SIST EN 15944:2011
(Main)Liquid petroleum products - Determination of nickel and vanadium content - Inductively coupled plasma optical emission spectrometry (ICP OES)
Liquid petroleum products - Determination of nickel and vanadium content - 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 nickel content in the range 4 mg/kg to 55 mg/kg and of vanadium content in the range 4 mg/kg to 150 mg/kg in fuel oils and residual fuel oils.
Flüssige Mineralölerzeugnisse - Bestimmung des Gehaltes an Nickel und Vanadium - Induktiv gekoppeltes Plasma Optisch-Emissionspektrometrisches direktes Prüfverfahren (IGP-OES)
Diese Europäische Norm legt ein emissionsspektrometrisches Verfahren mit induktiv gekoppeltem Plasma (ICP OES) zur Bestimmung des Gehaltes an Nickel (Ni) im Bereich von etwa 4 mg/kg bis 55 mg/kg und des Gehaltes an Vanadium (V) im Bereich von etwa 4 mg/kg bis 150 mg/kg in Heizölen und Rückstandsölen fest.
ANMERKUNG 1 Der Gehalt an Nickel kann auch im Bereich von 2 mg/kg bis 4 mg/kg und der Gehalt an Vanadium auch im Bereich von 1 mg/kg bis 4 mg/kg bestimmt werden. Da jedoch keine Nickel und Vanadiumproben aus diesen Bereichen in den Ringversuch einbezogen waren, konnte noch keine Präzision ermittelt werden. Proben mit höheren Nickel und Vanadiumgehalten als den zuvor angegebenen können nach Verdünnung bestimmt werden, jedoch wurde für verdünnte Proben keine Präzision ermittelt.
ANMERKUNG 2 Für den Zweck dieser Europäischen Norm darf das Symbol % (V/V) verwendet werden, um Volumen¬anteile in % (φ) auszudrücken.
WARNUNG - Die Anwendung dieser Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieser Norm ist dafür verantwortlich, vorher angemessene Maßnahmen in Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
Produits pétroliers liquides - Détermination de la teneur en nickel et vanadium - Méthode spectrométrique optique directe par plasma à couplage inductif (SOD-PCI)
La présente Norme européenne spécifie une méthode par spectrométrie d’émission atomique par plasma à couplage inductif (ICP OES) permettant de déterminer la teneur en nickel dans la plage comprise entre 4 mg/kg et 55 mg/kg et la teneur en vanadium dans la plage comprise entre 4 mg/kg et 150 mg/kg dans les fiouls et les fiouls résiduels.
NOTE 1 La teneur en nickel peut être déterminée de 2 mg/kg à 4 mg/kg et la teneur en vanadium peut être déterminée de 1 mg/kg à 4 mg/kg. La fidélité n’a cependant pas été établie car aucun échantillon ayant des teneurs en nickel et en vanadium comprises dans ces plages n’a été inclus dans l’essai interlaboratoires. Des teneurs en nickel et en vanadium supérieures à celles indiquées peuvent être déterminées après dilution de l’échantillon. La fidélité n’a cependant pas été établie pour les échantillons dilués.
NOTE 2 Pour les besoins du présent document, le terme "% (V/V)" représente la fraction volumique (ϕ).
AVERTISSEMENT - L'utilisation de la présente Norme européenne peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente norme européenne n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de consulter et d'établir des règles de sécurité et d'hygiène appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.
