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Physical & Chemical properties

Melting point / freezing point

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Administrative data

Link to relevant study record(s)

Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
30 November 2016 - 01 December 2016
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 for cross-reference:
reference to other study
Reason / purpose for cross-reference:
reference to same 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)
Remarks:
2015-03-05
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
°C
Atm. press.:
ca. 1 029.1 hPa
Decomposition:
no
Remarks:
No Melting point was observed. However a glass transition was observed from -47.7°C to -43.1°C.
Remarks on result:
other: First determination
Melting / freezing pt.:
°C
Atm. press.:
ca. 1 028.5 hPa
Decomposition:
no
Remarks:
No melting point is observed. However a glass transition was observed from -47.7°C to -42.8°C.
Remarks on result:
other: Second determination
Key result
Melting / freezing pt.:
°C
Remarks on result:
other: Final value - Mean of the two determinations - No Melting point was observed. However a glass transition was observed from -47.7°C to -42.8°C.

Pre-study:

Peaks assigned to the boiling of the substance were observed and measurement was stopped at 550°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

20

-150

10

17

He

60

YES

2

-150

-150

0

15

He

60

 YES
 3  -150 400   10  55  He  60  NO

*Gas injection rate in the furnace.

First Determination:

Mass taken: 14.11 mg

Results:  

No Melting point was observed. However a glass transition was observed from -47.7°C to -43.1°C.

Atmospheric pressure: 1029.1 hPa

Second Determination: 

Mass taken: 12.58 mg

Results:

No Melting point was observed. However a glass transition was observed from -47.7°C to -42.8°C.

Atmospheric pressure: 1028.5 hPa

Conclusions:
According to guideline OECD 102 and method EU A.1, no melting point of substance TERPENIC OLIGOMERS Batch 16-03 SI was observed from -20°C. However a glass transition was observed around -47.7°C to -42.8°C.
Executive summary:

A study was performed to determine the melting point/range of test item TERPENIC OLIGOMERS Batch 16 -03 SI. 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 -150°C.

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

Trial

Melting point/range

Ambient pressure

1

 /

1029.1 hPa

2

  /

1028.5 hPa

The melting point of the Indium respects the checking cards limits (156.5°C for a reference value of 156.6°C) so as its enthalpy (29.07 J/g for a reference value of 28.6 J/g). Therefore, this study is considered as valid.

No melting point was detected for both trials. However a glass transition was observed around -47.7°C to -42.8°C. This glass transition owns an endothermic peak. This peak characterizes the relaxation of mechanical strains into the test item during the glass transition.

Description of key information

The melting point was measured for terpenic oligomers.


 


No melting point was observed from -20°C. However a glass transition was observed  from -47.7°C to -42.8°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-20 °C

Additional information

Key studies 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 results can be used as the end point value.