1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationEssential oil of mandarin, Italian type (Citrus reticulataBlanco)BS ISO 3528:2012National forewordThis British Standard is the UK implementation of ISO 3528:2012.The UK participa
2、tion in its preparation was entrusted to Technical CommitteeAW/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 c
3、orrect application. The British Standards Institution 2012Published by BSI Standards Limited 2012 ISBN 978 0 580 68035 9 ICS 71.100.60Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and S
4、trategy Committee on 31 July 2012.Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS ISO 3528:2012 ISO 2012Essential oil of mandarin, Italian type (Citrus reticulata Blanco)Huile essentielle de mandarine, type Italie (Citrus reticulata Blanco)INTERNATIONAL STANDARDISO35
5、28Third edition2012-07-01Reference numberISO 3528:2012(E)BS ISO 3528:2012ISO 3528:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electro
6、nic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb w
7、ww.iso.orgPublished in SwitzerlandBS ISO 3528:2012ISO 3528:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references . 13 Terms and definitions . 14 Requirements . 14.1 Appearance . 14.2 Colour . 24.3 Odour 24.4 Relative density at 20 C, d2020. 24.5 Refractive i
8、ndex at 20 C . 24.6 Optical rotation at 20 C . 24.7 Residue on evaporation . 24.8 Miscibility with 90 % (volume fraction) ethanol at 20 C . 24.9 Acid value 34.10 Chromatographic profile . 34.11 Flashpoint 35 Sampling 36 Test methods 36.1 Relative density at 20 C, d2020. 36.2 Refractive index at 20 C
9、 . 46.3 Optical rotation at 20 C . 46.4 Residue on evaporation . 46.5 Miscibility with 90 % (volume fraction) ethanol at 20 C . 46.6 Acid value 46.7 Chromatographic profile . 47 Packaging, labelling, marking and storage 4Annex A (informative) Typical chromatograms of the analysis by gas chromatograp
10、hy of the essential oil of mandarin, Italian type (Citrus reticulata Blanco) . 5Annex B (informative) Flashpoint . 8Bibliography . 9BS ISO 3528:2012ISO 3528:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodi
11、es). 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 committee has been established has the right to be represented on that committee. International organizations, governmental and
12、non-governmental, in liaison 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, Pa
13、rt 2.The main task of 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
14、 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 identifying any or all such patent rights.ISO 3528 was prepared by Technical Committee ISO/TC 54, Essential oils.This third edition canc
15、els and replaces the second edition (ISO 3528:1997), which has been technically revised. It also incorporates the Technical Corrigendum ISO 3528:1997/Cor.1:1998.iv ISO 2012 All rights reservedBS ISO 3528:2012INTERNATIONAL STANDARD ISO 3528:2012(E)Essential oil of mandarin, Italian type (Citrus retic
16、ulata Blanco)1 ScopeThis International Standard specifies certain characteristics of the oil of mandarin, Italian type (Citrus reticulata Blanco) in order to facilitate assessment of its quality.2 Normative referencesThe following referenced documents are indispensable for the application of this do
17、cument. 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 storageISO/TR 211, Essential oils General rules for labellin
18、g and marking of containersISO 212, Essential oils SamplingISO 279, Essential oils Determination of relative density at 20 C Reference methodISO 280, Essential oils Determination of refractive indexISO 592, Essential oils Determination of optical rotationISO 875, Essential oils Evaluation of miscibi
19、lity in ethanolISO 1242, Essential oils Determination of acid valueISO 11024 (all parts), Essential oils General guidance on chromatographic profiles3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply3.1oil of mandarin, Italian typeessential oil obtain
