Automotive fuels - Determination of manganese and iron content in unleaded petrol - 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 from about 0,5 mg/l to about 7,5 mg/l
and of iron content from about 1,4 mg/l to about 6,0 mg/l in unleaded petrol containing up to 3,7 % (m/m)
oxygen.
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 as MMT and iron as ferrocene are added to petrol to increase anti-knock properties.
NOTE 2 Solutions of MMT in petrol are unstable when exposed to light. Low and erratic results are expected if petrol
samples are exposed to light prior the analysis.
Iron and manganese contents higher than 6,0 mg/l and 7,5 mg/l respectively may be measured after
preliminary dilution of the sample with a suitable solvent. However, the precision has not been established for
such a procedure. Further work regarding automotive ethanol (E85) fuel is on-going in CEN.
NOTE 3 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent the
mass fraction (μ) and the volume fraction (φ) of a material respectively.

Kraftstoffe für Kraftfahrzeuge - Bestimmung des Mangan- und Eisengehaltes in unverbleitem Ottokraftstoff - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES)

Diese Europäische Norm legt ein Verfahren auf Basis der optischen Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES, en: inductively coupled plasma optical emission spectrometry) für die Bestimmung des Mangangehaltes im Bereich von etwa 0,5 mg/l bis etwa 7,5 mg/l und des Eisengehaltes im Bereich von etwa 1,4 mg/l bis etwa 6,0 mg/l in unverbleitem Ottokraftstoff mit einem Sauerstoffgehalt von bis zu 3,7 % (m/m) fest.
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 im Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
ANMERKUNG 1   Mangan als MMT und Eisen als Ferrocen werden dem Ottokraftstoff zur Verbesserung der Antiklopfeigenschaften zugesetzt.
ANMERKUNG 2   MMT-Lösungen in Ottokraftstoff sind unter Lichteinwirkung instabil. Niedrige und irrige Ergebnisse sind zu erwarten, wenn Ottokraftstoff-Proben vor der Analyse dem Licht ausgesetzt werden.
Eisen- und Mangangehalte höher als 6 mg/l bzw. 7,5 mg/l dürfen nach vorhergehender Verdünnung der Probe mit einem zweckmäßigen Lösemittel gemessen werden. Für dieses Verfahren wurde jedoch keine Präzision bestimmt. Weitere Arbeiten bezüglich Ethanol-Kraftstoff (E85) werden derzeit bei CEN durchgeführt.
ANMERKUNG 3   Für die Zwecke dieser Europäischen Norm wird zur Angabe des Massenanteils (µ) einer Substanz der Ausdruck "% (m/m)" und für den Volumenanteil (...) einer Substanz der Ausdruck "% (V/V)" verwendet.

Carburants pour automobiles - Détermination des teneurs en fer et en manganèse dans les essences sans plomb - Méthode spectrométrique optique par plasma à couplage inductif (ICP OES)

La présente Norme européenne spécifie une méthode spectrométrique optique par plasma à couplage inductif (ICP OES) pour la détermination des teneurs en manganèse, de environ 0,5 mg/l à environ 7,5 mg/l, et en fer, de environ 1,4 mg/l à environ 6,0 mg/l dans l’essence sans plomb contenant jusqu’à 3,7 % (m/m) d’oxygène.
AVERTISSEMENT — L'utilisation de la présente Norme peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente Norme 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.
NOTE 1   Le manganèse sous forme de MMT est ajouté à l’essence afin d’en améliorer les propriétés antidétonantes.
NOTE 2   Les solutions de MMT dans l’essence sont instables en cas d’exposition à la lumière. Si les échantillons d’essence sont exposés à la lumière avant l’analyse, les résultats attendus seront trop bas et inconstants.
NOTE 3   Les teneurs en manganèse et en fer supérieures à 7,0 mg/l et 6,0 mg/l, respectivement, peuvent être mesurées après dilution préalable de l’échantillon avec un solvant approprié. Néanmoins la fidélité n’a pas été établie pour cette procédure. Une étude sur les carburants pour automobiles à base d’éthanol (E85) est en cours au CEN.
NOTE 4   Pour les besoins de la présente Norme européenne, les expressions «% (m/m)» et «% (V/V)» représentent respectivement les fractions massiques, µ,  et volumiques, φ, du produit.

