1、BRITISH STANDARDBS ISO 3061:2008Oil of black pepper (Piper nigrum L.)ICS 71.100.60g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS ISO 3061:2008Th
2、is British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2008 BSI 2008ISBN 978 0 580 55792 7National forewordThis British Standard is the UK implementation of ISO 3061:2008.The UK participation in its preparation was entrusted to Technical Comm
3、ittee AW/54, Essential oils.A list of organizations represented on this committee can be obtained on request to its secretary.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
4、cannot confer immunity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsReference numberISO 3061:2008(E)INTERNATIONAL STANDARD ISO3061Second edition2008-03-15Oil of black pepper (Piper nigrum L.) Huile essentielle de poivre noir (Piper nigrum L.) BS ISO 3061:2008ii i
5、iiForeword 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
6、 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 International Electrotechnical Commission (IEC) on all matte
7、rs 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 circula
8、ted 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 that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsibl
9、e for identifying any or all such patent rights. ISO 3061 was prepared by Technical Committee ISO/TC 54, Essential oils. This second edition cancels and replaces the first edition (ISO 3061:1979), which has been technically revised. BS ISO 3061:2008blank1Oil of black pepper (Piper nigrum L.) 1 Scope
10、 This International Standard specifies certain characteristics of oil of black pepper (Piper nigrum L.), with a view to facilitating the assessment of its quality. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references,
11、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 General rules for labelling and marking of containers
12、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, Essential oils Evaluation of miscibility in ethanol ISO 110
13、24-1, Essential oils General guidance on chromatographic 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 Term
14、s and definitions For the purposes of this document, the following terms and definitions apply. 3.1 essential oil of black pepper essential oil obtained by steam distillation of the whole or broken unripe fruits of Piper nigrum L. of the Piperaceae family. NOTE For information on the CAS number, see
15、 ISO/TR 210922. 4 Requirements 4.1 Appearance Clear mobile liquid. 4.2 Colour Colourless or light coloured (yellow, green, blue). 4.3 Odour Spicy, woody. 4.4 Relative density at 20 C, d2020IndiaSri Lanka Indonesia MadagascarMinimum 0,864 0,861 0,861 0,864 Maximum 0,880 0,876 0,885 0,884 BS ISO 3061:
16、20082 4.5 Refractive index at 20 C India Sri Lanka Indonesia MadagascarMinimum 1,478 1,475 1,480 1,475 Maximum 1,487 1,490 1,493 1,490 4.6 Optical rotation at 20 C India Sri Lanka Indonesia MadagascarMinimum 18 17 17 18 Maximum 7 8 6 +20 4.7 Miscibility with 95 % (volume fraction) ethanol at 20 C It
17、 shall not be necessary to use more than 3 volumes of 95 % (volume fraction) ethanol to obtain a clear solution with 1 volume of essential oil. 4.8 Chromatographic profile Analysis of the essential oil shall be carried out by gas chromatography. In the chromatogram obtained, the representative and c
18、haracteristics components shown in Table 1 shall be identified. The percentages of these components, indicated by the integrator, shall be as shown in Table 1. This constitutes the chromatographic profile of the essential oil. Table 1 Chromatographic profile India Sri Lanka Indonesia Madagascar Comp
19、onents Min. Max. Min. Max. Min. Max. Min. Max. Pinene 3 12 10 16 2,5 10 8 26 -Pinene 5 12 9 12 nda 3 7 15 Sabinene 6 15 10 17 4 10 nda 4 3-Carene 3 15 5 11 9 20 7 16 Limonene 10 17 13 16 7 12 10 25 -Elemene 0,5 3,5 0,5 3 0,5 3 0,5 4,5 -Copaene 0,5 4,5 1,5 4 0,2 1 nda 0,5 -Caryophyllene 12 29 12 21 2
20、5 40 10 25 Germacrene D nda 2 nda 1 nda 1 1 6,5 -Selinene 0,5 3,5 nda 2 3 6 1 4,5 -Selinene nda 3 0,5 2 2,5 5 0,5 3 Caryophyllene oxide nda 1 nda 1 nda 1 nda 1 a non-detectable. NOTE The chromatographic profile is normative, contrary to typical chromatograms given for information in Annex A. BS ISO
21、3061:200834.9 Flashpoint Information on the flashpoint is given in Annex B. 5 Sampling See ISO 212. Minimum volume of the final sample: 25 ml. NOTE This volume is sufficient for each of the tests specified in this International Standard to be carried out at least once. 6 Test methods 6.1 Relative de
22、nsity at 20 C, d2020See 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 with 95 % (volume fraction) ethanol at 20 C See ISO 875. 6.5 Chromatographic profile See ISO 11024-1 and ISO 11024-2. 7 Packing, labelling, marking and storage See ISO
23、/TR 210 and ISO/TR 211. BS ISO 3061:20084 Annex A (informative) Typical chromatogram of the analysis by gas chromatography of the essential oil of black pepper (Piper nigrum L.) Peak identification Operating conditions 1 -Thujene 2 -Pinene 3 Sabinene 4 -Pinene 5 Myrcene 6 -Phellandrene 7 3-Carene 8
