prEN ISO 22036
(Main)Soil, treated biowaste and sludge - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO/DIS 22036:2022)
Soil, treated biowaste and sludge - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO/DIS 22036:2022)
This European Standard 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).
The method has been validated for the elements given in Table A.1. The method is applicable for the other elements listed above, provided the user has verified the applicability.
Boden, behandelter Bioabfall und Schlamm– Bestimmung von Elementen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) (ISO/DIS 22036:2022)
Sols, bio-déchets traités et boues - Dosage d’éléments par spectroscopie d’émission optique avec plasma induit par haute fréquence (ICP-OES) (ISO/DIS 22036:2022)
Tla, obdelani biološki odpadki in blato - Določevanje elementov z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/OES) (ISO/DIS 22036:2022)
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN ISO 22036:2022
01-julij-2022
Tla, obdelani biološki odpadki in blato - Določevanje elementov z optično
emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/OES) (ISO/DIS
22036:2022)
Soil, treated biowaste and sludge - Determination of elements using inductively coupled
plasma optical emission spectrometry (ICP-OES) (ISO/DIS 22036:2022)
Boden, behandelter Bioabfall und Schlamm– Bestimmung von Elementen mittels
optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) (ISO/DIS
22036:2022)
Sols, bio-déchets traités et boues - Dosage d’éléments par spectroscopie d’émission
optique avec plasma induit par haute fréquence (ICP-OES) (ISO/DIS 22036:2022)
Ta slovenski standard je istoveten z: prEN ISO 22036
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
oSIST prEN ISO 22036:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 22036:2022
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oSIST prEN ISO 22036:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 22036
ISO/TC 190/SC 3 Secretariat: DIN
Voting begins on: Voting terminates on:
2022-06-14 2022-09-06
Soil, treated biowaste and sludge — Determination
of elements using inductively coupled plasma optical
emission spectrometry (ICP-OES)
ICS: 13.080.10
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 22036:2022(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2022
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oSIST prEN ISO 22036:2022
ISO/DIS 22036:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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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 Spectral interferences . 3
5.2 Non-spectral interferences . . 4
6 Reagents . 5
7 Instrumentation . 7
8 Procedure .8
8.1 Cleaning of glassware. 8
8.2 Instrument performance parameters . 8
8.3 Instrument optimization . 8
8.4 Instrument set-up . 8
8.4.1 General requirements . 8
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 . 9
8.4.6 Preliminary instrument check . 9
8.5 Calibration . 10
8.5.1 Linear calibration function . 10
8.5.2 Standard addition calibration . 10
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 . 11
8.6.6 Test solutions . 11
8.7 Measurement procedure . 11
9 Calculation .12
10 Expression of results .13
11 Performance characteristics .13
11.1 Calibration check .13
11.2 Interference . 13
11.3 Recovery . 13
11.4 Performance data .13
12 Test report .14
Annex A (informative) Repeatability and reproducibility data .15
Annex B (informative) Wavelengths and estimated instrumental detection limits .20
Annex C (informative) Inter-element correction .27
Bibliography .29
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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 ISO technical committees. Each member body interested in a subject for which a technical
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
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 documents 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).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
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www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3,
Chemical and physical characterization.
This document will supersede EN 16170:2017 and ISO 22036:2008.
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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
Biowaste Compost
Soil Soil
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oSIST prEN ISO 22036:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 22036:2022(E)
Soil, treated biowaste and sludge — 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 digest or extraction
solutions of soil, treated biowaste and sludge:
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), gallium (Ga), indium
(In), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg),
molybdenum (Mo), neodymium (Nd), nickel (Ni), phosphorus (P), potassium (K), praseodymium (Pr),
samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur
(S), tellurium (Te), thallium (Tl), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), zinc
(Zn) and zirconium (Zr).
This multi-element determination method is applicable to extracts obtained with nitric acid or aqua
regia. The method is also applicable for other extracts or digests originating from e.g. DTPA extraction,
[1-8]
fusion methods or total digestion methods, provided the user has verified the applicability .
The choice of calibration method depends on the extractant and can be adapted to the extractant
concentration.
The method has been validated for the elements given in Annex A. The method is applicable for the
other elements listed above, provided the user has verified the applicability.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 11074, Soil quality — Vocabulary
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
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3.1
blank calibration solution
solution prepared in the same way as the calibration solution but leaving out the analytes
3.2
blank test solution
solution prepared in the same way as the test sample solution but omitting the test portion
3.3
calibration solution
solution used to calibrate the instrument, prepared from stock solutions by adding acids, buffer,
reference element and salts as needed
3.4
instrument 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: EN ISO 11074:2015, 4.3.7]
3.6
linearity
straight-line relationship between the mean result of measurement and the quantity (concentration) of
the analyte
3.7
method detection limit
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 (6.4)
3.9
test sample
portion of material, resulting from the laboratory sample by means of an appropriate method of sample
pretreatment, and having the size (volume/mass) necessary for the desired testing or analysis
[SOURCE: EN ISO 11074:2015, 4.3.16]
3.10
test sample solution
solution prepared after extraction or digestion of the test sample 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 radiation (energy of photons), while the concentration of the element is
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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.
Table B.1 in 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 International Standard refers specifically to the use of ICP-OES. Users of this International
Standard 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
International Standard.
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. Certified Reference Materials should be used regularly to maintain the integrity of
the in-house reference materials and, thereby, the quality control system.
5 Interferences
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 have to be accounted for during analytical method
development. The following paragraphs characterize possible interferences in ICP-OES and discuss
procedures to detect and remedy their influence on the analytical result. Interferences are classified
either as non-spectral or spectral.
5.1 Spectral interferences
Spectral interferences often synonymously called matrix effects. Spectral interferences result in
a change of the analyte 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, e.g. 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 even 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. The alternative choice of a non-interfered
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). Additionally, measurements of
the sample spectrum and comparison to single element spectra in the relevant wavelength regions can
often indicate if alternative analyte emission lines might be better suited in the sample matrix at hand,
due to lesser or no spectral interference at the alternative wavelength position.
Such measurements also show if the background signal is best determined based on the interpolation of
a measurement on one side of the analytical emission line, or by interpolating the signal determined at
two background locations, on either side of the analytical peak. Therefore, the wavelength position(s)
or region(s) chosen for background signal determination in an analytical method is/are ultimately
determined by the structure and complexity of the sample emission spectrum in the vicinity of the
analytical emission line.
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For routine measurements, background measurement positions with no spectral off-peak interferences
(as e.g. inter-element or molecular band interferences) have to be chosen, ensuring that the background
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 has to 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 effected
by (typically multi-dimensional) mathematical spectral modelling approaches or (often iterative)
correction equations accounting for inter-element effects. To achieve accurate results with systems
employing inter-element correction equations, analyte and interfering elements have to 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
wavelengths of elements and common spectral interferences could be identified.
Modern ICP-OES systems are often equipped with manufacturer pre-set multi-dimensional
mathematical spectral modelling algorithms 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, also 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 e.g. be done by analyzing 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.
5.2 Non-spectral interferences
Apart from the spectral interferences described before, also non-spectral interferences can 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 by
the use of suitable sample introduction equipment, e.g. ‘slurry nebulizers’ for samples with high TDS.
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’, etc.), 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.
Easily Ionizable Elements Effect (EIEE): If large amounts of easily ionizable elements, e.g. 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.
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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 plasma-viewing orientation
dependent. 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 has
to be accounted and/or corr
...
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