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

Boiling point

Administrative data

Endpoint:

boiling 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:

guideline study

Remarks:

Study performed according to OECD 103 guideline and EU method A.2, under GLP, without deviation and with certificate of analysis included

Cross-reference

Cross-reference 1

Reason / purpose for cross-reference:

reference to same study

Cross-reference 2

Reason / purpose for cross-reference:

reference to other 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 103 (Boiling Point)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

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

Boiling point

Boiling point 1

Boiling pt.:

ca. 114.2 °C

Atm. press.:

ca. 975 hPa

Decomposition:

no

Remarks on result:

other: First determination

Boiling point 2

Boiling pt.:

ca. 111.1 °C

Atm. press.:

ca. 975 hPa

Decomposition:

no

Remarks on result:

other: Second determination

Boiling point 3

Boiling pt.:

ca. 111 °C

Atm. press.:

ca. 975 hPa

Decomposition:

no

Remarks on result:

other: Third determination

Boiling point 4

Key result

Boiling pt.:

ca. 112.3 °C

Atm. press.:

ca. 101.3 kPa

Remarks on result:

other: Corrected value with the Sydney Young equation (mean of 112.4°C for the second determination and 112.3°C for the third determination).

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.

Temperatures 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:

Initial boiling point is observed at 114.2°C (onset temperature of the first peak) and a corresponding mass loss is observed on the TG curve, showing that all the substance was evaporated at the end of the study.

The crucible was visually checked after the determination: by opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Atmospheric pressure: 975.0 hPa

Second Determination: 

Mass taken: 11.08 mg

Results:

Initial boiling point is observed at 111.1°C (onset temperature of the first peak) and a corresponding mass loss is observed on the TG curve, showing that all the substance was evaporated at the end of the study. 

The crucible was visually checked after the determination: by opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Atmospheric pressure: 975.0 hPa

Third Determination:

Mass taken: 9.58 mg

Results:

Initial boiling point is observed at 111.0°C(onset temperature of the first peak) and a corresponding mass loss is observed on the TG curve, showing that all the substance was evaporated at the end of the study. 

The crucible was visually checked after the determination: by opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Atmospheric pressure: 975.0 hPa

Applicant's summary and conclusion

Conclusions:

According to guideline OECD 103 and method EU A.2, the initial boiling point of substance REACTION MASS OF TOLUENE AND 2-VINYL-1,3-DIOXOLANE was determined as 112.3°C at 101.3 kPa after correction using the Sydney Young equation (mean of 112.4°C for the second determination and 112.3°C for the third determination).

Executive summary:

A study was performed to determine the boiling point 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.2. and OECD Test Guideline 103, "Boiling Point" (1995)

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	Initial boiling point*	Ambient pressure
1	114.2 °C	975.0 hPa
2	111.1 °C	975.0 hPa
3	111.0 °C	975.0 hPa

*: without Sydney-Young correction

The initial boiling point values of trials 2 and 3 respect validity criteria (less than 0.5°C of difference up to 326.85°C).

After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 112.3 °C at 101.3 kPa (mean of 112.4 °C for the second determination and 112.3 °C for the third determination).