Reaction Mass of (4R)-4-isopropenyl-1-methylcyclohexene and (4R)-4-(2-methoxypropan-2-yl)-1-methylcyclohexene

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 October - 21 December 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Study conducted in accordance with international guidelines and in acordance with GLP. All guideline validity criteria were met.

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:

method to determine freezing temperature

Specific details on test material used for the study:

RADIOLABELLING INFORMATION (if applicable)
- Radiochemical purity: n/a
- Specific activity: n/a
- Locations of the label: n/a
- Expiration date of radiochemical substance: n/a

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: ca. 4 ºC in the dark and under nitrogen.
- Stability under test conditions: Assumed stable
- Solubility and stability of the test substance in the solvent/vehicle: n/a
- Reactivity of the test substance with the solvent/vehicle of the cell culture medium: n/a

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: n/a
- Preliminary purification step (if any): n/a
- Final dilution of a dissolved solid, stock liquid or gel: n/a
- Final preparation of a solid: n/a

FORM AS APPLIED IN THE TEST (if different from that of starting material): n/a

OTHER SPECIFICS: n/a

Key result

Melting / freezing pt.:

< -20 °C

Decomposition:

no

Sublimation:

no

Table 1       Cooling data (determination 1)

Time (s)	Temperature (ºC)	Time (s)	Temperature (ºC)	Time (s)	Temperature (ºC)
0	20.0	390	-1.5	780	-14.0
30	19.0	420	-2.5	810	-15.0
60	17.0	450	-4.0	840	-16.0
90	15.0	480	-5.0	870	-16.5
120	13.5	510	-6.0	900	-17.0
150	12.5	540	-7.5	930	-18.0
180	9.5	570	-8.5	960	-18.5
210	8.0	600	-9.0	990	-19.0
240	6.0	630	-10.0	1020	-19.5
270	4.5	660	-11.0	1050	-20.0
300	2.5	690	-12.0	1080	-20.5
330	1.0	720	-13.0	1110	-21.0
360	0.0	750	-13.5	1140	-21.5

Result: freezing temperature < -20 ºC

Table 2       Cooling data (determination 2)

Time (s)	Temperature (ºC)	Time (s)	Temperature (ºC)	Time (s)	Temperature (ºC)
0	20.5	390	-2.5	750	-15.0
30	19.5	420	-4.0	780	-16.0
60	17.5	450	-6.0	810	-16.5
90	14.0	480	-6.5	840	-17.5
120	11.0	510	-7.5	870	-18.0
150	10.0	540	-9.0	900	-18.5
180	8.0	570	-10.0	930	-19.5
210	7.5	600	-11.0	960	-20.0
240	5.5	630	-12.0	990	-20.0
270	4.0	660	-13.0	1020	-20.5
300	1.5	690	-13.5	1050	-21.0
330	0.5	720	-14.5	1080	-21.0
360	-1.0

Result: freezing temperature < -20 ºC

Conclusions:

The freezing temperature of the test item was < - 20 ºC.

Executive summary:

EU Method A.1 (2017) - An aliquot (approximately 15 mL) of test item was placed into a test tube containing a thermometer. A wire loop with which the sample could be agitated was placed inside the tube to ensure sample homogeneity during cooling. The test tube was surrounded by a glass jacket and then placed into a large beaker containing a dry ice/acetone mixture. The temperature and observations of the test item were recorded approximately every 30 seconds. The dry ice/acetone bath was maintained until the sample temperature had reached below -20 °C or until the test item solidified. The determination was carried out in duplicate.

The freezing temperature of the test item was established as being < - 20 ºC.

Description of key information

Melting Point = < - 20 ºC; EU Method A.1; Anon. (2017)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

-20 °C

Additional information

In a study conducted in accordance with EU Method A.1, an aliquot (approximately 15 mL) of test item was placed into a test tube containing a thermometer. A wire loop with which the sample could be agitated was placed inside the tube to ensure sample homogeneity during cooling. The test tube was surrounded by a glass jacket and then placed into a large beaker containing a dry ice/acetone mixture. The temperature and observations of the test item were recorded approximately every 30 seconds. The dry ice/acetone bath was maintained until the sample temperature had reached below -20 °C or until the test item solidified. The determination was carried out in duplicate.

The freezing temperature of the test item was established as being < - 20 ºC.