1-methoxy-4-[3-methyl-4-(2-phenylethoxy)but-3-en-1-yl]benzene

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:

04-02-2021 to 26-03-2021

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Guideline study performed under GLP. All relevant validity criteria were met.

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

<= -66.7 °C

Atm. press.:

ca. 1 atm

Decomposition:

no

Sublimation:

no

Remarks on result:

other: mean melting point (n = 2)

(i) Preliminary study

Starting at 300°C, the weight of the sample decreased significantly. At 354°C, the sample weight had decreased by 25%. After the experiment it was observed that the test item was evaporated from the sample container.

 

(ii) Main study

- Experiment 1: During cooling, a glass transition between -60°C and -90°C was found. The effect was obtained due to crystallization of the test item. During heating a glass transition was observed between -90°C and -50°C followed by an endothermic effect starting at 200°C. The inflection temperature of the first effect was -66.873°C. The second endothermic effect was most likely obtained due to boiling of the test item. Since the boiling effect did not appear complete no onset temperature was calculated. After the experiment it was observed that the test item had evaporated from the sample container. The first endothermic effect (-66.873°C) was obtained due to melting of the test item.

- Experiment 2: Was conducted as a duplicate of experiment 1, to examine the glass transition and/or the extrapolated onset of the melting temperature peak. In order to investigate the endothermic effect, more test item (3.35 mg) was utilized (rather than 2.56 mg, experiment 1). Similar results as in experiment 1 were obtained. The first inflection temperature was -66.602°C. The first endothermic effect (-66.602°C) was obtained due to melting of the test item. Again, later in the run the second endothermic effect was most likely obtained due to boiling of the test item but did not look complete. After the experiment it was observed that the test item had evaporated from the sample container.

- Experiment 3: Was conducted to further examine the boiling temperature of the test item, no cooling cycle was completed. More test item (4.38 mg) was utilized. Similar results as in experiment 1 and 2 were obtained (an endothermic effect starting at ca. 200°C). The endothermic effect did not appear to be complete. After the experiment it was observed that the test item had evaporated from the sample container.

- Experiment 4: Was conducted to further examine the boiling temperature of the test item. More test item (3.28 mg) was utilized, comparable to experiment 2. A higher heating rate of +50°C/minute was utilized. An exothermic peak was observed between 150°C and 250°C and an endothermic effect starting at 250°C directly followed by an exothermic peak. Based on these results decomposition reactions were considered the reason for these observed effects. After the experiment it was observed that the test item had evaporated from the sample container and the lid was ripped open.

- Experiment 5: Was conducted to further examine the boiling temperature of the test item utilizing a closed DSC crucible and a heating rate of +20°C/minute (comparable to experiments 1, 2 and 3). The test item mass was 3.47 mg, comparable to experiment 1 and 2. The endothermic effect did not shift significantly to higher temperatures. It demonstrated that reaction and/or decomposition of the test item caused the endothermic effect. After the experiment it was observed that the test item had evaporated from the sample container and the lid was ripped open.

 

The melting temperature was determined as the mean melting temperature of Experiment 1 (-66.873°C) and Experiment 2 (-66.602°C). Mean (n=2) : -66.7°C.

The boiling temperature could not be determined. Reaction and/or decomposition of the test item was observed during DSC experiment between +150°C and +200°C (423K – 473K) and at +250°C (523K). Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started (i.e. ca. +150°C or 423.15). Under the conditions of this study, the test item has no determinable boiling temperature below its decomposition temperature (ca. +150°C or 423.15), at atmospheric pressure.

Conclusions:

The melting temperature of the test item has been determined to be -66.7 °C (or 206.45 K). At above this temperature the substance is considered to be liquid.

Executive summary:

The melting temperature was determined using OECD TG 102 and EU Method A.1 with the Differential Scanning Calorimetry method under GLP. The guideline defines the melting temperature as: the temperature at which the phase transition from solid to liquid state occurs at atmospheric pressure and this temperature ideally corresponds to the freezing temperature. During DSC cooling an exothermic effect was observed which were due to crystallization of the test item between -90°C and -50°C. Subsequently upon heating an endothermic effect was seen indicating melting of the test item. The melting temperature was determined as the mean melting temperature of Experiment 1 (-66.873°C) and Experiment 2 (-66.602°C), respectively. It was concluded that the melting temperature of the test item is -66.7°C (or 206.45K). At above this temperature the substance is considered to be liquid.

Description of key information

Mp: -66.7 °C (or 206.45 K) at 1 atmosphere, OECD TG 102 : DSC Method, 2021

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

-66.7 °C

Additional information

Key study : OECD TG 102, 2021 : The melting temperature was determined using OECD TG 102 and EU Method A.1 with the Differential Scanning Calorimetry method under GLP. The guideline defines the melting temperature as: the temperature at which the phase transition from solid to liquid state occurs at atmospheric pressure and this temperature ideally corresponds to the freezing temperature. During DSC cooling an exothermic effect was observed which were due to crystallization of the test item between -90°C and -50°C. Subsequently upon heating an endothermic effect was seen indicating melting of the test item. The melting temperature was determined as the mean melting temperature of Experiment 1 (-66.873°C) and Experiment 2 (-66.602°C), respectively. It was concluded that the melting temperature of the test item is -66.7°C (or 206.45K). At above this temperature the substance is considered to be liquid.