Registration Dossier
Registration Dossier
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EC number: - | CAS number: -
Melting point / freezing point
Administrative data
Link to relevant study record(s)
- Endpoint:
- melting point/freezing point
- Type of information:
- experimental study
- Adequacy of study:
- key study
- 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:
- differential scanning calorimetry
- Key result
- Remarks on result:
- other: No melting point was observed and evidence of decomposition was seen.
- Conclusions:
- No melting point was observed and evidence of decomposition was seen.
- Executive summary:
The objective of the study was to determine the melting point of the test substance according to OECD guideline 102 and EU method A.1. An initial test was carried out using the heating ramp specified in the protocol of 20°C to 400°C at 10°C/minute. This gave a broad endotherm with an onset of 108.73°C. It was suspected that this was due to loss of water as this was stated as an impurity. There was also the start of an exotherm with a start temperature of 333.30°C at the end of the run. As the appearance of the test substance had changed to a dark granular residue after the test, this exotherm was thought to be due to decomposition. A second test was carried out which confirmed the results of the first test. Further testing was then carried out using an open pan in the DSC instrument so as to be able to view any changes in the test substance during testing. Using an open pan, and ramping the temperature from 20°C to 140°C at 10°C/minute. This gave a broad endotherm with an onset at 23.42°C, possibly due to evaporation of moisture. The test substance remained unchanged in appearance (yellow powder). The weight loss was measured and found to be 4.97 mg, which was thought to be due to moisture loss. The pan and test substance were then returned to the DSC instrument and heated from 20°C to 220°C at 10°C/minute. A small endotherm with an onset at 143.74°C was observed. The test substance remained unchanged (yellow powder) and no significant weight change was observed. Finally, the pan and test substance were returned to the DSC instrument and heated from 20°C to 400°C at 10°C/minute. This time no endotherm was seen but the appearance of the test substance changed to a dark orange colour, which suggested that the original final exotherm was due to decomposition. This supports the suggestion that moisture loss was causing the endotherm. No melting point was observed and evidence of decomposition was seen.
Reference
Test 1
A broad endotherm with an onset at 108.73°C, possibly due to evaporation of moisture, was observed followed by an exotherm, starting at 333.30°C, probably due to decomposition. After the test, a dark granular residue remained in the DSC pan.
Test 2
A broad endotherm with an onset at 106.49°C, possibly due to evaporation of moisture, was observed followed by an exotherm, starting at 334.96°C, probably due to decomposition. After the test, a dark orange powder remained in the DSC pan.
Test 3
A broad endotherm with an onset at 23.42°C, possibly due to evaporation of moisture, was observed. The test substance remained unchanged. Weight loss of 4.97 mg was observed, probably due to the loss of moisture.
Test 3a
A small endotherm with an onset at 143.74°C was observed. The test substance remained unchanged. No further significant weight change was observed.
Test 3b
No endotherms were observed supporting the theory that the broad endotherm observed in test 1 and 2 was due to moisture loss. The test substance was a dark orange powder residue at the end of the test, supporting the theory that the exotherm observed in test 1 and 2 was due to decomposition.
No melting point was observed and evidence of decomposition was seen.
Description of key information
Key study: OECD guideline 102 and EC method A.1. GLP study.
No melting point was observed and evidence of decomposition was seen.
Key value for chemical safety assessment
Additional information
Key study: OECD guideline 102 and EC method A.1. GLP study.
No melting point was observed and evidence of decomposition was seen.
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