ISO/FDIS 13196

FINAL DRAFT
International
Standard
ISO/TC 190/SC 3
Soil quality — Screening soils
Secretariat: DIN
for selected elements by energy-
Voting begins on:
dispersive X-ray fluorescence
2026-03-11
spectrometry using a handheld or
Voting terminates on:
portable instrument
2026-05-06
Qualité du sol — Diagnostic rapide d’une sélection d’éléments
dans les sols à l’aide d’un spectromètre de fluorescence X à
dispersion d’énergie de type mobile ou pistolet
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
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IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
ISO/CEN PARALLEL PROCESSING LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
FINAL DRAFT
International
Standard
ISO/TC 190/SC 3
Soil quality — Screening soils
Secretariat: DIN
for selected elements by energy-
Voting begins on:
dispersive X-ray fluorescence
spectrometry using a handheld or
Voting terminates on:
portable instrument
Qualité du sol — Diagnostic rapide d’une sélection d’éléments
dans les sols à l’aide d’un spectromètre de fluorescence X à
dispersion d’énergie de type mobile ou pistolet
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 SUPPOR TING DOCUMENTATION.
© ISO 2026
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
ISO/CEN PARALLEL PROCESSING
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
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TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
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MADE IN NATIONAL REGULATIONS.
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Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 4
5 Apparatus . 4
5.1 XRF spectrometer .4
5.2 Container for sampling and preparation .4
5.3 Sampling equipment .5
5.4 Sieve .5
5.5 Sample cup for portable XRF spectrometers .5
5.6 Sample container for handheld XRF spectrometers .5
5.7 Drying device (optional) .5
6 Procedure . 6
6.1 General .6
6.2 Performance check of instrument .6
6.3 Calibration .6
6.4 Preparation in advance of site investigation .7
6.5 In-situ measurement (including strictly in-situ measurement) .7
6.5.1 Secure working area .7
6.5.2 Preparation of the measuring spot .7
6.5.3 Surface or spot measurement .7
6.6 Post-sampling measurement.8
6.6.1 Preparation of samples .8
6.6.2 Sample measurement and calculation .9
7 Specific applications: site-specific performance . 9
8 Quality assurance and control . 10
8.1 General .10
8.2 Performance test .10
8.2.1 XRF spectrometer performance .10
8.2.2 Test certified reference materials .10
8.3 XRF spectrometer energy calibration .11
8.4 Complementary analysis/validation for quantitative results .11
9 Test report .11
Annex A (informative) Conclusion of the interlaboratory trial .13
Annex B (informative) Energy dispersive X-ray fluorescence spectrometry (ED-XRF)
measurement usefulness .21
Bibliography .22

iii
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 committee
has been established has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work. 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).
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)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO’s adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see 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, 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 13196:2013), which has been technically
revised.
The main changes are as follows:
— the details of measurement options have been made clearer;
— suitable materials for the equipment for sampling and sample preparation are indicated;
— more information is provided for users of this document on requirements for:
— sieve;
— sample cup;
— basic operation of XRF spectrometers;
— safety instructions;
— sample preparation.
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
Introduction
X-ray fluorescence spectrometry (XRF) using battery or active source-powered handheld or portable
equipment is a quick method for the determination of total elemental compositions of soil samples. Unlike
laboratory analyses by inductively coupled plasma optical emission spectroscopy (ICP-OES) and atomic
absorption spectroscopy (AAS), XRF needs no digestion step to prepare a test solution to be analysed.
Consequently, handheld or portable equipment of energy dispersive XRF (ED-XRF) is suitable for the rapid
on-site determination of selected elements, mainly heavy metals, in screening processes. When performing
analyses at a site, it can be important to have information on the presence of an element (qualitative
analysis) and also to obtain results from semi-quantitative analysis. Typical elements that can be detected
and measured are Cr, As, Se, Cd, Hg and Pb, depending on the instrument (the elements validated for XRF
detection and measurement are listed in Note 3 in Clause 1). In these situations, factory pre-set calibrations
are used. For quantitative results, complementary analysis by alternative means is needed.
An ED-XRF exercise can comprise a single determination at one location, in accordance with the guidance in
this document, several determinations, or a large number of determinations.
Where XRF analysers are being used to assess concentrations of soil contaminants which are harmful
to humans or the environment, or both, there can be applicable national regulations with frameworks of
standards, guidance and codes of practice for such investigations.
This document does not aim to provide a strategy, tactics or methodology for environmental investigations,
or human health assessments of potentially contaminated land or soil, nor does it provide any such strategies
for the assessment of mineral resources.
Adherence to this document does not demonstrate compliance with any national contaminated land
investigation regulations.
v
FINAL DRAFT International Standard ISO/FDIS 13196:2026(en)
Soil quality — Screening soils for selected elements by
energy-dispersive X-ray fluorescence spectrometry using a
handheld or portable instrument
WARNING — Soil samples can contain toxic contaminants. Avoid direct contact of soil samples with
exposed parts of the body. Appropriate measures shall be taken to avoid ingestion and inhalation.
Exposure to X-rays can give rise to radiation damage throughout the body as well an increased risk
of cancer. XRF spectrometers are usually required to comply with national regulations. Those using,
managing or supervising the use of such equipment are usually required to be qualified to do so in
accordance with national regulations.
The XRF spectrometer to be used in accordance with this document shall employ a fail-safe
function to prevent the operator and the public from inadvertent exposure to the X-ray beams. XRF
users should engage a radiation protection officer to look at their proposed activity with the XRF
spectrometer and provide informed advice on the safety implications of those proposals.
For in-situ (including strictly in-situ) analysis, a safe working area or controlled area should be
established by signs and barriers, if necessary, in order to ensure bystanders are kept at a safe
distance.
1 Scope
This document specifies the procedure for screening soils for selected elements using handheld or portable
equipment for energy dispersive X-ray fluorescence spectrometry (ED-XRF). It covers the application of this
screening method to obtain qualitative or semi-quantitative data to assist decisions on a sampling strategy
for detailed assessment of soil quality employing laboratory analytical chemical methods.
NOTE 1 Screening methods generally provide qualitative or semi-quantitative concentration values that are
indicative of concentration values, although occasionally they can give quantitative results under specific or limited
conditions.
NOTE 2 The greater the effort applied to the pretreatment of soil samples, the better the analytical results that can
be expected (see e.g. Reference [19]).
This document does not explicitly specify elements for which it is applicable, since the applicability depends
on the performance of the apparatus and the objective of the screening. The elements which can be
determined are limited by the performance of the instrument used, the concentrations of particular elements
present in the soil, and the requirements of the investigation in terms of the minimum concentrations of
concern (e.g. guideline value).
NOTE 3 The XRF measurements of As, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Sb, Sn, V and Zn were validated as described in
Annex A.
NOTE 4 Annex B provides examples of when screening with a handheld ED-XRF spectrometer and a portable ED-
XRF spectrometer can be useful.
This document does not provide guidance on how to use the equipment to provide quantitative data for use
in detailed site assessments. This document does not cover how the results of multiple determinations are
synthesized to address the objectives of an ED-XRF determination.

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.
ISO 12404, Soil and waste — Guidance on the selection and application of screening methods
IEC 62495, Nuclear instrumentation — Portable X-ray fluorescence analysis equipment utilizing a miniature
X-ray tube
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
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
X-ray fluorescence spectrometer
XRF spectrometer
spectrometer to observe X-ray fluorescence emitted from elements for analysis
Note 1 to entry: In this document, X-ray fluorescence spectrometer (XRF spectrometer) means energy dispersive
X-ray fluorescence spectrometer (ED-XRF spectrometer).
3.2
handheld XRF spectrometer
XRF spectrometer (3.1) which can be used for in-situ analysis (e.g. strictly in-situ measurement (3.11), in-situ
measurement (3.12)) by handheld operation
Note 1 to entry: Handheld XRF spectrometers are applicable to both in-situ measurements (including strictly in-
situ measurements) and measurements with sampling or post-sampling measurements (3.13) where post-sampling
measurement means application of determination methods including XRF to samples which are collected and pre-
treated, if needed, at a site or in a laboratory.
Note 2 to entry: When applying an XRF spectrometer to samples at a spot just after collecting them from the ground
thereat, the operation is still in-situ measurement.
3.3
portable XRF spectrometer
XRF spectrometer for samples taken out of a spot at a site, which can be transported to the site
Note 1 to entry: Portable XRF spectrometers are applicable to in-situ measurements (3.12) and to post-sampling
measurements (3.13).
Note 2 to entry: Handheld XRF spectrometers (3.2) can be used at the bench top. However, the device works for
handheld operation as designated in 3.2.
3.4
fundamental parameter approach
method to obtain element composition through successive approximation of the theoretical X-ray
fluorescence intensities to the measured X-ray fluorescence intensities
Note 1 to entry: The calculation of the theoretical X-ray fluorescence intensities is carried out based on assumed
element composition, theoretical parameters and pre-determined sensitivity coefficients of the XRF spectrometer.

3.5
screening
application of any analytical semi-quantitative (3.8) method for exploratory analysis
[SOURCE: ISO 12404:2021, 3.1]
3.6
screening method
method which is used (often on site) to quickly explore a given area including target parameter distribution
or to test a set of samples and obtain data on sample characteristics
Note 1 to entry: It is not necessarily directly comparable with reference methods (3.7).
[SOURCE: ISO 12404:2021, 3.2]
3.7
reference method
method which is performed in accordance with national or international standards
[SOURCE: ISO 12404:2021, 3.3]
3.8
semi-quantitative
approximate and comparative rather than absolutely quantitative
3.9
semi-quantitative analysis
data analysis method that provides approximate and comparative measurements rather than absolute
quantification within a single experiment
Note 1 to entry: It combines elements of qualitative and quantitative analysis, allowing for the interpretation
of numerical values that reflect the degree or extent of a particular characteristic within a sample. Unlike fully
quantitative methods, which yield results that can be directly compared across different experiments, semi-
quantitative (3.8) methods provide information that is meaningful primarily within the context of a single experiment
or study.
3.10
qualitative analysis
data analysis method that focuses on detecting or identifying constituent elements without providing
specific concentrations
3.11
strictly in-situ measurement
directly observing the ground surface with a handheld device
3.12
in-situ measurement
observing at the sampling location samples collected from the ground, with a handheld or portable device
3.13
post-sampling measurement
observing, with a handheld or portable device, samples which are collected from the ground and then taken
to another place (e.g. sampling stations or laboratories) after collection
Note 1 to entry: On-site measurement includes strictly in-situ measurements (3.11) and in-situ measurements (3.12) as
well as post-sampling measurement when the measurement is carried out at the site but at a place different from the
sample collection spot after collection (e.g. sampling stations at a site).
Note 2 to entry: As strictly in-situ and in-situ measurements are carried out applying an XRF device to the surface of a
target ground spot and to a sample collected therefrom immediately after collection, they are in other words surface
measurement and spot measurement, respectively.

