Reaction mass of toluene and 2-vinyl-1,3-dioxolane

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

16 February 2018 - 21 February 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study performed according to OECD 102 guideline and EU method A.1, under GLP, without deviation and with certificate of analysis included.

Cross-reference

Cross-reference 1

Reason / purpose for cross-reference:

reference to other study

Cross-reference 2

Reason / purpose for cross-reference:

reference to same study

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:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

not specified

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

not specified

GLP compliance:

yes (incl. QA statement)

Remarks:

2017-01-10

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

2-vinyl-1,3-dioxolane

EC Number:

223-626-8

EC Name:

2-vinyl-1,3-dioxolane

Cas Number:

3984-22-3

Molecular formula:

C5H8O2

IUPAC Name:

2-vinyl-1,3-dioxolane

Constituent 2

Reference substance name:

Toluene

EC Number:

203-625-9

EC Name:

Toluene

Cas Number:

108-88-3

Molecular formula:

C7H8

IUPAC Name:

toluene

impurity 1

Reference substance name:

Acrylaldehyde

EC Number:

203-453-4

EC Name:

Acrylaldehyde

Cas Number:

107-02-8

Molecular formula:

C3H4O

IUPAC Name:

acrylaldehyde

impurity 2

Reference substance name:

Non identified impurities

Molecular formula:

Not applicable

IUPAC Name:

Non identified impurities

Test material form:

liquid

Details on test material:

Batch No.: 190971
Purity: 95.5% (sum of the two main constituents)
Name of test material (as cited in study report): REACTION MASS OF TOLUENE AND 2-VINYL-1,3-DIOXOLANE
Physical state: colourless liquid
Storage conditions: +2°C to +8°C, under nitrogen and protected from light
Expiry date: 10 April 2018

Results and discussion

Melting / freezing point

Melting / freezing point 1

Melting / freezing pt.:

< -20 °C

Atm. press.:

ca. 975 hPa

Decomposition:

no

Remarks on result:

other: First determination

Remarks:

No melting point was observed from -20.0°C

Melting / freezing point 2

Melting / freezing pt.:

< -20 °C

Atm. press.:

975 hPa

Decomposition:

no

Remarks on result:

other: Second determination

Remarks:

No melting point was observed from -20.0°C

Melting / freezing point 3

Melting / freezing pt.:

< -20 °C

Atm. press.:

975 hPa

Decomposition:

no

Remarks on result:

other: Third determination

Remarks:

No melting point was observed from -20°C

Melting / freezing point 4

Key result

Melting / freezing pt.:

< -20 °C

Atm. press.:

ca. 1 atm

Decomposition:

no

Sublimation:

no

Remarks on result:

other: Final values - Mean of the three determinations

Any other information on results incl. tables

Pre-study:

Peaks assigned to the boiling of the substance were observed and measurement was stopped at 175°C.

Temperature corresponding to these peaks were used to create the following temperature program:

Temperature program:

Step  Initial temperature (°C)  Final temperature (°C)  Heating rate (°C/min)  Duration (min) Furnace atmosphere   Rate* (mL/min)  Liquid nitrogen cooling  1  20  -120  10  14  He  60  Yes  2  -120  -120  0  5  He  60  NO 3   -120  160  10  28  He  60  NO  *Gas injection rate in the furnace. First Determination: Mass taken: 14.96 mg Results: No melting point was observed from -20.0°C. Atmospheric pressure: 975.0 hPa. Second Determination: Mass taken: 11.08 mg Results: No melting point was observed from -20.0°C. Atmospheric pressure: 975.0 hPa. Third Determination: Mass taken: 9.58 mg Results: No melting point was observed from -20.0°C. Atmospheric pressure: 975.0 hPa.

Applicant's summary and conclusion

Conclusions:

According to guideline OECD 102 and method EU A.1, no melting point of substance REACTION MASS OF TOLUENE AND 2-VINYL-1,3-DIOXOLANE was observed from - 20°C.

Executive summary:

A study was performed to determine the melting point/range of test item REACTION MASS OF TOLUENE AND 2-VINYL-1,3-DIOXOLANE.

The method used was Differential Scanning Calorimetry (DSC) and the test was according to Regulation EC No. 440/2008, method A.1 and OECD Test Guideline 102 ''Melting Point/Melting Range''.

In this method, two crucibles were put in the apparatus furnace under inert atmosphere (helium) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied.

The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram.

A cooling system using liquid nitrogen allowed experiments with low temperatures down to -120°C.

Three trials were conducted and corresponding thermograms were obtained, giving us the following results:

 

Trial  Melting point/range  Ambient pressure  1  < -20 °C  975.0 hPa  2  < -20 °C  975.0 hPa  3  < -20 °C  975.0 hPa

The melting point of the Indium respects the checking cards limits (156.5°C for a reference value of 156.6°C) so as its enthalpy (30.7 J/g for a reference value of 28.6 J/g).

The melting point of the substance was determined as < -20.0°C.