Reaction mass of 2-O-α-L-Rhamnopyranosyl-α-L-rhamnopyranosyl-β-hydroxydecanoyl-β-hydroxydecanoic acid and α-L-Rhamnopyranosyl-β-hydroxydecanoyl-β-hydroxydecanoic acid

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

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline 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

Key result

Melting / freezing pt.:

>= 131 - <= 133 °C

Atm. press.:

1 004 hPa

Decomposition:

yes

Decomp. temp.:

> 210 °C

DSC-measurements

The test item showed a first endothermic effect in the temperature range of 120 – 160 °C, which can be assigned to a melting of the test item. A second endothermic effect was observed in the temperature range of 170 – 280 °C, which transits into an exothermic effect with a mean decomposition energy of approx. -200 J/g. In DSC run PN14984 a second exothermic effect was detected in the temperature range of 450 – 480 °C with a decomposition energy of -40 J/g. The course of the DSC signal starting from a temperature of approx. 480 °C, may be caused by a pressure rise inside the crucible due to evaporating test item or gaseous decomposition products

Table: Results of the DSC-measurements

Sample weight / mg	Onset of effect / °C	Range of effect / °C	Weight loss / mg	Atmospheric pressure / hPa
6.86	132.58 - - -	120 - 160 (endo) 170 - 270 (endo) 270 - 400 (exo) 450 - 480 (exo)	5.31	1004
10.78	130.77 - -	130 - 160 (endo) 170 - 280 (endo) 280 - 400 (exo)	8.34	1004

According to the observations in the measurements by the capillary method, the first endothermic effect can be assigned to a melting of the test item. As the onset temperatures in both tests deviate by more than 0.5 K from their mean value of 131.68 °C, the test item has a melting range of 131 °C to 133 °C.

Measurements with the capillary method

Three additional measurements with the capillary method were performed in the temperature range of 100 – 270 °C with a heating rate of 10 K/min to verify the results of the DSC measurement.

Starting at a temperature of 120 °C the test item changed its appearance from off-white to crystalline (sintering) and starts melting at a temperature of approx. 150 °C. At a temperature of 160 °C the test item is completely liquid. Starting at a temperature of about 210 °C a formation of bubbles can be observed and the colour of the test item gets darker, which indicates a decomposition accompanied by a formation of gaseous decomposition products.

Conclusions:

melting range (at 1004 hPa): 131-133°C

Executive summary:

The test item 'Decanoicacid, 3-[[6-deoxy-2-O-(6-deoxy-α-L-mannopyranosyl)-α-L-mannopyranosil-1-(carboxymethyl)octyl ester, mixture with 1-(carboxymethyl)octyl 3-[(6-deoxy-α-L-mannopyranosyl)oxy]-decanoate' has a melting point range in the temperature range from 131 °C to 133 °C at atmospheric pressure (1004 hPa) as determined by differential scanning calorimetry and verified by capillary method according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Description of key information

melting point range [determined by differential scanning calorimetry and verified by capillary method according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995)]: 131 - 133 °C at 1004 hPa (arithmetic mean of two determinations)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

132 °C