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BRITISH STANDARD BS ISO

855:2003

Oil of lemon
[Citrus limon (L.)
Burm. f.], obtained by
expression

Confirmed
ICS 71.100.60 May 2009

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BS ISO 855:2003

National foreword
This British Standard reproduces verbatim ISO 855:2003 and implements it as
the UK national standard.
The UK participation in its preparation was entrusted to Technical Committee
AW/54, Essential oils, which has the responsibility to:

— aid enquirers to understand the text;

— present to the responsible international/European committee any


enquiries on the interpretation, or proposals for change, and keep the
UK interests informed;
— monitor related international and European developments and
promulgate them in the UK.

A list of organizations represented on this committee can be obtained on


request to its secretary.
Cross-references
The British Standards which implement international publications referred to
in this document may be found in the BSI Catalogue under the section entitled
“International Standards Correspondence Index”, or by using the “Search”
facility of the BSI Electronic Catalogue or of British Standards Online.
This publication does not purport to include all the necessary provisions of a
contract. Users are responsible for its correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, the ISO title page,
pages ii and iii, a blank page, pages 1 to 10, an inside back cover and a back
cover.
The BSI copyright notice displayed in this document indicates when the
document was last issued.

Amendments issued since publication


This British Standard was
published under the authority Amd. No. Date Comments
of the Standards Policy and
Strategy Committee on
17 December 2003

© BSI 17 December 2003

ISBN 0 580 43115 0


BS ISO 855:2003

INTERNATIONAL ISO
STANDARD 855

Second edition
2003-12-01

Oil of lemon [Citrus limon (L.) Burm. f.],


obtained by expression
Huile essentielle de citron [Citrus limon (L.) Burm. f.], obtenue par
expression

Reference number
ISO 855:2003(E)

© OSI 3002
BS ISO O3002(E)
IS:558 855:2003

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ii © ISO— 3002 Allr ihgtsser edevr


BS ISOO3002(E)
IS:558 855:2003

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Interna-
tional Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an Interna-
tional Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 855 was prepared by Technical Committee ISO/TC 54, Essential oils.

This second edition cancels and replaces the first edition (ISO 855:1981), which has been technically revised.

Together with the revised versions of ISO 3519 and ISO 8899, it will also cancel and replace ISO 7611:1985.

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BS ISO 855:2003

blank
BS ISO 855:2003
INTENRATIONAL TSANDADR IS:558 O3002(E)

Oil of lemon [Citrus limon (L.) Burm. f.], obtained by expression

1 Scope ISO 1271, Essential oils — Determination of car-


bonyl value — Free hydroxylamine method
This International Standard specifies certain
characteristics of the oil of lemon [Citrus limon (L.) ISO 4715, Essential oils — Quantitative evaluation
Burm. f.], obtained by expression, in order to facilitate of residue on evaporation
assessment of its quality.
ISO 4735, Oils of Citrus — Determination of CD
value by ultraviolet spectrometric analysis
2 Normative references
ISO 11024-1, Essential oils — General guidance on
The following referenced documents are indispen- chromatographic profiles — Part 1: Preparation of
sable for the application of this document. For dated chromatographic profiles for presentation in stan-
references, only the edition cited applies. For un- dards
dated references, the latest edition of the referenced
document (including any amendments) applies. ISO 11024-2, Essential oils — General guidance on
chromatographic profiles — Part 2: Utilization of
ISO/TR 210, Essential oils — General rules for chromatographic profiles of samples of essential oils
packaging, conditioning and storage

ISO/TR 211, Essential oils — General rules for la- 3 Terms and definitions
belling and marking of containers
For the purposes of this document, the following
ISO 212, Essential oils — Sampling terms and definitions apply.

ISO 279, Essential oils — Determination of relative 3.1


density at 20 ºC — Reference method oil of lemon
essential oil obtained by expression, without the aid
ISO 280, Essential oils — Determination of refrac- of heat and with or without previous separation of
tive index the pulp and the peel, from the fresh fruit of Citrus
limon (L.) Burm. f., of the Rutaceae family, growing
ISO 592, Essential oils — Determination of optical mainly in Argentina, Brazil, Cyprus, Italy, Ivory
rotation Coast, Spain, South Africa and United States.

