1、November 2011 Translation by DIN-Sprachendienst.English price group 15No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).I
2、CS 75.160.10!$xOj“1854471www.din.deDDIN EN 15410Solid recovered fuels Method for the determination of the content of major elements (Al, Ca,Fe, K, Mg, Na, P, Si, Ti)English translation of DIN EN 15410:2011-11Feste Sekundrbrennstoffe Verfahren zur Bestimmung des Gehaltes an Hauptelementen (Al, Ca, Fe
3、, K, Mg, Na, P,Si, Ti)Englische bersetzung von DIN EN 15410:2011-11Combustibles solides de rcupration Mthodes pour la dtermination de la teneur en lments majeurs (Al, Ca, Fe, K, Mg, Na,P, Si et Ti)Traduction anglaise de DIN EN 15410:2011-11SupersedesDIN CEN/TS 15410:2006-12www.beuth.deDocument compr
4、ises pagesIn case of doubt, the German-language original shall be considered authoritative.3111.11 31DIN EN 15410:2011-11 2 National foreword This standard has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels” (Secretariat: SFS, Finland). The responsible German body involved in
5、 its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-83 AA Sekundrbrennstoffe. The DIN Standards corresponding to the International Standards referred to in this document are as follows:s EN ISO 3696 DIN ISO 3696 ISO 5725-2 DIN
6、ISO 5725-2 ISO 9964-1 DIN 38406-14 ISO 9964-2 DIN 38406-13 ISO 9964-3 DIN ISO 9964-3 Amendments This standard differs from DIN CEN/TS 15410:2006-12 as follows: a) method C is informative; b) Annex B (informative) “Performance data” and Annex C (informative) “Major results of ruggedness testing” have
7、 been included; c) normative references and the Bibliography have been updated; d) the standard has been editorially revised. Previous editions DIN CEN/TS 15410: 2006-12 DIN EN 15410:2011-11 3 National Annex NA (informative) Bibliography DIN 38406-13, German standard methods for the examination of w
8、ater, waste water and sludge Cations (group E) Determination of potassium by atomic absorption spectrometry (AAS) using an air-acetylene flame (E 13) DIN 38406-14, German standard methods for the examination of water, waste water and sludge Cations (group E) Determination of sodium by atomic absorpt
9、ion spectrometry (ASS) using an air-acetylene flame (E 14) DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibi
10、lity of a standard measurement method DIN ISO 9964-3, Water quality Determination of sodium and potassium Part 3: Determination of sodium and potassium by flame emission spectrometry DIN EN 15410:2011-11 4 This page is intentionally blank. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15410 S
11、eptember 2011 ICS 75.160.10 Supersedes CEN/TS 15410:2006English Version Solid recovered fuels - Methods for the determination of the content of major elements (Al, Ca, Fe, K, Mg, Na, P, Si, Ti) Combustibles solides de rcupration - Pour la dtermination de la teneur en lments majeurs (Al, Ca, Fe, K, M
12、g, Na, P, Si et Ti) Feste Sekundrbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Hauptelementen (Al, Ca, Fe, K, Mg, Na, P, Si, Ti) This European Standard was approved by CEN on 15 July 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditio
13、ns 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
14、 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 standard
15、s 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 Unit
16、ed Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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 15410:2011:
17、EEN 15410:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .64 Safety remarks .65 Principle 66 Apparatus .77 Reagents .88 Procedure .88.1 Sample conservation and pre-treatment .88.2 Sample preparation .89 Digestion procedure 99.1 Method A .99
18、.2 Method B .99.3 Method C (informative) .910 Analysis of the digestion solutions .910.1 Preparation of the solution for analysis 910.2 Analytical step . 1010.3 XRF analysis on ashed samples sample preparation 1011 Expression of results . 1012 Quality control . 1113 Performance characteristics . 111
19、4 Test report . 11Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF . 12Annex B (informative) Performance data . 14Annex C (informative) Major results of ruggedness testing 23Bibliography . 27DIN EN 15410:2011-11EN 15410:2011 (E) 3 Foreword This d
20、ocument (EN 15410:2011) has been prepared by Technical Committee CEN/TC 343 “Solid Recovered Fuels”, the secretariat of which is held by SFS. 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
21、2012, and conflicting national standards shall be withdrawn at the latest by March 2012. 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 right
22、s. This document supersedes CEN/TS 15410:2006. This document differs from CEN/TS 15410:2006 only editorially. 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,
23、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 the United Kingdom. DIN EN 15410:2011-11EN 1
24、5410:2011 (E) 4 Introduction Accurate determination of trace element content in solid recovered fuels is important for environmental and technical reasons both in the production and combustion stage. The determination of major elements such as Al, Ca, Fe, Mg, P, K, Si, Na and Ti can be helpful to pr
25、edict the melting behaviour and slagging of the ash. After digestion of the solid recovered fuels using different methods, a number of analytical techniques can be used for the quantification of the trace element content. They include Inductively Coupled Plasma with optical or mass detection, Flame
26、Atomic Spectroscopy, Graphite Furnace Atomic Absorption Spectrometry and X-ray fluorescence spectrometry. X-ray fluorescence allows the simultaneous determination of these elements after ashing of solid recovered fuel (SRF). Direct analysis of the SRF material is not possible by XRF due to the sampl
27、e inhomogeneity and because suitable certified reference materials for calibration are not available. DIN EN 15410:2011-11EN 15410:2011 (E) 5 1 Scope This European Standard specifies three methods of digestion for solid recovered fuels: a) microwave assisted digestion with hydrofluoric, nitric and h
28、ydrochloric acid mixture; b) hot water bath digestion of with hydrofluoric, nitric and hydrochloric acid mixture, after ashing of the SRFs sample; c) oven digestion with nitric, perchloric and hydrofluoric acid mixture. Instrumental determination of Si, Al, K, Na, Ca, Mg, Fe, P, and Ti is performed