Goriva za motorna vozila - Določevanje mangana in železa v neosvinčenem motornem bencinu - Metoda z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP OES)

Ta evropski standard določa metodo na podlagi optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP OES) za določevanje vsebnosti mangana od približno 0,5 mg/l do približno 7,5 mg/l in železa od približno 1,4 mg/l do približno 6,0 mg/l v neosvinčenem motornem bencinu, ki vsebuje do 3,7 % (m/m) kisika.
OPOZORILO – Pri uporabi tega standarda so lahko prisotni nevarni materiali, postopki in oprema. Ta evropski standard ne obravnava vseh varnostnih težav, ki se nanašajo na njegovo uporabo. Za vzpostavitev ustreznih varnostnih in zdravstvenih praks ter za določitev uporabnosti regulativnih omejitev pred uporabo je odgovoren uporabnik tega evropskega standarda.
OPOMBA 1: Mangan kot MMT in železo kot ferocen se dodajata bencinu za izboljšanje lastnosti preprečevanja pojavov klenkanja.
OPOMBA 2: Raztopine z MMT v bencinu so nestabilne, če so izpostavljene svetlobi. Nizki in neredni rezultati se pričakujejo, če so vzorci bencina pred analizo izpostavljeni svetlobi.
Vsebnost železa, večja od 6,0 mg/l, in vsebnost mangana, večja od 7,5 mg/l, se lahko izmerita, če je vzorec predhodno razredčen z ustreznim topilom. Vendar natančnost takega postopka ni določena. Odbor CEN izvaja nadaljnje delo v zvezi z etanolom (E85), ki se uporablja kot motorno gorivo.
OPOMBA 3: V tem evropskem standardu sta uporabljeni oznaki % (m/m) in % (V/V), ki predstavljata masni delež (µ) oziroma prostornino (φ) materiala.

General Information

Status
Published
Public Enquiry End Date
01-Dec-2013
Publication Date
04-Mar-2015
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
18-Feb-2015
Due Date
25-Apr-2015
Completion Date
05-Mar-2015

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.QþHQHPGXNWLYQRKraftstoffe für Kraftfahrzeuge - Bestimmung des Mangan- und Eisengehaltes in unverbleitem Ottokraftstoff - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES)Carburants pour automobiles - Détermination des teneurs en fer et en manganèse dans les essences sans plomb - Méthode spectrométrique optique par plasma à couplage inductif (ICP OES)Automotive fuels - Determination of manganese and iron content in unleaded petrol - Inductively coupled plasma optical emission spectrometry (ICP OES) method75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 16136:2015SIST EN 16136:2015en,fr,de01-april-2015SIST EN 16136:2015SLOVENSKI

STANDARDSIST EN 16136:20121DGRPHãþD
SIST EN 16136:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16136
February 2015 ICS 71.080.60; 75.160.20 Supersedes EN 16136:2011English Version

Automotive fuels - Determination of manganese and iron content in unleaded petrol - Inductively coupled plasma optical emission spectrometry (ICP OES) method

Carburants pour automobiles - Détermination des teneurs en fer et en manganèse dans les essences sans plomb - Méthode spectrométrique optique par plasma à couplage inductif (ICP OES)

Kraftstoffe für Kraftfahrzeuge - Bestimmung des Gehaltes an Mangan und Eisen in unverbleitem Ottokraftstoff - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) This European Standard was approved by CEN on 12 December 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 © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16136:2015 ESIST EN 16136:2015

