EN ISO 22036:2024
(Main)Environmental solid matrices - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 22036:2024)
Environmental solid matrices - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 22036:2024)
This document specifies a method for the determination of the following elements in aqua regia, nitric acid or mixture of hydrochloric (HCl), nitric (HNO3) and tetrafluoroboric (HBF4)/hydrofluoric (HF) acid digests of soil, treated biowaste, waste, sludge and sediment:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gallium (Ga), gadolinium (Gd), 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), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum (Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr).
The method is also applicable to other extracts or digests originating from, for example, DTPA extraction, fusion methods or total digestion methods, provided the user has verified the applicability.
The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for other solid matrices and other elements as listed above, provided the user has verified the applicability.
This method is also applicable for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products (EN 17200[22]).
NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based products; plastics and rubbers; sealants and adhesives; paints and coatings.
Feste Umweltmatrizes - Bestimmung von Elementen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) (ISO 22036:2024)
Dieses Dokument legt ein Verfahren zur Bestimmung der folgenden Elemente in Königswasser, Salpetersäure oder einer Mischung aus Salzsäure (HCl), Salpetersäure (HNO3) und Tetrafluoroborsäure (HBF4)/Flusssäure (HF) in Aufschlüssen von Böden, behandelten Bioabfällen, Abfällen, Schlämmen und Sedimenten fest:
Aluminium (Al), Antimon (Sb), Arsen (As), Barium (Ba), Beryllium (Be), Bismut (Bi), Blei (Pb), Bor (B), Cadmium (Cd), Calcium (Ca), Cer (Ce), Chrom (Cr), Cobalt (Co), Eisen (Fe), Dysprosium (Dy), Erbium (Er), Europium (Eu), Gallium (Ga), Gadolinium (Gd), 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), Praseodym (Pr), Rhodium (Rh), Ruthenium (Ru), Quecksilber (Hg), Samarium (Sm), Scandium (Sc), Schwefel (S), Selen (Se), Silber (Ag), Silicium (Si), Strontium (Sr), Tantal (Ta), Tellur (Te), Terbium (Tb), Thallium (Tl),Thorium (Th), Thulium (Tm), Titan (Ti), Uran (U), Vanadium (V), Wolfram (W), Yttrium (Y), Ytterbium (Yb), Zink (Zn), Zinn (Sn) und Zirconium (Zr).
Dieses Verfahren ist auch für andere Extraktions- oder Aufschluss¬lösungen anwendbar, z. B. die DTPA-Extraktion (en: diethylenetriaminepentaacetic acid, Diethylentriamin¬pentaessigsäure), Lösungen, die mit einem Schmelzaufschlussverfahren oder mit einem Aufschlussverfahren zur Bestimmung von Element-Gesamtgehalten hergestellt wurden, sofern der Anwender die Anwendbarkeit überprüft hat.
Das Verfahren wurde für die in Tabelle A.1 (Schlämme), Tabelle A.2 (Kompost) und Tabelle A.3 (Böden) aufgeführten Elemente validiert. Das Verfahren ist für andere feste Matrices und andere als die oben aufgeführten Elemente anwendbar, sofern der Anwender die Anwendbarkeit überprüft hat.
Diese Methode ist auch für die Bestimmung von Haupt-, Neben- und Spurenelementen in Königswasser- und Salpetersäureaufschlüssen und in Eluaten von Bauprodukten anwendbar (EN 17200 [22]).
ANMERKUNG Bauprodukte umfassen z. B. Produkte auf Mineralbasis, bituminöse Produkte, Metalle, Produkte auf Holzbasis, Kunststoffe und Kautschuk, Dichtstoffe und Klebstoffe, Farben und Beschichtungen.
WARNUNG — Anwender dieses Dokuments sollten mit der üblichen Laborpraxis vertraut sein. Dieses Dokument gibt nicht vor, alle unter Umständen mit der Anwendung des Verfahrens verbundenen Sicherheitsaspekte anzusprechen. Es liegt in der Verantwortung des Anwenders, angemessene Sicherheits- und Schutzmaßnahmen zu treffen sowie die Einhaltung von nationalen Vorschriften sicherzustellen.