3.14
certified reference material
CRM
reference material (RM) characterized by a metrologically valid procedure for one or more specified
properties, accompanied by an RM certificate that provides the value for the specified property, its
associated uncertainty and a statement of metrological traceability
[SOURCE: ISO 17034:2016, 3.2, modified — Notes 1 to 4 to entry were removed.]
4 Principle
The concentrations of selected elements in soil are determined using a handheld or portable XRF
spectrometer in the field. Element concentrations are measured after sampling and limited pretreatment
(in-situ measurement), or directly in-situ (strictly in-situ measurement).
Whilst use of a handheld or portable ED-XRF spectrometer lends itself to making determinations at ad-
hoc locations based on on-site observations, it should be used in a structured way commensurate with the
intended purpose of the study for which it is being used.
NOTE 1 Guidance on sampling strategies in various contexts is provided in ISO 18400-104, ISO 18400-203 and
ISO 18400-205.
The test locations should be recorded together with background information such as site-observations and
photographs taken as necessary. The use of GPS to accurately record locations can be particularly useful
when test locations are selected on an ad-hoc basis rather than based on a predetermined plan.
The procedure described in this document, to screen soils for selected elements using handheld or portable
ED-XRF devices, gives semi-quantitative results. When desiring to know the relationship between the results
obtained and those from laboratory reference methods, compare them carefully selecting the alternative
laboratory methods bearing in mind their particular performance characteristics (see 8.2.2, Notes 1 and 2)
and recognize that any method (e.g. screening and laboratory reference methods) has errors originating
from its specific sampling and analytical principles (see 7.1 and 8.4).
NOTE 2 Examples of situations when screening with a handheld or portable ED-XRF spectrometer can be useful are
provided in Annex B.
5 Apparatus
5.1 XRF spectrometer
An appropriate battery or active source-powered handheld or portable ED-XRF device. Typical ED-XRF
devices are described in References [20] and [21].
Instruments shall have sufficient energy and depth penetration as well as suitable beam width to work
for use in soil matrices and to achieve suitable detection limits. These details are available from the
manufacturer or supplier.
A security system for the spectrometer shall be installed as designated in IEC 62495 where only the
permitted operators and supervisors of the spectrometer can activate it with a password given by the
supervisors. Automatic X-ray irradiation block mechanisms shall also work when no samples are found by
the spectrometer or human bodies are detected by an IR sensor fitted to the XRF device.
5.2 Container for sampling and preparation
A tray that can accommodate a sufficient amount of soil sample for the XRF measurement.
The tray should be of a suitable material, the wear of which will not introduce into the sample metal grains or
grains of coloured plastics which can contain metallic pigments. When it is decided to crush any aggregates
or to disaggregate lumps of soil, a mortar with a pestle made of a ceramic or other solid inert material such

as agate or chalcedony should be used. The XRF spectrometer can be used to test trays as well as mortars
and pestles for metals which can interfere with XRF.
5.3 Sampling equipment
Sampling equipment (such as sampling spoons, trowels, picks, spades, or post-hole spades) used to prepare
for sampling (e.g. at in-situ measurement locations) and to take samples should be in good conditions and
shall not contaminate the sample.
Use of stainless steel tools can be appropriate given the tiny amounts of a hard tool that can be introduced
into the soil during sampling. Where the slightest interference from the wear of sampling equipment is
possible, plastic trowels and spoons should be used. When carrying out in-situ tests on machine excavated
exposures, the use of steel digger buckets or bulldozer blades is unavoidable in the absence of plastic buckets
and blades for such machinery.
NOTE 1 Painted or zinc- or chrome-plated tools can introduce flakes of metals or paints with metallic pigments that
can influence sample analysis by XRF which is carried out by on-site and post-sampling measurements.
NOTE 2 Further guidance on the recovery of samples for chemical analysis is given in ISO 18400-102.
5.4 Sieve
A sieve of size 2 mm, for example as described in ISO 3310-1. Clean the sieve between samples.
The procedure described in this document is only validated for material passing a 2 mm sieve. The user may
choose to use a different sieve size (sieves are available with apertures less than, and greater than, 2 mm)
but the results obtained could be different from those obtained when using a 2 mm size sieve.
NOTE Reasons for choosing a smaller sieve size might be to obtain results likely to be more relevant to the
potential for inhalation, ingestion, or contact with contaminated material.
Where the slightest interference from the wear of the sieves is possible, the use of plastic sieves should be
considered. The sieves themselves can be tested with the XRF spectrometer to ensure that any potential
contamination of samples can be assessed properly.
5.5 Sample cup for portable XRF spectrometers
A plastic cup, which is suitable for the XRF spectrometer to be used, having a window at its bottom made of
polypropylene, polyethylene terephthalate or graphene. Alternatively, a plastic bag (e.g. clear polyethylene
one) can be used. The concentration of target elements in the cup or plastic bag material should be negligible.
This should be checked by testing stacks of cups or bags using the XRF spectrometer to confirm that only
‘light elements’ are detectable or that no elements are detected.
5.6 Sample container for handheld XRF spectrometers
Plastic containers or bags suitable for simple sample pretreatment and in-situ XRF measurement (for strictly
in-situ measurement, they are not used). The concentration of target elements in the container or bag should
be negligible. This can be confirmed by testing stacks of cups or bags using the XRF spectrometer.
5.7 Drying device (optional)
A portable electric drying oven, hot plate or similar powered by batteries, or a portable generator, or a heater
driven by exothermic chemical reactions, e.g. hydration of calcium oxide.

6 Procedure
6.1 General
Three measuring ways are available for analysis using XRF spectrometers, namely strictly in-situ, in-situ and
post-sampling measurements (where strictly in-situ and in-situ measurements are on-site measurements).
Note 1 to entry 3.13 explains the meaning of on-site measurement. As Note 2 to entry 3.13 mentions, strictly
in-situ and in-situ measurements can be said to be surface and spot measurements from the viewpoint
of operation characteristics. Handheld and portable XRF spectrometers can be used depending on the
measurement method used. See 6.5 for the procedures for strictly in-situ and in-situ measurements and 6.6
for post-sampling measurement.
Handheld XRF spectrometers can be used for strictly in-situ soil measurements as described in 6.5 or to make
measurements on soil samples extracted from the site, as described in 6.6 (post-sampling measurement),
subjected to appropriate pretreatment (e.g. sieving to obtain particles smaller than 2 mm). Portable XRF
spectrometers can be used for in-situ and post-sampling measurements.
If more highly quantitative results are needed, samples should be homogenized (see EN 15309) and
complementary analysis should be carried out using other quantitative methods, to confirm the performance
of the portable or handheld XRF spectrometer (see 8.4).
The parameters to be determined should be defined before starting calibration and measurements. It should
be checked that the concentrations of each element to be determined, which is thought likely or possibly
to be present, are within the working range of the instrument. Follow the manufacturer’s instructions and
perform tests with certified reference materials to calibrate the instrument.
Test duration should be determined by the time taken until error values fall stable for each element. This is
usually displayed by the analyser against each element and falls with time as the XRF test progresses. Once
this value has stopped falling or stabilised, for the element or elements under consideration, the test may be
ended.
The concepts and goals of screening measurement in this document shall be as designated in ISO 12404. For
sampling processes and pretreatment procedures, see e.g. ISO 18400-201 and ISO 11464.
When a portable XRF spectrometer is used, a work station should be established along the lines of the one
described in ISO 18400-301 so that the instrument and personnel have a sheltered working environment.
6.2 Performance check of instrument
Before analysis, follow the instrument manufacturer’s instructions for setup, conditioning, preparation and
maintenance. The performance control of the instrument should be carried out at least once a day to ensure
the stability of the instrument.
XRF occasionally has spectral overlap interferences. To confirm the performance of the instrument and
interference-correction software, the instrument should be tested by using multi-element certified reference
materials having elemental compositions that can be normally found in soil.
6.3 Calibration
Usually, periodical correction of the energy axis can be applied by using a standard function of the
instrument. However, calibration is not necessary since the pre-installed manufacturer’s calibration is
sufficient. If specific calibration is needed, follow the manufacturer’s instructions.
If site-specific calibration graphs are to be used, measurement shall be done under the same operation and
sample conditions that were employed in the calibration. For samples having large or unknown matrix
effects, a fundamental parameter approach (3.4) is recommended.
NOTE Some manufacturers supply instruments with automatic calibration for abscissa, and others those with
user-assisted abscissa calibration.

6.4 Preparation in advance of site investigation
Certain preparatory actions before visiting the site help ensure that the site visit is fruitful and fulfils the
intended purposes. For example:
— an appropriate preliminary investigation should be carried out (see ISO 18400-201);
— a preliminary conceptual site model (CSM) should be prepared [this need be no more detailed than
required by the task in hand (see ISO 21365)];
— a sampling plan should be prepared (see ISO 18400-101);
— any necessary permissions should be obtained for entry in the premises;
— safety plans should be prepared;
— standard operating procedures should be prepared;
— schedules and maps should be gathered for use in the field;
— required apparatus should be gathered (see Clause 5).
NOTE Helpful guidance which is adaptable for surveys employing handheld and portable XRF devices can be
found in ISO 18400-104, ISO 18400-203 and ISO 18400-205.
6.5 In-situ measurement (including strictly in-situ measurement)
6.5.1 Secure working area
Establish a safe working area or controlled area in accordance with the manufacturer’s information. National
regulations can also apply.
6.5.2 Preparation of the measuring spot
Remove extraneous materials from the targeted spot and smooth the surface with a suitable hand tool or
spoon.
6.5.3 Surface or spot measurement
NOTE 1 On surface or spot measurement, emitting X-ray beams produced by a handheld XRF spectrometer are
directed (i) to a target ground spot or (ii) to a collected and prepared sample. In the latter, operation (ii), a measurement
is made after sample collection, but this is still regarded as in-situ measurement because the measurement is applied
just around a spot to a sample collected from the spot (an original field sample), the measuring spot being prepared
immediately before taking a sample in the same way as with the former approach (i). To clarify, operation (i) is defined
as strictly in-situ measurement while operation (ii) in-situ measurement.
Start up the handheld XRF spectrometer following the manufacturer’s instructions.
Hold and apply the XRF spectrometer to the top layer of the soil targeted which is levelled and prepared as
in 6.5.2 for in-situ measurement, in accordance with the operating instructions of the spectrometer. Use the
targeting camera, if fitted, to ensure a good location arrangement between the nose of the spectrometer and
the soil surface and to ensure that no plants, insects or earthworms are present in the primary X-ray target
area.
If a portable XRF spectrometer is being used, place the soil sample into the sample cell after confirming the
absence of extraneous substances in the sample. In the case of a portable XRF spectrometer, refer to 6.6.
During the measurement, the spectrometer shall never be lifted away from the targeted ground or the
sample being analysed in the cell of the portable XRF spectrometer.
NOTE 2 Although most spectrometers have automatic safety interlocks which stop the X-ray emitter if no X-ray
return is detected, this can take a few seconds to work.

