Air quality — Bulk materials — Part 1: Sampling and qualitative determination of asbestos in commercial bulk materials

This part of ISO 22262 specifies methods for sampling bulk materials and identification of asbestos in commercial bulk materials. This part of ISO 22262 specifies appropriate sample preparation procedures and describes in detail the procedure for identification of asbestos by polarized light microscopy and dispersion staining. This part of ISO 22262 also specifies simple procedures for separation of asbestos fibres from matrix materials such as asphalt, cement, and plastics products. Optionally, identification of asbestos can be carried out using scanning electron microscopy or transmission electron microscopy with energy dispersive X-ray analysis. Information is also provided on common analytical problems, interferences and other types of fibre that may be encountered in the analysis. This part of ISO 22262 is applicable to qualitative identification of asbestos in specific types of manufactured asbestos-containing products and commercial minerals. This part of ISO 22262 is applicable to the analysis of fireproofing, thermal insulation, and other manufactured products or minerals in which asbestos fibres can readily be separated from matrix materials for identification. NOTE This part of ISO 22262 is intended for use by microscopists who are familiar with polarized light microscopy methods and the other analytical procedures specified (References [16]?[19]). It is not the intention of this part of ISO 22262 to provide instruction in the fundamental analytical techniques.

Qualité de l'air — Matériaux solides — Partie 1: Échantillonnage et dosage qualitatif de l'amiante dans les matériaux solides d'origine commerciale

La présente partie de l'ISO 22262 spécifie les méthodes d'échantillonnage de matériaux solides et d'identification de l'amiante dans les matériaux solides d'origine commerciale. La présente partie de l'ISO 22262 spécifie les procédures appropriées de préparation de l'échantillon et décrit en détail la procédure d'identification de l'amiante par microscopie en lumière polarisée et dispersion de coloration. La présente partie de l'ISO 22262 spécifie également des procédures simples de séparation des fibres d'amiante des matériaux matriciels tels que les produits bitumineux, à base de ciment et de plastique. L'identification de l'amiante peut également être effectuée en utilisant la microscopie électronique à balayage ou la microscopie électronique à transmission avec analyse en dispersion d'énergie des rayons X. Des informations sont également données sur les problèmes habituels d'analyse, les interférences et autres types de fibres susceptibles d'être rencontrés au cours de l'analyse. La présente partie de l'ISO 22262 est applicable à l'identification qualitative de l'amiante dans des types spécifiques de produits manufacturés et de minéraux commercialisés contenant de l'amiante. La présente partie de l'ISO 22262 est applicable à l'analyse des matériaux ignifuges, produits d'isolation thermique et autres produits manufacturés ou minéraux dans lesquels les fibres d'amiante peuvent être facilement séparées des matériaux matriciels pour être identifiées. NOTE La présente partie de l'ISO 22262 est destinée à être utilisée par les microscopistes familiarisés avec les méthodes de microscopie en lumière polarisée et par les personnes chargées de l'analyse, expérimentées et familiarisées avec les procédures d'analyse spécifiées (Références [16] à [19]). L'objectif de la présente partie de l'ISO 22262 n'est pas de fournir des informations sur les techniques d'analyse fondamentale.

Kakovost zraka - Razsuti materiali - 1. del: Vzorčenje in kvantitativno določevanje azbesta v razsutih materialih za prodajo

Ta del standarda ISO 22262 določa metode za vzorčenje razsutih materialov in določevanje azbesta v razsutih materialih za prodajo. Ta del standarda ISO 22262 določa ustrezne postopke za pripravo vzorcev in podrobno opisuje postopek za določevanje azbesta s polarizirano svetlobno mikroskopijo in disperzijskim obarvanjem. Ta del standarda ISO 22262 določa tudi preproste postopke za ločevanje azbestnih vlaken od matričnih materialov, kot so asfalt, cement in plastični izdelki. Po izbiri se lahko določevanje azbesta izvede tudi z uporabo vrstične elektronske mikroskopije ali presevne mikroskopije z energijsko-disperzivno rentgensko analizo. Zagotovljene so tudi informacije v zvezi s splošnimi analiznimi težavami, motnjami in drugimi vrstami vlaken, do katerih lahko pride med analizo. Ta del standarda ISO 22262 se uporablja za kvalitativno določevanje azbesta v posebnih vrstah proizvedenih izdelkov in mineralov za prodajo, ki vsebujejo azbest. Ta del standarda ISO 22262 se uporablja za analizo izdelkov ali mineralov za odpornost na ogenj in toplotno izolacijo ter drugih proizvedenih izdelkov ali mineralov, v katerih je mogoče azbestna vlakna preprosto ločiti od matričnih materialov za določevanje.

General Information

Status
Published
Publication Date
28-Jun-2012
Current Stage
9020 - International Standard under periodical review
Start Date
15-Apr-2017
Completion Date
15-Jul-2022

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INTERNATIONAL ISO
STANDARD 22262-1
First edition
2012-07-01
Air quality — Bulk materials —
Part 1:
Sampling and qualitative determination of
asbestos in commercial bulk materials
Qualité de l’air — Matériaux solides —
Partie 1: Échantillonnage et dosage qualitatif de l’amiante dans les
matériaux solides d’origine commerciale
Reference number
ISO 22262-1:2012(E)
ISO 2012
---------------------- Page: 1 ----------------------
ISO 22262-1:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s

member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 22262-1:2012(E)
Contents Page

Foreword ............................................................................................................................................................................. v

Introduction .......................................................................................................................................................................vi

1 Scope ...................................................................................................................................................................... 1

2 Terms and definitions ......................................................................................................................................... 1

3 Symbols and abbreviated terms ..................................................................................................................... 7

4 Principle ................................................................................................................................................................. 8

4.1 General ................................................................................................................................................................... 8

4.2 Substance determination .................................................................................................................................. 8

4.3 Type of sample ..................................................................................................................................................... 8

4.4 Range ...................................................................................................................................................................... 8

4.5 Limit of detection ................................................................................................................................................. 9

4.6 Limitations of PLM in the detection of asbestos ........................................................................................ 9

5 Sample collection ................................................................................................................................................ 9

5.1 Requirements ....................................................................................................................................................... 9

5.2 Procedure ............................................................................................................................................................10

6 Sample preparation ...........................................................................................................................................14

6.1 General .................................................................................................................................................................14

6.2 Removal of organic materials by ashing ....................................................................................................14

6.3 Removal of soluble constituents by acid treatment ................................................................................14

6.4 Sedimentation and flotation ...........................................................................................................................14

6.5 Combination of gravimetric reduction procedures ..................................................................................14

7 Analysis by PLM ................................................................................................................................................14

7.1 Requirements .....................................................................................................................................................14

7.2 Qualitative analysis by PLM ...........................................................................................................................19

8 Analysis by SEM ................................................................................................................................................29

8.1 General .................................................................................................................................................................29

8.2 Requirements .....................................................................................................................................................29

8.3 Calibration ...........................................................................................................................................................29

8.4 Sample preparation ...........................................................................................................................................30

8.5 Qualitative analysis by SEM ...........................................................................................................................30

9 Analysis by transmission electron microscope .......................................................................................31

9.1 General .................................................................................................................................................................31

9.2 Requirements .....................................................................................................................................................32

9.3 Calibration ...........................................................................................................................................................32

9.4 Sample preparation ...........................................................................................................................................33

9.5 Qualitative analysis by TEM ...........................................................................................................................33

10 Test report ...........................................................................................................................................................35

Annex A (normative) Types of commercial asbestos-containing material .......................................................36

Annex B (normative) Interference colour chart ........................................................................................................40

Annex C (normative) Dispersion staining charts .....................................................................................................41

Annex D (normative) Asbestos identification by PLM and dispersion staining in

commercial materials .......................................................................................................................................43

Annex E (normative) Asbestos identification by SEM in commercial materials .............................................52

Annex F (normative) Asbestos identification by TEM in commercial materials .............................................58

Annex G (informative) Example of sampling record ...............................................................................................67

Annex H (informative) Example of test report ...........................................................................................................68

© ISO 2012 – All rights reserved iii
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ISO 22262-1:2012(E)

Bibliography .....................................................................................................................................................................69

iv © ISO 2012 – All rights reserved
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ISO 22262-1:2012(E)
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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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

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

ISO 22262-1 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 3, Ambient

atmospheres.

