Oil of Eucalyptus Globulus - Specification: Indian Standard

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IS 328 : 1992

(Reaffirmed
( Reaffirmed1997)
2003 )
Edition 3.1
(1998-12)

Indian Standard
OIL OF EUCALYPTUS GLOBULUS —
SPECIFICATION
( Second Revision )
(Incorporating Amendment No. 1)

UDC 665.526.78

© BIS 2002

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Price Group 2
Natural and Synthetic Perfumery Materials Sectional Committee, PCD 18

FOREWORD

This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards, after the
draft finalized by the Natural and Synthetic Perfumery Materials Sectional Committee had been
approved by the Petroleum, Coal and Related Products Division Council.
This standard was originally published in 1952 and first revised in 1957. In the original version,
requirement for cineole content was prescribed as 55 percent minimum which was revised to 60
percent in 1957. Currently International Standard for the material prescribes minimum of 70
percent cineole content. Although cineole content of oil of Eucalyptus Globulus produced naturally
in India is around 60 to 63 percent which is upgraded to as high as 70 percent or even higher by
fractional distillation, the Committee responsible for formulation of this standard felt that limit of
cineole content need not be raised further from the present value of 60 percent as the standard
pertains to natural essential oil of Eucalyptus globulus, while the higher concentration of cineole
content is obtained only after processing.
In this second revision an additional requirement for freezing point is being included. Other
changes as necessary to bring the standard in line with current trade practices prevailing in the
industry have also been made. While keeping O-cresol method of analysis for determination of
citral content as referee method, GLC method of analysis has been included for guidance only.
This edition 3.1 incorporates Amendment No. 1 (December 1998). Side bar indicates modification
of the text as the result of incorporation of the amendment.
For the purpose of deciding whether a particular requirement of this standard is complied with the
final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off
in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )’. The number of
significant places retained in the rounded off values should be the same as that of the specified
value in this standard.
IS 328 : 1992

Indian Standard
OIL OF EUCALYPTUS GLOBULUS —
SPECIFICATION
( Second Revision )
1 SCOPE 4 SAMPLING
This standard prescribes the requirements and Representative samples of the material,
the methods of sampling and test for oil of shall be drawn as prescribed in
Eucalyptus globulus. IS 326 (Part 1) : 1984.

2 REFERENCES 5 REQUIREMENTS
The following Indian Standards are necessary 5.1 Description
adjuncts to this standard: The oil of eucalyptus shall be obtained by water
or steam distillation of fresh leaves of
IS No. Title
Eucalyptus globulus Labill, or from other
323 : 1959 Rectified spirit ( revised ) cineole-containing species of eucalyptus (family
326 Methods of sampling and Myrtaceae) and rectified. The oil shall be a
test for natural and synthetic clear liquid, free from sediment, suspended
perfumery materials: matter, separated water and added
(Part 1) : 1984 Sampling ( second revision ) adulterants.
(Part 2) : 1980 Preliminary examination of 5.2 Solubility
perfumery materials and The oil of eucalyptus shall be soluble in an
samples ( second revision ) equal volume of ethyl alcohol, 80 percent by
(Part 3) : 1980 Relative density ( second volume, when tested as prescribed in
revision ) IS 326 (Part 6) : 1986.
(Part 4) : 1980 Determination of optical 5.3 Aldehydes
rotation ( second revision )
The oil shall satisfy the test requirements for
(Part 5) : 1986 Determination of refractive
the limit of aldehydes given in Annex A.
index ( second revision )
(Part 6) : 1986 Determination of solubility 5.4 Phellandrene
in ethanol ( second revision ) The oil shall satisfy the requirements of the
(Part 13) : 1981 Determination of cineole test for absence of phellandrene given in
content ( second revision ) Annex B.
(Part 18) : 1984 Determination of freezing 5.5 Reaction
point ( second revision )
A solution of recently distilled oil of eucalyptus
695 : 1986 Acetic acid ( third revision ) in an equal volume of 80 percent by volume
1070 : 1992 Reagent grade water — ethyl alcohol shall be neutral to moistened blue
Specification ( third or red litmus paper.
revision )
5.6 The oil of eucalyptus shall also comply with
2284 : 1988 Method for olfactory the requirements given in Table 1.
assessment of natural and
synthetic perfumery 6 TESTS
materials ( first revision ) 6.1 Tests shall be conducted as prescribed in
6597 : 1988 Glossary of terms relating to col 4 of Table 1.
natural and synthetic
6.2 Quality of Reagents
perfumery materials ( first
revision ) Unless specified otherwise, pure chemicals
shall be employed in tests, and distilled water
3 TERMINOLOGY ( see IS 1070 : 1992 ) shall be employed in tests.
NOTE — ‘Pure chemicals’ shall mean chemicals that do
For the purpose of this standard, definitions not contain impurities which affect the results of
given under IS 6597 : 1988 shall apply. analysis.