Carry out the measurement and read the concentration indication of the target elements. The indication is
indicative of the concentration, but it is still qualitative or semi-quantitative if the indicated value or the XRF
screening method is not validated by alternative analysis as described in 8.4.
NOTE 3 When performing measurement of the ground, the surface thereof is measured. When doing measurement
of soil in a cup or bag, the outermost soil layer close to the cup or bag is measured through its material.
NOTE 4 Signal decay with depth is a significant confounding factor in obtaining accurate semi-quantitative results
in soils, particularly for the lighter elements. The selection of the right instrument and understanding its capabilities
are important in obtaining good results and reliably interpreting them.
6.6 Post-sampling measurement
6.6.1 Preparation of samples
If samples in their recovered conditions are not suitable for in-situ measurement using a portable XRF
spectrometer (e.g. requiring homogenisation), they should undergo further preparation as described below.
NOTE 1 Procedures are described in e.g. ISO 18400-201 for pretreatment including preparation of a smaller sample
(essentially a subsample) from the original field sample and for homogenisation in the field.
Take a sufficient mass of soil to ensure that the sample is representative of the sampling location. Where a
large sample is taken, a subsample should be taken to give a representative test portion. Remove extraneous
materials from the sample and crush the aggregates to fine soil particles by pressing them with a spoon in
the sample tray if possible or, for harder stones or clasts, using a mortar with a pestle made of solid inert
materials such as ceramic, agate or chalcedony.
Stones and other particles larger than approximately 2 mm diameter should be removed (e.g. by sieving) to
reduce the sizes of soil aggregates to similar dimensions. The amount and nature of the material retained on
the sieve should be recorded. The sample should be homogenized in the container e.g. by stirring.
When using a sieve (especially when apertures are not 2 mm), the amount and nature of the sample retained
on the sieve should be carefully observed.
The retained materials should be placed in a sample container, after crushing or pulverising if possible,
and tested with the XRF spectrometer. If the coarse material cannot directly be crushed, whole pieces or
clasts should be individually tested. If these coarse materials are found to contain significant amounts of the
metals under assessment, they should not be removed from the sample.
In this document, the use of a sieve size of 2 mm is validated. Screening results obtained following
instructions in this document have not been validated for other sizes (smaller or larger than 2 mm).
Pack a sample cup or bag with the pretreated soil sample. Tap the sample cup on a clean flat surface several
times to ensure close packing of the soil particles. For clay or moist samples, press the material into the
sample cup using the spoon. If there are visible voids on the film at the bottom of the sample cup, re-pack
the soil sample or repeat tapping to make the soil sample uniformly cover the entire surface of the film.
Depending on the type of soil, compress the sample to reduce the voids.
NOTE 2 Tapping or vibration of a partially compacted sample, fine grained sands and grit can cause particle re-
distribution and result in segregation of the finer-size grains and decreased sample homogeneity (especially at the
base and top of the sample), leading to unrepresentative instrumental results. The choice of sampling locality, however,
is more likely to have a large effect on XRF measurement results than the particle distributions or localization in a
sample cell caused by tapping and vibration.
NOTE 3 The difference in results obtained arising from the choice of sampling location is related to the spatial
variability with location and depth of the concentration (indeed even presence or not) of a target element including
the scale of such variability (e.g. over a few centimetres or tens of metres). Such “sampling errors” greatly exceed the
measurement errors, whether the measurement is made in the laboratory or in the field using an XRF spectrometer
following the procedures set out in this document. There are procedures for estimating and controlling sampling
errors that can be usefully adapted for use when employing an XRF spectrometer on site (see ISO 18400-104:2018,
Annex C).
If using a plastic bag in place of a sample cup, the bag should be shaken or moulded to create a flat, smooth
surface. The sample presented to the XRF spectrometer should be well mixed and not segregated to ensure
accurate results. Ensure that there is no airspace in the bag and fold the bag over to tightly enclose the
sample. The thickness of sample should be at least 10 mm, preferably 20 mm to 30 mm, to ensure that the
material on which the sample is resting (e.g. a table, a floor in a building or the ground) is not influencing the
test result.
NOTE 4 The minimum required thickness of the sample can be determined very simply by placing a metal object of
known metallurgy (preferably a metal which is not being detected in the soil) below the bag sample being tested, and
verifying whether the metal appears in the results.
A high moisture content of the sample leads to underestimation of the results. Drying of samples improves
the accuracy of the results. If the sample is moist, i.e. the water content is higher than 10 %, spread part
of the sorted and homogenized sample over a plastic plate and allow it to dry. Samples can be dried more
efficiently with a portable drying device. Repeat the measurement after drying.
6.6.2 Sample measurement and calculation
Set up the XRF spectrometer following the manufacturer’s instructions.
Determine the concentrations of target elements in the samples p
...

ISO/DISFDIS 13196:2025(en)
ISO/TC 190/SC 3
Secretariat: DIN
Date: 2025-12-222026-02-24
Soil quality — Screening soils for selected elements by energy-
dispersive X-ray fluorescence spectrometry using a handheld or
portable instrument
Qualité du sol — Diagnostic rapide d’une sélection d’éléments dans les sols à l’aide d’un spectromètre de
fluorescence X à dispersion d’énergie de type mobile ou pistolet
FDIS stage
TThhiis drs draafftt i is s susubbmmiitttteed d ttoo aa ppaarraallellel l vvoottee i inn IISSOO,, CCEEN.N.

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication
may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying,
or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO
at the address below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
EmailE-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO/DISFDIS 13196:20252026(en)
Contents
Foreword . iv
Introduction . vi
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 4
5 Apparatus . 4
5.1 XRF spectrometer . 4
5.2 Container for sampling and preparation . 5
5.3 Sampling equipment . 5
5.4 Sieve . 5
5.5 Sample cup for portable XRF spectrometers . 5
5.6 Sample container for handheld XRF spectrometers . 6
5.7 Drying device (optional) . 6
6 Procedure . 6
6.1 General . 6
6.2 Performance check of instrument . 7
6.3 Calibration . 7
6.4 Preparation in advance of site investigation . 7
6.5 In-situ measurement (including strictly in-situ measurement) . 7
6.6 Post-sampling measurement . 8
7 Specific applications: site-specific performance . 10
8 Quality assurance and control . 10
8.1 General . 10
8.2 Performance test . 11
8.3 XRF spectrometer energy calibration . 11
8.4 Complementary analysis/validation for quantitative results . 11
9 Test report . 12
Annex A (informative) Conclusion of the interlaboratory trial . 14
Annex B (informative) Energy dispersive X-ray fluorescence spectrometry (ED-XRF)
measurement usefulness . 24
Bibliography . 25

iii
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 committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. 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).
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) patent(s)
which may be required to implement this document. However, implementers are cautioned that this may not
represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO'sISO’s adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see 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, 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 13196:2013), which has been technically
revised.
The main changes are as follows:
— — the details of measurement options have been made clearer;
— — suitable materials for the equipment for sampling and sample preparation are indicated;
— — more information is provided for users of this document on requirements for:
— — sieve;
— — sample cup;
— — basic operation of XRF spectrometers;
— — safety instructions;
— — sample preparation.
iv
ISO/DISFDIS 13196:20252026(en)
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.
v
Introduction
X-ray fluorescence spectrometry (XRF) using battery or active source-powered handheld or portable
equipment is a quick method for the determination of total elemental compositions of soil samples. Unlike
laboratory analyses by inductively coupled plasma optical emission spectroscopy (ICP-OES) and atomic
absorption spectroscopy (AAS), XRF needs no digestion step to prepare a test solution to be analysed.
Consequently, handheld or portable equipment of energy -dispersive XRF (ED-XRF) is suitable for the rapid
on-site determination of selected elements, mainly heavy metals, in screening processes. When performing
analyses at a site, it can be important to have information on the presence of an element (qualitative analysis)
and also to obtain results from semi-quantitative analysis. Typical elements that can be detected and
measured are Cr, As, Se, Cd, Hg and Pb, depending on the instrument (Thethe elements validated for XRF
detection and measurement are listed in Note 3 in Clause 1Clause 1).). In these situations, factory pre-set
calibrations are used. For quantitative results, complementary analysis by alternative means is needed.
An ED-XRF exercise can comprise a single determination at one location, in accordance with the guidance in
this document, several determinations, or a large number of determinations.
Where XRF analysers are being used to assess concentrations of soil contaminants which are harmful to
humans or the environment, or both, there can be applicable national regulations with frameworks of
standards, guidance and codes of practice for such investigations.
This document does not aim to provide a strategy, tactics or methodology for environmental investigations,
or human health assessments of potentially contaminated land or soil, nor does it provide any such strategies
etc. for the assessment of mineral resources.
Adherence to this document does not demonstrate compliance with any national contaminated land
investigation regulations.
vi
DRAFT International Standard ISO/DIS 13196:2025(en)

