Juniper, Juniperus oxycedrus, ext.

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Mars 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Deviations:

yes

Remarks:

A Cottrell vessel with three openings and an additional thermometer in the sample was used instead of a vessel with two openings.

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

yes

Remarks:

A Cottrell vessel with three openings and an additional thermometer in the sample was used instead of a vessel with two openings.

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected on 13 and 14 October 2014 / signed on 08 April 2015

Type of method:

dynamic method

Remarks:

and Siwoloboff method and DSC (differential scanning calorimetry)

Specific details on test material used for the study:

None

Decomposition:

ambiguous

Remarks on result:

not determinable

Remarks:

No boiling point can be determined using the Siwoloboff, dynamic and DSC method.Signs of decompositions wer observed using Siwoloboff and dynamic method while only a sign of evaporation was observed using DSC method under inert gas.

Results Dynamic Method

Observations and measured values are presented in the following table.

Table 4.3/1     Observations

First determination	Second determination	temperature “F” thermometer sample	temperature “D” thermometer Cottrell pump
test vessel clouded		50 °C	25 °C
colourless condensate visible		81 °C	30 °C
condensate dropping back		124 °C	56.5 °C
again and again strong superheating		140 °C	-
maximum temperature		174 °C	102 °C

Unfortunately, no boiling indicated by pumping Cottrell pump could be observed up to 174°C (maximum temperature tested).

At the maximum temperature, bumping was observed and the test item splattered into the complete apparatus and almost destroyed the Cottrell pump the test is stopped.

The studies were stopped for safety reasons,

After cooling down, the test item appeared visual darker.

A further experiment was performed using the dynamic method and anti bumping (boiling stones) and slowly heated with an oil bath

but no boiling was determined and bumping occurred again

At a sample temperature of 174°C, dropping back condensate hit the surface of the sample and changed into gas phase immediately. At an oil bath temperature of 205°C the test was stopped, because the limit of the oil bath lay by 220°C.

After the test a slight but visible change of the colour was visible.

Considering the colour change observed and the bumping occurring in the Cottrell cell, no additional test was conducted.

DSC measurements :

Throughout the whole test no boiling point indicating by a clear endotherm event could be observed.In all four runs a partly turbulent baseline with very small events were detected, which are hardy visible. The events cover a range of max.0.19 mW. The signal noise of the instrument was measured with approx.3.5 µw. In accordance with the manufacturer only events which 3 times bigger than the signal noise are significant. In this case some events are above this limit.

For a better differentiation of artefacts a blank measurement was performed (empty aluminium crucible as sample).

By comparison the test item measurements with the blank measurement it is obvious that something happened. Including the fact that after all performed measurements thecrucible was nearly empty which is surly caused through evaporation of the test item.

It must be stated that the determination of the boiling point of Cade Oil is not feasible under this circumstances.

Conclusions:

No defined boiling point of the test item could be determined using Siwoloboff method, the dynamic method and the DSC method.

Executive summary:

The initial boiling point of the test item was tried to be determined under GLP according to OECD 103 / EU A2 guideline, by Siwoloboff method, the dynamic method and the DSC method.

During these tests some observations were reported (during the performance following Siwoloboff and the dynamic method), which may be the sign of decomposition of the substance: colourless condensate, strong superheating highlighted by the difference between the temperature of the Cottrell pump and the Cottrell vessel, colour change after the test.

During the DSC measurements none of these observations were observed. The measurements were performed under inert gas; therefore the test item was protected from the environment. Only evaporation could be detected.

Finally, the test was terminated considering that no boiling point can be determined using the Siwoloboff, the dynamic method and the DSC method.

Description of key information

No defined boiling point of the test item was determined

Additional information

A fully reliable experimental GLP study, conducted according to a recognized OECD 103 / EU A2 methods is available. It is considered as a key study.

The initial boiling point of the test item was tried to be performed using Siwoloboff, dynamic and DSC method but no defined boiling point of the test item could be determined using these methods.

 

Signs, which may be the proof of decomposition of the substance were observed during the Siwoloboff and dynamic tests) but the tests were stopped at about 165 -174°C for safety reasons (bumping) . Only sign of evaporation was observed using the DSC method under inert gas.