1、December 2016 English price group 16No 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 13.030.40!%x“2595785www.din.deD
2、IN EN 14582Characterization of waste Halogen and sulfur content Oxygen combustion in closed systems and determination methods;English version EN 14582:2016,English translation of DIN EN 14582:2016-12Charakterisierung von Abfllen Halogen und Schwefelgehalt Sauerstoffverbrennung in geschlossenen Syste
3、men und Bestimmungsverfahren;Englische Fassung EN 14582:2016,Englische bersetzung von DIN EN 14582:2016-12Caractrisation des dchets Teneur en halognes et en soufre Combustion sous oxygne en systmes ferms et mthodes de dosage;Version anglaise EN 14582:2016,Traduction anglaise de DIN EN 14582:2016-12S
4、upersedesDIN EN 14582:200706www.beuth.deDocument comprises 39 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN 14582:2016-12 2 A comma is used as the decimal marker. National foreword This document (EN 14582:2016) h
5、as been prepared by Technical Committee CEN/TC 292 “Characterization of waste” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-02-02 UA Chemische und phy
6、sikalische Verfahren. Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. In addition to the legal units of measurement, this standard also uses the unit “atm” in Subclause 7.1.8. It should, however, be noted that the Gesetz ber Einheit
7、en im Messwesen (German Law on units in metrology) prohibits the use of this unit for official and commercial purposes in Germany. The indication of this unit solely serves to facilitate the communication with those countries where this unit is used (import-export business). Conversion: 1 atm = 101
8、325 Pa = 0,101 325 MPa The DIN Standards corresponding to the International Standards referred to in this document are as follows, whereby EN ISO Standards are only listed below if these have not been published as DIN EN ISO Standards with the same number: EN ISO 3696 DIN ISO 3696 ISO 9297 DIN 38405
9、-1 ISO 10304-1 DIN EN ISO 10304-1 ISO 10304-3 DIN EN ISO 10304-3 ISO 10359-1 DIN 38405-4 Amendments This standard differs from DIN EN 14582:2007-06 as follows: a) the choice of absorption solutions to be used has been extended; b) information on recovery yields obtained for control mixtures with dif
10、ferent absorption solutions and analytical techniques has been included; c) the standard has been editorially revised. Previous editions DIN EN 14582: 2007-06 DIN EN 14582:2016-12 3 National Annex NA (informative) Bibliography DIN 38405-1, German standard methods for the examination of water, waste
11、water and sludge Anions (group D) Part 1: Determination of chloride ions (D 1) DIN 38405-4, German standard methods for the examination of water, waste water and sludge Anions (group D) Part 4: Determination of fluoride (D 4) DIN EN ISO 10304-1, Water quality Determination of dissolved anions by liq
12、uid chromatography of ions Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate DIN EN ISO 10304-3, Water quality Determination of dissolved anions by liquid chromatography of ions Part 3: Determination of chromate, iodide, sulfite, thiocyanate and thiosulfat
13、e DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN 14582:2016-12 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 14582 August 2016 ICS 13.030.40 Supersedes EN 14582:2007English Version Characterization of waste - Halogen
14、and sulfur content - Oxygen combustion in closed systems and determination methods Caractrisation des dchets - Teneur en halognes et en soufre - Combustion sous oxygne en systmes ferms et mthodes de dosage Charakterisierung von Abfllen - Halogen- und Schwefelgehalt - Sauerstoffverbrennung in geschlo
15、ssenen Systemen und BestimmungsmethodenThis European Standard was approved by CEN on 17 June 2016. 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-t
16、o-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 transla
17、tion 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,
18、 Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION C
19、OMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14582:2016 EEN 14582:2016 (E) 2 Contents Page Europe
20、an foreword . 4 Introduction 5 1 Scope 6 2 Normative references 6 3 Terms and definitions . 6 4 Principle . 6 5 Interferences 7 6 Hazards . 7 7 Reagents and control mixtures 7 7.1 Reagents . 7 7.2 Control mixtures 7 8 Sample conservation and pretreatment of test portion . 8 9 Equipment . 9 10 Proced
21、ure. 9 10.1 General 9 10.2 Choice of the absorption solution 10 10.3 Preparation of the bomb . 11 10.4 Combustion 11 10.5 Collection of the halides and sulphate 12 10.6 Cleaning procedure . 12 11 Recommended methods of determination . 13 12 Control measurements . 13 13 Evaluation . 13 14 Test report
22、 14 Annex A (informative) Performance characteristics . 15 Annex B (informative) Oxygen flask combustion by Schoeniger . 18 B.1 General . 18 B.2 Principle 18 B.3 Interferences and hazards 18 B.4 Reagents and control mixtures . 18 B.5 Equipment 18 B.6 Safety precautions . 19 B.7 Procedure 19 B.7.1 Ge
23、neral . 19 B.7.2 Choice of the absorption solution 19 DIN EN 14582:2016-12 EN 14582:2016 (E) 3 B.7.3 Sample preparation . 20 B.7.4 Combustion . 20 B.8 Determination methods; control measurements; data evaluation and test report . 20 B.9 Performance characteristics 21 Annex C (informative) Recovery y
24、ields obtained for control mixtures with different absorption solutions and analytical techniques . 24 Annex D (informative) Examples of possible control substances 27 Annex E (informative) Additional results of inter-laboratory tests 29 Annex F (informative) Summary of general requirements and reco
25、mmendations 31 Annex G (informative) Additional validation data 32 G.1 General . 32 G.2 Samples 32 G.3 Homogeneity and stability 33 DIN EN 14582:2016-12 Bibliography . 35 EN 14582:2016 (E) 4 European foreword This document (EN 14582:2016) has been prepared by Technical Committee CEN/TC 292 “Characte
26、rization of waste”, the secretariat of which is held by NEN. 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 February 2017, and conflicting national standards shall be withdrawn at the latest by F