Soil quality — Screening soils for selected elements by energy-
dispersive X-ray fluorescence spectrometry using a handheld or
portable instrument
WARNING — Soil samples can contain toxic contaminants. Avoid direct contact of soil samples with
exposed parts of the body. Appropriate measures shall be taken to avoid ingestion and inhalation.
Exposure to X-rays can give rise to radiation damage throughout the body as well an increased risk of
cancer. XRF spectrometers are usually required to comply with national regulations. Those using,
managing or supervising the use of such equipment are usually required to be qualified to do so in
accordance with national regulations.
The XRF spectrometer to be used in accordance with this document shall employ a fail-safe function
to prevent the operator and the public from inadvertent exposure to the X-ray beams. XRF users
should engage a radiation protection officer to look at their proposed activity with the XRF
spectrometer and provide informed advice on the safety implications of those proposals.
For in-situ (including strictstrictly in-situ) analysis, a safe working area or controlled area should be
established by signs and barriers, if necessary, in order to ensure bystanders are kept at a safe
distance.
1 Scope
This document specifies the procedure for screening soils for selected elements using handheld or portable
equipment for energy dispersive X-ray fluorescence spectrometry (ED-XRF). It covers the application of this
screening method to obtain qualitative or semi-quantitative data to assist decisions on a sampling strategy for
detailed assessment of soil quality employing laboratory analytical chemical methods.
Note NOTE 1 Screening methods generally provide qualitative or semi-quantitative concentration values that are
indicative of concentration values, although occasionally they can give quantitative results under specific or limited
conditions.
Note NOTE 2 The greater the effort applied to the pretreatment of soil samples, the better the analytical results that
can be expected (see e.g. Reference [19][11]).).
This document does not explicitly specify elements for which it is applicable, since the applicability depends
on the performance of the apparatus and the objective of the screening. The elements which can be determined
are limited by the performance of the instrument used, the concentrations of particular elements present in
the soil, and the requirements of the investigation in terms of the minimum concentrations of concern (e.g.
guideline value).
Note NOTE 3 The XRF measurements of As, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Sb, Sn, V and Zn were validated as described
in Annex AAnnex A.
NOTE 4 Annex BNote 4 Examples provides examples of when screening with a handheld ED-XRF spectrometer
and a portable ED-XRF spectrometer can be useful are provided in Annex B.
This document does not provide guidance on how to use the equipment to provide quantitative data for use
in detailed site assessments. This document does not cover how the results of multiple determinations are
synthesized to address the objectives of an ED-XRF determination.
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.
ISO 12404, Soil qualityand waste — Guidance on the selection and application of screening methods
ISO 18227, Soil quality — Determination of elemental composition by X-ray fluorescence
IEC 62495, Nuclear instrumentation — Portable X-ray fluorescence analysis equipment utilizing a miniature X-
ray tube
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
— — IEC Electropedia: available at https://www.electropedia.org/
3.1 3.1
X-ray fluorescence spectrometer
XRF spectrometer
spectrometer to observe X-ray fluorescence emitted from elements for analysis
Note 1 to entry: In this document, X-ray fluorescence spectrometer (XRF spectrometer) means energy dispersive X-ray
fluorescence spectrometer (ED-XRF spectrometer).
3.2 3.2
handheld XRF spectrometer
XRF spectrometer (3.1(3.1)) which can be used for in-situ analysis (e.g. strictstrictly in-situ measurement
(3.11[3.11],), in-situ measurement (3.12[3.12]))) by handheld operation
Note 1 to entry: Handheld XRF spectrometers are applicable to both in-situ measurements (including strictstrictly in-situ
measurementmeasurements) and measurements with sampling or post-sampling measurements (3.13) where post-
sampling measurement means application of determination methods including XRF to samples which are collected and
pre-treated, if needed, at a site or in a laboratory.
NOTE Note 2 to entry: When applying an XRF spectrometer to samples at a spot just after collecting them from the
ground thereat, the operation is still in-situ measurement in this document.
3.3 3.3
portable XRF spectrometer
XRF spectrometer for samples taken out of a spot at a site, which can be transported to the site
Note 1 to entry: Portable XRF spectrometers are applicable to in-situ measurements (3.12) and to post-sampling
measurements (3.13.).
NOTE Note 2 to entry: Handheld XRF spectrometers (3.2) can be used at the bench top. However, the device works
for handheld operation as designated in 3.23.2.
ISO/DISFDIS 13196:20252026(en)
3.4 3.4
fundamental parameter approach
method to obtain element composition through successive approximation of the theoretical X-ray
fluorescence intensities to the measured X-ray fluorescence intensities
Note 1 to entry: The calculation of the theoretical X-ray fluorescence intensities is carried out based on assumed element
composition, theoretical parameters and pre-determined sensitivity coefficients of the XRF spectrometer.
3.5 3.5
screening
application of any analytical semi-quantitative (3.8) method for exploratory analysis
[SOURCE: ISO /EN 12404:2021, 3.1]
3.6 3.6
screening method
method which is used (often on site) to quickly explore a given area including target parameter distribution
or to test a set of samples and obtain data on sample characteristics
Note 1 to entry: It is not necessarily directly comparable with reference methods (3.7(3.7).).
[SOURCE: ISO /EN 12404:2021, 3.2]
3.7 3.7
reference method
method which is performed in accordance with national or international standards
[SOURCE: ISO /EN 12404:2021, 3.3]
3.8 3.8
semi-quantitative
approximate and comparative rather than absolutely quantitative
3.9 3.9
semi-quantitative analysis
data analysis method that provides approximate and comparative measurements rather than absolute
quantification within a single experiment
Note 1 to entry: It combines elements of qualitative and quantitative analysis, allowing for the interpretation of
numerical values that reflect the degree or extent of a particular characteristic within a sample. Unlike fully quantitative
methods, which yield results that can be directly compared across different experiments, semi-quantitative (3.8) methods
provide information that is meaningful primarily within the context of a single experiment or study.
3.10 3.10
qualitative analysis
data analysis method that focuses on detecting or identifying constituent elements without providing specific
concentrations
3.11 3.11
strictly in-situ measurement
directly observing the ground surface with a handheld device
3.12 3.12
in-situ measurement
observing at the sampling location samples collected from the ground, with a handheld or portable device
3.13 3.13
post-sampling measurement
observing samples, with a handheld or portable device, samples which are collected from the ground and then
taken to another place (e.g. sampling stations or laboratories) after collection
NOTE Note 1 to entry: On-site measurement includes strictstrictly in-situ measurements (3.11) and in-situ measurements
(3.12) as well as post-sampling measurement when the measurement is carried out at the site but at a place different
from the sample collection spot after collection (e.g. sampling stations at a site).
NOTE Note 2 to entry: As strictstrictly in-situ and in-situ measurements are carried out applying an XRF device to the
surface of a target ground spot and to a sample collected therefrom immediately after collection, they are in other words
surface measurement and spot measurement, respectively.
3.14 3.14
certified reference material
CRM
reference material (RM) characterized by a metrologically valid procedure for one or more specified
properties, accompanied by an RM certificate that provides the value for the specified property, its associated
uncertainty and a statement of metrological traceability
[SOURCE: ISO /EN 17034:2016, 3.2], modified — Notes 1 to 4 to entry were removed.]
4 Principle
The concentrations of selected elements in soil are determined using a handheld or portable XRF spectrometer
in the field. Element concentrations are measured after sampling and limited pretreatment (in-situ
measurement), or directly in-situ (strictly in-situ measurement).
Whilst use of a handheld or portable ED-XRF spectrometer lends itself to making determinations at ad-hoc
locations based on on-site observations, it should be used in a structured way commensurate with the
intended purpose of the study for which it is being used.
NOTE 1 Guidance on sampling strategies shall be followed as appropriate, especiallyin various contexts is provided in
ISO 18400-104, ISO 18400-203 and ISO 18400-205.
The test locations should be recorded together with background information such as site-observations and
photographs taken as necessary. The use of GPS to accurately record locations can be particularly useful when
test locations are selected on an ad-hoc basis rather than tobased on a predetermined plan.
The procedure, which is described in this document, to screen soils for selected elements using handheld or
portable ED-XRF devices, gives semi-quantitative results. When desiring to know the relationship between
the results obtained and those from laboratory reference methods, compare them carefully selecting the
8.2.28.2.2,,
alternative laboratory methods bearing in mind their particular performance characteristics (see
Notes 1 and2and 2) and recognize that any method (e.g. screening and laboratory reference methods) has
errors originating from its specific sampling and analytical principles (see 7.1 and 8.48.4).).
NoteNOTE 2 Examples of situations when screening with a handheld or portable ED-XRF spectrometer can be useful
are provided in Annex BAnnex B.
5 Apparatus
5.1 XRF spectrometer
An appropriate battery or active source-powered handheld or portable ED-XRF device. Typical ED-XRF
devices are described in References [20]and[21][12, 13].
ISO/DISFDIS 13196:20252026(en)
Instruments shall have sufficient energy and depth penetration as well as suitable beam width to work for use
in soil matrices and to achieve suitable detection limits. These details are available from the manufacturer or
supplier.
A security system for the spectrometer shall be installed as designated in IEC 62495 where only the permitted
operators and supervisors of the spectrometer can activate it with a password given by the supervisors.
Automatic X-ray irradiation block mechanisms shall also work when no samples are found by the
spectrometer or human bodies are detected by an IR sensor fitted to the XRF device.
5.2 Container for sampling and preparation
A tray that can accommodate a sufficient amount of soil sample for the XRF measurement.
The tray should be of a suitable material, the wear of which will not introduce into the sample metal grains or
grains of coloured plastics which can contain metallic pigments. When it is decided to crush any aggregates or
to disaggregate lumps of soil, a mortar with a pestle made of a ceramic or other solid inert material such as a
agate or chalcedony should be used. The XRF spectrometer can be used to test trays as well as mortars and
pestles for metals which can interfere with XRF.
5.3 Sampling equipment
Sampling equipment (such as sampling spoons, trowels, picks, spades, or post-hole spades) used to prepare
for sampling (e.g. at in-situ measurement locations) and to take samples should be in good conditions and
shall not contaminate the sample.
Use of stainless steel tools can be appropriate given the tiny amounts of a hard tool that can be introduced into
the soil during sampling. Where the slightest interference from the wear of sampling equipment is possible,
plastic trowels and spoons should be used. When carrying out in-situ tests on machine excavated exposures,
the use of steel digger buckets or bulldozer blades is unavoidable in the absence of plastic buckets and blades
for such machinery.
NOTE 1 Painted or zinc- or chrome-plated tools can introduce flakes of metals or paints with metallic pigments that
can influence sample analysis by XRF which is carried out by on-site and post-sampling measurements.
NOTE 2 Further guidance on the recovery of samples for chemical analysis is given in ISO 18400-102.
5.4 Sieve
A sieve of size 2 mm, for example as described in ISO 3310-1. Clean the sieve between samples.
The procedure described in this document is only validated for material passing a 2 mm sieve. The user may
choose to use a different sieve size (sieves are available with apertures less than, and greater than, 2 mm) but
the results obtained could be different from those obtained when using a 2 mm size sieve.
NOTE Reasons for choosing a smaller sieve size might be to obtain results likely to be more relevant to the potential
for inhalation, ingestion, or contact with contaminated material.
Where the slightest interference from the wear of the sieves is possible, the use of plastic sieves should be
considered. The sieves themselves can be tested with the XRF spectrometer to ensure that any potential
contamination of samples can be assessed properly.
5.5 Sample cup for portable XRF spectrometers
A plastic cup, which is suitable for the XRF spectrometer to be used, having a window at its bottom made of
polypropylene, polyethylene terephthalate or graphene. Alternatively, a plastic bag (e.g. clear polyethylene
one) can be used. The concentration of target elements in the cup or plastic bag material should be negligible.
This should be checked by testing stacks of cups or bags using the XRF spectrometer to confirm that only ‘light
elements’ are detectable or nothingthat no elements are detected.
5.6 Sample container for handheld XRF spectrometers
Plastic containers or bags suitable for simple sample pretreatment and in-situ XRF measurement (for
strictstrictly in-situ measurement, they are not used). The concentration of target elements in the container
or bag should be negligible. This can be confirmed by testing stacks of cups or bags using the XRF
spectrometer.
5.7 Drying device (optional)
A portable electric drying oven, hot plate etc.or similar powered by batteries, or a portable generator, or a
heater driven by exothermic chemical reactions, e.g. hydration of calcium oxide.
6 Procedure
6.1 General
Three measuring ways are available for analysis using XRF spectrometers, which are strictnamely strictly in-
situ, in-situ and post-sampling measurements (where strictstrictly in-situ and in-situ measurements are on-
site measurements. To make sure about the difference between strict in-situ and in-situ measurements, see
3.11 and 3.12. Additionally, NOTE ). Note 1 to entry 3.13in 3.13 is helpful in understanding explains the
meaning of on-site measurement. As NOTE Note 2 in 3.13to entry 3.13 mentions, strictstrictly in-situ and in-
situ measurements can be said to be surface and spot measurements from the viewpoint of operation
characteristics. Handheld and portable XRF spectrometers can be used depending on the measurement way
takenmethod used. See 6.56.5 and 6.6 for the procedures for strictstrictly in-situ and in-situ measurements
and 6.6 for post-sampling measurement, respectively.
Handheld XRF spectrometers can be used for strictstrictly in-situ soil measurements as described in 6.56.5 or
to make measurements on soil samples extracted from the site, as described in 6.66.6 (post-sampling
measurement), subjected to appropriate pretreatment (e.g. sieving to obtain particles smaller than 2 mm).
Portable XRF spectrometers can be used for in-situ and post-sampling measurements.
If more highly quantitative results are needed, samples should be homogenized (see EN 15309) and
complementary analysis should be carried out using other quantitative methods, to confirm the performance
of the portable or handheld XRF spectrometer (see 8.48.4).).
The parameters to be determined should be defined before starting calibration and measurements. It should
be checked that the concentrations of each element to be determined, which is thought likely or possibly to be
present, are within the working range of the instrument. Follow the manufacturer’s instructions and perform
tests with certified reference materials to calibrate the instrument.
Test duration should be determined by the time taken until error values fall stable for each element. This is
usually displayed by the analyser against each element and falls with time as the XRF test progresses. Once
this value has stopped falling or stabilised, for the element or elements under consideration, the test may be
ended.
The concepts and goals of screening measurement in this document shall be as designated in ISO 12404. For
sampling processes and pretreatment procedures, see e.g. ISO 18400-201 and ISO 11464.
When a portable XRF spectrometer is used, a work station should be established along the lines of the one
described in ISO 18400-301 so that the instrument and personnel have a sheltered working environment.
ISO/DISFDIS 13196:20252026(en)
6.2 Performance check of instrument
Before analysis, follow the instrument manufacturer’s instructions for setup, conditioning, preparation and
maintenance. The performance control of the instrument should be carried out at least once a day to ensure
the stability of the instrument.
XRF occasionally has spectral overlap interferences. To confirm the performance of the instrument and
interference-correction software, the instrument should be tested by using multi-element certified reference
materials having elemental compositions that can be normally found in soil.
6.3 Calibration
Usually, periodical correction of the energy axis can be applied by using a standard function of the instrument.
However, calibration is not necessary since the pre-installed manufacturer'smanufacturer’s calibration is
sufficient. If specific calibration is needed, follow the manufacturer'smanufacturer’s instructions.
If site-specific calibration graphs are to be used, measurement shall be done under the same operation and
sample conditions that were employed in the calibration. For samples having large or unknown matrix effects,
a fundamental parameter approach (3.4(3.4)) is recommended.
NOTE Some manufacturers supply instruments with automatic calibration for abscissa, and others those with user-
assisted abscissa calibration.
6.4 Preparation in advance of site investigation
Before going to site certainCertain preparatory actions are required to before visiting the site help ensure that
the site visit is fruitful and fulfils the intended purposes. For example, they are:
— — an appropriate preliminary investigation should be carried out (see ISO 18400-201);
— — a preliminary conceptual site model (CSM) should be prepared ([this need be no more detailed
than required by the task in hand [(see ISO 21365]);)];
— — a sampling plan should be prepared (see ISO 18400-101);
— — any necessary permissions should be obtained for entry toin the premises;
— — safety plans should be prepared;
— — standard operating procedures should be prepared;
— — schedules and maps should be gathered for use in the field;
— — required apparatus should be gathered together (see Clause 5Clause 5).).
NoteNOTE Helpful guidance which is adaptable for surveys employing handheld and portable XRF devices can be found
in ISO 18400-104, ISO 18400-203 and ISO 18400-205.
6.5 In-situ measurement (including strictstrictly in-situ measurement)
6.5.1 Secure working area
Establish a safe working area or controlled area in accordance with the manufacturer’s information. National
regulations can also apply.
6.5.2 Preparation of the measuring spot
Remove extraneous materials from the targeted spot and smooth the surface with a suitable hand tool or
spoon.
6.5.3 Surface or spot measurement
NOTE 1 On surface or spot measurement, emitting X-ray beams produced by a handheld XRF spectrometer are
directed (i) to a target ground spot or (ii) to a collected and prepared sample. In the latter, operation (ii), a measurement
is made after sample collection, but this is still regarded as in-situ measurement because the measurement is applied just
around a spot to a sample collected from the spot (an original field sample), the measuring spot being prepared
rightimmediately before taking a sample in the same way as that forwith the former approach (i). To make these
clearclarify, operation (i) is defined as strictstrictly in-situ measurement while operation (ii) in-situ measurement.
Start up the handheld XRF spectrometer following the manufacturer'smanufacturer’s instructions.
Hold and apply the XRF spectrometer to the top layer of the soil targeted which is levelled and prepared as in
6.5.26.5.2 for in-situ measurement, in accordance with the operating instructions of the spectrometer. Use the
targeting camera, if fitted, to ensure a good location arrangement between the nose of the spectrometer and
the soil surface and to ensure that no plants, insects or earthworms are present in the primary X-ray target
area.
If a portable XRF spectrometer is being used, place the soil sample into the sample cell after confirming the
absence of extraneous substances in the sample. In the case of a portable XRF spectrometer, refer to 6.66.6.
During the measurement, the spectrometer shall never be lifted away from the targeted ground or the sample
being analysed in the cell of the portable XRF spectrometer.
NOTE 2 Although most spectrometers have automatic safety interlocks which stop the X-Rayray emitter if no X-
Rayray return is detected, this can take a few seconds to work.
Carry out the measurement and read the concentration indication of the target elements. The indication is
indicative of the concentration, but it is still qualitative or semi-quantitative if the indicated value or the XRF
screening method is not validated by alternative analysis as described in 8.48.4.
NOTE 3 When performing measurement of the ground, the surface thereof is measured. When doing measurement of
soil in a cup or bag, the outermost soil layer close to the cup or bag is measured through its material.
NOTE 4 Signal decay with depth is a significant confounding factor in obtaining accurate semi-quantitative results in
soils, particularly for the lighter elements. The selection of the right instrument and understanding its capabilities are
important in obtaining good results and reliably interpreting them.
6.6 Post-sampling measurement
6.6.1 Preparation of samples
If samples in their recovered conditions are not suitable for in-situ measurement using a portable XRF
spectrometer (e.g. requiring homogenisation), they should undergo further preparation as described below.
NOTE 1 Procedures are described in e.g. ISO 18400-201 for pretreatment including preparation of a smaller sample
(essentially a subsample) from the original field sample and for homogenisation in the field.
Take a sufficient mass of soil to ensure that the sample is representative of the sampling location. Where a
large sample is taken, a subsample should be taken to give a representative test portion. Remove extraneous
materials from the sample and crush the aggregates to fine soil particles by pressing them with a spoon in the
sample tray if possible or, for harder stones or clasts, using a mortar with a pestle made of solid inert materials
such as ceramic, agate or chalcedony.
ISO/DISFDIS 13196:20252026(en)
Stones and other particles larger than aboutapproximately 2 mm diameter should be removed (e.g. by sieving)
to reduce the sizes of soil aggregates to similar dimensions. The amount and nature of the material retained
on the sieve should be recorded. The sample should be homogenized in the container e.g. by stirring.
When using a sieve (especially ones, thewhen apertures of which are not 2 mm), the amount and nature of the
sample retained on the sieve should be carefully observed.
The retained materials should be placed in a sample container, after crushing or pulverising if possible, and
tested with the XRF spectrometer. If the coarse material cannot directly be crushed, whole pieces or clasts
should be individually tested. If these coarse materials are found to contain significant amounts of the metals
under assessment, they should not be removed from the sample.
In this document, the use of a sieve size of 2 mm is validated but other sizes (smaller or larger than 2 mm).
Note that screening. Screening results obtained following the guidanceinstructions in this document have not
been validated for other sizes (smaller or larger than the use of a 2 mm sieve.).
Pack a sample cup or bag with the pretreated soil sample. Tap the sample cup on a clean flat surface several
times to ensure close packing of the soil particles. For clay or moist samples, press the material into the sample
cup using the spoon. If there are visible voids on the film at the bottom of the sample cup, re-pack the soil
sample or repeat tapping to make the soil sample uniformly cover the entire surface of the film. Depending on
the type of soil, compress the sample to reduce the voids.
NOTE 2 Tapping or vibration of a partially compacted sample, fine grained sands and grit can cause particle re-
distribution and result in segregation of the finer-size grains and decreased sample homogeneity (especially at the base
and top of the sample), leading to unrepresentative instrumental results. The choice of sampling locality, however, is
more likely to have a large effect on XRF measurement results than the particle distributions or localization in a sample
cell caused by tapping and vibration.
NOTE 3 The difference in results obtained arising from the choice of sampling location is related to the spatial
variability with location and depth of the concentration (indeed even presence or not) of a target element including the
scale of such variability (e.g. over a few centimetres or tens of metres). Such “sampling errors” greatly exceed the
measurement errors, whether the measurement is made in the laboratory or in the field using an XRF spectrometer
following the procedures set out in this document. There are procedures for estimating and controlling sampling errors
that can be usefully adapted for use when employing an XRF spectrometer on site (see ISO 18400-104:2018, Annex C).
If using a plastic bag in place of a sample cup, the bag should be shaken or moulded to create a flat, smooth
surface. The sample presented to the XRF spectrometer should be well mixed and not segregated to ensure
accurate results. Ensure that there is no airspace in the bag and fold the bag over to tightly enclose the sample.
The thickness of sample should be at least 10 mm, preferably 20 mm to 30 mm, to ensure that the material on
which the sample is resting (e.g. a table, a floor in a building or the ground) is not influencing the test result.
NOTE 4 The minimum required thickness of the sample can be determined very simply to avoid any doubt by placing
a metal object of known metallurgy (preferably a metal which is not being detected in the soil) below the bag sample
being tested, and seeing ifverifying whether the metal appears in the results.
A high moisture content of the sample leads to underestimation of the results. Drying of samples improves the
accuracy of the results. If the sample is moist, i.e. the water content is higher than 10 %, spread part of the
sorted and homogenized sample over a plastic plate and allow it to dry. Samples can be dried more efficiently
with a portable drying device. Repeat the measurement after drying.
6.6.2 Sample measurement and calculation
Set up the XRF spectrometer following the manufacturer’s instructions.
Determine the concentrations of target elements in the samples prepared following the procedure in
6.6.16.6.1. If a targeted element is not detected, or if detected but the concentration cannot be measured, this
qualitative result should be recorded.
When site-specific calibration graphs are to be used, see 6.36.3.
NOTE Some XRF spectrometers are equipped with an image sensor to show what lies in the primary X-Rayray beam
target area. It is useful to choose appropriate analytical points avoiding voids, stones and organic matter.
7 Specific applications
87 Site: site-specific performance
To obtain an overview of the chemical status of an investigation site or area, especially ofwith regard to
contamination, try post-sampling measurement by applying an XRF spectrometer to a pre-treated (e.g. sub-
sampled and prepared for measurement) composite sample prepared by well mixing incremental samples
collected from the site (see ISO 18400-104 for guidance on composite sampling).
For other specific purposes (e.g. finding hot spots, estimating bulk concentrations), make the measurement
by applying an XRF spectrometer directly to the soil of the ground surface (strictstrictly in-situ measurement)
or to soil collected therefrom (in-situ measurement), at several locations having regard to the guidance in
ISO 18400-104 on sampling patterns. Calculating the averages of the element concentration values obtained
at each measurement point will give comparable results to those obtained by post-sampling measurement
applying an XRF spectrometer to a pre-treated composite sample (e.g. sub-sampled and prepared for
measurement).
A hot spot is an area within a site in which the concentrations of an element are higher than in the remainder
of the site. What constitutes a “hot spot”,, i.e. what concentration is significant, is decided by the investigator.
The size of the hot spot, and therefore the probability of detecting it, will usually depend on the magnitude of
the concentration considered worthy of note; this could be for example an arbitrary value, or a generic
assessment value (or a fraction or multiple thereof).
One way of detecting “hot spots” is to apply an XRF spectrometer to the surface at frequent intervals along one
or more transects. Handheld and portable XRF spectrometers can be applied to help delineate areas with
higher concentrations (hot spots). In this case, calculating the averages of contaminant concentrations
obtained while delineating a hot spot will give a semi-quantitative estimate of the contamination
concentrations in that part of a site. Calculating the average of the concentrations includingboth inside and
outside hot spots will give thatan estimate of the concentrations in the who
...

