CEN/TS 16171:2012
(Main)Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS)
Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS)
This Technical Specification specifies a method for the determination of the following elements in aqua regia or nitric acid digests of sludge, treated biowaste and soil:
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), rhenium (Re), rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (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).
The working range depends on the matrix and the interferences encountered.
The limit of detection of the method is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements.
The limit of detection will be higher in cases where the determination is likely to be interfered (see Clause 4) or in case of memory effects (see e.g. 8.2 of EN ISO 17294-1:2006).
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)
Diese Technische Spezifikation legt ein Verfahren fest, nach dem in Aufschlusslösungen von Schlamm, behandeltem Bioabfall und Boden nach Königswasser und Salpetersäureaufschluss die folgenden Elemente bestimmt werden:
Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Blei (Pb), Bor (B), Cadmium (Cd), Caesium (Cs), Calcium (Ca), Cer (Ce), Chrom (Cr), 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), Kobalt (Co), 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), Praseodym (Pr), Quecksilber (Hg), Rhenium (Re), Rhodium (Rh), Rubidium (Rb), Ruthenium (Ru), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silicium (Si), Strontium (Sr), Tellur (Te), Terbium (Tb), Thallium (Tl), Thorium (Th), Thulium (Tm), Titan (Ti), Uran (U), Vanadium (V), Wolfram (W), Wismut (Bi), Ytterbium (Yb), Yttrium (Y), Zink (Zn), Zinn (Sn) und Zirkonium (Zr).
Der Arbeitsbereich hängt von der Matrix und den zu erwartenden Störungen ab.
Die Nachweisgrenze des Verfahrens für die meisten Elemente liegt zwischen 0,1 mg/kg Trockenmasse und 2,0 mg/kg Trockenmasse.
Die Nachweisgrenze wird höher ausfallen, wenn bei der Bestimmung Störungen möglich sind (siehe Abschnitt 4), oder Memoryeffekte (Verschleppungseffekte) auftreten (siehe 8.2 in EN ISO 17294 1:2006).
Boues, bio-déchets traités et sols - Détermination des éléments en traces par spectrométrie de masse avec plasma induit par haute fréquence (ICP-MS)
La présente Spécification technique spécifie une méthode de détermination des éléments suivants dans des digestats d’eau régale ou d’acide nitrique de boues, de bio-déchets traités et de sols :
Aluminium (Al), antimoine (Sb), arsenic (As), baryum (Ba), béryllium (Be), bismuth (Bi), bore (B), cadmium (Cd), calcium (Ca), cérium (Ce), 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), lutécium (Lu), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène (Mo), néodyme (Nd), nickel (Ni), palladium (Pd), phosphore (P), platine (Pt), potassium (K), praseodyme (Pr), rhénium (Re), rhodium (Rh), rubidium (Rb), ruthénium (Ru), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), terbium (Tb), thallium (Tl), thulium (Tm), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), ytterbium(Yb), yttrium (Y), zinc (Zn) et zirconium (Zr).
L’étendue de mesure dépend de la matrice et des interférences rencontrées.
Les limites de détection de la méthode sont comprises entre 0,1 mg/kg de matière sèche et 2,0 mg/kg de matière sèche pour la plupart des éléments.
La limite de détection est plus élevée lorsque la détermination est sujette à des interférences (voir l’Article 4) ou en cas d’effets mémoire (voir 8.2 de l’EN ISO 17294-1:2006, par exemple).
Blato, obdelani biološki odpadki in tla - Določevanje elementov z masno spektrometrijo z induktivno sklopljeno plazmo (ICP/MS)
Ta tehnična specifikacija opredeljuje metodo za določevanje naslednjih elementov v zlatotopki ali izvlečku dušikove kisline blata, obdelanih bioloških odpadkov in tal: aluminij (Al), antimon (Sb), 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), renij (Re), rodij (Rh), rutenij (Ru), samarij (Sm), skandij (Sc), selen (Se), silicij (Si), srebro (Ag), natrij (Na), stroncij (Sr), žveplo (S), telurij (Te), terbij (Tb), talij (Tl), torij (Th), tulij (Tm), kositer (Sn), titan (Ti), volfram (W), uran (U), vanadij (V), iterbij (Yb), itrij (Y), cink (Zn) in cirkonij (Zr). Delovni razpon je odvisen od matrice in motenj, ki se pojavijo. Meja detekcije te metode za večino elementov je med 0,1 in 2,0 mg/kg suhe snovi. Meja detekcije bo višja v primerih, ko obstaja možnost motnje določevanja (glej točko 4), ali v primeru spominskih učinkov (glej npr. točko 8.2 standarda EN ISO 17294-1:2006).