1
IS 328 : 1992

Table 1 Requirements for Oil of Eucalyptus Globulus


( Clause 5.6 )
Sl No. Characteristic Requirement Method of Test, Ref to
(1) (2) (3) (4)

i) Colour and appearance Colourless or pale yellow liquid IS 326 (Part 2) : 1980
ii) Odour and taste Characteristic aromatic IS 2284 : 1988
camphoraceous sharp odour;
followed by a sensation of cold
iii) Relative density at 27°/27°C 0.898 5 to 0.905 5 IS 326 (Part 3) : 1980
iv) Optical rotation – 5° to + 10° IS 326 (Part 4) : 1980
v) Refractive index at 27°/27°C 1.456 1 – 1.466 9 IS 326 (Part 5) : 1986
vi) Cineole content, percent by 60 IS 326 (Part 13) : 1981
mass, Min
vii) Freezing point, °C 35 and above Annex C

ANNEX A
( Clause 5.3 )
DETECTION OF ALDEHYDES

A-1 REAGENTS A-1.6 Benzene


The following reagents are required.
A-2 APPARATUS
A-l.1 Ethyl Alcohol
A-2.1 Stoppered Tube
60 percent (by volume), obtained by diluting
rectified spirit (conforming to IS 323 : 1959) Approximately 150 mm in length and 25 mm in
A-1.2 Standard Hydrochloric Acid — 0.5 N. diameter.

A-1.3 Methyl Orange Indicator A-3 PROCEDURE


Prepare a 0.04 percent solution (w/v) of methyl
A-3.1 Mix 10 ml of the material in the
orange in alcohol.
stoppered tube with 4 ml of hydroxylamine
A-1.4 Standard Potassium Hydroxide hydrochloride solution and add 5 ml of benzene.
Solution Add one drop of methyl orange indicator and
titrate the liberated acid with standard
Approximately 0.5 N. Prepare the standard potassium hydroxide solution. Shake
solution in 60 percent alcohol and standardize vigorously for two minutes after each addition
against standard hydrochloric acid, using of standard potassium hydroxide solution and
methyl orange indicator. allow the layers to separate. Note the colour of
A-1.5 Hydroxylamine Hydrochloride the lower layer. The end point is reached when
the full yellow colour of the indicator is
Solution
permanent in the lower layer.
Dissolve 35 g of hydroxylamine hydrochloride
in 950 ml of ethyl alcohol and add about 3 ml of A-3.2 The limit prescribed shall be taken as not
methyl orange indicator. Add standard having been exceeded if the volume of standard
potassium hydroxide solution until the full potassium hydroxide solution (corrected to
yellow colour of the indicator is obtained. Make exactly 0.5 N) required for the titration does
up with ethyl alcohol to 1 000 ml. not exceed 2 ml.

2
IS 328 : 1992

ANNEX B
( Clause 5.4 )
DETECTION OF PHELLANDRENE

B.1 REAGENTS B-1.3 Glacial Acetic Acid

The following reagents are required. Conforming to IS 695 : 1986.


B-2 PROCEDURE
B-1.1 Light Petroleum
B-2.1 Mix 1 ml of the material with 5 ml of
Boiling range 50° to 60°C. light petroleum and add to the solution 2 ml of
sodium nitrite solution and then 2 ml of glacial
B-1.2 Sodium Nitrite Solution acetic acid. Shake the mixture gently.
B-2.2 Phellandrene shall be taken to be absent
A saturated solution of sodium nitrite in if no crystalline precipitate forms in the upper
distilled water. layer in 10 minutes.

