Tosyl chloride

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

November 2011- April 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Well conducted study, according to EU and OECD guidelines, certificate of analysis included in the report.

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Version / remarks:

Section 23: Differential scanning calorimetry (DSC) 27th July 1995

Deviations:

not specified

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

1.4.7 Differential scanning calorimetry (DSC)

Deviations:

not specified

Principles of method if other than guideline:

Extra information was generated from Simultaneous Thermo Gravimetric Analysis (TGA) - Differential Scanning Calorimetry. Thermo Graphical Analysis (TGA) because  this gives information on weight loss.
Distillation, NMR(Nuclear Magnetic Resonance) and FTIR ( Fourier Transform Infrared) to prove degradation.
 

GLP compliance:

no

Type of method:

differential scanning calorimetry

Key result

Decomposition:

yes

Decomp. temp.:

> 160 °C

Result TGA-DSC scans of the sample.

 

TGA: A decrease in weight starts at 90.5°C.

A second scan is made by heating to 150°C and cooling to 25°C. The material is inspected and found to be white after analysis; it was white before, so no evidence of degradation.

Evaporation is starting at 90.5°C. The weight loss is starting at 160°C.

 Result distillation.

 

Time minutes	Temperature ^0C	Observation
35	160	Colourless fluid
55	190	Light brown fluid, nothing has been gathered in the subboiled retort
60	195	Still nothing in the subboiled retort
90	211	Still nothing in the subboiled retort, the fluid is dark brown No vapour bubbles in the fluid. Heating is stopped
After cooling down		Beige and brown crystals

 

Conclusion: No boiling, but degradation.

 

 ResultsFTIR and NMR.

 

The sample which is expected to be a degradation product of para Toluene Sulpho Chloride is measured as such with FTIR and NMR. These measurements are compared to a reference.

With FTIR no significant differences can be observed between the delivered sample and a reference. With¹H-NMR some small amounts of impurities and degradation products can be observed.

The main component however still seems to be para-Toluene Sulpho Chloride.

Conclusions:

The decomposition of Para-Toluene Sulfo Chloride starts at 160°C.

Description of key information

The decomposition of Para-Toluene Sulfo Chloride starts at 160°C before boiling.