EN 14110:2019

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

This document specifies a method for the determination of the methanol content of fatty acid methyl esters (FAME) for use as diesel fuel and domestic heating fuel. The method is applicable to methanol contents between 0,01 % (m/m) and 0,5 % (m/m). The method is not applicable to mixtures of FAME containing other low boiling components.
NOTE   For the purposes of this document, the terms "% (m/m)" and "% (V/V)" are used to represent respectively the mass fraction and the volume fraction.
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 Methanolgehaltes

Dieses Dokument legt ein Verfahren zur Bestimmung des Methanolgehaltes von Fettsäure-Methyl-estern (FAME) fest, die für den Gebrauch als Dieselkraftstoff oder als Heizöl vorgesehen sind. Dieses Verfahren ist anwendbar auf Methanolgehalte von 0,01 % (m/m) bis 0,5 % (m/m). Dieses Verfahren ist nicht anwendbar auf FAME-Mischungen, die andere niedrig siedende Komponenten enthalten.
ANMERKUNG   Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck "% (m/m)" und für den Volumenanteil einer Substanz der Ausdruck "% (V/V)" verwendet.
WARNUNG - Die Anwendung dieser Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheits¬probleme 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.

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

Le présent document décrit une méthode de détermination de la teneur en méthanol des esters méthyliques d’acides gras (EMAG) utilisés dans le gazole et le combustible de chauffage domestique. Cette méthode est applicable aux teneurs en méthanol comprises entre 0,01 % (m/m) et 0,5 % (m/m). Elle n’est pas applicable aux mélanges d’EMAG qui contiennent d’autres composants à bas point d’ébullition.
NOTE   Pour les besoins du présent document, les termes « % (m/m) » et « % (V/V) » servent à représenter respectivement la fraction massique et la fraction volumique.
AVERTISSEMENT - L’utilisation du présent document peut impliquer des réactifs, manipulations ou matériels dangereux. Le présent document n’a pas pour but de traiter tous les problèmes de sécurité qui sont liés à son utilisation. Il est de la responsabilité des utilisateurs du présent document de prendre les mesures appropriées pour préserver la santé et garantir la sécurité du personnel avant application de la norme, et de s’assurer que les exigences réglementaires et légales sont respectées.

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

Ta evropski standard določa metodo določevanja vsebnosti metanola v metilnih estrih maščobnih kislin (FAME), ki se uporabljajo kot dizelsko gorivo in gorivo za ogrevanje gospodinjstev. Metoda se uporablja za koncentracijsko območje od 0,01 % do 0,5 % (m/m) metanola. Metoda se ne uporablja za mešanice metilnih estrov maščobnih kislin, ki vsebujejo druge komponente z nizkim vreliščem.

General Information

• Status: Published
• Publication Date: 09-Apr-2019
• Withdrawal Date: 30-Oct-2019
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: CEN/TC 307 - Oilseeds, vegetables and animal fats and oils and their by-products - Methods of sampling and analys
• Drafting Committee: CEN/TC 307 - Oilseeds, vegetables and animal fats and oils and their by-products - Methods of sampling and analys
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 03-Dec-2024
• Completion Date: 14-Apr-2025
• Mandate: M/245 - Mandate to CEN for the elaboration and adoption of standards concerning minimum requirement specifications including test methods for Fatty Acid MethylEster (FAME) as fuel for diesel engines and for space heating
• Ref Project: SIST EN 14110:2019 - Fat and oil derivatives - Fatty Acid Methyl Esters - Determination of methanol content

Relations

• Replaces: EN 14110:2003 - Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of methanol content
• Effective Date: 18-Jan-2017

Overview

EN 14110:2019 (CEN) specifies a laboratory method for the determination of methanol content in Fatty Acid Methyl Esters (FAME) intended for use as diesel fuel and domestic heating fuel. The method is applicable to methanol concentrations in FAME from 0,01 % (m/m) to 0,5 % (m/m) and is not applicable to FAME mixtures containing other low‑boiling components. The procedure uses headspace sampling and gas chromatography with flame ionization detection (GC‑FID) and allows quantification by either internal or external calibration.

Key topics and requirements

• Scope and limits: Valid for methanol in FAME between 0,01–0,5 % (m/m); excludes FAME with other low‑boiling components.
• Principle: Samples are sealed in headspace vials, heated (typical equilibrium temperature 80 °C, example equilibrium time 45 min) to desorb methanol to the gas phase; a defined gas phase volume is injected into GC and methanol is detected with FID.
• Calibration options:
  • Procedure A - Internal calibration (preferred for manual or small sample sets): uses 2‑propanol as internal standard.
  • Procedure B - External calibration: recommended with automatic headspace equipment for higher throughput.
• Calibration standards: Example calibration solutions at approximately 0,5 %, 0,1 % and 0,01 % (m/m) methanol prepared in reference FAME.
• Apparatus and consumables: headspace vials (20 ml), inert septa, syringes (10 µl and 500 µl gas syringe), GC with capillary column and FID. Suitable stationary phases include methylpolysiloxane (e.g., DB‑1/SE30) or polyethylene glycol (e.g., DBWAX/CARBOWAX).
• Analytical performance: GC conditions must achieve a resolution ≥ 1,5 between methanol and 2‑propanol; precision sections cover repeatability and reproducibility (see standard for interlaboratory results).
• Safety: Standard warns of hazardous materials and operations; users must follow applicable health, safety and regulatory requirements.

