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Boiling point

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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.  

Key value for chemical safety assessment

Additional information