1、November 2012 Translation by DIN-Sprachendienst.English price group 10No 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).I
2、CS 13.030.01; 13.080.10!$N“1924392www.din.deDDIN EN 16174Sludge, treated biowaste and soil Digestion of aqua regia soluble fractions of elements;English version EN 16174:2012,English translation of DIN EN 16174:2012-11Schlamm, behandelter Bioabfall und Boden Aufschluss von mit Knigswasser lslichen A
3、nteilen von Elementen;Englische Fassung EN 16174:2012,Englische bersetzung von DIN EN 16174:2012-11Boues, bio-dchets traits et sols Digestion des fractions solubles dans leau rgale;Version anglaise EN 16174:2012,Traduction anglaise de DIN EN 16174:2012-11www.beuth.deIn case of doubt, the German-lang
4、uage original shall be considered authoritative.Document comprises 16 pages 10.12 DIN EN 16174:2012-11 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 400 “Project Committee Horizontal standards in the fields of sludge, biowast
5、e and soil” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committees NA 119-01-02 Abfall- und Bodenuntersuchung and NA 119-01-02-02 AA Chemische und physikalische Verfahren. The D
6、IN Standards corresponding to the International Standards referred to in this document are as follows: ISO 8288 DIN 38406-21 ISO 11466 DIN ISO 11466 DIN EN 16174:2012-11 3 National Annex NA (informative) Bibliography DIN 38406-21, German standard methods for the examination of water, waste water and
7、 sludge; cations (group E) Determination of nine heavy metals (Ag, Bi, Cd, Co, Cu, Ni, Pb, Tl, Zn) (E21) DIN ISO 11466, Soil quality Extraction of trace elements soluble in aqua regia DIN EN 16174:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16174 A
8、ugust 2012 ICS 13.030.01; 13.080.10 English Version Sludge, treated biowaste and soil - Digestion of aqua regia soluble fractions of elements Boues, bio-dchets traits et sols - Digestion des lments solubles dans leau rgale Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Knigswasser lsl
9、ichen Anteilen von Elementen This European Standard was approved by CEN on 24 May 2012. 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 list
10、s 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
11、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, Former Yug
12、oslav 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 COMIT EUROPE
13、N DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16174:2012: EEN 16174:2012 (E) 2 Contents Page Foreword 3Introduction .41 S
14、cope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences and sources of errors 66 Reagents .67 Apparatus .68 Procedure .88.1 General 88.2 Blank test 88.3 Method A: Thermal heating under reflux conditions .98.4 Method B: Microwave heating with temperature control at (175 5
15、) C 99 Test report . 10Annex A (informative) Repeatability and reproducibility data . 11A.1 Materials used in the interlaboratory comparison study . 11Bibliography . 12DIN EN 16174:2012-11 EN 16174:2012 (E) 3 Foreword This document (EN 16174:2012) has been prepared by Technical Committee CEN/TC 400
16、“Project Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by DIN. 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 2013, and c
17、onflicting national standards shall be withdrawn at the latest by February 2013. 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
18、document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The preparation of this document by CEN is based on a mandate by the European Commission (Mandate M/330), which assigned the development of standards on sampling and analytical
19、 methods for hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. According to the CEN/CENELEC Internal Regulations, the national standards organization
20、s 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, Latvia, Lithuania, Luxembourg, Malta,
21、Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16174:2012-11 EN 16174:2012 (E) 4 Introduction This method is intended to provide a multi-element aqua regia digestion of sludge, treated biowaste and soil prior to a
22、nalysis. It is known that the digestion of environmental samples with aqua regia will not necessarily lead to a complete element breakdown, and that the extract from a test sample may not reflect the total concentrations of the target analytes. However, for most environmental applications the result
23、 is fit for the purpose. This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see also 19 for the results of the validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge
24、 Municipal sludge Industrial sludge Sludge from electronic industry Ink waste sludge Sewage sludge Biowaste (Method A) Compost Composted sludge Soil Agricultural soilSludge amended soils WARNING Persons using this European Standard should be familiar with usual laboratory practice. The reagents used
25、 in this European Standard are strongly corrosive and partly very toxic. Safety precautions are absolutely necessary, not only due to the strong corrosive reagents, but also to high temperature and high pressure. The use of laboratory-grade microwave equipment with isolated and corrosion resistant s
26、afety devices is required. Domestic (kitchen) type microwave ovens shall not be used, as corrosion by acid vapours may compromise the function of the safety devices and prevent the microwave magnetron from shutting off when the door is open, which could result in operator exposure to microwave energ
