SIST EN 14105:2011
(Main)Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents
This European Standard specifies a method to determine the free glycerol and residual mono-, di- and triglyceride contents in fatty acid methyl esters (FAME) intended for addition to mineral oils. The total glycerol content is then calculated from the results obtained.
This method is suitable for FAME from rapeseed, sunflower, soybean oils but is not suitable for FAME produced from or containing coconut and palm kernel oils because of overlapping of peaks.
WARNING - The 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 applicability of regulatory limitations prior to use.
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Gehaltes an freiem und Gesamtglycerin und Mono-, Di- und Triglyceriden
Diese Europäische Norm legt ein Verfahren fest, um freies Glycerin und Reste an Mono-, Di- und
Triglyceriden in Fettsäure-Methylester (FAME), die als Zugabe zu Mineralölen vorgesehen sind, zu
bestimmen. Der Gesamtglyceringehalt wird anschließend aus den erhaltenen Messwerten berechnet.
Die Nachweisgrenzen sind für die festgelegten analytischen Bedingungen 0,001 % (m/m) für Freies Glycerin
und 0,10 % (m/m) für alle Glyceride (Mono, Di- und Tri-). Das Verfahren ist einsetzbar für FAME aus Rapsöl,
Sonnenblumenöl und Sojaöl, Palmöl, für tierische Fette und Öle und für deren Mischungen. Es kann nicht
eingesetzt werden für FAME aus Kokosnuss- und Palmkernölen, da hier überlappende Peaks auftreten.
ANMERKUNG Für den Anwendungsbereich dieser Norm wird die Kennzeichnung „% (m/m)“ verwendet, um den
Massenanteil in Prozent, μ, darzustellen.
WARNUNG — Bei der Anwendung dieses Verfahrens kann das Benutzen gefährlicher Substanzen und
Ausrüstungen sowie das Durchführen gefährlicher Tätigkeiten erforderlich werden. Dieses Verfahren
nimmt nicht für sich in Anspruch, alle Sicherheitsprobleme, die bei seiner Anwendung auftreten
können, aufzuzeigen. Es liegt in der Verantwortung des Anwenders dieses Verfahrens, entsprechende
Sicherheitsmaßnahmen und Vorkehrungen zum Schutz der Gesundheit zu ergreifen.
Produits dérivés des corps gras - Esters méthyliques d'acides gras - Détermination de la teneur en glycérols libre et total et en mono-, di- et triglycérides
La présente Norme européenne a pour objet de déterminer les teneurs en glycérol libre et en mono-, di- et
triglycérides résiduels des esters méthyliques d’acides gras (EMAG) destinés à être incorporés dans des
huiles minérales. La teneur en glycérol total est ensuite calculée à partir des résultats obtenus.
Dans les conditions décrites, les limites de détection sont de 0,001 % (m/m) pour le glycérol libre et de
0,10 % (m/m) pour tous les glycérides (mono-, di- et tri-). Cette méthode convient pour les EMAG préparés à
partir d’huiles de colza, de tournesol, de soja, de palme, d’huiles et de graisses d’origine animale et d’un
mélange de celles-ci. Elle ne convient pas pour les EMAG produits à partir de, ou contenant des dérivés
d’huiles de noix de coco ou de palmiste en raison du chevauchement de différents pics de glycérides.
NOTE 1 Pour les besoins de la présente Norme européenne, le terme « % (m/m) » est employé pour représenter la
fraction massique respective (μ).
AVERTISSEMENT — La présente méthode peut impliquer l’utilisation d’opérations, de substances et
d’équipements dangereux. Elle n’a pas la prétention de prendre en compte tous les problèmes de
sécurité liés à son utilisation. Il est de la responsabilité de l’utilisateur d’établir et de mettre en oeuvre
des mesures appropriées en matière de sécurité et de santé, et de déterminer l’applicabilité de
restrictions réglementaires avant son utilisation.
Derivati maščob in olj - Metil estri maščobnih kislin (FAME) - Določevanje prostega in celotnega glicerola ter mono-, di- in trigliceridov
Ta evropski standard opredeljuje metodo za določevanje prostega glicerola in preostalih mono-, di- in trigliceridov v metilestrih maščobnih kislin (FAME) za dodajanje mineralnim oljem. Celotni glicerol se nato izračuna iz pridobljenih rezultatov.
Ta metoda je primerna za FAME iz olja repičnega semena, sončnic, soje, a ni primerna za FAME, ki je proizveden iz kokosovega olja in palmovega olja ali ju vsebuje, zaradi prekrivanja konic.
