Ambient air — Determination of numerical concentration of inorganic fibrous particles — Scanning electron microscopy method

This document specifies a method using scanning electron microscopy for determination of the concentration of inorganic fibrous particles in the air. The method specifies the use of gold-coated, capillary-pore, track-etched membrane filters, through which a known volume of air has been drawn. Using energy-dispersive X-ray analysis, the method can discriminate between fibres with compositions consistent with those of the asbestos varieties (e.g. serpentine and amphibole), gypsum, and other inorganic fibres. Annex C provides a summary of fibre types which can be measured. This document is applicable to the measurement of the concentrations of inorganic fibrous particles in ambient air. The method is also applicable for determining the numerical concentrations of inorganic fibrous particles in the interior atmospheres of buildings, for example to determine the concentration of airborne inorganic fibrous particles remaining after the removal of asbestos-containing products. The range of concentrations for fibres with lengths greater than 5 µm, in the range of widths which can be detected under standard measurement conditions (see 7.2), is approximately 3 fibres to 200 fibres per square millimetre of filter area. The air concentrations, in fibres per cubic metre, represented by these values are a function of the volume of air sampled. The ability of the method to detect and classify fibres with widths lower than 0,2 µm is limited. If airborne fibres in the atmosphere being sampled are predominantly [8] can be used to determine the smaller fibres.

Air ambiant — Détermination de la concentration en nombre des particules inorganiques fibreuses — Méthode par microscopie électronique à balayage

Zunanji zrak - Določevanje numerične koncentracije anorganskih vlaknastih delcev - Metoda štetja z elektronskim mikroskopom

General Information

Status
Published
Publication Date
12-Dec-2019
Current Stage
9020 - International Standard under periodical review
Start Date
15-Oct-2024
Completion Date
15-Oct-2024

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SLOVENSKI STANDARD
01-april-2020
Nadomešča:
SIST ISO 14966:2004
SIST ISO 14966:2004/Cor 1:2011
Zunanji zrak - Določevanje numerične koncentracije anorganskih vlaknastih
delcev - Metoda štetja z elektronskim mikroskopom
Ambient air - Determination of numerical concentration of inorganic fibrous particles -
Scanning electron microscopy method
Air ambiant - Détermination de la concentration en nombre des particules inorganiques
fibreuses - Méthode par microscopie électronique à balayage
Ta slovenski standard je istoveten z: ISO 14966:2019
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 14966
Second edition
2019-12
Ambient air — Determination of
numerical concentration of inorganic
fibrous particles — Scanning electron
microscopy method
Air ambiant — Détermination de la concentration en nombre des
particules inorganiques fibreuses — Méthode par microscopie
électronique à balayage
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 4
5 Principle . 4
6 Apparatus and materials. 4
6.1 Air sampling . 4
6.1.1 Sampling head . 4
6.1.2 Sampling train . 5
6.1.3 Sampling pump . 5
6.1.4 Needle valve . 6
6.1.5 Volumetric flowmeter (rotameter) . 6
6.1.6 Timer . 6
6.1.7 Dry type gas meter (optional) . 6
6.1.8 Meteorological instruments (optional) . 6
6.1.9 Instruments for unattended sampling (optional) . 7
6.2 Preparation of filters . 7
6.2.1 Vacuum evaporator . . 7
6.2.2 Plasma asher . 8
6.3 Sample analysis . 8
6.3.1 Scanning electron microscope (SEM) . 8
6.3.2 Energy-dispersive X-ray system . 8
6.3.3 Stereo-microscope . . 9
6.3.4 Gold-coated capillary-pore polycarbonate filters. 9
6.3.5 Backing filters . 9
6.3.6 Disposable plastic field monitors (optional) . 9
6.3.7 Technically pure oxygen . 9
6.3.8 Rubber connecting hoses . 9
6.3.9 Filter containers . 9
6.3.10 Routine electron microscopy tools and supplies . 9
6.3.11 Sample for resolution adjustment . 9
6.3.12 Sample for magnification calibration .10
7 Air sample collection and analysis .10
7.1 Measurement planning .10
7.2 Collection of air samples .10
7.3 SEM specimen preparation .13
7.4 Analysis in the scanning electron microscope .13
7.4.1 General instructions.13
7.4.2 Fibre-counting criteria .14
7.4.3 Fibre classification .19
7.4.4 Analysis using reference spectra and peak height ratios .26
7.4.5 Measurement of fibre dimensions .28
7.4.6 Recording of data on the fibre counting form .28
8 Calculation of results .28
8.1 Calculation of the mean fibre concentration .28
8.2 Calculation of the 95 % confidence interval .30
9 Performance characteristics .30
9.1 General .30
9.2 Measurement uncertainty .30
9.2.1 Systematic errors . . .30
9.2.2 Random errors .30
9.2.3 Errors due to sampling .31
9.2.4 Errors associated with the SEM examination .31
9.2.5 Total error of the measurement.31
9.2.6 Random errors due to fibre counting .32
9.3 Limit of detection .34
10 Test report .35
Annex A (normative) Preparation of filters for air sampling .37
Annex B (normative) Procedures for calibration and adjustment of the SEM .38
Annex C (informative) Characteristics and chemical composition of inorganic fibres .40
Annex D (informative) Poisson variability as a function of fibre density on sampling filter
and area of filter analysed .45
Annex E (informative) Combination of the results from multiple samples .47
Bibliography .48
iv © ISO 2019 – All rights reserved

