SIST EN 16476:2014
(Main)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)
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)
EN 16476 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 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)
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
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
SIST EN 16476:2014
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:
Avenue Marnix 17,
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
EN 16476:2014 (E) 2 Contents
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
SIST EN 16476:2014
EN 16476:2014 (E) 3 Foreword This document (EN 16476:2014) 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 November 2014 and conflicting national standards shall be withdrawn at the latest by November 2014. 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16476:2014
EN 16476:2014 (E) 4 Introduction This document specifies a method for determining concentration of the six most essential ash forming elements. The number of six was chosen in order to limit the complexity of the test and to be able to determine a decent method precision. The six elements were specified by the vehicle manufacturers. The test provides additional information to the more common ash concentration determination methods which do aim towards filter problems. Metals have more impact on the durability of modern DPF exhaust gas after-treatment systems in diesel vehicles than ash in general. SIST EN 16476:2014
EN 16476:2014 (E) 5 1 Scope 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. Table 1 — Application ranges for ash forming elements Element Range mg/kg Sodium 1,2 to 2,5 Potassium 0,9 to 2,5 Calcium 0,3 to 2,5 Phosphorus 0,9 to 2,5 Copper 0,2 to 2,5 Zinc 0,2 to 2,5 NOTE For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction, 3. WARNING — The use of this European Standard may involve hazardous materials, operations and equipment. This European Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 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 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042) EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171) 3 Principle A weighed amount of diesel fuel sample is diluted with an organic solvent. The solution is then introduced directly into an ICP OES spectrometer. Sodium, potassium, calcium, phosphorous, copper and zinc concentrations are determined by comparison with calibration solutions. An Internal Standard is employed to correct viscosity effects. 4 Reagents If not specified otherwise, only chemicals of a known high degree of purity shall be used. SIST EN 16476:2014
EN 16476:2014 (E) 6 4.1 Kerosene, boiling range between 175 °C and 250 °C, elements free. The solvent shall contain less than 0,1 mg/kg of each of the element under test. NOTE In case of unstable plasma or in case of special laboratory requirements, kerosene can be substituted by other suitable solvents, provided that they are free of analytes. 4.2 Sodium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg sodium. 4.3 Potassium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg potassium. 4.4 Calcium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg calcium. 4.5 Phosphorus Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg phosphorus. 4.6 Copper Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg copper. 4.7 Zinc Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg zinc. 4.8 Sodium, potassium, calcium, phosphorus, copper and zinc intermediate working Standard (50 mg/kg each). Weigh (1,00 g ± 0,01) g of each element Standard solution (4.2), (4.3), (4.4), (4.5), (4.6), (4.7) into a 50 ml bottle (5.2). Add kerosene (4.1) to (20,00 ± 0,20) g. Each mass shall be weighed to the nearest 0,001 g. In the case of using several mono-element Standard solutions, attention-shall be paid to ensure that they are free of other analyte elements. Some commercial element Standard solutions are furnished with higher concentration on the market. Those solutions may be used instead of the required solutions, but in this case an initial mass to mass dilution shall be done according to recommendations given in 7.1. Ready-made commercial multi-element Standard solutions may be used instead of the single element Standard solutions (4.2, 4.3, 4.4, 4.5, 4.6 and 4.7) as the method is designed to avoid interference at the wavelengths specified. 4.9 Internal Standard solution (cobalt, scandium, yttrium), commercially available in oil (analyte free), for example with 1 000 mg/kg per element, available as single element Standard. NOTE The internal Standard solutions are commonly available as single element Standards with various element concentrations. 4.10 Argon, with a mass fraction w (Ar) ≥ 99,996 %. Small amounts of oxygen may be added to the argon gas stream using a metering valve (for example 30 ml/min to
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