Fenugreek, ext.

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

Study period:

09 January - 28 March 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Justification for type of information:

The study was conducted according to an internationally recognised method, and under GLP. Test substance is adequately characterised. Therefore full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected on 20 and 21 June 2017 / signed on 04 September 2017

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

<= -20 °C

Results

DSC measurement

Two DSC measurements in an aluminium crucible with a hole were performed. The test item was cooled down with a cooling rate of 1 K/min (-50 °C for the first measurement and -80 °C for the second measurement), the minimum temperature was kept for 30 min (first measurement) and 300 min (second measurement) and afterwards the test item was heated up with a heating rate of 10 K/min (maximum temperature 500 °C for the first measurement and 25 °C for the second measurement). The measurements showed no endothermal effect in the temperature range of -80 to 25 °C.

The results of the DSC measurements are summarized in the table 4.2/1 below.

Table 4.2/1.- Melting point (DSC measurements)

Ident No.	Test item / mg	Starting temperature / °C	Final test temperature / °C	Temperature range (endo-thermal) / °C	Onset (melting) / °C	Crucible	Observations after the measurement
36809	17.91	See above	See above	---	---	Aluminium with a hole	---
36828	16.30	See above	See above	---	---	Aluminium with a hole	---

Graphical presentations of the DSC runs are shown in the experimental report.

Visual measurements

For clarification a sample each of the test item in a glass vial (approximately 5 ml) was placed into a fridge and a freezer. After 48 h these samples were observed visually (see Table 4.2/2).

Table 4.2/2.-Visual results after storage in fridge and freezer

Temperature	+3 °C for 48 h	-23 °C for 48 h
State of sample	Brown-yellow viscous mass with increased viscosity (liquid)	Brown-yellow viscous mass with significantly increased viscosity (liquid)

Even after 48 h at -23 °C the test item was still mostly in its original state (viscous liquid). Only the viscosity increased at lower temperatures. The test item remained as a viscous liquid at both temperatures.

Due to the results from the DSC-measurements and the visual inspection at lower temperatures, It was concluded that the test item was a liquid with no melting point above -20°C.

Final results

No melting point was measured above -80 °C with DSC method.

However, since melting may be hindered at low temperatures due to supercooling it should only be assumed that no melting point exists above ‑20 °C. This was confirmed by a visual inspection after storage at -23 °C for 48 h.

Conclusions:

The test item was a liquid with no melting point above -20°C.

Executive summary:

The study was performed in order to determine the melting point of test item according to OECD 102, resp. EU A.1 guideline, using the DSC method and visual method.

Description of key information

The test item was a liquid with no melting point above -20°C.

Additional information

A fully reliable experimental study, conducted according to OECD 102/ EU A1 guideline is available.

It is considered as a key study and the result is retained as key data.