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Physical & Chemical properties

Melting point / freezing point

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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: information from boiling point determination via DSC
Cross-reference
Reason / purpose:
reference to same study
Reference
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Decomposition:
yes
Decomp. temp.:
>= 240.8 °C
Remarks on result:
other: substance decomposes before melting
Conclusions:
The boiling point could not be determined under the test circumstances. In both DSC measurements two endothermic peaks were detected. Between those an exothermic behaviour was observed. The beginning of decomposition from 240.8 °C was evaluated with event marker function. The melting point was evaluated with onset function. Therefore, the melting point of the decomposition product was determined as: 253.46 ± 0.33°C (526.61 ± 0.33 K)
The study was performed according to the OECD TG109 and EU Method A.3 without deviations and therefore considered to be of the highest quality (reliability Klimisch 1).
Executive summary:

The boiling point of the test item was determined in a study according to OECD 103 resp. EU Method A.2 (DSC).

The test substance was filled into a sample tube containing a capillary tube in such a manner that the sealed part of the capillary was lying below the surface of the test substance and then set into the aluminium block. The block was heated with a quick heating rate. Heating was performed with a gas burner. All observations were observed.

A one-way aluminium crucible was prepared like described below. 2.85 mg test substance was weighed into a one-way aluminium crucible. The weight of the crucible with the test substance was recorded with 48.29 mg. The crucible was heated in the muffle furnace from room temperature to 450 °C.

After cooling down the crucible was inspected for visual changes and the weight of the crucible was recorded.

The DSC was calibrated for one-way aluminium crucibles with lid and a heating rate of 10 K/min using zinc and indium as standards.

An existing valid calibration was used (date: 16. Jan. 2018). The calibration was proved with indium (date: 19. Jun. 2018).

2.58 mg (first determination) and 2.89 mg (second determination) of the test item, respectively, were weighed into a one-way aluminium crucible and the crucible was closed with perforated aluminium lid using a capsule press. The mass of the crucible was documented.

The crucible containing the test item was heated under inert gas from 25°C to 340°C for the first determination and for the further determinations from 25 °C to 445 °C using a heating rate of 10 K/min. As reference an empty crucible of the same kind was used. The heat flow and temperature was recorded by the DSC during the test. After the test the appearance of the crucible was inspected for visual changes and the mass of the crucible was recorded.

The determination of the boiling point of Phosphoric acid, butyl ester was performed via DSC (differential scanning calorimetry).

In both DSC measurements two endothermic peaks were detected. Between those an exothermic behaviour was observed.

The beginning of decomposition from 240.8 °C was evaluated with event marker function. The melting point was evaluated with onset function. Therefore, the melting point of the decomposition product was determined as: 253.46 ± 0.33°C (526.61 ± 0.33 K)

The boiling point could not be determined under these test circumstances.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019
Report Date:
2019

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
other: OECD Guideline 103 (Boiling Point) and EU Method A.2 (Boiling Temperature)
GLP compliance:
no
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
- Storage conditions: Room Temperature (20 ± 5 °C)
- Expiry date: 16. Dec. 2019

Results and discussion

Melting / freezing point
Melting / freezing pt.:
253.46 °C
Decomposition:
yes
Decomp. temp.:
>= 240.8 °C
Sublimation:
no
Remarks on result:
other: melting point of the decomposition product was determined

Applicant's summary and conclusion

Conclusions:
In both DSC measurements two endothermic peaks were detected. Between those an exothermic behaviour was observed. The beginning of decomposition from 240.8 °C was evaluated with event marker function. The melting point was evaluated with onset function. Therefore, the melting point of the decomposition product was determined as: 253.46 ± 0.33°C (526.61 ± 0.33 K)