WICHTIG — Es ist unbedingt notwendig, dass Untersuchungen nach diesem Dokument von entsprechend ausgebildetem Personal durchgeführt werden.
Matrices solides environnementales - Dosage d’éléments par spectroscopie d’émission optique avec plasma induit par haute fréquence (ICP-OES) (ISO 22036:2024)
Le présent document spécifie une méthode de dosage des éléments suivants dans des digestats d’eau régale, d’acide nitrique ou de mélange d’acides chlorhydrique (HCl), nitrique (HNO3) et tétrafluoroborique (HBF4)/fluorhydrique (HF) de sols, de biodéchets traités, de déchets, de boues et de sédiment:
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), gallium (Ga), gadolinium (Gd), 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), praséodyme (Pr), rhodium (Rh), ruthénium (Ru), samarium (Sm), scandium (Sc), sélénium (Se), silicium (Si), argent (Ag), sodium (Na), strontium (Sr), soufre (S), tantale (Ta), tellure (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), étain (Sn), titane (Ti), tungstène (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) et zirconium (Zr).
Cette méthode s’applique également à d’autres extraits ou digestats issus, par exemple, de l’extraction au DTPA, de méthodes de fusion ou de méthodes de digestion totale, sous réserve que l’utilisateur ait vérifié l’applicabilité.
Cette méthode a été validée pour les éléments indiqués dans le Tableau A.1 (boues), le Tableau A.2 (compost) et le Tableau A.3 (sols). Elle est applicable à d’autres matrices solides et aux autres éléments énumérés ci-dessus, à condition que l’utilisateur ait vérifié l’applicabilité.
Cette méthode est également applicable au dosage des éléments majeurs, mineurs et à l’état de trace dans des digestats d’eau régale et d’acide nitrique ainsi que dans des éluats de produits de construction (EN 17200[22]).
NOTE Les produits de construction comprennent par exemple les produits minéraux; les produits bitumineux; les métaux; les produits ligneux; les matières plastiques et les caoutchoucs; les mastics et les adhésifs; les peintures et les revêtements.
Trdni matriksi v okolju - Določanje elementov z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/OES) (ISO 22036:2024)
ICS: 71.040.50, 13.080.10
Ta evropski standard določa metodo 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), živo srebro (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).
Metoda je bila potrjena za elemente v preglednici A.1. Metoda se uporablja za druge zgoraj navedene elemente, če uporabnik preveri uporabnost.
General Information
Relations
Overview
EN ISO 22036:2024 - "Environmental solid matrices - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES)" - is a CEN-endorsed international standard that specifies a validated ICP‑OES method for multi‑element determination in solid environmental matrices. The method covers soils, treated biowaste, waste, sludge and sediment, and is applicable to aqua regia, nitric acid or mixed acid (HCl/HNO3/HBF4/HF) digests. It is also applicable to other extract/digest types (e.g., DTPA extraction, fusion, total digestion) when the user verifies suitability, and to eluates of construction products (see EN 17200).
Key topics and technical requirements
- Scope and validated matrices: Validated for elements across a broad range (examples: Al, As, Cd, Cr, Cu, Fe, Ni, Pb, Zn, Hg and many rare earths and precious metals); specific validation data are provided for sludge, compost and soil (Annex A).
- Sample digestion: Describes acceptable digest/extract media (aqua regia, HNO3, HCl/HNO3/HBF4/HF) and requires user verification for alternative methods (DTPA, fusion, total digestion).
- ICP‑OES instrument setup: Requirements for instrument performance, optimization, wavelength selection, inter‑element correction and long‑term stability checks.
- Interferences and corrections: Treatment of spectral and non‑spectral interferences, with normative inter‑element correction procedures (Annex C).
- Calibration and quality control: Linear and standard‑addition calibration options, blank and calibration solutions, calibration checks, recovery and performance characteristics.
- Reporting and performance data: Calculation methods, expression of results, required test report content and reproducibility/repeatability data (Annex A); wavelengths and estimated detection limits in Annex B.
Practical applications and users
- Environmental and commercial laboratories performing elemental analysis of soils, sludges, sediments, treated biowaste and other solid wastes.
