DIN EN 15411-2011 Solid recovered fuels - Methods for the determination of the content of trace elements (As Ba Be Cd Co Cr Cu Hg Mo Mn Ni Pb Sb Se Tl V and Zn) German version EN 1.pdf

1、November 2011 Translation by DIN-Sprachendienst.English price group 13No 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!$vT.“1834911www.din.deDDIN EN 15411Solid recovered fuels Methods for the determination of the content of trace elements (As, Ba,Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)English translation of DIN EN 15411:2011-11Feste Sekundrbrennstoffe Verfahren zur Bestimmung des G

3、ehaltes an Spurenelementen (As, Ba, Be, Cd, Co, Cr,Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V und Zn)Englische bersetzung von DIN EN 15411:2011-11Combustibles solides de rcupration Mthodes de dtermination de la teneur en lments ltat de traces (As, Ba, Be, Cd,Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V

4、et Zn)Traduction anglaise de DIN EN 15411:2011-11SupersedesDIN CEN/TS 15411:2006-12www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 27 pages11.11 DIN EN 15411:2011-11 2 A comma is used as the decimal marker. National foreword This standa

5、rd has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels” (Secretariat: SFS, Finland). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-83 AA Sekundrbrennstoffe. Th

6、e DIN Standards corresponding to the International Standards referred to in this document are as follows: EN ISO 3696 DIN ISO 3696 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN CEN/TS 15411:2006-12 as follows: a) method B (9.2) and method C (9.3) of the digestion procedure are

7、informative; b) Annex B (informative) “Performance data” and Annex C (informative) “Major results of ruggedness testing” have been included; c) normative references and the Bibliography have been updated; d) the standard has been editorially revised. Previous editions DIN CEN/TS 15411: 2006-12 Natio

8、nal Annex NA (informative) Bibliography 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 reproducibility of a standard

9、measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15411 September 2011 ICS 75.160.10 Supersedes CEN/TS 15411:2006English Version Solid recovered fuels - Methods for the determination of the content of trace elements (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V

10、 and Zn) Combustibles solides de rcupration - Mthodes de dtermination de la teneur en lments ltat de traces (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V et Zn) Feste Sekundrbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Spurenelementen (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, M

11、n, Ni, Pb, Sb, Se, Tl, V und Zn) 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 standard without any alteration. Up-to-date

12、 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 u

13、nder 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, Franc

14、e, 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 DE NORMALISATION EUROPISCHES KOMITEE FR

15、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 15411:2011: EEN 15411:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and

16、definitions .54 Safety remarks .65 Principle 66 Apparatus .67 Reagents .78 Procedure .78.1 Sample conservation and pre-treatment .78.2 Sample preparation .89 Digestion procedure 89.1 Method A .89.2 Method B (informative) .89.3 Method C (informative) .810 Analysis of the digestion solutions .910.1 Pr

17、eparation of the solution for analysis 910.2 Analytical step 911 Expression of results 912 Quality control 913 Performance characteristics . 1014 Test report . 10Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF . 11Annex B (informative) Performan

18、ce data . 13Annex C (informative) Major results of ruggedness testing 22Bibliography . 25DIN EN 15411:2011-11 EN 15411:2011 (E) 3 Foreword This document (EN 15411:2011) has been prepared by Technical Committee CEN/TC 343 “Solid Recovered Fuels”, the secretariat of which is held by SFS. This European

19、 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 withdrawn at the latest by March 2012. Attention is drawn to the possibility that some of the elements of

20、 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 15411:2006. This document differs from CEN/TS 15411:2006 only editorially. According to the CEN/CENELEC Internal Regulat

21、ions, 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

22、, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15411:2011-11 EN 15411:2011 (E) 4 Introduction Accurate determination of trace element content in solid recovered fuels is important for environmental and technical reasons

23、 both in the production and combustion stage. 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, graphite furn

24、ace Atomic Absorption Spectrometry and, when available, dedicated specific method (e.g. for mercury). DIN EN 15411:2011-11 EN 15411:2011 (E) 5 1 Scope This European Standard specifies three methods of digestion for solid recovered fuels: a) microwave assisted digestion with hydrofluoric, nitric and

25、hydrochloric 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 As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn, Mo, Ni, Sb, S

