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Physical & Chemical properties

Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Remarks:
freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
November 4, 2017
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:
method to determine freezing temperature
Remarks:
method of crystallization tube in freezing mixture ice/acetone
Specific details on test material used for the study:
STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: room temperature.
Key result
Melting / freezing pt.:
ca. -8.2 °C
Atm. press.:
ca. 1 005 hPa
Decomposition:
no
Sublimation:
no

Table 1. Measurement of the freezing point of N,N’-(ethoxymethylsilylene)bis[N-methylbenzamide]

 

Measurement I

Measurement II

Time [min]

Temperature of the test item [°C]

Temperature of the freezing mixture [°C]

Time [min]

Temperature of the test item [°C]

Temperature of the freezing mixture [°C]

0.0

0.2

-2.0

0.0

0.6

-3.2

1.0

0.0

-2.1

1.0

0.3

-3.4

2.0

-0.1

-2.4

2.0

0.0

-3.6

3.0

-0.3

-2.7

3.0

-0.2

-3.6

4.0

-0.4

-3.1

4.0

-0.4

-3.7

5.0

-0.6

-3.5

5.0

-0.7

-3.9

6.0

-0.9

-3.8

6.0

-1.0

-4.0

7.0

-1.1

-4.1

7.0

-1.3

-4.2

8.0

-1.2

-4.3

8.0

-1.5

-4.3

9.0

-1.4

-4.7

9.0

-1.7

-4.4

10.0

-1.6

-5.1

10.0

-1.9

-4.7

11.0

-1.9

-5.3

11.0

-2.2

-5.0

12.0

-2.2

-5.5

12.0

-2.4

-5.3

13.0

-2.4

-5.8

13.0

-2.6

-5.6

14.0

-2.6

-6.2

14.0

-2.7

-5.9

15.0

-2.9

-6.5

15.0

-2.9

-6.1

16.0

-3.2

-6.9

16.0

-3.1

-6.3

17.0

-3.4

-7.2

17.0

-3.3

-6.7

18.0

-3.7

-7.5

18.0

-3.5

-7.1

19.0

-3.9

-7.8

19.0

-3.7

-7.3

20.0

-4.1

-8.0

20.0

-3.8

-7.6

21.0

-4.4

-8.3

21.0

-3.9

-7.7

22.0

-4.7

-8.7

22.0

-4.1

-7.9

23.0

-5.0

-9.0

23.0

-4.3

-8.2

24.0

-5.2

-9.3

24.0

-4.6

-8.5

25.0

-5.5

-9.6

25.0

-4.8

-8.7

26.0

-5.8

-9.8

26.0

-4.9

-8.9

27.0

-6.1

-10.1

27.0

-5.1

-9.1

28.0

-6.4

-10.3

28.0

-5.3

-9.1

29.0

-6.6

-10.5

29.0

-5.6

-9.3

30.0

-6.9

-10.8

30.0

-5.8

-9.4

31.0

-7.3

-11.0

31.0

-6.0

-9.6

32.0

-7.6

-11.3

32.0

-6.1

-9.8

33.0

-7.9

-11.6

33.0

-6.2

-9.9

34.0

-7.9

-11.9

34.0

-6.4

-10.1

34.5

-8.0

-12.0

34.5

-

-

35.0

-8.0

-12.2

35.0

-6.7

-10.3

36.0

-8.0

-12.3

36.0

-6.9

-10.5

 

 

Measurement I

Measurement II

Time [min]

Temperature of the test item [°C]

Temperature of the freezing mixture [°C]

Time [min]

Temperature of the test item [°C]

Temperature of the freezing mixture [°C]

