Construction products - Assessment of release of dangerous substances - Determination of activity concentrations of radium-226, thorium-232 and potassium-40 in construction products using semiconductor gamma-ray spectrometry

This TS specifies a method for the determination of the activity concentrations of the radionuclides 226Ra, 232Th and 40K in construction products using semiconductor gamma-ray spectrometry. The standard describes sampling, test sample preparation, and the execution of the test. It includes background subtraction, energy and efficiency calibration, analysis of the spectrum, calculation of the activity concentrations with the associated uncertainties, the decision threshold and detection limit, and reporting of the results.

Bauprodukte - Bewertung der Freisetzung von gefährlichen Stoffen - Messung der spezifischen Aktivität von Radium-226, Thorium-232 und Kalium-40 in Bauprodukten mittels Halbleiter-Gammaspektrometrie

Dieses Dokument beschreibt ein Prüfverfahren zur Bestimmung der spezifischen Aktivitäten der Radionuklide Radium-226, Thorium-232 und Kalium-40 in Bauprodukten durch Halbleiter-Gammaspektrometrie.
Dieses Dokument beschreibt die Probenahme einer Laborprobe, die Probenvorbereitung und die Messung der Probe durch Halbleiter-Gammaspektrometrie. Dazu gehört die Hintergrundsubtraktion, Energie- und Effizienzkalibrierung, Analyse des Spektrums, Berechnung der spezifischen Aktivitäten mit den zugehörigen Unsicherheiten, der Erkennungsgrenze und Nachweisgrenze und Angabe der Prüfergebnisse. Die Vor-bereitung der Laborprobe aus der ursprünglichen Produktprobe liegt außerhalb des Anwendungsbereichs und wird in den Produktnormen beschrieben.
Dieses Dokument soll in ihrem Anwendungsbereich nicht produktspezifisch sein, allerdings gibt es eine begrenzte Anzahl produktspezifischer Elemente, wie die Vorbereitung der Laborprobe und die Trocknung der Prüfmenge. Das Verfahren eignet sich für Produktproben, die aus einzelnen oder multiplen Material-komponenten bestehen.

Produits de construction - Evaluation de l'émission de substances dangereuses - Détermination de l’activité du radium-226, du thorium-232 et du potassium-40 dans les produits de construction par spectrométrie gamma

Gradbeni proizvodi - Ocenjevanje sproščanja nevarnih snovi - Določevanje koncentracije aktivnosti radija Ra-226, torija Th-232 in kalija K-40 v gradbenih proizvodih s polprevodniško gama spektrometrijo

Ta tehnična specifikacija določa metodo za določevanje koncentracije aktivnosti radionuklidov 226Ra, 232Th in 40K v gradbenih proizvodih s polprevodniško gama spektrometrijo. Standard opisuje vzorčenje, pripravo preskusnih vzorcev in izvedbo preskusa. Vključuje odstranjevanje ozadja, umerjanje energije in učinkovitosti, analizo spektra, izračun koncentracije aktivnosti s povezanimi negotovostmi, prag odločanja in omejitev zaznavanja ter objavo rezultatov.

General Information

Status
Published
Public Enquiry End Date
04-Apr-2018
Publication Date
30-Jan-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Nov-2018
Due Date
25-Jan-2019
Completion Date
31-Jan-2019

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17216:2019
01-marec-2019
*UDGEHQLSURL]YRGL2FHQMHYDQMHVSURãþDQMDQHYDUQLKVQRYL'RORþHYDQMH
NRQFHQWUDFLMHDNWLYQRVWLUDGLMD5DWRULMD7KLQNDOLMD.YJUDGEHQLK
SURL]YRGLKVSROSUHYRGQLãNRJDPDVSHNWURPHWULMR

Construction products - Assessment of release of dangerous substances - Determination

of activity concentrations of radium-226, thorium-232 and potassium-40 in construction

products using semiconductor gamma-ray spectrometry
Bauprodukte - Bewertung der Freisetzung von gefährlichen Stoffen - Messung der
spezifischen Aktivität von Radium-226, Thorium-232 und Kalium-40 in Bauprodukten
mittels Halbleiter-Gammaspektrometrie
Produits de construction - Evaluation de l'émission de substances dangereuses -