OPOZORILO: Uporaba te metode lahko vključuje nevarno opremo, materiale in operacije. Ta metoda ne pomeni obravnave vseh varnostnih problemov, povezanih z njeno uporabo, ampak je uporabnik odgovoren, da poišče in vzpostavi ustrezne varnostne in zdravstvene postopke in ugotovi veljavnost regulativnih omejitev pred uporabo.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Gehaltes an freiem und Gesamtglycerin und Mono-, Di- und TriglyceridenProduits dérivés des corps gras - Esters méthyliques d'acides gras - Détermination de la teneur en glycérols libre et total et en mono-, di- et triglycéridesFat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents67.200.10Animal and vegetable fats and oilsICS:Ta slovenski standard je istoveten z:EN 14105:2011SIST EN 14105:2011en,fr,de01-julij-2011SIST EN 14105:2011SLOVENSKI
STANDARDSIST EN 14105:20031DGRPHãþD
SIST EN 14105:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14105
April 2011 ICS 67.200.10 Supersedes EN 14105:2003English Version
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en glycérols libre et total et en mono-, di- et triglycérides
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Gehaltes an freiem und Gesamtglycerin und Mono-, Di-und Triglyceriden 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 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR 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 14105:2011: ESIST EN 14105:2011
EN 14105:2011 (E) 2 Contents Page Foreword .31 Scope .42 Principle .43 Reagents .44 Apparatus .55 Preparation of solutions .65.1 1,2,4-Butanetriol stock solution, 1 mg/ml .65.2 Glycerol stock solution, 0,5 mg/ml .65.3 Standard glycerides stock solution, 2,5 mg/ml .65.4 Commercial mixture of monoglycerides .65.5 Calibration solutions .66 Sampling .77 Procedure .77.1 Operating conditions .77.2 Analysis of the calibration solutions .77.3 Analysis of the commercial mixture of monoglycerides .77.4 Preparation and analysis of the samples .87.5 Identification .87.6 Calibration .87.7 Column performance control .88 Determination of results .98.1 Integration of the peaks .98.2 Glycerol calibration function .98.3 Free glycerol .98.4 Glycerides . 108.5 Total glycerol . 109 Expression of results . 1010 Precision . 1010.1 Interlaboratory test . 1010.2 Repeatability . 1110.3 Reproducibility . 1111 Test report . 11Annex A (informative)
Sample chromatogram . 12Annex B (normative)
Calibration function calculation . 16Annex C (informative)
Worked example. 18Annex D (informative)
Results of the interlaboratory trial . 19Bibliography . 21 SIST EN 14105:2011
EN 14105:2011 (E) 3 Foreword This document (EN 14105:2011) 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”, 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 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 14105:2003. The main modifications of the standard are: - the utilization of representative internal standards for monoglycérides, diglycerides and triglycerides in order to avoid using calibration solutions for these families of compounds; - the introduction of a performance criteria for the gas chromatography column calculated with the response factors for the diglyceride and triglyceride internal standards. The method has been updated to obtain better precision in general, needed for the limits required by European FAME specifications for automotive use [1]. This has been done by introducing separate internal standards for mono- (C19), di- (C38) and triglycerides (C57). Next an improvement of the integration has been incorporated and some evaluation of interference with minor components (i.e. dimers) has been done. Via a new Round Robin study, improvement of the precision of free glycerol and diglyceride measurement has been proven. The precision statement of the former standard could be confirmed for triglyceride determination, but no improvement was made. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 14105:2011
EN 14105:2011 (E) 4 1 Scope The purpose of this European Standard is to determine the free glycerol and residual mono-, di- and triglyceride contents in fatty acid methyl esters (FAME) intended for addition to mineral oils. The total glycerol content is then calculated from the obtained results. Under the conditions described, the quantification limits are 0,001 % (m/m) for free glycerol, 0,10 % (m/m) for all glycerides (mono-, di- and tri-). This method is suitable for FAME prepared from rapeseed, sunflower, soybean, palm, animal oils and fats and mixture of them. It is not suitable for FAME produced from or containing coconut and palm kernel oils derivatives because of overlapping of different glyceride peaks. NOTE For the purposes of this European Standard, the term “% (m/m)” is used to represent respectively the mass fraction. WARNING — The 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 applicability of regulatory limitations prior to use. 2 Principle Transformation of the glycerol and of the mono- and diglycerides into more volatile and stable silyl derivatives in presence of pyridine and of N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA). Analysis of the sample after silylation, by gas chromatography on a short capillary column with thin film thickness, with an on-column injector or equivalent device, and flame ionization detection. After a calibration procedure, the quantification of glycerol is carried out in presence of the internal standard 1,2,4-butanetriol. Mono-, di- and triglycerides are directly evaluated in presence of an internal standard for each glyceride category: glyceryl monononadecanoate (Mono C19) for monoglycerides; glyceryl dinonadecanoate (Di C38) for diglycerides; glyceryl trinonadecanoate (Tri C57) for triglycerides. 