1、BRITISH STANDARD BS ISO 9844:2006 Oil of bitter orange (Citrus aurantium L.)ICS 71.100.60 BS ISO 9844:2006 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 April 2006 BSI 2006 ISBN 0 580 48206 5 National foreword This British Standard repro
2、duces verbatim ISO 9844:2006 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: A list of organizations represented on this committee can be obtained on request to its sec
3、retary. 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
4、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. aid enquirers to understand the text; pr
5、esent to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an in
6、side front cover, the ISO title page, pages ii to iv, pages 1 to 11 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 9844:2006(E)INTERNATIONAL STANDARD IS
7、O 9844 Second edition 2006-03-01 Oil of bitter orange (Citrus aurantium L.) Huile essentielle dorange amre (Citrus aurantium L.) BS ISO 9844:2006ii iii Contents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Requirements 1 4.1 Appearance . 1 4.2 Colour. 1 4.3 Od
8、our . 1 4.4 Relative density at 20 C, 20 20 d . 2 4.5 Refractive index at 20 C 2 4.6 Optical rotation at 20 C . 2 4.7 Miscibility in ethanol, 90 % (volume fraction), at 20 C 2 4.8 Residue on evaporation . 2 4.9 Chromatographic profile 2 4.10 Flashpoint 2 5 Sampling 3 6 Test methods. 3 6.1 Relative d
9、ensity at 20 C, 20 20 d . 3 6.2 Refractive index at 20 C 3 6.3 Optical rotation at 20 C . 3 6.4 Miscibility in ethanol, 90 % (volume fraction), at 20 C 3 6.5 Residue on evaporation . 3 6.6 Chromatographic profile 3 7 Packaging, labelling, marking and storage 3 Annex A (informative) Typical chromatog
10、rams of the analysis by gas chromatography of the essential oil of bitter orange (Citrus aurantium L.) . 4 Annex B (informative) Flashpoint . 10 Bibliography . 11 BS ISO 9844:2006iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodi
11、es (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
12、, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the IS
13、O/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 International Standard requires approval by at least 75 % of the
14、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 9844 was prepared by Technical Committee ISO/TC 54, Essential oils.
15、 This second edition cancels and replaces the first edition (ISO 9844:1991), which has been technically revised. BS ISO 9844:20061 Oil of bitter orange (Citrus aurantium L.) 1 Scope This International Standard specifies certain characteristics of the oil of bitter orange (Citrus aurantium L.), in or
16、der to facilitate assessment of its quality. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any am
17、endments) applies. ISO/TR 210, Essential oils General rules for packaging, conditioning and storage ISO/TR 211, Essential oils General rules for labelling and marking of containers ISO 212, Essential oils Sampling ISO 279, Essential oils Determination of relative density at 20 C Reference method ISO
18、 280, Essential oils Determination of refractive index ISO 592, Essential oils Determination of optical rotation ISO 875, Essential oils Evaluation of miscibility in ethanol ISO 4715, Essential oils Quantitative evaluation of residue on evaporation ISO 11024-1, Essential oils General guidance on chr
19、omatographic profiles Part 1: Preparation of chromatographic profiles for presentation in standards ISO 11024-2, Essential oils General guidance on chromatographic profiles Part 2: Utilization of chromatographic profiles of samples of essential oils 3 Terms and definitions For the purposes of this d
20、ocument, the following terms and definitions apply. 3.1 oil of bitter orange essential oil obtained by expression, without heating, by mechanical treatment, from the pericarp of the fruit of Citrus aurantium L., of the Rutaceae family NOTE For information on the CAS number, see ISO/TR 21092. 4 Requi
21、rements 4.1 Appearance Liquid. 4.2 Colour Pale yellow to brownish green. 4.3 Odour Characteristic of the outer part of bitter orange peel. BS ISO 9844:20062 4.4 Relative density at 20 C, 20 20 d American type Equatorial type Mediterranean type min. max. min. max. min. max. 0,840 0,860 0,845 0,860 0,