26、e, Tl, V, Zn is performed by Inductively Coupled Plasma with optical or mass detection or graphite furnace Atomic Absorption Spectrometry. Hg can be analysed only after the microwave assisted procedure or, alternatively, by a direct analysis method (Hg direct AMA). The effectiveness of the digestion

27、 can be verified by qualitative X-ray fluorescence (XRF) analysis on the remaining residue. If necessary, an alternative digestion method (among those proposed) is used. Method a) is recommended for general use, but the amount of the test portion can be very low in case of high concentration of orga

28、nic matter. Method b) is recommended for Solid Recovered Fuel (SRF) with high organic matter concentration that can be difficult to digest with the other methods. This method is not suitable for mercury. Method c) is recommended for Solid Recovered Fuel (SRF) samples for which the other methods leav

29、e a significant insoluble residue. 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 Europ

30、ean Standard. For dated references, 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)

31、acid mixture for subsequent 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

32、EN 15414-3, Solid recovered 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) 3 Terms and definitions For the purpose of this document, the

33、 terms and definitions given in EN 15357:2011 and the following apply. DIN EN 15411:2011-11 EN 15411:2011 (E) 6 3.1 digestion mineralization of the organic 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 mi

34、crowave 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 should refer to. In addition the following information is given: Only experience

35、d 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 precautions are absolutely necessary due to strong corrosive reagents, high tempera

36、ture 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, especially when dealing with samples with a high organic content. Do not open pressuris

37、ed vessels before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products. 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 the most appropriate spectrometric technique,

38、such as atomic absorption or emission spectroscopy. 6 Apparatus 6.1 Microwave unit Intended for laboratory use and preferably equipped 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 o

39、f 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 vessels has to be inert to the acids used for digest

40、ion. 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 DIN EN 15411:2011-11 EN 15411:2011 (E) 7 Normal commerc

41、ial instrumentation with optical or mass spectrometric detector (ICP-OES, ICP-MS). 6.5 Atomic absorption spectrophotometer Normal commercial instrumentation, equipped with graphite furnace or hydride generation systems or cold vapour (GF-AAS, HG-AAS, CV-AAS). 6.6 X-ray fluorescence spectrometer Ener

42、gy or wavelength dispersion system suitable for qualitative analysis of the elements listed in this European Standard (with the exception of beryllium). 6.7 Balances Analytical balance resolution 0,1 mg. 6.8 General equipment General laboratory equipment, including volumetric graduated flasks and pi

43、pettes of adequate size. Filter equipment of adequate chemical resistance and purity or centrifuge. The use of glassware shall be excluded when free hydrofluoric acid is present. The glassware used in the digestion procedure should be carefully pre-cleaned with for example 10 % nitric acid solution.

44、 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 listed in Clause 2. NOTE Acids used in the preparation of standards and for s

45、ample processing are of high purity. Redistilled acids are recommended because of the high sensitivity of ICP-MS. Nitric acid at less than 2 % (v/v) is recommended for ICP-MS to minimize damage to the interface and to minimize isobaric molecular-ion interferences with the analytes. Many more molecul

46、ar-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), 1,14 g/ml. 7.4 Perchloric acid (HClO4), 70 % (w/w), 1,62 g/ml. 7.5 Hydrochlo

47、ric acid (HCl), 65 % (w/w), 1,40 g/ml. 8 Procedure 8.1 Sample conservation and pre-treatment The laboratory samples shall be stored according to guidelines defined in Annex A. DIN EN 15411:2011-11 EN 15411:2011 (E) 8 It is advisable to contact the people performing the sampling in order to agree a p

48、rocedure for the laboratory sample preparation and storage before delivering to the laboratory. In particular, any treatment procedure which can increase the temperature of the material above 40 C should be avoided, in order to avoid significant loss of mercury or other volatile compounds. Furthermo

49、re, any possible source of contamination during the laboratory sample preparation (e.g. grinding with metallic apparatus) shall be avoided or reduced as much as possible. The laboratory sample should be stored and delivered in sealed high-density plastic containers. 8.2 Sample preparation The test portion shall be prepared from the laboratory sample according to EN 15413. In addition, for the purposes of this method, t