Pentanediamide, N1,N5-dibutyl-2-[(2-ethyl-1-oxohexyl)amino]-, (2S)-

Melting point / freezing point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

10 February 2011

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:

capillary method

Melting / freezing pt.:

191.3 °C

Remarks on result:

other: ± 0.16 °C (95% confidence interval), in air atmosphere

Using a linear heating rate of 0.5 °C/min, the melting point of the test substance was found to be 191.3 ± 0.16 °C (95% confidence interval), i.e. 464.5 K. The details are summarised in Table 2.

During the tests the following transformation temperatures were recorded:

Temp. 1.: beginning of melting.

Temp. 2.: the shrunken sample begins to collapse downwards and liquefies

Temp. 3. final stage of melting (no solid particles)

Table 2. Measured temperatures corresponding to the melting of the test material (three experiments (I, II, III) with three parallel samples each (1, 2, 3)

	Measured Temperatures during the Main Study (°C)
	I / 1	I / 2	I /3	II / 1	II / 2	II / 3	III / 1	III / 2	III / 3	Mean
Temp. 1	186.8	186.8	186.8	186.9	186.9	186.9	187.1	187.1	187.1	186.9
Temp 2	189.3	189.9	189.3	188.8	189.5	189.0	189.4	189.4	189.4	189.3
Temp 3. Melting Point	191.1	191.3	191.3	191.1	191.6	191.1	191.6	191.5	191.4	191.3 ± 0.16

Conclusions:

Using a linear heating rate of 0.5 °C/min, the melting point of the test substance was found to be 191.3 ± 0.16 °C (95% confidence interval), i.e. 464.5 K.

Executive summary:

The melting point for the test substance was determined in accordance with guidelines OECD 102 and EU Method A.1.

For the determination of the melting point or melting range, the capillary method was used. A small amount of the test item was heated in the electronic controlled sample block and the temperature around the sample was displayed. The sample was observed visually while raising the temperature. The initial and final melting temperatures were determined.

Using a linear heating rate of 0.5°C/min the melting point of the test substance was found to be 191.3 ± 0.16 °C (95 % confidence interval), i.e. 464.5 K.

During the tests the following transformation temperatures were recorded:

- the beginning of melting: 186.9 °C

- the final stage of melting: 191.3 °C

- accuracy: <0.5 °C

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

2 April 2001 - 9 April 2001

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

capillary method

Melting / freezing pt.:

183.5 °C

Remarks on result:

other: The melting point of the test material was determined to be: 183.5 °C ± 0.9 °C (standard deviation) at atmospheric pressure.

Atmospheric pressure reading not specifically stated in study report.

In the preliminary DSC test, an endothermic heat effect, the melting, was observed at about 177 °C. After the experiment, the sample had lost about 94 % of its mass and the colour of the sample was changed to black.

In order to determine the melting point more precisely, further tests were performed using the capillary tester. A total of 4 samples were heated with a heating rate of 1 K/min. All samples were completely melted between 182.9 °C and 184.0 °C. After the measurement the samples were clear, yellowish melted.

Conclusions:

In conclusion, the melting point of the test material was determined to be 183.5 °C ± 0.9 °C.

Executive summary:

In a melting point determination study (793618), the melting point of the test material was determined to be 183.5 °C ± 0.9 °C, according to EU test method A.1.

Description of key information

Two melting point studies have been conducted by capillary methods; both were conducted to GLP using recognised test methods.

One gave a result of 183.5 °C ± 0.9 °C, and the other a result of 191.3 ± 0.16 °C (95% confidence interval), i.e. 464.5 K.

As the result of 191.3 ± 0.16 °C comes from a more recently conducted study, this is selected as the key result.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

191 °C

Additional information

Key Study

The melting point for the test substance was determined in accordance with guidelines OECD 102 and EU Method A.1.

For the determination of the melting point or melting range, the capillary method was used. A small amount of the test item was heated in the electronic controlled sample block and the temperature around the sample was displayed. The sample was observed visually while raising the temperature. The initial and final melting temperatures were determined.

Using a linear heating rate of 0.5°C/min the melting point of the test substance was found to be 191.3 ± 0.16 °C (95 % confidence interval), i.e. 464.5 K.

During the tests the following transformation temperatures were recorded:

- the beginning of melting: 186.9 °C

- the final stage of melting: 191.3 °C

- accuracy: <0.5 °C

Supporting Study

In a melting point determination study (793618), the melting point of the test material was determined to be 183.5 °C ± 0.9 °C, according to EU test method A.1.