SIST EN 16173:2013

Sludge, treated biowaste and soil - Digestion of nitric acid soluble fractions of elements

This European Standard 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), 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), 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 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.

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

Diese Europäische Norm legt ein Verfahren für den Aufschluss von Schlamm, behandeltem Bioabfall und Boden mittels Mikrowellengerät und Salpetersäure fest.
Das hier beschriebene Verfahren ist für den Säureaufschluss von Bioabfall, Schlamm und Boden mittels Mikrowellengerät auf folgende Elemente anwendbar:
Aluminium (Al), Arsen (As), Barium (Ba), Beryllium (Be), Bismuth (Bi), Blei (Pb), Bor (B), Cadmium (Cd), Cäsium (Cs), Calcium (Ca), Cerium (Ce), Chrom (Cr), Cobalt (Co), Dysprosium (Dy), Eisen (Fe), Erbium (Er), Europium (Eu), Gadolinium (Gd), Gallium (Ga), Germanium (Ge), Gold (Au), Hafnium (Hf), Holmium (Ho), Indium (In), Iridium (Ir), Kalium (K), Kupfer (Cu), Lanthan (La), Lithium (Li), Lutetium (Lu), Magnesium (Mg), Mangan (Mn), Molybdän (Mo), Natrium (Na), Neodym (Nd), Nickel (Ni), Palladium (Pd), Phosphor (P), Platin (Pt), Praseodymium (Pr), Quecksilber (Hg), Rhenium (Re), Rhodium (Rh), Rubidium (Rb), Ruthenium (Ru), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silicon (Si), Strontium (Sr), Tellur (Te), Terbium (Tb), Thallium (Tl), Thorium (Th), Thulium (Tm), Titan (Ti), Tungsten (W), Uran (U), Vanadium (V), Ytterbium (Yb), Yttrium (Y), Zink (Zn), and Zirconium (Zr).
Diese Europäische Norm darf auch für den Aufschluss anderer Elemente angewendet werden.
Der Aufschluss mit Salpetersäure führt nicht notwendigerweise zum vollständigen Abbau der Probe. Die extrahierten Konzentrationen der Analyten geben daher möglicherweise nicht den Gesamtgehalt in der Probe wieder.

Boue, biodéchet traité et sol - Digestion des éléments solubles dans l'acide nitrique

La présente Norme européenne spécifie une méthode de digestion par micro-ondes des boues, des biodéchets traités et des sols en utilisant de l'acide nitrique.
Cette méthode est applicable pour la digestion à l'acide nitrique assistée par micro-ondes des boues, des biodéchets traités et des sols pour les 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), 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'acide nitrique n'aboutit pas nécessairement à une minéralisation totale de l'échantillon. Les concentrations en analytes extraits ne reflètent pas nécessairement la teneur totale dans l'échantillon.

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

Ta evropski standard določa metodo za mikrovalovni razklop blata, bioloških odpadkov in tal z uporabo dušikove kisline. Ta metoda se uporablja za mikrovalovni razklop blata, obdelanih bioloških odpadkov in tal z dušikovo kislino za naslednje elemente: aluminij (Al), arzen (As), barij (Ba), berilij (Be), bizmut (Bi), bor (B), kadmij (Cd), kalcij (Ca), cerij (Ce), cezij (Cs), krom (Cr), kobalt (Co), baker (Cu), disprozij (Dy), erbij (Er), evropij (Eu), gadolinij (Gd), galij (Ga), germanij (Ge), zlato (Au), hafnij (Hf), holmij (Ho), indij (In), iridij (Ir), železo (Fe), lantan (La), svinec (Pb), litij (Li), lutecij (Lu), magnezij (Mg), mangan (Mn), živo srebro (Hg), molibden (Mo), neodim (Nd), nikelj (Ni), paladij (Pd), fosfor (P), platina (Pt), kalij (K), prazeodim (Pr), rubidij (Rb), renij (Re), rodij (Rh), rutenij (Ru), samarij (Sm), skandij (Sc), selen (Se), silicij (Si), natrij (Na), stroncij (Sr), žveplo (S), telurij (Te), terbij (Tb), talij (Tl), torij (Th), tulij (Tm), titan (Ti), volfram (W), uran (U), vanadij (V), iterbij (Yb), itrij (Y), cink (Zn) in cirkonij (Zr). Ta evropski standard se lahko uporablja tudi za razklop drugih elementov. Z razklopom z dušikovo kislino se ne doseže nujno popolna razgradnja vzorca. Iz ekstrahiranih koncentracij analita ni nujno razvidna skupna vsebina v vzorcu.