Détermination de l’activité du radium-226, du thorium-232 et du potassium-40 dans les

produits de construction par spectrométrie gamma
Ta slovenski standard je istoveten z: CEN/TS 17216:2018
ICS:
13.020.99 Drugi standardi v zvezi z Other standards related to
varstvom okolja environmental protection
17.240 Merjenje sevanja Radiation measurements
91.100.01 Gradbeni materiali na Construction materials in
splošno general
SIST-TS CEN/TS 17216:2019 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 17216:2019
CEN/TS 17216
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
October 2018
TECHNISCHE SPEZIFIKATION
ICS 91.100.01
English Version
Construction products - Assessment of release of
dangerous substances - Determination of activity
concentrations of radium-226, thorium-232 and
potassium-40 in construction products using
semiconductor gamma-ray spectrometry

Produits de construction - Evaluation de l'émission de Bauprodukte - Bewertung der Freisetzung von

substances dangereuses - Détermination de l'activité gefährlichen Stoffen - Messung der spezifischen

du radium-226, du thorium-232 et du potassium-40 Aktivität von Radium-226, Thorium-232 und Kalium-

dans les produits de construction par spectrométrie 40 in Bauprodukten mittels Halbleiter-

gamma Gammaspektrometrie

This Technical Specification (CEN/TS) was approved by CEN on 14 May 2018 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to

submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS

available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in

parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17216:2018 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 4

Introduction .................................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 6

2 Normative references .................................................................................................................................... 6

3 Terms and definitions ................................................................................................................................... 6

4 Symbols and abbreviations ......................................................................................................................... 8

5 Principles of the test method ................................................................................................................... 11

6 Sampling and sample preparation ......................................................................................................... 11

6.1 Sampling hierarchy ..................................................................................................................................... 11

6.2 Sampling and sub-sampling ..................................................................................................................... 14

6.3 Test specimen/test portion preparation ............................................................................................. 14

7 Test procedure .............................................................................................................................................. 18

7.1 General ............................................................................................................................................................. 18

7.2 Measurement ................................................................................................................................................. 18

8 Processing the test data ............................................................................................................................. 21

8.1 General ............................................................................................................................................................. 21

8.2 Analysis of counting spectrum ................................................................................................................ 22

8.3 Calculating activity concentration ......................................................................................................... 22

8.4 Standard uncertainty .................................................................................................................................. 24

8.5 Decision threshold ....................................................................................................................................... 27

8.6 Detection limit ............................................................................................................................................... 27

9 Test report ...................................................................................................................................................... 29

Annex A (normative) Method for the determination of the radon-tightness of a test

specimen container ..................................................................................................................................... 31

A.1 Principle .......................................................................................................................................................... 31

A.2 Apparatus, equipment and reagents ..................................................................................................... 31

A.3 Test .................................................................................................................................................................... 31

A.4 Processing experimental data ................................................................................................................. 32

Annex B (normative) Preparation of standardized calibration sources ................................................. 35

B.1 Principle .......................................................................................................................................................... 35

B.2 Apparatus, equipment and reagents ..................................................................................................... 35

B.3 Test .................................................................................................................................................................... 35

Annex C (normative) Method for the determination of the activity concentration in a

composite product ....................................................................................................................................... 39

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Annex D (informative) Complementary photopeaks to verify the activity concentration in

the test specimen .......................................................................................................................................... 40

Annex E (informative) Method for the determination of the corrected number of pulses in a

photopeak (only to be used for completely stand-alone single peaks) .................................... 41

Bibliography ................................................................................................................................................................. 42

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European foreword

This document (CEN/TS 17216:2018) has been prepared by Technical Committee CEN/TC 351

“Construction products - Assessment of release of dangerous substances”, the secretariat of which is

held by NEN.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association.

According to the CEN/CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
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Introduction

This document is a Technical Specification developed under Mandate M/366 issued by the European

Commission in the framework of the “Construction Products Directive” 89/106/EEC. This document

addresses the part of Mandate M/366 which provides for the preparation of horizontal

measurement/test methods for the determination of the activity concentrations of the radionuclides

radium-226, thorium-232 and potassium-40 in construction products using gamma-ray spectrometry.

Mandate M/366 is a complement to the product mandates issued by the European Commission to CEN

under the Construction Products Directive (CPD). The harmonized product standards (hEN) developed

in CEN under mandates (and ETAs developed in EOTA for products or kits) specify construction

product(s) as placed on the market and address their intended conditions of use.

The information produced by applying this Technical Specification can be used for purposes of CE

marking and evaluation/attestation of conformity. Product specification, standardization of

representative sampling and procedures for any product-specific laboratory sample preparation are the

responsibility of product TCs and are not covered in this Technical Specification.

