SIST EN 16576:2015
(Main)Automotive fuels - Determination of manganese and iron content in middle distillate fuels - Inductively coupled plasma optical emission spectrometry (ICP OES) method
Automotive fuels - Determination of manganese and iron content in middle distillate fuels - Inductively coupled plasma optical emission spectrometry (ICP OES) method
This European Standard specifies a method based on inductively coupled plasma optical emission spectrometry (ICP OES) for the determination of manganese content present as methylcyclopentadienyl manganese tricarbonyl (MMT) and iron content in distillate fuel from about 0,5 mg/l to about 8 mg/l. This test method is applicable to diesel fuel containing up to 30 % (V/V) of fatty acid methyl ester (FAME)
Kraftstoffe für Kraftfahrzeuge - Bestimmung des Gehaltes an Mangan und Eisen in Kraftstoffen aus Mitteldestillaten - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES)
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Mangan- und Eisengehalten mit Hilfe der optischen Emissionsspektroskopie mit induziert gekoppeltem Plasma (ICP OES) fest. Das Verfahren ist anwendbar auf Dieselkraftstoffe mit Gehalten an Fettsäuremethylester (FAME) von bis zu 10 % (V/V) für Mangan- bzw. Eisengehalte von jeweils 0,5 mg/l bis 7,0 mg/l.
WARNUNG — Die Anwendung dieses Dokuments kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle mit der Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieses Dokuments ist dafür verantwortlich, angemessene Maßnahmen in Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
ANMERKUNG 1 Mangan- und Eisengehalte über 7,0 mg/l können nach vorheriger Verdünnung der Probe mittels eines Lösungsmittels gemessen werden. Für dieses Verfahren wurde jedoch noch keine Präzision ermittelt.
ANMERKUNG 2 Für die Zwecke dieser Europäischen Norm wird zur Angabe des Volumenanteils () einer Substanz der Ausdruck „% (V/V)“ verwendet.
Carburants pour automobiles - Détermination de la teneur en manganèse et fer dans des distillatsmoyens - Méthode d'émission atomique à couplage inductif par plasma (ICP OES)
Goriva za motorna vozila - Določevanje mangana in železa v srednjih destilatih - Metoda z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP OES)
Ta evropski standard določa metodo na osnovi optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP OES) za določevanje vsebnosti mangana v obliki metilciklopentadienil manganovega trikarbonila (MMT) in železa v destilatnih gorivih od 0,5 mg/l do 8 mg/l. Ta preskusna metoda se uporablja za dizelska goriva z vsebnostjo metilnih estrov maščobnih kislin (FAME) do 30 % (V/V).
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.2(6Kraftstoffe für Kraftfahrzeuge - Bestimmung des Gehaltes an Mangan und Eisen in Kraftstoffen aus Mitteldestillaten - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES)Carburants pour automobiles - Détermination de la teneur en manganèse et fer dans des distillatsmoyens - Méthode d'émission atomique à couplage inductif par plasma (ICP OES)Automotive fuels - Determination of manganese and iron content in middle distillate fuels - Inductively coupled plasma optical emission spectrometry (ICP OES) method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 16576:2014SIST EN 16576:2015en,de01-januar-2015SIST EN 16576:2015SLOVENSKI
STANDARD
SIST EN 16576:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16576
November 2014 ICS 75.160.20 English Version
Automotive fuels - Determination of manganese and iron content in diesel - Inductively coupled plasma optical emission spectrometry (ICP OES) method
Carburants pour automobiles - Détermination des teneurs en manganèse et en fer dans carburants diesel - Méthode spectrométrique optique par plasma à couplage inductif
(ICP OES)
Kraftstoffe für Kraftfahrzeuge - Bestimmung des Gehaltes an Mangan und Eisen in Dieselkraftstoff - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) This European Standard was approved by CEN on 20 September 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 16576:2014 ESIST EN 16576:2015
EN 16576:2014 (E) 2 Contents
Page Foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 4 5 Apparatus . 5 6 Sampling . 6 7 Preparation of solutions . 6 7.1 General . 6 7.2 Preparation of the Internal standard solution for dilution . 6 7.3 Preparation of the manganese intermediate solution. 7 7.4 Preparation of the iron intermediate solution . 7 7.5 Preparation of the calibration solutions . 7 7.6 Preparation of manganese and iron quality control solution . 7 8 Calibration . 8 8.1 General . 8 8.2 Calibration of the ICP OES spectrometer . 8 8.3 Procedure A . 8 8.4 Procedure B . 8 8.5 Check of the calibration . 9 9 Sample analysis . 9 9.1 Sample solution preparation . 9 9.2 Sample solution measurement . 9 10 Calculation . 10 11 Expression of results . 10 12 Precision . 10 12.1 General . 10 12.2 Repeatability, r . 11 12.3 Reproducibility, R . 11 13 Test report . 11 Bibliography . 12
