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1、BRITISH STANDARD BS EN 13657:2002 Characterization of waste Digestion for subsequent determination of aqua regia soluble portion of elements The European Standard EN 13657:2002 has the status of a British Standard ICS 13.030.40 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00
2、:00 2006, Uncontrolled Copy, (c) BSI BS EN 13657:2002 This British Standard, having been prepared under the direction of the Building and Civil Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 22 October 2002 BSI 22
3、 October 2002 ISBN 0 580 40624 5 National foreword This British Standard is the official English language version of EN 13657:2002. The UK participation in its preparation was entrusted by Technical Committee B/508, Waste management, to Subcommittee B/508/3, Characterization of waste, which has the
4、responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section enti
5、tled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Complianc
6、e with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related int
7、ernational and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 26, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document wa
8、s last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13657 October 2002 ICS 13.030.40 English version Characterization o
9、f waste - Digestion for subsequent determination of aqua regia soluble portion of elements Caractrisation des dchets - Digestion en vue de la dtermination ultrieure de la part des lments solubles dans leau rgale contenus dans les dchets Charakterisierung von Abfllen - Aufschluss zur anschlieenden Be
10、stimmung des in Knigswasser lslichen Anteils an Elementen in Abfllen This European Standard was approved by CEN on 19 August 2002. 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 stand
11、ard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other lang
12、uage made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Ic
13、eland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2002 CENAll rights of ex
14、ploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13657:2002 E Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 2 Contents page Foreword3 Introduction.4 1Scope5 2Normative refer
15、ences5 3Terms and definitions.5 4Safety remarks.6 5Sample6 5.1Sample pre-treatment .6 5.2Mass of test portion.7 6Equipment7 6.1Closed vessel system .7 6.1.1Microwave unit7 6.1.2Digestion vessels7 6.2Semi-open vessel system .8 6.2.1Microwave unit8 6.2.2Digestion vessels8 6.3Apparatus for thermal heat
16、ing digestion .8 6.3.1Reaction vessels.8 6.3.2Reflux condenser8 6.3.3Absorption vessel8 6.3.4Roughened glass beards8 6.3.5Temperature-controlled heating apparatus 8 6.4General equipment8 7Reagents.9 8Interferences and sources of error9 8.1General informations.9 8.2Closed vessel system .9 8.3Semi-ope
17、n vessel system for microwave or thermal heating digestion10 9Procedure.10 9.1Blank test.10 9.2Procedure for microwave assisted digestion in closed vessels10 9.3Procedure for microwave assisted digestion in semi-open vessels11 9.3.1Amount of samples.11 9.3.2Digestion.11 9.3.3Preparation of the solut
18、ion for analysis 11 9.4Procedure for thermal heating digestion in reflux systems.11 9.4.1Amount of samples.11 9.4.2Digestion.12 9.4.3Preparation of the solution for analysis 12 10Test report12 Annex A (normative) Calibration of the power adjustment .14 Annex B (informative) Validation15 B.1Inter-lab
19、oratory study15 B.2Robustness study.23 Bibliography26 Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 3 Foreword This document EN 13657:2002 has been prepared by Technical Committee CEN/TC 292 “Characterization of waste“, t
20、he 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 April 2003, and conflicting national standards shall be withdrawn at the latest by April 2003. In this Europ
21、ean Standard the annex A is normative and the annexe B is informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany
22、, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 4 Introduction The aim of this European
23、 Standard is to describe suitable methods for the extraction of elements in waste, soluble by digestion with aqua regia, i. e. aqua regia soluble elements. For those types of waste, where the sample material by the described digestion with aqua regia are not brought totally in solution, the obtained
24、 results will not be the total amount of the elements in the waste. The obtained results of aqua regia soluble elements cannot be regarded as available for leaching, as the digestion with aqua regia is too vigorous to represent natural processes. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 2
25、9 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 5 1 Scope This European Standard specifies methods of digestion with aqua regia. Solutions produced by the methods are suitable for analysis e.g. by atomic absorption spectrometry (FLAAS, HGAAS, CVAAS, GFAAS), inductively couple
26、d plasma emission spectrometry (ICP-OES) and inductive coupled plasma mass spectrometry (ICP-MS). The digestion with aqua regia will not necessarily release all elements completely. However for most environmental application and waste characterization the results fit for the purpose. The method is a
27、pplicable to the digestion of waste for example for the following elements: Al, Sb, As, B, Ba, Be, Ca, Cd, Cr, Co, Cu, Fe, Pb, Mg, Mn, Hg, Mo, Ni, P, K, Se, Ag, S, Na, Sr, Sn, Te, Ti, Tl, V, Zn. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from
28、 other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendme
29、nt or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987). 3 Terms and definitions For the purposes of this European Standard, the fol
30、lowing terms and definitions apply. 3.1 aqua regia digestion solution obtained by mixing 1 volume of nitric acid (65 % m/m to 70 % m/m) and 3 volumes of hydrochloric acid (35 % m/m to 37 % m/m) 3.2 digestion mineralization of the organic matter of a sample and dissolution of its mineral part, more o
