1、BRITISH STANDARD BS ISO 3809:2004 Oil of lime (cold pressed), Mexican type Citrus aurantifolia (Christm.) Swingle, obtained by mechanical means ICS 71.100.60 BS ISO 3809:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 27 May 2004 BSI 27
2、May 2004 ISBN 0 580 43816 3 National foreword This British Standard reproduces verbatim ISO 3809:2004 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 organiza
3、tions 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”,
4、 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
5、immunity from legal obligations. 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
6、them in the UK. 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. Am
7、endments issued since publication Amd. No. Date Comments Reference number ISO 3809:2004(E) OSI 4002INTERNATIONAL STANDARD ISO 3809 Third edition 2004-05-15 Oil of lime (cold pressed), Mexican type Citrus aurantifolia (Christm.) Swingle, obtained by mechanical means Huile essentielle de limette (expr
8、ime froid), type Mexique Citrus aurantifolia (Christm.) Swingle, obtenue par procds mcaniques BSISO3809:2004IS:9083 O4002(E) DPlcsid Fremia ihTs PDF file may ctnoian emdebt dedyfepcaes. In ccaocnadrw eith Aebods licensilop gnic,y this file mairp eb ynted iv roweb detu slahl ton ide ebtlnu deess the
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13、hi n Switlrez dnaii ISO 4002 Allr ithgsr esedevrBSISO3809:2004IS:9083 O4002(E) I SO 4002 All irthgs ersedevr iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards
14、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 pa
15、rt 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 ISO/IEC Directives, Part 2. The main task of technical committees is to
16、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 member bodies casting a vote. Attention is drawn to the possibility th
17、at 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 3809 was prepared by Technical Committee ISO/TC 54, Essential oils. This third edition cancels and replaces the second edition (ISO 3809:
18、1987), which has been technically revised. BSISO3809:2004INTENRATIONAL TSANDADR IS:9083 O4002(E)I SO 4002 All irthgs ersedevr 1Oil of lime (cold pressed), Mexican type Citrus aurantifolia (Christm.) Swingle, obtained by mechanical means 1 Scope This International Standard specifies certain charact-
19、eristics of the oil of lime (cold pressed), Mexican type Citrus aurantifolia (Christm.) Swingle, in order to facilitate assessment of its quality. 2 Normative references The following referenced documents are indispen- sable for the application of this document. For dated references, only the editio
20、n cited applies. For undated references, the latest edition of the referenced document (including any amendments) 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, Essent
21、ial oils Sampling ISO 279, Essential oils Determination of relative density at 20 C Reference method ISO 280, Essential oils Determination of refractive index ISO 592, Essential oils Determination of optical rotation ISO 1271, Essential oils Determination of carbonyl value Free hydroxylamine method
22、ISO 4715, Essential oils Quantitative evaluation of residue on evaporation ISO 4735, Oils of citrus Determination of CD value by ultraviolet spectrophotometric analysis ISO 11024-1, Essential oils General guidance on chromatographic profiles Part 1: Preparation of chromatographic profiles for presen
23、tation 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 document, the following terms and definitions apply. 3.1 oil of lime (cold presse
