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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-09-07 to 2018-01-11
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reference:
Composition 0
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Test material information:
Composition 1
Atm. press.:
1 003.3 hPa
Decomposition:
yes
Decomp. temp.:
ca. 400 °C
Sublimation:
no
Remarks on result:
other: no melting point up to 500 °C

Melting Point (DSC)

In the temperature range of 160 °C – 240 °C, an endothermic effect was observed. In the temperature range 400 – 470 °C an exothermal decomposition with an average energy of -400 J/g was observed.

Results of the DSC-measurements

No.

Sample weight [mg]

Onset of Effect [°C]

Range of effect [°C]

Weight loss [mg]

Atmospheric pressure / hPa

PN14201

10.00

179.76

160 – 240 (endo)

400 – 470 (exo)

9.66

1003.6

PN14202

11.21

181.22

170 – 240 (endo)

420 – 470 (exo)

9.93

1003.0

Measurements by the Capillary Method

To verify the results of the DSC measurement, an additional measurement with the capillary method (Apparatus: Stuart Melting Point SMP 30) was performed in the temperature range of 50 °C – 400 °C with a heating rate of 10 K/min. No melting, boiling or change of the colour or of the physical state of the test item was observed during the measurement with the capillary method. According to the observations during the tests with the capillary method, the endothermic effect starting at 160 °C in the DSC measurements with open crucibles cannot be assigned to the melting of the test item.

Due to the fact that an exothermic effect was observed in the DSC measurements starting at a temperature of approx. 400 °C with a significant loss of weight, it can be stated that the test item has no melting point and no boiling point up to its decomposition.

Conclusions:
The test item zinc 5-nitroisophthalate has no melting point up to 500 °C at atmospheric pressure (1003.3 hPa), it decomposes at temperatures of approx. 400 °C as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
comparable to guideline study with acceptable restrictions
Reference:
Composition 0
Qualifier:
equivalent or similar to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
yes
Remarks:
chemical identity, accuracy of the method and number of measurements were not stated
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
Differential thermal analysis
Test material information:
Composition 1
Specific details on test material used for the study:
- Sicorin RZ (Standard)
- Sicorin RZ (neue Produktion) (batch no.: 857218 (Sept. 88))
- Sicorin RZ (vor der Mahlung) (Störfallprodukt)
- Sicorin RZ (nach der Mahlung) (verbrannte Ware)
Melting / freezing pt.:
> 350 °C
Decomposition:
no
Sublimation:
no
Remarks on result:
other: no exothermal reaction up to 350 °C
Conclusions:
The test item showed no exothermal reaction up to 350 °C in a differential thermal analysis.

Description of key information

Seitz (2018): The test item zinc 5-nitroisophthalate has no melting point up to 500 °C at atmospheric pressure (1003.3 hPa), it decomposes at temperatures of approx. 400 °C as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Löffler (1988): The test item showed no exothermal reaction up to 350 °C in a differential thermal analysis.

Key value for chemical safety assessment

Additional information