DIN EN 14103-2015 Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents German version EN 14103 2011《脂肪和油脂衍生物 .pdf

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1、May 2015 Translation by DIN-Sprachendienst.English price group 10No 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).ICS 67

2、.200.10!%BZ“2315591www.din.deDDIN EN 14103Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of ester and linolenic acid methyl ester contents;English version EN 14103:2011,English translation of DIN EN 14103:2015-05Erzeugnisse aus pflanzlichen und tierischen Fetten und len Fettsu

3、re-Methylester (FAME) Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensure-Methylester;Englische Fassung EN 14103:2011,Englische bersetzung von DIN EN 14103:2015-05Produits drivs des corps gras Esters mthyliques dacides gras (EMAG) Dtermination de la teneur en ester et en ester mthylique de

4、 lacide linolnique;Version anglaise EN 14103:2011,Traduction anglaise de DIN EN 14103:2015-05SupersedesDIN EN 14103:2011-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 15 pages 04.15 DIN EN 14103:2015-05 2 A comma is used as the deci

5、mal marker. National foreword This document (EN 14103:2011) has been prepared by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 19 “Gase

6、ous 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 DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 0

7、62-06-32-01 UA Prfung von FAME of the Fachausschuss Minerall- und Brennstoffnormung in collaboration with the DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 057-05-05 AA Gemeinschaftsausschuss fr die An

8、alytik von Fetten, len, Fett-produkten, verwandten Stoffen und Rohstoffen. Amendments This standard differs from DIN EN 14103:2003-10 as follows: a) the scope has been extended to C6 up to C24 (formerly C14 to C24); b) the scope of the method has been extended to include FAME from animal fat, by cha

9、nging the internal standard (FAME C19 instead of FAME C17); c) the preparation of the test portion has been improved; d) the apparatus and procedure have been updated; e) the precision data have been updated. Compared with DIN EN 14103:2011-07, the following corrections have been made to the German

10、version only and therefore do not affect the English text: a) in Table 1, line 1 (For ester content), column 2, formula r = 1,01 % (m/m) has been replaced by 1,01 % (m/m); b) in Table 2, line 1 (For ester content), column 2, formula R = 4,16 % (m/m) has been replaced by 4,16 % (m/m); c) in Table 2,

11、line 2 (For linolenic acid methyl ester), column 2, formula R = 0,387 2 X + 0,028 5 X has been replaced by R = 0,387 2 + 0,028 5 X. Previous editions DIN EN 14103: 2003-10, 2011-07 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 14103 April 2011 ICS 67.200.10 Supersedes EN 14103:2003English Ver

12、sion Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contentsProduits drivs des corps gras - Esters mthyliques dacides gras (EMAG) - Dtermination de la teneur en ester et en ester mthylique de lacide linolnique Erzeugnisse aus pflanz

13、lichen und tierischen Fetten und len - Fettsure-Methylester (FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensure-Methylester This European Standard was approved by CEN on 10 March 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the co

14、nditions 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 exi

15、sts 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 st

16、andards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland an

17、d United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14103:

18、2011: EEN 14103:2011 (E) 2 Contents Page Foreword 31 Scope 42 Principle 43 Reagents . 44 Apparatus . 45 Sampling . 56 Procedure . 57 Expression of results 68 Precision . 79 Test report 8Bibliography 13DIN EN 14103:2015-05 Annex A (informative) Chromatograms of a FAME samples - Determination of ester

19、 content - Summary of the analysis conditions 9Annex B(informative) Results of an interlaboratory trial 1. 2EN 14103:2011 (E) 3 Foreword This document (EN 14103:2011) has been prepared by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of

20、sampling and analysis”, the secretariat of which is held by AFNOR. 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 October 2011, and conflicting national standards shall be withdrawn at the latest

21、 by October 2011. 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. This document supersedes EN 14103:2003. The main modifications of th

22、e standard are intended: - to enlarge the scope of the method to FAME from animal fat, by changing the internal standard (FAME C19 instead of FAME C17); - to verify the purity of the internal standard as it was proven that some lots may have a purity not good enough; - to improve the precision data

23、by modifying the preparation of the test portion. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland,

24、France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 14103:2015-05 EN 14103:2011 (E) 4 1 Scope The purpose of this document is to desc

25、ribe a procedure for the determination of the ester content in fatty acid methyl esters (FAME) intended for incorporation into diesel oil. It also allows determining the linolenic acid methyl ester content. It allows verifying that the ester content of FAME is greater than 90 % (m/m) and that the li

26、nolenic acid content is between 1 % (m/m) and 15 % (m/m). This method is suitable for FAME which contains methyl esters between C6 and C24. NOTE For the purposes of this European Standard, the terms “% (m/m)” and “%(v/v)” are used to represent respectively the mass and volume fractions. WARNING The

27、use of this method may involve hazardous equipment, materials and operations. This method does not purport to address to all of the safety problems associated with its use, but it is the responsibility of the user to search and establish appropriate safety and health practices and determine the appl

28、icability of regulatory limitations prior to use. 2 Principle Determination of the percentage of total methyl esters of fatty acids and the percentage of linolenic acid methyl ester present in the sample, by gas chromatography according to a procedure using internal calibration (nonadecanoic acid me

29、thyl ester). 3 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 3.1 Toluene, analytical grade. 3.2 Nonadecanoic acid methyl ester (FAME C19), purity, min. 99,5 % (m/m)1). NOTE Standard should be kept in a dry storage in order to limit its water absorption. Its w

