DIN EN 15408-2011 Solid recovered fuels - Methods for the determination of sulphur (S) chlorine (Cl) fluorine (F) and bromine (Br) content German version EN 15408 2011《固体回收燃料 硫(S) .pdf

1、May 2011 Translation by DIN-Sprachendienst.English price group 11No 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).ICS 75

2、.160.10!$p_k“1776072www.din.deDDIN EN 15408Solid recovered fuels Methods for the determination of sulphur (S), chlorine (Cl), fluorine (F)and bromine (Br) contentEnglish translation of DIN EN 15408:2011-05Feste Sekundrbrennstoffe Verfahren zur Bestimmung des Gehaltes an Schwefel (S), Chlor (Cl), Flu

3、or (F) und Brom(Br)Englische bersetzung von DIN EN 15408:2011-05Combustibles solides de rcupration Mthodes pour la dtermination de la teneur en soufre (S), en chlore (Cl), en fluor (F), eten brome (Br)Traduction anglaise de DIN EN 15408:2011-05SupersedesDIN CEN/TS 15408:2006-12www.beuth.deDocument c

4、omprises pagesIn case of doubt, the German-language original shall be considered authoritative.2004.11 DIN EN 15408:2011-05 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels” (Secretariat: SFS, Finland).

5、The responsible German body involved in 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: IS

6、O 5725-5 DIN ISO 5725-5 ISO 9297 DIN 38405-1 ISO 10359-1 DIN 38405-4 EN ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN CEN/TS 15408:2006-12 as follows: a) the prestandard status has been changed to that of a full standard; b) Subclause 9.3 “Bomb combustion” has been extended; c) Ann

7、ex B “Data on performance characteristics” and Annex C “Major results of ruggedness testing” (both informative) have been included; d) the Bibliography has been updated; e) the standard has been editorially revised. Previous editions DIN CEN/TS 15408: 2006-12 National Annex NA (informative) Bibliogr

8、aphy DIN 38405-1, German standard methods for the examination of water, waste water and sludge Anions (group D) Determination of chloride ions (D 1) DIN 38405-4, German standard methods for the examination of water, waste water and sludge Anions (group D) Determination of fluoride (D 4) DIN ISO 3696

9、, Water for analytical laboratory use Specification and test methods DIN ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE

10、 NORM EN 15408 March 2011 ICS 75.160.10 Supersedes CEN/TS 15408:2006English Version Solid recovered fuels - Methods for the determination of sulphur (S), chlorine (Cl), fluorine (F) and bromine (Br) content Combustibles solides de rcupration - Mthodes pour la dtermination de la teneur en soufre (S),

11、 en chlore (Cl), en fluor (F), et en brome (Br) Feste Sekundrbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Schwefel (S), Chlor (Cl), Fluor (F) und Brom (Br) This European Standard was approved by CEN on 22 January 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulatio

12、ns 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. T

13、his 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 me

14、mbers 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, Spai

15、n, Sweden, Switzerland and United 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 Me

16、mbers. Ref. No. EN 15408:2011: EEN 15408:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Safety remarks .65 Principle 66 Apparatus .67 Reagents .78 Interferences and sources of error 89 Procedure .89.1 Sample conservation and pre-treatme

17、nt .89.2 Sample preparation89.3 Bomb combustion 89.4 Calibration 99.5 Analysis of calibrations samples 99.6 Analysis of samples .910 Calculation and evaluation .910.1 General 910.2 Total chlorine or total fluorine or total bromine . 1010.3 Total sulphur . 1011 Quality control . 1012 Performance char

18、acteristics . 1113 Test report . 11Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF 12Annex B (informative) Data on performance characteristics 14Annex C (informative) Major results of ruggedness testing 17Bibliography . 18DIN EN 15408:2011-05 EN

19、 15408:2011 (E) 3 Foreword This document (EN 15408:2011) 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 end

20、orsement, at the latest by September 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. This document supersedes CEN/TS 15408:2006. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/

21、or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document differs from CEN/TS 15408:2006 only editorially. According to the CEN

22、/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, Lit

23、huania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 15408:2011-05 EN 15408:2011 (E) 4 Introduction Determination of total sulphur, chlorine, fluorine and bromine content of solid recovered fuels (SRF) is

24、 necessary for environmental and technical reasons both in the production and combustion stage. During the combustion process they are usually converted to sulphates and halides. These reaction products contribute significantly to corrosion and environmentally harmful emissions. This method consists

25、 of an oxygen combustion procedure followed by trapping of sulphur, chloride, fluoride and bromide in an absorbing solution and subsequent determination by different techniques. Alternatively, direct automatic techniques can be used for S and Cl determination. Other methods could also be used provid

26、ed that it is demonstrated that they give the same results. DIN EN 15408:2011-05 EN 15408:2011 (E) 5 1 Scope This European Standard specifies the determination of S, Cl, F and Br in solid recovered fuels of various origin and composition after combustion in oxygen atmosphere. This method is applicab

27、le for concentrations over 0,025 g/kg, depending on the element and on the determination technique. In the case of fluorine this method is applicable for concentration over 0,015 g/kg. Insoluble halides and sulphate present in the original sample or produced during the combustion step are not comple

28、tely determined by these methods. This European Standard provides recommendations concerning standardised methods for determination of halides and sulphate in the solution obtained after combustion. 2 Normative references The following referenced documents are indispensable for the application of th

