BS EN 16300:2012 BS 2000-607:2012 BSI Standards Publication Automotive fuels — Determination of iodine value in fatty acid methyl esters (FAME) — Calculation method from gas chromatographic data BS EN 16300:2012 BS 2000-607:2012 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 16300:2012 The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on this committee can be obtained on request to its secretary Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods that would be Part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR Tel: 020 7467 7100 Fax: 020 7255 1472 This publication does not purport to include all the necessary provisions of a contract Users are responsible for its correct application © The British Standards Institution 2012 Published by BSI Standards Limited 2012 ISBN 978 580 75234 ICS 75.160.20 Compliance with a British Standard cannot confer immunity from legal obligations This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012 Amendments issued since publication Date Text affected EN 16300 EUROPEAN STANDARD BS EN 16300:2012 BS 2000-607:2012 NORME EUROPÉENNE EUROPÄISCHE NORM September 2012 ICS 75.160.20 English Version Automotive fuels - Determination of iodine value in fatty acid methyl esters (FAME) - Calculation method from gas chromatographic data Carburants pour automobiles - Détermination de l'indice d'iode dans les esters méthyliques d'acides gras - Méthode de calcul partir des données obtenues par chromatographie en phase gazeuse Kraftstoffe für Kraftfahrzeuge - Bestimmung der Iodzahl in Fettsäure-Methylester (FAME) - Berechnung aus gaschromatographischen Daten This European Standard was approved by CEN on 27 July 2012 CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member This European Standard exists in three official versions (English, French, German) A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 16300:2012: E BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Contents Page Foreword 3 Introduction .4 Scope 5 Normative references 5 Procedure .5 Expression of results 7 5.1 5.2 Precision .7 Repeatability, r .7 Reproducibility, R 8 Test report 8 Bibliography 9 BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Foreword This document (EN 16300:2012) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the secretariat of which is held by NEN This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2013, and conflicting national standards shall be withdrawn at the latest by March 2013 Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Introduction This European Standard has been developed in CEN/TC 19/JWG This document is a self-contained European test method based on the provisions given in Annex B of EN 14214:2008 [2] Some markets need a full test method to check FAME for compliance with EN 14214 The method is not intended as a replacement for EN 14111 [1] (see also Scope) The method is based on results for individual FAME components as determined by EN 14103 On the basis of EN 14103 up to the C24 esters can be determined and a calculation can be done The correlation is well within the repeatability of the existing test method BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Scope This European Standard specifies a calculation procedure for the determination of Iodine value (“CIV” “calculated iodine value”), of fatty acid methyl esters (FAME) to be used either as automotive or heating fuel for diesel engines as specified in EN 14214 [2] or as an extender for automotive fuel for diesel engines as specified in EN 590 [4] This procedure has originally been described in Annex B of EN 14214:2008 [2] The calculation procedure is now specified for methyl esters between C14 and C24 The calculation procedure uses as data entry the results from the gas chromatography determination (GC) according to EN 14103 of individual fatty acid methyl esters and is based on AOCS recommended practice Cd 1c – 85 for the determination of the iodine value of edible oil from its fatty acid composition It is important to recognise that the latest version of EN 14103 is to be used for the determination of individual FAME components NOTE Experience from the field and from several precision evaluation campaigns in Germany and elsewhere indicates that the results of the determination of iodine value by calculation specified here are very close to results obtained by titration with Wijs solvent according to EN 14111 Observed small differences were always found to be smaller than the reproducibility published in the actual EN 14111 For informative purposes only, but not for cases of dispute, EN 14331 [5] may also be used to extract the FAME contents from FAME containing diesel fuels (like B5, B7, B30, etc.) and to use the contents of the individual FAME components from this method as data entry for the calculation specified in this European Standard In principle, other fatty acid alkyl esters can also be analysed However, neither the close correlation to the titration method EN 14111 has been verified nor is any precision information available for such an extension of application range NOTE material For the purposes of this European Standard, the term “% (m/m)” is used to represent the mass fraction, µ, of a Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application For dated references, only the edition cited applies For undated references, the latest edition of the referenced document (including any amendments) applies EN 14103, Fat and oil derivatives — Fatty Acid Methyl Esters (FAME) — Determination of ester and linolenic acid methyl ester contents Procedure The contents