Registration Dossier

Administrative data

Endpoint:
boiling 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

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.2 (Boiling Temperature)
Version / remarks:
adopted in March 04, 2016
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Version / remarks:
adopted in July 27, 1995
Qualifier:
according to
Guideline:
EPA OPPTS 830.7220 (Boiling Point / Boiling Range)
Version / remarks:
adopted in August 1996
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

Boiling point
Boiling pt.:
244 °C
Atm. press.:
998.3 hPa

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.

In order to investigate the boiling peak, a higher heating rate of 50°C/minute was used in the Experiment 2. The extrapolated onset temperature was 245.259°C. The endothermic peak had not shifted to higher temperatures. It demonstrated that boiling of the test item caused the endothermic effect. The extrapolated onset temperature was not used for calculation of the boiling temperature since it was obtained with a higher heating rate. After the experiment it was observed that the test item had evaporated from the sample container.

In order to determine the boiling temperature, a higher amount of test item was used in Experiment 3 and Experiment 4. The extrapolated onset temperature was 243.741°C with Experiment 3 and 244.171°C with Experiment 4. After the experiments it was observed that the test item had evaporated from the sample container.

The boiling temperature was determined as the mean boiling temperature of Experiment 3 (243.741°C) and Experiment 4 (244.171°C).

 

Conclusion

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

The boiling temperature of the test item was 244.0°C (517.1K).

The atmospheric pressure was 998.3 ± 2.7 hPa.

Applicant's summary and conclusion