22、840 0,860 4.5 Refractive index at 20 C American type Equatorial type Mediterranean type min. max. min. max. min. max. 1,472 1,476 1,473 1,478 1,472 1,476 4.6 Optical rotation at 20 C American type Equatorial type Mediterranean type + 88 to + 98 + 88 to + 95 + 88 to + 98 4.7 Miscibility in ethanol, 9
23、0 % (volume fraction), at 20 C It shall not be necessary to use more than 8 volumes of ethanol, 90 % (volume fraction), to obtain a clear solution with 1 volume of essential oil. 4.8 Residue on evaporation American type Equatorial type Mediterranean type min. max. min. max. min. max. 3,5 % 6,0 % 3,0
24、 % 6,0 % 3,5 % 6,0 % 4.9 Chromatographic profile Analysis of the essential oil shall be carried out by gas chromatography. In the chromatogram obtained, the representative and characteristic components shown in Table 1 shall be identified. The proportions of these components, indicated by the integr
25、ator, shall be as shown in Table 1. This constitutes the chromatographic profile of the essential oil. 4.10 Flashpoint Information on the flashpoint is given in Annex B. BS ISO 9844:20063 Table 1 Chromatographic profile American type Equatorial type Mediterranean type Minimum Maximum Minimum Maximum
26、 Minimum Maximum Components % % % % % % -Pinene 0,3 0,7 0,3 0,6 0,2 0,7 -Pinene 0,3 1,2 0,3 0,8 0,2 1,2 Myrcene 1,6 2,0 1,6 2,0 1,5 3,0 Limonene 93,0 95,0 92,0 95,0 93,0 95,0 Linalool 0,1 0,4 0,1 0,4 0,1 0,4 Linalyl acetate 0,6 1,0 traces 0,5 0,5 1,0 Geranyl acetate 0,1 0,3 nd a0,3 0,1 0,3 -Caryophy
27、llene traces 0,2 traces 0,1 traces 0,2 Germacrene D 0,1 0,2 traces 0,1 traces 0,2 trans- -Nerolidol traces 0,2 nd a0,3 traces 0,2 Octanal traces 0,2 nd a0,3 traces 0,1 Decanal 0,1 0,2 nd a0,2 traces 0,3 aUndetected.NOTE The chromatographic profile is normative, contrary to the typical chromatograms
28、given for information in Annex A. 5 Sampling See ISO 212. Minimum volume of test sample: 50 ml NOTE This volume allows each of the tests specified in this International Standard to be carried out at least once. 6 Test methods 6.1 Relative density at 20 C, 20 20 d See ISO 279. 6.2 Refractive index at
29、 20 C See ISO 280. 6.3 Optical rotation at 20 C See ISO 592. 6.4 Miscibility in ethanol, 90 % (volume fraction), at 20 C See ISO 875. 6.5 Residue on evaporation See ISO 4715. 6.6 Chromatographic profile See ISO 11024-1 and ISO 11024-2. 7 Packaging, labelling, marking and storage See ISO/TR 210 and I
30、SO/TR 211. BS ISO 9844:20064 Annex A (informative) Typical chromatograms of the analysis by gas chromatography of the essential oil of bitter orange (Citrus aurantium L.) A.1 Typical chromatograms of the analysis by gas chromatography of the essential oil of bitter orange (Citrus aurantium L.), Amer
31、ican type Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12 -Pinene -Pinene Octanal Myrcene Limonene Linalool Decanal Linalyl acetate Geranyl acetate -Caryophyllene Germacrene D trans- -Nerolidol Column: methyl silicone; length 50 m; internal diameter 0,2 mm Stationary phase: poly(
32、dimethyl siloxane) (SP5 ) Film thickness: 0,33 m Oven temperature: temperature programming from 60 C to 240 C at a rate of 3 C/min, then isothermal at 240 C for 30 min Injector temperature: 270 C Detector temperature: 280 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,2 l C
33、arrier gas flow rate: 1 ml/min Split ratio: 1/50 Figure A.1 Typical chromatogram taken on an apolar column BS ISO 9844:20065Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12 -Pinene -Pinene Myrcene Limonene Octanal Decanal Linalool Linalyl acetate -Caryophyllene Germacrene D Gerany
34、l acetate trans- -Nerolidol Column: Carbowax; length 50 m; internal diameter 0,2 mm Stationary phase: poly(ethylene glycol) (Suplecowax-10 ) Film thickness: 0,4 m Oven temperature: temperature programming from 60 C to 240 C at a rate of 3 C/min, then isothermal at 240 C for 30 min Injector temperatu
35、re: 270 C Detector temperature: 280 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,2 l Carrier gas flow rate: 1 ml/min Split ratio: 1/50 Figure A.2 Typical chromatogram taken on a polar column BS ISO 9844:20066 A.2 Typical chromatograms of the analysis by gas chromatography
