EN 17057:2018
(Main)Automotive fuels and fat and oil derivates - Determination of saturated monoglycerides content in Fatty Acid Methyl Esters (FAME) - Method by GC-FID
Automotive fuels and fat and oil derivates - Determination of saturated monoglycerides content in Fatty Acid Methyl Esters (FAME) - Method by GC-FID
This document specifies a method to determine the saturated monoglyceride content in Fatty Acid Methyl Esters (FAME). This method only identifies and quantifies the following saturated monoglycerides: 1-C16:0, 2-C16:0 and 1-C18:0. The total saturated monoglyceride content is calculated by the summation of the contents of these three saturated monoglycerides. The precision has been established for FAMEs having saturated monoglycerides in the (200 to 1 500) mg/kg range.
This method is not suitable for FAME produced from or containing coconut and palm kernel oil derivatives because of overlapping of various peaks.
NOTE This Standard determines only three saturated monoglycerides, i.e. 1-C16:0, 2-C16:0 and 1-C18:0. FAMEs can contain also other saturated monoglycerides such as 1-C17:0, but these are generally much lower than the three targeted saturated monoglycerides and are therefore not included in the Standard's scope.
WARNING - The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard 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.
Kraftstoffe und Erzeugnisse aus Fetten und Ölen - Bestimmung des Gehalts an gesättigten Monoglyceriden in Fettsäure-Methylester (FAME) - Verfahren mit GC-FID
Dieses Dokument legt ein Verfahren zur Bestimmung des Gehaltes an gesättigten Monoglyceriden in Fettsäure-Methylestern (FAME) fest. Mit diesem Verfahren werden ausschließlich die folgenden gesättigten Monoglyceride bestimmt und quantifiziert: 1-C16:0, 2-C16:0 und 1-C18:0. Der Gesamtgehalt an gesättigten Monoglyceriden wird durch Aufsummieren der Einzelgehalte dieser drei gesättigten Monoglyceride berechnet. Die Präzision wurde für Fettsäure-Methylester mit einem Gehalt an gesättigten Monoglyceriden im Bereich von 200 mg/kg bis 1 500 mg/kg nachgewiesen.
Das Verfahren ist nicht geeignet für Fettsäure-Methylester, die auf der Basis von Kokosnuss- und Palmkernölderivaten gewonnen wurden, da sich verschiedene Peaks überschneiden.
ANMERKUNG Mit diesem Verfahren werden ausschließlich drei gesättigte Monoglyceride bestimmt, d. h. 1-C16:0, 2-C16:0 und 1-C18:0. Fettsäure-Methylester können auch andere gesättigte Monoglyceride wie 1-C17:0 enthalten; allerdings sind diese in der Regel in wesentlich geringerer Konzentration vorhanden als die drei vorgenannten gesättigten Monoglyceride und wurden somit nicht in den Anwendungsbereich dieser Norm aufgenommen.
WARNUNG - Die Anwendung dieser Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieser Norm, vor ihrer 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.
Carburants pour automobiles et produits dérivés des corps gras - Détermination de la teneur en monoglycérides saturés (SMG) des esters méthyliques d'acides gras (EMAG) - Méthode par GC-FID
Le présent document spécifie une méthode permettant de déterminer la teneur en monoglycérides saturés (SMG) dans les esters méthyliques d'acides gras (EMAG). Cette méthode identifie et quantifie uniquement les SMG suivants : 1-C16:0, 2-C16:0 et 1-C18:0. La teneur totale en monoglycérides saturés est calculée en additionnant les teneurs de ces trois SMG. La fidélité a été établie pour des EMAG contenant des monoglycérides saturés dans une proportion de (200 à 1 500) mg/kg.
Cette méthode ne convient pas aux EMAG produits à partir de dérivés d'huile de noix de coco et de palmiste, ou en contenant, en raison du chevauchement de différents pics.
NOTE La présente norme détermine uniquement trois monoglycérides saturés, à savoir les 1-C16:0, 2-C16:0 et 1-C18:0. Les EMAG peuvent également contenir d'autres SMG, tels que le 1-C17:0, mais ceux-ci ont généralement une teneur bien inférieure à celle des trois monoglycérides saturés ciblés, et ne sont donc pas inclus dans le domaine d’application de la présente norme.
AVERTISSEMENT — L'utilisation de la présente norme peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente norme ne prétend pas aborder tous les problèmes de sécurité associés à son utilisation. Il incombe à l'utilisateur de la présente norme de prendre les mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant l’application de la norme, et satisfaire aux exigences légales et réglementaires applicables à cet effet.