37.0

-8.1

-12.4

37.0

-7.1

-10.7

38.0

-8.3

-12.5

38.0

-7.4

-10.7

39.0

-8.6

-12.7

39.0

-7.6

-10.9

40.0

-8.9

-12.9

40.0

-7.8

-10.8

41.0

-9.1

-13.1

41.0

-7.9

-10.8

42.0

-9.3

-13.4

42.0

-8.1

-10.9

43.0

-9.4

-13.7

43.0

-8.3

-10.9

44.0

-9.5

-14.0

44.0

-8.5

-11.3

45.0

-9.6

-14.2

45.0

-8.5

-11.5

46.0

-9.8

-14.3

46.0

-8.5

-11.7

47.0

-10.1

-14.4

47.0

-8.6

-11.8

48.0

-10.4

-14.5

48.0

-8.6

-12.1

49.0

-10.5

-14.7

49.0

-8.6

-12.3

50.0

-10.8

-15.0

50.0

-8.6

-12.6

51.0

-11.0

-15.2

51.0

-8.7

-12.8

52.0

-11.3

-15.3

52.0

-8.9

-13.0

53.0

-11.5

-15.5

53.0

-8.9

-13.3

54.0

-11.7

-15.8

54.0

-9.0

-13.5

55.0

-11.9

-16.1

55.0

-9.2

-13.7

56.0

-12.1

-16.4

56.0

-9.5

-13.7

57.0

-12.1

-12.3

57.0

-9.7

-13.9

58.0

-

-

58.0

-9.9

-14.1

59.0

-

-

59.0

-10.2

-14.4

60.0

-

-

60.0

-10.4

-14.6

61.0

-

-

61.0

-10.7

-14.7

62.0

-

-

62.0

-11.0

-14.9

63.0

-

-

63.0

-11.2

-14.9

64.0

-

-

64.0

-11.4

-15.1

65.0

-

-

65.0

-11.7

-15.3

66.0

-

-

66.0

-11.9

-15.5

67.0

-

-

67.0

-12.0

-15.8

68.0

-

-

68.0

-12.2

-16.2

Initial value of freezing point [°C]

-7.9*

Initial value of freezing point [°C]

-8.5**

Average temperature of an initial freezing point±stand. Deviation, [°C]

8.2±0.4

  * As the value of an initial freezing point for the measurement No. 1 the value which corresponded to 33rdminute was assumed.

** As the value of an initial freezing point for the measurement No. 2 the value which corresponded to 44thminute was assumed.

During the test the temperature of samples initially decreased at a constant rate. For time ranging from 33 to 36 minute of measurement no. 1 and for time ranging from 44 to 50 minute, for measurement no. 2, the temperature of the test samples remained constant, which was related to release of crystallization heat. Test samples from the moment of temperature increase got cloudy and their viscosity increased (distinct increase in resistance to mixing).

Conclusions:
The average value of an initial freezing point of the test item is equal to 8.2 ± 0.4 ºC under atmospheric pressure of 1005 hPa.
Executive summary:

The freezing point was determine according to OECD 102 and EU method A.1, following GLP. The method of crystallization tube in freezing mixture ice/acetone was used. The liquid sample of the test item was placed in a Dewar vessel containing the freezing mixture. It was stirred and the temperature was recorded during cooling. The cooling temperature of the sample was read with an accuracy of 0.1 ºC. Two measurement runs were done. Both of them were performed under armospheric pressure of 1005 hPa. The average value of an initial freezing point of the test item is equal to -8.2 ± 0.4 ºC.

Description of key information

Key study: OECD 102 and EU method A.1. GLP study. The average value of an initial freezing point of the test item is equal to -8.2 ± 0.4 ºC under atmospheric pressure of 1005 hPa.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-8.2 °C

Additional information

Key study: The freezing point was determine according to OECD 102 and EU method A.1, following GLP. The method of crystallization tube in freezing mixture ice/acetone was used. The liquid sample of the test item was placed in a Dewar vessel containing the freezing mixture. It was stirred and the temperature was recorded during cooling. The cooling temperature of the sample was read with an accuracy of 0.1 ºC. Two measurement runs were done. Both of them were performed under armospheric pressure of 1005 hPa. The average value of an initial freezing point of the test item is equal to -8.2± 0.4 ºC.