EN 16476:2014

Liquid petroleum products - Determination of Sodium, Potassium, Calcium, Phosphorus, Copper and Zinc contents in diesel fuel - Method via Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES)

This European Standard specifies an inductively coupled plasma optical emission spectrometry (ICP OES) method for the determination of sodium, potassium, calcium, phosphorus, copper and zinc concentrations of diesel fuels, including those containing up to 30 % (V/V) fatty acid methyl ester (FAME), in the range detailed in Table 1. These six elements are considered as the most essential ash forming elements.

Flüssige Mineralölerzeugnisse - Bestimmung des Gehalts an Natrium, Kalium, Calcium, Phosphor, Kupfer, Zink in Dieselkraftstoffen - Direkte Bestimmung durch optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES)

Diese Europäische Norm legt ein Verfahren zur Bestimmung der Konzentrationen von Natrium, Kalium, Calcium, Phosphor, Kupfer und Zink von Dieselkraftstoffen im in Tabelle 1 angegebenen Bereich durch optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) fest, einschließlich solchen, die bis zu 30 % (V/V) Fettsäuremethylester (FAME) enthalten. Diese sechs Elemente gelten als die wichtigsten Asche bildenden Elemente.
ANMERKUNG   Für die Anwendung der vorliegenden Europäischen Norm wird der Ausdruck „% (V/V)“ verwendet, um den Volumenanteil  darzustellen.
WARNUNG  Die Anwendung dieser Europäischen Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Europäische Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieser Europäischen Norm ist dafür verantwortlich, vorher angemessene Maßnahmen in Hinblick auf Sicherheit

Produits pétroliers liquides - Détermination des concentrations en sodium, potassium, calcium, phosphore, cuivre et zinc dans le gazole - Méthode par spectrométrie d’émission atomique par plasma à couplage inductif (ICP OES)

Tekoči naftni proizvodi - Določevanje natrija, kalija, kalcija, fosforja, bakra in cinka v dizelskem gorivu - Metoda z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-OES)

Standard EN 16476 določa metodo optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP OES) za določevanje koncentracije natrija, kalija, kalcija, fosforja, bakra in cinka v dizelskih gorivih, vključno s tistimi, ki vsebujejo do 30 % (V/V) metilnih estrov maščobnih kislin (FAME), v mejah, določenih v tabeli 1. Teh šest elementov je ključnih pri ustvarjanju pepela.

General Information

• Status: Published
• Publication Date: 06-May-2014
• Withdrawal Date: 29-Nov-2014
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Drafting Committee: CEN/TC 19/WG 27 - Elemental analysis of petroleum and related products
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 23-Jul-2025
• Completion Date: 23-Sep-2025
• Ref Project: SIST EN 16476:2014 - Liquid Petroleum products - Determination of Sodium, Potassium, Calcium, Phosphorus, Copper and Zinc contents in diesel fuel - Method via Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

Overview

EN 16476:2014 (CEN) specifies an analytical method using Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) for the determination of six key ash‑forming elements - sodium, potassium, calcium, phosphorus, copper and zinc - in diesel fuel. The method applies to conventional diesel and diesel containing up to 30 % (V/V) fatty acid methyl ester (FAME). It defines sample preparation, instrumentation, calibration, and quality checks for accurate quantification within the ranges given in the standard.

