SIST-TS CEN/TS 16170:2013
(Main)Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES)
Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES)
This Technical Specification specifies a method for the determination of the following elements in aqua regia, nitric acid digest solutions of sludge, treated biowaste and soil: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), indium (In), iron (Fe), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), nickel (Ni), phosphorus (P), potassium (K), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), thallium (Tl), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn) and zirconium (Zr). Table A.1 lists the elements for which this method is applicable along with the recommended wavelength and typical instrumental detection limits for clean matrices.
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES)
Diese Europäische Norm legt ein Verfahren fest, nach dem in Schlamm, behandeltem Bioabfall und Boden nach Königswasser und Salpetersäureaufschluss die folgenden Elemente bestimmt werden:
Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Wismut (Bi), Bor (B), Cadmium (Cd), Calcium (Ca), Cer (Ce), Chrom (Cr), Kobalt (Co), Kupfer (Cu), Eisen (Fe), Lanthan (La), Blei (Pb), Lithium (Li), Magnesium (Mg), Mangan (Mn), Quecksilber (Hg), Molybdän (Mo), Neodym (Nd), Nickel (Ni), Phosphor (P), Kalium (K), Praseodym (Pr), Samarium (Sm), Scandium (Sc), Selen (Se), Silicium (Si), Silber (Ag), Natrium (Na), Strontium (Sr), Schwefel (S), Tellur (Te), Thallium (Tl), Thorium (Th), Zinn (Sn), Titan (Ti), Wolfram (W), Uran (U), Vanadium (V), Zink (Zn) und Zirkonium (Zr).
In Tabelle A.1 sind die Elemente aufgeführt, auf die dieses Verfahren anwendbar ist, sowie die empfohlenen Wellenlängen und die geräteabhängigen Nachweisgrenzen, die für saubere Matrices üblicherweise zutreffen.
ANMERKUNG Nach der Validierung wird der Anwendungsbereich genauer eingegrenzt.
Boues, bio-déchets et sols - Détermination des éléments en traces par spectrométrie d'émission optique avec plasma induit par haute fréquence (ICP-OES)
La présente Norme européenne spécifie une méthode de détermination des éléments suivants dans les digestats d'eau régale et 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), fer (Fe), lanthane (La), plomb (Pb), lithium (Li), magnésium (Mg), manganèse (Mn), mercure (Hg), molybdène (Mo), néodyme (Nd), nickel (Ni), phosphore (P), potassium (K), praséodyme (Pr), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tellure (Te), thorium (Th), thallium (Tl), étain (Sn), titane (Ti), tungstène (W), uranium (U), vanadium (V), zinc (Zn) et zirconium (Zr).
Le Tableau A.1 donne la liste des éléments pour lesquels la présente méthode est applicable ainsi que la longueur d'onde recommandée et les limites de détection typiques de l'instrument pour des matrices propres.
NOTE Le domaine d'application sera indiqué plus précisément après validation.
Blato, obdelani biološki odpadki in tla - Določevanje elementov z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/OES)
V tej tehnični specifikaciji je opredeljena metoda za določevanje naslednjih elementov v zlatotopki, raztopini izvlečka 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), krom (Cr), kobalt (Co), baker (Cu), galij (Ga), indij (In), železo (Fe), svinec (Pb), litij (Li), magnezij (Mg), mangan (Mn), merkur (Hg), molibden (Mo), nikelj (Ni), fosfor (P), kalij (K), selen (Se), silicij (Si), srebro (Ag), natrij (Na), stroncij (Sr), žveplo (S), talij (Tl), kositer (Sn), titan (Ti), volfram (W), uran (U), vanadij (V), cink (Zn) in cirkonij (Zr). V preglednici A.1 so navedeni elementi, za katere se lahko uporabi ta metoda, priporočene valovne dolžine in značilne meje detekcije instrumentov za čiste matrice.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 16170:2013
01-februar-2013
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHHOHPHQWRY]RSWLþQR
HPLVLMVNRVSHNWURPHWULMR]LQGXNWLYQRVNORSOMHQRSOD]PR ,&32(6
Sludge, treated biowaste and soil - Determination of elements using inductively coupled
plasma optical emission spectrometry (ICP-OES)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels
optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES)
Boues, bio-déchets et sols - Détermination des éléments en traces par spectrométrie
d'émission optique avec plasma induit par haute fréquence (ICP-OES)
Ta slovenski standard je istoveten z: CEN/TS 16170:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST-TS CEN/TS 16170:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 16170:2013
TECHNICAL SPECIFICATION
CEN/TS 16170
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 optical emission spectrometry
(ICP-OES)
Boues, bio-déchets et sols - Détermination des éléments Schlamm, behandelter Bioabfall und Boden - Bestimmung
en traces par spectrométrie d'émission optique avec von Elementen mittels optischer Emissionsspektrometrie
plasma induit par haute fréquence (ICP-OES) mit induktiv gekoppeltem Plasma (ICP-OES)
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 16170:2012: E
worldwide for CEN national Members.
