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

Boiling point

Administrative data

Endpoint:

boiling 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 103 (Boiling Point)

Version / remarks:

27. July 1995

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

GLP compliance:

no

Type of method:

other: DSC + DTG + detection of decomposition by NMR

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

Boiling point

Key result

Atm. press.:

1 010 hPa

Decomposition:

yes

Decomp. temp.:

> 275 °C

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

 

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.

 

The recorded main weight loss above 325.4 °C (estimated onset on TGA) may indicate a beginning evaporation (boiling). However, based on the visual inspection and the results of the DSC preliminary test (up to 250°C) where the test item showed a significant change of the melting behaviour (change of the melting point from 102.2 °C to 30.6 °C (peak top)) a product decomposition is more likely.

In order to provide evidence for this assumption, a degradation test was performed during which an aliquot of the sample was heated to 275 °C for 15 minutes. The remaining residue (94.6 % of the original material) war characterised by NMR spectroscopy. The NMR analysis confirms the decomposition of the product. Less than 20 % of the original Ceramide III b material were detected after heating.

Consequently, Ceramide III b does not provide a boiling point until disintegration at about 275 °C.

Applicant's summary and conclusion

Conclusions:

Ceramide IIIb does not provide a boiling point until disintegration at about 275 °C at 1010 hPa.

Executive summary:

The heating behaviour of Ceramide IIIb was tested according to OECD103 with visual detection, DTA, DTG and a NMR method. The substance has no melting point but disintegrates (decomposes) above 275 °C (1010 hPa).