29、is document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15357:2011, Solid recovered fuels Terminology, definitions and descriptions EN 154131), Solid recovered fuels Methods for th

30、e preparation of the test sample from the laboratory sample 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) E

31、N ISO 10304-1:2009, Water quality Determination of dissolved anions by liquid chromatography of ions Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate (ISO 10304-1:2007) EN ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrome

32、try (ICP-MS) Part 2: Determination of 62 elements (ISO 17294-2:2003) ISO 9297, Water quality Determination of chloride Silver nitrate titration with chromate indicator (Mohrs method) ISO 10359-1, Water quality Determination of fluoride Part 1: Electrochemical probe method for potable and lightly pol

33、luted water 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 halogen content sum of halogens contained as organic and inorganic compounds in the solid recovered fuels, which can be converted to halides (fluoride,

34、 chloride, bromide, iodide) by combustion and then absorbed or dissolved in aqueous solution 1)To be published. DIN EN 15408:2011-05 EN 15408:2011 (E) 6 NOTE The above definition is valid for this empirical European Standard only and do not comply with scientific definitions of halogen content. 3.2

35、oxygen combustion combustion of material in oxygen atmosphere 4 Safety remarks The safety in handling of potentially hazardous materials is dealt with relevant national and European regulations, which every laboratory should refer to. In addition the following information is given: only experienced

36、personnel can use the oxygen combustion apparatus, following the operating instructions described in the manufacturer manual; precautions shall be taken by the operator for reactive gas (oxygen) at high temperature and high pressure. 5 Principle The determination of S, Cl, F and Br is carried out in

37、 two steps or by using automatic equipment: the sample is oxidized by combustion in a bomb containing oxygen under pressure. Halogenated and sulphur compounds are converted respectively to fluoride, chloride, bromide and sulphate which are absorbed and/or dissolved in an absorption solution (water o

38、r KOH 0,2 mol/l solution); analysis of Cl, F and S and Br by ion chromatography or other suitable technique, are reported in the reference documents listed in Clause 2: for Cl, F, S and Br in EN ISO 10304-1, for F only in ISO 10359-1. Br is preferably determined by “Inductively Coupled Plasma Mass S

39、pectrometry” (ICP-MS) according to EN ISO 17294-2 since several oxidation states of Br occur after oxygen combustion. 6 Apparatus Apart ordinary laboratory apparatus, the following devices are required: 6.1 Oxygen combustor Equipped with a combustion bomb made of stainless steel or any other materia

40、l that will not be affected by the combustion process or products (the materials used may adsorb or react with acid gases formed during combustion or it may be not possible to clean the bomb completely between combustions). The bomb is equipped with oxygen inlet and safety valve and electrical conta

41、cts for spark generation. Many commercially available systems can be used. The combustion bomb may be the same as used for the determination of the calorific value. Carefully check the characteristics of the combustion bomb, in order to be sure that it is suitable for the processing of materials wit

42、h significant chlorine content (chlorine resistant combustion bombs are commercially available). The combustion apparatus is equipped with automatic ignition system and oxygen gas supply. DIN EN 15408:2011-05 EN 15408:2011 (E) 7 6.2 Balances Analytical balance resolution 0,1 mg; balance accuracy 0,1

43、 g. 6.3 Ion chromatograph An ion chromatograph with suitable anion separator column, pre-column, background suppressor and conductivity cell. 6.4 Apparatus for titrimetry Any suitable apparatus can be used, with colorimetric or potentiometric final point determination. 6.5 Inductively Coupled Plasma

44、 Mass Spectrometry (ICP-MS) Any suitable apparatus with normal resolution and pneumatic sample introduction system. 6.6 Automatic analyzer Commercial instruments for S and Cl determination. 7 Reagents All reagents shall be at least of analytical grade and suitable for their specific purposes. Partic

45、ularly, they shall be free of sulphur and halogens. 7.1 Water of grade 1 as specified by EN ISO 3696. 7.2 Oxygen Should be free of combustion material, minimum 99,99 % purity. 7.3 Nitrogen Should be chromatographic grade for the ion chromatograph. 7.4 Eluent for ion chromatography Carbonate/hydrogen

46、 carbonate mixed solution is suitable as eluent for ion chromatographic separation. Other eluents can be used, following the working instruction with the particular column used. 7.5 Absorbing solution Water is appropriate for most application. If the content of chlorine is 1 % or if bromine shall be

47、 determined, alkaline KOH 0,2 mol/l solution is more efficient for trapping the gases. As a preliminary check, XRF analysis can be used to check for the presence of Br or high chlorine content. 7.6 Stock standard solutions 1 000 mg/l chlorine, fluorine, bromine and sulphate commercially available st

48、andard solutions are used to prepared working and calibration solution by properly dilution. DIN EN 15408:2011-05 EN 15408:2011 (E) 8 7.7 Certified reference material (CRMs) The trapping yield can be checked using a material with characteristic similar to SRF, e.g. a solid waste certified reference

49、material. 7.8 Control mixtures To create an appropriate control mixture, choose the control substances in combination so that all elements that shall be determined in the samples are represented. The amount of halogen and sulphur contents shall be in the same range of the element contents of the samples and approximately in the middle of the working range of the determination techniques. The mixture of the contro