© ISO 2017 Essential oil of Melaleuca, terpinen 4 ol type (Tea Tree oil) Huile essentielle de Melaleuca, type terpinén 4 ol (huile essentielle de Tea Tree) INTERNATIONAL STANDARD ISO 4730 Third editio[.]
INTERNATIONAL STANDARD ISO 4730 Third edition 2017-02 Melaleuca, terpinen-4- Essential oil of ol type (Tea Tree oil) Huile essentielle de Melaleuca, type terpinén-4-ol (huile essentielle de Tea Tree) Reference number ISO 4730:2017(E) © ISO 2017 ISO 4730:2017(E) COPYRIGHT PROTECTED DOCUMENT © ISO 2017, Published in Switzerland All rights reserved Unless otherwise specified, no part o f this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission Permission can be requested from either ISO at the address below or ISO’s member body in the country o f the requester ISO copyright o ffice Ch de Blandonnet • CP 401 CH-1214 Vernier, Geneva, Switzerland Tel +41 22 749 01 11 Fax +41 22 749 09 47 copyright@iso.org www.iso.org ii © ISO 2017 – All rights reserved ISO 4730:2017(E) Contents Page Foreword iv Scope Normative references Terms and definitions Requirements Additional information Sampling 5.1 5.2 Flashpoint Enantiomeric distribution Packaging, labelling, marking and storage Annex A (informative) Typical chromatograms of the analysis by gas chromatography of the essential oil of , terpinen-4-ol type (Tea Tree oil) Melaleuca Annex B (informative) Flashpoint Annex C (informative) Enantiomeric distribution — General information Bibliography 10 © ISO 2017 – All rights reserved iii ISO 4730:2017(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies) The work o f 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 non-governmental, in liaison with ISO, also take part in the work ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f electrotechnical standardization The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part In particular the different approval criteria needed for the di fferent types o f ISO documents should be noted This document was dra fted in accordance with the editorial rules of the ISO/IEC Directives, Part (see www.iso org/directives) Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f patent rights ISO shall not be held responsible for identi fying any or all such patent rights Details o f any patent rights identified during the development o f the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso org/patents) Any trade name used in this document is in formation given for the convenience o f users and does not constitute an endorsement For an explanation on the voluntary nature o f standards, the meaning o f ISO specific terms and expressions related to formity assessment, as well as in formation about ISO’s adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso org/iso/foreword html This document was prepared by Technical Committee ISO/TC 54, Essential oils This third edition cancels and replaces the second edition (ISO 4730:2004), which has been technically revised iv © ISO 2017 – All rights reserved INTERNATIONAL STANDARD Essential oil of ISO 4730:2017(E) Melaleuca, terpinen-4-ol type (Tea Tree oil) Scope This document specifies certain characteristics o f the essential oil o f Melaleuca , terpinen-4-ol type (Tea Tree oil), in order to facilitate assessment o f its quality Normative references The following documents are re ferred to in the text in such a way that some or all o f their content constitutes requirements o f this document For dated re ferences, only the edition cited applies For undated re ferences, the latest edition o f the re ferenced document (including any amendments) applies ISO/TS 210, Essential oils — General rules for packaging, conditioning and storage ISO/TS 211, Essential oils — General 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, Essential oils — Evaluation of miscibility in ethanol ISO 11024 (all parts), Essential oils — General guidance on chromatographic profiles Terms and definitions For the purposes o f this document, the following terms and definitions apply ISO and IEC maintain terminological databases for use in standardization at the following addresses: — IEC Electropedia: available at http://www.electropedia org/ — ISO Online browsing platform: available at http://www iso org/obp 3.1 essential oil of Tea Tree oil Melaleuca, terpinen-4-ol type essential oil obtained by steam distillation o f the leaves and terminal branchlets o f Melaleuca alternifolia (Maiden