27、ebruary 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 14582:2007. According to the CEN-CENELEC Internal Regulatio
28、ns, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
29、 Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 14582:2016-12 EN 14582:2016 (E) 5 Introduction Sulfur and halogens (fluorine, chlorine, bromine and iodine) may be found in mat
30、erials in various forms. During the combustion of these materials, corrosive and harmful compounds may be released. The determination of sulfur and halogens by oxygen combustion may be used to assess the suitability of waste for incineration. The determination of the resultant halides and sulphate c
31、an be achieved by many different techniques, e.g. using atomic emission spectrometry, titrimetry or ion chromatography. Validation data of these different techniques are given in Annex A (informative). Another method, oxygen flask combustion by Schoeniger, did not pass the method validation due to l
32、ack of participants. This method is described in Annex B (informative). Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material irrespective of the parameter to be determined. Waste and sludge samples may contain hazardous (e.g. toxic, reactive, fl
33、ammable, infectious) substances, which can be liable to biological and/or chemical reaction. Consequently these samples should be handled with special care. Gases which may be produced by microbiological or chemical activity are potentially flammable and will pressurize sealed containers. Bursting b
34、ottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. DIN EN 14582:2016-12 EN 14582:2016 (E) 6 1 Scope This standard specifies a combustion method for the determination of halogen and s
35、ulfur contents in materials by combustion in a closed system containing oxygen (calorimetric bomb), and the subsequent analysis of the combustion product using different analytical techniques. This method is applicable to solid, pasty and liquid samples containing more than 0,025 g/kg of halogen and
36、/or 0,025 g/kg of sulfur content. The limit of detection depends on the element, the matrix and the determination technique used. Insoluble halides and sulphate present in the sample or produced during the combustion step are not completely determined by these methods. 2 Normative references The fol
37、lowing documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 14346, Char
38、acterization of waste - Calculation of dry matter by determination of dry residue or water content EN 15002, Characterization of waste - Preparation of test portions from the laboratory sample EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and de
39、finitions For the purposes of this document, the following terms and definitions apply. NOTE Be aware that the above definitions are valid for this empirical EN only and do not comply with scientific definitions of sulfur and halogen content. 3.1 sulfur content sum of sulfur contained as organic and
40、 inorganic compounds that can be converted to sulphate by combustion and then absorbed or dissolved in an aqueous solution 3.2 halogen content sum of halogens contained as organic and inorganic compounds that can be converted to halides (fluoride, chloride, bromide, iodide) by combustion and then ab
41、sorbed or dissolved in an aqueous solution 4 Principle The sample is oxidized by combustion in a closed system (a bomb containing oxygen under pressure). Halogenated and sulfur containing compounds are converted to fluoride, chloride, bromide, iodide and sulphate, which are absorbed and/or dissolved
42、 in an absorption solution. Several methods may be used for the determination of halides and sulphate concentrations in the absorption solution. The method may be used for samples that burn with difficulty, which involves the use of a combustion enhancer. DIN EN 14582:2016-12 EN 14582:2016 (E) 7 5 I
43、nterferences There are no interferences in the combustion step described in this standard but interferences may occur during the subsequent determination of sulphate and halides (see corresponding standards). Insoluble halides and sulphate present in the sample or produced during the combustion step
44、 are not completely determined by these methods. The choice of absorption solutions may introduce interferences depending on the analytical technique used. 6 Hazards Hydrogen peroxide is very caustic; potassium and sodium hydroxide are corrosive and hydrazine hydrate is harmful, toxic and carcinogen
45、ic. Thus the operator shall wear goggles and gloves and shall work under a fume hood when handling this reagent. As this method uses a gas (oxygen) at a high temperature and a high pressure, precautions shall be taken by the operator. 7 Reagents and control mixtures 7.1 Reagents 7.1.1 General All re
46、agents shall be at least of analytical grade and suitable for their specific purposes. Particularly, they shall be free of sulfur and halogens. The reagents correspond to the chemical compounds used for the preparation of the absorption solutions; they are not all necessary depending on the choice o
47、f the solutions made by the laboratory for the determination of halides and sulfur (see Annex C). 7.1.2 Water of grade 1 as specified in EN ISO 3696. 7.1.3 Sodium hydroxide (NaOH) or potassium hydroxide (KOH) pellets. 7.1.4 Sodium bicarbonate NaHCO3and sodium carbonate Na2CO3. 7.1.5 Hydrogen peroxid
48、e (about 30 %) (H2O2). 7.1.6 Hydrazine hydrate (H2N-NH2H2O), reagent grade about 50 % 60 %. 7.1.7 Ascorbic acid (C6H8O6). 7.1.8 Oxygen, free of combustible material, available at a pressure of 3 MPa to 4 MPa (30 atm to 40 atm) (e.g. medical grade). 7.1.9 Combustion enhancer (e.g. paraffin). 7.1.10 A
49、luminium oxide, Al2O3, neutral, particle size 200 m, pre-heated to 600 C. 7.1.11 Gelatine or aceto-butyrate capsules. 7.2 Control mixtures Select a certified reference material (CRM) or create an appropriate control mixture by choosing the control substances in combination so all elements that shall be determined in the samples are DIN EN 14582:2016-12 EN 14582:2016 (E) 8 represented. The amount of halogen and sulfur contents