This Technical Specification supports existing regulations and standardized practices, and is based on

methods described in standards, such as ISO 10703 [1], ISO 18589-2 [2], ISO 18589-3 [3] and NEN 5697

[4]. In summary, the Technical Specification describes the following:
— sampling, sub-sampling and test specimen preparation;
— measurement using gamma-ray spectrometry;

— background subtraction, energy and efficiency calibration, analysis of the spectrum;

— calculation of activity concentrations with associated uncertainties;
— reporting of test results.

Determination of the activity concentration is based on the principles of gamma-spectrometry, and

procedures for all stages of the testing are provided in this document. Although the tested material

sample rarely reflects a product’s form under its intended conditions of use, the measured activity

concentration is an intrinsic property of the material, which does not vary with the construction

product’s form. Consequently, the test results reflect the radiation behaviour of the product under its

intended use. In addition, the Technical Specification is intended to be non product-specific in scope,

with only a limited number of product-specific elements.
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1 Scope

This document describes a test method for the determination of the activity concentrations of the

radionuclides radium-226, thorium-232 and potassium-40 in construction products using

semiconductor gamma-ray spectrometry.

This document describes sampling from a laboratory sample, sample preparation, and the sample

measurement by semiconductor gamma-ray spectrometry. It includes background subtraction, energy

and efficiency calibration, analysis of the spectrum, calculation of the activity concentrations with the

associated uncertainties, the decision threshold and detection limit, and reporting of the results. The

preparation of the laboratory sample from the initial product sample lies outside its scope and is

described in product standards.

This document is intended to be non product-specific in scope, however, there are a limited number of

product-specific elements such as the preparation of the laboratory sample and drying of the test

portion. The method is applicable to samples from products consisting of single or multiple material

components.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

EN 16687:2015, Construction products - Assessment of release of dangerous substances - Terminology

ISO 11929, Determination of the characteristic limits (decision threshold, detection limit and limits of the

confidence interval) for measurements of ionizing radiation - Fundamentals and application

ISO IEC Guide 98-3, Uncertainty of measurement - Part 3: Guide to the expression of uncertainty in

measurement (GUM, 1995)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
blank

volume of demineralized or distilled water that corresponds to the volume and geometry of the test

specimen
3.2
calibration source

sample with known radioactivity concentration and material properties that corresponds to the volume

and geometry of the test specimen
[SOURCE: EN 16687:2015, 4.4.2]
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3.3
composite sample

sample that consist of two or more material components, put together in appropriate portions, from

which the mean value of a desired characteristic may be obtained

[SOURCE: EN 16687:2015, 3.1.1; modified to read 'material components' instead of 'increments']

3.4
crushed material
sample material prepared by crushing a portion of the laboratory sample
[SOURCE: EN 16687:2015, 4.4.4]
3.5
dead time

time during which the measurement system is actually processing the signal and is not able to accept

the next signal
[SOURCE: EN 16687:2015, 4.4.3]
3.6
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
[SOURCE: EN 16687:2015, 3.2.1]

Note 1 to entry: When the laboratory sample is further prepared by subdividing, cutting, sawing, coring, mixing,

drying, grinding, and curing or by combinations of these operations, the result is the test sample. When no

preparation of the laboratory sample is required, the laboratory sample is the test sample. A test portion is

removed from the test sample for the performance of the test/ analysis or for the preparation of a test specimen.

Note 2 to entry: The laboratory sample is the final sample from the point of view of sample collection but it is

the initial sample from the point of view of the laboratory.
3.7
product sample

construction product taken in whole or in part at the factory, on the market or on the construction site

representative of the construction product
[SOURCE: EN 16687:2015, 3.1.4]
3.8
test portion

amount of the test sample taken for testing/ analysis purposes, usually of known weight or volume

[SOURCE: EN 16687:2015, 3.2.3]
3.9
test sample

sample, prepared from the laboratory sample from which test portions are removed for testing or for

analysis
[SOURCE: EN 16687:2015, 3.2.2]
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3.10
test specimen

test portion specially prepared for testing in a test facility in order to simulate the radiation behaviour

of the product under intended conditions of use
[SOURCE: EN 16687:2015, 3.2.4]
3.11
test specimen container

holder shaped like a beaker or a vessel that can be sealed and that is used to make determinations on

the test specimen
[SOURCE: EN 16687:2015, 4.4.5]
4 Symbols and abbreviations

For the purposes of this document, the following symbols, names of quantities and units apply.