of individual fatty acid methyl esters (FAME) are determined according to the GC-determination of C18:3 which is specified in EN 14103 The contents, wi, expressed in % (m/m), obtained for each of the individual FAMEs (i) are then used to calculate the contributions to the iodine value from each FAME component as given in formula (1), using the contribution factors given in Table The calculated iodine value (CIV) is then determined as the sum of the individual contributions, disregarding (i.e without inclusion of) the FAME component used as internal standard in EN 14103 An example for this calculation is given Table CIV = ∑µ ⋅C i i (1) i where CIV is the calculated Iodine value of the sample, given in g Iodine per 100 g sample; BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) µi is the content of individual FAME component i, given in % (m/m); Ci is the contribution factor from FAME component i, listed in Table Table — Contribution factors Ci for individual commonly appearing FAME components FAME designator Molecular mass M Number of olefinic double bonds All saturated FAMEs Cn:0 n.a 0,000 Methyl myristoleate C14:1 240,389 1,056 C14:2 238,373 2,130 C16:1 268,43 0,946 C16:2 266,42 1,905 C17:1 282,46 0,899 C17:2 280,45 1,810 FAME componenta Methyl palmitoleate Methyl heptadecenoate ni Contribution factor Ci Methyl oleate C18:1 296,45 0,856 Methyl linoleate C18:2 294,47 1,724 Methyl linolenate C18:3 292,46 2,604 Methyl eicosenoate C20:1 324,54 0,782 C20:2 322,53 1,574 C20:3 320,51 2,376 C22:1 352,59 0,720 C22:2 350,58 1,448 C22:3 348,56 2,184 Methyl docosenoate Methyl tetracosenoate NOTE C24:1 380,65 0,667 C24:2b 378,63 1,341 C24:3 b 376,62 2,022 C24:4 b 374,60 2,710 Molecular weights are calculated using 12,01 (for C); 1,01 (for H); 16,00 (for O) and 253,81 (for I2) (all in g/mol) NOTE Attention is also drawn to the fact that for many FAME components like e.g C18:2, there may be more than one isomer in the sample All present isomers should be securely identified and included in the calculation a Other isomers are possible b C 24:2, C24:3 and C24:4 are not determined by EN 14103 Factors are given for information only The contribution factors Ci listed in Table for the individual FAME components i have been calculated according to Formula (2): Ci = 253,81 ⋅ ni M i where 253,81 is the molecular weight for the iodine molecule (I2); ni is the number of olefinic double bonds in FAME component i; Mi is the molecular mass for the FAME component i (methyl ester) (2) BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Table — Numeric example Example of component / isomer Double bond designation (FA Chain) Contribution factor Ci µi Effective contribution from FAME (i) Content of FAME (i) %(m/m) Methyl palmitoleate C14:0 0,000 0,30 0,00 C14:1 1,056 0,00 0,00 C14:2 2,130 0,00 0,00 C16:0 0,000 0,40 0,00 C16:1 0,946 1,10 1,04 C16:2 1,905 0,00 0,00 C17:1 0,899 0,00 0,00 C17:2 1,810 0,00 0,00 Methyl stearate C18:0 0,000 2,00 0,00 Methyl oleate C18:1 0,856 61,60 52,73 Methyl linoleate C18:2 1,724 20,10 34,65 Methyl linolenate C18:3 2,604 9,40 24,47 C20:0 0,000 0,40 0,00 C20:1 0,782 0,70 0,55 C20:2 1,574 0,00 0,00 C20:3 2,376 0,00 0,00 C22:0 0,000 0,70 0,00 C22:1 0,720 1,10 0,79 C22:2 1,448 0,00 0,00 C22:3 2,184 0,30 0,66 C24:1 0,667 0,00 0,00 C24:2 1,341 0,00 0,00 C24:3 2,022 0,00 0,00 C24:4 2,710 0,30 0,81 Methyl eicosenoate Methyl docosenoate Methyl tetracosenoate Total ester content, % (m/m) 98,40 Calculated Iodine Value, (CIV), g l2/100 g 115,7 Expression of results The calculated iodine value (CIV) shall be reported rounded to the nearest 0,1 g Iodine/100 g 5.1 Precision Repeatability, r The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would in the long run, in the normal and correct operation of the test method, exceed the values given by Formula (3) in only one case in twenty r = 0,003 X + 0,544 (3) BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) where X is the result or the mean of two results to be compared, in units of g Iodine/100 g 5.2 Reproducibility, R The difference between two single and independent test results, obtained by different operators working in different laboratories on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the values given by Formula (4) in only one case in twenty R = 0,053 X + 1,121 where X is the result or the mean of two results to be compared, in units of g Iodine/100 g Test report The test report shall contain at least the following information: a) reference to this European Standard, i.e EN 16300; b) type and complete identification of the product tested; c) result of the test (see Clause 4); d) any deviation, by agreement or otherwise, from the procedure specified; e) date of the test (4) BS EN 16300:2012 BS 2000-607:2012 EN 16300:2012 (E) Bibliography [1] EN 14111, Fat and oil derivatives — Fatty Acid Methyl Esters (FAME) — Determination of iodine value [2] EN 14214:2008/A1:2009, Automotive fuels – Fatty acid methyl esters (FAME) for diesel engines – Requirements and test methods [3] EN 14214:2012, Liquid petroleum products — Fatty acid methyl esters (FAME) for use in diesel engines and heating applications — Requirements and test methods [4] EN 590, Automotive fuels — Diesel — Requirements and test methods [5] EN 14331, Liquid petroleum products — Separation and characterisation of fatty acid methyl esters (FAME) from middle distillates — Liquid chromatography (LC)/gas chromatography (GC) method BS 2000 Series Energy Institute Buying Parts of BS 2000 Orders for BS 2000 publications should be addressed to 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