Reaction mass of dieuropium tricarbonate and digadolinium tricarbonate and disamarium tricarbonate

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:

28 September 2017 to 17 October 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Melting / freezing pt.:

> 600 °C

Decomposition:

no

Remarks on result:

other: Atmospheric pressure not specified.

Remarks:

Endothermic peaks observed from 100 °C to 220 °C, 300 °C to 350 °C and 375 °C to 400 °C may correspond to dehydration of the test item and release of carbon monoxide or carbon dioxide.

Two assays were performed during the test but no melting point was observed.

Assay No. 1

Gas used: Nitrogen

Ventilation: Yes

Crucible used: Aluminium, 120 μL, with lid

Mass of test item: 14.25 mg

Program Phase 1: Isotherm at 25°C for 5 min

Heating phase from 25°C to 600°C at 10°C/min

Several endothermic peaks were observed from 100°C to about 220°C and from about 300°C to 350°C and from 375°C to 400°C. They do not correspond to a melting point of the test material; the test material remained a white powder after the assay. They may correspond to dehydration of the test material and release of carbon monoxide or carbon dioxide. A loss of mass of 6.59 mg of test material was recorded corresponding to 46% of the initial mass.

 

Assay No. 2

Gas used: Nitrogen

Ventilation: Yes

Crucible used: Aluminium, 120 μL, with lid

Mass of test item: 17.46 mg

Program Phase 1: Isotherm at 25°C for 5 min

Heating phase from 25°C to 600°C at 10°C/min

The same endothermic peaks were recorded. A loss of mass of 8.15 mg of test material was recorded corresponding to 47% of the initial mass.

Conclusions:

Under the conditions of the test no melting point of the test material was recorded up to 600°C.

Executive summary:

The melting point of the test material was assessed according to EU Method A.1. and OECD Test Guideline 102.

An aliquot of test material was placed in a crucible. A lid was fitted and the crucible was placed in the DSC analyser. The heating procedure was performed from room temperature to 600°C. Several heating procedures were performed until two values for the melting point were in the range of the estimated accuracy of the method: 0.5°C up to 326.9°C and ± 2.0°C above 326.9°C.

The melting point was calculated automatically using the Setsoft program by linear integration of the curves obtained: “Heat flow as a function of the temperature”.

Several endothermic peaks were observed from 100°C to about 220°C and from about 300°C to 350°C and from 375°C to 400°C. They do not correspond to a melting point of the test material; the test material remained a white powder after the assay. They may correspond to dehydration of the test material and release of carbon monoxide or carbon dioxide. A loss of mass of 6.59 mg of test material was recorded corresponding to 46% of the initial mass. The same endothermic peaks were recorded in the second assay. A loss of mass of 8.15 mg of test material was recorded corresponding to 47% of the initial mass.

No melting point of the test item was recorded up to 600°C.

Description of key information

Under the conditions of the test no melting point of the test material was recorded up to 600°C.

Additional information

The melting point of the test material was assessed according to EU Method A.1. and OECD Test Guideline 102.

An aliquot of test material was placed in a crucible. A lid was fitted and the crucible was placed in the DSC analyser. The heating procedure was performed from room temperature to 600°C. Several heating procedures were performed until two values for the melting point were in the range of the estimated accuracy of the method: ± 0.5°C up to 326.9°C and ± 2.0°C above 326.9°C.

The melting point was calculated automatically using the Setsoft program by linear integration of the curves obtained: “Heat flow as a function of the temperature”.

Several endothermic peaks were observed from 100°C to about 220°C and from about 300°C to 350°C and from 375°C to 400°C. They do not correspond to a melting point of the test material; the test material remained a white powder after the assay. They may correspond to dehydration of the test material and release of carbon monoxide or carbon dioxide. A loss of mass of 6.59 mg of test material was recorded corresponding to 46% of the initial mass. The same endothermic peaks were recorded in the second assay. A loss of mass of 8.15 mg of test material was recorded corresponding to 47% of the initial mass.

No melting point of the test material was recorded up to 600°C.