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Physical & Chemical properties

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:
03 August 2015 - 05 August 2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Well documented study performed according to OECD 102 guideline and EU method A.1, under GLP and without deviation
Reason / purpose:
reference to other study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
2015-03-05
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
< -135.2 °C
Atm. press.:
ca. 1 011.6 hPa
Decomposition:
no
Remarks:
No melting point is observed from -20°C
Remarks on result:
other: First determination
Melting / freezing pt.:
< -135.5 °C
Atm. press.:
ca. 1 012.9 hPa
Decomposition:
no
Remarks:
No melting point is observed from -20°C
Remarks on result:
other: Second determination
Key result
Melting / freezing pt.:
< -135.3 °C
Remarks on result:
other: Final value - Mean of the two determinations

Pre-study:

Peaks assigned to the boiling of the substance were observed and measurement was stopped at 250°C.

Temperatures corresponding to these peaks were used to create the following temperature program:

 

Temperature program:

Step

Initial temperature (°C)

Final Temperature (°C)

Heating rate (°C/min)

Duration (min)

Furnace atmosphere

Rate* (mL/min)

Liquid nitrogen cooling

1

-195

-195

0

20

He

60

YES

2

-195

240

20

21'45

He

60

NO

*Gas injection rate in the furnace.

Even if our cooling system cannot reach -195°C, fixing this temperature allows the furnace to stabilize at approximately -170°C.

First Determination:

Mass taken: 13.70 mg

Results:  

Melting point is observed at -135.2°C.

Atmospheric pressure: 1011.6 hPa

Second Determination: 

Mass taken: 15.11 mg

Results:

Melting point was observed at -135.5°C.

Atmospheric pressure: 1012.9 hPa

Conclusions:
According to guideline OECD 102 and method EU A.1, no melting point of substance REACTION MASS OF BETA-PHELLANDRENE AND D-LIMONENE AND L-LIMONENE was observed from -20°C.
Executive summary:

A study was performed to determine the melting point/range of test item REACTION MASS OF BETA-PHELLANDRENE AND D-LIMONENE AND L-LIMONENE. The method used was Differential Scanning Calorimetry (DSC) and the test was conducted according to Regulation EC No. 440/2008 Method A.1 and OECD Test Guideline 102 , "Melting Point/Melting Range".

In this method, two crucibles were put in the apparatus furnace under inert atmosphere (helium) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied. The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram.

A cooling system using nitrogen allowed experiments with low temperature down to -170°C.

Two trials were conducted and corresponding thermograms were obtained, giving us the following results:

Trial

Melting point/range

Ambient pressure

1

 -135.2 °C

1011.6 hPa

2

  -135.5 °C

1012.9 hPa

The melting point values respect validity criteria (less than 0.5°C for the melting point).

Moreover, the melting point of the n-octane respects the checking cards limits (-57.6°C for a reference value of -56.8°C) so as the enthalpy of the indium (29.84 J/g for a reference value of 28.6 J/g). Therefore, this study is considered as valid.

No melting point of substance REACTION MASS OF BETA-PHELLANDRENE AND D-LIMONENE AND L-LIMONENE was observed from - 20°C. The melting point of the substance is -135.3°C.

Description of key information

The melting point of substance Reaction mass of beta-phellandrene and d-limonene and l-limonene is stated < -135.3°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-135 °C

Additional information

Key study conducted according to the OECD 102 Guideline and the EU A.1 method, under GLP without deviation and with certificate of analysis included. Therefore, a reliability of 1 is assigned and the result of this key study is proposed as the end point value.