Sludge, treated biowaste and soil - Digestion of aqua regia soluble fractions of elements

This European Standard specifies the pretreatment required for sludge, treated biowaste and soil (including soil-like materials), that are subject to the analysis of organic as well as inorganic chemical and physicochemical parameters. The pretreatment of samples aims at preparing a (small) test sample which is representative for the original sample. This European Standard describes the pretreatment which could be performed under field conditions if necessary and the sample pretreatment under laboratory conditions. For determining inorganic chemical and physico-chemical parameters this European Standard describes procedures to prepare: - test samples for tests under field moist conditions; - test samples for testing after drying, crushing, grinding, sieving etc.; - test samples of liquid sludge. For determination of organic compounds three pretreatment methods are specified: - a pretreatment method if volatile organic compounds are to be measured; - a pretreatment method if moderately volatile to non-volatile organic compounds are to be measured and the result of the following analysis will be accurate and reproducible; - a pretreatment method if moderately volatile to non-volatile organic compounds are to be measured and the extraction procedure prescribes a field moist sample or if only indicative results are required. The choice of the method depends above all on the volatility of the analyte. It also depends on the particle size distribution of the material, the heterogeneity of the sample and the following analytical procedure.

Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Königswasser löslichen Anteilen von Elementen

Diese Europäische Norm legt drei Verfahren zum Aufschluss von Schlamm, behandeltem Bioabfall und Boden mit Königswasser als Aufschlusslösung fest.
Diese Europäische Norm ist auf folgende Elemente anwendbar:
Arsen (As), Barium (Ba), Cadmium (Cd), Chrom (Cr), Cobalt (Co), Kupfer (Cu), Eisen (Fe), Blei (Pb), Quecksilber (Hg), Molybdän (Mo), Nickel (Ni), Selen (Se), Strontium (Sr), Thallium (Tl), Vanadium (V), Zink (Zn), Phosphor (P) und Schwefel (S).
Die Verfahren dürfen auch auf weitere Elemente angewendet werden.
Beim Aufschluss mit Königswasser, der verfahrensbedingt festgelegt ist, werden nicht unbedingt alle Elemente vollständig aufgeschlossen.

Boue, biodéchet traité et sol - Digestion des éléments solubles dans l'eau régale

La présente Norme européenne spécifie deux méthodes de digestion des boues, des biodéchets traités et des sols avec de l'eau régale comme solution de digestion.
La présente Norme européenne est applicable aux éléments suivants :
Aluminium (Al), antimoine (Sb), arsenic (As), baryum (Ba), béryllium (Be), bismuth (Bi), bore (B), cadmium (Cd), calcium (Ca), cérium (Ce), césium (Cs), chrome (Cr), cobalt (Co), cuivre (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), or (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), fer (Fe), lanthane (La), plomb (Pb), lithium (Li), lutétium (Lu), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène (Mo), néodyme (Nd), nickel (Ni), palladium (Pd), phosphore (P), platine (Pt), potassium (K), praséodyme (Pr), rubidium (Rb), rhénium (Re), rhodium (Rh), ruthénium (Ru), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn) et zirconium (Zr).
La présente Norme européenne peut également s'appliquer à la digestion d'autres éléments.
La digestion à l'eau régale n'aboutit pas nécessairement à une décomposition totale de l'échantillon. Les concentrations d'analytes extraits ne reflètent pas nécessairement les teneurs totales dans l'échantillon.

