IS 326-13: Methods of Sampling and Test for Natural and Synthetic Perfumery Materials, Part XIII: Determination of Cineole Content

2005·1 MB·English

by  Bureau of Indian Standards

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IS 326-13 (2005): Methods of Sampling and Test for Natural
and Synthetic Perfumery Materials, Part XIII: Determination
of Cineole Content [PCD 18: Natural and Synthetic Fragrance
Materials]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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4
IS 326( Part 13 ): 2005
ISO 1202:1981

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Indian Standard
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METHODS OF SAMPLING AND TEST FOR NATURAL
AND SYNTHETIC PERFUMERY MATERIALS
[
PART 13 DETERMINATION OF 1,8-CINEOLE CONTENT
Third Revision)
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ICS 71.100.60

@ 91S 2005
BUREAU OF INDIAN STANDARDS
I MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
~i3y 2005 Price Group 2
Natural and Synthetic Fragrance Materials Sectional Committee, PCD 18
NATIONAL FOREWORD
This Indian Standard ( Part 13 ) ( Third Revision ) which is identical with ISO 1202:1981 ‘Essential
oils— Determination of f,8-cineole content’ issued bythe International Organization for Standardization
( ISO ) was adopted by the Bureau of Indian Standards on the recommendations of the Natural and
Synthetic Fragrance Materials Sectional Committee and approval of the Petroleum, Coal and Related
Products Division Council.
The text of ISO Standard has been proposed to be approved as suitable for publication as an Indian
Standard without deviations. Certain conventions are, however, not identical to those used in Indian
Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they should be
read as ‘Indian Standard’.
b) Comma (, ) has been used as a decimal marker while inIndian Standards, the current practice
is to use a point ( . ) as the decimal marker.
In this adopted standard, reference appears to the following International Standard for which Indian
Standard also exists. The corresponding Indian Standard, which is to be substituted in its place, is
listed below along with its degree of equivalence for the edition indicated. However, that International
Standard cross-referred inthis adopted ISO Standard, which has subsequently been revised, position
in respect of that latest ISO Standard has been given:
International Standard Corresponding Indian Standard Degree of Equivalence
ISO 212: 1973 Essential oils — IS 326( Part 1 ): 1984 Methods of Equivalent
Sampling sampling and test for natural and

synthetic perfumery materials:

Part 1 Sampling ( second revision)
The Technical Committee responsible for the preparation of this standard has reviewed the provisions
of the following International Standard and decided that this is acceptable for use in conjunction with
this standard:
International Standard Title
ISO 356:1996 Essential oils — Preparation of test samples
For the purpose of deciding whether a particular requirement ofthis standard iscomplied with the final
value, observed orcalculated, expressing the resultofatest oranalysis shallbe rounded offinaccordance
with IS 2:1960 ‘Rules for rounding off numerical values ( revised)’. The ~mber of significant places
retained inthe rounded off value should be the same as that of the specified value inthis standard.

-.
,.”i. , . 7
IS 326 (Part 13) :2005
ISO 1202:1981
Indian Standard
METHODS OF SAMPLING AND TEST FOR NATURAL
AND SYNTHETIC PERFUMERY MATERIALS
PART 13 DETERMINATION OF 1,8-CINEOLE CONTENT
Third Revision)
(
1 Scope and field of application 4.2 1,8-Cineole, analyticalreagentgrade.
This International Standard specifies a method for the deter- The purity of cineole shall be checked, for example, by
minationofthecontent of 1,8-cineole inessentialoils,theprin- measurement of the refractive index at 20 CC,which shallbe
cipal constituents of which are 1,8-cineole and terpene between 1,4550 and 1,4600.
hydrocarbons.
4.3 1,8-Ckeole-o-cresol complex, prepared by mixing
The method isalso applicable to the essential oilsof cajuput
equimolecular proportions (in the ratio 154,24/108,13) of the
and niaouli, provided that an appropriate table isusad;sucha cineole (4.2) and the o-creeol (4.1), and purified bycrystalliza-
tablewillbeincluded inthe sectionentitled “Requirements” in tion from light petroleum (of analytical grade), of distillation
the relevant International Standards dealing with these essen-
range between 40 and 60 ‘C. The crystallization point of the
tial oils.
complex shallnot bebelow 65,2 ‘C.
Parallel to this method, methods for the determination of
1,8-cineole in certain essential oils, by gas chromatography,
5 Apparatus
will be the subject of future International Standards.
5.1 Calibrated thermometers, mercury in glass, fulfilling
the following requirements :
2 References
— length of bulb :10 to 15mm;
ISO 212, Essential oils – Sampling.
– diameter of bulb :5 to 6 mm;
ISO356, Essential oils – Preparation of test sample.
– graduation :0,1 ‘C;
3 Principle — calibration :0,1 ‘C.
Measurement ofthe crystallizationtemperature ofamixtureof
The satofthermometers usedshallpermitthemeasurement of
essential oil and o-crasol. This temperatu r e depends on the any temperature between 20 and 60 ‘C.
1,8-cineole content of the essentialoil.