ISO 22262 consists of the following parts, under the general title Air quality — Bulk materials:

— Part 1: Sampling and qualitative determination of asbestos in commercial bulk materials

The following part is under preparation:

— Part 2: Quantitative determination of asbestos by gravimetric and microscopical methods

© ISO 2012 – All rights reserved v
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ISO 22262-1:2012(E)
Introduction

In the past, asbestos was used in a wide range of products. Three varieties of asbestos found extensive

commercial application. Chrysotile accounted for approximately 95 % of consumption, and this variety is

therefore likely to be encountered most frequently during the analysis of samples. Materials containing high

proportions of chrysotile asbestos were used in buildings and in industry for fireproofing, thermal insulation,

and acoustic insulation. Chrysotile was also used to reinforce materials to improve fracture and bending

characteristics. A large proportion of the chrysotile produced was used in asbestos–cement products. These

include flat sheets, tiles and corrugated sheets for roofing, pipes and open troughs for the collection of rainwater,

as well as pressure pipes for supply of potable water. Chrysotile was also incorporated into products such as

decorative coatings and plasters, glues, sealants and resins, floor tiles, gaskets, and road paving. In some

products, chrysotile was incorporated to modify rheological properties, e.g. in the manufacture of ceiling tile

panels and oil drilling muds. Long textile grade chrysotile fibre was also used to manufacture woven, spun,

felted and paper products.

Amosite and crocidolite accounted for almost all of the remaining asbestos use. Amosite was widely used as

fireproofing and in thermal insulation products, e.g. pipe coverings and insulating boards. Crocidolite was also

used as fireproofing and in thermal insulation products, but was particularly prized because it is highly resistant

to acids, flexible enough to be spun and has high tensile strength for reinforcement. Crocidolite found application

as a reinforcing fibre in acid containers such as those used for lead–acid batteries, in high-performance textiles

and gaskets, and was particularly important for the manufacture of high-pressure asbestos cement pipes for

delivery of potable water.

Three other types of asbestos are currently regulated. Materials containing commercial anthophyllite are

relatively rare, but they have also been used as a filler and reinforcing fibre in composite materials, and as

a filtration medium. Tremolite asbestos and actinolite asbestos were not extensively used commercially, but

some occurrences of tremolite asbestos in surfacing materials and fireproofing have been found in Japan.

Tremolite asbestos and actinolite asbestos sometimes occur as contaminants of other commercial minerals.

Other minerals can also occur as asbestos. For example, richterite asbestos and winchite asbestos occur

at mass fractions between 0,1 % and 6 % associated with vermiculite, formerly mined at Libby, Montana,

USA. Vermiculite from this source was widely distributed and is often found as loose fill insulation and as a

constituent in a range of construction materials and fireproofing.

While the asbestos mass fraction in some products can be very high and in some cases approach 100 %, in

other products the mass fractions of asbestos used were significantly lower and often between 1 % and 15 %.

In some ceiling tile panels, the mass fraction of asbestos used was close to 1 %. There are only a few known

materials in which the asbestos mass fraction used was less than 1 %. Some adhesives, sealing compounds

and fillers were manufactured in which asbestos mass fractions were lower than 1 %. There are no known

materials in which asbestos was intentionally added at mass fractions lower than 0,1 %.

In this part of ISO 22262, procedures for collection of samples and qualitative analysis of commercial bulk

materials for the presence of asbestos are specified. The primary method used to identify asbestos is polarized

light microscopy. Because of the wide range of matrix materials into which asbestos was incorporated, polarized

light microscopy cannot provide reliable analysis of all types of asbestos-containing materials in untreated

samples. The applicability of polarized light microscopy can be extended by the use of simple treatments such

as ashing and treatment with acid. Optionally, either scanning electron microscopy or transmission electron

microscopy may be used as an alternative or confirmatory method to identify asbestos.

Although this part of ISO 22262 specifies that, optionally, a visual estimate of the asbestos mass fraction within

very broad ranges may also be made, it is recognized that the accuracy and reproducibility of such estimates

is very limited. Quantitative determination of the asbestos content can be needed for a number of reasons,

e.g. assessment and management of the risk from asbestos materials in buildings or to comply with regulatory

definitions for asbestos-containing materials. The necessity to quantify asbestos in a material depends on the

maximum mass fraction that has been adopted by the jurisdiction to define an asbestos-containing material

for the purpose of regulation. Definitions range from “any asbestos” to 0,1 %, 0,5 % or 1 %. For jurisdictions in

which an asbestos-containing material is defined as one containing “any asbestos”, a particular problem is how

to determine whether a material does not contain asbestos, since all methods have limits of detection.

vi © ISO 2012 – All rights reserved
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ISO 22262-1:2012(E)

For practical purposes, since no known commercial materials exist in which commercial asbestos was

intentionally added at mass fractions lower than 0,1 %, this part of ISO 22262 specifies that samples be

classified as asbestos-containing (i.e. containing more than 0,1 % asbestos) if either chrysotile, amosite,

crocidolite or anthophyllite, or any of these varieties in combination, is detected in the analysis. When the

definition of an asbestos-containing material is either 0,5 % or 1 %, depending on the nature of the product, it

is often necessary to proceed to other parts of this International Standard in order to quantify the asbestos for

the purpose of defining the regulatory status of the material.

The occurrence of tremolite, actinolite or richterite/winchite in a material is usually a consequence of natural

contamination of the constituents, and the detection of these minerals does not necessarily indicate that

the mass fraction is more than 0,1 % asbestos. Accordingly, determination of the regulatory status of these

materials by any of the criteria can often be achieved only by quantitative analysis. Since these minerals were

not specifically mined and utilized for their fibrous properties, they may also occur in materials as either non-

asbestiform or asbestiform analogues, or as mixtures of both. Evaluation of these types of material may require

a more detailed analysis.

Simple analytical procedures such as polarized light microscopy are not capable of detecting or reliably

identifying asbestos in some types of commercial products containing asbestos, either because the fibres are

below the resolution of optical microscopy or because the matrix material adheres too strongly to the fibres.

For these types of product, it may be necessary to utilize electron microscopy.
For a list of parts of this International Standard, see the Foreword.
[11] [13]

The method specified in this part of ISO 22262 is based on MDHS 77, VDI 3866 Part 1, VDI 3866 Part

[14] [15] [8] [10] [12]
4, , VDI 3866 Part 5, , AS 4964-2004, EPA/600/R-93/116, and NF X46-020:2008.
© ISO 2012 – All rights reserved vii
---------------------- Page: 7 ----------------------
INTERNATIONAL STANDARD ISO 22262-1:2012(E)
Air quality — Bulk materials — Part 1: Sampling and qualitative
determination of asbestos in commercial bulk materials

IMPORTANT — The electronic file of this document contains colours which are considered to be

useful for the correct understanding of the document. Users should therefore consider printing this

document using a colour printer.
1 Scope

This part of ISO 22262 specifies methods for sampling bulk materials and identification of asbestos in commercial

bulk materials. This part of ISO 22262 specifies appropriate sample preparation procedures and describes in

detail the procedure for identification of asbestos by polarized light microscopy and dispersion staining.

This part of ISO 22262 also specifies simple procedures for separation of asbestos fibres from matrix materials

such as asphalt, cement, and plastics products. Optionally, identification of asbestos can be carried out using

scanning electron microscopy or transmission electron microscopy with energy dispersive X-ray analysis.

Information is also provided on common analytical problems, interferences and other types of fibre that may

be encountered in the analysis.

This part of ISO 22262 is applicable to qualitative identification of asbestos in specific types of manufactured

asbestos-containing products and commercial minerals. This part of ISO 22262 is applicable to the analysis

of fireproofing, thermal insulation, and other manufactured products or minerals in which asbestos fibres can

readily be separated from matrix materials for identification.

NOTE This part of ISO 22262 is intended for use by microscopists who are familiar with polarized light microscopy

methods and the other analytical procedures specified (References [16]–[19]). It is not the intention of this part of ISO 22262

to provide instruction in the fundamental analytical techniques.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
achromat

microscope objective in which chromatic aberration is corrected for two wavelengths and spherical aberration

and other aperture-dependent defects are minimized for one other wavelength (usually about 550 nm)

EXAMPLE One wavelength less than about 500 nm, the other greater than about 600 nm.

