5-(methoxymethyl)-2-furaldehyde

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

July 1, 2011 - October 21, 2011

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: This study has been performed according to OECD 102 (1995) and EU Method A.1 (2008) and according to GLP principles.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2011

Report date:

2011

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

(1995)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

(2008)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Remarks:

(differential scanning calorimetry (DSC))

Test material

Test material information

Constituent 1

Reference substance name:

5-(methoxymethyl)furan-2-carbaldehyde

EC Number:

700-511-5

Cas Number:

1917-64-2

Molecular formula:

C7H8O3

IUPAC Name:

5-(methoxymethyl)furan-2-carbaldehyde

Details on test material:

- Name of test material (as cited in study report): MMF
- Description: Clear yellow liquid
- CAS Number: 1917-64-2

Results and discussion

Melting / freezing point

Melting / freezing point 1

Melting / freezing pt.:

-17 °C

Atm. press.:

>= 996 - <= 1 018 hPa

Melting / freezing point 2

Melting / freezing pt.:

256 K

Atm. press.:

>= 996 - <= 1 018 hPa

Any other information on results incl. tables

- First experiment: An exothermic peak between -50°C and -20°C was observed. This effect is most likely due to cold crystallisation of the test substance. This was immediately followed by an endothermic effect between -20°C and 0°C. The extrapolated onset temperature of the peak was -17.03°C. The effect was most likely obtained due to melting of the test substance. Another endothermic effect was observed between 200°C and 275°C. The extrapolated onset temperature of the peak was 234.50°C. The effect was most likely obtained due to evaporation of the test substance. After the experiment, a small amount of black residue remained in the sample container. It was observed as well that the majority of the test substance had evaporated from the sample container.

- Second experiment: To investigate the evaporation peak between 200°C and 275°C a hermetically sealed sample container was applied in the second experiment. Two endothermic effects were observed in the DSC-curve. The origin of the second peak is not completely understood. The extrapolated onset temperature of the evaporation peak was 223.83°C. After the experiment, a small amount of black residue remained in the sample container. It was observed as well that the majority of the test substance was evaporated from the sample container.

- Third experiment: To investigate the second endothermic peak observed in the second experiment, a lower heating rate of 5°C/minute was applied in the third experiment. The extrapolated onset temperature of the evaporation peak was 227.63°C. The endothermic peak shifted slightly to lower temperatures. It demonstrated that reaction and/or decomposition of the test substance could be the reason for the endothermic effect. After the experiment, a small amount of black residue remained in the sample container. It was observed that the majority of the test substance was evaporated from the sample container.

- Fourth experiment: The fourth experiment was performed as a duplicate measurement of the second experiment. The temperature program was similar as the program of the second experiment, as was the hermetically sealed sample container. Similar results as with the second experiment were obtained. The extrapolated onset of the evaporation peak was 229.04°C. After the experiment, a small amount of black residue remained in the sample container. It was observed as well that the majority of the test substance was evaporated from the sample container.

- Fifth experiment: The fifth experiment was performed as a duplicate measurement of the first experiment. The temperature program was similar as the program of the first experiment. Similar results as with the first experiment were obtained. The extrapolated onset of

the melting peak was -16.96°C The extrapolated onset of the evaporation peak was 233.71°C. After the experiment, a small amount of black residue remained in the sample container. It was observed as well that the majority of the test substance was evaporated from the sample container.

- Sixth experiment: The sixth experiment was performed as an additional measurement on the TGA in an attempt to explain the endothermic peak which is seen after the evaporation peak when a closed sample container is used. In this experiment an open sample container was used. The weight loss coincides with the evaporation peak.

- Seventh experiment: The seventh experiment was similar to the sixth except that in this experiment a closed sample container was used. The start of the significant weight loss slightly shifts to a higher temperature.

Based on the additional measurements can be concluded that the endothermic effect seen at ± 234°C is due to evaporation of the test substance.

Applicant's summary and conclusion

Conclusions:

The freezing temperature of the substance (a liquid under ambient conditions) was determined using DSC, in accordance with OECD 102 (1995) and EU Method A.1 (2008) and according to GLP principles. The freezing temperature of the substance was -17°C (256K).