29、by Inductively Coupled Plasma Spectrometry with optical detection or other suitable spectroscopic techniques such as Flame Atomic Spectroscopy. The effectiveness of the digestion can be verified by qualitative X-ray fluorescence (XRF) analysis on the remaining residue. If necessary, an alternative d
30、igestion method (among those proposed) shall be used. XRF can be used for the analysis of Si, Al, K, Na, Ca, Mg, Fe, P, Ti, after ashing (550 C) of the sample: other elements can be analysed by XRF provided that the concentration levels are above the instrumental detection limits of the XRF instrume
31、ntation and after proper preliminary testing. Method a) is recommended for general use, but the amount of the test portion can be very low in case of high concentration of organic matter. Method b) is recommended for SRFs with high organic matter concentration that can be difficult to digest with th
32、e other methods. Method c) is recommended for SRFs samples for which the other methods leave a significant insoluble residue. All the listed methods are suitable for the determination of Si, provided that closed containers are used for sample dissolution. XRF is highly recommended for Si, P and Ti a
33、nalysis. Alternative digestion methods can be applied if their performance is proved to be comparable with those of the methods mentioned in a) to c) (see Annex C). 2 Normative references The following referenced documents are indispensable for the application of this European Standard. For dated re
34、ferences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 13656, Characterization of waste Microwave assisted digestion with hydrofluoric (HF), nitric (HNO3) and hydrochloric (HCI) acid mixture for subsequen
35、t determination of elements EN 15357:2011, Solid recovered fuels Terminology, definitions and descriptions EN 15403, Solid recovered fuels Determination of ash content EN 15413, Solid recovered fuels Methods for the preparation of the test sample from the laboratory sample EN 15414-3, Solid recovere
36、d fuels Determination of moisture content using the oven dry method Part 3: Moisture in general analysis sample EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) DIN EN 15410:2011-11EN 15410:2011 (E) 6 EN ISO 11885, Water quality Determination of se
37、lected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885:2007) EN ISO 12020, Water quality Determination of aluminium Atomic absorption spectrometric methods (ISO 12020:1997) EN ISO 15586, Water quality Determination of trace elements using atomic absorption s
38、pectrometry with graphite furnace (ISO 15586:2003) ISO 9964 (all parts), Water quality Determination of sodium and potassium 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15357:2011 and the following apply. 3.1 digestion mineralization of the organi
39、c matter of a sample and dissolution of its mineral part, more or less completely, when reacted with a reagent mixture 3.2 microwave unit whole microwave digestion system (oven and associated equipment) 4 Safety remarks The safety in handling of potentially hazardous materials is dealt with by the r
40、elevant national and European regulations, which every laboratory should refer to. In addition the following information is given: Only experienced personnel can use the microwave apparatus, following the operating instructions described in the manufacturer manual; Most of the reagents used within t
41、his European Standard are strongly corrosive and toxic. Safety precautions are absolutely necessary due to strong corrosive reagents, high temperature and high pressure; All procedures have to be performed in a hood or in closed force-ventilated equipment. By the use of strong oxidising reagents the
42、 formation of explosive organic intermediates is possible especially when dealing with samples with a high organic content. Do not open pressurised vessels before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products; The X-ray fluorescence spectrometers on the ma
43、rket are generally approved fully protected apparatus. This means that the user is not subjected to any radiation when operating the apparatus. All the apparatus are subject to specific official approval and acceptance conditions; The person responsible for managing or supervising the operation of X
44、-ray equipment shall provide evidence of his knowledge of radiation protection according to national regulations. 5 Principle The test portion is digested using one of the proposed methods with a suitable acid mixture. The digested sample is then analysed by inductively coupled plasma atomic emissio
45、n spectroscopy. DIN EN 15410:2011-11EN 15410:2011 (E) 7 For XRF analysis, the sample is ashed at 550 C and the ash is homogenised in a ball mill to obtain a uniform size dimension of the particles. The ash is then pressed in the form of pellet or fused with tetraborate. Both techniques are suitable
46、for the analysis by XRF. Coal ash and other ashes of various origins can be used for instrument calibration. 6 Apparatus 6.1 Microwave unit Intended for laboratory use and preferably with temperature control. 6.2 Resistance heating oven A resistance heated oven or heating block that can be used at a
47、 temperature of at least 220 C and an accuracy of 10 C. 6.3 Digestion vessels The vessels used in the microwave unit shall be equipped with a pressure relieve valve or another technical equipment which avoids the bursting of the vessels at suddenly occurring excess pressure. The material of the vess
48、els has to be inert to the acids used for digestion. The digestion vessel shall withstand the pressure of at least 8 bar. If the amount of organic carbon exceeds 100 mg it has to be ensured that the digestion vessel is capable of withstanding higher pressures. 6.4 Inductively coupled plasma Normal c
49、ommercial instrumentation with optical or quadrupole mass detector (ICP-OES, ICP-MS). 6.5 X-ray fluorescence spectrometer Energy or wavelength dispersion system suitable for quantitative/qualitative analysis of the elements listed in this European Standard. 6.6 Atomic Absorption Spectrometer Normal commercial instrumentation with air-acetylene burner or with graphite tube atomizer and background correc
