Concrete of Cistus ladaniferus (Cistaceae) obtained from stems and leaves by organic solvents extraction

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:

15 April - 15 May 2014

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. Restrictions apply considering that the melting of the substance is difficult to observed and a piece of thin wire was used in order to detect melting. Otherwise, the substance is considered to be adequately characterised. Therefore validation with restrictions applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

dated 27. July 1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

dated 31. May 2008

Deviations:

no

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected on 29 and 30 November 2010 / signed on 11 April 2011

Type of method:

capillary method

Key result

Melting / freezing pt.:

>= 16.4 - <= 36.8 °C

In the pre-test, the test item was considered as solid at 5°C, - 20 °C and - 80 °C.

 

Table 4.2/1: Pre-Test

Room Temperature	5 °C	- 20 °C	- 80 °C
almost solid	solid	solid and turbid	solid

 

The following values were recorded during the Main test:

 

Table 4.2/2: Main Study

Melting point/range	Begin	End
First Determination	16.3 °C (289.5 K)	36.7 °C (309.9 K)
Second Determination	16.4 °C (289.6 K)	36.8 °C (310.0 K)

The means between both determinations give the following values for the melting range:

Melting range: 16.4 °C to 36.8 °C (289.6 K to 310.0 K)

Standard deviation: 0.1 (begin); 0.1 (end)

Estimated accuracy: ± 0.1 °C

 

Validity

All validity criteria were met, as can be taken from the following table.

 

Table 4.2/3: Validity

 

Parameter	Criterion	Found	Assessment
Difference between duplicate determinations	≤ 0.5 K	0.1 K	valid
Difference between begin and end of melting process	≤ 0.5 K	20.4 K	melting range is stated

 

The validity criterion “difference between duplicate determinations” was met. The test item showed a melting range, no melting point. As the test item is a mixture, this can be considered normal.

No observations were made which might cause doubts on the validity of the study outcome. Therefore, the result of the study is considered valid.

Conclusions:

The melting range of test substance was determined to be (16.4 °C - 36.8 °C) (289.6 K to 310.0 K).

Executive summary:

The melting point of the test substance was determined under GLP according to EU Method A.1 and OECD 102, using the capillary method.

A preliminary test indicated that the substance is solid at 5°C, -20°C and -80°C.

Then, the main test was carried out in duplicate.

Considering the nature of the substance, a sharp transition from liquid to solid was not anticipated. Therefore, a short piece of thin wire was used to detect melting.Thetemperature, at which the wire started to sink in the liquefying test item was recorded as begin of melting process. The end of melting process was recorded when the wire had fully moved into the test item.

The results were within accuracy limits of the method but a difference was observed between beginning and ending of melting process. Finally mean values of the two independant determinations were used to determine a melting range of this natural complex substance.

No indication of decomposition was recorded.

Description of key information

The melting range of the test item was determined to be (16.4°C - 36.8 °C) (289.6 K - 310.0 K).

Additional information

A reliable GLP experimental study, conducted according to a recognized OECD/EC guidelines using capillary method, is available and is considered as a key study.

Note that considering the complex nature of the substance,no sharp melting point could be determined experimentally. Therefore, the result is expressed as a melting range and no single key value can be retained for purpose of CSA.