Reaction mass of cobalt sulphide and nickel sulphide and trinickel disulphide

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:

2010-09-13 to 2010-10-08

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Guideline 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:

no

Type of method:

other: Differential scanning calorimetry

Melting / freezing pt.:

> 600 °C

Atm. press.:

1 013 mBar

Remarks on result:

other: The test item has no melting point under atmospheric conditions up to 600°C. There was no atm. pressuere stated, it was assumed to be 1013mbar.

Thermal Stability

The DSC-measurement in a closed glass crucible with the test item showed two endothermal effects in the temperature range of 130 °C to 195 °C and 205 °C to 292 °C, respectively.

Melting Point / Melting Range // Boiling Point / Boiling Range(DSC)

The DSC-run up to the maximum temperature of 600 °C in an aluminium crucible with a hole showed two endothermic effects in the temperature range of 70 °C to 170 °C (this first endothermic effect could at least partially be caused by the evaporation o0f water (water content 15.4% according to sponsor´s information)) and 340 °C to 570 °C(this second endothermic effect could be caused by some kind of physical change, e.g. changes of the crystal structure), respectively with an overall energy of 665 J/g. A mass loss of about 10 mg was detected.

An optical inspection after the measurement showed that the test item was unchanged (regarding both the physical form and the colour of the test item).

No.	Set point	Heating rate	End point	Melting properties	Remarks
1	50 °C	10 K/min	400 °C	no melting observed	Starting at about 100 °C some liquid separated and condensed at the “cold” surface of the glass tube outside the heating block. An optical inspection after the measurement showed that the solid test item was unchanged (black powder).

In the capillary measurement the main part of the test item showed no changes in the aggregate state. Thus it was concluded, that the test item does not melt or boil up to the temperature of 400 °C.

Conclusions:

The test item has no melting point under atmospheric conditions up to 600°C.

Description of key information

No melting point can be stated. Reaction mass of cobalt sulphide, nickel sulphide and trinickel disulphide had no melting point under atmospheric conditions up to 600°C.

Additional information

The melting point of the test substance was determined according to OECD guideline 102 with the differential scanning calorimetry method (DSC).The test item was heated up from ambient to the final temperature (600 °C) at a constant heating rate (10 K/min) in a defined atmosphere (nitrogen). The quantity of heat absorbed or released was measured and recorded. Aluminium crucibles with a small hole were used as containers for the test item and as empty reference crucible. A measurement in a capillary tube in a metal block was used to clarify the results from the DSC-measurement. The maximum temperature of this equipment is limited to 400 °C. Set point and maximum temperature were chosen according to the results of the DSC measurements. The results of the optical inspection and the capillary measurement suggest that reaction mass of cobalt sulphide, nickel sulphide and trinickel disulphide has no melting point at atmospheric condition up to the maximum temperature of 600 °C.