Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
26 Mar - 19 Apr 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Cross-reference
Reason / purpose:
reference to same study
Reference
Endpoint:
appearance / physical state / colour
Type of information:
experimental study
Adequacy of study:
key study
Study period:
26 Mar - 19 Apr 2018
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: Basic data given (comparable to guidelines/standards)
Reason / purpose:
reference to same study
Qualifier:
no guideline required
Principles of method if other than guideline:
Visual inspection during melting and boiling temperature measurement
GLP compliance:
no
Specific details on test material used for the study:
Test item storage:
At room temperature protected from light
Physical state at 20°C and 1013 hPa:
liquid
Form:
liquid
Colour:
colourless to pale yellow
Substance type:
organic

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
adopted in March 04, 2016
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted in July 27, 1995
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
adopted in March 1998
GLP compliance:
yes
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid
Specific details on test material used for the study:
Test item storage:
At room temperature protected from light

Results and discussion

Melting / freezing point
Melting / freezing pt.:
< -19 °C
Atm. press.:
998.3 hPa
Remarks on result:
other: storage experiment in the freezer

Any other information on results incl. tables

Preliminary Test

TGA: Starting at 175°C, the weight of the sample decreased significantly. However at 549°C the sample weight only decreased by 15%. The weight of the test item was therefore considered incorrect. It happened due to a technical error.

After the experiment, a colourless residue remained in the sample container (original colour: colourless to pale yellow).

Main Study

DSC:

Experiment 1: During cooling no effects were observed which were due to crystallization of the test item (results are archived in the raw data). During heating, an endothermic peak was observed between 25°C and 125°C. Based on the weight loss observed during the preliminary test, the endothermic effect was due to evaporation of volatile components. An endothermic peak was observed between 150°C and 275°C. The extrapolated onset temperature of the peak was 233.040°C. The endothermic effect was most likely obtained due to boiling of the test item. The extrapolated onset temperature was not used for the calculation of the boiling temperature, since the test item was most likely evaporated before the boiling temperature was reached. After the experiment it was observed that the test item had evaporated from the sample container.

An additional investigation of the melting temperature of the test item was performed placing two subsamples of the test item for 21 hours at -19.0 ± 0.2°C and at -80.3 ± 1.0°C respectively. It was observed after storage that the test item was a liquid (≤ -15°C freezer) and a solid (≤ -75°C freezer). According to this it was concluded that the melting temperature of the test item is < -19.0°C (< 254.2K).

 

Conclusion

The melting temperature of N-ethylcaprolactam was determined by DSC.

The melting temperature of the test item was < -19.0°C (< 254.2K) applying a storage experiment in the freezer.

The atmospheric pressure was 998.3 ± 2.7 hPa.

Applicant's summary and conclusion