- Regulatory agencies and consultants conducting compliance monitoring, risk assessment and site characterization.
- Waste management, remediation projects, agricultural soil testing, and construction product testing laboratories analyzing eluates per EN 17200.
- Research groups and method developers validating alternative digestion/extraction approaches for ICP‑OES multi‑element analysis.
Related standards
- EN 17200 - eluates of construction products (method compatibility noted)
- ISO 22036:2008 / EN 16170:2016 - earlier editions superseded by this consolidated 2024 edition
- ISO/TC 190 (Soil quality) publications - complementary guidance for soil characterization
This standard is essential for laboratories seeking a harmonized, CEN-endorsed ICP‑OES procedure for reliable multi‑element determination in environmental solid matrices.
Standards Content (Sample)
SLOVENSKI STANDARD
01-junij-2024
Nadomešča:
SIST EN 16170:2017
SIST ISO 22036:2019
Trdni matriksi v okolju - Določanje elementov z optično emisijsko spektrometrijo z
induktivno sklopljeno plazmo (ICP/OES) (ISO 22036:2024)
Environmental solid matrices - Determination of elements using inductively coupled
plasma optical emission spectrometry (ICP-OES) (ISO 22036:2024)
Feste Umweltmatrizes - Bestimmung von Elementen mittels optischer
Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) (ISO 22036:2024)
Matrices solides environnementales - Dosage d’éléments par spectroscopie d’émission
optique avec plasma induit par haute fréquence (ICP-OES) (ISO 22036:2024)
Ta slovenski standard je istoveten z: EN ISO 22036:2024
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 22036
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2024
EUROPÄISCHE NORM
ICS 13.080.10 Supersedes EN 16170:2016
English Version
Environmental solid matrices - Determination of elements
using inductively coupled plasma optical emission
spectrometry (ICP-OES) (ISO 22036:2024)
Matrices solides environnementales - Dosage Feste Umweltmatrizes - Bestimmung von Elementen
d'éléments par spectroscopie d'émission optique avec mittels optischer Emissionsspektrometrie mit induktiv
plasma induit par haute fréquence (ICP-OES) (ISO gekoppeltem Plasma (ICP-OES) (ISO 22036:2024)
22036:2024)
This European Standard was approved by CEN on 2 January 2024.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22036:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 22036:2024) has been prepared by Technical Committee ISO/TC 190 "Soil
quality" in collaboration with Technical Committee CEN/TC 444 “Environmental characterization of
solid matrices” the secretariat of which is held by NEN.
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 July 2024, and conflicting national standards shall be
withdrawn at the latest by July 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 16170:2016.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
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, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 22036:2024 has been approved by CEN as EN ISO 22036:2024 without any modification.
International
Standard
ISO 22036
Second edition
Environmental solid matrices —
2024-01
Determination of elements using
inductively coupled plasma optical
emission spectrometry (ICP-OES)
Matrices solides environnementales — Dosage d’éléments par
spectroscopie d’émission optique avec plasma induit par haute
fréquence (ICP-OES)
Reference number
ISO 22036:2024(en) © ISO 2024
ISO 22036:2024(en)
© ISO 2024
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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Published in Switzerland
ii
ISO 22036:2024(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Interferences . 3
5.1 General .3
5.2 Spectral interferences .3
5.3 Non-spectral interferences .4
6 Reagents . 5
7 Apparatus . 7
8 Procedure . 8
8.1 Cleaning of glassware.8
8.2 Instrument performance parameters .8
8.3 Instrument optimization .9
8.4 Instrument set-up .9
8.4.1 General requirements .9
8.4.2 Software method development, wavelength selection .9
8.4.3 Inter-element correction .9
8.4.4 Reference element .9
8.4.5 Long-term stability .10
8.4.6 Preliminary instrument check .10
8.5 Calibration .10
8.5.1 Linear calibration function .10
8.5.2 Standard addition calibration .11
8.6 Solutions to be prepared . . .11
8.6.1 General .11
8.6.2 Blank calibration solution .11
8.6.3 Blank test solution .11
8.6.4 Calibration solutions .11
8.6.5 Test sample solutions . 12
8.6.6 Test solutions . 12
8.7 Measurement procedure . 12
9 Calculation .12
10 Expression of results .13
11 Performance characteristics .13
11.1 Calibration check . 13
11.2 Interference . 13
11.3 Recovery .14
11.4 Performance data .14
12 Test report . 14
Annex A (informative) Repeatability and reproducibility data .15
Annex B (informative) Wavelengths and estimated instrumental detection limits .21
Annex C (normative) Inter-element correction .27
Bibliography .29
iii
ISO 22036:2024(en)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
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The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
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This document was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
and physical characterization, in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 444, Environmental characterization of solid matrices, in accordance with the
Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
This second edition cancels and replaces the first edition (ISO 22036:2008), which has been technically
revised.
