1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16174:2012Sludge, treated biowaste andsoil Digestion of aqua regiasoluble fractions of elementsBS EN 16174:2012 BRITISH STANDARDNational forewordThis British Standard is th
2、e UK implementation of EN 16174:2012. The UK participation in its preparation was entrusted to T e c h n i c a l Committee H/-/4, Environmental testing programmes.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to in
3、clude all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012Published by BSI Standards Limited 2012ISBN 978 0 580 56703 2 ICS 13.030.01; 13.080.10 Compliance with a British Standard cannot confer immunity from legal oblig
4、ations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS EN 16174:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16174 August 2012 ICS 13.030.01; 13.0
5、80.10 English Version Sludge, treated biowaste and soil - Digestion of aqua regia soluble fractions of elements Boues, biodchets traits et sols - Digestion des lments solubles dans leau rgale Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Knigswasser lslichen Anteilen von Elementen Th
6、is 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 lists and bibliographical reference
7、s 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 the responsibility of a CEN mem
8、ber 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 Yugoslav Republic of Macedonia, Fr
9、ance, 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 EUROPEN DE NORMALISATION EUROPISCHES
10、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: EBS EN 16174:2012EN 16174:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normati
11、ve 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) C 99 Test rep
12、ort . 10Annex A (informative) Repeatability and reproducibility data . 11A.1 Materials used in the interlaboratory comparison study . 11Bibliography . 12BS EN 16174:2012EN 16174:2012 (E) 3 Foreword This document (EN 16174:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee -
13、 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 conflicting national
14、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 document has been pr
15、epared 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 methods for hygieni
16、c 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 organizations of the following c
17、ountries 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, Netherlands, Norway,
18、 Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16174:2012EN 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 analysis. It is known that
19、 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 is fit for the purpose.
20、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 Municipal sludge Industr
21、ial 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 in this European Standar
22、d 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 safety devices is required
23、. 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 energy. All procedures shall b
24、e 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 they have cooled down. A
25、void 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. BS EN 16174:2012EN 16174:2012 (E) 5 1 Scope This European Standard specifies two methods for dige
26、stion 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), calcium (Ca), cerium (Ce), cesi
27、um (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 (Lu), magnesium (Mg), manganese
28、 (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), silver (Ag), sodium (Na), strontiu
29、m (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 the digestion of other element
30、s. 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 normatively referenced in this do
31、cument 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 Determination of total organic carbon (
32、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 and definitions apply. 3.1 aqu
33、a 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 reflux for 2 h, followed by fi
34、ltration 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. BS EN 16174:2012EN 16174:2012 (E) 6 5 Interferences and sources of errors Due to the volatility
35、 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. Contamination shall be avoided. Gl
36、ass 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, e.g. low soluble chlorides, fluori
37、des 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 without a sample. 6.1 Water, quality 2 a
38、ccording 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 agent, e.g. n-dodecane (C12H26) or Octa
39、nol (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 cleaning of the vessels shall be taken
40、. 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 shall not release substances to the di
41、gest 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 Reflux condenser adaptable to the di
42、gestion 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). BS EN 16174:2012EN 16174:2012 (E) 7 Key 1 absorption vessel 2 reflux condenser 3 digestion vess
43、el 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. BS EN 16174:2012EN 16174:2012 (E) 8 7.2 Apparatus used for Method B 7.2.1 Digestion v
44、essel, 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 temperature and pressure range applied, capable of
45、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 i
46、nert and shall not release contaminations to the digest solution. NOTE It may be necessary to periodically clean the reaction vessels with a suitable surfactant to remove persistent deposits. 7.2.2 Microwave digestion system, corrosion resistant and well ventilated. All electronics shall be protecte
47、d against corrosion for safe operation. Use a laboratory-grade microwave oven with temperature feedback control mechanisms. The microwave digestion system should be able to control the temperature with an accuracy of 5 C and automatically adjust the microwave field output power within 2 s of sensing
48、. Temperature sensors shall be accurate to 2 C, including the final reaction temperature of (175 5) C. Temperature feedback control provides the primary performance mechanism for the method. Due to the variability in sample matrix types and microwave digestion equipment (i.e. different vessel types
49、and microwave designs), control of the temperature during digestion is important for reproducible microwave heating and comparable data. The accuracy of the temperature measurement system should be periodically controlled at an elevated temperature according to the manufactures instructions. If the temperature deviates by more than 2 C from the temperature measured by an external, calibrated temperature measurement system, the microwave temperature measurement system should be calibrated. 7.2.