Key Topics

• Analytes and scope: Determination of Na, K, Ca, P, Cu and Zn - the six most essential ash‑forming elements identified by vehicle manufacturers. Applicable to diesel fuels including blends up to 30% FAME.
• Principle: Weigh sample, dilute with an oil‑free organic solvent (kerosene recommended), and directly introduce into an ICP OES. An internal standard (Co, Sc or Y) corrects viscosity and matrix effects.
• Sample handling & containers: Sampling per EN ISO 3170 / EN ISO 3171. Use plastic containers (HDPE, FEP, PP or PFA) or coated metallic containers to avoid contamination.
• Reagents & gases: High‑purity kerosene (low background element content) and argon (w(Ar) ≥ 99.996 %). Small oxygen additions to plasma gas may be used to reduce carbon deposits.
• Instrumentation & wavelengths: ICP OES configured for organic liquids with a feed pump and organic‑compatible tubing. The standard recommends specific analytical wavelengths for each element (e.g., Na and K resonance lines) and suggests a vertically oriented, radially observed plasma to minimize carbon interference.
• Calibration & QC: Preparation of multi‑level calibration solutions and an internal standard solution; calibration check solution to verify accuracy and sensitivity. Detailed procedures for calibration, calibration checks and sample measurement are provided.
• Safety & quality: Notes on potential hazards, contamination prevention (acid rinsing to avoid phosphate contamination), and laboratory best practices.

Applications

• Fuel testing laboratories performing regulatory or quality control analysis of diesel fuels and diesel/biodiesel blends.
• Refineries and fuel blenders monitoring metal contamination during production and storage.
• Vehicle and engine manufacturers assessing risks to diesel particulate filters (DPF) and after‑treatment systems - metals can have greater impact on DPF durability than bulk ash.
• Regulatory bodies and standards organizations requiring reproducible, comparable data for fuel specifications.

Related Standards

• EN ISO 3170 / EN ISO 3171 - sampling of petroleum liquids
• EN ISO 1042 - volumetric glassware (for preparation)
• Other CEN fuel testing standards and manufacturer specifications for ash and contaminant limits

Keywords: EN 16476:2014, ICP OES, diesel fuel analysis, sodium potassium calcium phosphorus copper zinc, FAME, ash forming elements, fuel testing laboratories, DPF.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.LQGXNWLYQRFlüssige Mineralölerzeugnisse - Bestimmung des Gehalts an Natrium, Kalium, Calcium, Phosphor, Kupfer, Zink in Dieselkraftstoffen - Direkte Bestimmung durch optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES)Produits pétroliers liquides - Détermination des teneurs en Sodium, Potassium, Calcium, Phosphore, Cuivre et Zinc dans le gazole - Méthode par spectrométrie d'émission atomique à couplage inductif par plasma (ICP OES)Liquid Petroleum products - Determination of Sodium, Potassium, Calcium, Phosphorus, Copper and Zinc contents in diesel fuel - Method via Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 16476:2014SIST EN 16476:2014en,fr,de01-julij-2014SIST EN 16476:2014SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16476
May 2014 ICS 75.160.20 English Version
Liquid petroleum products - Determination of Sodium, Potassium, Calcium, Phosphorus, Copper and Zinc contents in diesel fuel - Method via Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES)
Produits pétroliers liquides - Détermination des concentrations en sodium, potassium, calcium, phosphore, cuivre et zinc dans le gazole - Méthode par spectrométrie d'émission atomique par plasma à couplage inductif (ICP OES)
Flüssige Mineralölerzeugnisse - Bestimmung des Gehalts an Natrium, Kalium, Calcium, Phosphor, Kupfer, Zink in Dieselkraftstoffen - Direkte Bestimmung durch optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) This European Standard was approved by CEN on 20 March 2014.
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, 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:
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B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16476:2014 ESIST EN 16476:2014

Page Foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references . 5 3 Principle . 5 4 Reagents . 5 5 Apparatus . 6 6 Sampling . 8 7 Preparation of calibration solutions . 8 7.1 General . 8 7.2 Internal Standard solution . 8 7.3 Calibration solutions . 8 7.4 Calibration check solution . 9 8 Calibration . 9 8.1 General . 9 8.2 Calibration of the ICP OES spectrometer . 9 8.3 Procedure A . 10 8.4 Procedure B . 10 8.5 Check of calibration . 10 9 Sample analysis . 11 9.1 Sample preparation . 11 9.2 Sample measurement . 11 10 Calculation . 12 11 Expression of result . 12 12 Precision . 12 12.1 General . 12 12.2 Repeatability . 12 12.3 Reproducibility . 12 13 Test report . 13 Bibliography . 14
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