The main changes are as follows:
— the content of ISO 22036:2008 and EN 16170:2017 has been merged;
— the Scope has been widened to include treated biowaste, waste, sludge and sediment;
— the document has been developed parallel with CEN according to the Vienna Agreement;
— applicable digestion and extraction methods have been updated;
— the text has been editorially revised.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
ISO 22036:2024(en)
Introduction
This document is applicable and validated for several types of matrices as indicated in Table 1 (see Annex A
for the results of validation).
Table 1 — Matrices for which this International 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 Compost
Composted sludge
Soil Agricultural soil
Sludge amended soils
Waste City waste incineration fly ash ("oxidised" matrix)
City waste incineration bottom ash ("silicate" matrix)
Ink waste sludge (organic matrix)
Electronic industry sludge ("metallic" matrix)
BCR 146R (sewage sludge)
BCR 176 (city waste incineration ash)
Sediments ISE 859 (Sediment from de Bilt / Netherlands)
The choice of calibration method depends on the extractant and can be adapted to the extractant
concentration.
v
International Standard ISO 22036:2024(en)
Environmental solid matrices — Determination of elements
using inductively coupled plasma optical emission
spectrometry (ICP-OES)
WARNING — Persons using this document should be familiar with usual laboratory practice. This
document 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 document be carried
out by suitably trained staff.
1 Scope
This document specifies a method for the determination of the following elements in aqua regia, nitric acid
or mixture of hydrochloric (HCl), nitric (HNO ) and tetrafluoroboric (HBF )/hydrofluoric (HF) acid digests
3 4
of soil, treated biowaste, waste, sludge and sediment:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium
(Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er),
europium (Eu), gallium (Ga), gadolinium (Gd), 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), rhodium (Rh), ruthenium (Ru), samarium
(Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum
(Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten
(W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr).
The method is also applicable to other extracts or digests originating from, for example, DTPA extraction,
fusion methods or total digestion methods, provided the user has verified the applicability.
The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3
(soil). The method is applicable for other solid matrices and other elements as listed above, provided the
user has verified the applicability.
This method is also applicable for the determination of major, minor and trace elements in aqua regia and
[22]
nitric acid digests and in eluates of construction products (EN 17200 ).
NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based
products; plastics and rubbers; sealants and adhesives; paints and coatings.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
ISO 22036:2024(en)
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
blank calibration solution
solution prepared in the same way as the calibration solution (3.3) but leaving out the analytes
3.2
blank test solution
solution prepared in the same way as the test sample solution (3.10) but omitting the test portion
3.3
calibration solution
solution used to calibrate the instrument, prepared from stock solutions (3.8) by adding acids, buffer,
reference element and salts as needed
3.4
instrumental detection limit
lowest concentration that can be detected with a defined statistical probability using a clean instrument
and a clean solution
3.5
laboratory sample
sample intended for laboratory inspection or testing
[SOURCE: ISO 11074:2015, 4.3.7, modified — Notes to entry have been removed.]
