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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:
Feb-May 2013
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: A modern study conducted in compliance with GLP standards and followed OECD Guidelines
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling point/boiling range)
Deviations:
no
GLP compliance:
yes
Type of method:
method according to Siwoloboff
Specific details on test material used for the study:
Identifier: EXP1200078
Appearance: Very dark brown (almost black) viscous liquid
Batch: E00275-350
Sample Expiration Date: end-2013
Purity:100%
Key result
Boiling pt.:
> 178.3 - <= 400 °C
Atm. press.:
ca. 760 mm Hg
Decomposition:
ambiguous
Remarks:
Color change observed
Decomp. temp.:
ca. 300 °C
Remarks on result:
other: Boiling point not achieved; limitation of test instrumentation upper bound.

Determination of Melting Points for the Reference Standards

 

 

Reference Standard

Instrument Gradient

(°C/min.)

Date Verification Performed

Recorded Melting Point

(°C)

 

Average

Expected Melting Point/Range

(°C)

 

Caffeine

 

 

1.0

 

2/26/13

 

 

237.0

 

--

 

237

 

 

Anthraquinone

 

 

1.0

 

2/26/13

 

2/27/13

 

 

285.3

 

285.1

 

 

285.2

 

 

 

284-286

 

 

 

Benzophenone

 

 

1.0

 

2/26/13

 

2/27/13

 

 

49.5

 

49.3

 

 

49.4

 

 

 

49-51

 

 

 

Note: All calculations were performed using Microsoft®Excel 2000 in full precision mode.

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Determination of Boiling Point/Range for the Test Substance

 

 

Subsample
ID

Instrument
Gradient
(°C/min)

Barometric
Pressure
(mm Hg)

Start of

Boiling Range

 °C (K)1

End of Boiling Range
°C (K)1

Boiling
Point
°C (K)1

 

523C-189-BP-1

 

523C-189- BP-2

 

523C-189- BP-3

 

 

1.0

 

1.0

 

1.0

 

 

748

 

748

 

750

 

 

178.3 (451.5)

181.0 (454.2)

184.1 (457.3)

 

 

None Observed

None Observed

None Observed

 

 

None Observed

None Observed

None Observed

 

Overall Means:

Standard Deviations:

CV (%):

749

1

0.1

181.1 (454.3)

2.9 (2.9)

1.60 (0.64)

n/a

n/a

n/a

n/a

n/a

n/a

1K (Kelvin) = °C + 273.15   Note: All calculations were performed using Microsoft®Excel 2000 in full precision mode. Additionally, “n/a” denotes “not applicable”.

Conclusions:
The boiling point was determined using a modification of the Siwoloboff procedure which employed a Büchi Melting Point B-540 instrument with boiling point tubes and boiling point capillaries, also supplied by Büchi.

EXP1200078 thermally degraded as the instrument block temperature approached 350°C. No boiling point / range could be determined.
Executive summary:

The test substance thermally degraded as the instrument block temperature approached 350°C. No boiling point / range could be determined.

Description of key information

A Key GLP study conducted in accordance with OECD guideline.

The test substance thermally degraded as the instrument block temperature approached 350°C. No boiling point / range could be determined.

Key value for chemical safety assessment

Additional information

Boiling point > 178.3 which was the temperature at which capillary bubbling was first observed. The sample degraded with further temperature increase.