1、BRITISH STANDARDBS EN 14582:2007Characterization of waste Halogen and sulfur content Oxygen combustion in closed systems and determination methodsThe European Standard EN 14582:2007 has the status of a British StandardICS 13.030.40g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g
2、40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS EN 14582:2007This British Standard was published under the authority of the
3、 Standards Policy and Strategy Committee on 30 April 2007 BSI 2007ISBN 978 0 580 50585 0National forewordThis British Standard was published by BSI. It is the UK implementation of EN 14582:2007.The UK participation in its preparation was entrusted by Technical Committee B/508, Waste management, to S
4、ubcommittee B/508/3, Characterization of waste.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with
5、a British Standard cannot confer immunity from legal obligations. Amendments issued since publicationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14582March 2007ICS 13.030.40English
6、VersionCharacterization of waste - Halogen and sulfur content - Oxygencombustion in closed systems and determination methodsCaractrisation des dchets - Teneur en halognes et ensoufre - Combustion sous oxygne en systme ferm etmthodes de dosageCharakterisierung von Abfllen - Halogen- undSchwefelgehalt
7、 - Sauerstoffverbrennung in geschlossenenSystemen und BestimmungsmethodenThis European Standard was approved by CEN on 13 January 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national st
8、andard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other
9、 language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Fin
10、land,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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMIT
11、EE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14582:2007: ELicensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582
12、:2007 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle5 5 Interferences 6 6 Hazards .6 7 Reagents and control mixtures6 8 Sample conservation and pre-treatment of test portion .7 9 Equipment 8 10 Procedure .8 11 Recommended metho
13、ds of determination10 12 Control measurements11 13 Evaluation.12 14 Performance characteristics 13 15 Test report 15 Annex A (informative) Oxygen flask combustion by Schoeniger 16 A.1 Scope 16 A.2 Terms and definitions .16 A.3 Principle16 A.4 Interferences and hazards 16 A.5 Reagents and control mix
14、tures16 A.6 Equipment 17 A.7 Safety precautions.17 A.8 Procedure .17 A.9 Determination methods; control measurements; data evaluation and test report.19 A.10 Performance characteristics 19 Annex B (informative) Examples of possible control substances .22 Annex C (informative) Additional results of i
15、nter-laboratory tests 23 Annex D (informative) Summary of general requirements and recommendations 25 Annex E (informative) Additional validation data.26 E.1 General26 E.2 Samples 26 E.3 Homogeneity and stability 27 Bibliography 29 Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Unc
16、ontrolled Copy, (c) BSIEN 14582:2007 (E) 3 Foreword This document (EN 14582:2006) has been prepared by Technical Committee CEN/TC 292 “Characterization 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 o
17、f an identical text or by endorsement, at the latest by September 2007, and conflicting national standards shall be withdrawn at the latest by September 2007. Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material irrespective of the parameter to
18、be determined. Waste and sludge samples may contain hazardous (e. g. toxic, reactive, flammable, 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 chemi
19、cal activity are potentially flammable and will pressurise sealed bottles. Bursting bottles 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. According to the CEN/CENELEC Internal Regulati
20、ons, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherla
21、nds, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582:2007 (E) 4 Introduction Sulphur and halogens (fluorine, chlorine, bromine and iodine) may be
22、found in materials in various forms. During the combustion of these materials, corrosive and harmful compounds may be released. The determination of sulphur and halogens by oxygen combustion may be used to assess the suitability of waste for incineration. The determination of the resultant halides a
23、nd sulphate can be achieved by many different techniques, e. g. using atomic emission spectrometry, titrimetry or ion chromatography. Another method, oxygen flask combustion by Schoeniger, did not pass the method validation due to lack of participants. This method is described in Annex A (informativ
24、e). Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582:2007 (E) 5 1 Scope This standard specifies a combustion method for the determination of halogen and sulphur contents in materials by combustion in a closed system containing oxygen (calorimetric b
25、omb), 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/or 0,025 g/kg of sulphur content. The limit of detection depends on the element, the matrix a
26、nd the determination technique used. Insoluble halides and sulphate present in the original sample or produced during the combustion step are not completely determined by these methods. 2 Normative references The following referenced documents are indispensable for the application of this document.