3.6
linearity
straight-line relationship between the mean result of measurement and the quantity (concentration) of the
analyte
3.7
method detection limit
MDL
lowest concentration that can be detected using a specific analytical method with a defined statistical
probability for defined maximum matrix element concentrations
3.8
stock solution
solution with accurately known analyte concentration(s), prepared from pure chemicals
3.9
test sample
portion of material, resulting from the laboratory sample (3.5) by means of an appropriate method of sample
pretreatment, and having the size (volume/mass) necessary for the desired testing or analysis
[SOURCE: ISO 11074:2015, 4.3.16]
3.10
test sample solution
solution prepared after extraction or digestion of the test sample (3.9) according to appropriate specifications
4 Principle
Inductively coupled plasma optical emission spectrometry (ICP-OES) can be used to determine elements in
solution. The solution is dispersed by a suitable nebulizer; and the resulting aerosol is transported into the
plasma. In a radio-frequency inductively coupled plasma, the solvent is evaporated; the dried salts are then
vaporized, dissociated, atomized and ionized. The atoms or ions are excited thermally; and the number of
photons emitted during transition to a lower energy level are measured with optical emission spectrometry.
The spectra are dispersed by a grating spectrometer; and the intensities of the emission lines are monitored
by photosensitive devices. The identification of the element takes place by means of the wavelength of the
ISO 22036:2024(en)
radiation (energy of photons), while the concentration of the element is proportional to the intensity of the
radiation (number of photons). The ICP-OES method can be used to perform multi-element determinations
using an optical system.
Annex B shows examples of recommended wavelengths and detection limits for one particular instrument.
Data given are valid for a synthetical soil matrix (500 mg/l Al, Ca, Fe in 30 ml aqua regia filled up to 100 ml
with deionized water) with an optimized instrument. Using other instruments can lead to different detection
limits. Adoption of other wavelengths is possible.
This document refers specifically to the use of ICP-OES. Users of this document are advised to operate their
laboratories to accepted quality control procedures. Certified reference materials (CRM) should be used to
establish the amounts of the relevant elements in in-house reference materials. The latter can be used for
routine quality control of the procedures given in this document.
Results shall be established with control charts, for each element, within the laboratory. No result shall
be accepted which falls outside an agreed limit. Quality control procedures based on widely accepted
statistical techniques shall be used to establish such limits, that these are stable and that no long-term drift
is occurring. CRM should be used regularly to maintain the integrity of the in-house reference materials and,
thereby, the quality control system.
5 Interferences
5.1 General
The accurate and precise determination of trace element concentrations requires the correction of signal
contributions not caused by the analyte of interest (‘interferences’). Such interferences can result in both
lower and higher results and thus shall be accounted for during analytical method development. 5.2 and 5.3
characterize possible interferences in ICP-OES and discuss procedures to detect and remedy their influence
on the analytical result. Interferences are classified either as spectral or non-spectral.
5.2 Spectral interferences
Spectral interferences result in a change of the analyte instrumental signal, from a (partial) overlap of the
analyte emission by emission lines or spectra of other sample constituents (direct spectral interference,
inter-element or molecular (band) interference), by broad-band, continuous spectra, for example, from
recombination of sample constituents, or by spectrally overlapping signals resulting from stray light or
spectrally non-resolved molecular emissions.
Spectral interferences result in increased background signals that can obscure a weak analyte emission
line completely. Accordingly, using spectrally interfered analyte emission lines can reduce the analytical
capabilities and ultimately produce wrong results. Selecting a non-interfering analyte emission line, if
available, can normally reduce or avoid deleterious spectral interference effects.
Broad-band spectral background emissions and stray light can normally be accounted for by subtraction of
the background signal measured in immediate vicinity to the analyte emission line and extrapolated to the
analyte wavelength position (“off-peak” background correction).
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.
Such measurements also show if the background signal is best determined based on the interpolation of a
measurement on one side or on both sides of the analytical emission line or peak. The position selected for
the background-intensity measurement, on one or both sides of the analytical line, is determined by the
complexity of the spectrum adjacent to the analyte line. The position used should be as free as possible from
spectral interference, and should reflect the same change in background intensity as occurs at the analyte
wavelength measured.
For routine measurements, background measurement positions with no spectral off-peak interferences
(as e.g. inter-element or molecular band interferences) shall be chosen, ensuring that the background
ISO 22036:2024(en)
signal measured off-peak is not interfered and allows an accurate background signal determination from
its extrapolation to the analytical line wavelength position. If no interference-free off-peak background
measurement position can be found, a suitable correction shall be applied to allow background signal
determination from extrapolation of an off-peak background signal measurement.