Applications and users

• Who uses it: biodiesel and FAME producers, fuel quality control laboratories, heating fuel suppliers, conformity assessment bodies, regulatory authorities and testing laboratories.
• Practical value:
  • Ensures compliance of biodiesel/diesel blends and heating fuels with methanol limits.
  • Detects residual methanol that can affect fuel stability, engine performance and safety.
  • Supports quality control during production, storage and before commercialization.

Related standards

• EN ISO 3170, EN ISO 3171 - sampling of petroleum liquids (normative references for sample collection).
• EN 14110:2019 supersedes EN 14110:2003 (updated procedural and calibration details).

For implementation, consult the full EN 14110:2019 text for step‑by‑step procedures, calibration formulas, precision data and required reporting elements.

Standards Content (Sample)

SLOVENSKI STANDARD
01-julij-2019
Nadomešča:
SIST EN 14110:2003
Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje
metanola
Fat and oil derivatives - Fatty Acid Methyl Esters - Determination of methanol content
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester
(FAME) - Bestimmung des Methanolgehaltes
Produits dérivés des corps gras - Esters méthyliques d'acides gras - Détermination de la
teneur en méthanol
Ta slovenski standard je istoveten z: EN 14110:2019
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 14110
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2019
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14110:2003
English Version
Fat and oil derivatives - Fatty Acid Methyl Esters -
Determination of methanol content
Produits dérivés des corps gras - Esters méthyliques Erzeugnisse aus pflanzlichen und tierischen Fetten und
d'acides gras - Détermination de la teneur en méthanol Ölen - Fettsäure-Methylester (FAME) - Bestimmung
des Methanolgehaltes
This European Standard was approved by CEN on 13 December 2019.

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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14110:2019 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 Reagents . 4
6 Apparatus . 5
7 Sampling . 6
8 Operation conditions . 6
8.1 Analytical conditions . 6
8.2 Operation . 7
9 Calibration solutions . 7
10 Procedure. 7
10.1 General . 7
10.2 Procedure A — Internal calibration . 7
10.2.1 General . 7
10.2.2 Internal calibration . 8
10.2.3 Analysis and Calculation using internal calibration. 8
10.3 Procedure B — External calibration . 9
10.3.1 General . 9
10.3.2 External calibration . 9
10.3.3 Analysis and calculation using external calibration . 9
11 Precision . 9
11.1 General . 9
11.2 Repeatability . 9
11.3 Reproducibility . 10
12 Test report . 10
Annex A (informative) Results on an interlaboratory study . 11
Annex B (informative) Example of a chromatogram for procedure A . 12
Bibliography . 13

European foreword
This document (EN 14110:2019) 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 2019, and conflicting national standards shall
be withdrawn at the latest by October 2019.
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 14110:2003.
This document has been prepared under mandate M/245 on Fatty Acid Methyl Ester (FAME) given to
CEN by the European Commission and the European Free Trade Association.
Significant changes between this document and EN 14110:2003 are:
— Addition of Formula (1) — resolution between methanol and 2-propanol
— Correction of the Formula to calculate the methanol content based on external calibration
— Addition of Clause 2 — Normative References
— Addition of Clause 7 — Sampling
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, 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 for the determination of the methanol content of fatty acid methyl
esters (FAME) for use as diesel fuel and domestic heating fuel. The method is applicable to methanol
contents between 0,01 % (m/m) and 0,5 % (m/m). The method is not applicable to mixtures of FAME
containing other low boiling components.
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent
respectively the mass fraction and the volume fraction.
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 3170, Petroleum liquids — Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
The sample is heated at 80 °C in a hermetically sealed vial to allow desorption of contained methanol into
the gas phase. When the equilibrium is reached a defined part of the gas phase is injected into a gas
chromatograph, where methanol is detected with a flame ionization detector.
The amount of methanol can be determined either by internal calibration (procedure A) or by external
calibration (procedure B).
If only manual equipment is available then only internal standard calibration should be used.
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
5.1 Methanol, of known purity greater than 99,5 %.
5.2 2-propanol, of known purity, greater than 99,5 % (for procedure A, internal calibration).
5.3 Reference FAME, with a methanol content less than 0,001 % (m/m).
Reference FAME can either be obtained from commercial sources or by washing FAME three to five times
with distilled water in a separator funnel. FAME should be then dried by heating at 90 °C under stirring
and reduced pressure.
5.4 Carrier gas, nitrogen, helium or hydrogen, of know purity greater than 99 %.
6 Apparatus
6.1 Head space vials, 20 ml capacity.
1)
6.2 Inert septa (e.g. TFE or Viton ) and metallic caps.
6.3 Syringe, 10 µl, accurate to 0,1 µl.
6.4 Gas syringe 500 µl, fitted with a valve (for manual procedure).
6.5 Crimping pliers.
6.6 Pipettes, of 1 ml, 2 ml, 5 ml capacity.
6.7 Volumetric flasks, capacity 10 ml and 25 ml.
6.8 Gas chromatograph, equipped with a capillary column, suitable injector (automatic headspace
system or a split/splitless injector) and flame ionization detector, integrator.
6.9 Capillary column, the column shall elute methanol as a symmetrical peak. Stationary phases like
2) 2) 2) 2)
methylpolysiloxane (e.g. DB1 , SE30 ) or polyethylenglycol (e.g. DBWAX , CARBOWAX ) can be
used successfully and a film thickness of minimum 0,5 µm is recommended.
The use of a packed column equipped by one of the above mentioned stationary phases or of Chromosorb
2)
101 is also allowed.
6.10 Automatic headspace equipment
The automatic headspace equipment used shall have an accuracy of 1 % or better concerning
experimental conditions like equilibrium temperatur
...