24、d), Mexican type (type A) essential oil obtained by centrifuging the emulsion of water, juice and oil obtained by crushing the whole fruits of Citrus aurantifolia (Christm.) Swingle, of the Rutaceae family 3.2 oil of lime (cold pressed), Mexican type (type B) essential oil obtained by grating and/or
25、 squeezing the peel of fruits of Citrus aurantifolia (Christm.) Swingle, of the Rutaceae family, in the presence of water, followed by centrifuging the resulting emulsion of water and oil NOTE 1 The principal areas of production are Mexico, the countries of Central America and the islands of the Car
26、ibbean. NOTE 2 For information on the CAS number, see ISO/TR 21092. BSISO3809:2004IS:9083 O4002(E) 2 I SO 4002 All irthgs ersedevr4 Requirements 4.1 Appearance Type A Type B Clear liquid, in which a waxy precipitate is usually present 4.2 Colour Type A Type B From yellowish green to green Green to d
27、ark green 4.3 Odour Type A Type B Characteristic of fresh lime peel. Fresh citrus lime-like odour Fresh, with a note reminiscent of the pericarp. Fresh citrus lime odour with a pronounced juicy characteristic 4.4 Relative density at 20 C, 20 20 d Type A Type B min. max. min. max. 0,875 0 0,884 0 0,8
28、80 0 0,888 0 4.5 Refractive index at 20 C Type A Type B min. max. min. max. 1,482 0 1,486 0 1,484 0 1,488 0 4.6 Optical rotation at 20 C Type A Type B Between +35,0 and +41,0 This determination is often not possible because oils of this type are intensely coloured BSISO3809:2004IS:9083 O4002(E) I SO
29、 4002 All irthgs ersedevr 34.7 Carbonyl value Type A Type B min. max. min. max. 16 (corresponding to 4,5 % of carbonyl compounds expressed as citral) 31 (corresponding to 8,5 % of carbonyl compounds expressed as citral) 18 (corresponding to 5 % of carbonyl compounds expressed as citral) 35 (correspo
30、nding to 9,5 % of carbonyl compounds expressed as citral) 4.8 Residue on evaporation Type A Type B min. max. min. max. 10,0 % 14,5 % 13,0 % 19,0 % 4.9 CD value Type A Type B min. min. 18,2 23,6 4.10 Chromatographic profile Analysis of the essential oil shall be carried out by gas chromatography. In
31、the chromatogram obtained, the representative and characteristic components shown in Tables 1 and 2, for type A and type B respectively, shall be identified. The proportions of these components, indicated by the integrator, shall be as shown in Tables 1 and 2. This constitutes the chromatographic pr
32、ofile of the essential oil. 4.11 Flashpoint Information on the flashpoint is given in Annex B. 5 Sampling See ISO 212. Minimum volume of test sample: 25 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
33、 density at 20 C, 20 20 d See ISO 279. 6.2 Refractive index at 20 C See ISO 280. 6.3 Optical rotation at 20 C See ISO 592. 6.4 Carbonyl value See ISO 1271. Test portion: 5 g. Standing time: 15 min. 6.5 Residue on evaporation See ISO 4715. Test portion: 5 g. Evaporation time: 6 h. BSISO3809:2004IS:90
34、83 O4002(E) 4 I SO 4002 All irthgs ersedevr6.6 CD value See ISO 4735. Point B: 370 nm approximately. Maximum value: 312 nm to 315 nm approximately. Point A: 280 nm approximately. Dilution of 0,025 g of oil in 100 ml of 90 % ethanol (volume fraction). Table 1 Chromatographic profile (type A) Componen
35、t Minimum % Maximum % -Pinene 2,0 3,0 Sabinene 1,8 4,0 -Pinene 18,0 24,0 Myrcene 1,0 2,0 p-Cymene 0,5 Limonene 42,0 50,0 -Terpinene 8,0 11,0 Terpinen-4-ol 0,2 0,6 -Terpineol 0,2 0,6 n-Decanal 0,05 0,3 Neral 1,2 2,0 Geranial 2,0 3,0 Neryl acetate 0,1 0,35 Geranyl acetate 0,2 0,4 -Caryophyllene 0,5 1,
36、5 -Bergamotene 1,0 1,9 -Farnesene 0,75 1,75 -Bisabolene 1,0 1,5 NOTE 1 The chromatographic profile is normative, contrary to typical chromatograms given for information in Annex A. NOTE 2 Expressed oils of lime may contain furo- coumarins. The bergapten content should be less than 2 000 mg/kg. 6.7 C