PROJET
Norme
internationale
ISO/DIS 13196
ISO/TC 190/SC 3
Qualité du sol — Diagnostic rapide
Secrétariat: DIN
d’une sélection d’éléments dans
Début de vote:
les sols à l’aide d’un spectromètre
2025-01-24
de fluorescence X à dispersion
Vote clos le:
d’énergie de type mobile ou pistolet
2025-04-18
Soil quality — Screening soils for selected elements by energy-
dispersive X-ray fluorescence spectrometry using a handheld or
portable instrument
ICS: 13.080.10
CE DOCUMENT EST UN PROJET DIFFUSÉ
POUR OBSERVATIONS ET APPROBATION. IL
EST DONC SUSCEPTIBLE DE MODIFICATION
ET NE PEUT ÊTRE CITÉ COMME NORME
INTERNATIONALE AVANT SA PUBLICATION EN
TANT QUE TELLE.
Le présent document est distribué tel qu’il est parvenu du secrétariat
du comité. OUTRE LE FAIT D’ÊTRE EXAMINÉS POUR
ÉTABLIR S’ILS SONT ACCEPTABLES À DES
FINS INDUSTRIELLES, TECHNOLOGIQUES ET
COMMERCIALES, AINSI QUE DU POINT DE VUE
DES UTILISATEURS, LES PROJETS DE NORMES
INTERNATIONALES DOIVENT PARFOIS ÊTRE
TRAITEMENT PARALLÈLE ISO/CEN
CONSIDÉRÉS DU POINT DE VUE DE LEUR
POSSIBILITÉ DE DEVENIR DES NORMES
POUVANT SERVIR DE RÉFÉRENCE DANS LA
RÉGLEMENTATION NATIONALE.
LES DESTINATAIRES DU PRÉSENT PROJET
SONT INVITÉS À PRÉSENTER, AVEC LEURS
OBSERVATIONS, NOTIFICATION DES DROITS
DE PROPRIÉTÉ DONT ILS AURAIENT
ÉVENTUELLEMENT CONNAISSANCE
ET À FOURNIR UNE DOCUMENTATION
EXPLICATIVE.
Numéro de référence
ISO/DIS 13196:2025(fr)
ISO/DIS 13196:2025(fr)
ISO/DIS 13196:2025(fr)
Ȁ 190/ 3
‡…”±–ƒ”‹ƒ– : DIN
ƒ–‡ǣ ʹͲʹͷǦͲͳǦʹͶ
Qualité du sol — Diagnostic rapide d’une sélection d’éléments dans les sols
à l’aide d’un spectromètre de fluorescence X à dispersion d’énergie de type
mobile ou pistolet
Soil quality — Screening soils for selected elements by energy dispersive X-ray fluorescence spectrometry
using a handheld or portable instrument
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2025
Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette
publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,
y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut
être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
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Publié en Suisse

