[No public or meaningful name is available]

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

04 December 2020 - 19 February 2021

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Well documented study performed according to OECD 103 guideline and EU method A.2, under GLP and without deviation

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to other 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

GLP compliance:

yes (incl. QA statement)

Remarks:

2018-11-15

Type of method:

differential scanning calorimetry

Boiling pt.:

290 °C

Atm. press.:

101.3 kPa

Remarks on result:

other: First determination - Corrected value following Sydney-Young equation

Boiling pt.:

288.3 °C

Atm. press.:

101.3 kPa

Remarks on result:

other: Second determination - Corrected value following Sydney-Young equation

Boiling pt.:

290.4 °C

Atm. press.:

101.3 kPa

Remarks on result:

other: Third determination - Corrected value following Sydney-Young equation

Boiling pt.:

288.7 °C

Atm. press.:

98.5 kPa

Decomposition:

no

Remarks on result:

other: First determination

Boiling pt.:

287 °C

Atm. press.:

98.5 kPa

Decomposition:

no

Remarks on result:

other: Second determination

Boiling pt.:

289.1 °C

Atm. press.:

98.6 kPa

Decomposition:

no

Remarks on result:

other: Third determination

Boiling pt.:

ca. 290.2 °C

Atm. press.:

ca. 101.3 kPa

Remarks on result:

other: Corrected value with the Sydney Young equation (mean of the first and third determination)

Pre-study:

Peaks assigned to the boiling of the substance was observed and measurement was stopped at 340°C (Figure 1).

The initial boiling point of the substance was observed at 285.7°C.
A corresponding mass loss was observed between the beginning and the end of the boiling peak.
Temperatures corresponding to these peaks were used to create the following temperature program:

 

Temperature program:

Step	Initial temperature (°C)	Final Temperature (°C)	Heating rate (°C/min)	Duration (min)	Furnace atmosphere	Rate* (mL/min)	Liquid nitrogen cooling
1	20	-120	-10	14	He	60	YES
2	-120	-120	0	10	He	60	YES
3	-120	350	10	47	He	60	NO

*Gas injection rate in the furnace. 

 

First Determination: 

Mass taken: 13.81 mg

Temperature calibration file: CAN03-Al-He-10K-04

Sensitivity calibration file: CAN03-Al-He-10K-04

File name: DSC 20-036 01
The thermogram of the first determination is shown in Figure 2.

Results: Initial boiling point was observed at 288.7°C (onset temperature of the peak) and a mass loss of 13.743 mg (99.5%) was observed between the beginning and the end of the boiling peak.
The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 98.5 kPa.

 

Second Determination:

Mass taken: 13.05 mg

Temperature calibration file: CAN03-Al-He-10K-04
Sensitivity calibration file: CAN03-Al-He-10K-04
File name: DSC 20-036 02
The thermogram of the second determination is shown in Figure 3:

Results: Initial boiling point was observed at 287.0°C (onset temperature of the peak) and a mass loss of 12.811 mg (98.2%) was observed between the beginning and the end of the boiling peak.
The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
As the boiling point values of determinations 1 and 2 did not respect validity criteria (no more than 0.5°C of difference up to 326.85°C), a third determination was performed.
Atmospheric pressure: 98.5 kPa.

 

Third Determination: 

Mass taken: 13.74 mg

Temperature calibration file: CAN03-Al-He-10K-04
Sensitivity calibration file: CAN03-Al-He-10K-04
File name: DSC 20-036 03
The thermogram of the third determination is shown in Figure 4:

Results: Initial boiling point was observed at 289.1°C (onset temperature of the peak) and a mass loss of 13.737 mg (100.0%) was observed between the beginning and the end of the boiling peak.
The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.
Atmospheric pressure: 98.6 kPa.

 

Sydney-Young Correction: 

In case of small pressure deviations the boiling temperature at standard pressure can be calculated following the equation of Sydney-Young:
Tn = T + (ƒ x Δp)
With
Tn = boiling point at 101.325 kPa in K
T = measured boiling point in K
ƒ = correction factor (tabulated value)
Δp = (101.325 – p) kPa
P = measured atmospheric pressure in kPa
Correction factor is obtained by regressing the values from the following table:

 

Temperature	ƒT (K/kPa)
323.15	0.26
348.15	0.28
373.15	0.31
398.15	0.33
423.15	0.35
448.15	0.37
473.15	0.39
498.15	0.41
523.15	0.44
548.15	0.45
573.15	0.47

The corrected values at 101.3 kPa following Sydney-Young equation were determined to be 290.0°C for the first determination, 288.3°C for the second determination and 290.4°C for the third determination.

Conclusions:

After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 290.2°C at 101.3 kPa (mean of 290.0°C for the first determination and 290.4°C for the third determination).

Executive summary:

A study was performed to determine the boiling point of the test item using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.2. and OECD Test Guideline No. 103, "Boiling Point" (1995).

In this method, two crucibles, with pierced lid, were put in the apparatus furnace under inert atmosphere (helium) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied.
The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram.
A cooling system using liquid nitrogen allowed experiments with low temperatures down to -120°C.

 

Three trials were conducted and corresponding thermograms were obtained, giving us the following results:

 

Trial	Initial boiling point	Ambient pressure	Corrected (normal) boiling point
1	288.7 °C	98.5 kPa	290.0 °C
2	287.0 °C	98.5 kPa	288.3 °C
3	289.1 °C	98.5 kPa	290.4 °C

Both melting and boiling occur as a single peak. The melting point and initial boiling point values from trials 1 and 3 respect validity criteria (no more than 0.5°C of difference up to 326.85°C).
Moreover, the melting point of the Indium respects the checking cards limits (156.4°C for a reference value of 156.6°C) so as its enthalpy (29.16 J/g for a reference value of 28.6 J/g).

After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 290.2°C at 101.3 kPa (mean of 290.0°C for the first determination and 290.4°C for the third determination).

Description of key information

Bp: 290 ºC at ca. 101.3 kPa, OECD TG 103

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

290 °C

Additional information

A study was performed to determine the boiling point of the test item using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.2. and OECD Test Guideline No. 103, "Boiling Point" (1995).

After correction using the Sydney Young equation, the initial boiling point of the substance was determined as 290.2°C at 101.3 kPa (mean of 290.0°C for the first determination and 290.4°C for the third determination).