SIST EN 14106:2003

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.JOLFHURORYErzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Gehaltes an freiem GlycerinProduits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en glycérol libreFat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free glycerol content67.200.10Animal and vegetable fats and oilsICS:Ta slovenski standard je istoveten z:EN 14106:2003SIST EN 14106:2003en01-november-2003SIST EN 14106:2003SLOVENSKI
STANDARD



SIST EN 14106:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14106April 2003ICS 67.200.10English versionFat and oil derivatives - Fatty Acid Methyl Esters (FAME) -Determination of free glycerol contentProduits dérivés des corps gras - Esters méthyliquesd'acides gras (EMAG) - Détermination de la teneur englycérol libreErzeugnisse aus pflanzlichen und tierischen Fetten undÖlen - Fettsäure-Methylester (FAME) - Bestimmung desGehaltes an freiem GlycerinThis European Standard was approved by CEN on 2 January 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14106:2003 ESIST EN 14106:2003



EN 14106:2003 (E)2ForewordThis document (EN 14106:2003) has been prepared by Technical Committee CEN/TC 307 "Oilseeds, vegetableand animal fats and oils and their by-products - Methods of sampling and analysis", the secretariat of which is heldby AFNOR.This European Standard
shall be given the status of a national standard, either by publication of an identical textor by endorsement, at the latest by October 2003 and conflicting national standards shall be withdrawn at the latestby October 2003.This document has been prepared under Mandate M/245 on Fatty Acid Methylester (FAME) given to CEN by theEuropean Commission and the European Free Trade Association.Annex A is informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 14106:2003



EN 14106:2003 (E)31 ScopeThis European Standard specifies a gas chromatographic method for the determination of free glycerol content inFatty Acid Methyl Esters (FAME) in the range of 0,005 % to 0,070 %, hereinafter referred as FAME.This method aims to evaluate the FAME quality, in terms of transesterification by-products content such asglycerol, whose concentration may affect the fuel behaviour.WARNING — The use of this method may involve hazardous equipment, materials and operations. Thismethod does not purport to address to all of the safety problems associated with its use, but it is theresponsibility of the user to search and establish appropriate safety and health practices and determinethe applicability of regulatory limitations prior to use.NOTEIn the context of this method (m/m) and (v/v) can be used.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN ISO 661, Animal and vegetable fats and oils - Preparation of test sample (ISO 661:1989).3 Terms and definitionsFor the purposes of this European Standard, the following term and definition apply.3.1free glycerol contentis the residual glycerol remaining in FAME after the vegetable oil transesterification reaction and the separation ofso obtained glycerol4 Principle of methodEthyl alcohol, water and hexane and a known amount of internal standard are added to a known quantity ofsample. The addition of these solvents causes the formation of two phases and free glycerol is quantitativelytransferred into the lower one.The gas chromatographic analysis of lower phase allows to quantify the concentration of free glycerol.5 ReagentsUse only reagents of recognized analytical grade, unless otherwise specified.5.1Hexane.5.21,4 Butanediol, 99 % minimum.5.3Ethyl alcohol, 95 % minimum.5.4Formic acid, 99 % minimum.5.5Glycerol, 99 % minimum.SIST EN 14106:2003



EN 14106:2003 (E)45.6Carrier gas : helium, GLC grade.5.7Auxiliary gases:¾ hydrogen, purity 99 % minimum, free from moisture and organic compounds;¾ air, free from organic compounds.5.8Internal Standard Solution : weigh approximately 80 mg (accuracy ± 0,0001 g) of 1,4 Butanediol in avolumetric flask, 100 ml capacity. Dissolve in some ml of distilled water, add 1 ml of formic acid and fill up to themark using distilled water. The so prepared solution is stable for 24 h if stored at ambient temperature.6 Apparatus6.1Gas chromatograph equipped by the following devices:6.1.1Thermostatic oven for column, able to maintain the set temperature with an accuracy of ± 1 °C.6.1.2Thermostatic injection port, equipped for capillary column in split-splitless mode or, alternatively, for packedcolumn.6.1.3Flame ionisation detector (FID) and converter/amplifier device.6.1.4Recorder/integrator, capable to run with the converter/amplifier with a response time of 1 s maximum andvariable chart speed.6.1.5Capillary column, type PoraPLOT Q, length = 10 m, diameter 0,32 mm, film thickness = 10 µm (Note) or,alternatively packed column filled with CHROMOSORB 101, diameter 4 mm, length = 1 m.NOTESome problems and discrepancies on capillary column behaviour from different suppliers have been noticed. SomeAuthors refer also the possibility to use capillary columns coated with FFAP (Free Fatty Acid Phase) or polyethyleneglycolphases instead of the suggested stationary phase. Nevertheless the choice of column should be based on the following criteria:· the separation between glycerol and internal standard peak
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