3 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 3.1 N-methyl-N-trimethysilyltrifluoroacetamide (MSTFA) 3.2 Pyridine, max. 0,1 % water, stored on molecular sieve NOTE Pyridine silyl grade (3.10) can also be used. 3.3 Tetrahydrofurane (THF) 3.4 n-Heptane 3.5 Glycerol SIST EN 14105:2011
EN 14105:2011 (E) 5 3.6 1,2,4-Butanetriol 3.7 1 - Glyceryl monononadecanoate (Mono C19)1) 3.8 1-3 Glyceryl dinonadecanoate (Di C38)2) 3.9 Glyceryl trinonadecanoate (Tri C57)3) 3.10 Pyridine, silyl grade 4 Apparatus Usual laboratory apparatus and, in particular, the following. 4.1 Gas chromatograph, equipped with an on-column injector or equivalent device, a temperature-programmable oven and a flame ionization detector. 4.2 Capillary column, capable of being programmed up to 400 °C ("high temperature" type) for which the following characteristics are advised: 100 % dimethylpolysiloxane or 95 % dimethyl-5 % diphenylpolysiloxane stationary phase; length 15 m; internal diameter 0,32 mm; film thickness 0,1 µm. 4.3 Volumetric flask, 50 ml capacity 4.4 Volumetric flasks, 20 ml capacity 4.5 Volumetric flasks, 10 ml capacity 4.6 Screw-cap vials with PTFE-faced septa, 10 ml capacity 4.7 Precision pipette, 1 ml capacity 4.8 Microsyringe, 100 µl capacity 4.9 Microsyringe, 500 µl capacity 4.10 Microsyringe, 5 µl or 10 µl capacity specially designed for on-column operation 4.11 Graduated cylinder, 10 ml capacity 4.12 Analytical balance, with an accuracy of ± 0,1 mg
1) Monononadecaoin available from Larodan, ref. 31-1900-11 (www.larodan.se) 2) 1,3-dinonadecaoin available from Larodan, ref.
32-1903-8 (www.larodan.se) 3) Trinonadecaoin available from Larodan, ref.
33-1900-13 (www.larodan.se), or from Sigma , ref. T4632-1G (www.sigmaaldrich.com) SIST EN 14105:2011
EN 14105:2011 (E) 6 4.13 Carrier gas, hydrogen or helium 4.14 Auxiliary gases, such as air, hydrogen and nitrogen 5 Preparation of solutions 5.1 1,2,4-Butanetriol stock solution, 1 mg/ml Accurately weigh approximately 50 mg (accuracy ± 0,1 mg) of 1,2,4-butanetriol (3.6) in a 50 ml volumetric flask (4.3) and make up to the mark with pyridine (3.2). 5.2 Glycerol stock solution, 0,5 mg/ml Accurately weigh approximately 50 mg (accuracy ± 0,1 mg) of glycerol (3.5) in a 10 ml volumetric flask (4.5) and make up to the mark with pyridine (3.2). Using a pipette (4.7), transfer 1 ml of this solution into a 10 ml volumetric flask (4.5) and make up to the mark with pyridine (3.2). 5.3 Standard glycerides stock solution, 2,5 mg/ml For each reference glyceride, monononadecanoate (3.7), dinonadecanoate (3.8) and trinonadecanoate (3.9), accurately weigh approximately 50 mg (accuracy ± 0,1 mg) in a unique 20 ml volumetric flask (4.4) and make up to the mark with tetrahydrofurane (3.3).
The solution shall be perfectly limpid at ambient temperature. After storage in refrigerator at 4 °C the solution might show a precipitate that must re-dissolve spontaneously when restored at ambient temperature, without any external heating. NOTE If stored at 4 °C the solution is stable for almost 3 months. 5.4 Commercial mixture of monoglycerides Made up of mono-palmitoylglycerol (monopalmitin), mono-stearoylglycerol (monostearin) and of mono-oleoylglycerol (monoolein), present in quantities having an identical mass. Prepare a stock solution of this mixture by weighing approximately 100 mg in a 10 ml volumetric flask (4.5) and make up to the mark with pyridine (3.2).
This solution may be used to locate the relevant peaks in GC paths. 5.5 Calibration solutions Prepare four calibration solutions by transferring into a series of vials (4.6) the volumes of stock solutions of glycerol (5.2) and of 1,2,4-butanetriol (5.1) given in Table 1, using the 100 µl microsyringes (4.8). Do not use syringe at maximum capacity, but dispense the half volume twice (i.e.: in case of 100 µI dosing using a 100 µI syringe, load 50 µI twice). Make sure that needle and body of the syringe are free from air bubbles, and measure volumes only by difference (i.e.: when dispensing 80 µI, fill syringe up to 100 µI and supply solution up to the 20 µI mark). SIST EN 14105:2011
EN 14105:2011 (E) 7 Table 1 — Preparation of calibration solutions Stock solution 1 2 3
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