Tobacco, ext.

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Testing was conducted between 6 August 2018 and 8 August 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Justification for type of information:

The study was conducted according to an internationally recognised method, and under GLP. The test substance is adequately characterised. Therefore full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

Inspected on 4,5 and 6 July 2016/ Signed on 10 January 2017

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

>= -3.4 - <= 51.2 °C

Results

All the raw data (calibration, pre-test and main tests) is in the experimental report.

Pre-study

Mass taken: 11.11 mg

Heating rate: 10°C/min

Melting range was observed between 0.8 °C (onset temperature of the first melting peak) and 52.1°C (top of the last melting peak).

Main tests:

-Test 1:

Mass taken: 11.98 mg

A glass transition was observed near -72.9°C and was followed by an exothermic peak at -25.5°C (onset temperature) that seems to be a crystallization as no mass variation was observed. Then a melting range was detectedon the thermogram from -3.3°C (onset temperature of the first endothermic peak) to 51.4°C (peak temperature of the second endothermic peak).These peaks may correspond to the melting of two different crystalline phases.

-Test 2:

Mass taken: 10.87 mg

A glass transition was observed near -75.8°C and was followed by an exothermic peak at -26.8°C (onset temperature) that seems to be a crystallization as no mass variation was observed. Then a melting range was detected on the thermogram from -3.7°C (onset temperature of the first endothermic peak) to 51.0°C (peak temperature of the second endothermic peak). These peaks may correspond to the melting of two different crystalline phases.

-Test 3:

Mass taken: 12.37 mg

A glass transition was observed near -75.1°C and was followed by an exothermic peak at -26.4°C (onset temperature) that seems to be a crystallization as no mass variation was observed. Then a melting range was detected on the thermogram from -3.6°C (onset temperature of the first endothermic peak) to 51.0°C (peak temperature of the second endothermic peak). These peaks may correspond to the melting of two different crystalline phases.

Apparatus check:

-Temperature:

Reference substance: Indium

Expected melting point: 156.6 +/- 0.5°C

Obtained melting point: 156.5°C

-Sensitivity

Reference substance: Indium

Expected enthalpy: 28.6 +/- 2.9 J/g

Obtained enthalpy: 29.75 J/g

Conclusion

A glass transition followed by a crystallization (exothermic peak without mass variation) is observed before the melting.

The melting range of the substance was determined as – 3.4°C to 51.2°C (mean oftrials 1 and 3) and may correspond to the melting of two different crystalline phases.

Conclusions:

The melting range of the substance was determined as – 3.4°C to 51.2°C.

Executive summary:

The study was performed in order to determine the melting point of test item according to OECD 102, resp. EU A.1 guideline, using the DSC method.

3 trials were performed.A glass transition followed by a crystallization (exothermic peak without mass variation) is observed before the melting.

The melting range of the substance was determined as – 3.4°C to 51.2°C (mean of trials 1 and 3) and may correspond to the melting of two different crystalline phases.

Description of key information

A glass transition followed by a crystallization (exothermic peak without mass variation) is observed before the melting.

The melting range of the substance was determined as – 3.4°C to 51.2°C (mean of trials 1 and 3) and may correspond to the melting of two different crystalline phases.

Additional information

A fully reliable experimental study conducted according to OECD 102/ EU A1 guideline is available.

It is considered as a key study.