EN 16136:2015 (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 .....................................................................................7 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 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 ............................................................................................................................................9 8.5 Check of calibration ..............................................................................................................................9 9 Sample analysis .................................................................................................................................. 10 9.1 Sample solution preparation ............................................................................................................. 10 9.2 Sample solution measurement .......................................................................................................... 10 10 Calculation ........................................................................................................................................... 10 11 Expression of results ......................................................................................................................... 11 12 Precision .............................................................................................................................................. 11 12.1 General ................................................................................................................................................. 11 12.2 Repeatability, r .................................................................................................................................... 11 12.3 Reproducibility, R ............................................................................................................................... 11 13 Test report ........................................................................................................................................... 11 Bibliography ..................................................................................................................................................... 13

SIST EN 16136:2015

EN 16136:2015 (E) 3 Foreword This document (EN 16136:2015) 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 August 2015, and conflicting national standards shall be withdrawn at the latest by August 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 supersedes EN 16136:2011. The major updates are the lowering of the manganese content to allow a specification setting of 2 mg/l of manganese in line with the FQD requirement per 2014-01-01, and the introduction in the scope of determination of iron content, which can be added into petrol as ferrocene. This document answers requirements originating from the amended Fuels Quality Directive (FQD, [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 16136:2015

EN 16136:2015 (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 from about 0,5 mg/l to about 7,5 mg/l and of iron content from about 1,4 mg/l to about 6,0 mg/l in unleaded petrol containing up to 3,7 % (m/m) oxygen. 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 as MMT and iron as ferrocene are added to petrol to increase anti-knock properties. NOTE 2 Solutions of MMT in petrol are unstable when exposed to light. Low and erratic results are expected if petrol samples are exposed to light prior the analysis. Iron and manganese contents higher than 6,0 mg/l and 7,5 mg/l respectively may be measured after preliminary dilution of the sample with a suitable solvent. However, the precision has not been established for such a procedure. Further work regarding automotive ethanol (E85) fuel is on-going in CEN. NOTE 3 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent the mass fraction (µ) and the volume fraction (3) of a material respectively. 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) EN ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density — Hydrometer method (ISO 3675) EN ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube method (ISO 12185) 3 Principle A petrol 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 and vapour pressure effects. 4 Reagents Unless specified otherwise, only chemicals which are known to have a high degree of purity shall be used. Some ready-made commercial multi-element Standard solutions may be used instead of the single element Standard solution (4.4 and 4.5). SIST EN 16136:2015

EN 16136:2015 (E) 5 IMPORTANT — In the case of using several mono-element Standard solutions, attention shall be paid to ensure that they are free of other analyte elements. 4.1 Kerosene, boiling range between 150 °C and 250 °C, analytical reagent grade. Other grades of kerosene with analyte concentrations below the detection limit of the instrument for the elements under investigation may be used. In this case, perform a wavelength scan for analyte elements to check spectral interferences. 4.2 Heptane, analytical reagent grade. 4.3 Solvent, add 25 ml heptane (4.2) to a 500 ml HDPE bottle (5.1.2) and fill to 500 ml with kerosene (4.1). 4.4 Manganese Standard solution, commercially available in oil, c(Mn) = 100 mg/kg. 4.5 Iron Standard solution, commercially available in oil, c(Fe) = 100 mg/kg. Some commercial element Standard solutions are furnished with higher content on the market. Those solutions may be used instead of the required solutions, but an initial mass to mass dilution has to be done according to recommendations given in 7.4. 4.6 Element Standard solution, of one of the elements cobalt, scandium, yttrium, etc. commercially available in oil (analyte free), for example with 1 000 mg/kg per element, available as single element standards. NOTE The internal Standard solutions are commonly available as single element standards with various element contents. 4.7 Argon, with a purity of ≥ 99,995 % (V/V). Small amounts of oxygen (purity ≥ 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: All glassware shall be cleaned carefully before use. 5.1.1 Glassware, usual laboratory glassware, together with the following: 5.1.1.1 Beakers, 50 ml. 5.1.1.2 Volumetric flasks, 20 ml, 50 ml and 500 ml according to EN ISO 1042, with taper sleeve and plug. 5.1.2 Bottles, 50 ml and 500

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