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Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Principle .5
4 Interferences .5
5 Reagents .6
6 Apparatus .8
7 Procedure .9
7.1 Test sample solution .9
7.2 Test solution .9
7.3 Instrument set-up.9
7.4 Calibration . 10
7.5 Sample measurement . 10
8 Calculation . 11
9 Expression of results . 11
10 Performance characteristics . 11
10.1 Calibration check . 11
10.2 Interference . 11
10.3 Recovery . 12
10.4 Precision . 12
11 Test report . 12
Annex A (informative) Wavelengths, spectral interferences and estimated instrumental detection
limits . 13
Annex B (informative) Precision data . 16
Annex C (informative) Inter-element correction . 19
Bibliography . 21
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Foreword
This document (CEN/TS 16170:2012) 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.
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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.
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1 Scope
This Technical Specification specifies a method for the determination of the following elements in aqua regia,
nitric acid digest solutions of sludge, treated biowaste and soil:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium
(Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), indium (In), iron (Fe), lead (Pb),
lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), nickel (Ni), phosphorus (P),
potassium (K), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), thallium (Tl), tin
(Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn) and zirconium (Zr).
Table A.1 lists the elements for which this method is applicable along with the recommended wavelength and
typical instrumental detection limits for clean matrices.
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)
3 Principle
Digests of sludge, treated biowaste or soil with nitric acid or aqua regia (see EN 16173 and EN 16174) are
analysed by inductively coupled plasma optical emission spectrometry (ICP-OES) using sequential or
simultaneous optical systems and axial or radial viewing of the plasma.
The instrument measures characteristic emission spectra by optical spectrometry. Analyte species originating
in the digest solution are nebulised and the resulting aerosol is transported to the plasma torch. Element-
specific emission spectra are produced by a radio-frequency inductively coupled plasma. The spectra are
dispersed by a grating spectrometer, and the intensities of the emission lines are monitored by photosensitive
devices.
4 Interferences
Background correction is required for trace element determination. Background correction is not required in
cases of line broadening where a background correction measurement would actually degrade the analytical
result. Additional interferences and matrix effects shall be recognised and appropriate corrections made. Tests
for their presence are described below.
Spectral interferences are caused by background emission from continuous or recombination phenomena,
stray light which causes background increase or overlap of a spectral line from another element, or
unresolved overlap of molecular band spectra.
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Background emission and stray light can usually be compensated for by subtracting the background emission
determined by measurements adjacent to the analyte wavelength peak. Spectral scans of samples compared
with single element solutions in the analyte regions may indicate when alternate wavelengths are desirable
because of severe spectral interference. These scans will also show whether the most appropriate estimate of
the background emission is provided by an interpolation from measurements on both sides of the wavelength
peak or by measured emission on only one side. The locations selected for the measurement of background
intensity will be determined by the complexity of the spectrum adjacent to the wavelength peak. The locations
used for routine measurement shall be free of off-line spectral interference (inter-element or molecular) or
adequately corrected to reflect the same change in background intensity as occurs at the wavelength peak.
Spectral overlaps may be avoided by using an alternate wavelength. Alternatively they can be corrected by
multiple dimensional spectra fitting methods or by equations that correct for inter-element contributions.
Instruments that use equations for inter-element correction require the interfering elements to be analysed at
the same time as the element of interest. When operative and uncorrected, interferences will produce false
positive determinations and would be reported as analyte concentrations. The interferences are listed in
Table A.1.
If available, the user should apply multiple dimensional spectra fitting methods provided by the manufacturer,
as a corrective action. In this case, the selection of background points for correction is not necessary, since all
adjacent wavelengths are processed.