Goriva za motorna vozila ter maščobni in oljni derivati - Določevanje nasičenih monogliceridov v metilnih estrih maščobnih kislin (FAME) - Metoda z GC-FID
Družina komunikacijskih profilov 1 (splošno znana kot FOUNDATION™ Fieldbus1) opredeljuje komunikacijske profile, osnovane na IEC 61158-2, tipu 1, IEC 61158-3-1, IEC 61158-4-1, IEC 61158-5-5, IEC 61158-5-9, IEC 61158-6-5 in IEC 61158-6-9. Osnovni profili CP 1/1 (FF H1) in CP 1/2 (FF HSE) so določeni v IEC 61784-1. Ta del IEC 62453 podaja informacije za integriranje FOUNDATION™ Fieldbus (FF) protokola v standard orodja procesne naprave (IEC 62453-2). Standard opisuje definicije komunikacij, za protokol značilne podaljške ter pomene prikaza bloka (npr. pretvornik, izvorni ali funkcijski blok). Definicije, značilne za novi protokol, so osnovane na specifikacijah FF za protokola H1 in HSE. Poleg tega definicije vsebujejo informacije, ki jih potrebujejo sistemi za konfiguracijo naprav FF. Obseg je omejen na FOUNDATION™ Fieldbus napravo ter na definicije, ki so značilne za sistem.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-april-2018
*RULYD]DPRWRUQDYR]LODWHUPDãþREQLLQROMQLGHULYDWL'RORþHYDQMHQDVLþHQLK
PRQRJOLFHULGRYYPHWLOQLKHVWULKPDãþREQLKNLVOLQ)$0(0HWRGD]*&),'
Automotive fuels and fat and oil derivates - Determination of saturated monoglycerides
content in Fatty Acid methyl Esters (FAME) - Method by GC-FID
Autoraftstoffe und erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen -
Bestimmung des Gehalts von gesättigter Monoglyceride in Fettsäure-Methylester
(FAME) - Methode mittels GC-FID
Combustibles et produits dérivés des corps gras - Détermination de la teneur des
monoglycerides saturés en esters méthyliques d'acides gras (EMAG) - Méthode par GC-
FID
Ta slovenski standard je istoveten z: EN 17057:2018
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17057
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2018
EUROPÄISCHE NORM
ICS 75.160.20
English Version
Automotive fuels and fat and oil derivates - Determination
of saturated monoglycerides content in Fatty Acid Methyl
Esters (FAME) - Method by GC-FID
Carburants pour automobiles et produits dérivés des Kraftstoffe und Erzeugnisse aus Fetten und Ölen -
corps gras - Détermination de la teneur en Bestimmung des Gehalts an gesättigten
monoglycérides saturés (SMG) des esters méthyliques Monoglyceriden in Fettsäure-Methylester (FAME) -
d'acides gras (EMAG) - Méthode par GC-FID Verfahren mit GC-FID
This European Standard was approved by CEN on 19 November 2017.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey 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
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17057:2018 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Principle . 4
4 Reagents and materials . 4
5 Apparatus . 5
6 Preparation of solutions . 5
6.1 Glyceryl monononadecanoate stock solution, 2,5 mg/ml . 5
6.2 Reference solution . 6
7 Sampling . 6
8 Procedure. 6
8.1 Operating conditions . 6
8.2 Column evaluation . 7
8.3 Analysis of the reference solution . 7
8.4 Preparation and analysis of the samples . 8
8.5 Identification . 8
8.6 Calibration . 8
9 Determination of results . 8
9.1 Integration of the peaks . 8
9.2 Calculation . 9
10 Expression of results . 9
11 Precision . 9
11.1 General . 9
11.2 Repeatability, r . 10
11.3 Reproducibility, R . 10
12 Test report . 10
Annex A (informative) Saturated monoglyceride standards . 11
Annex B (informative) Calculation of column performance . 12
Annex C (informative) Example chromatograms . 14
Bibliography . 15
European foreword
This document (EN 17057:2018) has been prepared by Technical Committee CEN/TC 19 “Gaseous and
liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the
secretariat of which is held by NEN.
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 July 2018 and conflicting national standards shall be
withdrawn at the latest by July 2018.
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.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
1 Scope
This document specifies a method to determine the saturated monoglyceride content in Fatty Acid
Methyl Esters (FAME). This method only identifies and quantifies the following saturated
monoglycerides: 1-C16:0, 2-C16:0 and 1-C18:0. The total saturated monoglyceride content is calculated
by the summation of the contents of these three saturated monoglycerides. The precision has been
established for FAMEs having saturated monoglycerides in the (200 to 1 500) mg/kg range.