et Betche) Cheel or of M linariifolia Sm Note to entry: For in formation on the CAS number, see ISO/TR 21092 © ISO 2017 – All rights reserved ISO 4730:2017(E) Requirements Essential oil of Melaleuca Table 4.1 , terp inen- 4- o l typ e (Tea Tree o il) s hall meet the requirements as given in Table — Requirements for the essential oil of Characteristics Melaleuca, terpinen-4-ol type (Tea Tree oil) Requirements Appearance Colour Odour ISO test method Clear, mobile liquid — — — ISO 279 ISO 280 ISO 592 C olou rle s s to p a le yel low Characteristic 0,885 to 0,906 1,475 to 1,482 20 d20 Rel ative den s ity at ° C , Re frac tive i nde x at ° C Optical rotation B e twe en +7 ° a nd +1 ° I t s h a l l no t b e ne ce s s a r y to u s e more th a n volumes o f ethanol, 85 % (volume M iscibility in ethanol 85 % (volume frac tio n) C h r o m a t o g r a p h i c p r o f i l ISO 875 fraction) , to obtain a clear solution with volume of essential oil at ° C e C arr y out the ana lys i s o f the e s s entia l oi l b y ga s ch romato graphy D e term i ne the ch romato graph ic pro fi le in accorda nce with the ISO 102 s erie s I denti fy in the ch romato gram ob tai ne d , the representative and characteristic components shown in Table The proportions of these components, Table of the essential oil i nd ic ate d b y the i ntegrator, sh a l l b e a s shown i n T a b l e — C h Components α-P i nene Sabinene α-Ter pi nene Limonene p- C ymene 1,8-Cineole γ-Ter pi nene Terpinolene Terpinen-4-ol α-Ter pi ne ol Aromadendrene L e dene (s yn vi r id i flo rene) δ - C ad i nene Globulol Vi r id i floro l a r o T h i s s titute s the ch romato graph ic pro fi le m a t o g r a p h i c p r o f i l e Min Max % % 1,0 traces a 6,0 0,5 0,5 traces a 14,0 1,5 35,0 2,0 0,2 0,1 0,2 traces a traces a 4,0 3,5 12,0 1,5 8,0 10,0 28,0 5,0 48,0 5,0 3,0 3,0 3,0 1,0 1,0 trace s : < , % NO T E T he ch ro m ato g rap h ic p ro fi le i s no r m ati ve , co ntra r y to t yp ic a l chromatograms given for information in Annex A © ISO 2017 – All rights reserved ISO 4730:2017(E) Additional information 5.1 Flashpoint I n formation on the fla shp oi nt i s given i n Annex B 5.2 Enantiomeric distribution Information concerning enantiomeric distribution is given in Annex C Sampling Sampling shall be performed in accordance with ISO 212 Minimum volume of test sample is 50 ml NO TE T h i s volu me a l lows e ach o f the te s ts s p e c i fie d i n th i s c u ment to b e c a r r ie d out at le a s t o nce Packaging, labelling, marking and storage These items shall be in accordance with ISO/TS 210 and ISO/TS 211 © ISO 2017 – All rights reserved ISO 4730:2017(E) Annex A (informative) Typical chromatograms of the analysis by gas chromatography of the essential oil of , terpinen-4-ol type (Tea Tree oil) Melaleuca © ISO 2017 – All rights reserved ISO 4730:2017(E) 10 11 12 13 14 15 16 17 18 19 a P e a k i d e n t i f i c a t i o Operating conditions n fus ed α-Thuj ene C o lumn: α- Pinene S tatio nary p has e: p o ly(dimethyl s iloxane) (OV- 1 Sabinene s ilica cap illary; length m; internal diameter , mm ® a) Film thicknes s : , μm β - Pinene O ven temp erature: temp erature p rogramming M yrcene °C /min α- Phellandrene I nj ecto r temp erature: °C α-Terp inene D etecto r temp erature: °C p - Cymene D etecto r: flame io nizatio n typ e , - C ineo le + β - p hellandrene C arrier gas : hydro gen Limonene fro m °C to 2 °C at a rate o f Vo lume inj ected: , μl γ-Terp inene C arrier gas flow rate: , ml/min Terpinolene Terpinen-4-ol Split ratio: 1/100 α-Terp ineo l Aromadendrene Ledene (viridiflo rene) δ - C adinene Globulol Viridiflo ro l OV-101 ® is an examp le o f a s uitab le p ro duct availab le co mmercially This in fo rmatio n is given fo r the co nvenience o f us ers o f this cument and es no t co ns titute an endo rs ement by I S O o f this p ro duct Figure A.1 — Typical chromatogram taken on an apolar column © ISO 2017 – All rights reserved ISO 4730:2017(E) 10 11 12 13 14 15 16 17 18 19 20 P e a k i d e n t i f i c a t i o α-Thujene α-Pinene Sabinene β-Pinene Myrcene α-Phellandrene α-Terpinene Limonene β-Phellandrene p -Cymene 1,8-Cineole γ-Terpinene Terpinolene Terpinen-4-ol α-Terpineol Operating conditions n Column: FSOT; length 60 m; internal diameter 0,25 mm Stationary phase: (35 %)-diphenyl-(65 %)-methylsiloxane copolymer (AT-35 ® a) Film thickness: 0,25 μm Oven temperature: isothermal at 50 °C for min, then temperature programming from 50 °C to 250 °C at a rate o f 10 °C/min and isothermal at 250 °C for Injector temperature: 200 °C Detector temperature: 300 °C Detector: flame ionization type Carrier gas: hydrogen Volume injected: μl (1 % in ethanol) Carrier gas flow rate: 1,0 ml/min Split ratio: 1/50 Aromadendrene Ledene (viridiflorene) δ-Cadinene Globulol Viridiflorol a AT-35® is an example o f a suitable product available commercially This information is given for the convenience o f users o f this document and does not constitute an endorsement by ISO o f this product Figure A.2 — Typical chromatogram taken on an intermediate polarity column © ISO 2017 – All rights reserved ISO 4730:2017(E) 10 11 12 13 14 15 16 17 18 19 20 a P e a k i d e n t i f i c a t i o Operating conditions n fus ed α- Pinene C o lumn: α-Thuj ene S tatio nary p has e: p o ly(ethylene glyco l) 0 0 (B P- β - Pinene Film thicknes s : , μm Sabinene s ilica cap illary; length m; internal diameter , 3 mm O ven temp erature: is o thermal at °C fro m p ro gramming α- Phellandrene 2 °C α-Terp inene I nj ecto r temp erature: 40 °C Limonene min, then temp erature °C to 2 °C at a rate o f °C /min and is o thermal at M yrcene fo r fo r ® a) D etecto r temp erature: 40 °C β - Phellandrene D etecto r: flame io nizatio n typ e γ-Terp inene Vo lume inj ected: , μl (3 % in hexane) 1,8-Cineole Carrier gas: helium p - Cymene Terpinolene Terpinen-4-ol Aromadendrene C arrier gas flow rate: , ml/min Split ratio: 1/100 α-Terp ineo l Ledene (viridiflo rene) δ - C adinene Globulol Viridiflo ro l BP-20 ® is an examp le o f a s uitab le p ro duct availab le co mmercially This in fo rmatio n is given fo r the co nvenience o f us ers o f this cument and es no t co ns titute an endo rs ement by I S O o f this p ro duct Figure A.3 — Typical chromatogram taken on a polar column © ISO 2017 – All rights reserved ISO 4730:2017(E) Annex B (informative) Flashpoint B.1 General information For sa fety reasons, transport companies, insurance companies and people in charge o f sa fety services require in formation on the flash points o f essential oils, which in most cases are flammable products A comparative study on the relevant methods o f analysis (see ISO/TR 11018) concluded that it was di fficult to recommend a single apparatus for standardization purposes, given that: — there is a wide variation in the chemical composition o f essential oils; — the volume o f the sample needed in certain requirements would be too costly for high-priced essential oils — as there are several di fferent types o f 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 document, for information, in order to meet the requirements of the interested parties The equipment with which this value was obtained shall be specified For further in formation, see ISO/TR 11018 B.2 Flashpoint of the essential oil of Melaleuca, terpinen-4-ol (Tea Tree oil) The mean value is +59 °C NOTE Obtained with “closed cup” equipment © ISO 2017 – All rights reserved ISO 4730:2017(E) Annex C (informative) Enantiomeric distribution — General information Some essential oil components can exist in two enantiomeric forms designated as (R) or (S), D or L or ff the right form is critical Also, pure natural essential oils contain enantiomers in characteristic ratios f f ff enantiomeric ratios [4] in f an informative annex of appropriate isolates in International Standards, provides an extra measure of (+) or (-) i s omers M any ena ntiomers h ave d i s ti nc tly d i T h i s ratio i s up s e t b y the add ition o C on s e quently, the me as u rement o erent prop er tie s a nd hence thei r pre s ence i n adu lterants i nclud i ng s ynthe tic maj or comp onents o di erent enantiomeric exce s s or ena ntiomeric ratio a s p er I S O 2 e s s entia l o i l authentic ity T he ena ntiomeric d i s tribution © ISO 2017 – All rights reserved for ter pi nen- - ol i s (R) (+) 67 % - 71 % and (S ) (-) % - 3 % ISO 4730:2017(E) Bibliography [1] [2] [3] [4] 10 ISO 3218, Essential oils — Principles of nomenclature ISO/TR 11018, Essential oils — General guidance on the determination of flashpoint ISO/TR 21092, Essential oils — Characterization ISO 22972, Essential oils — Analysis by gas chromatography on chiral capillary columns — General method © ISO 2017 – All rights reserved ISO 4730:2017(E) I CS 71 00.60 Price based on 10 pages © ISO 2017 – All rights reserved