Determination of Safrole Content of Essential Oils - [www.rhodium.

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09-Mar-15

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DETERMINATION OF SAFROLE CONTENT OF ESSENTIAL OILS THROUGH CONGEALING POINT

DETERMINATION
A CHEAP AND EASY METHOD REQUIRING A MINIMAL AMOUNT OF EQUIPMENT

PROCEDURE1
Place about 10 mL of the oil in a dry test tube of 18-20
mm. diameter. Cool in w ater or in a suitable freezing
mixture, the temperature of w hich should be about 5
degrees low er than the supposed congealing point of the
liquid. To initiate congelation, rub the inner w alls of the
tube w ith a thermometer, or add a small amount of the
substance previously solidified by excessive freezing. The
thermometer should be rubbed quickly up and dow n in
the mixture in order to cause a rapid congelation
throughout, w ith its subsequent liberation of heat. The
temperature should be read frequently; at first the rise of
temperature is rapid, but soon approaches a constant
value for a brief interval of time. This value is taken as the
congealing point of the oil. The process described above
should be repeated several times to assure obtaining the
true congealing point.

Safrole Content Congealing Point

100%

+11.0C

90%

+7.5C

80%

+4.6C

70%

+1.7C

60%

-1.3C

Determine the congealing point of the sassafras oil, and estimate the safrole content from the
adjacent table, it w ill give values of the safrole content w ith an accuracy of about 2% if the congealing
point is above 2C.

CONGEALING POINTS OF
OCOTEA CYMBARUM OIL
SAMPLES VARYING IN
SAFROLE CONTENT2
Safrole
Congealing
Content
Point
(weight%)
69.1%

2.4C

73.3%

3.7C

76%

4.4C

79%

5.2C

82%

6.1C

85%

6.9C

86%

7.2C

87%

7.5C

88%

7.8C

89%

8.0C

90%

8.3C

91%

8.6C

92%

8.8C

93%

9.2C

94%

9.4C

95%

9.7C

96%

10.0C

97%

10.3C

98%

10.6C

99.5%

11.0C

The congealing point offers a distinct advantage over the melting point and
the titer, in the case of mixtures, such as essential oils. In determining the
congealing point, the oil is supercooled so that, upon congelation, immediate
crystallization w ith liberation of heat occurs. This results in a rapid rise of
temperature, w hich soon approaches a constant value and remains at this
temperature for a period of time. This point is know n as the "congealing
point." W ith increasing percentage of crystalline material in an oil, the
congealing point w ill approach a maximum. Hence, this physical property is a
good criterion of the percentage of such material. The congealing point is
important in the evaluation of anise, sassafras and fennel oils, as w ell as oil of
Ocotea cymbarum.
The thermometer used should be calibrated in 0.1C units and should be
accurately standardized. A thermometer covering the range of -5C to +50C
is satisfactory for most determinations. Before the oil is tested, it should be
thoroughly dried w ith sodium sulfate since the presence of small amounts of
w ater w ill often materially low er the congealing point. In the case of sassafras
oils, it is w ell to initiate the congelation by the addition of a small piece of solid
safrole since sassafras oil can be congealed only w ith great difficuly if no
"seed" is used. For a more exact determination of the congealing point, the
test tube containing the supercooled oil may be insulated by means of an air
jacket. This is frequently of particular importance w hen determining
congealing points w hich are much below room temperature, as, for example,
the congealing point of euclayptus (sic) oils. Gildemeister and Hoffmann
recommend the use of the Beckman apparatus, frequently used for the
determination of molecular w eights by the low ering of the freezing point. The
use of a larger sample (up to 100 mL) may make the congealing point
sharper. This method has an accuracy of 0.7% according to the paper2.

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COMPARATIVE ANALYSES OF SAMPLES

OF OIL OF OCOTEA CYMBARUM2
Congealing Safrole content Safrole content
Oil Point
(from table)
(Hg analysis)
A

8.7C

91.4%

92.1%

7.2C

86.0%

85.4%

8.1C

89.3%

88.6%

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Determination of Safrole Content of Essential Oils - [www.rhodium.ws]

09-Mar-15

REFERENCES
1. Guenther's "Essential Oils", Volume 1
2. Journal of Analytical Chemistry, Volume 20, Book 3, 1948 p.248-249

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