Endset of effect (°C)

Left Limit (°C)

Right Limit (°C)

Area (mJ)

Test item ΔH (J/g)

Peak 1

98.08

113.71

50.49

118.87

-7564.37

750.43 (endothermic)

Peak 2

120.16

126.44

118.91

128.34

-166.39

16.51 (endothermic)

Peak 3

280.43

303.94

251.82

343.82

3488.71

+346.10 (exothermic)

Conclusions:
The substance melts approx. at 96 - 127 °C.
Executive summary:

The thermal behaviour of test item was investigated using differential scanning calorimetry method, in accordance with OECD guidelines 102 and 113.

A small amount of test item was weighed into a one-way 40 µl aluminum crucible and sealed with closed aluminum lid using a capsule presser. Thus, prepared capsule was inserted into the furnace of the DSC device and heated from 25 to 500 °C with 10 °C/minutes heating rate. The experiment was performed in duplicate.

Before the test the appearance of test item was red, clay; after the experiments the test item became black melts with bubbles in the melt.

During the heating two consecutive endotherm peaks were observed in the temperature range of approx. 96 ˗ 127 °C, which can be associated with the melting of the test item. Afterwards, in the temperature range of approx. 252 ˗ 344 °C two contiguous exothermic decomposition reaction peaks were observed.

Conclusion

The substance melts approx. at 96 - 127 °C.

Description of key information

The substance melts approx. at 96 - 127 °C.

Key value for chemical safety assessment

Additional information

OECD 102/113 - differential scanning calorimetry method