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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:
2012-05-29
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
, 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
, 2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Atm. press.:
1 013 mBar
Decomposition:
yes
Decomp. temp.:
320 °C
Remarks on result:
other: only atmospheric pressure was stated, 1013mbar were assumed

In the thermograms of the DSC runs in closed crucibles under N2, were two endothermic effects observed, in the temperature range of 25 °C - 500 °C. The first was between 90 - 230 °C and the second was between 300 - 350 °C. The test material did not melt during the test but turned black. This color change indicates presumably a thermal decomposition.

No.

Sample weight / mg

Onset of Effect / °C

Range of effect / °C

Weight loss / mg

1

10.22

123
315

90 - 230
300 - 340

0

2

9.75

129
326

90 - 230
300 - 340

0

Another qualitative experiment using a melting-point apparatus (Büchi B-540) was carried out to investigate melting and decomposition of the test item further. In an open melting tube, the test material did not change colour up to 230 °C. Starting at 250 °C, the sample turned darker and turned completely black at ca. 320 °C. A melting of the test material could not be observed.

In sum, the following effects were observed in two DSC-measurements in glass crucibles without oxygen:

1.   Endothermic effect due to evaporation of H2O in the temperature range up to 190 °C.

2.   Endothermic effect due to thermal decomposition in the temperature range of 300 ‑ 350 °C with an onset temperature of 320 °C.

Conclusions:
Vanadium, oxalate complexes did not melt at test temperatures ranging from 25 °C to 500 °C and atmospheric pressure but started to decompose a 320 °C.

Description of key information

Vanadium, oxalate complexes decomposes at 320 °C.

Key value for chemical safety assessment

Additional information

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