1、BRITISH STANDARDBS EN 14346:2006Characterization of waste Calculation of dry matter by determination of dry residue or water contentThe European Standard EN 14346:2006 has the status of a British StandardICS 13.030.01g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54
2、g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14346:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2007 BSI 2007ISBN 978 0 580 50298 9National forew
3、ordThis British Standard was published by BSI. It is the UK implementation of EN 14346:2006.The UK participation in its preparation was entrusted by Technical Committee B/508, Waste management, to Subcommittee B/508/3, Characterization of waste.A list of organizations represented on B/508/3 can be o
4、btained 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 a British Standard cannot confer immunity from legal obligations. Amendments issued since publicationAmd. No.
5、 Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14346December 2006ICS 13.030.01English VersionCharacterization of waste - Calculation of dry matter bydetermination of dry residue or water contentCaractrisation des dchets - Calcul de la teneur enmatire sche par dtermination du rsidu s
6、ec ou de lateneur en eauCharakterisierung von Abfllen - Berechnung derTrockenmasse durch Bestimmung des Trockenrckstandesoder des WassergehaltesThis European Standard was approved by CEN on 25 November 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the
7、 conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in thr
8、ee official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austr
9、ia, Belgium, 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 STAN
10、DARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14346:2006: EEN 14346:2006 (E) 2 Contents Page Forewor
11、d3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle5 5 Sample preparation and storage6 6 Method A Drying at 105 C .6 7 Method B Direct Karl-Fischer-titration (volumetric/coulometric detection)8 8 Performance characteristics 10 9 Calculation of dry matter 11 1
12、0 Test report 12 Annex A (informative) Additional validation data 13 Annex B (informative) Azeotropic distillation with toluene 16 Annex C (informative) Summary of general requirements and recommendations20 EN 14346:2006 (E) 3 Foreword This document (EN 14346:2006) has been prepared by Technical Com
13、mittee 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 of an identical text or by endorsement, at the latest by June 2007, and conflicting national standards shall be withd
14、rawn at the latest by June 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 be determined. Waste and sludge samples may contain hazardous (e.g. toxic, reactive, flammable, infectious) substances, which
15、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 pressurise sealed bottles. Bursting bottles are likely to result in hazardous s
16、hrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Be
17、lgium, 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. EN 14346:2006 (E) 4 Introducti
18、on In case of waste analysis water is usually not considered as part of the sample and results are generally related to dry matter, which can be calculated from the water content or the dry residue. For this purpose two methods are described in this European Standard. The choice of the method depend
19、s on the type of sample and its content of volatile substances excluding water. As a result of the validation study the determination of water content by azeotropic distillation has been replaced by Karl-Fischer-titration. Nevertheless the distillation may be useful in certain cases. This method is
20、described in Annex B (informative). EN 14346:2006 (E) 5 1 Scope This European Standard specifies methods for the calculation of the dry matter of samples for which the results of performed analysis are to be calculated to the dry matter basis. Depending on the nature of the sample, the calculation i
21、s based on a determination of the dry residue (Method A) or a determination of the water content (Method B). It applies to samples containing more than 1 % (m/m) of dry residue or more than 1 % (m/m) of water. 2 Normative references The following referenced documents are indispensable for the applic
22、ation 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 15002, Characterization of waste Preparation of test portions from the laboratory sample 3 Terms and definitions
23、For the purposes of this document, the following terms and definitions apply. NOTE These definitions only apply to waste. In standards dealing with other matrices other terms and definitions exist for technical reasons. 3.1 dry residue wdrremaining mass fraction of a sample after a drying process at
24、 105 C as specified in this European Standard 3.2 water content wwmass fraction of water in a sample determined by Karl-Fischer-titration as specified in this European Standard 3.3 dry matter wdmmass fraction of a sample excluding water expressed as a percentage by mass calculated by determination o
25、f dry residue or water content according to this European Standard 4 Principle 4.1 General Depending on the nature of the sample (liquid, solid or multiphase) either the water content or the dry residue is to be determined. The results from the determination of water content or dry residue are used
26、to calculate the dry matter. In case of multiphase samples these samples shall be homogenized. If homogenization is not possible, a phase separation according to EN 15002 shall be applicable and the phases are analysed separately. EN 14346:2006 (E) 6 4.2 Principle of Method A Drying at 105 C (dry re
27、sidue) The sample is dried to a constant mass in an oven at (105 3) C. This method applies to solid samples and samples which become solid during the drying process. Solid samples containing amounts of volatiles which are expected to affect the results shall be analysed by Method B. 4.3 Principle of
28、 Method B Karl-Fischer-titration (water content) The water content of a sample is determined by direct Karl-Fischer-titration and either volumetric or coulometric detection. Liquid samples are directly added to the cell, while solid samples are extracted by use of methanol. The method usually applie
29、s to liquid samples and homogenised multiphase samples. It could also be used for solid samples in case the “water content” is of interest and in case volatiles are expected to interfere with the determination according to Method A. 5 Sample preparation and storage Specification of sample preparatio