5.2 Ordinary thermometer.
4 Reagents
5.3 Test tube, about20mmdiameterandlMI mmlong.
4.1 o-Cresol, purified, anhydrous, melting-point not lass
than 30,5 ‘C.
5.4 Stout-walled test tube, about 30mm diameter and
125mm long.
As this reagent is hydroscopic, it should be stored in small,
well-stoppered bottles, or preferably in sealed flasks. These
containers should alsobe protected from light. 5.5 Apparatus assembly for determination of freezing
point. (See the figure, which isgiven asan example.)
When the o-cresolisnot inthe condition specifiedabove, itis
possibleto purify itasfollows : It consists of a widwmuthed jar or bottle of about 500 ml
capacity, provided with a bored cork or rubbar stopper into
Melt aquantity of o-cresd (analytical reagent grade), add 5 % which thestout-walled testtube (5.4) isinsmed. The testtuba
of its mass of distilled water, and allow to crystallize at a (5.3) isfitted intothe stout walled test tube (5.4) by means of
temperature of 20 to 25 ‘C. Drain the crystals, and transfer another bored corkor rubberstoppar.
them toaflaskfittedwithafractionating column. Distilthefirst
10 % (V/V) and discard it. Replace the column by a similar If necessary, the above-mentioned vessel may be filled with
one, butdry, anddktil 80 % (V/ V), the residueintheflaskba- coldwaterforcoolingpriortothe preliminarytest(see7.2) and
ing discarded. Allow the main fraction to crystallize. If its to the actualdetermination{see7.3).
melting point is still below 30,5 ‘C, repeat the distillation as
before, asmany times asisnecessarytoobtainaproduct hav- Thethermometer (5.1)isinsertedintotheteattube (5.3)sothat
ingameltingpointnotlassthan30,5 ‘C, whichiscolorless on the centraofthe mercurybulbislocatedat the centreof the li-
melting. quid.
1
IS 326 (Part 13) :2005
ISO 1202:1981
5.6 Water bath. Repeatthe determination untilthe two highestvaluesobtained
for t2do notdiffer bymorethan 0,2 ‘C.
5.7 Agitator.
If supercooling occurs, induce the crystallizationby adding a
smallcrystalof the 1,6-cineole-o-cresol complex (4.3).
6 Sampling
[ft2 is below 27,4 ‘C, repeat the determination after the addi-
tion of 5,10 gof the 1,6-cineole-o-cresol complex (4.3).
See ISO 212.
7 Procedure
8 Expression of results
7.1 Preparation of test sample
See ISO 356. The content of 1,6-cineole, corresponding to the highest
temperature observed(f2), isgivenin”the table.
7.2 Preliminary test
If 5,10 g of the 1,6-cineole-o-cresol complex (4.3) has been
added, the 1,6-cirteolecontent of the sample, expressedss a
Weigh, to the nearest0,001 g, 3 gofthe freshlypreparedtest percentage bymass,isgivenbytheformula.
sample (see7.1)inthe test tube (5.3) carefullydried, and add
2,10 g of the melted o-cresol (4.1).
2(A –50)
Placethe tube inthe apparatus (5.5) and allow the mixture to whereA isthe percentageof 1,6-cineole indicatedinthetable.
crystallizeby cooling, stirringwith the agitator (5.7).
The resultsshall be expressedto two significant figures. The
When crystallization takes place, there isa smell increase in content of 1,6-cineole, corresponding to the highest tem-
temperature. Note the maximum valueobtained, [1. perature observed(t2), isobtained, where necessary,byinter-
polationfrom the data inthe table.
7.3 Determination
Remeltthemixture, atatemperature notexceeding (1bymore
than5 ‘C, usingthe water bath (5.6). Placethe testtubs (5.3)
into the apparatus (5.5) maintained at a temperature 5 ‘C 9 Test report
below 11,checking with the ordinarythermometer (5.2).
The test reportshallstate the method usedand the resultob-
When crystallization begins, or when the temperature of the tained. It shall also mention any operating conditions not
mixturehasfallentoavalue3 ‘C belowt l, stircontinuouslyby specified in this International Standard, or regarded as op-

meansof the agitator (5.7). Take carethat th ebulbofthether- tional, sewell esany circumstancesthat might have affected

mometer isalwayscompletelyimmersed. Inducethecrystalliza- the results.
tion by rubbing the wall of the test tube with the bulb of the
thermometer. Note the maximum temperature at which tha Thetestreportshallincludealldetailsrequiredforthecomplete
mixture crystallizes,tz. identificati& of the sample.
Table – l,S-Cineole content, as a percentage by mess, aa e function of the crystallization temperature
of the essential oil-o-cresol mixture
Crystallization 1,8-Cineola Crystallization 1,6-Cinaola Crystallization 1,6-Cinaole Crystallization 1,8-Cineole
temperature contant temperature contant tamf.mrature content temperature contant
Oc % (m/m) Qc % (m/m) Oc % (m/mt Oc % {m/m)
24 45,5 32 56 40 67 46 62
25 47 33 57 41 66,5 49 64
26 46,5 34 56,5 42 m,5 50 86
27 48,5 35 60 43 72,5 51 86,5
26 50,5 36 61 44 74 52 91
29 62 37 62,5 45 76 63 93,5
30 53,5 36 63,5 46 78 64 96
31 54,5 39 65 47 80 55 98

....,.
IS 326 (Part 13) :2005
ISO 1202:1981
Approximatedimensionsinmillimetraa
I
Essential
m—
— . —
—
-— ..
—.
! —. .
20 –
.—
—-— -
Water,meltingice
————
oranyfraezingmixture
—— — — —
— ——— —.
Figure – Example of apparatua aaaambly for determination of fraezing point

3
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Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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