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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:
2017-06-08 to 2017-08-14
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted 27 July, 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
30 May, 2008
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
243 °C
Atm. press.:
1 013 hPa
Decomposition:
yes
Remarks:
after melting
Decomp. temp.:
370 °C
Sublimation:
no

Preliminary test:

Two steps were registered with maxima at 329°C resp. 495°C. A total mass loss of 99.4 % at the final temperature could be observed (mass change in the range until 370°C: 80.0 %; mass change in the range from 370 to 600°C: 19.4 %). No significant mass loss occurred due to purging.

After cooling the residue was brown-black on the inside of the crucible and also on its cover.

Main test:

The DSC measurements were performed twice in the temperature range from 20 - 350°C resp. from 20 - 450°C. A sharp endothermic peak indicating a melting point could be observed (peak maximum: 245°C/ 246°C; extrapolated onset temperature: 242.78°C/ 242.85°C; rounded mean of both determinations: 243°C). Upon further heating the DSC-curve showed no more sharp peaks but the typical fluctuating course indicating decomposition. Reweighing after the measurement showed that the sample had lost 39.3 %/61.6 % of its mass. After the first run the residue looked liquid and colourless with single black parts, after the second run the residue looked liquid and dark-brown discoloured.

Conclusions:
The melting temperature of n-Butyltriphenylphosphonium bromide was determined to be 243°C.

Description of key information

melting point: 243 °C

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
243 °C

Additional information

GLP study according to OECD Guideline 102 (27 July 1995) and EU Method A.1 (30 May, 2008) using differential scanning calorimetry

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