6-butyltetrahydro-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

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

>= 271.2 - <= 274.9 °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. 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.

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).

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-butyltetrahydro-2H-pyran-2-one

EC Number:

221-974-5

EC Name:

6-butyltetrahydro-2H-pyran-2-one

Cas Number:

3301-94-8

Molecular formula:

C9H16O2

IUPAC Name:

6-butyloxan-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.:

-28.8 °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 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).

Applicant's summary and conclusion

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.