NOTE This term does not imply any degree of correction for curvature of image field; coma and astigmatism are

minimized for wavelengths within the achromatic range.
[3]
[ISO 10934-1:2002, 2.6]
2.2
acicular

shape shown by an extremely slender crystal with cross-sectional dimensions which are small relative to its

length, i.e. needle-like
[4]
[ISO 13794:1999, 2.1]
2.3
alpha refractive index
lowest refractive index exhibited by a fibre
© ISO 2012 – All rights reserved 1
---------------------- Page: 8 ----------------------
ISO 22262-1:2012(E)
2.4
amphibole

group of rock-forming ferromagnesium silicate minerals, closely related in crystal form and composition, and

having the nominal formula:
A B C T O (OH,F,Cl)
0-1 2 5 8 22 2
where
A is K, Na
B is Fe , Mn, Mg, Ca, Na
3+ 2+
C is Al, Cr, Ti, Fe , Mg, Fe
T is Si, Al, Cr, Fe , Ti

NOTE In some varieties of amphibole, these elements can be partially substituted by Li, Pb, or Zn. Amphibole is

characterized by a cross-linked double chain of Si-O tetrahedra with a silicon:oxygen ratio of 4:11, by columnar or fibrous

prismatic crystals and by good prismatic cleavage in two directions parallel to the crystal faces and intersecting at angles

of about 56° and 124°.
[4]
[ISO 13794:1999, 2.2]
2.5
amphibole asbestos
amphibole in an asbestiform habit
[4]
[ISO 13794:1999, 2.3]
2.6
analyser

polar used after the object to determine optical effects produced by the object on the light, polarized or

otherwise, with which it is illuminated
NOTE It is usually positioned between the objective and the primary image plane.
[3]
[ISO 10934-1:2002, 2.117.1]
2.7
anisotropy
state or quality of having different properties along different axes

EXAMPLE An anisotropic transparent particle can show different refractive indices with the vibration direction of

incident light.
2.8
asbestiform

specific type of mineral fibrosity in which the fibres and fibrils possess high tensile strength and flexibility

[4]
[ISO 13794:1999, 2.6]
2.9
asbestos

term applied to a group of silicate minerals belonging to the serpentine and amphibole groups which have

crystallized in the asbestiform habit, causing them to be easily separated into long, thin, flexible, strong fibres

when crushed or processed

NOTE 1 The Chemical Abstracts Service Registry Numbers of the most common asbestos varieties are: chrysotile

(12001-29-5), crocidolite (12001-28-4), grunerite asbestos (amosite) (12172-73-5), anthophyllite asbestos (77536-67-5),

tremolite asbestos (77536-68-6) and actinolite asbestos (77536-66-4).
2 © ISO 2012 – All rights reserved
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ISO 22262-1:2012(E)
[4]
[ISO 13794:1999, 2.7]

NOTE 2 Other varieties of asbestiform amphibole, such as richterite asbestos and winchite asbestos (Reference [20]),

are also found in some products such as vermiculite and talc.
2.10
aspect ratio
ratio of length to width of a particle
[4]
[ISO 13794:1999, 2.10]
2.11
Bertrand lens

intermediate lens which transfers an image of the back focal plane of the objective into the primary image plane

NOTE The Bertrand lens is used for conoscopic observation in polarized light microscopy and for adjustment of the

microscope illuminating system, especially in phase-contrast and modulation-contrast microscopy.

[3]
[ISO 10934-1:2002, 2.87.2]
2.12
birefringence

quantitative expression of the maximum difference in refractive index due to double refraction

[3]
[ISO 10934-1:2002, 2.16]
2.13
camera length

equivalent projection length between the specimen and its electron diffraction pattern, in the absence of lens action

[4]
[ISO 13794:1999, 2.12]
2.14
chrysotile
fibrous mineral of the serpentine group which has the nominal composition:
Mg Si O (OH)
3 2 5 4

NOTE Most natural chrysotile deviates little from this nominal composition. In some varieties of chrysotile, minor

3+ 3+ 2+ 3+ 2+ 2+ 2+

substitution of silicon by Al may occur. Minor substitution of magnesium by Al , Fe , Fe , Ni , Mn and Co may

also be present. Chrysotile is the most prevalent type of asbestos.
[4]
[ISO 13794:1999, 2.13]
2.15
cleavage
breaking of a mineral along one of its crystallographic directions
[4]
[ISO 13794:1999, 2.14]
2.16
cleavage fragment
fragment of a crystal that is bounded by cleavage faces

NOTE Crushing of non-asbestiform amphibole generally yields elongated fragments that conform to the definition of

a fibre, but rarely have aspect ratios exceeding 30:1.
2.17
crossed polars

state in which the polarization directions of the polars (polarizer and analyser) are mutually perpendicular

[3]
[ISO 10934-1:2002, 2.117.2]
© ISO 2012 – All rights reserved 3
---------------------- Page: 10 ----------------------
ISO 22262-1:2012(E)
2.18
d-spacing
distance between identical adjacent and parallel planes of atoms in a crystal
[4]
[ISO 13794:1999, 2.18]
2.19
dispersion
variation of refractive index with wavelength of light
[1]
[ISO 7348:1992, 05.03.26]
2.20
dispersion staining

effect produced when a transparent object is immersed in a surrounding medium, the refractive index of which

is equal to that of the object at a wavelength in the visible range, but which has a significantly higher optical

dispersion than the object

NOTE Only the light refracted at the edges of the object is imaged, and this gives rise to colours at the interface

between the object and the surrounding medium. The particular colour is a measure of the wavelength at which the

refractive index of the object and that of the medium are equal.
2.21
electron diffraction

technique in electron microscopy by which the crystal structure of a specimen is examined

[4]
[ISO 13794:1999, 2.19]
2.22
electron scattering power

extent to which a thin layer of substance scatters impinging electrons from their original directions

[4]
[ISO 13794:1999, 2.20]
2.23
energy dispersive X-ray analysis
EDXA

measurement of the energies and intensities of X-rays by use of a solid-state detector and multichannel

analyser system
[4]
[ISO 13794:1999, 2.22]
2.24
eucentric

condition in which the area of interest of an object is placed on a tilting axis, at the intersection of the electron

beam with that axis, and is in the plane of focus
[4]
[ISO 13794:1999, 2.23]
2.25
extinction

condition in which an optically anisotropic object appears dark when observed between crossed polars

[3]
[ISO 10934-1:2002, 2.51]

NOTE Extinction occurs when the vibration directions of the crystal are parallel to the vibration directions in the

polarizer and analyser.
2.26
extinction angle

angle between the extinction position and the position at which the length of a fibre is parallel to the polarizer

or analyser vibration directions
4 © ISO 2012 – All rights reserved
---------------------- Page: 11 ----------------------
ISO 22262-1:2012(E)
2.27
fibril

single fibre of asbestos which cannot be further separated longitudinally into smaller components without

losing its fibrous properties or appearances
[4]
[ISO 13794:1999, 2.25]
2.28
fibre
elongated particle which has parallel or stepped sides
[4]
[ISO 13794:1999, 2.26]

NOTE For the purposes of this part of ISO 22262, a fibre is defined to have an aspect ratio greater than or equal to 3:1.

2.29
fibre bundle

structure composed of parallel, smaller diameter fibres attached along their lengths

NOTE A fibre bundle may exhibit diverging fibres at one or both ends.
[4]
[ISO 13794:1999, 2.27]
2.30
gamma refractive index
highest refractive index exhibited by a fibre
2.31
habit

characteristic crystal growth form, or combination of these forms, of a mineral, including characteristic

irregularities
[4]
[ISO 13794:1999, 2.30]
2.32
high-efficiency particulate air filter
HEPA
filter that is at least 99,97 % efficient by volume on 0,3 µm particles
[6]
[ISO 14952-1:2003, 2.13]
2.33
isotropic
having the same properties in all directions
[5]
[ISO 14686:2003, 2.23]
2.34
Köhler illumination

method of illuminating specimens in which an image of the illumination source is projected by a collector into

the plane of the aperture diaphragm in the front focal plane of the condenser, which then projects an image of

an illuminated field diaphragm at the opening of the collector into the specimen plane

2.35
lamda zero

matching wavelength corresponding to the dispersion staining colour shown by a particle in an immersion medium

NOTE At this wavelength, the particle and the immersion medium have the same refractive index.

© ISO 2012 – All rights reserved 5
---------------------- Page: 12 ----------------------
ISO 22262-1:2012(E)
2.36
matrix
material in a laboratory sample within which fibres are dispersed
2.37
Miller index

set of either three or four integer numbers used to specify the orientation of a crystallographic plane in relation

to the crystal axes
[4]
[ISO 13794:1999, 2.33]
2.38
pleochroism

property of an optically anisotropic medium by which it exhibits different brightness and/or colour for different

directions of light propagation, or for different vibrations, on account of variation in selective spectral absorption

of transmitted light
2.39
polarized light

light in which the vibrations are partially or completely suppressed in certain directions at any given instant

NOTE The vector of vibration may describe a linear, circular or elliptical shape.

[3]
[ISO 10934-1:2002, 2.88.1]
2.40
polarizer
polar placed in the light path before the object
[3]
[ISO 10934-1:2002, 2.117.4]
2.41
polar
device whic
...

