N,N-Dimethyl-9-dodecenamide

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:

03 February- 10 February 2022

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

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

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Melting / freezing pt.:

-8.7 °C

Atm. press.:

>= 98.4 - <= 98.5 kPa

Decomposition:

no

Sublimation:

no

Pre study

The melting point of the substance was observed at -9.8°C (onset temperature of the peak). The freezing point was observed at -21.4°C (endset temperature of the peak).

The initial boiling point of the substance was observed at 318.1°C (onset temperature of the peak).

A corresponding mass loss was observed from the beginning of the boiling peak.

First determination

The melting point of the substance was observed at -8.6°C (onset temperature of the peak). The freezing point was observed at -22.4°C (endset temperature of the peak).

Initial boiling point was observed at 320.4°C (onset temperature of the peak) and a mass loss of 97.38% was observed between the beginning and the end of the boiling peak.

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Atmospheric pressure: 98.4 kPa.

Second determination

The melting point of the substance was observed at -8.8°C (onset temperature of the peak). The freezing point was observed at -23.3°C (endset temperature of the peak).

Initial boiling point was observed at 320.4°C (onset temperature of the peak) and a mass loss of 97.21% was observed between the beginning and the end of the boiling peak.

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Atmospheric pressure: 98.5 kPa.

The Sydney-Young equation was used to determine the boiling points at 101.3 kPa.

Validation of results:

Results are considered as valid as the following conditions are satisfied:

- The temperature difference obtained between the two samples tested is less than 0.5°C.

- The melting point obtained on the reference substance, Zinc, is included in the checking chart limits.

- The corrected sensitivity, i.e. the enthalpy measured during the melting of indium, does not differ by more than 10% from the expected value.

Executive summary:

A study was performed to determine the melting point/range and boiling point of the test item N,N-dimethyl dodec-9-enamide using the Differential Scanning Calorimetry (DSC). The method followed was designed to be compliant with Regulation EC No. 440/2008 Method A.1 and A.2. and OECD Test Guideline No. 102, "Melting Point/Melting Range" and No. 103, "Boiling Point" (1995).

In this method, two crucibles, with pierced lid, were put in the apparatus furnace under inert atmosphere (helium) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied. The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram. A cooling system using liquid nitrogen allowed experiments with low temperatures down to -120°C.

Two trials were conducted and corresponding thermograms were obtained.

The initial boiling point values respect validity criteria (no more than 0.5°C of difference up to 326.85°C).

Freezing points were observed at -22.4°C for the first trial and -23.3°C for the second trial.

Moreover, the melting point of the zinc respects the checking chart limits (420.4°C for a reference value of 419.5 ± 2.0 °C) so as the enthalpy of Indium (27.12 J/g for a reference value of 28.6 ± 2.9 J/g).

The melting point of N,N-dimethyl dodec-9-enamide was determined as -8.7°C.

After correction using the Sydney Young equation, the initial boiling point of N,N-dimethyl dodec-9-enamide was determined as 321.8°C at 101.3 kPa (same value for both determinations).

Description of key information

The melting point was determined to be -8.7°C in a test performed using Differential Scanning Calorimetry according to OECD TG 102 and EU Method A.1.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

-8.7 °C