1、BRITISH STANDARD BS ISO 3053:2004 Oil of grapefruit (Citrus paradisi Macfad.), obtained by expression ICS 71.100.60 BS ISO 3053:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 8 October 2004 BSI 8 October 2004 ISBN 0 580 44563 1 National
2、 foreword This British Standard reproduces verbatim ISO 3053:2004 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 organizations represented on this committee
3、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 o
4、f 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. aid
5、 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. Summary of pages Thi
6、s document comprises a front cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 7 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 Re
7、ference number ISO 3053:2004(E)INTERNATIONAL STANDARD ISO 3053 Second edition 2004-10-01 Oil of grapefruit (Citrus paradisi Macfad.), obtained by expression Huile essentielle de pamplemousse (Citrus paradisi Macfad.), obtenue par expression BSISO3053:2004ii BSISO3053:2004ISO 3053:2004(E) iiiForeword
8、 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
9、 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 el
10、ectrotechnical 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 t
11、he 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
12、identifying any or all such patent rights. ISO 3053 was prepared by Technical Committee ISO/TC 54, Essential oils. This second edition cancels and replaces the first edition (ISO 3053:1975), which has been technically revised. BSISO3053:2004blank BSISO3053:2004INTENRATIONAL TSANDADR IS:3503 O4002(E)
13、1Oil of grapefruit (Citrus paradisi Macfad.), obtained by expression 1 Scope This International Standard specifies certain characteristics of the oil of grapefruit (Citrus paradisi Macfad.), obtained by expression, in order to facilitate assessment of its quality. 2 Normative references The followin
14、g referenced documents are indispen- sable for the application of this document. For dated references, only the edition cited applies. For un- dated references, the latest edition of the referenced document (including any amendments) applies. ISO/TR 210, Essential oils General rules for packaging, c
15、onditioning and storage ISO/TR 211, Essential oils General rules for la- belling and marking of containers ISO 212, Essential oils Sampling ISO 279, Essential oils Determination of relative density at 20 C Reference method ISO 280, Essential oils Determination of refrac- tive index ISO 592, Essentia
16、l oils Determination of optical rotation ISO 1271, Essential oils Determination of car- bonyl value Free hydroxilamine method ISO 4715, Essential oils Quantitative evaluation of residue on evaporation ISO 11024-1, Essential oils General guidance on chromatographic profiles Part 1: Preparation of chr
17、omatographic profiles for presentation in stan- dards 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 a
18、pply. 3.1 oil of grapefruit essential oil obtained, without heating, by mechani- cal processing from the external part of the pericarp of the fruit of Citrus paradisi Macfad., of the Ruta- ceae family NOTE 1 The principal areas of production are the United States, Israel, Argentina, Cyprus, South Af
19、rica and Brazil. NOTE 2 For information on the CAS number, see ISO/TR 21092. 4 Requirements 4.1 Appearance Clear liquid with possible traces of precipitated waxes. 4.2 Colour Yellow to pinkish orange. 4.3 Odour A fresh citrus-like odour, characteristic of grapefruit peel. 4.4 Relative density at 20
20、C, 20 20 d Minimum: 0,852 0 Maximum: 0,860 0 4.5 Refractive index at 20 C Minimum: 1,474 0 Maximum: 1,479 0 BSISO3053:2004ISO 3053:2004(E) 2 4.6 Optical rotation at 20 C Between + 91 and + 96. 4.7 Total content of aldehydes Minimum: 0,28 % Maximum: 2,00 % expressed as decanal (M r= 156,3) 4.8 Residu
21、e on evaporation Maximum: 10 % 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
22、the integrator, shall be as shown in Table 1. This constitutes the chromato- graphic profile of the essential oil. See ISO 7609. Table 1 Chromatographic profile Component Minimum % Maximum % -Pinene 0,2 0,6 Sabinene 0,1 0,6 -Pinene 0,05 0,2 Myrcene 1,5 2,5 Limonene a92 96 n-Octanal 0,2 0,8 n-Nonanal