This method is not suitable for FAME produced from or containing coconut and palm kernel oil
derivatives because of overlapping of various peaks.
NOTE This Standard determines only three saturated monoglycerides, i.e. 1-C16:0, 2-C16:0 and 1-C18:0.
FAMEs can contain also other saturated monoglycerides such as 1-C17:0, but these are generally much lower than
the three targeted saturated monoglycerides and are therefore not included in the Standard's scope.
WARNING — The use of this standard can involve hazardous materials, operations and
equipment. This standard does not purport to address all of the safety problems associated with
its use. It is the responsibility of the user of this standard 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, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171)
3 Principle
The saturated monoglycerides are converted into more stable and volatile silyl derivatives in the
presence of pyridine and N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA).
After silylation, the sample is analysed by gas chromatography on a capillary column with thin film
thickness, an on-column injector or equivalent device (e.g. programmed-temperature vaporizing
injector), and a flame ionization detector.
The quantification of the saturated monoglycerides is performed against the internal standard (IS)
Glyceryl monononadecanoate (mono C19), using a relative response factor of 1,00.
4 Reagents and materials
Use only reagents of recognized analytical grade. The reagents should not contain components that
chromatographically co-elute with the target components, i.e. 1-C16:0, 2-C16:0 and 1-C18:0.
NOTE Annex A shows a list of suppliers for saturated monoglyceride standards.
4.1 N-methyl-N-trimethysilyltrifluoroacetamide (MSTFA) [CAS: 24589-78-4], p.a.
4.2 Pyridine, [CAS: 110-86-1], max. 0,1 % water, stored on molecular sieve.
4.3 n-Heptane, [CAS: 142-82-5], p.a.
4.4 2-Hexadecanoyl-glycerol ( 2 −C ), [CAS: 23470-00-0], of > 99,0 % purity.
16:0
4.5 1-Hexadecanoyl-rac-glycerol ( 1 −C ), [CAS: 542-44-9], of > 99,0 % purity.
16:0
4.6 1-Octadecanoyl-rac-glycerol ( 1 −C ), [CAS: 123-94-4], of > 99,0 % purity.
18:0
4.7 1-Nonadecanoyl-rac-glycerol ( 1 −C ), [CAS: 112340-30-4], of > 99,0 % purity.
19:0
4.8 Squalene [CAS: 111-02-4] ((6E,10E,14E,18E)-2,6,10,15,19,23-Hexamethyltetracosa-
2,6,10,14,18,22-hexaene), of > 99,0 % purity.
4.9 n-Hexacosane [CAS: 630-01-3] (n-C26), of > 99,0 % purity.
4.10 n-Octacosane [CAS: 630-02-4] (n-C28), of > 99,0 % purity.
4.11 Carrier gas, hydrogen or helium, minimum 99,999 % purity.
4.12 Auxiliary gases, such as air, hydrogen and nitrogen, minimum 99,995 % purity.
5 Apparatus
Usual laboratory apparatus and glassware, together with the following:
5.1 Gas chromatograph, equipped with an on-column injector or equivalent device (e.g. PTV:
Programmed Temperature Vaporisor), a temperature programmable oven and a flame ionization
detector.
5.2 Capillary column, capable of being programmed up to 400 °C (“high temperature” type), e.g.
5.2.1 or 5.2.2. Other columns with similar performance may be used. Such columns should be tested
first before being selected as co-elution may occur.
5.2.1 DB 5HT (5 % phenyl, 95 % methylpolysiloxane), 30 m x 0,25 mm, 0,1 µm film thickness.
5.2.2 CP9078, 15 m x 0,32 mm, 0,1 µm film thickness.
5.3 Volumetric flasks, 10, 20 and 50 ml capacity.
5.4 Screw-cap vials with PTFE-faced septa, 10 ml capacity.
5.5 Precision pipette, 1 ml capacity.
5.6 Microsyringes, 100 μl and 500 μl capacity.
5.7 Graduated cylinder, 10 ml capacity.
5.8 Analytical balance, with an accuracy of ± 0,1 mg.
6 Preparation of solutions
6.1 Glyceryl monononadecanoate stock solution, 2,5 mg/ml
Accurately weigh approximately 50 mg (accuracy ± 0,1 mg) of glyceryl monononadecanoate (1-C19:0,
4.7) in a 20 ml volumetric flask (5.3) and make up to the mark with pyridine (4.2).
The solution shall be perfectly clear at ambient temperature. After storage in refrigerator at 4 °C the
solution might show a precipitate that shall spontaneously re-dissolve when put at ambient
temperature, without any external heat
...
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