Another possibility to avoid spectral interferences is the use of alternative emission wavelengths for the
analyte of interest, if available. Finally, a correction of spectral interferences can also be performed by
(typically multi-dimensional) mathematical spectral modelling approaches or (often iterative) correction
formulae accounting for inter-element effects. To achieve accurate results with systems employing inter-
element correction formulae, analyte and interfering elements shall be measured simultaneously. Spectral
interferences that remain undetected and uncorrected lead to wrong positive results for the interfered
analyte(s) in the sample under investigation. Table B.1 lists recommended and alternative wavelengths of
elements.
Modern ICP-OES systems are often equipped with multi-dimensional mathematical spectral modelling
algorithms pre-set by the manufacturer for interference correction. Such approaches typically do not
require the selection of dedicated wavelength positions for background signal measurements during
method development, but instead utilize complete wavelength regions around the analyte emission line
for modelling and correction. As with all interference correction techniques, the use of multi-dimensional
spectral modelling algorithms requires a careful verification of their effectiveness and of the resulting
accuracy, in the sample matrix of interest, to avoid wrong analytical results. This can, for example, be done
by analysing matrix-matched samples of known analyte concentration(s), advisably in the range expected
for the real samples or required from the analytical task at hand, e.g. the control of limiting values.
5.3 Non-spectral interferences
Apart from the spectral interferences described in 5.2, non-spectral interferences can also occur, reducing
the analytical accuracy and precision if undetected and uncorrected for. Non-spectral interferences can be
subdivided into physical, chemical and memory interferences.
Physical interferences are effects that occur in conjunction with sample transport and nebulization.
Differences in sample viscosity or surface tension can result in significant interference effects, especially
for samples with high concentrations of acids or dissolved solids. Physical interferences can be reduced
by sample dilution, by adjustment of acid concentrations among the samples, by matrix matching or using
suitable sample introduction equipment, e.g. ‘slurry nebulizers’ for samples with high TDS (total dissolved
solids). Physical interferences can be corrected for by the application of suitable reference element within
the analytical methodology.
The formation of molecular compounds, together with sample evaporation and ionization effects are all
examples of chemical interferences. Excluding the easily ionizable elements effect (EIEE) relevant under
axial plasma observation, chemical interferences typically do not occur significantly in ICP-OES techniques.
However, should chemical interferences still arise, they can normally be minimized by a careful choice of the
plasma parameters (e.g. RF power, observation height, nebulizer gas flow rate, ‘robust plasma’), by suitably
buffering the samples, by matrix-matching or by employing the method of standard additions. In general,
chemical interferences are highly dependent on the type of sample matrix and the analyte element(s) of
interest.
If large amounts of easily ionizable elements, for example, alkaline or earth-alkaline elements (I. and II.
Group of the periodic table), reach the ICP, the plasma ionization equilibrium, i.e. the ratio of neutral atom to
ion and electron number densities, can shift, resulting in a changed emission line excitation probability for
neutral or ionized analyte atoms. Ultimately, this results in different analyte signals for the same amount
of analyte in samples containing different amounts of easily ionizable elements. Especially for the easily
ionizable elements themselves, the EIEE leads to substantial calibration function non-linearities that can
result in significant analytical errors.
Since the EIEE is a plasma effect, its occurrence is independent from the plasma-viewing orientation
(radially of axially) employed. However, its effect on the analytical result is dependent on the plasma-viewing
orientation. For an axially viewed plasma, all processes along the analytical channel viewed contribute
to the analytical signal; accordingly, the EIEE influence on the measurement results is relevant and shall
be accounted and/or corrected for in any case. Possibilities to do so include the use of an ionization buffer
ISO 22036:2024(en)
(e.g. CsCl) added to all samples, or to employ radial plasma view for the elements affected. For radial view,
where only a small plasma region contributes to the measurement signal, the influence of the EIEE on the
analytical results can usually be ignored. However, radially viewing the plasma often also results in lower
measurement sensitivities. Accordingly, such trade-offs in figures of merit shall be accounted for during any
analytical method development.
Memory-Interferences (“memory effects”) occur when the analyte signals of the current sample are
influenced (usually resulting in positive deviations from the correct value) by the sample(s) measured before.