Tekoči naftni proizvodi - Določevanje niklja in vanadija - Optična emisijska spektrometrija z induktivno sklopljeno plazmo (ICP OES)
Ta evropski standard določa metodo optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP OES) za določevanje niklja v razponu od 4 mg/kg do 55mg/kg in vanadija v razponu 4 mg/kg do 150mg/kg v kurilnih oljih in mazutih.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Flüssige Mineralölerzeugnisse - Bestimmung des Gehaltes an Nickel und Vanadium - Induktiv gekoppeltes Plasma Optisch-Emissionspektrometrisches direktes Prüfverfahren (IGP-OES)Produits pétroliers liquides - Détermination de la teneur en nickel et vanadium - Méthode spectrométrique optique directe par plasma à couplage inductif (SOD-PCI)Liquid petroleum products - Determination of nickel and vanadium content - Inductively coupled plasma optical emission spectrometry (ICP OES)75.080Naftni proizvodi na splošnoPetroleum products in generalICS:Ta slovenski standard je istoveten z:EN 15944:2010SIST EN 15944:2011en,fr,de01-januar-2011SIST EN 15944:2011SLOVENSKI
STANDARD
SIST EN 15944:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15944
November 2010 ICS 75.100 English Version
Liquid petroleum products - Determination of nickel and vanadium content - Inductively coupled plasma optical emission spectrometry method (ICP OES)
Produits pétroliers liquides - Détermination de la teneur en nickel et vanadium - Méthode directement par spectrométrie d'émission atomique à couplage inductif par plasma (SOD-PCI)
Flüssige Mineralölerzeugnisse - Bestimmung des Gehaltes an Nickel und Vanadium - Optische Emissionsspektralanalyse mit induktiv gekopppeltem Plasma (ICP OES) This European Standard was approved by CEN on 9 October 2010.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15944:2010: ESIST EN 15944:2011
EN 15944:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Reagents .45Apparatus .56Sampling .67Preparation of calibration solutions .67.1General .67.2Calibration solutions .67.3Internal standard solution .77.4Working solutions.78Calibration .78.1General .78.2Calibration of the ICP OES spectrometer .78.3Procedure A .78.4Procedure B .88.5Check of calibration .89Sample analysis .89.1Sample preparation .89.2Sample measurement .910Calculation .910.1Procedure A .910.2Procedure B .911Expression of results . 1012Precision . 1012.1General . 1012.2Repeatability, r . 1012.3Reproducibility, R . 1013Test report . 10Bibliography . 11 SIST EN 15944:2011
EN 15944:2010 (E) 3 Foreword This document (EN 15944:2010) 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 2011, and conflicting national standards shall be withdrawn at the latest by May 2011. 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. The method described in this document is based on DIN 51790-6 [1]. It has been developed originally as an alternative to (second part of) EN 13131 [2], but as the method enables the use of an instrumental technique more and more employed in analytical laboratories, it was decided to have it as a stand-alone method. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15944:2011
EN 15944:2010 (E) 4 1 Scope This European Standard specifies an inductively coupled plasma optical emission spectrometry (ICP OES) method for the determination of nickel content in the range 4 mg/kg to 55 mg/kg and of vanadium content in the range 4 mg/kg to 150 mg/kg in fuel oils and residual fuel oils. NOTE 1 Nickel content can be determined from 2 mg/kg to 4 mg/kg and vanadium content can be determined from 1 mg/kg to 4 mg/kg. However, the precision was not established as no samples with nickel and vanadium contents in these ranges were included in the interlaboratory test. Nickel and vanadium contents higher than those reported can be determined after sample dilution. However, the precision was not established for diluted samples. NOTE 2 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction (3). WARNING — The use of this standard may 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 establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application 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 1042, Laboratory glassware
One-mark volumetric flasks (ISO 1042:1998) EN ISO 3170, Petroleum liquids
Manual sampling (ISO 3170:2004) EN ISO 3171, Petroleum liquids
Automatic pipeline sampling (ISO 3171:1988) 3 Principle The sample is diluted with an organic solvent. The solution is then introduced directly into the ICP OES spectrometer. Vanadium and nickel contents are determined by comparison with calibration solutions. An internal standard is employed to correct viscosity effects. 4 Reagents
4.1 Paraffin oil, with viscosity between 1,5 mm2/s and 6,0 mm2/s, Pharmacopeia (EUPHARM EP5), e.g. Merck 107174 1). 4.2 Kerosene, boiling range included between 150 °C and 325 °C, e.g. Aldrich 32.946-0 1).
4.3 Xylene, analytical reagent grade. 4.4 2-Ethyl hexanoic acid, analytical reagent grade or other suitable stabilizer for element standard solution.
1) This information is given for the convenience of the users of this European Standard and does not constitute an endorsement by CEN of these products. Equivalent products may be used if they can be shown to lead to the same results. SIST EN 15944:2011
EN 15944:2010 (E) 5 4.5 Element standard solutions, dissolved in oil, for example with 500 mg/kg per element, available as single element standards, or at least partially as multi-element standards. NOTE Some commercial element standard solutions on the market are furnished with higher content. Those solutions may be used instead of the required solutions, but an initial mass to mass dilution should be done according to recommendations given in 7.1.
4.6 Argon, with minimum purity 3(Ar) = 99,996 % (V/V). NOTE Small amounts of oxygen (minimum purity 3(O2) ≥ 99,995 % (V/V)) may be added 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 All glassware shall be cleaned carefully before use to remove soluble constituents. Fill new glass vessels with xylene (4.3) and allow to stand for at least two days. 5.1.1 Glassware 5.1.1.1 Beakers, tall type, 150 ml. 5.1.1.2 Erlenmeyer flasks with wide neck and plug, 50 ml. 5.1.1.3 Volumet
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