SIST EN 15297:2011

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Feste Biobrennstoffe - Bestimmung von Spurenelementen - As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V und ZnBiocombustibles solides - Détermination des éléments mineurs - As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V et ZnSolid biofuels - Determination of minor elements - As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V and Zn75.160.10Trda gorivaSolid fuelsICS:Ta slovenski standard je istoveten z:EN 15297:2011SIST EN 15297:2011en,de01-april-2011SIST EN 15297:2011SLOVENSKI
STANDARDSIST-TS CEN/TS 15297:20061DGRPHãþD



SIST EN 15297:2011



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15297
February 2011 ICS 75.160.10 Supersedes CEN/TS 15297:2006English Version
Solid biofuels - Determination of minor elements - As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V and Zn
Biocombustibles solides - Détermination des éléments mineurs - As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V et Zn
Feste Biobrennstoffe - Bestimmung von Spurenelementen -As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V und Zn This European Standard was approved by CEN on 25 December 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 © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15297:2011: ESIST EN 15297:2011



EN 15297:2011 (E) 2 Contents Page Foreword .3Introduction .41Scope .52Normative references .53Terms and definitions .54Symbols and abbreviations .64.1Symbols .64.2Abbreviations .65Principle .66Reagents .76.1General .76.2Water .76.3Hydrofluoric acid (HF) .76.4Hydrogen peroxide (H2O2) .76.5Nitric acid (HNO3) .76.6Boric acid (H3BO3).76.7Use of Certified Reference Materials (CRM or SRM) .77Apparatus .78Preparation of the test sample .89Procedure .89.1Digestion .89.2Detection methods.99.3Calibration of the apparatus .99.4Analysis of the digests .99.5Blank test .910Calculations . 1011Performance characteristics . 1012Test report . 10Annex A (informative)
Performance data . 11Bibliography . 15 SIST EN 15297:2011



EN 15297:2011 (E) 3 Foreword This document (EN 15297:2011) has been prepared by Technical Committee CEN/TC 335 “Solid biofuels”, the secretariat of which is held by SIS. 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 2011, and conflicting national standards shall be withdrawn at the latest by August 2011. This document supersedes CEN/TS 15297:2006. In the pre-normative project BIONORM I&II a robustness test has been performed to find out if all critical parameters in the standard were addressed. Based on the results of that test it has been concluded that all critical parameters were covered. Only minor technical changes were necessary which have been implemented in the revised text. The revision also includes a change of deliverable from Technical Specification to European Standard and updated normative references. 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. 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 United Kingdom.
SIST EN 15297:2011



EN 15297:2011 (E) 4 Introduction The minor elements present in solid biofuels can in some cases be of environmental concern, e.g. it has been shown that certain energy crops will concentrate cadmium and in polluted areas other toxic elements may be found at elevated concentrations in the biofuels. This can be a problem if, for example, the ash from the combustion is to be put back in the forest as a fertilizer. Trace elements in biofuels are often present at very low concentrations requiring great care to avoid contamination in the sample preparation and decomposition steps. The typical concentrations of minor elements in solid biofuels can be found in EN 14961-1 [1]. In this European Standard wet chemical methods are described. Alternative methods such as X-ray fluorescence (XRF) or direct mercury analysers may be used when validated with suitable materials (biomass reference materials). SIST EN 15297:2011



EN 15297:2011 (E) 5 1 Scope This European Standard is intended for determination of the minor elements Arsenic, Cadmium, Cobalt, Chromium, Copper, Mercury, Manganese, Molybdenum, Nickel, Lead, Antimony, Vanadium and Zinc in all solid biofuels. Further it specifies methods for sample decomposition and suggests suitable instrumental methods for the determination of the elements of interest in the digests. The determination of other elements as Selenium, Tin and Thallium is also possible with the method described in this European Standard. 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 12338, Water quality  Determination of mercury  Enrichment methods by amalgamation EN 14588:2010, Solid biofuels  Terminology, definitions and descriptions EN 14774-3, Solid biofuels  Determination of moisture content  Oven dry method  Part 3: Moisture in general analysis sample FprEN 14780, Solid biofuels  Methods for sample preparation EN 15296, Solid biofuels  Conversion of analytical results from one basis to another EN ISO 11885, Water quality  Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885:2007) EN ISO 11969, Water quality  Determination of arsenic  Atomic absorption spectrometric method (hydride technique) (ISO 11969:1996) EN ISO 17294-2, Water quality  Application of inductively coupled plasma mass spectrometry (ICP-MS)  Part 2: Determination of 62 elements (ISO 17294-2:2003) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 14588:2010 and the following apply. 3.1 Reference Material RM material or substance, one or more of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials 3.2 Certified Reference Material CRM reference material, accompanied by a certificate, one or more of whose property values are certified by a procedure which establishes traceability to an accurate realization of the unit in which the property values are expressed, and for which each certified value is accompanied by an uncertainty at a stated level of confidence SIST EN 15297:2011



EN 15297:2011 (E) 6 3.3 NIST Standard Reference Material® SRM CRM issued by NIST that also meets additional NIST-specific certification criteria and is issued with a certificate or certificate of analysis that reports the results of its characterisations and provides information regarding the appropriate use(s) of the material 4 Symbols and abbreviations 4.1 Symbols As Arsenic Cd Cadmium Co Cobalt Cr Chromium Cu Copper Hg Mercury Mn Manganese Mo Molybdenum Ni Nickel Pb Lead Sb Antimony V Vanadium Zn Zinc 4.2 Abbreviations CV-AAS
Cold vapour atomic absorption spectrometry GF-AAS Graphite furnace atomic absorption spectrometry HG-AAS Hydride generation atomic absorption spectrometry ICP-OES
Inductively coupled plasma optical emission spectrometry ICP-MS
Inductively coupled plasma mass spectrometry 5 Principle The analysis sample is digested in a closed vessel made from a fluoropolymer using nitric acid, hydrogen peroxide and hydrofluoric acid in a microwave oven or a resistance oven or heating block. The digest is then diluted and the elements determined with suitable instruments. SIST EN 15297:2011



EN 15297:2011 (E) 7 6 Reagents 6.1 General All reagents shall be of analytical grade or better. If the blank level is unacceptably high i.e. more then 30 % of the determined value, the use of ultra pure reagents should be investigated. 6.2 Water Water containing negligible amounts of the minor elements i.e. amounts that do not contribute significantly to the determinations. Deionised water or doubly distilled water will normally fulfil this requirement. NOTE The water used for analytical trace metal work is normally produced using a system for production of ultra pure water for laboratory use conductivity = 0,056 µS/cm. 6.3 Hydrofluoric acid (HF) 40 % (w/w), ρ = 1,13 g/ml CAUTION — Hydrofluori
...