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Administrative data

Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-02-20 to 2017-04-28
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:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-02-20 to 2017-04-28
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted 27 July 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
30 May, 2008
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Remarks:
and thermogravimetric measurement
Key result
Melting / freezing pt.:
> 48 - <= 86 °C
Atm. press.:
1 013 Pa
Decomposition:
yes
Decomp. temp.:
> 298 °C
Remarks on result:
not determinable
Remarks:
Substance is considered to undergo solid/solid transition or at least partial melting before decomposition

In a preliminary thermogravimetric measurement performed over a temperature range from room temperature to approx. 600 °C two steps were registered with maxima at 266 °C resp. 397 °C. A total mass loss of 99.9 % at the final temperature could be observed (mass change in the range from 20- 285 °C: 91.9 %; mass change in the range from 285 to 600 °C: 8.0 %). No significant mass loss occurred due to purging.The DSC measurements were performed twice in the temperature range from 20 - 500 °C.

First two endothermic peaks without corresponding mass loss could be observed (peak maxima: 49 °C/86 °C [first run] resp. 48 °C/85 °C [second run]).

This may be due to solid/solid-conversion with subsequent melting or due to partial melting. But no clear melting point could be detected. Upon further heating the DSC-curve showed one endothermic peak (peak maximum: 299 °C [first run] resp. 298 °C [second run]; onset temp. 293 °C resp. 292 °C). The shape of the peak as well as the missing complete mass loss (see thermogravimetry) indicates that the test item does not have a clear boiling point. Probably the peak is due to boiling of the main component with simultaneously decomposition.

The following course of the curve with a maximum at 387 °C could not be interpreted.

Conclusions:
The present GLP-study according to OECD test guideline 102/103 was conducted in order to determine the melting point of 1,4-Dioxane-2,5-dione using differential scanning calorimetry. In a preliminary test the test item was heated under controlled conditions up to 600°C. The registered maxima were detected at 266 °C and 397°C. The SC measurements were performed in the temperature range of 20 - 500°C. In sum four peaks each were detected during two independent runs. The first two peaks were detected at appr. 48°C and 85°C (without mass lost) and the second two peaks were detected at 298°C and 387°C, respectively. At the lower temperatures a solid/solid conversion or partial melting was assumed to be the reason for the occurrence of the two peaks. The shape of the second peak at 298°C and the missing complete mass lost were considered indicative for boiling of the main component with simultaneously decomposition. The third peak could not be interpreted.
Thus, 1,4-Dioxane-2,5-dione has no melting or boiling point due to solid/solid conversions and decomposition.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
adopted 27 July, 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Version / remarks:
30 May, 2008
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Remarks:
and thermogravimetric measurement

Test material

Constituent 1
Chemical structure
Reference substance name:
1,4-dioxane-2,5-dione
EC Number:
207-954-9
EC Name:
1,4-dioxane-2,5-dione
Cas Number:
502-97-6
Molecular formula:
C4H4O4
IUPAC Name:
1,4-dioxane-2,5-dione
Test material form:
solid: particulate/powder

Results and discussion

Boiling point
Key result
Atm. press.:
1 013 Pa
Decomposition:
yes
Decomp. temp.:
> 298 °C
Remarks on result:
other: Decomposition occurred at 298°C but a second peak was detected at 387°C resulting in the missing 8% mass loss. This peak cannot be interpreted.

Any other information on results incl. tables

In a preliminary thermogravimetric measurement performed over a temperature range from room temperature to approx. 600 °C two steps were registered with maxima at 266 °C resp. 397 °C. A total mass loss of 99.9 % at the final temperature could be observed (mass change in the range from 20- 285 °C: 91.9 %; mass change in the range from 285 to 600 °C: 8.0 %). No significant mass loss occurred due to purging.The DSC measurements were performed twice in the temperature range from 20 - 500 °C.

First two endothermic peaks without corresponding mass loss could be observed (peak maxima: 49 °C/86 °C [first run] resp. 48 °C/85 °C [second run]).

But no clear melting point could be detected. Upon further heating the DSC-curve showed one endothermic peak (peak maximum: 299 °C [first run] resp. 298 °C [second run]; onset temp. 293 °C resp. 292 °C). The shape of the peak as well as the missing complete mass loss (see thermogravimetry) indicates that the test item does not have a clear boiling point. Probably the peak is due to boiling of the main component with simultaneous decomposition.

The following course of the curve with a maximum at 387 °C could not be interpreted.

Applicant's summary and conclusion

Conclusions:
The present GLP-study according to OECD test guideline 102/103 was conducted in order to determine the boiling point of 1,4-Dioxane-2,5-dione using differential scanning calorimetry. In a preliminary test the test item was heated under controlled conditions up to 600°C. The registered maxima were detected at 266 °C and 397°C. The DSC measurements were performed in the temperature range of 20 - 500°C. In sum four peaks each were detected during two independent runs. The first two peaks were detected at appr. 48°C and 85°C (without mass lost) and the second two peaks were detected at 298°C and 387°C, respectively. At the lower temperatures a solid/solid conversion or partial melting was assumed to be the reason for the occurrence of the two peaks. The shape of the second peak at 298°C and the missing complete mass lost were considered indicative for boiling of the main component with simultaneously decomposition. The third peak could not be interpreted.
Thus, 1,4-Dioxane-2,5-dione has no melting or boiling point due to solid/solid conversions and decomposition.