SLOVENSKI STANDARD
SIST ISO 22262-1:2013
01-april-2013

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Air quality - Bulk materials - Part 1: Sampling and qualitative determination of asbestos in

commercial bulk materials

Qualité de l'air - Matériaux solides - Partie 1: Échantillonnage et dosage qualitatif de

l'amiante dans les matériaux solides d'origine commerciale
Ta slovenski standard je istoveten z: ISO 22262-1:2012
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST ISO 22262-1:2013 en,fr

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

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SIST ISO 22262-1:2013
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SIST ISO 22262-1:2013
INTERNATIONAL ISO
STANDARD 22262-1
First edition
2012-07-01
Air quality — Bulk materials —
Part 1:
Sampling and qualitative determination of
asbestos in commercial bulk materials
Qualité de l’air — Matériaux solides —
Partie 1: Échantillonnage et dosage qualitatif de l’amiante dans les
matériaux solides d’origine commerciale
Reference number
ISO 22262-1:2012(E)
ISO 2012
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SIST ISO 22262-1:2013
ISO 22262-1:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s

member body in the country of the requester.
ISO copyright office
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Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
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SIST ISO 22262-1:2013
ISO 22262-1:2012(E)
Contents Page

Foreword ............................................................................................................................................................................. v

Introduction .......................................................................................................................................................................vi

1 Scope ...................................................................................................................................................................... 1

2 Terms and definitions ......................................................................................................................................... 1

3 Symbols and abbreviated terms ..................................................................................................................... 7

4 Principle ................................................................................................................................................................. 8

4.1 General ................................................................................................................................................................... 8

4.2 Substance determination .................................................................................................................................. 8

4.3 Type of sample ..................................................................................................................................................... 8

4.4 Range ...................................................................................................................................................................... 8

4.5 Limit of detection ................................................................................................................................................. 9

4.6 Limitations of PLM in the detection of asbestos ........................................................................................ 9

5 Sample collection ................................................................................................................................................ 9

5.1 Requirements ....................................................................................................................................................... 9

5.2 Procedure ............................................................................................................................................................10

6 Sample preparation ...........................................................................................................................................14

6.1 General .................................................................................................................................................................14

6.2 Removal of organic materials by ashing ....................................................................................................14

6.3 Removal of soluble constituents by acid treatment ................................................................................14

6.4 Sedimentation and flotation ...........................................................................................................................14

6.5 Combination of gravimetric reduction procedures ..................................................................................14

7 Analysis by PLM ................................................................................................................................................14

7.1 Requirements .....................................................................................................................................................14

7.2 Qualitative analysis by PLM ...........................................................................................................................19

8 Analysis by SEM ................................................................................................................................................29

8.1 General .................................................................................................................................................................29

8.2 Requirements .....................................................................................................................................................29

8.3 Calibration ...........................................................................................................................................................29

8.4 Sample preparation ...........................................................................................................................................30

8.5 Qualitative analysis by SEM ...........................................................................................................................30

9 Analysis by transmission electron microscope .......................................................................................31

9.1 General .................................................................................................................................................................31

9.2 Requirements .....................................................................................................................................................32

9.3 Calibration ...........................................................................................................................................................32

9.4 Sample preparation ...........................................................................................................................................33

9.5 Qualitative analysis by TEM ...........................................................................................................................33

10 Test report ...........................................................................................................................................................35

Annex A (normative) Types of commercial asbestos-containing material .......................................................36

Annex B (normative) Interference colour chart ........................................................................................................40

Annex C (normative) Dispersion staining charts .....................................................................................................41

Annex D (normative) Asbestos identification by PLM and dispersion staining in

commercial materials .......................................................................................................................................43

Annex E (normative) Asbestos identification by SEM in commercial materials .............................................52

Annex F (normative) Asbestos identification by TEM in commercial materials .............................................58

Annex G (informative) Example of sampling record ...............................................................................................67

Annex H (informative) Example of test report ...........................................................................................................68

© ISO 2012 – All rights reserved iii
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SIST ISO 22262-1:2013
ISO 22262-1:2012(E)

Bibliography .....................................................................................................................................................................69

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SIST ISO 22262-1:2013
ISO 22262-1:2012(E)
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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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

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

ISO 22262-1 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 3, Ambient

atmospheres.

ISO 22262 consists of the following parts, under the general title Air quality — Bulk materials:

— Part 1: Sampling and qualitative determination of asbestos in commercial bulk materials

The following part is under preparation:

— Part 2: Quantitative determination of asbestos by gravimetric and microscopical methods

© ISO 2012 – All rights reserved v
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Introduction

In the past, asbestos was used in a wide range of products. Three varieties of asbestos found extensive

commercial application. Chrysotile accounted for approximately 95 % of consumption, and this variety is

therefore likely to be encountered most frequently during the analysis of samples. Materials containing high

proportions of chrysotile asbestos were used in buildings and in industry for fireproofing, thermal insulation,

and acoustic insulation. Chrysotile was also used to reinforce materials to improve fracture and bending

characteristics. A large proportion of the chrysotile produced was used in asbestos–cement products. These

include flat sheets, tiles and corrugated sheets for roofing, pipes and open troughs for the collection of rainwater,

as well as pressure pipes for supply of potable water. Chrysotile was also incorporated into products such as

decorative coatings and plasters, glues, sealants and resins, floor tiles, gaskets, and road paving. In some

products, chrysotile was incorporated to modify rheological properties, e.g. in the manufacture of ceiling tile

panels and oil drilling muds. Long textile grade chrysotile fibre was also used to manufacture woven, spun,

felted and paper products.

Amosite and crocidolite accounted for almost all of the remaining asbestos use. Amosite was widely used as

fireproofing and in thermal insulation products, e.g. pipe coverings and insulating boards. Crocidolite was also

used as fireproofing and in thermal insulation products, but was particularly prized because it is highly resistant

to acids, flexible enough to be spun and has high tensile strength for reinforcement. Crocidolite found application

as a reinforcing fibre in acid containers such as those used for lead–acid batteries, in high-performance textiles

and gaskets, and was particularly important for the manufacture of high-pressure asbestos cement pipes for

delivery of potable water.

Three other types of asbestos are currently regulated. Materials containing commercial anthophyllite are

relatively rare, but they have also been used as a filler and reinforcing fibre in composite materials, and as

a filtration medium. Tremolite asbestos and actinolite asbestos were not extensively used commercially, but

some occurrences of tremolite asbestos in surfacing materials and fireproofing have been found in Japan.

Tremolite asbestos and actinolite asbestos sometimes occur as contaminants of other commercial minerals.

Other minerals can also occur as asbestos. For example, richterite asbestos and winchite asbestos occur

at mass fractions between 0,1 % and 6 % associated with vermiculite, formerly mined at Libby, Montana,

USA. Vermiculite from this source was widely distributed and is often found as loose fill insulation and as a

constituent in a range of construction materials and fireproofing.

While the asbestos mass fraction in some products can be very high and in some cases approach 100 %, in

other products the mass fractions of asbestos used were significantly lower and often between 1 % and 15 %.

In some ceiling tile panels, the mass fraction of asbestos used was close to 1 %. There are only a few known

materials in which the asbestos mass fraction used was less than 1 %. Some adhesives, sealing compounds

and fillers were manufactured in which asbestos mass fractions were lower than 1 %. There are no known

materials in which asbestos was intentionally added at mass fractions lower than 0,1 %.

In this part of ISO 22262, procedures for collection of samples and qualitative analysis of commercial bulk

materials for the presence of asbestos are specified. The primary method used to identify asbestos is polarized

light microscopy. Because of the wide range of matrix materials into which asbestos was incorporated, polarized

light microscopy cannot provide reliable analysis of all types of asbestos-containing materials in untreated

samples. The applicability of polarized light microscopy can be extended by the use of simple treatments such

as ashing and treatment with acid. Optionally, either scanning electron microscopy or transmission electron

microscopy may be used as an alternative or confirmatory method to identify asbestos.

Although this part of ISO 22262 specifies that, optionally, a visual estimate of the asbestos mass fraction within

very broad ranges may also be made, it is recognized that the accuracy and reproducibility of such estimates

is very limited. Quantitative determination of the asbestos content can be needed for a number of reasons,

e.g. assessment and management of the risk from asbestos materials in buildings or to comply with regulatory

definitions for asbestos-containing materials. The necessity to quantify asbestos in a material depends on the

maximum mass fraction that has been adopted by the jurisdiction to define an asbestos-containing material

for the purpose of regulation. Definitions range from “any asbestos” to 0,1 %, 0,5 % or 1 %. For jurisdictions in

which an asbestos-containing material is defined as one containing “any asbestos”, a particular problem is how

to determine whether a material does not contain asbestos, since all methods have limits of detection.

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For practical purposes, since no known commercial materials exist in which commercial asbestos was

intentionally added at mass fractions lower than 0,1 %, this part of ISO 22262 specifies that samples be

classified as asbestos-containing (i.e. containing more than 0,1 % asbestos) if either chrysotile, amosite,

crocidolite or anthophyllite, or any of these varieties in combination, is detected in the analysis. When the

definition of an asbestos-containing material is either 0,5 % or 1 %, depending on the nature of the product, it

is often necessary to proceed to other parts of this International Standard in order to quantify the asbestos for

the purpose of defining the regulatory status of the material.

