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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:

04 December 2020 - 19 February 2021

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study performed according to OECD Test Guideline No. 102, "Melting Point/Melting Range" and Regulation EC No. 440/2008 Method A.1, under GLP, without deviation and with certificate of analysis included.

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:

not specified

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

not specified

GLP compliance:

yes (incl. QA statement)

Remarks:

2018-11-15

Type of method:

differential scanning calorimetry

Melting / freezing pt.:

-89.6 °C

Atm. press.:

98.5 kPa

Decomposition:

no

Melting / freezing pt.:

-90.1 °C

Atm. press.:

98.5 kPa

Decomposition:

no

Melting / freezing pt.:

-89.6 °C

Atm. press.:

98.6 kPa

Decomposition:

no

Key result

Melting / freezing pt.:

-89.6 °C

Decomposition:

no

Sublimation:

no

Remarks on result:

other: mean of determinations 1 and 3

Results:

Pre-Study: 

Peaks assigned to the freezing, melting and boiling of the substance were observed and measurement was stopped at 340°C (Figure 1).

The melting point of the substance was observed at -88.4°C.

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

Step	Initial Temperature (°C)	Final Temperature (°C)	Heating (or cooling) rate (°C/min)	Duration (min)	Furnace atmosphere	Rate* (mL/min)	Liquid nitrogen cooling
1	20	-120	-10	14	He	60	YES
2	-120	-120	0	10	He	60	YES
3	-120	350	10	47	He	60	NO

*Gas injection rate in the furnace.

 

First Determination:

Mass taken: 13.81 mg
Temperature calibration file: CAN03-Al-He-10K-04
Sensitivity calibration file: CAN03-Al-He-10K-04
File name: DSC 20-036 01
The thermogram of the first determination is shown in Figure 2

Results:
The melting point of the substance was observed at -89.6°C (onset temperature of the peak).

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 98.5 kPa.

 

Second Determination:

Mass taken: 13.05 mg
Temperature calibration file: CAN03-Al-He-10K-04
Sensitivity calibration file: CAN03-Al-He-10K-04
File name: DSC 20-036 02
The thermogram of the second determination is shown in Figure 3

Results:
The melting point of the substance was observed at -90.1°C (onset temperature of the peak).

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
As the boiling point values of determinations 1 and 2 did not respect validity criteria (no more than 0.5°C of difference up to 326.85°C), a third determination was performed.
Atmospheric pressure: 98.5 kPa.

 

Third Determination:

Mass taken: 13.74 mg
Temperature calibration file: CAN03-Al-He-10K-04
Sensitivity calibration file: CAN03-Al-He-10K-04
File name: DSC 20-036 03
The thermogram of the third determination is shown in Figure 4

Results:
The melting point of the substance was observed at -89.6°C (onset temperature of the peak).

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 98.6 kPa.

 

Conclusions:

The melting point of the substance was determined as -89.6°C (mean of determinations 1 and 3).

Executive summary:

A study was performed to determine the melting point/range and boiling point of the test item using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.1 and OECD Test Guideline No. 102, "Melting Point/Melting Range"(1995).

In this method, two crucibles, with pierced lid, 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 liquid nitrogen allowed experiments with low temperatures down to -120°C.
Results. Three trials were conducted and corresponding thermograms were obtained, giving us the following results:
Table: Results

Trial	Melting point	Ambient pressure
1	-89.6 °C	98.5 kPa
2	-90.1°C	98.5 kPa
3	-89.6°C	98.6 kPa

 

Melting point occur as a single peak. The melting point values from trials 1 and 3 respect validity criteria (no more than 0.5°C of difference up to 326.85°C).
Moreover, the melting point of the Indium respects the checking cards limits (156.4°C for a reference value of 156.6°C) so as its enthalpy (29.16 J/g for a reference value of 28.6 J/g).

The melting point of the substance was determined as -89.6°C (mean of determinations 1 and 3).

Description of key information

Mp: -89.6 ºC at 98.6 kPa, OECD TG 102

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

-89.6 °C

Additional information

A study was performed to determine the melting point/range and boiling point of the test item using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.1 and OECD Test Guideline No. 102, "Melting Point/Melting Range"(1995).

The melting point of the substance was determined as -89.6°C (mean of determinations 1 and 3).