9-Octadecenamide, N-[(1S,2S,3R)-2,3-dihydroxy-1-(hydroxymethyl)heptadecyl]-, (9Z)-

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-04-21 to 2017-10-26

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 guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

adopted 27 July 1995

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

GLP compliance:

no

Type of method:

differential scanning calorimetry

Remarks:

Additionally: visual methods

Test material

Test material information

Constituent 1

Reference substance name:

Ceramide IIIB

IUPAC Name:

Ceramide IIIB

Test material form:

solid: particulate/powder

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

100.1 °C

Atm. press.:

1 010 hPa

Decomposition:

no

Sublimation:

no

Remarks on result:

other: Mp: ±0.4 °C; by DSC and visual methods

Any other information on results incl. tables

Capillary method

The melting point / range was determined using a using a melting point system (MP80, Mettler Toledo) according DIN EN ISO 3143 (previous version: DIN 53736). Two runs were done. The onset-temperature is 101 °C. The clear point was reached at 104 °C.

The thermic behaviour ofCeramide III bwas tested with a boiling point capillary from room temperature up to 300 °C with a heating rate of 10 °C/min.

Bubbles rose from approx. 250°C to 275 °C. Finally, after cooling, the content of the tube is colored and brownish residues are obvious at the wall of the tube.

DSC / TGA

As preliminary tests first TGA and DSC runs were performed.

As the substance was obviously modified within the first heating period to 250 °C, the DSC main test was focused on the melting behavior

According to the visual inspection,Ceramide III bstarts liquefying at 101 °C.

For the determination of the melting point, the main DSC test was performed in triplicate.

The melting points were read from the second and the third heating run of each test as the peak

top temperature of the allocated melting peak.

After the test procedure, the samples were re-weighed in order to check for a significant sample loss indicating potential interfering non-melting processes. For none of the samples a significant weight loss was recorded (< 0.5 %).

 

Test[		Peak temperature [°C] °C] Mid	Enthalpy (normalised) [J/g]
		100.6	79.1
	Test 1	99.8	72.6
		m100.2	m75.9
		100.5	81.0
	Test 2	99.7	74.0
		m100.1	m77.5
		100.5	81
	Test 3	99.7	74
		m100.1	m77.5
	Average	100.1	77.0
	SD	0.4	3.8
	CV [%]	0.44%	4.99%

 

In the TGA test, a sample of the test item was heated from 30 °C to 675 °C in an inert gas atmosphere (N2). A first drop was detected beginning at 225.0 °C (onset) attended by a weight loss of about 10 %. The main drop was detected beginning at 325.4 °C (onset). Up to 400.2 °C a total weight loss of 99.9 % was recorded.

 

By means of DSC forCeramide III ban average melting point of 100.1 ± 0.4 °C was measured which is in accordance with the one measured by visual observation in the melt microscope (start liquefaction at 101 °C).

Applicant's summary and conclusion

Conclusions:

Melting point is 100.1 °C ± 0.4 °C at 1010 hPa, without decomposition and sublimation.

Executive summary:

The melting temperature of Ceramide IIIB was determined according to Guideline OECD 102 with differential scanning calorimetry and visual methods. The melting point is 100.1 °C ± 0.4 °C at 1010 hPa, without decomposition and sublimation.