1、BRITISH STANDARD BS ISO 3033-2:2005 Oil of spearmint Part 2: Chinese type (80 % and 60 %) (Mentha viridis L. var. crispa Benth.), redistilled oil ICS 71.100.60BS ISO 3033-2:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 7 November 2005
2、BSI 7 November 2005 ISBN 0 580 46749 X National foreword aid enquirers to understand the text; present 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 developm
3、ents 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 en
4、titled “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. Complia
5、nce 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 dis
6、played in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments This British Standard reproduces verbatim ISO 3033-2:2005 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical
7、Committee AW/54, Essential oils, which has the responsibility to: Reference number ISO 3033-2:2005(E)INTERNATIONAL STANDARD ISO 3033-2 First edition 2005-09-01 Oil of spearmint Part 2: Chinese type (80 % and 60 %) (Mentha viridis L. var. crispa Benth.), redistilled oil Huile essentielle de menthe cr
8、pue (ou menthe verte) Partie 2: Type Chine (80 % et 60 %) (Mentha viridis L. var. crispa Benth.), huile bidistille BS ISO 3033-2:2005ii iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of prepar
9、ing 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 li
10、aison 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 ISO/IEC Directives, Part 2. The main task of
11、 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 member bodies casting a vote. Attention is
12、 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 3033-2 was prepared by Technical Committee ISO/TC 54, Essential oils. This first edition of ISO 3033-2, toget
13、her with ISO 3033-1:2005, ISO 3033-3:2005 and ISO 3033-4:2005, cancels and replaces ISO 3033:1988, which has been technically revised. ISO 3033 consists of the following parts, under the general title Oil of spearmint: Part 1: Native type (Mentha spicata L.) Part 2: Chinese type (80 % and 60 %) (Men
14、tha viridis L. var. crispa Benth.), redistilled oil Part 3: Indian type (Mentha spicata L.), redistilled oil Part 4: Scotch variety (Mentha gracilis Sole) BS ISO 3033-2:2005blank1 Oil of spearmint Part 2: Chinese type (80 % and 60 %) (Mentha viridis L. var. crispa Benth.), redistilled oil 1 Scope Th
15、is part of ISO 3033 specifies certain characteristics of the oil of spearmint, Chinese type (80 % and 60 %) (Mentha viridis L. var. crispa Benth.), redistilled oil, in order to facilitate assessment of its quality. 2 Normative references The following referenced documents are indispensable for the a
16、pplication of this document. For dated references, only the edition 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 Gen
17、eral 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 280, Essential oils Determination of refractive index ISO 592, Essential oils Determination of optical rotation ISO 875, Essentia
18、l oils Evaluation of miscibility in ethanol ISO 1271, Essential oils Determination of carbonyl value Free hydroxylamine method ISO 11024-1, Essential oils General guidance on chromatographic profiles Part 1: Preparation of chromatographic profiles for presentation in standards ISO 11024-2, Essential
19、 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 spearmint, Chinese type, redistilled essential oil obtained
20、 by steam distillation from the fresh above-ground parts of the flowering plant of Mentha viridis L. var. crispa Benth., of Lamiaceae family NOTE 1 Mentha viridis L. var. crispa Benth. is also called Mentha spicata L. var. crispa Benth. NOTE 2 It may be enriched in carvone by redistillation. NOTE 3
21、For the 80 % Chinese type, the oil obtained by steam distillation is redistilled to yield a carvone content of 80 % minimum. For the 60 % Chinese type, the oil obtained by steam distillation is redistilled to yield a carvone content of 60 % minimum. NOTE 4 For information on the CAS number, see ISO/
22、TR 21092. 4 Requirements 4.1 Appearance Clear mobile liquid. 4.2 Colour From colourless to pale yellow. BS ISO 3033-2:2005BS ISO 3033-2:2005 2 4.3 Odour Characteristic odour of carvone with a herbaceous note. 4.4 Relative density at 20 C, 20 20 d Chinese type, 80 % Chinese type, 60 % min. max. min.