27、For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 14346, Characterization of waste Calculation of dry matter by determination of dry residue or water content EN 15002, Characterization of
28、 waste Preparation of test portions from the laboratory sample EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 sulphur content sum of sulphur cont
29、ained as organic and 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 co
30、mbustion and then absorbed or dissolved in an aqueous solution NOTE Be aware that the above definitions are valid for this empirical EN only and do not comply with scientific definitions of sulphur and halogen content. 4 Principle The sample is oxidized by combustion in a closed system (a bomb conta
31、ining oxygen under pressure). Halogenated and sulphur containing compounds are converted to fluoride, chloride, bromide, iodide and sulphate, which are absorbed and/or dissolved in an absorption solution. Several methods may be used for the determination of halides and sulphate concentrations in the
32、 absorption solution. In general this method is applicable for concentrations over 0,025 g/kg depending on the element, matrix and the determination technique. It may be used for aqueous samples or samples that burn with difficulty, which involves the use of a combustion enhancer. Licensed Copy: Wan
33、g Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582:2007 (E) 6 5 Interferences 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 standar
34、ds). Insoluble halides and sulphate present in the original sample or produced during the combustion step are not completely determined by these methods. 6 Hazards Hydrogen peroxide is very caustic, thus the operator shall wear goggles and gloves and shall work under a fume hood when handling this r
35、eagent. 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 reagents shall be at least of analytical grade and suitable for their specific purposes. Particularly, they
36、 shall be free of sulphur and halogens. 7.1.2 Water of grade 1 as specified in EN ISO 3696. 7.1.3 Hydrogen peroxide (about 30 %) (H2O2). 7.1.4 Absorption solution 1, for the determination of fluorine, chlorine, bromine and sulphur, the nature and concentration of which may depend on the end-determin
37、ation technique and on the expected content of halogens and sulphur. For example: water (7.1.2.); or 0,3 mol/l potassium or sodium hydroxide solution: dissolve 16,8 g of KOH or 12,0 g of NaOH pellets in water (7.1.2.) and dilute to 1 l; or carbonate/bicarbonate solution: dissolve 2,52 g sodium bicar
38、bonate NaHCO3and 2,54 g sodium carbonate Na2CO3in water (7.1.2.) and dilute to 1 l. 7.1.5 Absorption solution 2 for the determination of iodine Ascorbic acid-solution, (C6H8O3), w = 1 %. 7.1.6 Oxygen, free of combustible material, available at a pressure of 3 MPa to 4 MPa (30 atm to 40 atm) (e. g. m
39、edical grade). 7.1.7 Combustion enhancer (e. g. paraffin). 7.1.8 Aluminium oxide, Al2O3, neutral, particle size 200 m, pre-heated to 600 C. 7.1.9 Gelatine or aceto-butyrate capsules. Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582:2007 (E) 7 7.2 Co
40、ntrol mixtures Table B.1 lists examples of control substances that give complete (90 % to 110 %) recoveries of halogen and sulphur. To create an appropriate control mixture, choose the control substances in combination so all elements that shall be determined in the samples are represented. The amou
41、nt 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. If necessary, dilute with cellulose or aluminium oxide to get a suitable element content. The mixture of the cont
42、rol substances and the cellulose or aluminium oxide needs to be homogenized, e. g. using a pebble mill. NOTE Combined combustion of iodine and sulphur may interact to improve the reduction of iodine to iodide and the oxidation of sulphur to sulphate. If the actual samples only contain one of the ele
43、ments a combined control mixture may give false assurance of the method capacity. An example of a mixture of control substances for the determination of fluorine, chlorine, and sulphur is: Mix 0,50 g 4-fluoro-benzoic acid; 2,0 g 4-chloro-benzoic acid; 2,0 g sulfanilic acid and 55,5 g cellulose. An e
44、xample of a mixture of control substances for the determination of bromine and iodine is: Mix 0,25 g 4-bromo-benzoic acid; 0,25 g 4-iodo-benzoic acid and 59,5 g cellulose. Homogenize the mixtures, e. g. in a pebble mill. This first mixture of fluorine, chlorine, and sulphur contains 1,130 g/kg fluor
45、ine; 7,547 g/kg chlorine and 6,170 g/kg sulphur. The second mixture of iodine and bromine contains 1,656 g/kg bromine and 2,132 g/kg iodine. 8 Sample conservation and pre-treatment of test portion Biological active laboratory samples should be stored at 4 C and the analyses of halogen and sulphur sh
46、ould be carried out within seven days after sampling. If this is not possible, the samples should be further preserved by e. g. freezing, if possible, to minimize biodegradation and loss of volatile halogenated and sulphur compounds. The test sample is prepared according to EN 15002. For solid mater
47、ials the particle size should be less than 200 m. During preparation of the test sample the use of halogenated polymers, e. g. PVC gloves, should be avoided. Drying the laboratory sample may be carried out for homogenisation purposes if the sample, according to the accuracy of the method, contains o
48、nly negligible amounts of halogen and sulphur compounds volatile at the temperature intended for the drying process. Dry matter is determined according to EN 14346 on a separate sub sample (the result will be used for calculation). NOTE Heterogeneous moist or paste like samples may be mixed with alu
49、minium oxide (7.1.8) until granular material is obtained and then reduced to a granular powder, preferably with a particle size less than 200 m. In this case, the ratio of aluminium oxide to sample should be incorporated into the calculation of the halogen and sulphur content and combustion enhancer should be added if necessary. Licensed Copy: Wang Bin, na, Tue Aug 21 00:37:08 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14582:2007 (E) 8 9 Equipment 9.1 Calorimetric bomb, with a capacity of not less than 200 ml and equipped with a purging system This bomb