The occurrence of tremolite, actinolite or richterite/winchite in a material is usually a consequence of natural

contamination of the constituents, and the detection of these minerals does not necessarily indicate that

the mass fraction is more than 0,1 % asbestos. Accordingly, determination of the regulatory status of these

materials by any of the criteria can often be achieved only by quantitative analysis. Since these minerals were

not specifically mined and utilized for their fibrous properties, they may also occur in materials as either non-

asbestiform or asbestiform analogues, or as mixtures of both. Evaluation of these types of material may require

a more detailed analysis.

Simple analytical procedures such as polarized light microscopy are not capable of detecting or reliably

identifying asbestos in some types of commercial products containing asbestos, either because the fibres are

below the resolution of optical microscopy or because the matrix material adheres too strongly to the fibres.

For these types of product, it may be necessary to utilize electron microscopy.
For a list of parts of this International Standard, see the Foreword.
[11] [13]

The method specified in this part of ISO 22262 is based on MDHS 77, VDI 3866 Part 1, VDI 3866 Part

[14] [15] [8] [10] [12]
4, , VDI 3866 Part 5, , AS 4964-2004, EPA/600/R-93/116, and NF X46-020:2008.
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SIST ISO 22262-1:2013
INTERNATIONAL STANDARD ISO 22262-1:2012(E)
Air quality — Bulk materials — Part 1: Sampling and qualitative
determination of asbestos in commercial bulk materials

IMPORTANT — The electronic file of this document contains colours which are considered to be

useful for the correct understanding of the document. Users should therefore consider printing this

document using a colour printer.
1 Scope

This part of ISO 22262 specifies methods for sampling bulk materials and identification of asbestos in commercial

bulk materials. This part of ISO 22262 specifies appropriate sample preparation procedures and describes in

detail the procedure for identification of asbestos by polarized light microscopy and dispersion staining.

This part of ISO 22262 also specifies simple procedures for separation of asbestos fibres from matrix materials

such as asphalt, cement, and plastics products. Optionally, identification of asbestos can be carried out using

scanning electron microscopy or transmission electron microscopy with energy dispersive X-ray analysis.

Information is also provided on common analytical problems, interferences and other types of fibre that may

be encountered in the analysis.

This part of ISO 22262 is applicable to qualitative identification of asbestos in specific types of manufactured

asbestos-containing products and commercial minerals. This part of ISO 22262 is applicable to the analysis

of fireproofing, thermal insulation, and other manufactured products or minerals in which asbestos fibres can

readily be separated from matrix materials for identification.

NOTE This part of ISO 22262 is intended for use by microscopists who are familiar with polarized light microscopy

methods and the other analytical procedures specified (References [16]–[19]). It is not the intention of this part of ISO 22262

to provide instruction in the fundamental analytical techniques.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
achromat

microscope objective in which chromatic aberration is corrected for two wavelengths and spherical aberration

and other aperture-dependent defects are minimized for one other wavelength (usually about 550 nm)

EXAMPLE One wavelength less than about 500 nm, the other greater than about 600 nm.

NOTE This term does not imply any degree of correction for curvature of image field; coma and astigmatism are

minimized for wavelengths within the achromatic range.
[3]
[ISO 10934-1:2002, 2.6]
2.2
acicular

shape shown by an extremely slender crystal with cross-sectional dimensions which are small relative to its

length, i.e. needle-like
[4]
[ISO 13794:1999, 2.1]
2.3
alpha refractive index
lowest refractive index exhibited by a fibre
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2.4
amphibole

group of rock-forming ferromagnesium silicate minerals, closely related in crystal form and composition, and

having the nominal formula:
A B C T O (OH,F,Cl)
0-1 2 5 8 22 2
where
A is K, Na
B is Fe , Mn, Mg, Ca, Na
3+ 2+
C is Al, Cr, Ti, Fe , Mg, Fe
T is Si, Al, Cr, Fe , Ti

NOTE In some varieties of amphibole, these elements can be partially substituted by Li, Pb, or Zn. Amphibole is

characterized by a cross-linked double chain of Si-O tetrahedra with a silicon:oxygen ratio of 4:11, by columnar or fibrous

prismatic crystals and by good prismatic cleavage in two directions parallel to the crystal faces and intersecting at angles

of about 56° and 124°.
[4]
[ISO 13794:1999, 2.2]
2.5
amphibole asbestos
amphibole in an asbestiform habit
[4]
[ISO 13794:1999, 2.3]
2.6
analyser

polar used after the object to determine optical effects produced by the object on the light, polarized or

otherwise, with which it is illuminated
NOTE It is usually positioned between the objective and the primary image plane.
[3]
[ISO 10934-1:2002, 2.117.1]
2.7
anisotropy
state or quality of having different properties along different axes

EXAMPLE An anisotropic transparent particle can show different refractive indices with the vibration direction of

incident light.
2.8
asbestiform

specific type of mineral fibrosity in which the fibres and fibrils possess high tensile strength and flexibility

[4]
[ISO 13794:1999, 2.6]
2.9
asbestos

term applied to a group of silicate minerals belonging to the serpentine and amphibole groups which have

crystallized in the asbestiform habit, causing them to be easily separated into long, thin, flexible, strong fibres

when crushed or processed

NOTE 1 The Chemical Abstracts Service Registry Numbers of the most common asbestos varieties are: chrysotile

(12001-29-5), crocidolite (12001-28-4), grunerite asbestos (amosite) (12172-73-5), anthophyllite asbestos (77536-67-5),

tremolite asbestos (77536-68-6) and actinolite asbestos (77536-66-4).
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[4]
[ISO 13794:1999, 2.7]

NOTE 2 Other varieties of asbestiform amphibole, such as richterite asbestos and winchite asbestos (Reference [20]),

are also found in some products such as vermiculite and talc.
2.10
aspect ratio
ratio of length to width of a particle
[4]
[ISO 13794:1999, 2.10]
2.11
Bertrand lens

intermediate lens which transfers an image of the back focal plane of the objective into the primary image plane

NOTE The Bertrand lens is used for conoscopic observation in polarized light microscopy and for adjustment of the

microscope illuminating system, especially in phase-contrast and modulation-contrast microscopy.

[3]
[ISO 10934-1:2002, 2.87.2]
2.12
birefringence

quantitative expression of the maximum difference in refractive index due to double refraction

[3]
[ISO 10934-1:2002, 2.16]
2.13
camera length

equivalent projection length between the specimen and its electron diffraction pattern, in the absence of lens action

[4]
[ISO 13794:1999, 2.12]
2.14
chrysotile
fibrous mineral of the serpentine group which has the nominal composition:
Mg Si O (OH)
3 2 5 4

NOTE Most natural chrysotile deviates little from this nominal composition. In some varieties of chrysotile, minor

3+ 3+ 2+ 3+ 2+ 2+ 2+

substitution of silicon by Al may occur. Minor substitution of magnesium by Al , Fe , Fe , Ni , Mn and Co may

also be present. Chrysotile is the most prevalent type of asbestos.
[4]
[ISO 13794:1999, 2.13]
2.15
cleavage
breaking of a mineral along one of its crystallographic directions
[4]
[ISO 13794:1999, 2.14]
2.16
cleavage fragment
fragment of a crystal that is bounded by cleavage faces

NOTE Crushing of non-asbestiform amphibole generally yields elongated fragments that conform to the definition of

a fibre, but rarely have aspect ratios exceeding 30:1.
2.17
crossed polars

state in which the polarization directions of the polars (polarizer and analyser) are mutually perpendicular

[3]
[ISO 10934-1:2002, 2.117.2]
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2.18
d-spacing
distance between identical adjacent and parallel planes of atoms in a crystal
[4]
[ISO 13794:1999, 2.18]
2.19
dispersion
variation of refractive index with wavelength of light
[1]
[ISO 7348:1992, 05.03.26]
2.20
dispersion staining

effect produced when a transparent object is immersed in a surrounding medium, the refractive index of which

is equal to that of the object at a wavelength in the visible range, but which has a significantly higher optical

dispersion than the object

NOTE Only the light refracted at the edges of the object is imaged, and this gives rise to colours at the interface

between the object and the surrounding medium. The particular colour is a measure of the wavelength at which the

refractive index of the object and that of the medium are equal.
2.21
electron diffraction

technique in electron microscopy by which the crystal structure of a specimen is examined

[4]
[ISO 13794:1999, 2.19]
2.22
electron scattering power

extent to which a thin layer of substance scatters impinging electrons from their original directions

[4]
[ISO 13794:1999, 2.20]
2.23
energy dispersive X-ray analysis
EDXA

measurement of the energies and intensities of X-rays by use of a solid-state detector and multichannel

analyser system
[4]
[ISO 13794:1999, 2.22]
2.24
eucentric

condition in which the area of interest of an object is placed on a tilting axis, at the intersection of the electron

beam with that axis, and is in the plane of focus
[4]
[ISO 13794:1999, 2.23]
2.25
extinction

condition in which an optically anisotropic object appears dark when observed between crossed polars

[3]
[ISO 10934-1:2002, 2.51]

NOTE Extinction occurs when the vibration directions of the crystal are parallel to the vibration directions in the

polarizer and analyser.
2.26
extinction angle

angle between the extinction position and the position at which the length of a fibre is parallel to the polarizer

or analyser vibration directions
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2.27
fibril

single fibre of asbestos which cannot be further separated longitudinally into smaller components without

losing its fibrous properties or appearances
[4]
[ISO 13794:1999, 2.25]
2.28
fibre
elongated particle which has parallel or stepped sides
[4]
[ISO 13794:1999, 2.26]

NOTE For the purposes of this part of ISO 22262, a fibre is defined to have an aspect ratio greater than or equal to 3:1.

