6-hexyltetrahydro-2H-pyran-2-one

Melting point / freezing point

Administrative data

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

Cross-reference

Reason / purpose for cross-reference:

reference to same study

Reference

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

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

2016

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Version / remarks:

1996

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

306.2 °C

Atm. press.:

>= 1 013 - <= 1 015 hPa

Remarks on result:

other: mean of 2 measurements

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

DSC EXPERIMENT 1

During cooling, an exothermic peak between -30°C and -40°C was found (due to crystallization of the test item). During heating, two endothermic peaks and an exothermic peak were observed between -25°C and 25°C followed by an endothermic peak between 275°C and 325°C. The effects between -40°C and 25°C were ascribed to melting, re-crystallisation and melting of the substance (see endpoint 4.2). A third endothermic effect with an extrapolated onset temperature of 306.240°C was observed, probably 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 endothermic peak between 275°C and 325°C, a higher heating rate of 50°C/minute was used in Experiment 2. The extrapolated onset temperature of the observed endothermic effect was 306.549°C. Since the endothermic peak had not shifted to higher temperature, this test 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. Since a higher heating rate was used, the extrapolated onset temperature was not used in the calculation of the boiling point. 

 

DSC EXPERIMENT 3

Experiment 3 was performed as a duplicate of Experiment 1. Similar results as in Experiment 1 were obtained. The extrapolated onset temperature of the boiling peak was 306.206°C. 

 

DATA HANDLING

The boiling temperature was determined as the mean extrapolated onset temperature of the third endothermic effect measured in Experiment 1 (306.240°C) and Experiment 3 (306.206°C).

Conclusions:

The boiling temperature of the substance was determined to be 306.2°C (at 1014 ± 1 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 duplicate experiments, the boiling temperature was determined to be 306.2°C (at 1014 ± 1 hPa).

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Test guideline 3

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

Test material

Test material information

Constituent 1

Reference substance name:

6-hexyltetrahydro-2H-pyran-2-one

EC Number:

211-915-1

EC Name:

6-hexyltetrahydro-2H-pyran-2-one

Cas Number:

710-04-3

Molecular formula:

C11H20O2

IUPAC Name:

6-hexyltetrahydro-2H-pyran-2-one

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

Melting / freezing point

Key result

Melting / freezing pt.:

1.7 °C

Atm. press.:

>= 1 013 - <= 1 015 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 -30°C and -40°C was found (due to crystallization of the test item). During heating, two endothermic peaks and an exothermic peak were observed between -25°C and 25°C followed by an endothermic peak between 275°C and 325°C. The effects between -25°C and 25°C were most likely obtained due to melting, followed by re-crystallisation and melting of the test item. The peak maximum of the second endothermic peak was 1.596°C. A third endothermic effect observed between 275°C and 310°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 peak maximum of the second melting peak was 1.732°C.  

STORAGE EXPERIMENT IN FREEZER

Two subsamples of the test item were placed overnight in a ≤ ‑15°C freezer and a ≤ -75°C freezer. It was observed after overnight storage that the test item was a liquid (≤ ‑15°C freezer; actual temperature -18.7 ± 0.3°C) and a solid (≤ -75°C freezer; actual temperature -83.3 ± 1.7°C). The subsample that had been stored in the ≤ -75°C freezer was transferred into the ≤ -15°C freezer. After three days of storage at an actual temperature of -18.8 ± 0.2°C, the test item was still a solid. Based on this, the second endothermic peak observed in Experiment 1 and Experiment 3 was reported as the melting point.

DATA HANDLING

The mean of the second melting peak of Experiment 1 (peak maximum temperature: 1.596°C) and Experiment 3 (peak maximum temperature: 1.732°C) was reported as the melting temperature.

 

Applicant's summary and conclusion

Conclusions:

The melting temperature of the substance was determined to be 1.7°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.

During heating, an endothermic peak, an exothermic peak and again an endothermic peak were observed between -25°C and 25°C. These effects were most likely obtained due to melting, followed by re-crystallisation and melting of the test item. The peak maximum of the second endothermic peak was used for the determination of the melting temperature of the substance.

The melting temperature of the substance was determined in duplicate obtaining a mean value of 1.7°C.