23、max. 0,942 0,955 0,918 0,938 4.5 Refractive index at 20 C Chinese type, 80 % Chinese type, 60 % min. max. min. max. 1,488 1,496 1,484 1,491 4.6 Optical rotation at 20 C Chinese type, 80 % Chinese type, 60 % Between 55 and 50 Between 60 and 48 4.7 Miscibility in ethanol, 70 % (volume fraction), at 20
24、 C It shall not be necessary to use more than 3 volumes of ethanol, 70 % (volume fraction), to obtain a clear solution with 1 volume of essential oil. 4.8 Carbonyl value Minimum: 224, corresponding to a carbonyl compound content of 60 %, expressed as carvone. Minimum: 299, corresponding to a carbony
25、l compound content of 80 %, expressed as carvone. 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 compon
26、ents, indicated by the integrator, shall be as shown in Table 1. This constitutes the chromato- graphic profile of the essential oil. Table 1 Chromatographic profile Chinese type, 80 % Chinese type, 60 % Component min. % max. % min. % max. % Limonenea0,5 3,0 10,0 22,0 3-Octanol traces 0,4 0,2 0,8 Me
27、nthoneb0,8 2,0 0,8 2,0 trans-Sabinene hydrate 0,1 0,1 cis-Dihydrocarvone 2,0 4,0 2,0 4,0 Carvonec78,0 84,0 57,0 66,0 trans-Dihydrocarvyl acetate 1,5 4,0 1,5 3,5 cis-Carvyl acetate 0,1 0,3 0,1 0,3 cis-Jasmone 0,1 0,1 -Bourbonene 0,5 1,2 0,5 1,2 Viridiflorol not detectable not detectable a The limonen
28、e found is regarded to be predominantly L-limonene based on the physical testing. It is believed that there might be a small amount of D-limonene present but the exact quantity is unknown. b The menthone found is regarded to be predominantly L-menthone based on the physical testing. It is believed t
29、hat there might be a small amount of D-menthone present but the exact quantity is unknown. c The carvone found is regarded to be predominantly L-carvone based on the physical testing. It is believed that there might be a small amount of D-carvone present but the exact quantity is unknown. NOTE The c
30、hromatographic profile is normative, contrary to typical chromatograms given for information in Annex A. 4.10 Flashpoint Information on the flashpoint is given in Annex B. 5 Sampling See ISO 212. Minimum volume of test sample: 50 ml. NOTE This volume allows each of the tests specified in this part o
31、f ISO 3033 to be carried out at least once. BS ISO 3033-2:2005 3 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 Miscibility in ethanol, 70 % (volume fraction), at 20 C See ISO 875. 6.5 Carbonyl
32、 value See ISO 1271. Test portion: 1 g. Reflux time: 3 h. Relative molar mass of carvone: 150,21. 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. 4 Annex A (informative) Typical chromatograms of the analysis by g
33、as chromatography of the essential oil of spearmint, Chinese type (80 % and 60 %) (Mentha viridis L. var. crispa Benth.), redistilled oil A.1 Chinese type, 80 % BS ISO 3033-2:20055Peak identification Operating conditions 1 3-Octanol 2 Limonene 3 trans-Sabinene hydrate 4 Menthone 5 cis-Dihydrocarvone
34、 6 Carvone 7 trans-Dihydrocarvyl acetate 8 cis-Carvyl acetate 9 cis-Jasmone 10 -Bourbonene 11 Viridiflorol Column: fused silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: poly(dimethyl siloxane) (DB-1 ) Film thickness: 0,25 m Oven temperature: isothermal at 75 C for 5 min, t
35、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 8,34 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,1 l Carrier gas flow
36、rate: 1 ml/min Split ratio: 1/100 Figure A.1 Typical chromatogram of Chinese type, 80 %, taken on an apolar column BS ISO 3033-2:20056 Peak identification Operating conditions 1 Limonene 2 3-Octanol 3 Menthone 4 trans-Sabinene hydrate 5 -Bourbonene 6 cis-Dihydrocarvone 7 trans-Dihydrocarvyl acetate
37、8 Carvone 9 cis-Carvyl acetate 10 cis-Jasmone 11 Viridiflorol (not detected) Column: fused silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: poly(ethylene glycol) (DB-WAX ) Film thickness: 0,25 m Oven temperature: isothermal at 75 C for 5 min, then temperature programming fr
38、om 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 8,34 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,1 l Carrier gas flow rate: 1 ml/min Split ratio: 1/
39、100 Figure A.2 Typical chromatogram of Chinese type, 80 %, taken on a polar column BS ISO 3033-2:20057 A.2 Chinese type, 60 % Peak identification Operating conditions 1 3-Octanol 2 Limonene 3 trans-Sabinene hydrate 4 Menthone 5 cis-Dihydrocarvone 6 Carvone 7 trans-Dihydrocarvyl acetate 8 cis-Carvyl
40、acetate 9 cis-Jasmone 10 -Bourbonene 11 Viridiflorol Column: fused silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: poly(dimethyl siloxane) (DB-1 ) Film thickness: 0,25 m Oven temperature: isothermal at 75 C for 5 min, then temperature programming from 75 C to 100 C at a ra
41、te of 5 C/min, then from 100 C to 220 C at a rate of 6 C/min and isothermal at 220 C for 8,34 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,1 l Carrier gas flow rate: 1 ml/min Split ratio: 1/100 Figure A.3 Typical c
42、hromatogram of Chinese type, 60 %, taken on an apolar column BS ISO 3033-2:20058 Peak identification Operating conditions 1 Limonene 2 3-Octanol 3 Menthone 4 trans-Sabinene hydrate 5 -Bourbonene 6 cis-Dihydrocarvone 7 trans-Dihydrocarvyl acetate 8 Carvone 9 cis-Carvyl acetate 10 cis-Jasmone 11 Virid
43、iflorol (not detected) Column: fused silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: poly(ethylene glycol) (DB-WAX ) Film thickness: 0,25 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
44、 to 220 C at a rate of 6 C/min and isothermal at 220 C for 8,34 min Injector temperature: 230 C Detector temperature: 260 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,1 l Carrier gas flow rate: 1 ml/min Split ratio: 1/100 Figure A.4 Typical chromatogram of Chinese type, 6
45、0 %, taken on a polar column BS ISO 3033-2:20059 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
46、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 standardization purposes, given that: there is wide variation in the chemical composition of essential oils; the volume of the sample needed in cer
47、tain requirements would be too costly for 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 inform
48、ative annex to each International Standard, in order to meet the requirements of the interested parties. The equipment with which this value was obtained should be specified. For further information see ISO/TR 11018. B.2 Flashpoint of the essential oil of spearmint, Chinese type (80 % and 60 %), red
49、istilled oil The mean value for Chinese type, 60 %, is +58 C. The mean value for Chinese type, 80 %, is +74 C. NOTE Obtained with “Setaflash” equipment. BS ISO 3033-2:200510 Bibliography 1 ISO/TR 11018, Essential oils General guidance on the determination of flashpoint 2 ISO/TR 21092, Essential oils Characterization BS ISO 3033-2:2005