2.29
fibre bundle

structure composed of parallel, smaller diameter fibres attached along their lengths

NOTE A fibre bundle may exhibit diverging fibres at one or both ends.
[4]
[ISO 13794:1999, 2.27]
2.30
gamma refractive index
highest refractive index exhibited by a fibre
2.31
habit

characteristic crystal growth form, or combination of these forms, of a mineral, including characteristic

irregularities
[4]
[ISO 13794:1999, 2.30]
2.32
high-efficiency particulate air filter
HEPA
filter that is at least 99,97 % efficient by volume on 0,3 µm particles
[6]
[ISO 14952-1:2003, 2.13]
2.33
isotropic
having the same properties in all directions
[5]
[ISO 14686:2003, 2.23]
2.34
Köhler illumination

method of illuminating specimens in which an image of the illumination source is projected by a collector into

the plane of the aperture diaphragm in the front focal plane of the condenser, which then projects an image of

an illuminated field diaphragm at the opening of the collector into the specimen plane

2.35
lamda zero
matc
...

NORME ISO
INTERNATIONALE 22262-1
Première édition
2012-07-01
Qualité de l’air — Matériaux solides —
Partie 1:
Échantillonnage et dosage qualitatif de
l’amiante dans les matériaux solides
d’origine commerciale
Air quality — Bulk materials —
Part 1: Sampling and qualitative determination of asbestos in
commercial bulk materials
Numéro de référence
ISO 22262-1:2012(F)
ISO 2012
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ISO 22262-1:2012(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2012

Droits de reproduction réservés. Sauf prescription différente, 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 et les microfilms, sans l’accord écrit

de l’ISO à l’adresse ci-après ou du comité membre de l’ISO dans le pays du demandeur.

ISO copyright office
Case postale 56 • CH-1211 Geneva 20
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E-mail copyright@iso.org
Web www.iso.org
Publié en Suisse
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ISO 22262-1:2012(F)
Sommaire Page

Avant-propos ...................................................................................................................................................................... v

Introduction .......................................................................................................................................................................vi

1 Domaine d’application ....................................................................................................................................... 1

2 Termes et définitions .......................................................................................................................................... 1

3 Symboles et termes abrégés ............................................................................................................................ 8

4 Principe .................................................................................................................................................................. 8

4.1 Généralités ............................................................................................................................................................ 8

4.2 Détection de la substance ................................................................................................................................. 9

4.3 Type d’échantillon ............................................................................................................................................... 9

4.4 Étendue de mesure ............................................................................................................................................. 9

4.5 Limite de détection ............................................................................................................................................. 9

4.6 Limitations du MOLP dans la détection de l’amiante ................................................................................ 9

5 Prélèvement de l’échantillon ..........................................................................................................................10

5.1 Exigences ............................................................................................................................................................10

5.2 Mode opératoire ................................................................................................................................................. 11

6 Préparation de l’échantillon ...........................................................................................................................15

6.1 Généralités ..........................................................................................................................................................15

6.2 Élimination des matériaux organiques par calcination ..........................................................................15

6.3 Élimination des constituants solubles par traitement à l’acide ...........................................................15

6.4 Sédimentation et flottation..............................................................................................................................15

6.5 Combinaison des procédures de réduction gravimétrique ...................................................................16

7 Analyse par MOLP .............................................................................................................................................16

7.1 Exigences ............................................................................................................................................................16

7.2 Analyse qualitative par MOLP ........................................................................................................................20

8 Analyse par MEB ...............................................................................................................................................31

8.1 Généralités ..........................................................................................................................................................31

8.2 Exigences ............................................................................................................................................................31

8.3 Étalonnage ..........................................................................................................................................................32

8.4 Préparation de l’échantillon ...........................................................................................................................32

8.5 Analyse qualitative par MEB ..........................................................................................................................32

9 Analyse par microscope électronique à transmission ...........................................................................34

9.1 Généralités ..........................................................................................................................................................34

9.2 Exigences ............................................................................................................................................................34

9.3 Étalonnage ..........................................................................................................................................................35

9.4 Préparation de l’échantillon ...........................................................................................................................35

9.5 Analyse qualitative par MET ...........................................................................................................................36

10 Rapport d’essai ..................................................................................................................................................37

Annexe A (normative) Types de matériaux contenant de l’amiante d’origine commerciale ........................39

Annexe B (normative) Échelle des teintes d’interférence .....................................................................................43

Annexe C (normative) Échelle des couleurs de dispersion ..................................................................................44

Annexe D (normative) Identification de l’amiante par MOLP et dispersion de coloration dans les

matériaux d’origine commerciale .................................................................................................................46

Annexe E (normative) Identification de l’amiante par MEB dans les matériaux d’origine commerciale ..55

Annexe F (normative) Identification de l’amiante par MET dans les matériaux d’origine commerciale ..61

Annexe G (informative) Exemple de rapport d’échantillonnage ..........................................................................70

Annexe H (informative) Exemple de rapport d’essai ...............................................................................................71

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Bibliographie ....................................................................................................................................................................72

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ISO 22262-1:2012(F)
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 (CEI) en ce qui concerne la normalisation électrotechnique.

Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI, Partie 2.

La tâche principale des comités techniques est d’élaborer les Normes internationales. Les projets de Normes

internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur publication

comme Normes internationales requiert l’approbation de 75 % au moins des comités membres votants.

L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de droits

de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable de ne pas avoir

identifié de tels droits de propriété et averti de leur existence.

L’ISO 22262-1 a été élaborée par le comité technique ISO/TC 146, Qualité de l’air, sous-comité SC 3,

Atmosphères ambiantes.

L’ISO 22262 comprend les parties suivantes, présentées sous le titre général Qualité de l’air — Matériaux solides:

— Partie 1: Échantillonnage et dosage qualitatif de l’amiante dans les matériaux solides d’origine commerciale

La partie suivante est en cours d’élaboration:

— Partie 2: Dosage quantitatif de l’amiante en utilisant les méthodes gravimétrique et microscopique

© ISO 2012 – Tous droits réservés v
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ISO 22262-1:2012(F)
Introduction

L’amiante était auparavant utilisé dans une vaste gamme de produits. Trois variétés d’amiante ont été très

utilisées dans le commerce. Le chrysotile représentait environ 95 % de la consommation. Il est donc la variété

la plus fréquemment rencontrée lors de l’analyse des échantillons. Des matériaux contenant de grandes

proportions de chrysotile étaient utilisés dans les secteurs de la construction et de l’industrie pour l’ignifugation,

l’isolation thermique et l’isolation phonique. Le chrysotile était également utilisé pour renforcer les matériaux

et pour améliorer les caractéristiques de rupture et de flexion. Une grande proportion du chrysotile produit

était utilisée dans les produits en amiante-ciment, notamment les plaques planes, les tuiles et les plaques

ondulées pour la couverture, les tuyaux et gouttières pour la récupération d’eau de pluie ainsi que les tuyaux

sous pression pour l’alimentation en eau potable. Le chrysotile était également incorporé dans des produits

tels que les revêtements et les enduits décoratifs, les colles, les mastics, les résines, les dalles, les joints

et les revêtements routiers. Dans certains produits, du chrysotile était ajouté pour modifier les propriétés

rhéologiques, par exemple dans la fabrication de panneaux de faux plafond et les boues de forage pétrolier. Le

chrysotile de qualité textile (longue fibre) était également utilisé pour fabriquer des produits tissés, filés, feutrés

et en papier.

L’amosite et la crocidolite représentaient la quasi-totalité du reste. L’amosite était généralement utilisée comme

matériau ignifuge ou dans les produits d’isolation thermique, tels que calorifugeage de tuyaux et panneaux

isolants. La crocidolite était également utilisée comme matériau ignifuge et dans les produits d’isolation

thermique; en outre, elle était particulièrement prisée pour sa grande résistance aux acides, était suffisamment

souple pour se prêter au filage et présentait une grande résistance à la traction. La crocidolite était également

employée comme fibre de renfort dans les récipients d’acide tels que ceux utilisés pour les accumulateurs au

plomb, dans des textiles de haute performance et dans des joints. Elle a également joué un rôle important dans

la fabrication de canalisations haute pression en amiante-ciment pour l’alimentation en eau potable.