37、hromatographic profile See ISO 11024-1 and ISO 11024-2. 7 Packaging, labelling, marking and storage See ISO/TR 210 and ISO/TR 211. Table 2 Chromatographic profile (type B) Component Minimum % Maximum % -Pinene 1,7 2,0 Sabinene 2,0 3,0 -Pinene 17,0 19,0 Myrcene 1,4 1,8 Neryl acetate 0,0 0,25 -Terpine
38、ne 9,0 9,7 Terpinen-4-ol 0,2 0,6 p-Cymene 0,5 Limonene 38,0 44,0 -Terpineol 0,3 0,6 n-Decanal 0,15 0,35 Neral 2,0 2,5 Geranial 3,0 3,7 Geranyl acetate 0,3 0,6 -Caryophyllene 1,5 1,9 -Bergamotene 0,5 0,7 -Bisabolene 4,0 4,5 NOTE 1 The chromatographic profile is normative, contrary to typical chromato
39、grams given for information in Annex A. NOTE 2 Expressed oils of lime may contain furo- coumarins. The bergapten content should be less than 2 000 mg/kg. BSISO3809:2004IS:9083 O4002(E) I SO 4002 All irthgs ersedevr 5Annex A (informative) Typical chromatograms of the analysis by gas chromatography of
40、 the essential oil of lime (cold pressed), Mexican type Citrus aurantifolia (Christm.) Swingle, obtained by mechanical means Peak identification Operating conditions 1 -Pinene 2 Sabinene 3 -Pinene 4 Myrcene 5 p-Cymene 6 Limonene 7 -Terpinene 8 Terpinen-4-ol 9 -Terpineol 10 n-Decanal 11 Neral 12 Gera
41、nial 13 Neryl acetate 14 Geranyl acetate 15 -Caryophyllene 16 -Bergamotene 17 -Farnesene 18 -Bisabolene Column: capillary; length 30 m; internal diameter 0,20 mm Stationary phase: poly(5 % diphenyl/95 % dimethyl siloxane) (SP-5 ) Film thickness: 20 m Oven temperature: isothermal at 75 C for 5 min, t
42、hen temperature programming from 75 C to 100 C at a rate of 5 C/min, then from 100 C to 220 C at a rate of 6 C/min, and isothermal at 220 C for 8,5 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 1 l Carrier gas flow ra
43、te: 206,84 kPa Split ratio: 1/100 Figure A.1 Typical chromatogram taken on an apolar column (type A) BSISO3809:2004IS:9083 O4002(E) 6 I SO 4002 All irthgs ersedevrPeak identification Operating conditions 1 -Pinene 2 -Pinene 3 Sabinene 4 Myrcene 5 Limonene 6 -Terpinene 7 p-Cymene 8 -Bergamotene 9 -Ca
44、ryophyllene 10 Neral 11 -Terpineol 12 -Bisabolene 13 Neryl acetate Column: capillary; length 30 m; internal diameter 0,20 mm Stationary phase: poly(ethylene glycol) (Carbowax ) Film thickness: 20 m Oven temperature: isothermal at 75 C for 5 min, then temperature programming from 75 C to 100 C at a r
45、ate of 5 C/min, then from 100 C to 220 C at a rate of 6 C/min and isothermal at 220 C for 8,5 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 1 l Carrier gas flow rate: 206,84 kPa Split ratio: 1/100 Figure A.2 Typical c
46、hromatogram taken on a polar column (type A) BSISO3809:2004IS:9083 O4002(E) I SO 4002 All irthgs ersedevr 7Peak identification Operating conditions 1 -Pinene 2 Sabinene 3 -Pinene 4 Myrcene 5 p-Cymene 6 Limonene 7 -Terpinene 8 Terpinen-4-ol 9 -Terpineol 10 n-Decanal 11 Neral 12 Geranial 13 Neryl acet
47、ate 14 Geranyl acetate 15 -Caryophyllene 16 -Bergamotene 17 -Farnesene 18 -Bisabolene Column: capillary; length 30 m; internal diameter 0,20 mm Stationary phase: poly(5 % diphenyl/95 % dimethyl siloxane) (SP-5 ) Film thickness: 20 m Oven temperature: isothermal at 75 C for 5 min, then temperature pr
48、ogramming from 75 C to 100 C at a rate of 5 C/min, then from 100 C to 220 C at a rate of 6 C/min, and isothermal at 220 C for 8,5 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 1 l Carrier gas flow rate: 206,84 kPa Spl
49、it ratio: 1/100 Figure A.3 Typical chromatogram taken on an apolar column (type B) BSISO3809:2004IS:9083 O4002(E) 8 I SO 4002 All irthgs ersedevrPeak identification Operating conditions 1 -Pinene 2 -Pinene 3 Sabinene 4 Myrcene 5 Limonene 6 -Terpinene 7 p-Cymene 8 -Bergamotene 9 -Caryophyllene 10 Nera
