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.

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23-Jan-2018
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SLOVENSKI STANDARD
SIST EN 17057:2018
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
SIST EN 17057:2018 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17057:2018
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SIST EN 17057:2018
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.
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SIST EN 17057:2018
EN 17057:2018 (E)
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

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SIST EN 17057:2018
EN 17057:2018 (E)
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.
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SIST EN 17057:2018
EN 17057:2018 (E)
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.
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SIST EN 17057:2018
EN 17057:2018 (E)
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. Oth
...

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