23、 0,04 0,1 n-Decanal 0,1 0,6 Neral 0,02 0,04 -Caryophyllene 0,2 0,5 Nootkatone 0,01 0,8 NOTE The chromatographic profile is normative, contrary to typical chromatograms given for information in Annexes A and B. aIn accordance with the present knowledge on this oil and the results of several physical
24、tests carried out in this International Standard, it can be assured that this component is, predominantly, D-limonene. 4.10 Flashpoint Information on the flashpoint is given in Annex C. 5 Sampling See ISO 212. Minimum volume of test sample: 25 ml. NOTE This volume allows each of the tests specified
25、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 20 C See ISO 280. 6.3 Optical rotation at 20 C See ISO 592. 6.4 Total aldehyde content See ISO 1271. Test portion: 10 g Reflux time: 0,5 h 6.5 Res
26、idue on evaporation See ISO 4715. Test portion: 3 g Evaporation time: 5 h 6.6 Chromatographic profile See ISO 11024-1 and ISO 11024-2. 7 Packaging, labelling, marking and storage See ISO/TR 210 and ISO/TR 211. BSISO3053:2004ISO 3053:2004(E) 3Annex A (informative) Typical chromatograms of the analysi
27、s by gas chromatography of the essential oil of grapefruit (Citrus paradisi Macfad.), obtained by expression Peak identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 -Pinene -Pinene Sabinene n-Octanal Myrcene Limonene n-Nonanal n-Decanal Neral -Caryophyllene Nootkatone Column: capillary; len
28、gth 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 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 isother
29、mal at 220 C for 8,5 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Carrier gas flow rate: 22 ml/min Volume injected: 1 l Split ratio: 1/100 Figure A.1 Typical chromatogram taken on an apolar column BSISO3053:2004ISO 3053:2004(E) 4 Pea
30、k identification Operating conditions 1 2 3 4 5 6 7 8 9 10 11 -Pinene Sabinene -Pinene Myrcene Limonene n-Octanal n-Nonanal n-Decanal Neral -Caryophyllene Nootkatone Column: capillary; length 30 m; internal diameter 0,20 mm Stationary phase: poly(ethylene glycol) (Carbowax ) Film thickness: 20 m Ove
31、n temperature: isothermal at 75 C for 5 min, then 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: he
32、lium Carrier gas flow rate: 22 ml/min Volume injected: 1 l Split ratio: 1/100 Figure A.2 Typical chromatogram taken on a polar column BSISO3053:2004ISO 3053:2004(E) 5Annex B (informative) Typical chromatogram of the analysis by high-pressure liquid chroma- tography (HPLC) of the essential oil of gra
33、pefruit (Citrus paradisi Macfad.), obtained by expression Peak identification 1 Bergamottin 2 Aurapten 3 Osthol 4 Bergapten 5 Epoxybergamottin 6 Epoxyaurapten 7 Isomeranzin 8 Meranzin Operating conditions Column: C 18 bonded silica (Sherisorb 5 ods or equivalent 1) ) Eluents: A: water/acetic acid (9
34、8 %/2 %) B: acetonitrile Flow rate 1,5 ml/min Volume injected: 5,0 l UV detection: wavelength of 280 nm from t = 0 min to t = 20 min and then wavelength of 313 nm until the end Figure B.1 Typical chromatogram of the analysis by HPLC 1) Sherisorb 5 ods is an example of a suitable product available co
35、mmercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. BSISO3053:2004ISO 3053:2004(E) 6 Annex C (informative) Flashpoint C.1 General information For safety reasons, transport companies, insuranc
36、e 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 relevant methods of analysis (see ISO/TR 11018) concluded that it was difficult to recommend a single apparatus for sta
37、ndardization purposes, given that: there is a wide variation in the chemical composition of essential oils; 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 dete
38、rmination, 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 the requirements of the interested parties. The equipment with which this value was obtain
39、ed should be specified. For further information, see ISO/TR 11018. C.2 Flashpoint of the essential oil of grapefruit The mean value is + 43 C. NOTE Obtained with “Luchaire” equipment. BSISO3053:2004ISO 3053:2004(E) 7Bibliography 1 ISO/TR 11018:1997, Essential oils General guidance on the determinati
40、on of flashpoint 2 ISO/TR 21092:2004, Essential oils Characterization BSISO3053:2004BS ISO 3053:2004 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Eu
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