27、y. All procedures shall be performed in a fume hood or in closed force-ventilated equipment. By the use of strong oxidising reagents, the formation of explosive organic intermediates is possible, especially when dealing with samples with a high organic content. Do not open pressurized vessels before
28、 they have cooled down. Avoid contact with the chemicals and the gaseous reaction products. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16174:2012-11 EN 16174:2012 (E) 5 1 Scope This European Standard
29、specifies two methods for digestion of sludge, treated biowaste and soil by the use of aqua regia as digestion solution. This European Standard is applicable for the following elements: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), c
30、alcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (
31、Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rubidium (Rb), rhenium (Re), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silv
32、er (Ag), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr). This European Standard may also be applicable for
33、the digestion of other elements. Digestion with aqua regia will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations may not necessarily reflect the total content in the sample. 2 Normative references The following documents, in whole or in part, are nor
34、matively 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 15936, Sludge, treated biowaste, soil and waste Determina
35、tion of total organic carbon (TOC) by dry combustion EN 16179, Sludge, treated biowaste and soil Guidance for sample pretreatment EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the following terms
36、and definitions apply. 3.1 aqua regia digestion solution obtained by mixing one volume of concentrated nitric acid and three volumes of concentrated hydrochloric acid 4 Principle A test portion is digested with aqua regia according to one of the following heating procedures: Method A: boiling under
37、reflux for 2 h, followed by filtration and adjusting the volume in a volumetric flask; Method B: microwave digestion at (175 5) C for (10 1) min in a closed vessel followed by filtration and adjusting the volume in a volumetric flask. DIN EN 16174:2012-11 EN 16174:2012 (E) 6 5 Interferences and sour
38、ces of errors Due to the volatility of some compounds care shall be taken, that the sample is not heated before the digestion and that any volatile reaction products formed during the digestion do not escape. High acid and solute concentrations in the digest may cause interferences at determination.
39、 Contamination shall be avoided. Glass containing e.g. B, Na, K, Al can contaminate samples. Ensure that all of the test portion is brought into contact with the acid mixture in the digestion vessel. Some elements of interest can be lost due to precipitation with ions present in the digest solution,
40、 e.g. low soluble chlorides, fluorides and sulfates. 6 Reagents Use only acids and reagents of recognized analytical grade to avoid high blank values for subsequent analytical measurements. Use a test blank solution throughout the procedure applying all steps with the same amount of acids, but witho
41、ut a sample. 6.1 Water, quality 2 according to EN ISO 3696 or better. 6.2 Hydrochloric acid, c(HCl) = 12 mol/l; = 1,18 kg/l. 6.3 Nitric acid, c(HNO3) = 15 mol/l, = 1,4 kg/l. 6.4 Nitric acid, c(HNO3) = 0,5 mol/l, = 1,0 kg/l. Dilute 35 ml nitric acid (6.3) to 1 l with water (6.1). 6.5 Antifoaming agen
42、t, e.g. n-dodecane (C12H26) or Octanol (C8H18O) are suitable. 7 Apparatus Usual laboratory apparatus. All glassware and plastics ware shall be adequately cleaned and stored in order to avoid any contamination. Depending on the concentration of the element of interest, a particular caution to the cle
43、aning of the vessels shall be taken. 7.1 Apparatus used for Method A 7.1.1 Digestion vessel, see Figure 1, temperature- and pressure-resistant and capable of containing the mixture of sample and digest solution, for example a glass flask of 250 ml. The inner wall of the vessel shall be inert and sha
44、ll not release substances to the digest in excess of the purity requirements of the subsequent analysis. NOTE 1 Quartz vessels can be used instead of glass vessels. NOTE 2 It may be necessary to periodically clean the reaction vessels with a suitable surfactant to remove persistent deposits. 7.1.2 R
45、eflux condenser adaptable to the digestion vessel (7.1.1). 7.1.3 Absorption vessel, volatile species trap, in an open digestion system capable of trapping one or more volatile measurement species, adaptable to the reflux condenser (7.1.2). DIN EN 16174:2012-11 EN 16174:2012 (E) 7 Key 1 absorption ve
46、ssel 2 reflux condenser 3 digestion vessel Figure 1 Digestion vessel (7.1.1), reflux condenser (7.1.2) and absorption vessel (7.1.3), assembled 7.1.4 Heating device, for example a heating mantle, thermostatic controlled, or an aluminium block thermostat. DIN EN 16174:2012-11 EN 16174:2012 (E) 8 7.2
47、Apparatus used for Method B 7.2.1 Digestion vessel, for pressurized microwave digestion, preferably of 100 ml volume, reagent-, temperature- and pressure-resistant and capable of containing the mixture of sample and digest solution. The vessel shall be suitable for the safe application in the temper
48、ature and pressure range applied, capable of withstanding pressures of at least 3 000 kPa. Digestion vessels made of perfluoro alkoxyl alkane (PFA), modified polytetrafluoroethene (PTFE) or quartz glass, and equipped with a safety pressure releasing system to avoid explosion of the vessel, shall be used. The inner wall of the vessel shall be inert and shall not release contaminations to the digest solution. NOTE It may be necessary to periodically cle