ii
ISO/DIS 13196 :2025(fr)
Sommaire
Avant-propos . iv
Introduction . vi
1 Domaine d’application . 1
2 Références normatives . 2
3 Termes et définitions . 2
4 Principe . 4
5 Appareillage . 4
5.1 Spectromètre XRF . 4
5.2 Récipient pour échantillonnage et préparation . 4
5.3 Matériel d’échantillonnage . 4
5.4 Tamis (facultatif) . 5
5.5 Godet à échantillon pour spectromètres XRF de type mobile . 5
5.6 Récipient à échantillon pour spectromètres XRF de type pistolet . 5
5.7 Dispositif de séchage (facultatif) . 5
6 Procédure . 5
6.1 Généralités . 5
6.2 Contrôle de performance des instruments . 6
6.3 Étalonnage . 6
6.4 Mesurage in situ . 6
6.4.1 Sécurisation de la zone de travail . 6
6.4.2 Préparation du point de mesure . 7
6.4.3 Mesurage de point ou de surface . 7
6.5 Mesurage après échantillonnage . 7
6.5.1 Préparation des échantillons . 7
6.5.2 Mesurage des échantillons et calcul . 9
7 Contrôle de la qualité . 9
7.1 Essai de performance . 9
7.1.1 Performances du spectromètre XRF . 9
7.1.2 Matériaux de référence pour essais . 9
7.1.3 Performances spécifiques au site . 10
7.2 Amélioration de la qualité des investigations sur site . 11
7.3 Étalonnage de l’énergie des spectromètres XRF . 11
7.4 Validation complémentaire pour les résultats quantitatifs . 11
8 Rapport d’essai . 11
Annexe A (informative) Résultats de fidélité . 12
A.1 Conclusions d’un essai interlaboratoires . 12
Annexe B (informative) Utilité de la mesure ED-XRF . 19
B.1 Utilité de la mesure ED-XRF . 19
Bibliographie . 21

iii
ISO/DIS 13196 :2025(fr)
Avant-propos
L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes
nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est en
général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude a le droit
de faire partie du comité technique créé à cet effet. Les organisations internationales, gouvernementales
et non gouvernementales, en liaison avec l’ISO, participent également aux travaux. L’ISO collabore
étroitement avec la Commission électrotechnique internationale (IEC) en ce qui concerne la
normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir
www.iso.org/directives).
L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de
droits de brevet ou de droits analogues. L’ISO ne saurait être tenue pour responsable de ne pas avoir
identifié de tels droits de brevet et averti de leur existence. Les détails concernant les références aux
droits de brevet ou autres droits analogues identifiés lors de l’élaboration du document sont indiqués
dans l’Introduction et/ou dans la liste des déclarations de brevets reçues par l’ISO (voir
www.iso.org/brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l’ISO liés à l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion
de l’ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (TBT), voir www.iso.org/avant-propos.
Le présent document a été élaboré par le comité technique ISO/TC 190, Qualité du sol, sous-comité SC 3,
Méthodes chimiques et caractéristiques physiques.
Cette seconde édition annule et remplace la première édition (ISO 13196 :2013), qui a fait l’objet d’une
révision technique, sans toucher au principe et à la procédure définis dans la première version.
Les principales modifications sont les suivantes :
— les informations relatives aux options de mesurage ont été clarifiées ;
— les matériaux adaptés au matériel d’échantillonnage et de préparation des échantillons sont
indiqués ;
— de plus amples informations sont fournies aux utilisateurs de la Norme internationale concernant les
exigences relatives :
— au tamis ;
— au godet à échantillon ;
— au fonctionnement de base des spectromètres XRF ;
— aux instructions de sécurité ;
iv
ISO/DIS 13196 :2025(fr)
— à la préparation des échantillons.
Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent
document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l’adresse www.iso.org/fr/members.html.
v
ISO/DIS 13196 :2025(fr)
Introduction
La spectrométrie de fluorescence X (XRF) à l’aide d’un équipement de type mobile ou pistolet alimenté
par batterie ou source active est une méthode de détermination rapide des compositions élémentaires
totales des échantillons de sol. Contrairement aux analyses en laboratoire par spectroscopie d’émission
atomique à plasma à couplage inductif (ICP-OES) et spectroscopie d’absorption atomique (AAS), la
spectrométrie XRF à l’aide d’un équipement de type mobile ou pistolet ne nécessite aucune étape de
digestion pour préparer la solution d’essai à analyser. De ce fait, un équipement XRF à dispersion
d’énergie (ED-XRF) de type mobile ou pistolet convient à la détermination rapide sur site d’une sélection
d’éléments, principalement les métaux lourds dans les démarches de diagnostic rapide. Lors de la
réalisation d’une analyse sur un site, il peut être important de disposer d’informations sur la présence
d’un élément (analyse qualitative) et également d’obtenir des résultats semi-quantitatifs. Les éléments
typiques qu’il est possible de détecter et de mesurer sont Cr, As, Se, Cd, Hg et Pb, selon l’instrument. Il est
souvent impossible de procéder à l’étalonnage à partir de matériaux de référence sur un site à examiner.
Dans ce type de situation, il convient d’utiliser les étalonnages prédéfinis en usine. Concernant les
résultats quantitatifs, une analyse complémentaire est requise à l’aide de moyens alternatifs.
Un exercice ED-XRF peut comporter une seule détermination en un seul lieu, conformément aux
recommandations du présent document, plusieurs déterminations ou un grand nombre de
déterminations. La manière dont les résultats de déterminations multiples doivent être synthétisés pour
répondre aux objectifs de l’exercice ne relève pas du domaine d’application du présent document. Voir
l’Annexe B pour des exemples de cas où il peut être utile d’effectuer un diagnostic rapide à l’aide d’un
spectromètre ED-XRF de type mobile ou pistolet.
Lorsque des analyseurs XRF sont utilisés pour évaluer les concentrations des contaminants du sol
toxiques pour l’homme et/ou l’environnement, des réglementations nationales peuvent être applicables
avec des cadres de normes, de recommandations et de codes de bonne pratique pour de telles
investigations.
Le présent document ne vise pas à définir une stratégie, une tactique ou une méthodologie pour réaliser
des investigations environnementales, des évaluations de l’impact des terres ou des sols potentiellement
contaminés sur la santé humaine ou une évaluation des ressources minérales.
L’adhésion au présent document ne démontre pas la conformité aux réglementations nationales relatives
aux investigations des terres contaminées.
vi
PROJET de Norme internationale ISO/DIS 13196 :2025(fr)