Memory effects can result from sample deposits or accumulation in pump tubing, nebulizer, spray chamber
or plasma torch. Occurrence of memory effects is element-specific and often can be reduced by rinsing the
complete system thoroughly with a suitable clean rinse solution before the introduction of a new sample.
Possible memory effects during analytical measurements shall be assessed and reduced, e.g. by an inter-
sample rinse with a clean rinse solution for an appropriate time. The required rinse time is element-specific
and shall be determined during method development, usually by defining a maximum tolerable background
signal resulting from samples measured before, for each analyte affected by memory interferences.
6 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.
-1
6.1 Water, with an electrical conductivity less than 0,1 mS m (equivalent to resistivity greater than
0,01 MΩ m at 25 °C). The water used should be obtained from a purification system that delivers ultrapure
water having a resistivity greater than 0,18 MΩ m (usually expressed by manufacturers of water purification
systems as 18 MΩ cm). For all sample preparations and dilutions.
6.2 Nitric acid, HNO , e.g. ρ(HNO ) = 1,4 g/ml, c(HNO ) ≈ 15 mol/l, w(HNO ) ≈ 65 % (m/m) to 70 % (m/m).
3 3 3 3
6.3 Hydrochloric acid, HCl, e.g. ρ(HCl) = 1,18 g/ml, c(HCl) ≈ 12 mol/l, w(HCl) ≈ 32 % (m/m) to 37 %
(m/m).
6.4 Tetrafluoroboric acid (HBF ), c(HBF4) ≈ 6 mol/l, w(HBF ) ≈ 38 % (m/m) to 48 % (m/m).
4 4
6.5 Hydrofluoric acid (HF), c(HF) ≈ 23 mol/l, w(HF) ≈ 40 % (m/m) to 45 % (m/m).
6.6 Boric acid (B(OH) ), solid.
NOTE Boric acid can be used to mask the fluoride ions. However, there is a risk of incorrect analysis results due to
contaminated boric acid.
6.7 Boric acid (B(OH) ) solution, e.g. 4 % (m/m) solution
Dissolve 40 g of boric acid (6.6) in 1 l of water (6.1).
6.8 Single element standard stock solutions
For example, Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Ho, Hg, In, Ir, K, La,
Li, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pd, Pr, Pt, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Th, Tm, Ti, Tl, V, W,
Y, Yb, 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 the manufacturer guarantee statement.
ISO 22036:2024(en)
6.9 Multi-element standard stock solutions
6.9.1 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.
6.9.2 Multi-element standard stock solution A
This solution at the mg/l level can contain the following elements:
Al, As, B, Ba, Be, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Li, Mn, Ni, Pb, Se, Sr, Te, Tl, U, V, Zn.
Use nitric acid (6.2) for stabilisation of multi-element standard stock solution A.
6.9.3 Multi-element standard stock solution B
This solution at the mg/l level can contain the following elements:
Ge, Mo, Sb, Si, Sn, Ti, W, Zr, P, S.
Use hydrochloric acid (6.3) for stabilisation of multi-element standard stock solution B.
Other elements of interest can be added to the standard stock solution, provided that the resulting multi-
element solution is stable.
6.9.4 Multi-element standard stock solution C
This solution at the mg/l level can contain the following elements:
Ca, Mg, Na, K
Use nitric acid (6.2) for stabilisation of multi-element standard stock solution C.
6.9.5 Multi-element standard stock solution D
This solution at the mg/l level can contain the following elements:
Ce, Dy, Er, Eu, Gd, Ho, La, Nd, Pr, Sc, Sm, Tb, Tm, Th, Yb.
Use nitric acid (6.2) for stabilisation of multi-element standard stock solution D.
6.9.6 Multi-element standard stock solution E
This solution at the mg/l level can contain the following elements:
Au, Ir, Pd, Pt, Rh, Ru.
Use hydrochloric acid (6.3) for stabilisation of multi-element standard stock solution E.
6.10 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.
ISO 22036:2024(en)
Add acids (6.2 or 6.3 or a mixture of 6.2, 6.3, 6.4, 6.5 and 6.7) 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.