Symbol Name of quantity Unit
a, b, c free parameters used in an e-power formula –
A the activity of the standardized calibration source j at energy E Bq
i;j i
b ordinal –
the average activity concentration of radionuclide i Bq/kg
C the activity concentration of radionuclide i in the test specimen k Bq/kg
i;k
# is the detection limit of radionuclide i of test specimen k Bq/kg
ik;
* is the decision threshold of radionuclide i of test specimen k Bq/kg
ik;
E energy used for determining radionuclide i keV
f ordinal –
i ordinal –
j ordinal –
k ordinal –
k the uncertainty coverage factor –
k the uncertainty coverage factor with a default value of 1,65 at α = 0,05 –
1−α
k the uncertainty coverage factor with a default value of 1,65 at β = 0,05 –
1−β
m the mass of matrix material j kg
j;mat
m the mass of sub sample k of standardized material j kg
j;k;stand
m the mass of the test specimen k kg
n number of test specimens –
N the corrected number of pulses in the photopeak –
N the number of pulses collected in channel q –
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Symbol Name of quantity Unit
the average number of pulses per channel before the peak –
the average number of pulses per channel after the peak –
N the net number of pulses in the photopeak that corresponds to energy E of –
i;j i
standardized calibration source j

N the number of pulses that is collected in the continuum under the photopeak when –

cont;k
counting the test specimen k

N the number of pulses that is collected in the continuum under the photopeak with –

cont;i;j;mat
energy Ei of matrix material j

Ncont;i;j;k;stand the number of pulses that is collected in the continuum under the photopeak with –

energy Ei of sub sample k of standardized material j

Ntot;i;j;mat the total number of pulses that is collected in the channels belonging to the –

photopeak with energy Ei of matrix material j

Ntot;i;j;k;stand the total number of pulses that is collected in the channels belonging to the –

photopeak with energy Ei of sub sample k of standardized material j

Ntot;k the total number of pulses that is collected in the channels belonging to the –

photopeak when counting the test specimen k
p ordinal –
q ordinal –

R the counting rate of the blank that is determined from the number of pulses that is s

cont;0
collected in the continuum under the photopeak

R the counting rate of the test specimen k that is determined from the number of pulses s

cont;k
that is collected in the continuum under the photopeak

R the counting rate in spectrum w that is determined from the number of pulses that is s

cont;w
collected in the continuum under the photopeak
R the corrected counting rate of the blank s
cor;0
R the corrected specific counting rate of matrix material j at energy E (s·kg)
cor;i;j;spec;mat i

Rcor;i;j;spec;stand the average specific corrected counting rate of all subsamples k of (s·kg)

standardized material j at energy E

R the corrected specific counting rate of sub sample k of standardized material jat (s·kg)

cor;i;j;k;spec;stand
energy E

R the corrected counting rate of the test specimen k that is determined for the s

cor;k
photopeak

R the corrected counting rate in spectrum w that is determined for the photopeak s

cor;w

Rtot;0 the total counting rate of the blank that is determined from the total number of pulses s

that is collected in the channels belonging to the photopeak

Rtot;k the total counting rate of the test specimen k that is determined from the total s

number of pulses that is collected in the channels belonging to the photopeak

Rtot;w the total counting rate in spectrum w that is determined from the total number of s

pulses that is collected under the photopeak
S the total radon production in the building material Bq/s
t the counting time s
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Symbol Name of quantity Unit
t the counting time of the blank corrected for the dead time s
t the counting time of the calibration source j corrected for the dead time s
tj;mat the counting time of matrix material j corrected for the dead time s

tj;k;stand the counting time of sub sample k of standardized material j corrected for the dead s

time
tk the counting time of the test specimen k corrected for the dead time s

tw the counting time of the gas sample in spectrum w corrected for the dead time s

u the uncertainty is the uncertainty in the free parameter a of the radon-tightness test s

u the external uncertainty of the mass activity of radionuclide i Bq/kg
i;ext

ui;ie is the internal or external uncertainty of the activity of radionuclide i Bq/kg

ui;int the internal uncertainty of the mass activity of radionuclide i Bq/kg
u the uncertainty of radionuclide i of the test specimen k Bq/kg
i;k
u the total uncertainty of the activity of radionuclide i Bq/kg
i,tot
u(Rcor;w) the uncertainty of the corrected counting rate Rcor;w Bq/kg
V the volume m
w ordinal –
α the probability of a first order error with a default value of 0,05 –
β the probability of a second order error with a default value of 0,05 –

