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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:
12.05.2004 - 07.07.2004
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Principles of method if other than guideline:
For the determination of the melting point of the test item three different methods were employed (OECD Guideline 102, EU-Method A.1., and the Penetrometer-Test.
Penetrometer-Test: The apparatus consists of a guide rod bar (47.5 g ± 0.05 g), a sieve plate (102.5 g ± 0.05 g) with cone shaped holes and a container with an internal diameter of 72-80 mm. The sample was put in the container, the container was closed and subsequently tempered for at least 2 h in thermostat (35 and 50°C) or in a drying chamber (75, 90, and 110°C), respectively. The sample container was placed on the table of the penetrometer beneath the sieve plate. The point of the sieve plate was placed on the surface of the test item. Subsequently the guide rod was loosen and the penetration of the sieve plate in the test item was measured as a function of time. At least three tests were performed. The test item is a solid if the penetration at 35°C ± 0.5°C
-after a time of 5 s ± 0.1 s is less than 15.0 mm ± 0.3 mm or
-after a time of 5 s ± 0.1 s is more than 15 mm ± 0.3 mm but the additional penetration after additional 55 s ± 0.5 s is less than 5.0 mm ± 0.5 mm. The same classification scheme was used for the evaluation of the tests at elevated temperature.
GLP compliance:
yes (incl. QA statement)
Type of method:
other: differential scanning calorimetry, capillary method and penetrometer test were conducted
Melting / freezing pt.:
> 85 - < 110 °C
Remarks on result:
other: the test item is a solid up to a temperature of 85°C and has no specific melting point

The melting point of partially unsaturated TEA-Esterquat was investigated using three different methods:

-OECD Guideline 102 and EU-Method A.1. (differential scanning calorimetry): The measurements in aluminium crucibles with a small hole showed a broad endothermic signal in the temperature range 20 -70°C. Due to the course of the endothermic effect and due to the differences between the two heating rates it was concluded that the endothermic signal did not represent a melting point of the test item

-OECD Guideline 102 and EU-Method A.1. (capillary method): two measurements were conducted but unclear results were obtained.

Due to this facts additional tests with

-the Penetrometer were performed: up to 85°C the test item was solid, at 110°C the test item was fluid.

According to the observation with the three different methods the following conclusion can be drawn:

The test item is a solid at ambient temperature and has the character of a waxy, viscous solidified liquid. The test item has no specific melting point. With increasing temperature, the viscosity of the test item decreases. According to the Penetrometer-Test, the test item is a solid up to a temperature of 85°C.

Conclusions:
The melting point of partially unsaturated TEA-Esterquat was investigated using three different methods (OECD Guideline 102 and EU-Method A.1., differential scanning calorimetry and capillary method) and the Penetrometer-Test. The test item has no specific melting point. With increasing temperature, the viscosity of the test item decreases. According to the Penetrometer-Test, the test item is a solid up to a temperature of 85°C. The test item is fluid at 110°C (mp:>85-110°C).
Executive summary:

The melting point of partially unsaturated TEA-Esterquat was investigated using three different methods (OECD Guideline 102 and EU-Method A.1., differential scanning calorimetry and capillary method) and the Penetrometer-Test. According to the observation with the three different methods the following conclusion can be drawn: The test item is a solid at ambient temperature and has the character of a waxy, viscous solidified liquid. The test item has no specific melting point. With increasing temperature, the viscosity of the test item decreases. According to the Penetrometer-Test, the test item is a solid up to a temperature of 85°C. The test item is fluid at 110°C.

Description of key information

Melting range: 85 - 110°C (EU method A.1, differential scanning calorimetry, capillary method); GLP; RL1

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
85 °C

Additional information

The melting point of partially unsaturated TEA-Esterquat was investigated using three different methods (OECD Guideline 102 and EU-Method A.1., differential scanning calorimetry and capillary method) and the Penetrometer-Test. The test item has no specific melting point. With increasing temperature, the viscosity of the test item decreases. According to the Penetrometer-Test, the test item is a solid up to a temperature of 85°C. The test item is fluid at 110°C (mp:>85-110°C).

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