Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of methanol content

This European Standard specifies a method for the determination of methanol content in fatty acid methyl esters (FAME) for use as diesel fuel and domestic heating fuel. The method is applicable for a concentration range from 0,01 % to 0,5 % (m/m) methanol. The method is not applicable to mixtures of FAME which contain other low boiling components.

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Methanolgehaltes

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Methanol in Fettsäure-Methylestern (FAME) für deren Gebrauch als Dieselkraftstoff oder als Heizöl fest. Dieses Verfahren ist anwendbar auf einen Konzentrationsbereich von 0,01 % (m/m) bis 0,5 % (m/m) Methanol. Dieses Verfahren ist nicht anwendbar auf FAME-Mischungen, die andere niedrig siedende Komponenten enthalten.

Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en méthanol

La présente Norme européenne décrit une méthode de dosage du méthanol dans les esters méthyliques d'acides gras (EMAG) utilisable pour le gazole et le combustible de chauffage domestique. Cette méthode est applicable sur une plage de concentrations en méthanol comprise entre 0,01 % et 0,5 % (m/m). Elle n'est pas applicable aux mélanges d'EMAG qui contiennent des composants a faible point d'ébullition.

Derivati maščob in olj - Metil estri maščobnih kislin (FAME) - Določevanje metanola

General Information

Status
Withdrawn
Publication Date
31-Oct-2003
Withdrawal Date
20-May-2019
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
17-May-2019
Due Date
09-Jun-2019
Completion Date
21-May-2019

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.ORþHYDQMHPHWDQRODErzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des MethanolgehaltesProduits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en méthanolFat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of methanol content67.200.10Animal and vegetable fats and oilsICS:Ta slovenski standard je istoveten z:EN 14110:2003SIST EN 14110:2003en01-november-2003SIST EN 14110:2003SLOVENSKI

STANDARD
SIST EN 14110:2003

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14110April 2003ICS 67.200.10English versionFat and oil derivatives - Fatty Acid Methyl Esters (FAME) -Determination of methanol contentProduits dérivés des corps gras - Esters méthyliquesd'acides gras (EMAG) - Détermination de la teneur enméthanolErzeugnisse aus pflanzlichen und tierischen Fetten undÖlen - Fettsäure-Methylester (FAME) - Bestimmung desMethanolgehaltesThis 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 14110:2003 ESIST EN 14110:2003

EN 14110:2003 (E)2ForewordThis document (EN 14110:2003) 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 text orby 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, and supports essential requirements of EUDirective(s).Annexes A and B are 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 14110:2003

EN 14110:2003 (E)31 ScopeThis European Standard specifies a method for the determination of methanol content in fatty acid methyl esters(FAME) for use as diesel fuel and domestic heating fuel. The method is applicable for a concentration range from0,01 % (m/m) to 0,5 % (m/m) methanol. The method is not applicable to mixtures of FAME which contain other lowboiling components.2 PrincipleThe sample is heated at 80 °C in a hermetically sealed vial to allow desorption of contained methanol into the gasphase. When equilibrium is reached, a defined part of the gas phase is injected into a gas chromatograph, wheremethanol is detected with a flame ionisation detector. Normally methanol is the only peak in the chromatogram.The amount of methanol is calculated by reference to an external calibration. Methanol can also be determinedafter addition of an internal standard to the sample before heating, followed by calculation with the use of aninternal calibration factor.NOTEIf only manual equipment is available then only internal standard calibration should be used.3 ReagentsUse only reagents of recognized analytical grade, unless otherwise specified.3.1Methanol, of known purity greater than 99,5 %.3.22-propanol, of known purity, greater than 99,5 % (for procedure A, internal calibration).3.3Reference FAME, with a methanol content less than 0,001 % (m/m).NOTEReference FAME can either be obtained from commercial sources or by washing by three or five times with distilledwater in a separator funnel. FAME should be then dried by heating at 90 °C under stirring and reduced pressure.3.4Carrier gas, nitrogen, helium or hydrogen, of know purity greater than 99 %.4 Apparatus4.1Septum vials, 20 ml capacity.4.2Inert septa (e.g. TFE or Viton 1)) and metallic caps.4.3Syringe, 10 µl, accurate to 0,1 µl.4.4Gas syringe 500 µl, fitted with a valve (for manual procedure).4.5Crimping pliers.4.6Pipettes, of 1 ml, 2 ml, 5 ml capacity.4.7Volumetric flask, capacity 10 ml and 25 ml.

1)This information is given for the convenience of users of this European Standard and does not constitute an endorsementby CEN of these products. Equivalent products may be used if they can be shown to lead to the same results.SIST EN 14110:2003

EN 14110:2003 (E)44.8Gas chromatograph, equipped with a capillary column, suitable injector (automatic headspace system or asplit/splitless injector) and flame ionisation detector, integrator.4.9Capillary column, the column shall eluate methanol as a symmetrical peak. Stationary phases likemethylpolysiloxane (e.g. DB1 2), SE30 2)) or polyethylenglycol (e.g. DBWAX 2), CAR-BOWAX 2)) can be usedsuccessfully and a film thickness of minimum 0,5 µm is recommended.NOTEThe use of a packed column equipped by one of the above mentioned stationary phases or of Chromosorb 1012) isalso allowed.4.10Automatic headspace equipmentThe automatic headspace equipment used shall have a repeatability of 1 % or better concerning experimentalconditions like equilibrium temperature, heating times, and headspace sampling volume. This can be checked, ifnecessary, by repeated analysis of the same sample.NOTEAutomatic headspace equipment is recommended because apart, from its better repeatability, it allows forautomated and fast analysis using external calibration. Manual equipment can also be used, however, extreme care should beexercised when gas volumes are taken manually from the vials and when injecting them into the gas chromatograph.4.11Analytical balance with a resolution of 0,0001 g.4.12Thermostatically controlled bath or oven, 80 °C.4.13Thermostatically controlled oven, 60 °C.5 Procedure5.1 Analytical conditionsThe GC working conditions shall be chosen taking into account the characteristics of the column and the type ofcarrier gas to reach the desired resolution which is fixed at minimum 1,5 for the methanol and 2-propanol peaks.NOTE 1The following parameters are given as an example:¾ column DB1 (length = 30 m, internal diameter = 0,32 mm, film thickness = 3 µm);¾ split injector (flow rate : 50 ml/min);¾ injector and detector temperature:150°C;¾ oven and column temperature:50 °C;¾ carrier gas (hydrogen) pressure:40 kPa;¾ volume injected:500 µl.NOTE 2The following head space sampling conditions are given as an example:¾ equilibrium temperature:80 °C;¾ equilibrium time:45 min;¾ sampling volume:500 µl.

2)This information is given for the convenience of users of this European Standard and does not constitute an endorsementby CEN of these products. Equivalent products may be used if they can be shown to lead to the same results.SIST EN 14110:2003

EN 14110:2003 (E)55.2 OperationThe gas chromatograph shall be set up and operated according to the manufacturer’s instructions.6 Calibration solutionsThree calibration solutions with approximately the following methanol concentrations in FAME (3.3) shall beprepared as described below.NOTEThree calibration solutions have proven sufficient in daily practise for a reliable coverage of the concentration rangegiven in the scope of this method. For other concentrat

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