NOTE For information on the CAS number, see


ISO 875, Essential oils — Evaluation of miscibility in
ISO/TR 21092.
ethanol

ISO 1242, Essential oils — Determination of acid


value

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BS ISO O3002(E)
IS:558 855:2003

4 Requirements

4.1 Appearance

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
Mobile, clear liquid, which may become cloudy by lowering the temperature

4.2 Colour

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
From pale yellow to dark green

4.3 Odour

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
Characteristic of fresh lemon pericarp

20
4.4 Relative density, at 20 °C, d 20

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
0,851 0,857 0,849 0,854 0,849 0,858 0,850 0,858 0,845 0,854

4.5 Refractive index at 20 °C

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
1,473 0 1,476 0 1,473 0 1,476 0 1,473 0 1,476 0 1,473 0 1,476 0 1,473 0 1,479 0

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BS ISOO3002(E)
IS:558 855:2003

4.6 Optical rotation at 20 °C

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
Between +57° Between +67° Between +57° Between +57° Between +57°
and +66° and +78° and +66° and +66° and +70°

4.7 Residue on evaporation

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
1,75 3,90 n.a. n.a. 1,50 3,90 1,50 3,90 1,50 4,00

4.8 Acid value (max.)

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
2 2 2 2 2

4.9 Carbonyl value

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
8,0 14,0 6,25 12,0 11,0 17,0 11,0 17,0 6,0 17,0

4.10 CD value

American type Mediterranean type Equatorial


Ivory Coast,
Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
0,20 n.a. 0,20 n.a. 0,40 0,90 0,45 0,90 0,20 0,96

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BS ISO O3002(E)
IS:558 855:2003

4.11 Chromatographic profile 6.4 Residue on evaporation

Analysis of the essential oil shall be carried out by See ISO 4715.
gas chromatography. In the chromatogram obtained, Test portion: 5 g.
the representative and characteristics components Evaporation time: 5 h.
shown in Table 1 shall be identified. The proportions
of these components, indicated by the integrator,
6.5 Acid value
shall be as shown in Table 1. This constitutes the
chromatographic profile of the essential oil.
See ISO 1242.
4.12 Flashpoint Test portion: 2 g.

Information on the flashpoint is given in Annex B. 6.6 Carbonyl value

See ISO 1271.


5 Sampling
Test portion: 10 g.
See ISO 212. Period of standing: 15 min.
Relative molecular mass: 152,23.
Minimum volume of test sample: 25 ml.
6.7 CD value
NOTE This volume allows each of the tests specified
in this International Standard to be carried out at least
once. See ISO 4735.
Point B: 285 nm approximately.
6 Test methods Maximum value (point D): 315 nm approximately.
Point A: 365 nm approximately.
20
6.1 Relative density at 20 °C, d 20 Dilution of 0,25 g of oil in 100 ml of 95 % (volume
fraction) ethanol.
See ISO 279.
6.8 Chromatographic profile
6.2 Refractive index at 20 °C
See ISO 11024-1 and ISO 11024-2.
See ISO 280.
7 Packaging, labelling, marking and
6.3 Optical rotation at 20 °C storage
See ISO 592. See ISO/TR 210 and ISO/TR 211.

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BS ISOO3002(E)
IS:558 855:2003

Table 1 — Chromatographic profile


Values in percent

American type Mediterranean type Equatorial


Ivory Coast,
Components Coastal type Desert type Spain Italy
Brazil
min. max. min. max. min. max. min. max. min. max.
α-Thujene 0,2 0,5 0,2 0,5 0,2 0,5 0,2 0,5 0,2 0,5

α-Pinene 1,5 2,5 1,4 2,5 1,5 3,0 1,5 3,0 1,4 3,0
Sabinene 1,5 2,5 1,3 2,5 1,5 3,0 1,5 3,0 1,4 3,0
β-Pinene 9,0 14,0 10,0 13,0 10,0 16,5 10,0 16,5 7,0 16,0
p-Cymene 0,05 0,35 0,01 0,35 traces 0,40 0,05 0,35 0,05 0,35

Limonenea 63,0 70,0 70,0 80,0 60,0 70,0 60,0 68,0 59,0 75,0

γ-Terpinene 8,3 9,5 6,5 8,0 8,0 12,0 8,0 12,0 6,0 12,0

α-Terpineol 0,10 0,25 0,06 0,15 0,09 0,35 0,10 0,30 0,00 0,40
Neral 0,6 0,9 0,3 0,6 0,4 1,0 0,6 1,2 0,2 1,2
Geranial 1,0 2,0 0,5 0,9 0,6 2,0 0,8 2,0 0,5 2,0
β-Bisabolene 0,45 0,9 0,40 0,7 0,45 0,9 0,45 0,9 0,20 0,9
Neryl acetate 0,35 0,60 0,30 0,50 0,30 0,60 0,20 0,50 0,10 0,50
Geranyl acetate 0,20 0,50 0,10 0,30 0,20 0,65 0,30 0,65 traces 0,30
NOTE The chromatographic profile is normative, contrary to typical chromatograms given for information in Annex A.
a This is regarded as being completely D-limonene by independent chemical and physical analysis.

