Specification For Oil of Citronella (Java) : Indian Standard
Specification For Oil of Citronella (Java) : Indian Standard
(Reaffirmed 1998)
( Reaffirmed 2003 )
Edition 3.1
(1997-05)
Indian Standard
SPECIFICATION FOR
OIL OF CITRONELLA (JAVA)
( Second Revision )
(Incorporating Amendment No. 1)
UDC 665.524.22
© BIS 2002
Price Group 2
IS : 512 - 1988
Indian Standard
SPECIFICATION FOR
OIL OF CITRONELLA (JAVA)
( Second Revision )
0. F O R E W O R D
0.1 This Indian Standard (Second Revision) citronellal and their derivatives. The oil as such
was adopted by the Bureau of Indian Standards also finds extensive use in perfumery, various
on 25 February 1988, after the draft finalized household cleansers, technical products,
by the Natural and Synthetic Perfumery insecticides, etc.
Materials Sectional Committee had been 0.5 Earlier this oil was imported in India.
approved by the Petroleum, Coal and Related However, in the recent past, citronella grass of
Products Division Council. Java type is being cultivated extensively in
0.2 This standard was originally published various parts of India particularly in Assam
in 1954 and subsequently revised in 1961 after (Eastern regions). The oil produced in India has
incorporating the new requirement for steam been found to be, by and large, comparable with
distillation residue. The revised standard the imported Java type oil.
covered two types of citronella oil namely, 0.6 In the preparation of this standard,
Ceylon type and Java type as the oil produced considerable assistance has been derived from
in Sri Lanka approximates closely to Java type E.O.A. No. 14, ‘Citronella Oil Java type’,
oil. The Sectional Committee responsible for published by Essential Oil Association of USA,
the preparation of this standard felt that it New York and ISO 3848 : 1976 Oil of Java
should be revised in the light of prevalent trade citronella, published by the International
practices in perfumery technology and also to Organization for Standardization.
suit the material currently being manufactured
and sold in the country. 0.7 This edition 3.1 incorporates Amendment
No. 1 (May 1997). Side bar indicates
0.3 In the present revision, the Committee modification of the text as the result of
decided to confine the requirements to only incorporation of the amendment.
Java type oil of citronella and eliminating the
specification of Ceylon type oil of citronella 0.8 For the purpose of deciding whether a
since the latter is not yet produced particular requirement of this standard is
commercially in India. Gas chromatographic complied with, the final value, observed or
method for determination of purity of oil which calculated, expressing the result of a test or
is progressively used in the country, has been analysis, shall be rounded off in accordance
included in Appendix A for guidance only. with IS : 2-1960*. The number of significant
places retained in the rounded off value should
0.4 Oil of citronella (Java) is one of the most be the same as that of the specified value in
important essential oils used in perfumery this standard.
industry. It acts as main starting material for
the production of numerous important
perfumery materials such as geraniol, *Rules for rounding off numerical values ( revised ).
†Glossary of terms relating to natural and synthetic ‡Methods of sampling and test for natural and synthetic
perfumery materials ( first revision ). perfumery materials: Part 6 Determination of solubility.
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IS : 512 - 1988
Indian Standard Appendix
(1) (2) (3) (4) (5)
i) Colour and appearance Pale yellow to light tan clear liquid IS : 326 (Part 2) - 1980* —
ii) Odour Characteristic citrus grassy with rose IS : 2284 - 1988† —
undertone
iii) ‡Relative density at 27°C 0.874 3 to 0.889 3 IS : 326 (Part 3) - 1980* —
iv) Optical rotation – 0.5 to – 5° IS : 326 (Part 4) - 1980* —
v) ‡Refractive index 1.462 4 to 1.471 4 IS : 326 (Part 5) - 1986* —
vi) Total acetylizable matter calculated 85 IS : 326 (Part 9) - 1980* —
as geraniol, percent by mass, Min
vii) §Total carbonyl compounds 35 to 45 IS : 326 (Part 11) - 1986* —
calculated as citronellal, percent by
mass, Min (using 1 g of test sample,
standing time of 15 minutes, by
hydroxylammonium chloride method)
viii) Mineral oil No readable separation of mineral oil IS : 326 (Part 15) - 1984* —
ix) Steam distillation residue percent by 3 — B
mass, Max
*Methods of sampling and test for natural and synthetic perfumery materials:
Part 2 Preliminary examination of perfumery materials and samples ( second revision ).
Part 3 Relative density ( second revision ).
Part 4 Determination of optical rotation ( second revision ).
Part 5 Determination of refractive index ( second revision ).