Qualité du sol — Diagnostic rapide d’une sélection d’éléments
dans les sols à l’aide d’un spectromètre de fluorescence X à
dispersion d’énergie de type mobile ou pistolet
AVERTISSEMENT — Les échantillons de sol peuvent contenir des contaminants toxiques. Éviter le
contact direct des échantillons de sol avec les parties exposées du corps humain. Des mesures
appropriées doivent être prises pour éviter l’ingestion et l’inhalation.
L’exposition aux rayons X peut entraîner des brûlures par irradiation dans tout le corps, ainsi
qu’un risque accru de cancer, parmi de nombreux autres effets néfastes. Les spectromètres XRF
doivent généralement satisfaire aux réglementations nationales. Les personnes qui gèrent ou
supervisent l’utilisation de tels équipements doivent généralement être qualifiées pour le faire
conformément aux réglementations nationales.
Le spectromètre XRF à utiliser conformément au présent document doit présenter une fonction
de sécurité intégrée afin d’empêcher l’opérateur et le public d’être exposés par inadvertance aux
faisceaux de rayons X. Un système de sécurité pour le spectromètre doit être installé
conformément à l’IEC 62495. Ce système assurera que seuls les opérateurs et les superviseurs
autorisés puissent activer le spectromètre, et ce, à l’aide d’un mot de passe donné par les
superviseurs. Les mécanismes de blocage automatique de l’irradiation aux rayons X doivent
également fonctionner lorsqu’aucun échantillon n’est trouvé par le spectromètre ou que des
corps humains sont détectés par un capteur infrarouge dont il est équipé. Il convient que les
utilisateurs de spectromètres XRF fassent appel à un responsable en radioprotection afin qu’il
examine leurs propositions d’activité avec le spectromètre XRF et leur fournisse un avis éclairé
sur les implications de ces propositions en termes de sécurité.
Pour les analyses in situ, il convient d’établir une zone de travail sécurisée ou une zone contrôlée
à l’aide de panneaux et de barrières, si nécessaire, conformément aux lignes directrices
nationales en matière de santé et de sécurité, afin de s’assurer que les personnes présentes sont
tenues à distance.
1 Domaine d’application
Le présent document spécifie la procédure de diagnostic rapide (3.5) d’une sélection d’éléments dans les
sols à l’aide d’un équipement ED-XRF de type mobile ou pistolet. Il traite principalement de l’application
de cette méthode ou de la méthode de diagnostic rapide (3.6) sur site, pour obtenir des données
qualitatives ou semi-quantitatives qui aident à décider d’une stratégie d’échantillonnage pour
l’évaluation détaillée de la qualité du sol à l’aide de méthodes d’analyse chimique en laboratoire.
Note 1 Les méthodes de diagnostic rapide donnent généralement des valeurs de concentration qualitatives ou
semi-quantitatives qui correspondent à des niveaux de concentration, tandis que les autres méthodes donnent
occasionnellement des résultats quantitatifs dans des conditions spécifiques ou limitées. Voir 3.5 et 3.6 pour les
définitions et les caractéristiques des méthodes de diagnostic rapide.
Note 2 Plus les efforts de traitement préalable des échantillons de sol sont importants, plus on peut s’attendre à
des résultats d’analyse de qualité (voir, par exemple, la Référence [11]).
Le présent document ne spécifie pas de façon explicite les éléments pour lesquels il est applicable dans
la mesure où ses possibilités d’application dépendent des performances de l’appareil et des objectifs du
ISO/DIS 13196 :2025(fr)
diagnostic rapide. Les éléments qui peuvent être déterminés sont limités par les performances de
l’instrument utilisé, les concentrations des éléments particuliers présents dans le sol, et les exigences de
l’investigation concernant les concentrations minimales préoccupantes (par exemple la valeur de
référence).
Note 3 Les mesures XRF de As, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Sb, Sn, V et Zn ont été validées tel que décrit à
l’Annexe A.
Note 4 Des exemples de cas où il peut être utile d’effectuer un diagnostic rapide à l’aide d’un spectromètre ED-
XRF de type mobile ou pistolet sont fournis à l’Annexe B.
Le présent document ne fournit pas de recommandations relatives à la manière d’utiliser l’équipement
pour obtenir des données quantitatives en vue de les utiliser dans les évaluations détaillées des sites.
2 Références normatives
Les documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.
Pour les références non datées, la dernière édition du document de référence s’applique (y compris les
éventuels amendements).
ISO/EN 12404, Qualité du sol — Lignes directrices pour la sélection et l’application des méthodes de
diagnostic rapide
ISO 18227, Qualité du sol — Détermination de la composition élémentaire par fluorescence X
IEC 62495, Nuclear instrumentation — Portable X-ray fluorescence analysis equipment utilizing a
miniature X-ray tube
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s’appliquent.
L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes :
— Plateforme de consultation en ligne ISO : disponible à l’adresse https://www.iso.org/obp
— IEC Electropedia : disponible à l’adresse https://www.electropedia.org/
3.1
spectromètre XRF
spectromètre de fluorescence X
3.2
spectromètre XRF de type pistolet
spectromètre XRF qui peut être utilisé à la main pour analyser les sols in situ (restant en place)
Note 1 à l’article : Les spectromètres XRF de type pistolet peuvent être utilisés à la fois pour les mesurages in situ et
les mesurages avec échantillonnage ou les mesurages après échantillonnage. Par mesurage après échantillonnage,
on entend l’application de méthodes de détermination, y compris la spectrométrie XRF, à des échantillons prélevés
et, si nécessaire, préalablement traités, sur un site ou dans un laboratoire.
ISO/DIS 13196 :2025(fr)
3.3
spectromètre XRF de type mobile
spectromètre XRF qui peut être transporté jusqu’au site pour analyser les échantillons qui y ont été
prélevés
Note 1 à l’article : Les spectromètres XRF de type mobile peuvent être utilisés pour les mesurages après
échantillonnage.
3.4
approche des paramètres fondamentaux
méthode permettant d’obtenir la composition élémentaire par le biais d’une approximation successive
des intensités théoriques de fluorescence X par rapport aux intensités mesurées de fluorescence X
Note 1 à l’article : Le calcul des intensités théoriques de fluorescence X est réalisé à partir de la composition
élémentaire présumée, de paramètres théoriques et de coefficients de sensibilité prédéterminés du spectromètre
XRF.
3.5
diagnostic rapide
application d’une méthode d’analyse semi-quantitative à des fins exploratoires
[SOURCE : ISO/EN 12404 :2021, 3.1]
3.6
méthode de diagnostic rapide
méthode utilisée (souvent sur site) pour explorer rapidement une zone donnée, y compris la répartition
de paramètres cibles, ou pour soumettre à essai un ensemble d’échantillons et obtenir des données sur
les caractéristiques des échantillons
Note 1 à l’article : Une méthode de diagnostic rapide n’est pas toujours directement comparable à des méthodes de
référence (3.7).
[SOURCE : ISO/EN 12404 :2021, 3.2]
3.7
méthode de référence
méthode mise en œuvre conformément à des normes nationales ou internationales
[SOURCE : ISO/EN 12404 :2021, 3.3]
3.8
analyse semi-quantitative
méthode d’analyse des données qui fournit des mesures approximatives et comparatives plutôt qu’une
quantification absolue dans le cadre d’une seule expérimentation
Note 1 à l’article : Elle combine des éléments d’analyse qualitative et quantitative, permettant l’interprétation de
valeurs numériques qui reflètent le degré ou l’étendue d’une caractéristique particulière dans un échantillon.
Contrairement aux méthodes entièrement quantitatives, qui donnent des résultats pouvant être directement
comparés entre différentes expérimentations, les méthodes semi-quantitatives fournissent des informations qui
sont principalement significatives dans le contexte d’une seule expérimentation.
3.9
analyse qualitative
méthode d’analyse des données qui se concentre sur la détection ou l’identification des éléments
constituants sans fournir de concentrations spécifiques
ISO/DIS 13196 :2025(fr)
4 Principe
Les concentrations d’une sélection d’éléments dans le sol sont déterminées à l’aide d’un spectromètre
XRF de type mobile ou pistolet. Les concentrations des éléments sont mesurées après échantillonnage et
traitement préalable limité ou directement dans le sol en place (in situ).
Bien que l’utilisation d’un spectromètre ED-XRF de type mobile ou pistolet se prête à la réalisation de
déterminations en des lieux ad hoc en fonction des observations effectuées sur site, il convient de l’utiliser
de manière structurée et proportionnée à l’objectif de l’étude pour laquelle il est utilisé. Il convient que
les recommandations relatives aux stratégies d’échantillonnage (par exemple ISO 18400-104,
ISO 18400-203, ISO 18400-205) soient suivies selon le cas.
Il convient d’enregistrer les lieux d’essai, de même que les informations contextuelles telles que les
observations effectuées sur site et les photographies prises le cas échéant. L’emploi d’un GPS peut être
particulièrement utile pour enregistrer les lieux d’essai avec précision lorsqu’ils sont choisis sur une base
ad hoc plutôt que selon un plan prédéterminé.
Il peut être jugé souhaitable de comparer les résultats obtenus avec les résultats de laboratoire, mais,
sauf lorsque cela est effectué sur une base ad hoc, il convient de le faire de manière réfléchie (voir 7.1.3
et 7.4).
Note Des exemples de cas où il peut être utile d’effectuer un diagnostic rapide à l’aide d’un spectromètre ED-
XRF de type mobile ou pistolet sont fournis dans l’Introduction.
5 Appareillage
5.1 Spectromètre XRF
Un dispositif ED-XRF approprié, de type mobile ou pistolet alimenté par batterie ou source active. Des
dispositifs ED-XRF typiques sont décrits dans les Références [12, 13].
Note Les instruments doivent être dotés d’une énergie et d’une pénétration en profondeur suffisantes ainsi que
d’une largeur de faisceau adaptée pour pouvoir être utilisés dans les matrices du sol et atteindre des limites de
détection appropriées. Ces informations sont disponibles auprès du fabricant ou du fournisseur.
5.2 Récipient pour échantillonnage et préparation
Un plateau qui peut contenir une quantité suffisante d’échantillon de sol pour la mesure XRF.
Il convient que le plateau soit fait d’un matériau approprié dont l’usure ne risque pas d’introduire dans
l’échantillon des grains métalliques ou des grains de plastiques colorés pouvant contenir des pigments
métalliques. Si l’on décide de concasser des agrégats ou de désagréger des mottes de terre, on peut utiliser
un mortier et un pilon fabriqués dans des matériaux inertes solides tels que la céramique, l’agate et la
calcédoine. Le spectromètre XRF peut être utilisé pour soumettre à essai les plateaux, mortiers et pilons
afin de détecter les métaux qui peuvent interférer avec la XRF.
5.3 Matériel d’échantillonnage
Il convient que le matériel d’échantillonnage (tel que les cuillères, les truelles, les pioches, les bêches ou
les bêches à trous) utilisé pour préparer l’échantillonnage (par exemple sur des lieux de mesure in situ)
et pour prélever les échantillons soit en bon état et qu’il ne contamine pas l’échantillon.
L’utilisation d’outils en acier inoxydable peut s’avérer appropriée compte tenu des quantités infimes d’un
outil dur qui peuvent être introduites dans le sol en un point sur un site ou dans les échantillons. Lorsque
la moindre interférence due à l’usure du matériel d’échantillonnage est possible, il convient d’utiliser des
truelles et des cuillères en plastique. Lors de la réalisation d’essais in situ sur des expositions excavées à
ISO/DIS 13196 :2025(fr)
la machine, l’utilisation de godets de pelle ou de lames de bulldozer en acier est inévitable en l’absence
de godets et de lames en plastique pour de telles machines.
Note 1 Les outils peints, zingués ou chromés peuvent introduire des paillettes de métaux ou de peintures
contenant des pigments métalliques qui peuvent influencer l’analyse in situ et l’analyse des échantillons par mesure
XRF.
Note 2 L’ISO 18400-102 donne des recommandations supplémentaires relatives à la récupération des
échantillons pour analyse chimique.
5.4 Tamis (facultatif)
Un tamis d’une taille de maille de 2 mm tel que décrit dans l’ISO 3310-1. Nettoyer le tamis entre chaque
échantillon.
La procédure décrite dans le présent document n’est validée que pour les matériaux passant au tamis de
2 mm. L’utilisateur peut choisir d’utiliser une taille de maille différente (il existe des tamis dont les mailles
sont inférieures ou supérieures à 2 mm), mais les résultats obtenus peuvent être différents de ceux
obtenus avec un tamis d’une taille de maille de 2 mm.
Note Le choix d’une taille de maille plus petite peut être motivé par la volonté d’obtenir des résultats
susceptibles d’être plus en rapport avec la possibilité d’inhalation, d’ingestion ou de contact avec des matériaux
contaminés.
Lorsque la moindre interférence due à l’usure des tamis est possible, il convient d’envisager d’utiliser des
tamis en plastique. Les tamis eux-mêmes peuvent être soumis à essai avec le spectromètre XRF afin de
s’assurer que toute contamination potentielle des échantillons peut être correctement évaluée.
5.5 Godet à échantillon pour spectromètres XRF de type mobile
Un godet en plastique, adapté au spectromètre XRF à utiliser, équipé d’une fenêtre dans sa partie
inférieure, en polypropylène, polyéthylène téréphtalate ou graphène. En guise d’alternative, un sac en
plastique (par exemple, un sac en polyéthylène transparent) peut aussi être utilisé. Il convient que la
concentration des éléments cibles du godet ou du sac en plastique soit négligeable. Il convient de vérifier
cela en soumettant à essai des piles de godets ou une épaisseur de plusieurs sacs à l’aide du spectromètre
XRF afin de confirmer qu’il détecte uniquement des « éléments légers », voire aucun élément.
5.6 Récipient à échantillon pour spectromètres XRF de type pistolet
Récipients ou sacs en plastique adaptés au traitement préalable simple des échantillons et à la mesure
XRF directe. Il convient que la concentration des éléments cibles du récipient ou du sac soit négligeable
et qu’elle soit vérifiée en soumettant à essai des piles de godets ou une épaisseur de plusieurs sacs à l’aide