Physical interferences are effects associated with the sample nebulisation and transport processes. Changes
in viscosity and surface tension can cause significant inaccuracies, especially in samples containing high
dissolved solids or high acid concentrations. If physical interferences are present, they shall be reduced by
diluting the sample, matching the acid concentration, matrix-matching, or a high solid nebuliser. They can be
corrected for by using an internal standard.
Chemical interferences include molecular compound formation, ionisation effects, and solute vaporisation
effects. Normally, these effects are not significant with the ICP technique, but if observed, can be minimised
by careful selection of operating conditions (e. g. radio frequency (RF) power, observation position, gas flow
rate and so forth), by buffering of the sample, by matrix matching, and by standard addition procedures.
Chemical interferences are highly dependent on matrix type and the specific analyte element.
Memory interferences result when analytes in a previous sample contribute to the signals measured in a new
sample. Memory effects can result from sample deposition in the uptake tubing or to the nebuliser and from
the build-up of sample material in the plasma torch and spray chamber. The occurrence memory effects
depend on the element and can be minimised by flushing the system with a rinse blank between samples. The
possibility of memory interferences should be recognised within an analytical run and suitable rinse times
should be used to reduce them. The rinse times necessary for a particular element shall be estimated prior to
analysis during method development.
5 Reagents
For the determination of elements at trace and ultra-trace level, the reagents shall be of adequate purity. The
concentration of the analyte or interfering substances in the reagents and the water should be negligible
compared to the lowest concentration to be determined.
5.1 Water, grade 2 as specified in EN ISO 3696 for all sample preparations and dilutions.
5.2 Nitric acid, HNO , ρ(HNO ) = 1,4g/ml, c(HNO ) = 15 mol/l, w(HNO ) = 650 g/kg.
3 3 3 3
5.3 Hydrochloric acid, HCl, ρ(HCl) = 1,18 g/ml, c(HCl) = 12 mol/l, w(HCl) = 370 g/kg.
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5.4 Single-element standard stock solutions
Ag, Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, Hg, In, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sb, Se, Si,
Sn, Sr, Te, Th, Ti, Tl, U, V, W, Zn, Zr, ρ(element) = 1 000 mg/l each.
Both single-element standard stock solutions and multi-element standard stock solutions with adequate
specification stating the acid used and the preparation technique are commercially available. Single-element
standard stock solutions can be made from high purity metals.
For stability of the solutions refer to manufacturer guarantee statement.
5.5 Multi-element standard stock solutions
5.5.1 General
Depending on the scope, different multi-element standard stock solutions may be necessary. In general, when
combining multi-element standard solutions, their chemical compatibility and the possible hydrolysis of the
components shall be regarded. Care shall be taken to prevent chemical reactions (e.g. precipitation).
The multi-element standard stock solutions are considered to be stable for several months if stored in the
dark. This does not apply to multi-element standard stock solutions that are prone to hydrolysis, in particular
solutions of Bi, Mo, Sn, Sb, Te, W, and Zr.
5.5.2 Multi-element standard stock solution A at the mg/l level may contain the following elements:
Ag, Al, As, B, Ba, Be, Bi, Cd, Co, Cr, Cu, Fe, Ga, Hg, In, Li, Mn, Ni, Pb, Se, Sr, Ti, Tl, U, V, Zn.
Use nitric acid (5.2) for stabilisation of multi-element standard stock solution A.
5.5.3 Multi-element standard stock solution B at the mg/l level may contain the following elements:
Mo, Sb, Si, Sn, W, Zr.
Use hydrochloric acid (5.3) for stabilisation of multi-element standard stock solution B.
Other elements of interest may be added to the standard stock solution, provided that the resulting multi-
element solution is stable.
5.5.4 Multi-element standard stock solution C at the mg/l level may contain the following elements:
Ca, Mg, Na, K, P, S.
Use nitric acid (5.2) for stabilisation of multi-element standard stock solution C.
5.6 Multi-element calibration solutions
Prepare in one or more steps calibration solutions at the highest concentration of interest. If more
concentration levels are needed, prepare those similarly in an equidistant concentration range.
Add acids (5.2 and/or 5.3) to match the acid concentration of samples closely.
If traceability of the values is not established, check the validity by comparison with a (traceable) independent
standard.
Check the stability of the calibration solutions.
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5.7 Internal standard solution
The choice of elements for the internal standard solution depends on the analytical problem. The internal
standards elements shall not be analytes and the concentrations of the selected elements should be negligibly
low in the digests of samples. The elements Sc, Y and Lu have been fo
...
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