DIN EN 16300-2012 Automotive fuels - Determination of iodine value in fatty acid methyl esters (FAME) - Calculation method from gas chromatographic data German version EN 16300 201.pdf

1、November 2012 Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 75.160.20!$Jf“1923967www.din.deDDIN EN 16300Automotive fuels Determination of iodine value in fatty acid methyl esters (FAME) Calculation method from gas chromatographic data;English version EN 16300:2012,English translation of DIN EN 16300:2012-11Kraftstoffe fr Kraftfahrzeuge Bestimmung der Iodza

3、hl in Fettsure-Methylester (FAME) Berechnung aus gaschromatographischen Daten;Englische Fassung EN 16300:2012,Englische bersetzung von DIN EN 16300:2012-11Carburants pour automobiles Dtermination de lindice diode dans les esters mthyliques dacides gras Mthode de calcul partir des donnes obtenues par

4、 chromatographie en phasegazeuse;Version anglaise EN 16300:2012,Traduction anglaise de DIN EN 16300:2012-11www.beuth.deDocument comprises 11 pagesIn case of doubt, the German-language original shall be considered authoritative.10.12 DIN EN 16300:2012-11 2 A comma is used as the decimal marker. Natio

5、nal foreword This standard has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Mat

6、erialprfung (Materials Testing Standards Committee), Working Committee NA 062-06-32-01 UA Prfung von FAME of the Fachausschuss Minerall- und Brennstoffnormung (FAM). EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16300 September 2012 ICS 75.160.20 English Version Automotive fuels - Determinati

7、on of iodine value in fatty acid methyl esters (FAME) - Calculation method from gas chromatographic data Carburants pour automobiles - Dtermination de lindice diode dans les esters mthyliques dacides gras - Mthode de calcul partir des donnes obtenues par chromatographie en phase gazeuse Kraftstoffe

8、fr Kraftfahrzeuge - Bestimmung der Iodzahl in Fettsure-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

9、 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 ve

10、rsions (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 Austri

11、a, 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,

12、 Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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 Memb

13、ers. Ref. No. EN 16300:2012: EEN 16300:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Procedure .54 Expression of results 75 Precision .75.1 Repeatability, r .75.2 Reproducibility, R 86 Test report 8Bibliography 9DIN EN 16300:2012-11 EN 16300:2012 (E) 3 Foreword

14、 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 standar

15、d, 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 a

16、nd/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, Cz

17、ech 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 Kingd

18、om. DIN EN 16300:2012-11 EN 16300:2012 (E) 4 Introduction This European Standard has been developed in CEN/TC 19/JWG 1. 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 complianc

19、e 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 wel

20、l within the repeatability of the existing test method. DIN EN 16300:2012-11 EN 16300:2012 (E) 5 1 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 automot

21、ive 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 an

22、d 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 c

23、omposition. It is important to recognise that the latest version of EN 14103 is to be used for the determination of individual FAME components. NOTE 1 Experience from the field and from several precision evaluation campaigns in Germany and elsewhere indicates that the results of the determination of

24、 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

25、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

26、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 2 For the purposes of this European Standard, the term “% (m/m)” is used to re

27、present the mass fraction, , of a material. 2 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

28、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 3 Procedure The contents of individual fatty acid methyl esters (FAME) are determined according to the GC-dete

29、rmination 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 1.

30、 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 2. =iiiCCIV (1) where CIV is the calculated Iodine value

31、 of the sample, given in g Iodine per 100 g sample; DIN EN 16300:2012-11 EN 16300:2012 (E) 6 iis the content of individual FAME component i, given in % (m/m); Ciis the contribution factor from FAME component i, listed in Table 1. Table 1 Contribution factors Ci for individual commonly appearing FAME

32、 components FAME componentaFAME designator Molecular mass M Number of olefinic double bonds niContribution factor CiAll saturated FAMEs Cn:0 n.a. 0 0,000 Methyl myristoleate C14:1 240,389 1 1,056 C14:2 238,373 2 2,130Methyl palmitoleate C16:1 268,43 1 0,946 C16:2 266,42 2 1,905Methyl heptadecenoate

33、C17:1 282,46 1 0,899 C17:2 280,45 2 1,810Methyl oleate C18:1 296,45 1 0,856 Methyl linoleate C18:2 294,47 2 1,724 Methyl linolenate C18:3 292,46 3 2,604 Methyl eicosenoate C20:1 324,54 1 0,782 C20:2 322,53 2 1,57420:3 320,51 3 2,376Methyl docosenoate C22:1 352,59 1 0,720 C22:2 350,58 2 1,44822:3 348

34、,56 3 2,184Methyl tetracosenoate C24:1 380,65 1 0,667 C24:2b378,63 2 1,341C24:3b376,62 3 2,022 C24:4b374,60 4 2,710NOTE 1 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 2 Attention is also drawn to the fact that for many FAM

35、E 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. aOther 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 contrib

36、ution factors Cilisted in Table 1 for the individual FAME components i have been calculated according to Formula (2): iiiMnC = 81,253(2) where 253,81 is the molecular weight for the iodine molecule (I2); niis the number of olefinic double bonds in FAME component i; Miis the molecular mass for the FA

37、ME component i (methyl ester). DIN EN 16300:2012-11 EN 16300:2012 (E) 7 Table 2 Numeric example Example of component / isomer Double bond designation (FA Chain) Contribution factor CiContent of FAME (i) i%(m/m) Effective contribution from FAME (i) C14:0 0,000 0,30 0,00 C14:1 1,056 0,00 0,00 C14:2 2,

38、130 0,00 0,00 C16:0 0,000 0,40 0,00 Methyl palmitoleate 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 24,4

39、7 C20:0 0,000 0,40 0,00 Methyl eicosenoate 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 Methyl docosenoate C22:1 0,720 1,10 0,79 C22:2 1,448 0,00 0,00 C22:3 2,184 0,30 0,66 Methyl tetracosenoate C24:1 0,667 0,00 0,00 C24:2 1,341 0,00 0,00 C24:3 2,022 0,00 0

40、,00 C24:4 2,710 0,30 0,81 Total ester content, % (m/m) 98,40 Calculated Iodine Value, (CIV), g l2/100 g 115,7 4 Expression of results The calculated iodine value (CIV) shall be reported rounded to the nearest 0,1 g Iodine/100 g. 5 Precision 5.1 Repeatability, r The difference between two test result

41、s, 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 7 (3) DIN EN 1

42、6300:2012-11 EN 16300:2012 (E) 8 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 mat

43、erial, 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 6 (4) where X is the result or the mean of two results to be compared, in units of g Iodine/100 g. 6 Test report The test repor

44、t 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.

45、DIN EN 16300:2012-11 EN 16300:2012 (E) 9 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 p

46、etroleum 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 DIN EN 16300:2012-11