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BS ISO O3002(E)
IS:558 855:2003

Annex A
(informative)

Typical chromatograms of the analysis by gas chromatography of the


essential oil of lemon [Citrus limon (L.) Burm. f.]

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IS:558 855:2003

Peak identification Operating conditions


1 α-Thujene Column: fused silica capillary; length 30 m; internal diameter 0,25 mm
2 α-Pinene Stationary phase: poly(dimethyl siloxane) (DB-1®)
3 Sabinene Thickness of film: 0,25 µm
4 β-Pinene Oven temperature: temperature programming from 75 °C to 100 °C, at a rate of
5 Myrcene 5 °C/min and from 100 °C to 220 °C at 6 °C/min
6 p-Cymene Injector temperature: 230 °C
7 Limonene Detector temperature: 260 °C
8 γ-Terpinene Detector: flame ionization type
9 α-Terpineol Carrier gas: helium
10 Neral Volume injected: 0,2 µl
11 Geranial Carrier gas flow rate: 1 ml/min
12 Neryl acetate Split ratio: 100/1
13 Geranyl acetate
14 β-Caryophyllene
15 α-Bergamotene
16 β-Bisabolene

Figure A.1 — Typical chromatogram taken on a non-polar column

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BS ISO O3002(E)
IS:558 855:2003

Peak identification Operating conditions


1 α-Pinene Column: fused silica capillary; length 30 m; internal diameter 0,25 mm
2 β-Pinene Stationary phase: poly(ethylene glycol) (Carbowax 20 M®)
3 Sabinene Thickness of film: 0,25 µm
4 Limonene Oven temperature: temperature programming from 75 °C to 100 °C at a rate of
5 γ-Terpinene 5 °C/min and from 100 °C to 220 °C at 6 °C/min
6 Neral Injector temperature: 230 °C
7 α-Terpineol Detector temperature: 260 °C
8 β-Bisabolene Detector: flame ionization type
9 Neryl acetate Carrier gas: helium
10 Geranial Volume injected: 0,2 µl
11 Geranyl acetate Carrier gas flow rate: 1 ml/min
Split ratio: 100/1

Figure A.2 — Typical chromatogram taken on a polar column

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BS ISOO3002(E)
IS:558 855:2003

Annex B
(informative)

Flashpoint

B.1 General information Consequently, it was decided to give a mean value for
the flashpoint in an informative annex to each
For safety reasons, transport companies, insurance International Standard, for information, in order to
companies and people in charge of safety services meet the requirements of the interested parties.
require information on the flashpoints of essential oils,
which in most cases are flammable products. The equipment with which this value was obtained
should be specified.
A comparative study on the relevant methods of
analysis (see ISO/TR 11018) concluded that it was For further information, see ISO/TR 11018.
difficult to recommend a single apparatus for
standardization purposes, given that: B.2 Flashpoint of oil of lemon
 there is wide variation in the chemical compo- The mean value is +46 °C.
sition of essential oils;
NOTE Obtained with “Luchaire” equipment.
 the volume of the sample needed for certain
requirements would be too costly for high-
priced essential oils;

 as there are several different types of equip-


ment which can be used for the determination,
users cannot be expected to use one specified
type only.

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BS ISO O3002(E)
IS:558 855:2003

Bibliography

[1] ISO 3519, Oil of lime (Citrus aurantifolia (Christm.) Swingle), obtained by distillation

[2] ISO 7611, Oils of lemon and petitgrain citronnier, and oil of lime obtained by a mechanical process —
Determination of citral (neral + geranial) content — Gas chromatographic method on capillary columns

[3] ISO 8899, Oil of lemon petitgrain [Citrus limon (L.) Burm. f.]

[4] ISO/TR 11018, Essential oils — General guidance on the determination of flashpoint

[5] ISO/TR 21092:—1), Essential oils — Characterization

1) To be published.

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BS ISO
855:2003
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