36、 of the essential oil of bitter orange (Citrus aurantium L.), Equatorial type Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12 -Pinene -Pinene Octanal Myrcene Limonene Linalool Decanal Linalyl acetate Geranyl acetate -Caryophyllene Germacrene D trans- -Nerolidol Column: silica cap
37、illary; length 60 m; internal diameter 0,25 mm Stationary phase: poly(dimethyl siloxane) (SolGel-1ms) Film thickness: 0,25 m Oven temperature: isothermal at 60 C for 10 min, then temperature programming from 60 C to 300 C at a rate of 2 C/min, then isothermal at 300 C for 20 min Injector temperature
38、: 250 C Detector temperature: 250 C Detector: mass spectrometer Carrier gas: helium Volume injected: 0,2 l Carrier gas flow rate: 1 ml/min Split ratio: 1/60 Figure A.3 Typical chromatogram taken on an apolar column BS ISO 9844:20067Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12
39、-Pinene -Pinene Sabinene Myrcene Limonene -Phellandrene Octanal Nonanal Decanal Linalool Linalyl acetate -Caryophyllene Column: silica capillary; length 20 m; internal diameter 0,10 mm Stationary phase: poly(ethylene glycol) (Suplecowax-10 ) Film thickness: 0,20 m Oven temperature: isothermal at 50
40、C for 1 min, then temperature programming from 50 C to 200 C at a rate of 10 C/min, then isothermal for 13 min Injector temperature: 250 C Detector temperature: 250 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,2 l Carrier gas flow rate: 30 ml/min Split ratio: 1/650 Figure
41、 A.4 Typical chromatogram taken on a polar column BS ISO 9844:20068 A.3 Typical chromatograms of the analysis by gas chromatography of the essential oil of bitter orange (Citrus aurantium L.), Mediterranean type Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12 -Pinene -Pinene Myrc
42、ene Octanal Limonene Linalool Decanal Linalyl acetate Geranyl acetate -Caryophyllene Germacrene D trans- -Nerolidol Column: silica capillary; length 60 m; internal diameter 0,25 mm Stationary phase: poly(5 % diphenyl/95 % dimethyl siloxane) (DB5 MS ) Film thickness: 0,25 m Oven temperature: isotherm
43、al at 40 C for 5 min, then temperature programming from 40 C to 220 C at a rate of 4 C/min, then isothermal at 220 C for 5 min Injector temperature: 260 C Detector temperature: 280 C Detector: MS type, Full Scan (50-200) Carrier gas: helium Volume injected: 0,3 l Carrier gas flow rate: 1 ml/min Spli
44、t ratio: 1/150 Figure A.5 Typical chromatogram taken on an apolar column BS ISO 9844:20069Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 12 -Pinene -Pinene Myrcene Limonene Octanal Decanal Linalool Linalyl acetate -Caryophyllene Germacrene D Geranyl acetate trans- -Nerolidol Column
45、: silica capillary; length 60 m, internal diameter 0,32 mm Stationary phase: poly(ethylene glycol) (Suplecowax-10 ) Film thickness: 0,25 m Oven temperature: isothermal at 75 C for 4 min, then temperature programming from 75 C to 150 C at a rate of 2 C/min, then from 150 C to 240 C at a rate of 5 C/m
46、in, then isothermal at 240 C for 20 min Injector temperature: 225 C Detector temperature: 225 C Detector: MS type, Full Scan (50-200) Carrier gas: helium Volume injected: 0,03 l Carrier gas flow rate: 1,5 ml/min Split ratio: 1/100 Figure A.6 Typical chromatogram taken on a polar column BS ISO 9844:2
47、00610 Annex B (informative) Flashpoint B.1 General information For safety reasons, transport companies, insurance companies, and people in charge of safety services require information on the flashpoints of essential oils, which in most cases are flammable products. A comparative study on the releva
48、nt methods of analysis (see ISO/TR 11018) concluded that it was difficult to recommend a single apparatus for standardization purposes, given that there is a wide variation in the chemical composition of essential oils; the volume of the sample needed in certain test methods would be too costly for
49、high-priced essential oils; as there are several different types of equipment which can be used for the determination, users cannot be expected to use one specified type only. Consequently, it was decided to give a mean value for the flashpoint in an informative annex to each International Standard in order to meet t
