1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15410:2011Solid recovered fuels Methods for the determinationof the content of majorelements (Al, Ca, Fe, K, Mg, Na,P, Si, Ti)BS EN 15410:2011 BRITISH STANDARDNational fore
2、wordThis British Standard is the UK implementation of EN 15410:2011. Itsupersedes DD CEN/TS 15410:2006 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/17, Solid biofuels.A list of organizations represented on this committee can beobtained on request
3、 to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 69793 7ICS 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard
4、 was published under the authority of theStandards Policy and Strategy Committee on 30 September 2011.Amendments issued since publicationDate Text affectedBS EN 15410:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15410 September 2011 ICS 75.160.10 Supersedes CEN/TS 15410:2006English Versi
5、on 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, Mg, Na, P, Si et Ti) Feste Sekundrbrennstoffe - Verfahren zur Bestimmu
6、ng des Gehaltes an Hauptbestandteilen (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 conditions for giving this European Standard the status of a national sta
7、ndard 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
8、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 Re
9、public, 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 COMIT EUROPEN
10、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: EBS EN 15410:2011EN 15410:2011 (E) 2 Contents Page Foreword 3Intr
11、oduction .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 .99.2 Method B .99.3 Method C (informative) .910 Ana
12、lysis 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 . 1114 Test report . 11Annex A (normative) Guidelines
13、- Characteristics of the laboratory sample for chemical analysis of SRF . 12Annex B (informative) Performance data . 14Annex C (informative) Major results of ruggedness testing 23Bibliography . 27BS EN 15410:2011EN 15410:2011 (E) 3 Foreword This document (EN 15410:2011) has been prepared by Technica
14、l 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 2012, and conflicting national standards shall be wit
15、hdrawn 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 rights. This document supersedes CEN/TS 15410:2006. This d
16、ocument 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, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Fi
17、nland, 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. BS EN 15410:2011EN 15410:2011 (E) 4 Introduction Accurate determination of tr
18、ace 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 predict the melting behaviour and slagging of the ash. Afte
19、r 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 Atomic Spectroscopy, Graphite Furnace Atomic Absorption S
20、pectrometry 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 sample inhomogeneity and because suitable certified reference
21、materials for calibration are not available. BS EN 15410:2011EN 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 hydrochloric acid mixture; b) hot water bath digestion of with
22、 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 by Inductively Coupled Plasma Spectrometry with optical detec
23、tion 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 digestion method (among those proposed) shall be used. XRF can
24、 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 instrumentation and after proper preliminary testing. Method a) is re
25、commended 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 the other methods. Method c) is recommended for SRFs samples fo
26、r 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 analysis. Alternative digestion methods can be applied if thei
27、r 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 references, only the edition cited applies. For undated referen
28、ces, 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 subsequent determination of elements EN 15357:2011, Solid recovered fu
29、els 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 recovered fuels Determination of moisture content using the oven dry
30、method Part 3: Moisture in general analysis sample EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) BS EN 15410:2011EN 15410:2011 (E) 6 EN ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission sp
31、ectrometry (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 spectrometry with graphite furnace (ISO 15586:2003) ISO 9964 (all
32、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 organic matter of a sample and dissolution of its mineral part, more or
33、 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 relevant national and European regulations, which every laboratory
34、 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 this European Standard are strongly corrosive and toxic. Safety pr
35、ecautions 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 formation of explosive organic intermediates is possible especia
36、lly 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 market are generally approved fully protected apparatus. This means
37、 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-ray equipment shall provide evidence of his knowledge of radiati
38、on 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 emission spectroscopy. BS EN 15410:2011EN 15410:2011 (E) 7 For XRF analy
39、sis, 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 for the analysis by XRF. Coal ash and other ashes of various origins
40、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 temperature of at least 220 C and an accuracy of 10 C. 6.3 Digestion
41、 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 vessels has to be inert to the acids used for digestion. The digestion ve
42、ssel 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 commercial instrumentation with optical or quadrupole mass detector (I
43、CP-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
44、 tube atomizer and background correction system and with hollow cathode lamps or electrodeless discharge lamp. 6.7 Press 6.8 Balance Analytical balance with a resolution of 0,1 mg. 6.9 General equipment General laboratory equipment, including volumetric graduated flasks and pipettes of adequate size
45、. Filter equipment of adequate chemical resistance and purity or centrifuge. The use of glassware shall be excluded when free hydrofluoric acid is present. When using hydrofluoric acid, a special fume cupboard can be required. The glassware used in the digestion procedure should be accurately pre-cl
46、eaned with 10 % nitric acid solution. BS EN 15410:2011EN 15410:2011 (E) 8 7 Reagents All reagents shall be at least of analytical grade and suitable for their specific purposes. Other specific reagents are listed and described in the reference methods for digestion or instrumental determination list
47、ed in Clause 2. NOTE Acids used in the preparation of standards and for sample processing should be of high purity. Redistilled acids are recommended because of the high sensitivity of ICP-MS. Nitric acid at less than 2 % (v/v) is required for ICP-MS to minimize damage to the interface and to minimi
48、ze isobaric molecular-ion interferences with the analytes. Many more molecular-ion interferences are observed when hydrochloric and sulphuric acids are used. 7.1 Water of grade 1 as specified by EN ISO 3696:1995. 7.2 Nitric acid (HNO3), 65 % (w/w), = 1,40 g/ml. 7.3 Hydrofluoric acid (HF), 40 % (w/w)
49、, = 1,14 g/ml. 7.4 Perchloric acid (HClO4), 70 % (w/w), = 1,62 g/ml. 7.5 Hydrochloric acid (HCl), 36 % (w/w), = 1,179 g/ml. 7.6 Helium (He), minimum 99,99 purity for use as a chamber purge gas for the analysis of light elements when the vacuum is not used. 7.7 Argon (Ar), with a minimum purity of 99,99 %. 8 Procedure 8.1 Sample conservation and pre-treatment The laboratory samples shall be stored according to guidelines defin
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