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IS 15529 (2004): Citrus fruits and derived products -Determination of essential oils content (reference method)[FAD 10: Processed Fruits and Vegetable Products]

IS 15529:2004ISO 1955:1982

*qm&mm?l?qTwlmi-Wf%-rdaami?-mmm(ktim)

Indian Standard

CITRUS FRUITS AND DERIVED PRODUCTS —DETERMINATION OF ESSENTIAL OILS CONTENT

( REFERENCE METHOD)

ICS 67.080.10

(3 BIS 2004

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

October 2004 Price Group 2

Processed Fruits and Vegetable Products Sectional Committee, FAD 10

NATIONAL FOREWORD

This Indian Standard which is identical with ISO 1955 : 1982 ‘Citrus fruits and derived

products — Determination of essential oils content ( Reference method )’ issued by the InternationalOrganization for Standardization ( ISO ) was adopted by the Bureau of Indian Standards on therecommendations of the Processed Fruits and Vegetable Products Sectional Committee and approvalof the Food and Agriculture Division Council.

In the adopted standard certain terminology and conventions are not identical to those used in theIndian Standards. Attention is particularly drawn to the following:

a) Wherever the words ‘International Standard’ appear referring to this standard, they should beread as ‘Indian Standard’.

b) Comma ( , ) has been used as a decimal marker while in Indian Standards, the current practiceis to use a point ( . ) as the decimal marker.

In reporting the result of a test or analysis made in accordance with this standard, if the finalvalue, observed or calculated, is to be rounded off, it shall be done in accordance withIS 2:1960 ‘Rules for rounding off numerical values ( revised)’.

-“1

IS 15529:2004

ISO 1955: 1982

Indian Standard

CITRUS FRUITS AND DERIVED PRODUCTS —DETERMINATION OF ESSENTIAL OILS CONTENT

( REFERENCE METHOD )

1 Scope and field of application

This International Standard specifies the reference method for

the determination of the total essential oils content of citrus

fruits and their derived products (whole fruits, fruits cut into

small pieces, skins, juices, concentrates, beverage bases

sweetened products etc. ).

2 Principle

Boiling of a test portion, diluted or undiluted, and steam en-trainment of the essential oils which are collected in a

graduated tube; after cooling, direct reading from this tube of

the volume of essential oils separated from the distillate.

Citrus fruit juices, for example, shall be used after simply stir-ring; thick, pulpy or syrupy products shall be thoroughly mixed

with an equal mass of water.

4.1.2 Products rich in essential oilsz}

Suitably dilute the test sample to obtain an essential oils con-tent of less than 0,1 ml per 100 ml or per 100 g of product.

4.1.3 Products very rich in essentialoils (used as bases for

carbonated drinks)zj

Mix thoroughly by diluting with water in the proportion in-

dicated in 4.1.2, operating in a high-speed mechanical mill in

order to avoid separation.

4.1.4 Whole fruits, fruits cut into small pieces, and skins3 Apparatus

Grind the sample finely and proceed as specified in 4.1.3.

3.1 ApparatusI), for entrainment and recovery of essentialoils, comprising a condenser and a trap terminating in a tube,of diameter 8 to 10 mm, graduated in 0,05 ml divisions, having

a capacity of 4 ml.

3.2 Flask, of capacity 3 Iitres, suitable for connection to theapparatus (3.1).

3.3 Graduated measuring cylinders, of capacity 2 Iitres.

3.4 Boiling aid.

4 Procedure

4.2 Preparation of apparatus [3.1)

Start the circulation of water through the condenser and, if

possible, moisten the inside of the condenser with a wetting

agent, for example sodium seconda~ alkylsulphate.

Fill the trap with distilled water. If possible, immerse the trap

itself in a large beaker of cold water during the test.

4.3 Test portionzl

Transfer 2 Iitres of the test sample (4.1), measured by means of

the graduated measuring cylinder (3.3) and corresponding to a

volume VO or a mass m of the product before dilution, to theflask (3.2). If necessary, add the boiling aid (3.4).

4.1 Preparation of the test sample

4.4 DeterminationNOTE – Sufficient test sample is required to provide test portions of

2 Iitres.

4.1.1 Products having low essential oils content (less

than 0,1 ml per 100 ml or per 100 g of product)

Connect the flask to the apparatus (3.1) and start heating.When the liquid begins to boil, reduce the rate of heating so

that only about one drop of distillate falls from the condenser

per second.

1) An apparatus of the modified Clevenger type is illustrated, for information only, in the annex,

2) For products which are rich, or very rich, in essential oils (4, 1.2 and 4. 1.3), it is possible to reduce the volume of the test portion to 1 Iitrer modify-

ing the capacity of the apparatus and the degree of dilution accordingly.

1

IS 15529:2004

ISO 1955: 1982

Allow to boil for 1 to 3 h; the essential oils accumulate in the

trap. When the volume of essential oils has not increased for 15

to 30 rein, stop heating and allow the trap to cool.

If possible, rinse the condenser with water from a wash-bottle,

then bring the lower boundary of the essential oils phase to the

“O” mark of the graduated tube, by running out water through

the tap, Allow the trap to drain for at least 5 rein, then read thevolume, to the nearest half-division, indicated by the upper

meniscus.

4.5 Number of determinations

Carry out two determinations on the same test sample

5 Expression of results

5.1

5.1.1

Method of calculation and formula

Samples taken by volume

The essential oils content, expressed as a percentage by

volume of product, is given by the formula

VI—X looV.

where

V. is the volume, in millilitres, of product present in thetest portion (4.3);

v, is the volume, in millilitres, of essential oils, measured

in 4.4,

5.1.2 Samples taken by mass

The essential oils content, expressed in millilitres per 100 g of

product, is given by the formula

v,— x 100m

where

m is the mass, in grams, of product present in the test poction (4.3);

VI has the same meaning as in 5.1.1.

5.1.3 Result

Take as the result the arithmetic mean of the values obtained in

the two determinations (4.5), provided that the requirement for

repeatability (see 5.2) is fulfilled.

5.2 Repeatability

The difference between the values obtained in the two deter-

minations (4.5), carried out simultaneously or in rapid succes-

sion by the same analyst, shall not exceed 5 ‘k (relative) of themean.

6 Test report

The test report shall show the method used and the result ob-

tained. It shall also mention any operating conditions not

specified in this International Standard, or regarded as op-tional, as well as any circumstances that may have influenced

the result.

The test report shall include all the information necessary for

the complete identification of the sample.

Graduated tube —

oml

Bulb

AnnexIS 15529:2004

ISO 1955:1982

apparatus (modified Clevenger type)

%

Dimensions in millimetres

IiII

@35

IIII

~

40

[

4 ml

3 ml

2 ml

1 ml

y—conden”r

)4?0>

-9

I

150

5

I

3

Bureau of Indian Standards

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Review of Indian Standards

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This Indian Standard has been developed from DOC : No. FAD 10 ( 1358 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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