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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:
02 June 2016 - 16 June 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
> 2.6 - < 3.7 °C
Atm. press.:
> 1 006 - < 1 008 hPa
Decomposition:
yes
Remarks:
Decomposition energy of -270 J/g
Decomp. temp.:
> 380 - < 470 °C

During the cooling phase an exothermic effect could be observed in the temperature range of approximately -10 to -30 °C, which can be assigned to the freezing of the test item. In the subsequent heating phase an endothermic effect was detected inthe temperature range of -10 to 20 °C, which can be assigned to the melting of the test item. As the onset temperatures in both tests deviate by more than 0.5 K from their mean value of 3.12 °C, the test item has a melting range of 2.6 to 3.7 °C.

Due to the low energy of the melting peak, the melting of the test item was verified. A small amount of the test item in a test tube was cooled down to -24.5 °C in a freezer. At this temperature the test item was solid. For warming up, the frozen sample was placed in a refrigerator at 3.5 °C. After eight hours the sample was still frozen. After 10 minutes at room temperature the test item was liquefied. Therefore the melting point in the DSC-measurement was confirmed.

No.

Sample weight / mg

Onset of Effect / °C

Range of effect / °C

Weight loss / mg

Atmospheric pressure / hPa

Remark

PN11224

14.49

3.65
303.09

-10 – 20 (endo)
120 – 320 (endo)

14.49

1007.9

Figure 1

PN11234

16.70

2.59
302.18

0 – 20 (endo)
120 – 320 (endo)

16.58

1005.9

Figure 2

Conclusions:
The test Item reaction mass of N-butylphthalimide and N-sec-phthalimide and N-propylphthalimide has a melting range of 2.6 to 3.7 °C at atmospheric pressure (1006 or 1008 hPa, respectively ) as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).
Executive summary:

The test item reaction mass of N-butylphthalimide and N-sec-phthalimide and N-propylphthalimide has a melting range of 2.6 to 3.7 °C at atmospheric pressure (1006 or 1008 hPa, respectively) as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Description of key information

The test item has a melting range of 2.6 to 3.7 °C at atmospheric pressure (1006 or 1008 hPa, respectively) as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Key value for chemical safety assessment

Additional information

Melting point range of 2.6 to 3.7 °C.