Solid recovered fuels - Methods for the determination of sulphur (S), chlorine (Cl), fluorine (F) and bromine (Br) content

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 applicable 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 completely determined by these methods.
This European Standard provides recommendations concerning standardised methods for  determination of halides and sulphate in the solution obtained after combustion.

Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Schwefel (S), Chlor (Cl), Fluor (F) und Brom (Br)

Diese Europäische Norm legt die Bestimmung von S, Cl, F und Br in festen Sekundärbrennstoffen unterschiedlicher Herkunft und Zusammensetzung nach dem Verbrennen in einer Sauerstoffatmosphäre fest. Dieses Verfahren gilt für Massenanteile größer 0,025 g/kg; die Massenanteile sind abhängig vom Element und von den Bestimmungsverfahren. Im Fall von Fluor ist dieses Verfahren bei einem Massenanteil größer 0,015 g/kg anwendbar. In der Ausgangsprobe vorliegende oder beim Verbrennungsschritt entstandene unlösliche Halogenide und Sulfate werden mit diesen Verfahren nicht vollständig bestimmt. Diese Europäische Norm gibt Empfehlungen hinsichtlich genormter Verfahren zur Bestimmung von Haloge-niden und Sulfaten in der nach der Verbrennung erhaltenen Lösung.

Combustibles solides de récupération - Méthodes pour la détermination de la teneur en soufre (S), en chlore (Cl), en fluor (F), et en brome (Br)

La présente Norme européenne décrit la détermination du S, du Cl, du F et du Br dans les combustibles solides de récupération présentant des origines et des compositions diverses, après combustion dans une atmosphère en présence d’oxygène. Cette méthode s’applique à des concentrations supérieures à 0,025 g/kg, en fonction de l’élément et de la technique de détermination. Dans le cas du fluor, cette méthode est applicable à une concentration supérieure à 0,015 g/kg. Ces méthodes ne permettent pas de déterminer totalement les sulfates et halogénures insolubles présents dans l’échantillon d’origine ou produits au cours de l’étape de combustion. La présente Norme européenne apporte des recommandations concernant les méthodes normalisées de détermination des halogénures et sulfates dans la solution obtenue après combustion.

Trdna alternativna goriva - Metode za določevanje žvepla (S), klora (Cl), fluora (F) in broma (Br)

Ta evropski standard opredeljuje določevanje S, Cl, F in Br v trdnih alternativnih gorivih različnega izvora in sestave po zgorevanju v kisikovi atmosferi. Ta metoda velja za koncentracije nad 0,025 g/kg, odvisno od elementa in tehnike določevanja. Pri fluoru velja metoda za koncentracije nad 0,015 g/kg.
Netopnih halidov in sulfata, ki so prisotni v prvotnem vzorcu ali ki nastanejo med zgorevanjem, te metode ne določijo popolnoma.
Ta evropski standard zagotavlja priporočila v zvezi s standardiziranimi metodami za določevanje halidov in sulfata v raztopini, pridobljeni po zgorevanju.

General Information

Status
Published
Public Enquiry End Date
07-Oct-2009
Publication Date
07-Apr-2011
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
16-Mar-2011
Due Date
21-May-2011
Completion Date
08-Apr-2011

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Schwefel (S), Chlor (Cl), Fluor (F) und Brom (Br)Combustibles solides de récupération - Méthodes pour la détermination de la teneur en soufre (S), en chlore (Cl), en fluor (F), et en brome (Br)Solid recovered fuels - Methods for the determination of sulphur (S), chlorine (Cl), fluorine (F) and bromine (Br) content75.160.10Trda gorivaSolid fuelsICS:Ta slovenski standard je istoveten z:EN 15408:2011SIST EN 15408:2011en,fr,de01-maj-2011SIST EN 15408:2011SLOVENSKI

STANDARDSIST-TS CEN/TS 15408:20071DGRPHãþD
SIST EN 15408:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE 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 récupération - Méthodes pour la détermination de la teneur en soufre (S), en chlore (Cl), en fluor (F), et en brome (Br)

Feste Sekundärbrennstoffe - 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 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 15408:2011: ESIST EN 15408:2011

EN 15408:2011 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41Scope ......................................................................................................................................................52Normative references ............................................................................................................................53Terms and definitions ...........................................................................................................................54Safety remarks .......................................................................................................................................65Principle ..................................................................................................................................................66Apparatus ...............................................................................................................................................67Reagents .................................................................................................................................................78Interferences and sources of error ......................................................................................................89Procedure ...............................................................................................................................................89.1Sample conservation and pre-treatment .................................................................................................89.2Sample preparation..................................................................................................................................89.3Bomb combustion ....................................................................................................................................89.4Calibration ................................................................................................................................................99.5Analysis of calibrations samples ..............................................................................................................99.6Analysis of samples .................................................................................................................................910Calculation and evaluation ...................................................................................................................910.1General ....................................................................................................................................................910.2Total chlorine or total fluorine or total bromine ..................................................................................... 1010.3Total sulphur ......................................................................................................................................... 1011Quality control ..................................................................................................................................... 1012Performance characteristics ............................................................................................................. 1113Test 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 ..................................................................................................................................................... 18

SIST EN 15408:2011

EN 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 endorsement, 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/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/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 15408:2011

EN 15408:2011 (E) 4 Introduction Determination of total sulphur, chlorine, fluorine and bromine content of solid recovered fuels (SRF) is 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 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 provided that it is demonstrated that they give the same results.

SIST EN 15408:2011

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 applicable 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 completely 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 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 15357:2011, Solid recovered fuels — Terminology, definitions and descriptions EN 154131), 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 method — Part 3: Moisture in general analysis sample EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) EN 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 spectrometry (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 (Mohr’s method) ISO 10359-1, Water quality — Determination of fluoride — Part 1: Electrochemical probe method for potable and lightly polluted 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, chloride, bromide, iodide) by combustion and then absorbed or dissolved in aqueous solution

1) To be published. SIST EN 15408:2011

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 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 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 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 or 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 Spectrometry” (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 material 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 contacts 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 with significant chlorine content (chlorine resistant combustion bombs are commercially available). The combustion apparatus is equipped with automatic ignition system and oxygen gas supply. SIST EN 15408:2011

EN 15408:2011 (E) 7 6.2 Balances  Analytical balance resolution ± 0,1 mg;  balance accuracy ± 0,1 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 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. Particularly, 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 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 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 standard solutions are used to prepared working and calibration solution by properly dilution. SIST EN 15408:2011

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 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 ra

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