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Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

from 2018-03-16 to 2018-05-24

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Remarks:

DSC results confirmed by capillary method

Key result

Boiling pt.:

>= 100.1 - <= 101.3 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

In the temperature range of 50 – 140 °C a further endothermic effect occurred (after determination of the melting point). Between 240 and 290 °C one or two small endothermic effects, respectively, as well as one small exothermic could be detected.

Table 1: Results of DSC measurement

No.	Sample weight  (mg)	Onset of effect (°C)	Range of effect (°C)	Atmospheric pressure (hPa)
PN15220	9.26	99.30 267.24	50 – 130 (endo) 250 – 270 (endo) 270 – 300 (exo)	988.7
PN15221	16.33	100.52 243.63 264.70	70 – 130 (endo) 240 – 250 (endo) 250 – 270 (endo) 270 – 280 (exo)	988.7
PN15248	10.17	101.40 245.71 264.21	60 – 140 (endo) 240 – 250 (endo) 250 – 270 (endo) 270 – 300 (exo)	1015.2

During the heating phase three small endothermic effects were observed, which can’t be clearly assigned to a melting of the test item. Thus, the capillary method as well as a test in a test tube were performed for a verification of the DSC measurements.

The test item was filled in a test tube and heated up by means of a lighter. It showed the start of boiling at 86.4 °C. At this temperature, the test item got dark coloured.

For the capillary method, two capillaries were filled with the test item up to a height of 9 mm. The capillaries were heated up from 90 to 130 °C with a constant heating rate of 1 K/min in the BÜCHI melting point apparatus. The test item was visually observed while increasing the temperature. The boiling of the test item could be observed at 99.1 and 99.0 °C at a pressure of 991 hPa.

The endothermic effect in the DSC in the temperature range of 50 to 140 °C was determined as boiling point of the test item under decomposition. For the correction of the boiling temperature to normal pressure the test item was assigned to chemical group 3 (e.g. Ester). According to appendix 8.1 a correction value φ = 4.95 was used for a temperature of 90 – 100 °C. The lowest measured onset temperature corrected to the normal pressure was 100.10 °C and the highest onset temperature was 101.34 °C. The corrected boiling point temperatures differed more than 0.5 °C from the mean value of 100.92 °C. The boiling range of the test item under decomposition was determined to be 100 to 101 °C at 1013 hPa.

Conclusions:

The boiling range of the test item under decomposition was determined to be 100.1 to 101.3 °C at 1013 hPa.

Executive summary:

A study was conducted according to OECD test guideline 103, Regulation (EC) No 440/2008 method A.2 and EPA OCSPP test guideline 830.7220 to determine the boiling point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Three tests were performed. As reference crucible, an empty aluminium crucible was used. When heating up during DSC measurement three endothermic and one exothermic effect were observed and the boiling point of the test item could not clearly be assigned. Thus, the results of the DSC method were confirmed by a test in a test cube and the measurement with the capillary method. Finally and after correction of the temperatures to normal pressure the boiling range of the test item under decomposition was determined to be 100.1 °C to 101.3 °C (lowest and highest onset temperature) at 1013 hPa.

Description of key information

The boiling range of the test item under decomposition was determined to be 100.1 to 101.3 °C at 1013 hPa.

Additional information

A study was conducted according to OECD test guideline 103, Regulation (EC) No 440/2008 method A.2 and EPA OCSPP test guideline 830.7220 to determine the boiling point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Three tests were performed. As reference crucible, an empty aluminium crucible was used. When heating up during DSC measurement three endothermic and one exothermic effect were observed and the boiling point of the test item could not clearly be assigned. Thus, the results of the DSC method were confirmed by a test in a test cube and the measurement with the capillary method. Finally and after correction of the temperatures to normal pressure the boiling range of the test item under decomposition was determined to be 100.1 °C to 101.3 °C (lowest and highest onset temperature) at 1013 hPa.