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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:
09 September 2016 to 12 September 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline 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)
Type of method:
differential scanning calorimetry
Key result
Decomposition:
yes
Decomp. temp.:
ca. 70 °C

The DSC measurement in an aluminium crucible with a hole showed an exothermal effect starting at approx. 70 °C. In the temperature range of 100 – 170 °C a multistage endothermal effect was observed. After the measurement, the test item was discoloured to black. The mass loss after the DSC measurement amounted to 51 %.

An additional measurement with the capillary method was performed in order to clarify the results. A high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. Under consideration of the results from the DSC measurement and the capillary method it was concluded that the test item had no melting point at atmospheric conditions

Table1: DSC measurements

No.

Test item /

mg

Starting temperature /

°C

Final test temperature /

°C

Temperature range /

°C

Crucible

Observations after the measurement

1

14.56

25

500

70 – 100
(exothermal)

100 – 170
(endothermal, multistage)

Aluminium with a hole

Test item was black after the measurement; mass loss: 51 %

Table2: Results of the capillary method

No.


Set point /
°C

Heating rate / K/min

End
point /
°C

Remarks

1

60

10

220

Approx. 88 °C:    test item became darker

Approx. 101 °C:  test item started to melt

Approx. 120 °C:  test item discoloured to grey-brown

Approx. 133 °C:  test item discoloured to black

Approx. 142 °C:  test item was partly melted, formation of bubbles

Approx. 150 °C:  formation of condensate at the cold top of the capillary

Approx. 173 °C:  test item not completely melted, appeared like a black residue

Approx. 220 °C:  no further effect observed
Conclusions:
The test item had no melting point at atmospheric conditions. Decomposition started at approximately 70 °C.

Executive summary:

This is a GLP compliant, study following OECD guideline 102 and is considered suitable for use as the key study for this endpoint. The melting point / melting range were determined by differential scanning calorimetry (DSC) and capillary tube in a metal block.

The test item had no melting point at atmospheric conditions. Decomposition started at approx. 70 °C.

Description of key information

The test item had no melting point at atmospheric conditions. Decomposition started at approximately 70 °C.

Key value for chemical safety assessment

Additional information

A GLP study following OECD guideline 102 was performed to determine the melting point of palladium (II) nitrate hydrate (Nau 2016). The study is considered reliable and suitable for use as a key study for this endpoint. It was concluded that the test item had no melting point at atmospheric conditions as decomposition started at approximately 70 °C.