30、n is not included in this European Standard. As the dry matter content is calculated in order to convert obtained results for a sample to the dry matter basis, the determination of dry residue or water content shall be carried out on the identical portions of the same test sample. By that the sample
31、 preparation is as specified in the actual analysis standard. Storage of samples may cause changes as e.g. uptake or liberation of water, carbon dioxide and other volatiles. If it is not possible to carry out the determination of dry residue or water content parallel to the analyses, samples shall b
32、e stored in air-tight containers. Biologically active samples shall be stored at about 4 C and analysed within 3 days. 6 Method A Drying at 105 C 6.1 General When carrying out one or more analysis on a sample, the dry matter shall be determined on an identical test portion in parallel in order to re
33、calculate the results of the other analysis to the dry matter basis. 6.2 Interferences The samples can change during the drying process, e.g. by absorption of carbon dioxide in the case of alkaline samples, or of oxygen by reducing substances. Volatile compounds evaporating at 105 C are measured as
34、water using this procedure. NOTE For alkaline samples or samples susceptible to oxidation the drying could be carried out in a nitrogen atmosphere. 6.3 Hazards Flammable or explosive gases may be released in the drying process. 6.4 Equipment 6.4.1 Drying system thermostatically controlled and capabl
35、e of maintaining a temperature of (105 3) C; e.g. drying oven, infrared system, halogen lamp system. 6.4.2 Desiccator with an active drying agent such as silica gel. 6.4.3 Analytical balance with an accuracy of 1 mg or better. EN 14346:2006 (E) 7 6.4.4 Evaporating dish or crucible. Temperature toler
36、ant laboratory vessel withstanding 105 C. Suitable materials are metallic or ceramic. NOTE 1 If the sample is to be ashed following this procedure, it should be ensured that the material will withstand the elevated temperatures. NOTE 2 The material of the evaporating dish or crucible should be compa
37、tible with the nature of the waste to avoid interferences upon weighing due to possible oxidations. 6.5 Procedure Place an evaporating dish or crucible (6.4.4) in the drying system (6.4.1) set at (105 3) C for a minimum of 30 min. After cooling in the desiccator (6.4.2) to ambient temperature, weigh
38、 the basin to the nearest 1 mg (ma). Depending on the expected dry residue, weigh into the evaporating dish or crucible a suitable amount of material so that the residue obtained has a weight of at least 0,5 g. Weigh the loaded basin to the nearest 1 mg (mb). Place the evaporating dish or crucible (
39、6.4.4) containing the sample in the drying system (6.4.1) set at (105 3) C until the residue appears dry, typically overnight. NOTE 1 For some samples e.g. sludge, there is a risk of formation of a cake surface, which hinders an even drying. To avoid this, a glass rod can be weighed along with the d
40、ish. If cake formation occurs during drying, the glass rod is used to stir the sample, to break up the cake. This should be repeated as necessary. The rod should be reweighed afterwards. After cooling in the desiccator (6.4.2) weigh the evaporating dish or crucible and contents for the first time, (
41、mc). The dry residue (mc ma) shall be regarded as constant if the mass obtained after a further one hour of drying does not differ by more than 0,5 % of the previous value or 2 mg whichever is the greater. Otherwise repeat the drying process. NOTE 2 In case of weight inconstancy after three cycles t
42、he drying process may be stopped (after at least 12 h). The result of the last weighing should be recorded in the test report. In case of infrared or halogen lamp drying systems the corresponding manufacturers instructions apply. The technique of choice has to be noted in the test report. Other tech
43、niques than oven drying (infrared/halogen) are allowed, provided they are proven to give comparable results. 6.6 Calculation of results The dry residue, expressed as mass fraction in per cent or in grams per kilogram, is calculated according to Equation (1): ()()fmmmmw =abacdr(1) where wdris the dry
44、 residue of the sample, expressed as mass fraction in per cent % or in grams per kilogram g/kg; mais the mass of the empty dish or crucible, expressed in grams g; EN 14346:2006 (E) 8 mbis the mass of the dish or crucible containing the sample, expressed in grams g; mcis the mass of the dish or cruci
45、ble containing the dried sample, expressed in grams g; f is the conversion factor f = 100 for expression of results as mass fraction in per cent % and f = 1 000 for expression of results in grams per kilogram g/kg. The analysis is performed at least in duplicate; the mean value is calculated and rep
46、orted. 7 Method B Direct Karl-Fischer-titration (volumetric/coulometric detection) 7.1 Interferences Substances like peroxides, oxides, hydroxides, ammonia, carbonates, hydrogen carbonates, disulfites, nitrite, sulfite, thiosulfate, hydrazine and derivatives, iron (II), copper (I), tin (II), silanol
47、es, arsenite, arsenate, selenite, tellurite, phenols, boric compounds, aldehydes, acetone and other reactive ketones may interfere. Especially all reductive or oxidative reagents are potentially interfering. In case of concern about interferences results can be verified by azeotropic distillation (A
48、nnex B). Most of the interferences are reduced in case of extraction with methanol before analysis. 7.2 Reagents All reagents used shall be at least analytical grade and suitable for their specific purposes. Hygroscopic substances shall be stored in a desiccator. 7.2.1 Karl-Fischer reagent as recomm
49、ended by provider of KF-system. 7.2.2 Methanol. The methanol used shall not contain more than a mass fraction of 0,005 % water. 7.2.3 Toluene if necessary to solve a sample. 7.3 Equipment Usual laboratory glassware and the following equipment shall be used. 7.3.1 Apparatus suitable for Karl-Fischer-titration. 7.3.2 Shaking apparatus. 7.3.3 Weighing pipette. 7.3.4 Conical flasks of 250 ml with ground glass neck and stopper. 7.4 Procedure 7.4.1 Determination of the equivalence factor Fill a clean and dry titration vessel (7.3
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