30、ater content should be verified by Karl-Fischer when a new lot of standard is open. 3.3 Carrier gas, hydrogen or helium. 3.4 Auxiliary gases: air; hydrogen. 4 Apparatus Usual laboratory apparatus and, in particular, the following. 1) Nonadecanoic FAME with acceptable quality is available from Fluka

31、- Ref: 74208 () or from Nu Chek Prep - Ref: N-19-M (www.nu-) or Dr. Ehrenstorfer GmbH ref 15 622 360 (www.analytical-). This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. DIN EN 14103:2015-05 EN 14103:2011

32、 (E) 5 4.1 Gas chromatograph, equipped with a variable split flow injector or equivalent device, a temperature programmable oven and a flame ionization detector. 4.2 Capillary column, coated with polyethylene glycol (Carbowax 20M) stationary phase, the following characteristics have been found suita

33、ble: length: 30 m, internal diameter: 0,25 mm, film thickness: 0,25 m. NOTE Stationary phase other than polyethylene glycol should be tested first before being selected as co-elution between the internal standard (FAME C19) and other fatty acid methyl esters may exist. Indeed, there is a co-elution

34、between FAME C19 and linoleic acid methyl ester (FAME C18:2) when using a column with a stationary phase such as 70 % cyanopropyl-polysilphenyl-siloxane. 4.3 Glass mono-use tubes equipped with plastic mono-use stopper, 10 ml capacity. 4.4 Pipette, 10 ml capacity. 4.5 Analytical balance, accuracy 0,1

35、 mg. 5 Sampling Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN ISO 5555 1. 6 Procedure 6.1 Operating conditions The chromatographic analysis conditions will be chosen taking into account the characteristics of the column being use

36、d and the type of carrier gas (hydrogen or helium). By way of indication, an example of analysis conditions is described below: column temperature: 60 C hold for 2 min, programmed at 10 C.min-1up to 200 C, programmed at 5 C.min-1up to 240 C, final temperature hold for 7 min; injector temperature car

37、rier gas flow rate 1-2 ml.min-1, a minimum flow rate of 1 ml.min-1shall be warranted when operating at the maximum temperature; injected volume: 1 l; hydrogen pressure = 70 KPa; split flow = 100 ml.min-1. 6.2 Internal standard purity determination Prepare a solution of nonadecanoic acid methyl ester

38、 (3.2) in toluene (3.1) approximately at 10 mg.ml-1. Analyse 1 l of this solution by gas chromatography according to the conditions described in (6.1), but the final temperature should be held for 20 min at 240 C, instead of 7 min. Calculate the purity of the nonadecanoic acid methyl ester taking in

39、to account all the peak eluted in the chromatogram, excepted the solvent peak. The purity of nonadecanoic acid methyl ester should be at least 99,5 % (m/m). If the purity is lower than 99,5 % (m/m) do not use this standard for this determination. NOTE No correction of the purity of the internal stan

40、dard is performed for the calculation of the FAME content. DINEN 14103:2015-05EN 14103:2011 (E) 6 6.3 FAME sample preparation and analysis Accurately weigh approximately 100 mg (accuracy 0,1 mg) of homogenized sample in a 10 ml tube (4.3), and approximately 100 mg (accuracy 0,1 mg) of nonadecanoic a

41、cid methyl ester (3.2), and dilute with 10 ml of toluene (3.1). NOTE Standard and samples should be let at ambient temperature, in their container closed, at least 3 h prior being weighed, in order to limit the water absorption during weighting. Analyse 1 l of this solution by gas chromatography acc

42、ording to the conditions described in (6.1). For each sample, two test portions are prepared and give rise, each one, to two chromatographic analyses. 6.4 Identification The chromatographic conditions (injected quantity, oven temperature, carrier gas pressure and split flow rate) shall be adjusted s

43、o as to correctly visualize the methyl ester peaks of the lignoceric (C24:0) and nervonic (C24:1) acids. The integration shall be carried out as from the hexanoic acid methyl ester (C6:0) peak up to that of the nervonic acid methyl ester (C24:1) taking all the peaks identified as fatty acid methyl e

44、sters into consideration. In order to identify properly the fatty acid methyl esters, some commercial solutions may be used 2). NOTE If some unknown thin peaks are found (others than saturated and mono-unsaturated FAME) between the linolenic acid methyl ester (C18:3) and the nervonic acid methyl est

45、er (C24:1), presence of fish oil in the sample can be suspected. As a general rule, the separation is done according to carbon atom chain length, unsaturated FAME are eluted after the corresponding saturated ones. 7 Expression of results 7.1 Determination of ester content The ester C content, expres

46、sed as a mass percentage, is calculated using the following equation: 100EIEIEI=WWAAAC (1) where A is the total peak area from the methyl ester in C6:0 to that in C24:1; AEIis the peak area corresponding to nonadecanoic acid methyl ester; WEIis the weight, in milligrams, of the nonadecanoic acid met

47、hyl ester being used as internal standard; W is the weight, in milligrams, of the sample. NOTE 1 In the case of vegetable oils, the result of the calculation based on relative areas is considered to represent a percentage by mass. 2) Commercial solutions of mixtures of fatty acid methyl esters are a

48、vailable from Sigma Ref. 18918-1AMP () or from Nu Chek Prep Ref.17a (www.nu-). This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. DIN EN 14103:2015-05 EN 14103:2011 (E) 7 NOTE 2 If the average of two determinations is higher than 100 % then discard the results and v