Tributyl-2-methoxypropylphosphonium salt with 4,4'-[2,2,2-trifluoro-1-(trifluoromethyl)ethylidene]bis[phenol]

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

01 August 2005 - 30 August 2005

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: This study was conducted in accordance with OECD TG 102 and is compliant with GLP standards.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2005

Report date:

2005

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

GLP compliance:

yes

Type of method:

other: Differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

MTDID 3285

IUPAC Name:

MTDID 3285

Details on test material:

- Name of test material (as cited in study report): MTDID 3285
- Physical state: solid
- Analytical purity: Min 80%
- Stability under test conditions: stable
- Storage condition of test material: at room temperature in the dark

Results and discussion

Melting / freezing point

Melting / freezing pt.:

79 °C

Decomposition:

yes

Remarks:

Reaction or decomposition of MTDID 3285 was observed immediately after melting of MTDID 3285

Any other information on results incl. tables

The test was performed using a Q100 differential scanning calorimeter (DSC, TA Instruments, New Castle, Delaware, USA): Detection limit: approximately 1 uW

Sample container: aluminum; closed

Reference: empty sample container

A preliminary test was performed using a Q50 thermogravimetric analyzer (TGA, TA Instruments).

For the preliminary test, 25.3 mg MTDID 3285 was heated up in the TGA from room temperature to 647 °C (the point where 90% weight loss was observed) with a rate of 20 °C/minute. After the experiment, the sample was cooled to 50 °C and the consistency of the test substance was determined. From approximately 225 °C upwards the weight of the sample significantly decreased. At 316 °C, the sample weight was decreased by 25%. After the experiment, the sample had a black color (original color: light brown). The change of the color of MTDID 3285 may indicate reaction or decomposition.

The melting point of MTDID 3285 was measured using differential scanning calorimetry (DSC) in two trials. In DSC, when the test substance undergoes a transition, such as melting/freezing, it is indicated by a deviation from the base line of the heat-flow record. During melting, heat is consumed and the deviation from the base line is in the endothermic direction. In the first experiment (25 °C - 125 °C), an endothermic effect followed by an exothermic and another endothermic effect was observed between 65 °C and 120 °C (see Figure 1). Melting of the test substance likely caused the first endothermic effect. The exothermic and the second endothermic effect were probably caused by reaction or decomposition of the test substance followed by further melting of the decomposed test substance. The extrapolated onset temperature of the first endothermic effect (melting) was 79 °C.

In the second experiment (25 °C - 93 °C), a lower end temperature was used in order to determine if melting of the test substance caused the first endothermic effect (see Figure 2). The endothermic effect started at 60 °C. The extrapolated onset temperature of this effect was 79 °C. After the experiment, the sample had coalesced which was probably caused by melting of the test substance. Reaction or decomposition of the test substance was observed immediately after melting of the test substance.

Heat flow curve, first experiment see Figure 1

Heat flow curve, second experiment see Figure 2

Applicant's summary and conclusion

Conclusions:

The melting point of MTDID 3285 is 79 °C at normal atmospheric pressure

Executive summary:

The melting point of MTDID 3285 was measured using differential scanning calorimetry (DSC). In DSC, when the test substance undergoes a transition, such as melting, freezing or boiling, it is indicated by a deviation from the base line of the heat-flow record. In two trials, endothermic deviations in the DSC curve were observed and the extrapolated melting point of the test substance is determined to be 79 °C at normal atmospheric pressure. Immediately after melting, reaction or decomposition of the MTDID 3285 was observed. This study was conducted in accordance with OECD TG 102 and is compliant with GLP standards. Therefore, this study is classified as reliable without restrictions.