SIST EN 15290:2011

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Feste Biobrennstoffe - Bestimmung von Hauptelementen - Al, Ca, Fe, Mg, P, K, Si, Na und TiBiocombustibles solides - Dosage des éléments majeurs - Al, Ca, Fe, Mg, P, K, Si, Na et TiSolid biofuels - Determination of major elements - Al, Ca, Fe, Mg, P, K, Si, Na and Ti75.160.10Trda gorivaSolid fuelsICS:Ta slovenski standard je istoveten z:EN 15290:2011SIST EN 15290:2011en,deSIST EN 15290:2011SLOVENSKI
STANDARDSIST-TS CEN/TS 15290:20061DGRPHãþD



SIST EN 15290:2011



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15290
February 2011 ICS 75.160.10 Supersedes CEN/TS 15290:2006English Version
Solid biofuels - Determination of major elements - Al, Ca, Fe, Mg, P, K, Si, Na and Ti
Biocombustibles solides - Dosage des éléments majeurs - Al, Ca, Fe, Mg, P, K, Si, Na et Ti
Feste Biobrennstoffe - Bestimmung von Hauptelementen - Al, Ca, Fe, Mg, P, K, Si, Na und Ti 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 15290:2011: ESIST EN 15290:2011



EN 15290:2011 (E) 2 Contents Page Foreword .3Introduction .41Scope .52Normative references .53Terms and definitions .54Symbols and abbreviations .64.1Symbols .64.2Abbreviations .65Principle .76Reagents .76.1General .76.2Water .76.3Nitric acid (HNO3) .76.4Hydrogen peroxide (H2O2) .76.5Hydrofluoric acid (HF) .76.6Boric acid (H3BO3).76.7Use of Certified Reference Materials (CRM or SRM) .77Apparatus .88Preparation of the test sample .89Procedure .89.1Digestion .89.1.1Part A: Direct determination on the fuel .89.1.2Part B: Determination on a prepared 550 °C ash.99.2Detection methods. 109.3Calibration of the apparatus . 109.4Analysis of digests . 109.5Blank test . 1010Calculations . 1111Performance characteristics . 1112Test report . 12Annex A (informative)
List of conversion factors . 13Annex B (informative)
Performance data . 14Bibliography . 17 SIST EN 15290:2011



EN 15290:2011 (E) 3 Foreword This document (EN 15290:2011) 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 15290:2006. 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 15290:2011



EN 15290:2011 (E) 4 Introduction The elements described as major elements of solid biofuels are in fact major elements of the fuel ashes more than of the fuels. The determination of these elements may be used to assess ash behaviour in a thermal conversion process or to assess utilisation of ashes. Moreover, fuel contamination or process additives are indicated by high values of certain elements. Contamination of fuel with sand or soil is indicated by high values of several elements. In this European Standard, wet chemical methods are described. As an alternative, X-ray fluorescence (XRF) may be used when validated with suitable materials (biomass reference materials). SIST EN 15290:2011



EN 15290:2011 (E) 5 1 Scope This European Standard specifies methods for the determination of major elements of solid biofuels respectively of their ashes, which are Al, Ca, Fe, Mg, P, K, Si, Na, Ti. The determination of other elements such as barium (Ba) and manganese (Mn) is also possible with the methods described in this European Standard. The European Standard includes two parts: Part A describes the direct determination on the fuel, this method is also applicable for sulfur and minor elements, Part B gives a method of determination on a prepared 550 °C ash. 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 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 EN 14775, Solid biofuels  Determination of ash content FprEN 14780, Solid biofuels  Sample preparation EN 15296, Solid biofuels  Conversion of analytical results from one basis to another EN ISO 7980, Water quality  Determination of calcium and magnesium  Atomic absorption spectrometric method (ISO 7980:1986) EN ISO 11885, Water quality  Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885:2007) 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) ISO 9964-1, Water quality  Determination of sodium and potassium  Part 1: Determination of sodium by atomic absorption spectrometry ISO 9964-2, Water quality  Determination of sodium and potassium  Part 2: Determination of potassium by atomic absorption spectrometry ISO 9964-3, Water quality  Determination of sodium and potassium  Part 3: Determination of sodium and potassium by flame emission spectrometry 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 14588:2010 and the following apply. SIST EN 15290:2011



EN 15290:2011 (E) 6 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 realisation 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 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 Al Aluminium Ca Calcium Fe Iron Mg Magnesium P Phosphorus K Potassium Si Silicon Na Sodium Ti Titanium 4.2 Abbreviations CRM Certified Reference Material ICP-OES Inductively Coupled Plasma – Optical Emission Spectrometry ICP-MS Inductively Coupled Plasma – Mass Spectrometry FAAS Flame Atomic Absorption Spectrometry FES Flame Emission Spectrometry SRM Standard Reference Material SIST EN 15290:2011



EN 15290:2011 (E) 7 5 Principle The sample is digested in a closed vessel by the help of reagents, temperature and pressure. The digestion is either carried out directly on the fuel (part A) or on a 550 °C prepared ash (part B). The detection of the elements may be done by ICP-OES, ICP-MS, FAAS or FES. 6 Reagents 6.1 General All reagents should be of analytical grade or better. If minor elements are also to be determined, the best qualities should be used. 6.2 Water Water containing negligible amounts of major elements, i.e. amounts that do not contribute significant to the determinations. Deionised water will normally fulfil this requirement. 6.3 Nitric acid (HNO3) ≥ 65 % (w/w), ρ = 1,41 g/ml 6.4 Hydrogen peroxide (H2O2)
30 % (w/w), ρ = 1,11 g/ml 6.5 Hydrofluoric acid (HF) 40 % (w/w),
= 1,13 g/ml CAUTION — Hydrofluoric acid may lead to health hazards. 6.6 Boric acid (H3BO3) 4 % (w/w) 6.7 Use of Certified Reference Materials (CRM or SRM) Use certified reference materials, issued by an internationally recognized authority, to check if the accuracy of the calibration meets the required performance characteristics. Examples of certified reference materials are: NBS 1570 spinach leaves, NBS 1571 orchard leaves, NBS 1573 tomato leaves and NBS 1575 pine needles. When, due to matrix effects or concentration range limitations, no good recoveries for the certified reference materials can be obtained, calibration with at least two CRM or SRM materials may solve these problems. In that case CRM or SRM materials other than used for the calibration shall be used for verification purposes. NOTE A CRM or SRM is prepared and used for three main purposes: (1) to help deve
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