Part 9 Determination of ester value after acetylation and free alcohols ( second revision ).
Part 11 Determination of carbonyl value and content of carbonyl compounds.
Part 15 Detection of petroleum and mineral oils ( second revision ).
†Method for olfactory assessment of natural and synthetic perfumery materials ( first revision ).
‡The correction factors for relative density and refractive index for each degree Celsius change in temperature
are 0.000 64 and 0.000 38, resectively.
§Low values are obtained for this isolate, if the usual hydroxylamine hydrochloride technique is used. Fairly
satisfactory results may be obtained, if the solution is well cooled and the titration is carried out at low temperature
(like – 10°C).
2
IS : 512 - 1988
APPENDIX A
( Clause 0.3 )
GAS CHROMATOGRAPHIC ANALYSIS OF OIL OF CITRONELLA (JAVA)
A-0. GENERAL
A-0.1 The chromatographic conditions given a) Column:
here are for guidance only. i) Material Stainless steel
ii) Length 5.49 m
A-0.2 Outline of the Method — A sample of iii) OD 0.635 cm
the material is dissolved in a suitable solvent iv) ID 0.318 cm
(for example, cyclohexane and diethyl ether)
v) Stationery phase FFAP*, 10 percent
and is injected into the gas chromatograph
by mass
when it is carried by the carrier gas from one
vi) Solid support Chromosorb WHP
end of the column to the other. During its
(80-100 mesh)
movement, the constituents of the sample
b) Carrier Gas: Nitrogen
undergo distribution at different rates and
ultimately get separated from one another. The Flow rate 30 ml/min
separated constituents emerge from the end of c) Conditions:
the column one after another and are detected i) Column temperature, 140°C
by suitable means whose response is related to isothermal
the amount of a specific component leaving the ii) Injection port 250°C
column. temperature
d) Detector:
A-1. APPARATUS i) Type F.I.D.
A-1.1 Any gas chromatograph capable of being ii) Temperature 250°C
operated under conditions suitable for resolving
A-2. CALCULATION
the individual constituents into distinct peaks
may be used. The typical chromatogram for A-2.1 Area Measurement ( see Note ) —
citronella (Java) using a chromatograph with Since* normal peaks approximate a triangle,
the following chromatographic conditions is the area is measured by multiplying the
shown in Fig. 1.
*Free fatty acid phase (FFAP) in carbowax 20 M treated
with nitrophthalic acid.
peak height with the width of half-height. A-2.2 Area Normalization ( see Note ) — By
The normal peak base is not taken since normalizing, it is meant, calculating the
large deviations may be observed due to percentage composition by measuring the area
tailing or adsorption. This technique is of each and dividing the individual areas by
rapid, simple and fairly accurate when peaks total area, for example,
are symmetrical and of reasonable width.
Area of A
NOTE — Other methods of area measurement, namely, Percentage of A = ---------------------------- × 100
triangulation, disc integrator and electronic digital Total area
integrator, if fixed with GLC machine, would be of great NOTE — Internal standardization can be used if pure
advantage appropriate internal standard is available. This method
is relative or indirect calibration.
APPENDIX B
[ Table 1, Item ( ix ) ]
DETERMINATION OF STEAM DISTILLATION RESIDUE
B-1. REAGENTS aqueous layer, transfer the petroleum ether
solution to a flask together with
B-1.1 Petroleum Ether — double distilled, sodium-sulphate.
having boiling point range 40 to 50°C.
B-2.2 Filter the petroleum ether solution
B-1.2 Sodium Sulphate — anhydrous through a filter paper in a previously weighed
( see IS : 255 - 1982* ). saponification flask containing some pumice
stone. Rinse the flask and filter paper once
B-2. PROCEDURE
more with some ether.
B-2.1 Place 5 g of the material, accurately Gently distil off or evaporate the petroleum
weighed to the nearest mg, in a 500-ml ether and dry the residue to constant mass
distilling flask. Distil the material with steam within 0.01 g, at 80 ± 1°C.
under atmospheric pressure for at
least 3 hours. Transfer the mixture of water B-3. CALCULATION
and residue to a separator, rinsing the flask Steam distillation residue, M × 100
with two successive 20 ml portions of petroleum 1
percent by mass = ------------------------
ether. Add the rinsings to the separator and M2
where
shake vigorously for one minute. Allow to
separate for 30 minutes or more, reject the M1 = mass in g of the residue, and
M2 = mass in g of the sample taken for the
*Specification for sodium sulphate, anhydrous test.
(technical grade) ( second revision ).
4
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