Pregna-1,4-diene-3,20-dione, 9-bromo-6-fluoro-11-hydroxy-16-methyl-21-[(1-oxopentyl)oxy]-, (6.alpha.,11.beta.,16.alpha.)-

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

08 July 2016

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

GLP compliance:

no

Other quality assurance:

ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)

Type of method:

thermal analysis

Remarks:

Differential Thermal Analysis (DTA) / Differential Scanning Calorimetry (DSC)

Key result

Melting / freezing pt.:

>= 100 - <= 130 °C

Decomposition:

yes

Remarks on result:

other: mean of two determinations in an open crucible

RESULTS:

1. Thermal stability and decomposition:

- At room temperature the test item is a powdery solid

- Between approx. 65 °C – 140 °C an endothermic phase could be detected which indicates the melting range

- After the melting process an endothermic phase between 145 and 160 °C which went over directly to a exothermic phase between approx. 160 -215 °C was observed; this exothermic phase indicates transformation and decomposition, respectively, of the test item

 

2. Melting Point:

- Endothermic effects were visible already at 65 °C (These effects lead to the assumption that, while melting, transformation and decomposition could occurre)

- In the closed crucible no melting could be observed

 

The test item recrystallized after the melting process:

- In the open crucible the residue was a light orange powder

- In the closed crucible the residue was a dark red-brownish melt which indicates transformation of the substance

 

Validity criteria for the measurement of the melting point:

Target condition according to guideline:	Actual condition according to the study:	Validity criteria met:
The heating rate should not exceed 2 K/min.	Heating rate 5 K/min.	No
The mean of at least two measurements which are in the range of the estimated accuracy is reported as the melting temperature.	Two values were determined, in a closed crucible.	Yes
If the substance decomposes or sublimes before the melting temperature is reached, the temperature at which the effect is observed shall be reported.	The test substance was heated up to a temperature of 130°C - no melting was observed in closed crucible.	Yes

 

Conclusions:

The melting range lies between 100 and 130°C and no pressure was reported.
The study is regarded as valid, only the heating rate of the sample is higher than requested by the OECD. This is however not regarded as relevant to the outcome of the study.

Executive summary:

A differential thermoanalysis method (DTA) was used to determine the melting point which conforms with the procedure Test method A.1, "Determination of the melting point", described in the EC-Guideline. The melting temperature was observed in a range between 100 and 130 °C (mean of two determinations in an open crucible). Endothermic effects were visible already at 65 °C. These effects lead to the assumption that, while melting, transformation and decomposition could occurre. In the closed crucible no melting could be observed. Bromhydrin-valerat recrystallized after the melting process. In the open crucible the residue was a light orange powder. In the closed crucible the residue was a dark red-brownish melt which indicates transformation of the substance.

Description of key information

The melting range lies between 100 and 130 °C and no pressure was reported.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

115 °C

Additional information

Endothermic effects were visible already at 65 °C. These effects lead to the assumption that, while melting, transformation and decomposition occurred. In the closed crucible no melting could be observed. Bromhydrin-valerat recrystallized after the melting process.