SIST EN 14105:2024
(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 document specifies a method to determine the free glycerol and residual mono-, di- and triglyceride contents in fatty acid methyl esters (FAME). 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 1 For the purposes of this document, the term "% (m/m)" is used to represent the mass fraction.
NOTE 2 Under the common EN 14105 GC conditions, squalene can coelute with alpha glycerol monostearate. If the presence of squalene is suspected, EN 17057 can be used to discriminate between squalene and glycerol monostearate.
WARNING - The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this document to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose.
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Gehaltes an freiem und Gesamtglycerin und Mono-, Di- und Triglyceriden
Dieses Dokument legt ein Verfahren fest, um den Gehalt an freiem Glycerin und restlichen Mono-, Di- und Triglyceriden in Fettsäure-Methylestern (FAME) zu bestimmen. Der Gesamtglyceringehalt wird anschließend aus den erhaltenen Ergebnissen berechnet.
Die Bestimmungsgrenzen sind unter den beschriebenen Bedingungen 0,001 % (m/m) für freies Glycerin und 0,10 % (m/m) für alle Glyceride (Mono-, Di- und Tri-). Das Verfahren ist geeignet für FAME aus Rapsöl, Sonnenblumenöl, Sojaöl, Palmöl, tierischen Ölen und Fetten und für deren Mischungen. Es ist nicht geeignet für FAME aus oder mit Kokosnuss- und Palmkernölderivaten, da hier verschiedene überlappende Glyceridpeaks auftreten.
ANMERKUNG 1 Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck „% (m/m)“ verwendet.
ANMERKUNG 2 Unter den allgemeinen GC-Bedingungen nach EN 14105 kann Squalen mit Alpha-Glycerin-Monostearat koeluieren. Falls die Anwesenheit von Squalen vermutet wird, kann EN 17057 zur Unterscheidung zwischen Squalen und Glycerin-Monostearat angewendet werden.
WARNUNG — Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieses Dokuments, vor der Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen, und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.
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
Le présent document spécifie une méthode de détermination des teneurs en glycérol libre et en mono-, di- et triglycérides résiduels des esters méthyliques d’acides gras (EMAG). La teneur en glycérol total est ensuite calculée à partir des résultats obtenus.
Dans les conditions décrites, les limites de quantification 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 dérivés d’huiles de coprah ou de palmiste, ou contenant ces dérivés, en raison du chevauchement de différents pics de glycérides.
NOTE 1 Pour les besoins du présent document, l’expression « % (m/m) » est utilisée pour représenter la fraction massique.
NOTE 2 Dans les conditions de CPG courantes indiquées dans l’EN 14105, le squalène peut coéluer avec le monostéarate de glycérol alpha. Si la présence de squalène est suspectée, l’EN 17057 peut être utilisée pour distinguer le squalène du monostéarate de glycérol.
AVERTISSEMENT - L’utilisation du présent document peut impliquer la mise en oeuvre de matériaux, d’opérations et de matériels dangereux. Ce document ne prétend pas couvrir tous les problèmes de sécurité liés à son utilisation. Il incombe aux utilisateurs du présent document de prendre, avant son application, des mesures appropriées de protection de la sécurité et de la santé du personnel et de s’assurer que les exigences statutaires et réglementaires sont satisfaites.
Derivati maščob in olj - Metil estri maščobnih kislin (FAME) - Določevanje vsebnosti prostega in celotnega glicerola ter mono-, di- in trigliceridov
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2024
Nadomešča:
SIST EN 14105:2021
Derivati maščob in olj - Metil estri maščobnih kislin (FAME) - Določevanje
vsebnosti prostega in celotnega glicerola ter mono-, di- in trigliceridov
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and
total glycerol and mono-, di-, triglyceride contents
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester
(FAME) - Bestimmung des Gehaltes an freiem und Gesamtglycerin und Mono-, Di- und
Triglyceriden
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
Ta slovenski standard je istoveten z: EN 14105:2024
ICS:
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 14105
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2024
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14105:2020
English 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 Erzeugnisse aus pflanzlichen und tierischen Fetten und
d'acides gras (EMAG) - Détermination de la teneur en Ölen - Fettsäure-Methylester (FAME) - Bestimmung
glycérols libre et total et en mono-, di- et triglycérides des Gehaltes an freiem und Gesamtglycerin und Mono-,
Di- und Triglyceriden
This European Standard was approved by CEN on 12 August 2024.
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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14105:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Chemicals . 5
6 Apparatus . 5
7 Preparation of solutions . 6
7.1 1,2,4-Butanetriol stock solution, 1 mg/ml . 6
7.2 Glycerol stock solution, 0,5 mg/ml . 6
7.3 Standard glycerides stock solution, 2,5 mg/ml. 6
7.4 Commercial mixture of monoglycerides . 6
7.5 Calibration solutions . 6
8 Sampling . 7
9 Procedure . 7
9.1 Operating conditions . 7
9.2 Analysis of the calibration solutions. 7
9.3 Analysis of the commercial mixture of monoglycerides . 7
9.4 Preparation and analysis of the samples . 8
9.5 Identification . 8
9.6 Calibration . 8
9.7 Column performance control . 8
10 Determination of results . 9
10.1 Integration of the peaks . 9
10.2 Glycerol calibration function . 9
10.3 Free glycerol . 9
10.4 Glycerides . 9
10.5 Total glycerol . 10
11 Expression of results . 10
12 Precision . 10
12.1 Interlaboratory study (ILS) . 10
12.2 Repeatability, r . 10
12.3 Reproducibility, R . 11
13 Test report . 11
Annex A (informative) Sample chromatogram . 12
Annex B (informative) Calibration function calculation. 21
Annex C (informative) Worked example of calibration function calculation . 23
Annex D (informative) Results of the interlaboratory trial . 25
Bibliography . 27
European foreword
This document (EN 14105:2024) 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 April 2025, and conflicting national standards shall be
withdrawn at the latest by April 2025.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 14105:2020.
In comparison with the previous edition, the following technical modifications have been made:
— the weighing accuracy is specified.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
1 Scope
This document specifies a method to determine the free glycerol and residual mono-, di- and
triglyceride contents in fatty acid methyl esters (FAME). 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 1 For the purposes of this document, the term “% (m/m)” is used to represent the mass fraction.
NOTE 2 Under the common EN 14105 GC conditions, squalene can coelute with alpha glycerol monostearate. If
the presence of squalene is suspected, EN 17057 can be used to discriminate between squalene and glycerol
monostearate.
WARNING — The use of this document can involve hazardous materials, operations and equipment.
This document does not purport to address all of the safety problems associated with its use. It is the
responsibility of users of this document to take appropriate measures to ensure the safety and health of
personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this
purpose.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 5555, Animal and vegetable fats and oils — Sampling (ISO 5555)
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
The glycerol and the mono- and diglycerides are transformed into more volatile and stable silyl
derivatives in presence of pyridine and of N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA).
The sample after silylation is analysed 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.
5 Chemicals
Use only chemicals of recognized analytical grade, unless otherwise specified.
5.1 N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA).
5.2 Pyridine, max. 0,1 % water, stored on molecular sieve.
Pyridine silyl grade (5.10) can also be used.
5.3 Tetrahydrofurane (THF).
5.4 n-Heptane.
5.5 Glycerol.
5.6 1,2,4-Butanetriol.
5.7 1-Glyceryl monononadecanoate (Mono C19).
5.8 1-3 Glyceryl dinonadecanoate (Di C38).
5.9 Glyceryl trinonadecanoate (Tri C57).
5.10 Pyridine, silyl grade.
6 Apparatus
Usual l
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