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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:
2018-02-09 to 2018-09-11
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to
Guideline:
other: Thermal Stability (OECD 113)
Version / remarks:
1981
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
signed 2017-02-28
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage conditions: Room temperature tightly closed
Decomposition:
yes
Decomp. temp.:
> 215 °C

Melting and Boiling Point (DSC)

In the DSC run PN16300 four endothermic effects were observed in the temperature ranges of approx. -30 to 0 °C, 60 °C – 110 °C, 200 °C – 270 °C and 480 °C – 560 °C. In the DSC run PN16335 two endothermic effects were detected in the temperature ranges of approx. -30 °C to 10 °C and 180 °C – 270 °C.

Results of the DSC-measurements

No.

Sample weight

[mg]

Onset of Effect

[°C]

Range of effect

[°C]

Weight loss

[mg]

Atmospheric pressure

[hPa]

PN16300 15.71

-26.90

68.41

209.34

483.14

-30 to 0 (endo)

60 – 110 (endo)

200 – 270 (endo)

480 – 560 (endo)

13.17

84 %

1002.8
PN16335 24.79

-24.14

214.73

-30 to 10 (endo)

180 – 270 (endo)

13.01

88 %

1010.7

During the cooling phase, no thermal effects were observed, which can be assigned to the freezing of the test item.

In view of the fact that the measured weight loss of each sample was only between 84 % and 88 % of the respective initial sample weight, the observed endothermic effects cannot be definitely assigned to the boiling of fatty acids, C9-C13-neo, copper salts.

Measurements by the Test Tube

Due to the fact that only a very small endothermic peak at approx. -20 °C in the DSC was observed, the melting of the test item was verified in a test tube. In the temperature range of -30 to approx. -15 °C the test item was solid. The appearance of the test item during warming up was from approx. -5 °C to ambient temperature very pasty. The test item shows a softening in the temperature range of approx. -15°C to -5 °C, but remained pasty.

Measurements by the Capillary Method

For verification of the results the test item was additionally tested with the capillary method. At approx. 60 °C the test item became more viscous. In the temperature range of 95 °C to 120 °C the evolution of separate gas bubbles were observed. Above 182 °C faster bubbles occurred. In the temperature range of 215 °C to 220 °C continuous fast bubbles combined with changing of the colour to black were observed. The test item changed the colour from black to brown at approx. 235 °C and slowly bubbles were observed. In the temperature range from 240 °C to 245 °C the test item was orange and turbid, like a suspension. From 260 °C to 300 °C the test item was partly red/brown/turbid/solid and partly liquid. The visual inspection of the measurement showed a boiling (215 °C to 220 °C), accompanied by the release of volatile decomposition products of the test item in the temperature range of the endothermic effect detected in the DSC.

Thermal Stability (DSC)

The test item fatty acids, C9-C13-neo, copper salts showed two endothermic effects in the temperature range of 200 °C - 230 °C and 240 °C - 290 °C, respectively. No exothermic effect was observed until the maximum test temperature of 600 °C. A pressure rise at approx. 330 °C was observed.

Results of the DSC-measurements

No. Sample weight [mg] Start of effect [°C] Energy  [J/g]
PN14651 6.33

200 (endothermic)

240 (endothermic)

+50

+30

PN14652 7.11

200 (endothermic)

240 (endothermic)

+50

+40

Conclusions:
Melting and Boiling Point
No definitive signs of melting of the test item fatty acids, C9-C13-neo, copper salts were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, from -90 °C up to 600 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995) at atmospheric pressure (1003 – 1011 hPa).
In a test tube the test item shows a softening in the temperature range of approx. -15 °C to -5 °C at atmospheric pressure (1010 hPa).
No definitive signs of boiling of the test item fatty acids, C9-C13-neo, copper salts were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 300 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.2. and OECD Test Guideline 103 (1995) at atmospheric pressure (1003 – 1011 hPa). It is assumed that the test item boiled under decomposition at temperatures >215 °C.

Thermal Stability
In DSC measurements (closed glass crucible under air, from room temperature up to 600 °C, heating rate of 3 K/min) according to OECD guideline 113 (1981) the test item fatty acids, C9-C13-neo, copper salts showed two endothermic effects in the temperature range of 200 °C – 230 °C and 240 °C – 290 °C, respectively, and no exothermic effects until the maximum test temperature of 600 °C. Only a pressure rise starting at approx. 330 °C was observed.

Description of key information

Fatty acids, C9-C13-neo, copper salts has no defined melting and boiling point. It boiled under decomposition at temperatures >215 °C.

Key value for chemical safety assessment

Additional information

Melting and Boiling Point

No definitive signs of melting of the test item fatty acids, C9-C13-neo, copper salts were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, from -90 °C up to 600 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995) at atmospheric pressure (1003 – 1011 hPa).

In a test tube the test item shows a softening in the temperature range of approx. -15 °C to -5 °C at atmospheric pressure (1010 hPa).

No definitive signs of boiling of the test item fatty acids, C9-C13-neo, copper salts were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 300 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.2. and OECD Test Guideline 103 (1995) at atmospheric pressure (1003 – 1011 hPa). It is assumed that the test item boiled under decomposition at temperatures >215 °C.

Thermal Stability

In DSC measurements (closed glass crucible under air, from room temperature up to 600 °C, heating rate of 3 K/min) according to OECD guideline 113 (1981) the test item fatty acids, C9-C13-neo, copper salts showed two endothermic effects in the temperature range of 200 °C – 230 °C and 240 °C – 290 °C, respectively, and no exothermic effects until the maximum test temperature of 600 °C. Only a pressure rise starting at approx. 330 °C was observed.