du spectromètre XRF.
5.7 Dispositif de séchage (facultatif)
Un four de séchage électrique portable, une plaque chauffante, etc., alimentés par des batteries ou un
générateur portable, ou un élément chauffant alimenté par des réactions chimiques exothermiques, par
exemple l’hydratation de l’oxyde de calcium.
6 Procédure
6.1 Généralités
Les spectromètres XRF de type pistolet peuvent être utilisés pour effectuer des mesurages in situ directs
du sol tel que décrit en 6.4 ou des mesurages sur des échantillons de sol extraits du site et soumis à un
ISO/DIS 13196 :2025(fr)
traitement préalable approprié (par exemple, un tamisage pour obtenir des particules d’une taille
inférieure à 2 mm) tel que décrit en 6.5.
Note Si des résultats hautement quantitatifs sont nécessaires, il convient d’homogénéiser les échantillons (voir
l’EN 15309) et de réaliser une analyse complémentaire à l’aide d’autres méthodes quantitatives, afin de confirmer
les performances du spectromètre XRF de type mobile ou pistolet.
Il convient de définir les paramètres à déterminer avant le démarrage de l’étalonnage et des mesurages,
et de vérifier que les concentrations de chaque élément à déterminer dont la présence est jugée possible
ou probable sont compatibles avec la capacité de l’instrument utilisé. Suivre les instructions du fabricant
et réaliser des essais avec des matériaux de référence étalons pour étalonner l’instrument.
Il convient de déterminer la durée d’essai par le temps nécessaire pour que les valeurs d’erreur
deviennent stables pour chaque élément. Elle est généralement affichée par l’analyseur pour chaque
élément et diminue au fur et à mesure que l’essai XRF progresse. Dès lors que cette valeur a cessé de
diminuer ou s’est stabilisée pour l’élément ou les éléments étudiés, l’essai peut être arrêté.
Note 1 Pour des recommandations relatives au traitement préalable sur le terrain, voir l’ISO 18400-201 et pour
le traitement préalable en laboratoire, voir l’ISO 11464.
Pour de plus amples informations sur le concept et les objectifs du mesurage par diagnostic rapide, voir
l’ISO 12404. Pour les processus d’échantillonnage et les procédures de traitement préalable, voir par
exemple l’ISO 18400-201 et l’ISO 11464, respectivement.
Note 2 L’ISO 11464 va être regroupée avec plusieurs autres normes internationales et européennes relatives aux
méthodes de traitement préalable en laboratoire dans une nouvelle norme complète, à savoir l’ISO/EN 21744.
6.2 Contrôle de performance des instruments
Avant l’analyse, suivre les instructions du fabricant concernant le réglage, le conditionnement, la
préparation et l’entretien de l’instrument. Il convient de réaliser le contrôle de performance de
l’instrument au minimum une fois par jour pour assurer sa stabilité.
La spectrométrie XRF peut parfois avoir des interférences spectrales par chevauchement de raies. Afin
de confirmer les performances de l’instrument et du logiciel de correction des interférences, il convient
de soumettre à essai l’instrument en utilisant des matériaux de référence à multiples éléments ayant des
compositions élémentaires que l’on trouve normalement dans le sol.
6.3 Étalonnage
En règle générale, la correction périodique de l’axe énergétique peut être appliquée en utilisant une
fonction standard de l’instrument. Toutefois, l’étalonnage n’est pas nécessaire, car l’étalonnage
préinstallé par le fabricant suffit. Si un étalonnage spécifique est nécessaire, suivre les instructions du
fabricant.
Si les graphiques d’étalonnage spécifiques au site doivent être utilisés, le mesurage doit être réalisé dans
les mêmes conditions de fonctionnement et de prélèvement que celles utilisées pour l’étalonnage. Pour
les échantillons présentant des effets de matrice significatifs ou non connus, l’approche des paramètres
fondamentaux (3.4) est recommandée.
Note Certains fabricants fournissent des instruments avec un étalonnage automatique de l’abscisse, et d’autres
avec un étalonnage de l’abscisse assisté par l’utilisateur.
6.4 Mesurage in situ
6.4.1 Sécurisation de la zone de travail
Établir une zone de travail sécurisée ou une zone contrôlée conformément aux réglementations
nationales et aux informations du fabricant.
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6.4.2 Préparation du point de mesure
Retirer les corps étrangers du point ciblé et lisser la surface du sol avec un outil à main approprié ou une
cuillère.
6.4.3 Mesurage de point ou de surface
Note 1 Lors du mesurage d’un point ou d’une surface, les faisceaux de rayons X émis par un spectromètre XRF de
type pistolet sont dirigés (i) vers un point cible au sol ou (ii) vers un échantillon prélevé et préparé. Dans la seconde
opération (ii), un mesurage après échantillonnage est effectué, mais il est toujours considéré comme un mesurage
in situ car il est appliqué à un échantillon prélevé directement à partir d’un point sur un site du terrain, le point de
mesure étant préparé juste avant de prélever un échantillon de la même manière que pour la première approche
(i).
Démarrer le spectromètre XRF de type pistolet suivant les instructions du fabricant.
Maintenir et appliquer le spectromètre XRF sur la couche supérieure du sol ciblé qui est nivelée et
préparée en 6.4.2 pour le mesurage in situ, conformément aux instructions d’utilisation du spectromètre.
Utiliser la caméra de ciblage, si elle est installée, pour s’assurer que la disposition du lieu situé entre le
nez du spectromètre et la surface du sol est bonne et que des plantes, des insectes ou des vers de terre ne
sont pas présents dans la zone cible des rayons X primaires.
Si un spectromètre XRF de type mobile est utilisé, placer l’échantillon de sol dans la cellule à échantillon
après avoir confirmé l’absence de telles substances étrangères dans l’échantillon. Dans le cas d’un
spectromètre XRF de type mobile pour le mesurage après échantillonnage, se référer à 6.5.
Note 2 Pendant le mesurage, le spectromètre ne doit jamais être écarté du sol ciblé ou de l’échantillon en cours
d’analyse dans la cellule du spectromètre XRF de type mobile. Bien que la plupart des spectromètres soient munis
de verrouillages de sécurité automatiques qui arrêtent l’émetteur de rayons X si aucun retour de rayons X n’est
détecté, ces dispositifs peuvent mettre quelques secondes à fonctionner.
Procéder au mesurage et enregistrer les concentrations des éléments cibles. En plus de l’information
qualitative sur la nature des éléments présents, les niveaux de concentration peuvent être obtenus.
Note 3 Fondamentalement, le mesurage direct du sol mesure la surface du sol. Le mesurage du sol dans un godet
ou dans un sac mesure la couche superficielle du sol, proche du matériau du godet ou du sac.
Note 4 La décroissance du signal avec la profondeur est un facteur de confusion important dans l’obtention de
résultats semi-quantitatifs précis dans les sols, en particulier pour les éléments les plus légers. Le choix de
l’instrument adapté et la compréhension de ses capacités sont importants pour obtenir de bons résultats et les
interpréter de manière fiable.
6.5 Mesurage après échantillonnage
6.5.1 Préparation des échantillons
Si les échantillons ne sont pas adaptés au mesurage dans un spectromètre XRF de type mobile ou s’ils
nécessitent une meilleure homogénéisation, il convient alors de les soumettre à une préparation
supplémentaire, comme décrit ci-dessous.
Note 1 Les procédures sont décrites, par exemple, dans l’ISO 18400-201 pour le traitement préalable, y compris
la préparation d’un échantillon plus petit (essentiellement un sous-échantillon) à partir de l’échantillon d’origine
prélevé sur le terrain, et pour l’homogénéisation sur le terrain.
Prendre une masse de sol suffisante pour s’assurer que l’échantillon est représentatif du lieu de
prélèvement. Là où un grand échantillon est prélevé, il convient de prélever un sous-échantillon pour
constituer une portion d’essai représentative. Retirer de l’échantillon les matériaux étrangers et
concasser les agrégats en fines particules de sol en les pressant à l’aide d’une cuillère dans le plateau à
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échantillon si possible ou, pour les pierres plus dures ou les clastes, à l’aide d’un mortier et d’un pilon
fabriqués dans des matériaux inertes solides tels que la céramique, l’agate et la calcédoine.
Retirer les pierres et autres particules d’un diamètre supérieur à 2 mm environ (par exemple en
tamisant) et réduire la taille des agrégats de sol à des dimensions similaires. Homogénéiser l’échantillon
dans le récipient, par exemple en agitant.
Lors de l’utilisation d’un tamis (notamment ceux dont les mailles ne sont pas de 2 mm), il convient
d’observer attentivement la quantité et la nature de l’échantillon retenu sur le tamis.
Il convient que les matériaux retenus soient ensuite placés dans un récipient à échantillon, après avoir
été concassés ou pulvérisés si possible, et soumis à essai avec le spectromètre XRF. Si le matériau grossier
ne peut être directement concassé, il convient que des morceaux ou des clastes entiers soient soumis à
essai individuellement. S’il s’avère que ces matériaux grossiers contiennent des quantités significatives
de métaux faisant l’objet de l’évaluation, il convient de ne pas les retirer de l’échantillon.
Note 2 L’utilisation d’une taille de maille de 2 mm est définie en 5.4, mais l’utilisation du tamis est facultative. En
outre, l’utilisateur peut choisir d’utiliser une taille de maille différente (inférieure ou supérieure à 2 mm). Toutefois,
il est important de noter que les résultats de diagnostic rapide obtenus conformément aux recommandations du
présent document n’ont pas été validés pour une utilisation autre que celle d’un tamis d’une taille de maille de 2 mm.
Remplir un godet ou un sac à échantillon avec l’échantillon de sol préalablement traité. Taper plusieurs
fois le godet à échantillon sur une surface plane propre pour s’assurer que les particules de sol soient
bien tassées, mais voir la Note 3. Pour les échantillons humides ou argileux, presser le matériau dans le
godet en utilisant la cuillère. S’il y a des vides visibles sur le film au fond du godet, tasser à nouveau
l’échantillon de sol ou répéter le tapotement pour que l’échantillon de sol couvre de façon uniforme toute
la surface du film. Selon le type de sol, une compression de l’échantillon pour réduire les vides peut être
nécessaire pour améliorer les résultats.
Note 3 Le tapotement ou la vibration d’un échantillon partiellement compacté, de sables à grains fins et de
gravillons peut provoquer une redistribution des particules et entraîner une séparation des grains les plus fins ainsi
qu’une diminution de l’homogénéité de l’échantillon (notamment à la base et au sommet de l’échantillon), ce qui
conduit à des résultats instrumentaux non représentatifs. Le choix du lieu d’échantillonnage est toutefois plus
susceptible d’avoir un effet significatif sur les résultats des mesures XRF que la distribution ou la localisation des
particules dans une cellule à échantillon, provoquée par le tapotement et la vibration.
Note 4 La différence entre les résultats obtenus due au choix du lieu d’échantillonnage est liée à la variabilité
spatiale en fonction de la localisation et de la profondeur de la concentration (voire de la présence ou non) d’un
élément cible, y compris l’échelle d’une telle variabilité (par exemple, sur quelques centimètres ou des dizaines de
mètres). De telles « erreurs d’échantillonnage » dépassent largement les erreurs de mesure, que le mesurage soit
effectué en laboratoire ou sur le terrain à l’aide d’un spectromètre XRF suivant les procédures définies dans le
présent document. Il existe des procédures d’estimation et de contrôle des erreurs d’échantillonnage qui peuvent
être utilement adaptées lors de l’utilisation d’un spectromètre XRF sur site (voir l’ISO 18400-104:2018, Annexe C).
En cas d’utilisation d’un sac en plastique au lieu d’un godet, le sac doit être secoué ou moulé pour créer
une surface plate et lisse. Il est essentiel que l’échantillon présenté au spectromètre XRF soit bien mélangé
et non séparé afin de garantir des résultats précis. S’assurer qu’il n’y a pas de volume d’air dans le sac et
replier celui-ci pour envelopper fermement l’échantillon. Il convient que l’épaisseur de l’échantillon soit
d’au moins 10 mm, de préférence de 20 mm à 30 mm, afin de s’assurer que le matériau situé sous celui-
ci (une table, un plancher dans un bâtiment ou le sol) n’influence pas le résultat de l’essai.
Note 5 L’épaisseur minimale requise de l’échantillon peut être déterminée très simplement, pour écarter tout
doute, en plaçant un objet métallique dont la métallurgie est connue (de préférence un métal qui n’est pas détecté
dans le sol) sous l’échantillon en sac soumis à essai et en vérifiant si le métal apparaît dans les résultats.
Une teneur élevée en eau de l’échantillon donne lieu à une sous-estimation. Le séchage des échantillons
améliore la justesse des résultats. Si l’échantillon est humide, c’est-à-dire si la teneur en eau est
supérieure à 10 %, étaler une partie de l’échantillon trié et homogénéisé sur un plateau en plastique et
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attendre qu’elle sèche. Les échantillons peuvent être séchés de façon plus efficace à l’aide d’un dispositif
de séchage portable. Répéter le mesurage après séchage.
6.5.2 Mesurage des échantillons et calcul
Régler le spectromètre XRF suivant les instructions du fabricant.
Déterminer les concentrations des éléments cibles dans les échantillons préparés suivant la procédure
décrite en 6.5.1. Si un élément ciblé n’est pas détecté, ou s’il est détecté mais que sa concentration ne peut
pas être mesurée, il convient d’enregistrer ce résultat qualitatif.
Si les graphiques d’étalonnage spécifiques au site doivent être utilisés, il convient de réaliser les
mesurages dans les mêmes conditions de fonctionnement et de prélèvement que celles utilisées pour
l’étalonnage. Pour les échantillons présentant des effets de matrice significatifs ou non connus, il convient
d’adopter l’approche des paramètres fondamentaux (3.4).
Note Certains spectromètres XRF sont équipés d’un capteur d’image pour montrer ce qui se trouve dans la zone
cible du faiscea
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