Blato, obdelani biološki odpadki in tla - Razklop v zlatotopki topnih frakcij elementov

Ta evropski standard določa pripravo blata, obdelanih bioloških odpadkov in tal (vključno z materiali, ki so podobni tlom), ki so obravnavani v analizi organskih in anorganskih kemijskih in fizikalno-kemijskih parametrov. Priprava vzorcev je namenjena pripravi (majhnega) preskusnega vzorca, ki je reprezentativen za izvorni vzorec. V tem evropskem standardu sta opisani priprava, ki se lahko po potrebi izvede na prostem, in priprava vzorca v laboratorijskih pogojih. V tem evropskem standardu so za določitev anorganskih kemijskih in fizikalno-kemijskih parametrov opisani postopki za pripravo: – preskusnih vzorcev za preskuse v vlažnih razmerah na prostem; – preskusnih vzorcev za preskušanje po sušenju, drobljenju, mletju, sejanju itd.; – preskusnih vzorcev tekočega blata. Za določanje organskih spojin so opredeljene tri metode priprave: – metoda priprave v primeru merjenja hlapnih organskih spojin; – metoda priprave, če se merijo slabo hlapne do nehlapne organske spojine, pri čemer bo rezultat naslednje analize natančen in ponovljiv; – metoda priprave, če se merijo slabo hlapne do nehlapne organske spojine in je za postopek ekstrakcije potreben vzorec vlage na prostem ali če so potrebni samo nakazalni rezultati. Izbira metode je odvisna predvsem od hlapnosti analita. Odvisna je tudi od razporeditve delcev po velikosti materiala, raznovrstnosti vzorca in naslednjega analiznega postopka.

General Information

Status
Published
Public Enquiry End Date
19-Feb-2011
Publication Date
07-Jan-2013
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Jan-2013
Due Date
11-Mar-2013
Completion Date
08-Jan-2013

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Blato, obdelani biološki odpadki in tla - Razklop v zlatotopki topnih frakcij elementovSchlamm, behandelter Bioabfall und Boden - Aufschluss von mit Königswasser löslichen Anteilen von ElementenBoue, biodéchet traité et sol - Digestion des éléments solubles dans l'eau régaleSludge, treated biowaste and soil - Digestion of aqua regia soluble fractions of elements13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16174:2012SIST EN 16174:2013en,fr,de01-februar-2013SIST EN 16174:2013SLOVENSKI

STANDARD
SIST EN 16174:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16174
August 2012 ICS 13.030.01; 13.080.10 English Version

Sludge, treated biowaste and soil - Digestion of aqua regia soluble fractions of elements

Boues, biodéchets traités et sols - Digestion des éléments solubles dans l'eau régale

Schlamm, behandelter Bioabfall und Boden - Aufschluss von mit Königswasser 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.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR 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: ESIST EN 16174:2013

EN 16174:2012 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41 Scope ......................................................................................................................................................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) °C ..........................................99 Test report ........................................................................................................................................... 10Annex A (informative)

Repeatability and reproducibility data ..................................................................... 11A.1 Materials used in the interlaboratory comparison study ............................................................... 11Bibliography ..................................................................................................................................................... 12 SIST EN 16174:2013

EN 16174:2012 (E) 3 Foreword This document (EN 16174:2012) 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 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 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 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 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 organizations 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

SIST EN 16174:2013

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 analysis. 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 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 Municipal sludge

Industrial sludge Sludge from electronic industry Ink waste sludge

Sewage sludge Biowaste (Method A) Compost Composted sludge Soil Agricultural soil 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 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 16174:2013

EN 16174:2012 (E) 5 1 Scope This European Standard 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), 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), silver (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 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 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 15936, Sludge, treated biowaste, soil and waste — Determination 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 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 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. SIST EN 16174:2013

EN 16174:2012 (E) 6 5 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. High acid and solute concentrations in the digest may cause interferences at determination. 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, 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 without a sample. 6.1 Water, quality 2 according to EN ISO 3696 or better. 6.2 Hydrochloric acid, c(HCl) = 12 mol/l; ρ = 1,18 kg/l. 6.3 Nitric acid, c(HNO3) = 15 mol/l, ρ = 1,4 kg/l. 6.4 Nitric acid, c(HNO3) = 0,5 mol/l, ρ = 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 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 cleaning 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 shall not release substances to the digest in excess of the purity requirements of the subsequent analysis. NOTE 1 Q

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