BS-EN-ISO-8754-2003 BS-2000-336-2003.pdf

BRITISH STANDARD BS 2000-336:2003 BS EN ISO 8754:2003 Incorporating Corrigendum No. 1 Methods of test for petroleum and its products BS 2000-336: Petroleum products Determination of sulfur content Energy-dispersive X-ray fluorescence spectrometry (Identical with IP 336-2004) The European Standard EN ISO 8754:2003:2003 has the status of a British Standard ICS 75.080 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 2000-336:2003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 14 August 2003 © Institute of Petroleum and BSI 27 October 2003 ISBN 0 580 42400 6 National foreword This British Standard is the official English language version of EN ISO 8754:2003. It is identical with ISO 8754:2003. It supersedes BS 2000-336/BS EN ISO 8754:1995 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. The Institute of Petroleum publishes and sells all parts of BS 2000, and all BS EN petroleum test methods that would be part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 parts” and individually. Further information is available from: The Institute of Petroleum, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467 7100. Fax: 020 7255 1472. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 7, the Annex ZA page and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments 14812 Corrigendum No. 1 27 October 2003Correction to EN ISO foreword page, and incorporating the Annex ZA page Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 8754 July 2003 ICS 75.080Supersedes EN ISO 8754:1995 English version Petroleum products - Determination of sulfur content - Energy- dispersive X-ray fluorescence spectrometry (ISO 8754:2003) Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de fluorescence X dispersive en énergie (ISO 8754:2003) Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Energiedispersives Röntgenfluoreszenz-Verfahren (ISO/FDIS 8754:2003) This European Standard was approved by CEN on 10 July 2003. 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 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, 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 © 2003 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 8754:2003 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I NESO 78:4502( 30E) 2 CORRECTED 2003-10-01 Foreword This document (EN ISO 8754:2003) has been prepared by Technical Committee ISO/TC 28 “Petroleum products and lubricants“ in collaboration with Technical Committee CEN/TC 19 “Petroleum products, lubricants and related products“, 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 January 2004, and conflicting national standards shall be withdrawn at the latest by January 2004. This document supersedes EN ISO 8754:1995. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 8754:2003 has been approved by CEN as EN ISO 8754:2003 without any modifications. NOTE Normative references to International Standards are listed in Annex ZA (normative). EN ISO 8754:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 8754:2003(E) © OSI 3002 INTERNATIONAL STANDARD ISO 8754 Second edition 2003-07-15 Petroleum products Determination of sulfur content Energy-dispersive X-ray fluorescence spectrometry Produits pétroliers Détermination de la teneur en soufre Spectrométrie de fluorescence de rayons X dispersive en énergie EN ISO 8754:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:4578 O3002(E) I ©SO 3002 All irhgts seredevr iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 8754 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants. This second edition cancels and replaces the first edition (ISO 8754:1992), which has been technically revised. EN ISO 8754:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:4578 O3002(E) iv I ©SO 3002 All irhgts seredevr Introduction Specialized procedures, using the analytical technique described in this International Standard, for automotive fuels with sulfur contents below 0,20 % (m/m), are under development. EN ISO 8754:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADR IS:4578 O3002(E) I ©SO 3002 All irhgts seredevr 1 Petroleum products Determination of sulfur content Energy-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 petroleum products, such as naphthas, unleaded motor gasolines, middle distillates, residual fuel oils, base lubricating oils and components. The method is applicable to products having sulfur contents in the range 0,03 % (m/m) to 5,00 % (m/m). NOTE For the purposes of this International Standard, the term “% (m/m)“ is used to represent the mass fraction of a material. Heavy metal additives, such as lead alkyls, may interfere with the determination. Elements such as silicon, phosphorus, calcium, oxygen, potassium, zinc, molybdenum, barium and halogens interfere, if present in concentrations of more than a few hundred milligrams per kilogram. Some modern instruments allow the analyst to compensate for matrix and spectral interferences by spectra deconvolution and inter-element correction by multiple regression. For samples varying in composition of aromatic hydrocarbons and paraffinic hydrocarbons, the ratio of carbon to hydrocarbon in a sample (C/H ratio) may also interfere with the determination, when the ratio of the sample differs by one or more from that of the reference materials from which the calibration is obtained. 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 3170:1), Petroleum liquids Manual sampling ISO 3171:1988, Petroleum liquids Automatic pipeline sampling 3 Principle The test portion is placed in the beam emitted from an X-ray source. The excitation energy may be derived from a radioactive source, such as 55Fe, or from an X-ray tube. The resultant excited characteristic X radiation is measured, and the accumulated count is compared with a calibration graph plotting counts against sulfur content as percentage by mass % (m/m), on a series of calibration samples covering the range of sulfur contents under examination. 1) To be published. (Revision of ISO 3170:1988) EN ISO 8754:2003 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:48:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS:4578 O3002(E) 2 I ©SO 3002 All irhgts seredevr 4 Reagents and materials 4.1 White oil (light paraffin oil), of high purity grade, with a maximum sulfur content of 20 mg/kg. For measurements at very low levels of sulfur content below approximately 0,1 % (m/m), matrix effects are minimized if a diluent of a type similar to the product being analysed is used for the production of the calibration standards described in Clause 8. Such a diluent should be of very low sulfur content, preferably below 2 mg/kg. 4.2 Sulfur compounds, of known sulfur content, used for the preparation of the primary standards. NOTE The compounds given in 4.2.1 to 4.2.3 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 concentrations and nature of all impurities are to be known. 4.2.1 Dibenzothiophene (DBT), with a nominal sulfur content of 17,399 % (m/m). 4.2.2 Dibutylsulfide (DBS), with a nominal sulfur content of 21,915 % (m/m). 4.2.3 Thionaphthene (benzothiophene) (TNA), with a nominal sulfur content of 23,89 % (m/m). 4.3 Certified reference materials: use materials from a national standards body or accredited supplier, with a range of certified sulfur contents for the production of calibration curves for routine analysis. However, particularly for some heavier materials, the excitation is slightly affected by the background matrix. Therefore, in cases of dispute, the parties shall agree on a common range of certified standards, or shall both prepare standards from the materials described in 4.1 and 4.2. 5 Apparatus 5.1 Energy-dispersive X-ray fluorescence analyser: use any suitable model, provided that the design incorporates the features given in 5.1.1 to 5.1.6. It shall be set up according to the manufacturers instructions. 5.1.1 Source of X-ray excitation, with significant X-ray flux at energies above 2,5 keV. 5.1.2 Removable sample cup, providing a sample depth of at least 3 mm, and equipped with replaceable X-ray transparent film. NOTE Window material is normally 6 µm polyester, polypropylene or polycarbonate film. Commercial polyester film may contain small but variable amounts of calcium, which may interfere. Samples of very high aromatic content may dissolve polycarbonate film. 5.1.3 X-ray detector, with high sensitivity at 2,3 keV. 5.1.4 Filters, or other means of discriminating between sulfur K radiation and other X-rays. 5.1.5 Signal-conditioning electronics, that include the functions of pulse counting and pulse-height analysis. 5.1.6 Display or printer, that provides a readout in counts, sulfur content as a percentage by mass % (m/m), or both. CAUTION If the analyser contains a radioactive source, the equipment and manner of use shall comply with the regulations governing the use of ionizing radiation and/or recommendations of the International Commission on Radiological Protection. The radiation source shall be checked for radiation leakage at intervals as required by the regulations. All attention to the source shall only be carried out by fully trained and competent persons, using the correct shielding techniques. 5.2 Analytical balance, capable of weighing to the nearest 0,1 mg. EN