Trois autres types d’amiante sont actuellement soumis à réglementation. Les matériaux contenant de

l’anthophyllite d’origine commerciale sont relativement rares, mais ils ont également été utilisés comme

colmatant et fibre de renfort dans les matériaux composites, et comme milieu filtrant. L’amiante trémolite et

l’amiante actinote ont été peu utilisés dans le commerce, mais la présence d’amiante trémolite a été parfois

détectée dans des matériaux de surfaçage et des matériaux ignifuges au Japon. L’amiante trémolite et l’amiante

actinote ont parfois été le résultat d’une contamination d’autres minéraux commercialisés. D’autres minéraux

peuvent également apparaître sous forme d’amiante. Par exemple, l’amiante richtérite et l’amiante winchite

apparaissent à des fractions massiques comprises entre 0,1 % et 6% dans la vermiculite anciennement

extraite de la mine de Libby, Montana, États-Unis. La vermiculite de cette origine a été largement distribuée

et sert souvent d’isolant en vrac et de constituant dans une vaste gamme de matériaux de construction et de

matériaux ignifuges.

Alors que la fraction massique d’amiante dans certains produits peut être très élevée et approcher parfois

les 100 %, les fractions massiques d’amiante dans d’autres produits étaient nettement inférieures et souvent

comprises entre 1 % et 15 %. Dans certains panneaux de faux plafond, la fraction massique d’amiante

utilisée était proche de 1 %. Il n’existe que quelques matériaux connus dans lesquels la fraction massique

d’amiante était inférieure à 1 %. Certains adhésifs, produits d’étanchéité et mastics ont été fabriqués avec des

fractions massiques d’amiante inférieures à 1 %. On ne connaît aucun matériau dans lequel de l’amiante a été

intentionnellement ajouté à des fractions massiques inférieures à 0,1 %.

Dans la présente partie de l’ISO 22262 sont décrites les procédures de prélèvement d’échantillons et d’analyse

qualitative des matériaux solides d’origine commerciale pour la détection d’amiante. La microscopie en

lumière polarisée constitue la principale méthode d’identification de l’amiante. En raison de la vaste gamme

de matériaux matriciels dans lesquels de l’amiante a été incorporé, la microscopie en lumière polarisée ne

permet pas d’effectuer des analyses fiables de tous les types de matériaux contenant de l’amiante dans les

échantillons non traités. L’applicabilité de la microscopie en lumière polarisée peut être élargie en utilisant des

traitements simples tels que la calcination et le traitement à l’acide. Pour identifier l’amiante, il est également

possible d’utiliser la microscopie électronique à balayage ou la microscopie électronique à transmission comme

méthode alternative ou de confirmation.

Bien que la présente partie de l’ISO 22262 spécifie qu’une estimation visuelle de la concentration en

amiante peut éventuellement être réalisée dans de très vastes gammes, il est reconnu que l’exactitude

et la reproductibilité de ces estimations sont très limitées. La procédure de quantification de la teneur en

vi © ISO 2012 – Tous droits réservés
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ISO 22262-1:2012(F)

amiante peut être nécessaire pour un certain nombre de raisons telles que, par exemple, l’évaluation et la

gestion du risque lié aux matériaux contenant de l’amiante dans les bâtiments pour répondre aux définitions

réglementaires relatives aux matériaux contenant de l’amiante. La nécessité de quantifier la teneur en amiante

dans un matériau dépend de la fraction massique maximale adoptée par la réglementation pour définir un

matériau contenant de l’amiante à des fins de réglementation. Les définitions vont de «tout amiante» jusqu’à

0,1 %, 0,5 % ou 1 %. Pour les réglementations dans lesquelles un matériau contenant de l’amiante est défini

comme contenant «tout amiante», il se pose un problème particulier concernant la manière de déterminer si un

matériau contient ou non de l’amiante, car toutes les méthodes ont des limites de détection.

Pour des raisons pratiques, étant donné qu’on ne connaît aucun matériau commercial dans lequel de l’amiante

d’origine commerciale a été intentionnellement ajouté à des fractions massiques inférieures à 0,1 %, la présente

partie de l’ISO 22262 spécifie que les échantillons doivent être classés comme contenant de l’amiante (c’est-

à-dire contenant plus de 0,1 % d’amiante) si du chrysotile, de l’amosite, de la crocidolite ou de l’anthophyllite,

ou des combinaisons de ces variétés, sont détectés au cours de l’analyse. Lorsque les matériaux contenant

de l’amiante sont définis comme étant des matériaux contenant 0,5 % ou 1 % d’amiante, selon la nature du

produit, il est souvent nécessaire de se référer aux autres parties de l’ISO 22262 pour quantifier l’amiante afin

de définir le statut réglementaire des matériaux.

La présence de trémolite, d’actinote ou de richtérite/winchite dans un matériau est en général le résultat de la

contamination naturelle des constituants, et la détection de ces minéraux ne signifie pas nécessairement que la

fraction massique d’amiante est supérieure à 0,1 %. En conséquence, il arrive souvent que la détermination du

statut réglementaire de ces matériaux par l’un quelconque des critères ne puisse se faire que par une analyse

quantitative. Ces minéraux n’ayant pas été spécifiquement extraits des mines et utilisés pour leurs propriétés

fibreuses, ils peuvent également apparaître dans les matériaux comme des analogues non asbestiformes ou

asbestiformes, ou comme un mélange des deux. L’évaluation de ces types de matériaux peut requérir une

analyse plus détaillée.

Les procédures d’analyse simples, telles que la microscopie en lumière polarisée, ne permettent pas de détecter

ou d’identifier de manière fiable l’amiante contenu dans certains types de produits commerciaux comprenant

des matériaux contenant de l’amiante; soit parce que la taille des fibres est inférieure à la résolution de la

microscopie optique, soit parce que le matériau matriciel adhère trop aux fibres. Pour ces types de produits, il

peut être nécessaire d’utiliser la microscopie électronique.

Voir l’Avant-propos pour la liste des autres parties de la présente Norme internationale.

[11]

La méthode spécifiée dans la présente partie de l’ISO 22262 s’appuie sur les documents MDHS 77 ,

[13] [14] [15] [8] [10]

VDI 3866 Partie 1 , VDI 3866 Partie 4 , VDI 3866 Partie 5 , AS 4964-2004 , EPA/600/R-93/116

[12]
et NF X46-020:2008 .
© ISO 2012 – Tous droits réservés vii
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NORME INTERNATIONALE ISO 22262-1:2012(F)
Qualité de l’air — Matériaux solides —
Partie 1:
Échantillonnage et dosage qualitatif de l’amiante dans les
matériaux solides d’origine commerciale

IMPORTANT — Le fichier électronique du présent document contient des couleurs qui sont jugées

utiles pour la bonne compréhension du document. Il convient donc aux utilisateurs de considérer

l’emploi d’une imprimante couleur pour l’impression du présent document.
1 Domaine d’application

La présente partie de l’ISO 22262 spécifie les méthodes d’échantillonnage de matériaux solides et d’identification

de l’amiante dans les matériaux solides d’origine commerciale. La présente partie de l’ISO 22262 spécifie

les procédures appropriées de préparation de l’échantillon et décrit en détail la procédure d’identification de

l’amiante par microscopie en lumière polarisée et dispersion de coloration.

La présente partie de l’ISO 22262 spécifie également des procédures simples de séparation des fibres

d’amiante des matériaux matriciels tels que les produits bitumineux, à base de ciment et de plastique.

L’identification de l’amiante peut également être effectuée en utilisant la microscopie électronique à balayage

ou la microscopie électronique à transmission avec analyse en dispersion d’énergie des rayons X. Des

informations sont également données sur les problèmes habituels d’analyse, les interférences et autres types

de fibres susceptibles d’être rencontrés au cours de l’analyse.

La présente partie de l’ISO 22262 est applicable à l’identification qualitative de l’amiante dans des types

spécifiques de produits manufacturés et de minéraux commercialisés contenant de l’amiante. La présente

partie de l’ISO 22262 est applicable à l’analyse des matériaux ignifuges, produits d’isolation thermique et

autres produits manufacturés ou minéraux dans lesquels les fibres d’amiante peuvent être facilement séparées

des matériaux matriciels pour être identifiées.