The stability of calibration solution can be checked by comparison with freshly prepared solutions on a
regular basis.
Care should be taken when preparing the mixed standards to ensure that the elements are compatible and
stable together. Other elements combinations are also possible and depend on the analytical task. To avoid
cross-contamination, only pure chemicals should be used. The diluted solutions should be stored in clean
PFA-, FEP-fluorocarbon, HDPE or PP bottles.
Applying digestion with aqua regia or nitric acid to sludge, treated biowaste or soil, ubiquitous elements like
Al, Na, K, Ca, Mg, Ti and Fe can be co-extracted resulting in concentrations of several hundreds of mg/l. The
efficiency of the method selected to compensate spectral interferences, background subtraction, transport
interference shall be checked by analysis of control samples and interference control samples. Otherwise,
the sample matrix elements shall be adapted in calibration solutions for each batch of sample types.
Alternatively, the standard addition method shall be used.
6.11 Reference element solution
The choice of elements for the reference element (synonymously called internal standard) solution depends
on the analytical problem. The reference elements shall not be analytes; and the concentrations of the
selected elements should be negligibly low in the digests of samples. The elements Y, Rh and Lu have been
found suitable for this purpose.
Generally, a suitable concentration of the reference element in samples and calibration solutions is 1 mg/l to
10 mg/l.
6.12 Calibration check solution
Prepare the calibration check solution using an independent multi-element standard stock solution, adapted
to the same acid concentrations at an upper concentration level.
6.13 Interference check solution
If interferences cannot be excluded, prepare an interference check solution to detect the interference, with
known concentrations of interfering elements. The choice of the concentration and interfering element are
matrix dependent.
Avoid two or more interferents for an analyte in the same interference check solution. Spike the sample with
the analytes of interest, particularly those with known interferences at 0,5 mg/l to 1 mg/l. In the absence
of measurable analyte, overcorrection can go undetected because a negative value can be reported as zero.
If the particular instrument displays overcorrection as a negative number, this spiking procedure is not
necessary.
This interference check should be made once at installation of a new instrument.
7 Apparatus
7.1 Inductively coupled argon plasma emission spectrometer
The ICP atomic emission spectrometer consi
...
Frequently Asked Questions
EN ISO 22036:2024 is a standard published by the European Committee for Standardization (CEN). Its full title is "Environmental solid matrices - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 22036:2024)". This standard covers: This document specifies a method for the determination of the following elements in aqua regia, nitric acid or mixture of hydrochloric (HCl), nitric (HNO3) and tetrafluoroboric (HBF4)/hydrofluoric (HF) acid digests of soil, treated biowaste, waste, sludge and sediment: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gallium (Ga), gadolinium (Gd), 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), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum (Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr). The method is also applicable to other extracts or digests originating from, for example, DTPA extraction, fusion methods or total digestion methods, provided the user has verified the applicability. The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for other solid matrices and other elements as listed above, provided the user has verified the applicability. This method is also applicable for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products (EN 17200[22]). NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based products; plastics and rubbers; sealants and adhesives; paints and coatings.
This document specifies a method for the determination of the following elements in aqua regia, nitric acid or mixture of hydrochloric (HCl), nitric (HNO3) and tetrafluoroboric (HBF4)/hydrofluoric (HF) acid digests of soil, treated biowaste, waste, sludge and sediment: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gallium (Ga), gadolinium (Gd), 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), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum (Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr). The method is also applicable to other extracts or digests originating from, for example, DTPA extraction, fusion methods or total digestion methods, provided the user has verified the applicability. The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for other solid matrices and other elements as listed above, provided the user has verified the applicability. This method is also applicable for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products (EN 17200[22]). NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based products; plastics and rubbers; sealants and adhesives; paints and coatings.
EN ISO 22036:2024 is classified under the following ICS (International Classification for Standards) categories: 13.080.10 - Chemical characteristics of soils. The ICS classification helps identify the subject area and facilitates finding related standards.
EN ISO 22036:2024 has the following relationships with other standards: It is inter standard links to EN 16170:2016. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
You can purchase EN ISO 22036:2024 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of CEN standards.








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