General Information

• Status: Published
• Public Enquiry End Date: 19-Feb-2011
• Publication Date: 20-Jan-2013
• ICS: 13.030.20 - Liquid wastes. Sludge
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 07-Jan-2013
• Due Date: 14-Mar-2013
• Completion Date: 21-Jan-2013
• Directive: 86/278/EEC - Protection of the environment, and in particular of the soil, when sewage sludge is used in agriculture
• Mandate: M/330 - Mandate given to CEN for the development of horizontal standards in the fields of sludge, biowaste and soil.
• Ref Project: EN 16173:2012 - Sludge, treated biowaste and soil - Digestion of nitric acid soluble fractions of elements

Overview

SIST EN 16173:2013 (CEN) defines a standardized method for microwave-assisted nitric acid digestion of sludge, treated biowaste and soil. The procedure is an operationally defined sample preparation step to extract nitric-acid soluble fractions of elements prior to instrumental multi-element analysis. The method is validated for common environmental matrices (municipal sludge, compost, soil and sludge-amended soils) and is intended for routine environmental monitoring and laboratory workflows.

Key points:

• The method uses concentrated HNO3 in sealed microwave vessels to digest a test portion.
• It is applicable to a broad range of elements (e.g., Al, As, Cd, Cr, Cu, Fe, Hg, Pb, Zn, U and various rare earths) and may be used for additional elements where appropriate.
• Digestion with nitric acid does not necessarily achieve total decomposition; results represent the nitric-acid soluble fraction, which is often fit for environmental applications.

Key Topics

• Principle: A weighed test portion is combined with concentrated nitric acid in microwave-transparent vessels (PFA/PTFE or quartz), heated under controlled temperature/pressure, cooled, then filtered or centrifuged and diluted to volume for analysis.

• Temperature control: The method requires controlled heating (typical final reaction temperature (175 ± 5) °C) with feedback temperature control and accurate sensors. Heating rates around 10–15 °C/min are recommended and a hold time is specified for consistent digestion.

• Apparatus and materials: Laboratory-grade microwave digestion system with corrosion-resistant components, pressure-rated vessels (≥3 000 kPa), turntable, acid-cleaned glassware or polymerware, and analytical balance are specified.

• Quality assurance: Include reagent blanks, use analytical-grade reagents and grade-2 or better water (EN ISO 3696), and follow validated sample pre-treatment guidance (EN 16179).

• Limitations & interferences: Volatile species, refractory matrix components (silicates, oxides) and container contamination can affect results. Careful handling, appropriate sample sizes for reactive matrices and attention to filtration/cleaning are required.

Applications

• Routine environmental monitoring of heavy metals and trace elements in sludge, treated biowaste and soils.
• Pre-treatment prior to ICP-OES, ICP-MS or other multi-element analytical techniques.
• Comparing nitric-acid soluble fractions across treatment processes, composting, soil amendment assessments and regulatory reporting where operationally-defined extracts are acceptable.

Related Standards

• EN 16179 - Guidance for sample pretreatment of sludge, biowaste and soil (referenced for sample preparation).
• EN ISO 3696 - Water for analytical laboratory use (specifies water grade for reagent preparation).

Safety note: Reagents are strongly corrosive and potentially toxic. Use laboratory-grade microwave equipment, perform work in fume hoods or closed ventilated systems, follow manufacturer instructions for vessel handling, and ensure trained personnel conduct the procedure.

This summary highlights practical requirements and applications of SIST EN 16173:2013 while emphasizing method scope, equipment, and safety considerations for reliable nitric-acid microwave digestion and subsequent element analysis.

Standards Content (Sample)

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.
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 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
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