Registration Dossier

Administrative data

Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
from 20 March 2018 to 24 April 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Cross-reference
Reason / purpose:
reference to same study
Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
from 20 March 2018 to 24 April 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2016
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
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.:
-28.8 °C
Atm. press.:
>= 996.6 - <= 1 000 hPa
Remarks on result:
other: mean of 2 measurements

Four experiments were performed to investigate the melting and boiling behaviour of the substance.

DSC EXPERIMENT 1

During cooling, an exothermic peak between -90°C and -50°C was found (due to crystallization of the test item). During heating, an exothermic peak was observed between -75°C and -50°C. The exothermic effect was due to (re)crystallization of the test item. An endothermic (melting) peak was observed between -50°C and 0°C (extrapolated onset temperature: -28.701°C).  A second endothermic peak was observed between 200°C and 300°C and ascribed to boiling (see endpoint 4.3.

DSC EXPERIMENT 2

Investigation of the presumed boiling peak, see endpoint 4.3.

DSC EXPERIMENT 3

Experiment 3 was performed as a duplicate of Experiment 1. Similar results as in Experiment 1 were obtained. The extrapolated onset of the melting peak was -28.812°C. 

DSC EXPERIMENT 4

Investigation of the difference in boiling temperatures (observed in Experiment 1 and Experiment 3), see endpoint 4.3. 

DATA HANDLING

The melting temperature was determined as the mean extrapolated onset temperature of Experiment 1 (-28.701°C) and Experiment 3 (-28.812°C).

Conclusions:
The melting temperature of the substance was determined to be -28.8°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 -28.8°C.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
EU Method A.2 (Boiling Temperature)
Version / remarks:
2016
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7220 (Boiling Point / Boiling Range)
Version / remarks:
1996
Deviations:
no
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid
Details on test material:
Appearance: Clear colourless to pale yellow liquid
Test item storage: In refrigerator (2-8°C)

Results and discussion

Boiling point
Key result
Boiling pt.:
>= 271.2 - <= 274.9 °C
Atm. press.:
>= 996.6 - <= 1 000 hPa
Remarks on result:
other: mean of 2 measurements

Any other information on results incl. tables

Four experiments were performed to investigate the melting and boiling behaviour of the substance.

DSC EXPERIMENT 1

During cooling, an exothermic peak between -90°C and -50°C was found (due to crystallization of the test item). During heating, an exothermic peak was observed between -75°C and -50°C. The exothermic effect was due to (re)crystallization of the test item. An endothermic (melting) peak was observed between -50°C and 0°C (extrapolated onset temperature: -28.701°C).  A second endothermic peak was observed between 200°C and 300°C. The extrapolated onset temperature of the peak was 274.929°C. This endothermic effect was most likely caused by boiling of the test item. After the experiment it was observed that the test item had evaporated from the sample container.

DSC EXPERIMENT 2

In order to investigate the boiling peak, a higher heating rate of 50°C/minute was used in the Experiment 2. The extrapolated onset temperature was 275.858°C. The endothermic peak had not shifted to higher temperatures. It demonstrated that boiling of the test item caused the endothermic effect. After the experiment it was observed that the test item had evaporated from the sample container. The extrapolated onset temperature was not used for calculation of the boiling temperature since it was obtained with a higher heating rate.

DSC EXPERIMENT 3

Experiment 3 was performed as a duplicate of Experiment 1. Similar results as in Experiment 1 were obtained. The extrapolated onset of the boiling peak was 271.207°C. 

DSC EXPERIMENT 4

Since a difference in boiling temperatures was observed between Experiment 1 and Experiment 3, Experiment 4 was performed.  The extrapolated onset of the boiling peak was 273.049°C. 

DATA HANDLING

No reason was found for the different boiling temperatures measured during Experiment 1 (274.929°C), Experiment 3 (271.207°C) and Experiment 4 (273.049°C). Therefore, a boiling range was given instead of a boiling temperature.

Applicant's summary and conclusion

Conclusions:
The boiling range of the substance was determined to be 271.2 – 274.9°C (at 998.3 ± 1.7 hPa).
Executive summary:

The boiling temperature of the substance was determined using Differential Scanning Calorimetry in a GLP study according to EC A.2, OECD 103 and OPPTS 830.7220.

From three experiments, a boiling range of the substance was determined to be 271.2 – 274.9°C (at 998.3 ± 1.7 hPa).