1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16173:2012Sludge, treated biowaste andsoil Digestion of nitric acidsoluble fractions of elementsBS EN 16173:2012 BRITISH STANDARDNational forewordThis British Standard is t
2、he UK implementation of EN 16173:2012. 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 i
3、nclude 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 56699 8 ICS 13.030.01; 13.080.10 Compliance with a British Standard cannot confer immunity from legal obli
4、gations.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 16173:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16173 August 2012 ICS 13.080.10; 13.
5、030.01 English Version Sludge, treated biowaste and soil - Digestion of nitric acid soluble fractions of elements Boues, biodchets traits et sols - Digestion des lments solubles dans lacide nitrique Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Salpetersure lslichen Anteilen von Elem
6、enten 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 lists and bibliographical r
7、eferences 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
8、 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 Yugoslav Republic of Maced
9、onia, 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 EUROPEN DE NORMALISATION EURO
10、PISCHES 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 16173:2012: EBS EN 16173:2012EN 16173:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52
11、 Normative references 53 Principle 54 Interferences and sources of errors 55 Reagents .66 Apparatus .67 Digestion procedure 78 Test report 8Annex A (informative) Repeatability and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results
12、 .9Bibliography . 11BS EN 16173:2012EN 16173:2012 (E) 3 Foreword This document (EN 16173:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by DIN. This European Standard sh
13、all 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 standards shall be withdrawn at the latest by February 2013. Attention is drawn to the possibility that some of the elements of this
14、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 prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The preparation of this docum
15、ent 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 hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treat
16、ed biowaste and soil as far as this is technically feasible. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia
17、, Finland, Former Yugoslav 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 the United Kingdom. BS EN 16173:2012EN 16173:2
18、012 (E) 4 Introduction This method is intended to provide a multi-element digestion of sludge, treated biowaste and soil prior to analysis. It is known that the digestion of environmental samples with nitric acid does not necessarily lead to a complete element breakdown, and the extract from a test
19、sample may not reflect the total concentrations of the target analytes. However, for most environmental applications the result is fit for the purpose. This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see also Annex A for the results of the va
20、lidation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste CompostSoil Sludge amended soils WARNING Persons using this European Standard should be familiar with usual laboratory practice. The reagents
21、 used 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 resist
22、ant safety 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
23、energy. 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 b
24、efore 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. BS EN 16173:2012EN 16173:2012 (E) 5 1 Scope This European Standard
25、specifies a method for microwave digestion of sludge, treated biowaste and soil using nitric acid. This method is applicable for microwave-assisted nitric acid digestion of sludge, treated biowaste and soils for the following elements: Aluminium (Al), arsenic (As), barium (Ba), beryllium (Be), bismu
26、th (Bi), boron (B), cadmium (Cd), calcium (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),
27、lead (Pb), lithium (Li), lutetium (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)
28、, selenium (Se), silicon (Si), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr). This European Standard may also be app
29、licable for the digestion of other elements. Digestion with nitric acid 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
30、part, are normatively 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 16179, Sludge, treated biowaste and soil Gui
31、dance for sample pretreatment EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Principle A test portion is digested in concentrated nitric acid by means of microwave heating with a suitable laboratory microwave unit. The sample and the nitric acid are plac
32、ed in a fluorocarbon polymer or quartz microwave vessel. The vessel is sealed and heated in the microwave unit. After cooling, the vessel contents are filtered, centrifuged or allowed to settle and the clear solution is then transferred into a volumetric flask and diluted to volume and analysed by t
33、he appropriate measurement method. 4 Interferences and sources 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. The container in which the sample
34、 is delivered and stored can be a source of errors. The material shall be chosen according to the elements to be determined; e.g. elemental Hg can penetrate polyethylene walls very fast in both directions. Glass containing e.g. B, Na, K, Al can contaminate samples. A few refractory sample matrix con
35、stituents, such as quartz, silicates, titanium dioxide, alumina and other oxides may not be dissolved. The bound elements are considered non-mobile in the environment and are excluded from most aquatic pollution transport mechanisms. High acid and solute concentrations in the digest that cause inter
36、ferences shall be properly addressed during determination. BS EN 16173:2012EN 16173:2012 (E) 6 Ensure that the complete test portion is brought into contact with the acid mixture in the digestion vessel. There is a potential for vigorous reaction, especially with samples containing volatile or easil
37、y oxidizable species. When digesting a matrix of this type, use no more than 0,1 g sample to begin with. If a vigorous reaction occurs upon addition of nitric acid, allow the sample to pre-digest in the uncapped digestion vessel until the reaction ceases. Heat may be added in this step for safety co
38、nsiderations (for example, the rapid release of carbon dioxide from carbonates, easily oxidizable organic matter). Once the initial reaction has ceased, the sample may continue through the digestion procedure. If the digested solution is filtrated, take care that the filtration procedure does not in
39、troduce contamination. 5 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. 5.1 Water, grade
40、2 as specified in EN ISO 3696 or better. The water for preparation of reagents shall meet the requirements of the subsequent analysis. Verify the purity by performing a blank test. 5.2 Nitric acid, c(HNO3) = 15 mol/l, = 1,4 kg/l. 5.3 Nitric acid, c(HNO3) = 0,5 mol/l; = 1,0 kg/l. 6 Apparatus Usual la
41、boratory 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. 6.1 Microwave digestion system, corrosion res
42、istant and well ventilated. All electronics shall be protected 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
43、adjust the microwave field output power within 2 s of sensing. 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 an
44、d microwave digestion equipment (i.e. different vessel types 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 te
45、mperature 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. 6.2 Rotating turntable, with a minimum speed
46、of 3 min1. 6.3 Sample containers, plastics and glass containers are both suitable. All containers shall be adequately acid cleaned and stored in order to avoid any contamination. BS EN 16173:2012EN 16173:2012 (E) 7 6.4 Digestion vessels of microwave transparent and reagent and temperature resistant
47、materials, such as fluorocarbon (e.g. perfluoro alkoxyl alkane (PFA), modified polytetrafluoroethene (PTFE) or quartz. The vessels may contain layers of different microwave transparent materials for strength, durability and safety. The internal volume shall be at least 45 ml, and the vessel shall be
48、 capable of withstanding pressures of at least 3 000 kPa and capable of controlled pressure relief. The inner wall of the vessel shall be inert and shall not release substances to the digest in excess of the purity requirements of the subsequent analysis. The vessel shall be suitable for the safe ap
49、plication in the temperature and pressure range applied. Energy regulation of the microwave digestion system shall be based on the temperature in the digestion solutions. Depending on the construction of the unit used temperature is measured indirectly in every vessel, outside the vessels with optical systems or only in one vessel. All digestion vessels shall be adequately acid cleaned and stored in order to avoid any contamination. NOTE Digestion vessels may be cleaned in e.g. 10 % nitric acid. 6.5 Filter paper, cellul
