BS ISO 17412-2008 Oil of bitter fennel (Foeniculum vulgare Mill ssp vulgare var vulgare)《香精油苦茴香(Foeniculum vulgare Mill ssp vulgare var vulgare)》.pdf

1、BRITISH STANDARDBS ISO 17412:2007Oil of bitter fennel (Foeniculum vulgare Mill. ssp. vulgare var. vulgare)ICS 71.100.60g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g

2、42g43g55g3g47g36g58BS ISO 17412:2007This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2008 BSI 2008ISBN 978 0 580 54628 0National forewordThis British Standard is the UK implementation of ISO 17412:2007.The UK participation in its pr

3、eparation was entrusted to Technical Committee 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 applic

4、ation.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsReference numberISO 17412:2007(E)INTERNATIONAL STANDARD ISO17412First edition2007-12-01Oil of bitter fennel (Foeniculum vulgare Mill. ssp. vulgare var. vu

5、lgare) Huile essentielle de fenouil amer (Foeniculum vulgare Mill. ssp. vulgare var. vulgare) BS ISO 17412:2007ii iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Stand

6、ards 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 ta

7、ke 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 technical committees i

8、s 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 drawn to the possibili

9、ty 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 17412 was prepared by Technical Committee ISO/TC 54, Essential oils. BS ISO 17412:2007blank1Oil of bitter fennel (Foeniculum vulgare

10、 Mill. ssp. vulgare var. vulgare) 1 Scope This International Standard specifies certain characteristics of the oil of bitter fennel (Foeniculum vulgare Mill. ssp. vulgare var. vulgare), in order to facilitate assessment of its quality. 2 Normative references The following referenced documents are in

11、dispensable 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 amendments) applies. ISO/TR 210, Essential oils General rules for packaging, conditioning and storage ISO/TR 21

12、1, Essential oils General rules for labelling and marking 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

13、 ISO 875, Essential oils Evaluation of miscibility in ethanol ISO 1041, Essential oils Determination of freezing point ISO 11024-1, Essential oils General guidance on chromatographic profiles Part 1: Preparation of chromatographic profiles for presentation in standards ISO 11024-2, Essential oils Ge

14、neral 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 bitter fennel essential oil obtained by steam distillation, with or

15、 without subsequent rectification, of the fruits and aerial parts of Foeniculum vulgare Mill. ssp. vulgare var. vulgare of the Apiaceae family; some authors use the name Foeniculum vulgare Miller ssp. vulgare var. amara NOTE For information on CAS number, see ISO/TR 21092. 4 Requirements 4.1 Appeara

16、nce trans-Anethole type Phellandrene type Clear liquid or crystalline mass Mobile liquid 4.2 Colour trans-Anethole type Phellandrene type Colourless to pale yellow liquid Pale yellow to intense yellow liquid 4.3 Odour trans-Anethole type Phellandrene type Characteristic, recalling that of anethole S

17、weet, herbaceous, characteristic 4.4 Taste Sweet with a bitter after-taste. BS ISO 17412:20072 4.5 Relative density at 20 C, 2020d trans-Anethole type Phellandrene type Min. 0,944 0,877 Max. 0,973 0,920 4.6 Refractive index at 20 C trans-Anethole type Phellandrene type Min. 1,514 1,487 Max. 1,538 1,

18、501 4.7 Optical rotation at 20 C trans-Anethole type Phellandrene type Min. +11 +42 Max. +29 +68 4.8 Miscibility in ethanol at 20 C trans-Anethole type Phellandrene type It shall not be necessary to use more than 10 volumes of ethanol 85 % (volume fraction) to obtain a clear solution with 1 volume o

19、f essential oil. It shall not be necessary to use more than 2 volumes of ethanol 90 % (volume fraction) to obtain a clear solution with 1 volume of essential oil. 4.9 Freezing point trans-Anethole type Min. +3 C Max. +10 C NOTE Freezing points higher than 10 C often indicate adulteration with anisee