NOTE La présente partie de l’ISO 22262 est destinée à être utilisée par les microscopistes familiarisés avec les

méthodes de microscopie en lumière polarisée et par les personnes chargées de l’analyse, expérimentées et familiarisées

avec les procédures d’analyse spécifiées (Références [16] à [19]). L’objectif de la présente partie de l’ISO 22262 n’est pas

de fournir des informations sur les techniques d’analyse fondamentale.
2 Termes et définitions

Pour les besoins du présent document, les termes et définitions suivants s’appliquent.

2.1
achromat

objectif de microscope dans lequel l’aberration chromatique est corrigée pour deux longueurs d’onde et

l’aberration sphérique, ainsi que les autres défauts dépendant de l’ouverture, sont minimisés pour une autre

longueur d’onde (généralement environ 550 nm)

EXEMPLE Une longueur d’onde inférieure à 500 nm environ, l’autre supérieure à 600 nm environ.

NOTE Ce terme n’implique pas un degré quelconque de correction pour la courbure du champ d’image; la coma et

l’astigmatisme sont minimisés pour les longueurs d’ondes situées dans la gamme achromatique.

[3]
[ISO 10934-1:2002 , 2.6]
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ISO 22262-1:2012(F)
2.2
aciculaire

forme présentée par un cristal extrêmement fin dont les dimensions transversales sont petites par rapport à sa

longueur, c’est-à-dire en forme d’aiguille
[4]
[ISO 13794:1999 , 2.1]
2.3
indice de réfraction alpha
indice de réfraction minimal présenté par une fibre
2.4
amphibole

groupe de minéraux cardinaux de silicate de ferromagnésium, étroitement proches en termes de forme et de

composition cristallines, et de formule nominale:
A B C T O (OH,F,Cl)
0-1 2 5 8 22 2
A est K, Na;
B est Fe , Mn, Mg, Ca, Na;
3+ 2+
C est Al, Cr, Ti, Fe , Mg, Fe ;
T est Si, Al, Cr, Fe , Ti

NOTE Dans certaines variétés d’amphibole, ces éléments peuvent être partiellement substitués par Li, Pb ou Zn.

L’amphibole est caractérisée par une double chaîne de tétraèdres Si-O avec un rapport silicium:oxygène de 4:11, par des

cristaux prismatiques fibreux ou en colonnes et par un clivage prismatique bien marqué dans deux directions parallèles

aux faces du cristal et se coupant à des angles d’environ 56° et 124°.
[4]
[ISO 13794:1999 , 2.2]
2.5
amiante amphibole
amphibole de forme asbestiforme
[4]
[ISO 13794:1999 , 2.3]
2.6
analyseur

polaroïd placé après l’objet pour déterminer les effets optiques produits par l’objet sur la lumière, polarisée ou

autre, qui l’éclaire

NOTE L’analyseur est placé généralement entre l’objectif et le plan d’image primaire.

[3]
[ISO 10934-1:2002 , 2.117.1]
2.7
anisotropie

état ou qualité d’avoir des caractéristiques différentes selon des axes différents

EXEMPLE Une particule transparente anisotrope peut avoir différents indices de réfraction en fonction de la direction

de vibration de la lumière incidente.
2 © ISO 2012 – Tous droits réservés
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ISO 22262-1:2012(F)
2.8
asbestiforme

type de fibrosité minérale spécifique dans lequel les fibres et les fibrilles possèdent une résistance à la traction

et une flexibilité élevées
[4]
[ISO 13794:1999 , 2.6]
2.9
amiante

terme s’appliquant à un groupe de minéraux de silicates appartenant aux groupes des amphiboles et des

serpentines qui se sont cristallisés en faciès asbestiforme, ce qui permet, lorsqu’ils sont traités ou broyés, de

les séparer facilement en fibres longues, minces, flexibles et solides

NOTE 1 Les numéros de registre CAS des variétés d’amiante les plus courantes sont: chrysotile (12001-29-5),

crocidolite (12001-28-4), amiante grunérite (amosite) (12172-73-5), amiante anthophyllite (77536-67-5), amiante trémolite

(77536-68-6) et amiante actinote (77536-66-4).
[4]
[ISO 13794:1999 , 2.7]

NOTE 2 D’autres variétés d’amphibole asbestiforme, notamment l’amiante richtérite et l’amiante winchite

(Référence [20]), sont également présentes dans certains produits tels que la vermiculite et le talc.

2.10
rapport largeur/longueur
rapport de la longueur d’une particule à sa largeur
[4]
[ISO 13794:1999 , 2.10]
2.11
lentille de Bertrand

lentille intermédiaire qui transfère une image du foyer-image de l’objectif sur le plan d’image primaire

NOTE La lentille de Bertrand est utilisée pour observation conoscopique en microscopie de polarisation et pour réglage

du système d’éclairage d’un microscope, notamment en microscopie à contraste de phase et à contraste de modulation.

[3]
[ISO 10934-1:2002 , 2.87.2]
2.12
biréfringence

expression quantitative de la différence maximale dans l’indice de réfraction due à la double réfraction

[3]
[ISO 10934-1:2002 , 2.16]
2.13
longueur de caméra

longueur de projection équivalente entre l’échantillon et son diagramme de diffraction électronique, en l’absence

d’action de la lentille
[4]
[ISO 13794:1999 , 2.12]
2.14
chrysotile
minéral fibreux du groupe des serpentines, de composition nominale:
Mg Si O (OH)
3 2 5 4

NOTE La majeure partie du chrysotile naturel possède une composition nominale proche de celle-ci. Dans certaines

variétés de chrysotile, une substitution mineure du silicium par Al peut survenir. Une substitution mineure du magnésium

3+ 2+ 3+ 2+ 2+ 2+

par Al , Fe , Fe , Ni , Mn et Co peut également se produire. Le chrysotile est le principal type d’amiante.

[4]
[ISO 13794:1999 , 2.13]
© ISO 2012 – Tous droits réservés 3
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ISO 22262-1:2012(F)
2.15
clivage
fissuration d’un minéral dans une de ses directions cristallographiques
[4]
[ISO 13794:1999 , 2.14]
2.16
fragment de clivage
fragment d’un cristal lié par les faces de clivage

NOTE En général, le broyage de l’amphibole non asbestiforme produit des fragments allongés conformes à la

définition d’une fibre, mais dont les rapports largeur/longueur dépassent rarement 30:1.

2.17
polaroïds croisés

état dans lequel les directions de polarisation des polaires (polariseur et analyseur) sont perpendiculaires

l’une à l’autre
[3]
[ISO 10934-1:2002 , 2.117.2]
2.18
espacement d

distance entre des plans adjacents et parallèles identiques d’atomes dans un cristal

[4]
[ISO 13794:1999 , 2.18]
2.19
dispersion

variation de l’indice de réfraction en fonction de la longueur d’onde de la lumière

[1]
[ISO 7348:1992 , 05.03.26]
2.20
dispersion de coloration

effet produit lorsqu’un objet transparent est immergé dans un milieu environnant, dont l’indice de réfraction

est égal à celui de l’objet à une longueur d’onde dans la gamme visible, mais dont la dispersion optique est

nettement supérieure à l’objet

NOTE Seule la lumière réfractée aux bords de l’objet apparaît sur l’image, ce qui produit des couleurs au niveau de

l’interface entre l’objet et le milieu environnant. La couleur particulière est une mesure de la longueur d’onde à laquelle

l’indice de réfraction de l’objet et celui du milieu sont égaux.
2.21
diffraction électronique

technique de microscopie électronique consistant à examiner la structure cristalline d’un échantillon

[4]
[ISO 13794:1999 , 2.19]
2.22
puissance de diffusion des électrons

degré de diffusion des électrons d’une mince couche de substance depuis leurs directions d’origine

[4]
[ISO 13794:1999 , 2.20]
2.23
analyse en dispersion d’énergie des rayons X
EDXA

mesure des énergies et des intensités des rayons X à l’aide d’un détecteur à semi-conducteurs et d’un

analyseur multicanal
[4]
[ISO 13794:1999 , 2.22]
4 © ISO 2012 – Tous droits réservés
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ISO 22262-1:2012(F)
2.24
eucentrique

condition dans laquelle la région d’intérêt d’un objet est placée sur un axe de basculement, à l’intersection du

faisceau d’électrons et de cet axe, et se trouve dans le plan focal
[4]
[ISO 13794:1999 , 2.23]
2.25
extinction

condition dans laquelle un objet optiquement anisotrope apparaît foncé lorsqu’il est observé entre polaroïds croisés

[3]
[ISO 10934-1:2002 , 2.51]

NOTE L’extinction se produit lorsque les directions de vibration du cristal sont parallèles aux directions de vibration

du polariseur et de l’analyseur.
2.26
angle d’extinction

angle entre la position d’extinction et la position à laquelle la longueur d’une fibre est parallèle aux directions

de vibration du polariseur ou de l’analyseur
2.27
fibrille
fibre d’amiante unique, qui ne peut pas être d
...

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