EN 16173:2012

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Blato, obdelani biološki odpadki in tla - Razklop v dušikovi kislini topnih frakcij elementovSchlamm behandelter Bioabfall und Boden - Aufschluss von mit Salpetersäure löslichen Anteilen von ElementenBoue, biodéchet traité et sol - Digestion des éléments solubles dans l'acide nitriqueSludge, treated biowaste and soil - Digestion of nitric acid soluble fractions of elements13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16173:2012SIST EN 16173:2013en,fr,de01-februar-2013SIST EN 16173:2013SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE 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, biodéchets traités et sols - Digestion des éléments solubles dans l'acide nitrique
Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Salpetersäure löslichen 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 lists 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 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 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 United Kingdom.
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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: ESIST EN 16173:2013

Repeatability and reproducibility data .9A.1 Materials used in the interlaboratory comparison study .9A.2 Interlaboratory comparison results .9Bibliography . 11 SIST EN 16173:2013

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 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. 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 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 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. SIST EN 16173:2013

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 (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), 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), 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 applicable 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 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 — Guidance 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 placed 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 the 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 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 constituents, 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 interferences shall be properly addressed during determination. SIST EN 16173:2013

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 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. Verify the purity by performing a blank test. 5.2 Nitric acid, c(HNO3) = 15 mol/l, ρ = 1,4 kg/l. 5.3 Nitric acid, c(HNO3) = 0,5 mol/l; ρ = 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. 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 resistant 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 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 and 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 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. 6.2 Rotating turntable, with a minimum speed of 3 min–1.
6.3 Sample containers, plastics and glass con
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