24、Limonene + 1,8-Cineole 9 -Elemene 10 -Copaene 11 -Caryophyllene 12 -Humulene 13 Germacrene D 14 -Selinene 15 -Selinene 16 Caryophyllene oxide Column: silica capillary; length 50 m; internal diameter 0,2 mm Stationary phase: polydimethylsiloxane HP11) Film thickness: 0,25 m Oven temperature: 65 C to
25、230 C, at a rate of 2 C/min Injector temperature: 230 C Detector temperature: 250 C Detector: flame ionization type Carrier gas: hydrogen Volume injected: 0,2 l Carrier gas flow rate: 1 ml/min Split ratio: 1/100 Figure A.1 Typical chromatogram taken on an apolar column, Madagascar type 1) Example of
26、 a suitable product available commercially. This information is given for the convenience of users of this International Standard, and does not constitute an endorsement of this product by ISO. Equivalent products may be used if they can be shown to lead to the same results. BS ISO 3061:20085Peak id
27、entification Operating conditions 1 -Pinene + -Thujene 2 -Pinene 3 Sabinene 4 3-Carene 5 -Phellandrene + Myrcene 6 Limonene 7 p-Cymene 8 Terpinolene 9 -Elemene 10 -Copaene 11 -Caryophyllene + Terpinen-4-ol 12 -Humulene 13 Germacrene D 14 -Selinene 15 -Selinene 16 Caryophyllene oxide Column: silica c
28、apillary; length 50 m; internal diameter 0,2 mm Stationary phase: poly(ethylene glycol) Carbowax 2) Film thickness: 0,25 m Oven temperature: 65 C to 230 C, at a rate of 10 C/min Injector temperature: 230 C Detector temperature: 250 C Detector: flame ionization type Carrier gas: hydrogen Volume injec
29、ted: 0,2 l Carrier gas flow rate: 1,1 ml/min Split ratio: 1/100 Figure A.2 Typical chromatogram taken on a polar column, Madagascar type 2) Example of a suitable product available commercially. This information is given for the convenience of users of this International Standard, and does not consti
30、tute an endorsement of this product by ISO. Equivalent products may be used if they can be shown to lead to the same results. BS ISO 3061:20086 Peak identification Operating conditions 1 -Thujene 2 -Pinene 3 Sabinene 4 -Pinene 5 Myrcene 6 -Phellandrene 7 3-Carene 8 Limonene + 1,8-Cineole 9 -Elemene
31、10 -Copaene 11 -Caryophyllene 12 -Humulene 13 Germacrene D 14 -Selinene 15 -Selinene 16 Caryophyllene oxide Column: silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: polydimethylsiloxane HP-13) Film thickness: 0,25 m Oven temperature: isothermal at 60 C for 1 min, then progr
32、amming temperature from 60 C to 240 C at a rate of 2 C/min, then isothermal at 240 C for 10 min Injector temperature: 250 C Detector temperature: 300 C Detector: flame ionization type Carrier gas: hydrogen Volume injected: 0,5 l Carrier gas flow rate: 100 ml/min Split ratio: 1/100 Figure A.3 Typical
33、 chromatogram taken on an apolar column, Indian type 3) Example of a suitable product available commercially. This information is given for the convenience of users of this International Standard, and does not constitute an endorsement of this product by ISO. Equivalent products may be used if they
34、can be shown to lead to the same results. BS ISO 3061:20087Peak identification Operating conditions 1 -Pinene + -Thujene 2 -Pinene 3 Sabinene 4 3-Carene 5 -Phellandrene + Myrcene 6 Limonene 7 p-Cymene 8 Terpinolene 9 -Elemene 10 -Copaene 11 -Caryophyllene + Terpinen-4-ol 12 -Humulene 13 Germacrene D
35、 14 -Selinene 15 -Selinene 16 Caryophyllene oxide Column: silica capillary; length 30 m; internal diameter 0,25 mm Stationary phase: poly(ethylene glycol) Innowax4) Film thickness: 0,25 m Oven temperature: isothermal at 60 C for 1 min, then programming temperature from 60 C to 240 C at a rate of 2 C
36、/min, then isothermal at 240 C for 10 min Injector temperature: 250 C Detector temperature: 300 C Detector: flame ionization type Carrier gas: hydrogen Volume injected: 0,5 l Carrier gas flow rate: 100 ml/min Split ratio: 1/100 Figure A.4 Typical chromatogram taken on a polar column, Indian type 4)
37、Example of a suitable product available commercially. This information is given for the convenience of users of this International Standard, and does not constitute an endorsement of this product by ISO. Equivalent products may be used if they can be shown to lead to the same results. BS ISO 3061:20
38、088 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 relevant
39、 methods of analysis (see ISO/TR 110181) 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 requirements would be too costly for
40、high priced essential oils; as there are several different types of equipment which can be used for the determination, users cannot be expected to purchase one specified type only. Consequently, it was decided to give a mean value for the flashpoint annexed to each International Standard, for inform
41、ation, in order to meet the requirements of the interested parties. The equipment with which this value was obtained has to be specified. For further information, see ISO/TR 110181. B.2 Flashpoint of the essential oil of black pepper (Piper nigrum L.) The mean value is +48 C (obtained using Madagasc
42、ar type). NOTE Obtained with “Setaflash” equipment. BS ISO 3061:20089Bibliography 1 ISO/TR 11018, Essential oils General guidance on the determination of flashpoint 2 ISO/TR 21092, Essential oils Characterization BS ISO 3061:2008BS ISO 3061:2008BSI389 Chiswick High RoadLondonW4 4ALBSI British Standa
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