20、d oil or pure anethole. The freezing point is not a relevant requirement for the phellandrene type, due to the low anethole content. 4.10 Chromatographic profile Analysis of the essential oil shall be carried out by gas chromatography. There are two types of bitter fennel oil: trans-anethole and phe

21、llandrene. In the chromatogram obtained, the representative and characteristics components shown in Table 1 and Table 2 shall be identified. The proportions of these components, indicated by the integrator, shall be as shown in Table 1 and Table 2. This constitutes the chromatographic profile of the

22、 essential oil. Table 1 trans-Anethole type chromatographic profile Component Min. % Max.% -Pinene 2,0 11,0 -Pinene trace 1,0 Myrcene 0,5 2,0 -Phellandrene trace 8,5 Limonene 1,0 6,0 Fenchone 10,0 25,0 Methyl chavicol (estragole) 1,0 6,0 trans-Anethole 50,0 78,0 cis-Anethole nd a0,5 Anisaldehyde tra

23、ce 1,0 1-(4-Methoxyphenyl)propan-2-one (anise ketone) nd a1,0 NOTE The chromatographic profile is normative, contrary to typical chromatograms given for information in Annex A. aNon-detectable. BS ISO 17412:20073Table 2 Phellandrene type chromatographic profile Component Min.% Max.% -Pinene 2,0 8,0

24、-Pinene 1,0 4,0 Myrcene 1,0 12,0 -Phellandrene 8,0 25,0 Limonene 8,0 30,0 Fenchone 7,0 16,0 Methyl chavicol (estragole) 2,0 7,0 trans-Anethole 15,0 30,0 cis-Anethole trace0,5 Anisaldehyde trace 0,3 1-(4-Methoxyphenyl)propan-2-one (anise ketone) trace 0,05 NOTE The chromatographic profile is normativ

25、e, contrary to typical chromatograms given for information in Annex A. 4.11 Flashpoint Information on the flashpoint is given in Annex B. 5 Sampling See ISO 212. The minimum volume of test sample is 50 ml. NOTE The volume allows each of the tests specified in this International Standard to be carrie

26、d out at least once. 6 Test methods 6.1 Relative density at 20 C, 2020d 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 at 20 C See ISO 875. 6.5 Freezing point See ISO 1041. 6.6 Chromatographic profile See ISO 11024-1 and IS

27、O 11024-2. 7 Packaging labelling, marking and storage See ISO/TR 210 and ISO/TR 211. BS ISO 17412:20074 Annex A (informative) Typical chromatograms of the analysis by gas chromatography of the essential oil of bitter fennel (Foeniculum vulgare Mill. ssp. vulgare var. vulgare) Peak identification Ope

28、rating conditions 1 -Pinene 2 -Pinene 3 Myrcene 4 -Phellandrene 5 Limonene 6 Fenchone 7 Methyl chavicol (estragole) 8 Anisaldehyde 9 cis-Anethole 10 trans-Anethole 11 1-(4-Methoxyphenyl)propan-2-one Column: FSOT, length 50 m, internal diameter 0,25 mm Stationary phase: methyl silicone BP11) Film thi

29、ckness: 0,20 m Oven temperature: isothermal at 65 C for 1 min, then temperature programming from 65 C to 180 C at a rate of 2 C/min and then isothermal at 180 C for 10 min Injector temperature: 200 C Detector temperature: 300 C Detector: flame ionization type Carrier gas: hydrogen Volume injected: 0

30、,1 l Carrier gas flow rate: 3,5 ml/min Split ratio: 1:50 Figure A.1 Typical chromatogram of trans-anethole type taken using an apolar column 1) Example of a suitable product available commercially. This information is given for the convenience of users of this International Standard and does not con

31、stitute an endorsement by ISO of this product. BS ISO 17412:20075Peak identification Operating conditions 1 -Pinene 2 -Pinene 3 Myrcene 4 -Phellandrene 5 Limonene 6 Fenchone 7 Methyl chavicol (estragole) 8 cis-Anethole 9 trans-Anethole 10 Anisaldehyde 11 1-(4-Methoxyphenyl)propan-2-one Column: FSOT,