εi;j the radionuclide-specific counting efficiency for energy Ei and the standardized (Bq·s)

calibration source j

εi;k the radionuclide-specific counting efficiency for energy Ei and a counting (Bq·s)

sample with mass m
ηk the correction factor for dry mass of the test specimen k –
λl the tightness of a test specimen container s
λ the decay constant of radon-222 s
ν the coefficient of variation of the corrected specific counting rate of –
i;j;ext
sub sample k of standardized material j at energy Ei
ν the coefficient of variation due to radon-222 leakage from the test specimen –
i;l
container
ν the total relative uncertainty of the activity of radionuclide i –
i,tot
ν the relative uncertainty in the counting efficiency of radionuclide i –
i;ε
νi;ρ the relative uncertainty in the density correction of radionuclide i –
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5 Principles of the test method

The activity concentrations of the gamma-emitting radionuclides in construction products are

determined using gamma-ray spectrometry. Activity concentration is a material-property and not a

function of the physical form of a construction product.

The activity of gamma-emitting radionuclides present in the test specimen is based on the analysis of

the energies and the peak areas obtained from the full-energy peaks of the gamma lines that allow the

identification and the quantification of the radionuclides.

The test method requires accurate energy and efficiency calibrations. Such calibration is performed

using a calibration material with a known activity source that is similar in chemical composition and

density to the materials that are to be tested. The calibration is based on a pre-selected set of

photopeaks used for the determination of the activity concentration. Selected photopeaks are either

emitted by the radionuclide itself or by one of its progeny nuclides.

The activity concentration is measured using a homogeneous, mostly granular, test specimen held in a

container with a predefined geometry. This determination, requiring as it does a test specimen of

granular material to be presented to the spectrometer, will only rarely reflect a product's form under its

intended conditions of use. Nevertheless, because the activity concentration is an intrinsic material

property, the test results will simulate the radiation behaviour of the product under its intended

conditions of use.

For radium-226 and thorium-232 the activity concentration is determined using a progeny nuclide,

while for potassium-40 the concentration is based on the photopeak from the nuclide itself. In those

cases where the activity is determined using a progeny nuclide, a secular equilibrium between the

progeny nuclide and its originating nuclide is necessary. To reach such equilibrium the test specimen is

stored in a radon-tight container for a period of at least three weeks in order to ensure there is no

degradation in the equilibrium due to a leakage of radon activity.

Despite the required waiting time of three weeks a disequilibrium in the thorium-232 decay chain can

be present. Such disequilibrium is caused by different dissolution ratios between thorium and radium,

particular hydrogeological history and effects of industrial processes. In case of such disequilibrium the

thorium-232 activity is approximated.

NOTE 1 Thorium-232 with a half-life of 1,41 × 10 years is the parent nuclide of the thorium decay chain.

Thorium-232 has a line at 63,81 keV with a very low emission probability of 0,263 % which overlaps a line of

thorium-234 at 63,28 keV with a higher emission probability of 4,1 %, so that thorium-232 cannot be determined

directly by gamma spectrometry. Determination through its decay radionuclides actinium-228, lead-212 and

thallium-208 can be performed only if one assumes that these radionuclides are in radioactive equilibrium with

thorium-232.

NOTE 2 Where the activity concentration between thorium-228 and radium-228 is considerably different

alternative measurement techniques or procedures to determine the thorium-232 more accurately are available

but are outside the scope of this document.
6 Sampling and sample preparation
6.1 Sampling hierarchy

A diagram of the sampling hierarchy (Figure 1) is presented and followed by a sketch with a physical

description of the samples (Figure 2) in support of the relevant definitions given in Clause 3.

NOTE The test method described in this Technical Specification starts with a laboratory sample received by

the laboratory. The preparation of a product sample lies outside the scope of this Technical Specification and is

described in product standards.
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Figure 1 — Diagram of the sample hierarchy
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Key
1 sampling
a) Product sample – sample of a construction product
b) Composite sample – sample consisting of a number of components
Key
1 laboratory
c) Laboratory sample – sample sent to or received by the laboratory
d) Test sample – sample to provide material for all analytical testing
e) Test portion – sample for general analytical testing
f) Test specimen – sample for radiation testing
Figure 2 — Sketch of the samples with a physical description
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6.2 Sampling and sub-sampling
6.2.1 General
The method starts with a laboratory sample receive
...

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