Oxacycloheptadecan-2-one

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:

12 December 2015 - 23 May 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

35 °C

Atm. press.:

>= 979 - <= 1 037 hPa

TGA EXPERIMENT (PRELIMINARY TEST)

From 125°C upwards the weight of the sample decreased significantly. At 197°C the sample weight had decreased by 25%. After the experiment it was observed that the test item was evaporated from the sample container.

 

DSC EXPERIMENT 1

An endothermic peak was observed between 0°C and 50°C. The effect was most likely obtained due to melting of the test item. Another endothermic effect was seen between 150°C and 250°C. The endothermic effect is most likely due to boiling of the test item. A third endothermic effect was observed between 250°C and 325°C. No onset temperatures could be calculated from this experiment. After the experiment, it was observed that the test item had evaporated from the sample container.

DSC EXPERIMENTS 2 AND 3

Experiment 2 was performed with a hermetically closed pan. In Experiment 3, a sample pan closed with a lid in which a small hole was drilled (prefabricated) was used. In both experiments, the test item was cooled to -90°C. In both Experiment 2 and Experiment 3, an endothermic peak was observed between 25°C and 75°C. The effect was most likely obtained due to melting of the test item. In Experiment 2, a second endothermic effect was seen between 250°C and 375°C. In Experiment 3, a second endothermic effect was seen between 100°C and 250°C. The difference is caused by the difference in pan used and shows that the effect is due to boiling. In Experiment 3, a third endothermic effect was observed between 275°C and 375°C. No onset temperatures could be calculated from these experiments. After the experiments, it was observed that the test item had evaporated from the sample containers.

DSC EXPERIMENTS 4 AND 5

In Experiment 4 and Experiment 5, the sample was melted prior to loading the sample pan in order to optimise the loading process and reduce the sample mass. The sampling procedure caused a shift of the first endothermic effect to a lower temperature and was therefore not taken into account for further calculation of melting temperature. The second endothermic effect was not affected by the sampling procedure. The extrapolated onset was 270.23°C in Experiment 4 and 267.46°C in Experiment 5. After the experiments, it was observed that the test item had evaporated from the sample containers.

DSC EXPERIMENT 7

A hermetically sealed sample container was used in Experiment 7. The extrapolated onset of the melting peak could not be accurately determined due to a small endothermic effect before the melting peak. The extrapolated onset of the boiling peak was 274.79°C. That no shift to higher temperature was observed as in Experiment 2 is most probably due to the fact that the sample pan had not been completely closed. After the experiment, it was observed that the test item had evaporated from the sample containers.

DSC EXPERIMENTS 8 AND 9

In Experiment 8 and Experiment 9, the temperature program was similar to the program of Experiment 7. The extrapolated onset of the melting peak was 34.95°C (Experiment 8) and 34.53°C (Experiment 9). The extrapolated onset of the boiling peak was 264.54°C in Experiment 8. The extrapolated onset of the boiling peak in Experiment 9 could not be determined accurately. This data was not used for boiling point determination. After the experiment it was observed that the test item had evaporated from the sample container.

The melting temperature was determined as the average obtained from Experiment 8 (34.95°C) and Experiment 9 (34.53°C).

Conclusions:

The melting temperature of the substance was determined to be 35°C.

Executive summary:

Differential Scanning Calorimetry (DSC) experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200.

The melting temperature of the substance was determined in duplicate obtaining a mean value of 35°C.

Description of key information

The melting temperature of the substance was determined to be 35°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

35 °C

Additional information

Determined using Differential Scanning Calorimetry (DSC) experiments in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200.