31、r less completely, when reacted with a reagent mixture 3.3 sample portion of material selected from a larger quantity of material ENV 12506:2001 3.4 laboratory sample sample or subsample(s) sent to or received by the laboratory ENV 12506:2001 3.5 test sample; analytical sample sample, prepared from
32、the laboratory sample, from which test portions are removed for testing or analysis ENV 12506:2001 Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 6 3.6 test portion; analytical portion quantity of material of proper size f
33、or measurement of the concentration or other properties of interest, removed from the test sample ENV 12506:2001 NOTE 1 The test portion may be taken from the laboratory sample directly if no preparation of sample is required (e. g. with liquids), but usually it is taken from the prepared test sampl
34、e. NOTE 2 A unit or increment of proper homogeneity, size and fineness, needing no further preparation, may be a test portion. 3.7 dry residue dry matter expressed as a percentage by mass after drying at 105 C 5 C to the constancy of weight 3.8 digestion vessel special flask where the test portion a
35、nd the acid mixture are filled in and the digestion is performed 3.9 microwave unit whole microwave digestion system (oven and associated equipment) 3.10 microwave unit cavity the inner part of the microwave unit in which the digestion vessel is located and the microwave digestion is performed 3.11
36、focused microwave unit microwave unit in which a precise control of the electric field is made by using a wave guide NOTEMicrowaves are focused at the bottom part of the digestion vessel. 4 Safety remarks All this work has to be performed by skilled persons. The reagents used within this EN are stro
37、ngly corrosive and partly very toxic. Safety precautions are absolutely necessary due to strong corrosive reagents, high temperature and high pressure. All procedures have to be performed in a hood or in closed force-ventilated equipment. By the use of strong oxidising reagents the formation of expl
38、osive organic intermediates is possible especially when dealing with samples with a high organic content. Do not open pressurised vessels before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products. Samples and solutions have to be disposed of according to regula
39、tions. 5 Sample 5.1 Sample pre-treatment The test portion should be transferred into the vessel as it is without any pre-treatment if possible.This is applicable only if the test portion is representative for the laboratory sample and the effectiveness of the digestion is proven. Licensed Copy: shef
40、fieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 7 If these conditions are not met a pre-treatment of the laboratory sample is necessary. This procedure shall not change the concentration of the elements of interest. Pre-treatment should inclu
41、de drying or grain size reduction below a particle size of 250 m for solid waste or homogenizing by use of a high speed mixer or sonification for liquid samples. The mass of laboratory samples shall be sufficient for the multiple digestion procedures and determination of the dry residue. 5.2 Mass of
42、 test portion The mass of test portion for a single digestion has to be selected in a way, that: it is representative for the laboratory sample; it complies with the specifications of manufacturer of the digestion unit. NOTEIf the representative test portion exceeds the manufacturers specifications
43、the test portion should be devided into smaller quantities and digested seperately. The individual digests should be combined prior to analysis. For representativity reason mass above 200 mg is to be preferred. Unless recommended by the manufacturer the amount of organic carbon shall not exceed 100
44、mg because of safety reasons in the case of closed digestion vessel. 6 Equipment 6.1 Closed vessel system 6.1.1 Microwave unit The microwave unit shall provide programmable power which can be programmed to within 10 W of the required power. Typical units provide a nominal 600 W to 1 200 W of power.
45、If necessary (referring to manufactures specifications) calibration of the microwave unit has to be performed (see annex A). The microwave unit has to comply to European and national regulations relevant to microwave radiation. The microwave unit cavity has to be well ventilated. It has to have an e
46、xhaust air tube which is connected to a corrosion resistant laboratory air outlet system or the instrument is provided for use in a laboratory hood. All electronics are sufficiently protected against corrosion for safe operation. All parts which could have contact with acids or their vapours have to
47、 be corrosion resistant. The microwave unit shall be designed in a way that guarantees homogeneous heating of the samples. The microwave unit cavity has to be built in a way that even in case of leakage or explosion of the vessels the safety of the operators can be guaranteed. Household instruments
48、are not suitable for laboratory use. NOTEThe microwave unit should include a temperature and/or pressure control system. 6.1.2 Digestion vessels The vessels used in the microwave unit shall be equiped with a pressure relieve valve or another technical equipment which avoids the bursting of the vesse
49、ls at suddenly occuring excess pressure. The material of the vessels has to be inert to the acids used for digestion. The digestion vessel shall withstand the pressure of at least 8 bar. If the amount of organic carbon exceeds 100 mg it has to be ensured that the digestion vessel is capable of withstanding higher pressures. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13657:2002 (E) 8 6.2 Semi-open vessel system 6
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