20、ed by expression, without the aid of heat and with or without previous separation of the pulp and the peel, from the fresh fruit of Citrus reticulata Blanco of the Rutaceae familyNOTE For information on CAS number, see ISO/TR 210922.4 Requirements4.1 AppearanceClear mobile liquid. ISO 2012 All right
21、s reserved 1BS ISO 3528:2012ISO 3528:2012(E)4.2 ColourThe colour depends on the season of harvest.Green Yellow RedLight green to dark green, with a blue fluorescenceLight yellow to dark orange, with a blue fluorescenceReddish to dark red, with a blue fluorescence4.3 OdourThe odour from the fresh per
22、icarp of the fruit is characteristic.4.4 Relative density at 20 C, d2020Green Yellow RedMinimum 0,847 0,846 0,844Maximum 0,855 0,854 0,8534.5 Refractive index at 20 CGreen Yellow RedMinimum 1,473 2 1,472 6 1,472 2Maximum 1,475 8 1,475 3 1,474 64.6 Optical rotation at 20 CGreen Yellow RedMinimum +69
23、+69 +70Maximum +75 +76 +794.7 Residue on evaporationGreen Yellow RedMinimum 1,90 % mass fraction 1,80 % mass fraction 1,40 % mass fractionMaximum 3,90 % mass fraction 3,90 % mass fraction 3,30 % mass fraction4.8 Miscibility with 90 % (volume fraction) ethanol at 20 CIt shall not be necessary to use
24、more than 10 volumes of 90 % (volume fraction) ethanol at 20 C to obtain an opalescent solution with 1 volume of essential oil.2 ISO 2012 All rights reservedBS ISO 3528:2012ISO 3528:2012(E)4.9 Acid valueGreen Yellow RedMaximum 2,0 2,0 2,04.10 Chromatographic profileCarry out the analysis of the esse
25、ntial oil by gas chromatography. Identify in the chromatogram obtained, the representative and characteristic components shown in Table 1. The proportions of these components, indicated by the integrator, shall be as shown in Table 1. This constitutes the chromatographic profile of the essential oil
26、.Table 1 Chromatographic profileComponentGreen Yellow RedMinimum Maximum Minimum Maximum Minimum Maximum% % % % % %-Pinene 1,6 2,7 1,6 2,7 1,8 3-Pinene 1 2 1 2 1,2 2Myrcene 1,4 2 1,4 2 1,5 2n-Octanal 0,08 0,14 0,05 0,14 0,03 0,08p-Cymene n.d.a0,4 n.d.a0,5 n.d.a0,8-Terpinene 17 22 16 22 16 22Limonene
27、 65 74 65 75 65 75Linalool 0,05 0,2 0,05 0,2 0,03 0,2n-Decanal 0,04 0,14 0,04 0,14 0,04 0,12Methyl N-methylanthranilate 0,4 0,7 0,3 0,6 0,3 0,6-Sinensal 0,2 0,5 0,2 0,5 0,1 0,5NOTE The chromatographic profile is normative, contrary to typical chromatograms given for information in Annex A.aNot detec
28、table.4.11 FlashpointInformation on the flashpoint is given in Annex B.5 SamplingSampling shall be performed in accordance with ISO 212.Minimum volume of test sample: 50 mlNOTE This volume allows each of the tests specified in this International Standard to be carried out at least once.6 Test method
29、s6.1 Relative density at 20 C, d2020Determine the relative density in accordance with ISO 279. ISO 2012 All rights reserved 3BS ISO 3528:2012ISO 3528:2012(E)6.2 Refractive index at 20 CDetermine the refractive index in accordance with ISO 280.6.3 Optical rotation at 20 CDetermine the optical rotatio
30、n in accordance with ISO 592.6.4 Residue on evaporationDetermine the residue on evaporation in accordance with ISO 1242.Test portion: 5 gEvaporation time: 6 h6.5 Miscibility with 90 % (volume fraction) ethanol at 20 CDetermine the miscibility in accordance with ISO 875.6.6 Acid valueDetermine the ac
31、id value in accordance with ISO 1242.6.7 Chromatographic profileDetermine the chromatographic profile in accordance with ISO 11024.7 Packaging, labelling, marking and storageThese items shall be in accordance with ISO/TR 210 and ISO/TR 211.NOTE This essential oil is particularly susceptible to oxidi
32、zation. 4 ISO 2012 All rights reservedBS ISO 3528:2012ISO 3528:2012(E)Annex A (informative) Typical chromatograms of the analysis by gas chromatography of the essential oil of mandarin, Italian type (Citrus reticulata Blanco) ISO 2012 All rights reserved 5BS ISO 3528:2012ISO 3528:2012(E)Peak identif
