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 13.080.10; 13.030.01!$O“1924404www.din.deDDIN EN 16173Sludge, treated biowaste and soil Digestion of nitric acid soluble fractions of elements;English version EN 16173:2012,English translation of DIN EN 16173:2012-11Schlamm, behandelter Bioabfall und Boden Aufschluss von mit Salpetersure lslichen
3、 Anteilen von Elementen;Englische Fassung EN 16173:2012,Englische bersetzung von DIN EN 16173:2012-11Boues, bio-dchets traits et sols Digestion des lments solubles dans lacide nitrique;Version anglaise EN 16173:2012,Traduction anglaise de DIN EN 16173:2012-11www.beuth.deIn case of doubt, the German-
4、language original shall be considered authoritative.Document comprises 13 pages 10.12 DIN EN 16173:2012-11 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, bio
5、waste 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 NA119-01-02-02 AA Chemische und physikalische Verfahren. Th
6、e DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determinatio
7、n of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16173 August 2012 ICS 13.080.10; 13.030.01 English Version Sludge, treated biowaste and soil - Digestion of nitric acid soluble fractions of elements Boues, bio-dchets traits
8、et sols - Digestion des lments solubles dans lacide nitrique Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Salpetersure lslichen 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
9、 which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. Thi
10、s 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 member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN memb
11、ers are the national standards bodies of 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, Poland, Portug
12、al, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN 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
13、 means reserved worldwide for CEN national Members. Ref. No. EN 16173:2012: EEN 16173:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Principle 54 Interferences and sources of errors 55 Reagents .66 Apparatus .67 Digestion procedure 78 Test report 8Annex A (infor
14、mative) Repeatability and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results .9Bibliography . 11DIN EN 16173:2012-11 EN 16173:2012 (E) 3 Foreword This document (EN 16173:2012) has been prepared by Technical Committee CEN/TC 400 “P
15、roject 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 con
16、flicting 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 do
17、cument 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 m
18、ethods 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 organizations
19、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, Ne
20、therlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16173:2012-11 EN 16173:2012 (E) 4 Introduction This method is intended to provide a multi-element digestion of sludge, treated biowaste and soil prior to analysis. It i
21、s 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 sample may not reflect the total concentrations of the target analytes. However, for most environmental applications the result is fit for the p
22、urpose. 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 validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal s
23、ludge Biowaste CompostSoil Sludge amended soils WARNING Persons using this European Standard should be familiar with usual laboratory practice. The reagents used in this European Standard are strongly corrosive and partly very toxic. Safety precautions are absolutely necessary, not only due to the s
24、trong 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. Domestic (kitchen) type microwave ovens shall not be used, as corrosion by acid vapours may compromise the funct
25、ion 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 be performed in a fume hood or in closed force-ventilated equipment. By the use of strong oxidising reagents, the f
26、ormation 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. Avoid contact with the chemicals and the gaseous reaction products. IMPORTANT It is absolutely essential that tests
27、 conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16173:2012-11 EN 16173:2012 (E) 5 1 Scope This European Standard specifies a method for microwave digestion of sludge, treated biowaste and soil using nitric acid. This method is applicable for microwave-
28、assisted nitric acid digestion of sludge, treated biowaste and soils for the following elements: Aluminium (Al), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium
29、(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 (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladi
30、um (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), sodium (Na), strontium (Sr), sulphur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium
31、 (Tm), 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 elements. Digestion with nitric acid will not necessarily accomplish total decomposition of the sample.
32、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 document and are indispensable for its application. For dated references, only the edition cited a
33、pplies. For undated references, the latest edition of the referenced document (including any amendments) applies. 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 Principle A test
34、 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 placed in a fluorocarbon polymer or quartz microwave vessel. The vessel is sealed and heated in the microwave unit. After cooling, the vessel c
35、ontents 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 the appropriate measurement method. 4 Interferences and sources of errors Due to the volatility of some compounds care shall be taken that t
36、he 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 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
37、 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 constituents, such as quartz, silicates, titanium dioxide, alumina and other oxides may not be dissolved. The bound elements are considered no
38、n-mobile in the environment and are excluded from most aquatic pollution transport mechanisms. High acid and solute concentrations in the digest that cause interferences shall be properly addressed during determination. DIN EN 16173:2012-11 EN 16173:2012 (E) 6 Ensure that the complete test portion i
39、s brought into contact with the acid mixture in the digestion vessel. There is a potential for vigorous reaction, especially with samples containing volatile or easily 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
40、 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 considerations (for example, the rapid release of carbon dioxide from carbonates, easily oxidizable organic matter). Once the initial re
41、action has ceased, the sample may continue through the digestion procedure. If the digested solution is filtrated, take care that the filtration procedure does not introduce contamination. 5 Reagents Use only acids and reagents of recognized analytical grade to avoid high blank values for subsequent
42、 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 2 as specified in EN ISO 3696 or better. The water for preparation of reagents shall meet the requirements of the subsequent analysis.
43、 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 laboratory apparatus. All glassware and plastics ware shall be adequately cleaned and stored in order to avoid any contamination. Depend
44、ing 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 resistant and well ventilated. All electronics shall be protected against corrosion for safe operation. Use a laboratory-grade microwave
45、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. Temperature sensors shall be accurate to 2 C, including the final react
46、ion 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 and microwave designs), control of the temperature during digestion is im
47、portant 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
48、 external, calibrated temperature measurement system, the microwave temperature measurement system should be calibrated. 6.2 Rotating turntable, with a minimum speed 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. DIN EN 16173:2012-11 EN 16173:2012 (E) 7 6.4 Digestion vessels of microwave transparent and reagent and temperature resistant materials, such as f
