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EC number: 271-668-0 | CAS number: 68603-62-3
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
- Study period:
- 10 July 2017 - 19 January 2018
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Remarks:
- Study was conducted in accordance with international guidelines and in accordance with GLP. All guideline validity criteria were met.
- Qualifier:
- according to guideline
- Guideline:
- EU Method A.1 (Melting / Freezing Temperature)
- Version / remarks:
- Regulation (EC) 440/2008 of 30 May 2008
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 102 (Melting point / Melting Range)
- Version / remarks:
- July 1995
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Type of method:
- differential scanning calorimetry
- Key result
- Melting / freezing pt.:
- >= -40 - <= 0 °C
- Atm. press.:
- >= 996 - <= 997 hPa
- Decomposition:
- no
- Sublimation:
- no
- Remarks on result:
- other: Range determined on the basis of two measurements.
- Remarks:
- A range rather than a mean is reported because the measured values deviated by more than 0.5 K.
- Conclusions:
- The melting point range/ freezing point range of the test item was determined to be: -40 ℃ - 0 ℃.
- Executive summary:
EU Method A.1. – The melting point/freezing point of the test item was determined using differential scanning calorimetry. The procedure employed was designed to be compatible with Method A.1. Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008.
Aliquots of test item (0.0083 - 0.0154 g) were placed in crucibles and subjected to a thermal program from -100 °C to 500 °C. Cooling at a constant rate of 0.25 K/min was followed by a waiting period of 30 minutes at -100 °C and heating at a constant rate of 10 K/min to 500 °C. Two determinations were carried out. Both determinations were conducted under an inert atmosphere.
A melting/freezing point range of –40.0 °C – 0 °C for the test item was determined at atmospheric pressure (996 – 997 hPa).
Reference
Table 2: Results of the DSC-measurements
No. |
Sample weight (mg) |
Onset of Effect (°C) |
Range of effect (°C)* |
Weight loss (mg) |
Atmospheric pressure (hPa) |
PN13868 |
8.32 |
248.91 |
160 to 410 (endo) |
7.90 |
996.9 |
PN13873 |
15.35 |
248.63 |
160 to 410 (endo) |
14.79 |
996.1 |
*positive heat flow for exothermic processes, negative heat flow for endothermic processes
To verify the results of the DSC measurement, an additional measurement with the test tube method was performed in the temperature range of 23.1 – 233.4 °C. Therefore, 8.12 g of the test item was heated up by a lighter. The observations during the test with the test tube method are summarized in Table 3.
Table 3: Observations during the test with the test tube
Temperature |
Observation |
Start (23.1 °C) |
High viscous yellow liquid |
89.3 °C |
Test item changes colour from yellow to brown |
163.2 °C |
Small bubbles slowly rise in the test item |
188.9 °C |
Test item boils and evaporates as withe fog, Apperance: dark brown liquid |
233.4 °C |
Stop of measurement |
According to the observations during the test with the test tube method, the endothermic effect in the temperature range of 160 – 410°C in the DSC measurements can be assigned to a boiling of the test item.
Description of key information
Melting Point Range: -40 °C - 0 °C (233.15 - 273.15 K) at 996 - 997 hPa; EU Method A.1.; S Seitz (2017)
Key value for chemical safety assessment
- Melting / freezing point at 101 325 Pa:
- -20 °C
Additional information
EU Method A.1. – The melting point/freezing point of the test item was determined using differential scanning calorimetry. The procedure employed was designed to be compatible with Method A.1. Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008.
Aliquots of test item (0.0083 - 0.0154 g) were placed in crucibles and subjected to a thermal program from -100 °C to 500 °C. Cooling at a constant rate of 0.25 K/min was followed by a waiting period of 30 minutes at -100 °C and heating at a constant rate of 10 K/min to 500 °C. Two determinations were carried out. Both determinations were conducted under an inert atmosphere.
A melting/freezing point range of –40.0 °C – 0 °C for the test item was determined at atmospheric pressure (996 – 997 hPa).
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