33、ication Operating conditions1 -Thujene2 -Pinene3 Camphene4 Sabinene5 -Pinene6 Myrcene7 n-Octanal8 -Terpinene9 p-Cymene10 Limonene11 -Phellandrene12 -Terpinene13 (Z)-Sabinene hydrate14 Terpinolene15 Linalool16 n-Nonanal17 Citronellal18 Terpinen-4-ol19 -Terpineol20 n-Decanal21 Thymol22 Methyl N-methyl
34、anthranilate23 -Caryophyllene24 (E,E)-Farnesene25 -Sinensaln countst timeColumn: capillary, fused silica, 50 m long and 0,25 mm internal diameterFilm thickness: 1,00 mStationary phase: poly (5 % diphenyl95 % dimethylsiloxane)Oven temperature:isothermal at 46 C for 1 min and temperature programming f
35、rom 46 C to 100 C at a rate of 5 C/minthen from 100 C to 230 C at a rate of 2 C/min, isothermal at 230 C for 13 minInjector temperature: 230 CDetector temperature: 250 CDetector 1: flame ionization typeDetector 2: quadrupole mass spectrometer 40 amu to 300 amuCarrier gas: helium 99,999 % volume frac
36、tionInjection volume: 0,1 lCarrier gas flow rate: 1,5 ml/min constant flowSplit ratio: 1:50Figure A.1 Typical chromatogram taken on an apolar column6 ISO 2012 All rights reservedBS ISO 3528:2012ISO 3528:2012(E)Peak identification Operating conditions1 -Thujene2 -Pinene3 Camphene4 Sabinene5 -Pinene6
37、Myrcene7 n-Octanal8 -Terpinene9 p-Cymene10 Limonene11 -Phellandrene12 -Terpinene13 (Z)-Sabinene hydrate14 Terpinolene15 Linalool16 n-Nonanal17 Citronellal18 Terpinen-4-ol19 -Terpineol20 n-Decanal21 Thymol22 Methyl N-methylanthranilate23 -Caryophyllene24 (E,E)-Farnesene25 -Sinensaly relative abundanc
38、et timeColumn: capillary, fused silica, 60 m long and 0,25 mm internal diameterFilm thickness: 0,25 mStationary phase: polyethyleneglycol CW 20M1)Oven temperature:isothermal at 46 C for 1 min and temperature programming from 46 C to 100 C at a rate of 5 C/minthen from 100 C to 230 C at a rate of 2 C
39、/min, isothermal at 230 C for 13 minInjector temperature: 230 CDetector temperature: 250 CDetector 1: flame ionization typeDetector 2: quadrupole mass spectrometer 40 amu to 300 amuCarrier gas: helium 99,999 % volume fractionInjection volume: 0,1 lCarrier gas flow rate: 2,2 ml/min constant flowSplit
40、 ratio: 1:50Figure A.2 Typical chromatogram taken on a polar column1) CW 20M is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product. ISO 2012 All rights reserved
41、 7BS ISO 3528:2012ISO 3528:2012(E)Annex B (informative) FlashpointB.1 General informationFor 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 compar
42、ative study on the relevant 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 requiremen
43、ts 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 annexed to each International
44、 Standard, for information, 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 mandarin, Italian typeThe mean value is +48 C.NOTE Obtained w
45、ith Pensky-Martens2)equipment.2) Equipment available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product.8 ISO 2012 All rights reservedBS ISO 3528:2012ISO 3528:2012(E)Bibliography1 ISO/TR 11018, Essential
46、 oils General guidance on the determination of flashpoint2 ISO/TR 21092, Essential oils Characterization ISO 2012 All rights reserved 9BS ISO 3528:2012This page deliberately left blankThis page deliberately left blankBSI is the independent national body responsible for preparing British Standards an
47、d other standards-related publications, information and services. It presents the UK view on standards in Europe and at the international level. BSI is incorporated by Royal Charter. British Standards and other standardisation products are published by BSI Standards Limited.British Standards Institu
48、tion (BSI)raising standards worldwideBSI389 Chiswick High Road London W4 4AL UKTel +44 (0)20 8996 9001Fax +44 (0)20 8996 Standards and PASs are periodically updated by amendment or revision. Users of British Standards and PASs should make sure that they possess the latest amendments or editions.It
49、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 British Standards would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside frontcover. Similary for PASs, please notify BSI Customer Services.Tel:
