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psbkphpq^ka^oa ppjbkfplnqrvswommt Fastställd/Approved: 2007-09-27 Publicerad/Published: 2007-10-18 Utgåva/Edition: 2 Språk/Language: engelska/english ICS: 75.080; 75.160.

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3 Europastandarden SS-EN ISO 14596:2007 gäller som svensk standard. Detta dokument innehåller den officiella engelska versionen av SS-EN ISO 14596:2007. Denna standard ersätter SS-EN ISO 14596, utgåva 1. The European Standard SS-EN ISO 14596:2007 has the status of a Swedish Standard. This document contains the official English version of SS-EN ISO 14596:2007. This standard supersedes the Swedish Standard SS-EN ISO 14596, edition 1. >«`çéóêáöüílrééüçîëê ííéåíáääçéåå~éêççìâííáääü êpfpipïéçáëüpí~åç~êçëfåëíáíìíéipíçåâüçäãipîéêáöék^åî åçåáåöéå ~îçéåå~éêççìâíêéöäéê~ë~îëäìí~åî åç~êäáåéåëéåëçã íéêñáååëáçéåå~éêççìâíiëéëí~åç~êçéåëëáëí~ëáççêk «`çéóêáöüípfpipïéçáëüpí~åç~êçëfåëíáíìíéipíçåâüçäãipïéçéåk^ääêáöüíëêéëéêîéçkqüéìëéçñíüáëéêççìåíáëöçîéêåéç ÄóíÜÉÉåÇJìëÉêäáÅÉåÅÉÑçêíÜáëéêçÇìÅíKvçìïáääÑáåÇíÜÉäáÅÉåÅÉáåíÜÉÉåÇçÑíÜáëÇçÅìãÉåíK rééäóëåáåö~êçãë~âáååéü ääéíáëí~åç~êçéåä ãå~ë~îpfpipïéçáëüpí~åç~êçëfåëíáíìíéiíéäéñçåmujrrrrommmk pí~åç~êçéêâ~åäéëí ää~ëüçëpfpc êä~ö^_ëçã îéåä ãå~ê~ääã åå~ìééäóëåáåö~êçãëîéåëâçåüìíä åçëâëí~åç~êçk fåñçêã~íáçå~äçìííüéåçåíéåíçñíüéëí~åç~êçáë~î~áä~ääéñêçãíüépïéçáëüpí~åç~êçëfåëíáíìíéepfpfiíéähqsurrrrommmk pí~åç~êçëã~óäéçêçéêéçñêçãpfpc êä~ö^_iïüçå~å~äëçéêçîáçéöéåéê~äáåñçêã~íáçå~äçìípïéçáëü~åçñçêéáöåëí~åç~êçëk pfpc êä~ö^_ipbnnuumpíçåâüçäãipïéçéåkqéäwhqsurrrropnmkc~ñwhqsurrrropnnk bjã~áäwëáëkë~äéë]ëáëkëéfåíéêåéíwïïïkëáëkëé

4 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO September 2007 ICS Supersedes EN ISO 14596:1998 English Version Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:2007) Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de fluorescence X dispersive en longueur d'onde (ISO 14596:2007) Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Wellenlängendispersive Röntgenfluoreszenz-Analyse (ISO 14596:2007) This European Standard was approved by CEN on 8 September 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 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14596:2007: E

5 EN ISO 14596:2007 (E) Contents Page Foreword... vi 1 Scope Normative references Principle Reagents and materials Apparatus Samples and sampling Calibration solutions Calibration Procedure Calculation Expression of results Precision Test report...8 v

6 EN ISO 14596:2007 (E) Foreword This document (EN ISO 14596:2007) has been prepared by Technical Committee ISO/TC 28 "Petroleum products and lubricants" in collaboration with 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 March 2008, and conflicting national standards shall be withdrawn at the latest by March This document supersedes EN ISO 14596:1998. 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, 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.. Endorsement notice The text of ISO 14596:2007 has been approved by CEN as a EN ISO 14596:2007 without any modification. vi