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-2013
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHHOHPHQWRY]PDVQR
VSHNWURPHWULMR]LQGXNWLYQRVNORSOMHQRSOD]PR ,&306
Sludge, treated biowaste and soil - Determination of elements using inductively coupled
plasma mass spectrometry (ICP-MS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels
Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)
Boues, bio-déchets traités et sols - Détermination des éléments en traces par
spectrométrie de masse avec plasma induit par haute fréquence (ICP-MS)
Ta slovenski standard je istoveten z: CEN/TS 16171:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 16171
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2012
ICS 13.030.01; 13.080.10
English Version
Sludge, treated biowaste and soil - Determination of elements
using inductively coupled plasma mass spectrometry (ICP-MS)
Boues, bio-déchets traités et sols - Détermination des Schlamm, behandelter Bioabfall und Boden - Bestimmung
éléments en traces par spectrométrie de masse avec von Elementen mittels Massenspektrometrie mit induktiv
plasma induit par haute fréquence (ICP-MS) gekoppeltem Plasma (ICP-MS)
This Technical Specification (CEN/TS) was approved by CEN on 16 July 2012 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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 Ref. No. CEN/TS 16171:2012: E
worldwide for CEN national Members.
Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Principle .5
4 Interferences .6
4.1 General .6
4.2 Spectral interferences .6
4.2.1 Isobaric elemental interferences .6
4.2.2 Isobaric molecular and doubly-charged ion interferences .6
4.2.3 Non-spectral interferences .6
5 Reagents .7
6 Apparatus .9
7 Procedure . 10
7.1 Test sample solution . 10
7.2 Test solution . 11
7.3 Instrument set-up. 11
7.4 Calibration . 11
7.4.1 Linear calibration function . 11
7.4.2 Standard addition calibration . 12
7.4.3 Determination of correction factors. 12
7.4.4 Variable isotope ratio . 12
7.5 Sample measurement . 12
8 Calculation . 13
9 Expression of results . 13
10 Performance characteristics . 13
10.1 Blank . 13
10.2 Calibration check . 14
10.3 Internal standard response . 14
10.4 Interference . 14
10.5 Recovery . 14
10.6 Precision . 14
11 Test report . 14
Annex A (informative) Selected isotopes and spectral interferences for quadrupole ICP-MS
instruments . 15
Bibliography . 16
Foreword
This document (CEN/TS 16171:2012) 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.
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 organisations of the following
countries are bound to announce 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.
Introduction
This Technical Specification is applicable for several types of matrices as indicated in Table 1.
Table 1 — Matrices for which this Technical Specification is applicable
Matrix Materials tested
Sludge Municipal sludge
Biowaste Compost
Soil Sludge amended soils
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this Technical
Specification be carried out by suitably trained staff.
1 Scope
This Technical Specification specifies a method for the determination of the following elements in aqua regia
or nitric acid digests of sludge, treated biowaste and soil:
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), rhenium (Re),
rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si),
silver (Ag), sodium (Na), strontium (Sr), sulfur (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).
The working range depends on the matrix and the interferences encountered.
The limit of detection of the method is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most
elements.
The limit of detection will be higher in cases where the determination is likely to be interfered (see Clause 4) or
in case of memory effects (see e.g. 8.2 of EN ISO 17294-1:2006).
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 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after determination of
dry residue or water content
EN 16173, Sludge, treated biowaste and soil — Digestion of nitric acid soluble fractions of elements
EN 16174, Sludge, treated biowaste and soil — Digestion of aqua regia soluble fractions of elements
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
EN ISO 17294-1:2006, Water quality — Application of inductively coupled plasma mass spectrometry
(ICP-MS) — Part 1: General guidelines (ISO 17294-1:2004)
3 Principle
Digests of sludge, treated biowaste or soil with nitric acid or aqua regia (see EN 16173 and EN 16174) are
analysed by ICP-MS to get a multi-elemental determination of analytes.
The method measures ions produced by a radio-frequency inductively coupled plasma. Analyte species
originating in the digest solution are nebulised and the resulting aerosol is transported by argon gas into the
plasma. The ions produced by the high temperatures of the plasma are entrained in the plasma gas and
introduced, by means of an interface, into a mass spectrometer, sorted according to their mass-to-charge
ratios and quantified with a detector (e.g. channel electron multiplier).
4 Interferences
4.1 General
Interferences shall be assessed and valid corrections applied. Interference correction shall include
compensation for background ions contributed by the plasma gas, reagents, and constituents of the sample
matrix.
Detailed information on spectral and non-spectral interferences is given in EN ISO 17294-1:20
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.