32、 length 60 m, internal diameter 0,53 mm Stationary phase: polyethylene glycol DB-Wax2) Film thickness: 1,0 m Oven temperature: isothermal at 50 C for 5 min, then temperature programming from 50 C to 220 C at a rate of 3 C/min and then isothermal at 220 C for 15 min Injector temperature: 220 C Detect

33、or temperature: 220 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,02 l Carrier gas flow rate: 4 ml/min Split ratio: nil Figure A.2 Typical chromatogram of trans-anethole type taken using a polar column 2) Example of a suitable product available commercially. This informati

34、on is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. BS ISO 17412:20076 Peak identification Operating conditions 1 -Pinene 2 -Pinene 3 Myrcene 4 -Phellandrene 5 Limonene 6 Fenchone 7 Methyl chavicol (estragole) 8 cis-A

35、nethole + anisaldehyde 9 trans-Anethole 10 1-(4-Methoxyphenyl)propan-2-one Column: capillary, fused silica, length 30 m, internal diameter 0,25 mm Stationary phase: 5 % diphenyl-95 % dimethyl siloxane SPB-53) Film thickness: 0,25 m Oven temperature: temperature programming from 55 C to 100 C at a ra

36、te of 5,5 C/min, then temperature programming from 100 C to 200 C at a rate of 8 C/min and then isothermal at 200 C for 10 min Injector temperature: 250 C Detector temperature: 250 C Detector: flame ionization type Carrier gas: helium Volume injected: 0,1 l Carrier gas flow rate: 1 ml/min Split rati

37、o: 1:100 Figure A.3 Typical chromatogram of phellandrene type taken using an apolar column 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 by ISO of this product. BS

38、ISO 17412:20077Peak identification Operating conditions 1 -Pinene 2 -Pinene 3 Myrcene 4 -Phellandrene 5 Limonene 6 Fenchone 7 Methyl chavicol (estragole) 8 cis-Anethole 9 trans-Anethole 10 Anisaldehyde 11 1-(4-Methoxyphenyl)propan-2-one Column: capillary, fused silica, length 60 m, internal diameter

39、 0,25 mm Stationary phase: polyethylene glycol SP-10004) Film thickness: 0,25 m Oven temperature: temperature programming from 95 C to 190 C at a rate of 4 C/min and then isothermal at 190 C for 8 min Injector temperature: 250 C Detector temperature: 250 C Detector: flame ionization type Carrier gas

40、: nitrogen Volume injected: 0,1 l Carrier gas flow rate: 1 ml/min Split ratio: 1:100 Figure A.4 Typical chromatogram of phellandrene type taken using a polar column 4) Example of a suitable product available commercially. This information is given for the convenience of users of this International S

41、tandard and does not constitute an endorsement by ISO of this product. BS ISO 17412:20078 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

42、 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 standardization purposes, given that: there is a wide variation in the chemical composition of essential o

43、ils; the volume of the sample needed in certain 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

44、mean value for the flashpoint (see Table B.1) 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 obtained should be specified. For further information see ISO/TR 11018. B.2 Flashpoint of the esse

45、ntial oil of bitter fennel trans-Anethole type Phellandrene type +63 C +48 C NOTE Obtained with Pensky-Martens5)equipment. NOTE Obtained with Setaflash6)equipment. _ 5) Example of a suitable product available commercially. This information is given for the convenience of users of this International

46、Standard and does not constitute an endorsement by ISO of this product. 6) 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 by ISO of this product. BS ISO 17412:20079Bibl

47、iography 1 ISO/TR 11018:1997, Essential oils General guidance on the determination of flashpoint 2 ISO/TR 21092, Essential oils Characterization BS ISO 17412:2007BS ISO 17412:2007BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible fo

48、r preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter.RevisionsBritish Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or ed

49、itions.It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: +44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400.BSI offers members an individual updating service called PLUS which e