7 EN ISO 14596:2007 (E) Petroleum products Determination of sulfur content Wavelength-dispersive X-ray fluorescence spectrometry WARNING The use of this International Standard may involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifies a method for the determination of the sulfur content of liquid petroleum products, additives for petroleum products, and semi-solid and solid petroleum products that are either liquefied by moderate heating or soluble in organic solvents (see 4.1) of negligible or accurately known sulfur content. The method is applicable to products or additives having sulfur contents in the range 0,001 % (m/m) to 2,50 % (m/m); higher contents can be determined by appropriate dilution. Other elements do not interfere at concentrations anticipated in the materials subject to this analysis. NOTE material. For the purposes of this International Standard, the term % (m/m) is used to represent the mass fraction of a High concentrations of phosphorus or chlorine [typically above 3 % (m/m)] can cause bias in the sulfur result by absorbing Zr-L and S-K to different extents. It is necessary in these cases to carry out studies to determine whether this potential interference is significant. When larger amounts of molybdenum are present (typically above 50 mg/kg to 100 mg/kg), increased background radiation and spectral overlap with the sulfur signal can occur. It is necessary in these cases to inspect the relevant spectral regions, for example, to investigate the significance of this potential source of bias. 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. ISO 3170:2004, Petroleum liquids Manual sampling ISO 3171:1988, Petroleum liquids Automatic pipeline sampling 1

8 EN ISO 14596:2007 (E) 3 Principle The test portion and a zirconium solution as internal standard are mixed in a given mass ratio and exposed, in a sample cell, to the primary radiation of an X-ray tube. The count rates of the S-K at 0,537 3 nm and Zr-L 1 at 0,607 0 nm fluorescence thus excited and the count rate of the background radiation at 0,545 nm are measured and the ratio of these net count rates calculated. The sulfur content of the sample is determined from a calibration curve prepared on the basis of sulfur calibration standards. NOTE The Siegbahn X-ray line notation (S-K ) is used in this International Standard; the corresponding IUPAC X-ray line notation is S K-L 2,3. 4 Reagents and materials 4.1 White oil (light paraffin oil, paraffinum perliquidum), high-purity grade, sulfur content 1 mg/kg maximum. 4.2 Sulfur compounds, of sulfur content accurately known to the nearest 0,01 % (m/m), used for the preparation of the primary standards. The compounds given in to are suitable, and their nominal sulfur contents are given. Where the purity of these compounds is less than 99 %, certified materials are required, or the nature of all impurities and their contents should be accurately known to the nearest 0,01 % (m/m) Dibenzothiophene (DBT), with a nominal sulfur content of 17,399 % (m/m) Dibutyl sulfide (DBS), with a nominal sulfur content of 21,915 % (m/m) Thionaphthene (benzothiophene) (TNA), with a nominal sulfur content of 23,890 % (m/m). 4.3 Certified sulfur reference materials. Use materials from a national standards body or accredited suppliers, if available. 4.4 Zirconium solution A. Zirconium octoate solution with a zirconium content in the range of 12 % (m/m) to 18 % (m/m) or another oilsoluble, sulfur-free zirconium compound dissolved in white oil (4.1) to provide a zirconium mass fraction in the range of 12 % (m/m) to 18 % (m/m). 4.5 Zirconium solution B. Dissolve the zirconium solution A (4.4) with white oil (4.1) to provide a zirconium mass fraction of approximately 1 % (m/m). 5 Apparatus 5.1 Wavelength-dispersive X-ray fluorescence (WDXRF) spectrometer, consisting of any suitable spectrometer that incorporates the design features listed in Table 1. It shall be set up according to the manufacturer's instructions. 2

Petroleumprodukter Bestämning av låga blyhalter i bensin Våglängdsdispersiv röntgenfluorescensspektrofotometri (XRF)

SVENSK STANDARD SS-EN 13723 Fastställd 2002-08-09 Utgåva 1 Petroleumprodukter Bestämning av låga blyhalter i bensin Våglängdsdispersiv röntgenfluorescensspektrofotometri (XRF) Petroleum products Determination