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Administrative data

Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2014

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry

Test material

Constituent 1
Chemical structure
Reference substance name:
3,3',5,5'-tetramethylbiphenyl-2,2'-diol
EC Number:
607-957-9
Cas Number:
26567-10-2
Molecular formula:
C16 H18 O2
IUPAC Name:
3,3',5,5'-tetramethylbiphenyl-2,2'-diol

Results and discussion

Boiling point
Boiling pt.:
> 341 °C
Atm. press.:
1 013 hPa
Decomposition:
yes
Decomp. temp.:
>= 341 °C
Remarks on result:
other: The decomposition takes place under air atmosphere.

Any other information on results incl. tables

The boiling point was tried to be determined by differential scanning calorimetry (DSC). A visual determination using a Büchi melting point apparatus was also applied. In the preliminary DSC screening an endothermic boiling peak was detected in a temperature range of 370°C to 390°C.

The DSC test was performed with a heat flux differential scanning calorimeter.

Parameters Test 1 / Pre-Test Test 2 Test 3

System

DSC 821

DSC 821

DSC 821

Start Temp. [°C]

320 

320 

320 

Rate (heating 1) [K/min]

10 

10

10

End Temp. [°C]

420 

420

420

Crucible type

aluminium, high

aluminium, high

aluminium, high

Open / Sealed

open (perforated)

open (perforated)

open (perforated

Test atmosphere

air

air

air

Air pressure

ambient

 ambient

ambient

Amount [mg]

12.96

19.80

30.82

Mass loss [mg] / [%]    

12.07 / 93

18.50 / 93

28.86 / 94

 

The solid test item was weighed into an aluminium crucible and was measured against a sealed reference aluminium crucible filled with 12.89 mg aluminium oxide. The sample crucible was sealed with a perforated lid at ambient atmosphere (air) and then the test program was started. For the visual test using the Büchi melting point tester a small amount of the solid test item was filled into a melting point capillary and measured directly.

The measured boiling points of the test item show a very high standard deviation. In addition to this the thermograms of the test item are irreproducible, some of them with shoulders at the side of the boiling peak. Due to these observations a visual test using a Büchi melting point tester was performed. In the Büchi apparatus a capillary containing the test item was heated from 300°C to 375°C at a heating rate of 2 K/min. The test item directly melted on inserting the capillary into the apparatus. With heating formation of bubbles in the test item was observed (beginning boiling process) accompanied by a change of the colour of the test item from beige to black. As the mass loss shows, almost the total amount of the test item is evaporated from the aluminium crucible in this process.

Result:

The boiling point of the test item could not be determined. The boiling process was accompanied by thermal decomposition starting at a minimum temperature of 341°C.

   

Applicant's summary and conclusion

Conclusions:
The boiling point of the test item could not be determined. The boiling process was accompanied by thermal decomposition starting at a minimum
temperature of 341°C.

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