SIST EN 16576:2015
EN 16576:2014 (E) 3 Foreword This document (EN 16576:2014) 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 May 2015 and conflicting national standards shall be withdrawn at the latest by May 2015. 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. This document answers requirements originating from the amended Fuels Quality Directive (FQD, [1]). A similar technique for unleaded petrol is described in EN 16136 [2]. 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 16576:2015
EN 16576:2014 (E) 4 1 Scope This European Standard specifies a method based on inductively coupled plasma optical emission spectrometry (ICP OES) for the determination of manganese content and of iron content, each from about 0,5 mg/l to about 7,0 mg/l in diesel fuels including those containing up to about 10 % (V/V) fatty acid methylester (FAME). 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 to determine the applicability of regulatory limitations prior to use. NOTE 1 Manganese and iron contents higher than 7,0 mg/l can be measured after preliminary dilution of the sample with a suitable solvent. However, the precision has not been established for such a procedure. NOTE 2 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction (m) of a material. 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, -mark volumetric flasks bfpl 1M4l) EN ISO 3170,
EN ISO 3171, eline sampling bfpl m171) EN ISO 3675, eydrometer method bfpl mp7o) EN ISO 12185, -tube method bfpl 1l1ro) 3 Principle A diesel fuel sample is diluted with a hydrocarbon solvent. The solution is introduced directly into the plasma of an ICP OES spectrometer. Iron and manganese contents are calculated by comparison with calibration solutions prepared from suitable iron and manganese compounds. An internal standard is employed to correct viscosity effects. 4 Reagents Unless specified otherwise, only chemicals which are known to have a high degree of purity shall be used. 4.1 Kerosene, boiling range between 150 °C and 250 °C, analytical reagent grade. Other grades of kerosene with analyte concentrations below the detection limits for the two elements under investigation may be used. In this case, perform a wavelength check for absence of signals from the corresponding elements as well as for absence of spectral interference. 4.2 Manganese standard solution, dissolved in oil, µ(Mn) = 100 mg/kg. SIST EN 16576:2015
EN 16576:2014 (E) 5 A multi-element standard solution may also be used instead of the single element standard solution. Some element standard solutions are supplied with different element content on the market. These solutions may be used instead of the required solutions, but an initial mass to mass dilution has to be done. 4.3 Iron standard solution, dissolved in oil, µ(Fe) = 100 mg/kg. A multi-element standard solution may also be used instead of the single element standard solution. Some element standard solutions are supplied with different element content on the market. These solutions may be used instead of the required solutions, but an initial mass to mass dilution has to be done. 4.4 Internal standard solutions (cobalt, scandium, yttrium), dissolved in oil, for example with 1 000 mg/kg per element, available as single element standards. NOTE The element standard solutions are commonly available as single element standards with various element content. 4.5 Argon, with a purity of ≥ 99,995 % (V/V). Small amounts of oxygen (purity O2 ≥ 99,995 % (V/V)) may be added, for instance in accordance with the operating instructions of the equipment manufacturer, to the argon gas stream using a metering valve (30 ml/min to 100 ml/min) to prevent carbon deposits in the area of the plasma torch. 5 Apparatus 5.1 Laboratory equipment 5.1.1 General All glassware shall be cleaned carefully before use. 5.1.2 Glassware, usual laboratory glassware, together with the following: 5.1.2.1 Beakers, 50 ml. 5.1.2.2 Volumetric flasks, 20 ml, 50 ml and 500 ml, according to EN ISO 1042, with taper sleeve and plug. 5.1.3 Bottles, 50 ml and 500 ml,
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