ANNEX C
[ Table 1, Sl No. (vii) ]
DETERMINATION OF FREEZING POINT

C-0 GENERAL previously dried with anhydrous sodium


sulphate. Add to it 2.1 g of melted O-cresol.
Cineole content in oil of Eucalyptus globulus
Insert a thermometer (C-1.2) and stir the
may be determined by refering to a table within
mixture well in order to induce crystallization.
an accuracy of about ± 3 percent if the freezing
Note the highest reading of the thermometer.
congealing point is determined accurately.
Cocking’s O-cresol method is being prescribed C-3.1.1 Warm the tube gently until the
here for determination of freezing point. contents are thoroughly melted and insert the
tube through a bored cork into a wide mouthed
C-1 APPARATUS bottle which is to act as an air jacket. The
thermometer should be suspended from a ring
C-1.1 Test Tube — stout walled about 95 mm
stand in such a way that it does not touch the
diameter, 80 mm long.
walls of the inner tube. Allow the mixture to
C-1.2 Calibrated Thermometer — cool slowly until crystallization commences, or
graduated in fifths of a degree. until the temperature has fallen to the point
C-1.3 Bottle — wide mouthed. previously noted. Stir the contents of the tube
vigorously with the thermometer, rubbing the
C-2 REAGENTS latter with the sides of the tube with an up and
down motion in order to induce rapid
C-2.1 Sodium Sulphate Anhydrous crystallization.
C-2.2 O-Cresol — pure and dry, with a C-3.1.1.1 Continue stirring and rubbing as long
freezing point below 30°C. It is hygroscopic, as the temperature rises. Take the highest
therefore should be stored in small well point as the freezing point. Repeat this
stoppered bottle. procedure until two readings agree
within 0.1°C. Report the freezing point.
C-3 PROCEDURE
C-3.2 The percentage of cineole content
C-3.1 In a stout walled test tube (C-1.1) place may be computed from Table 1 of
about 3 g of accurately weighed oil sample, IS 326 (Part 13) : 1981.

3
IS 328 : 1992

ANNEX D
( Foreword )
DETERMINATION OF CINEOLE CONTENT BY GAS CHROMATOGRAPHIC METHOD
D-0 GENERAL Conditions
D-0.1 The chromatographic conditions given Column temperature 120°C
here are for guidance only. isothermal
Injection port 200°C
D-0.2 Outline of the Method
temperature
A sample of the material is dissolved in a Detector
suitable solvent (for example, hexane, Type F. I. D.
cyclohexane and petroleum ether) and is Temperature 285°C
injected into the gas chromatograph where it is
carried by the carrier gas from one end of the D-2 Clause deleted
column to the other. During its movement, the
constituents of the sample undergo distribution
at different rates and ultimately get separated
from one another. The separated constituents
emerge from the end of the column one after
another and are detected by suitable means
whose response is related to the amount of a
specific component leaving the column.
D-1 APPARATUS
D-1.1 Any gas chromatograph capable of being
operated under conditions suitable for resolving
the individual constituents into distinct peaks
may be used. The typical chromatogram for oil
of Eucalyptus globulus using a chromatograph
with the following*chromatographic conditions
is shown in Fig. 1.
Column
Material Stainless Steel
Length 3m
OD 0.32 cm
ID 0.20 cm
Stationary phase FFAP*, 10 percent
by mass
Solid support Chromosorb WAW
60 to 80 mesh
Carrier Gas Nitrogen
FIG. 1 A TYPICAL CHROMATOGRAM OF
EUCALYPTUS OIL (GLOBULUS)
*Free fatty acid phase (FFAP) in carbowax 20M treated
with nitrophthalic acid.

4
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The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards
Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on products
covered by an Indian Standard conveys the assurance that they have been produced to comply
with the requirements of that standard under a well defined system of inspection, testing and
quality control which is devised and supervised by BIS and operated. by the producer.
Standard marked products are also continuously checked by BIS for conformity to that
standard as a further safeguard. Details of conditions under which a licence for the use of the
Standard Mark may be granted to manufacturers or producers may be obtained from the
Bureau of Indian Standards.
Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods and
attending to connected matters in the country.

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implementing the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no
changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of
Indian Standards should ascertain that they are in possession of the latest amendments or edition by
referring to the latest issue of ‘BIS Catalogue’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Doc : No. PCD 18 (1056)

Amendments Issued Since Publication


Amend No. Date of Issue
Amd. No. 1 Decemmber 1998

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