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Direc
...


INTERNATIONAL ISO
STANDARD 14966
Second edition
2019-12
Ambient air — Determination of
numerical concentration of inorganic
fibrous particles — Scanning electron
microscopy method
Air ambiant — Détermination de la concentration en nombre des
particules inorganiques fibreuses — Méthode par microscopie
électronique à balayage
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 4
5 Principle . 4
6 Apparatus and materials. 4
6.1 Air sampling . 4
6.1.1 Sampling head . 4
6.1.2 Sampling train . 5
6.1.3 Sampling pump . 5
6.1.4 Needle valve . 6
6.1.5 Volumetric flowmeter (rotameter) . 6
6.1.6 Timer . 6
6.1.7 Dry type gas meter (optional) . 6
6.1.8 Meteorological instruments (optional) . 6
6.1.9 Instruments for unattended sampling (optional) . 7
6.2 Preparation of filters . 7
6.2.1 Vacuum evaporator . . 7
6.2.2 Plasma asher . 8
6.3 Sample analysis . 8
6.3.1 Scanning electron microscope (SEM) . 8
6.3.2 Energy-dispersive X-ray system . 8
6.3.3 Stereo-microscope . . 9
6.3.4 Gold-coated capillary-pore polycarbonate filters. 9
6.3.5 Backing filters . 9
6.3.6 Disposable plastic field monitors (optional) . 9
6.3.7 Technically pure oxygen . 9
6.3.8 Rubber connecting hoses . 9
6.3.9 Filter containers . 9
6.3.10 Routine electron microscopy tools and supplies . 9
6.3.11 Sample for resolution adjustment . 9
6.3.12 Sample for magnification calibration .10
7 Air sample collection and analysis .10
7.1 Measurement planning .10
7.2 Collection of air samples .10
7.3 SEM specimen preparation .13
7.4 Analysis in the scanning electron microscope .13
7.4.1 General instructions.13
7.4.2 Fibre-counting criteria .14
7.4.3 Fibre classification .19
7.4.4 Analysis using reference spectra and peak height ratios .26
7.4.5 Measurement of fibre dimensions .28
7.4.6 Recording of data on the fibre counting form .28
8 Calculation of results .28
8.1 Calculation of the mean fibre concentration .28
8.2 Calculation of the 95 % confidence interval .30
9 Performance characteristics .30
9.1 General .30
9.2 Measurement uncertainty .30
9.2.1 Systematic errors . . .30
9.2.2 Random errors .30
9.2.3 Errors due to sampling .31
9.2.4 Errors associated with the SEM examination .31
9.2.5 Total error of the measurement.31
9.2.6 Random errors due to fibre counting .32
9.3 Limit of detection .34
10 Test report .35
Annex A (normative) Preparation of filters for air sampling .37
Annex B (normative) Procedures for calibration and adjustment of the SEM .38
Annex C (informative) Characteristics and chemical composition of inorganic fibres .40
Annex D (informative) Poisson variability as a function of fibre density on sampling filter
and area of filter analysed .45
Annex E (informative) Combination of the results from multiple samples .47
Bibliography .48
iv © ISO 2019 – All rights reserved

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organizat
...


INTERNATIONAL ISO
STANDARD 14966
Second edition
2019-12
Ambient air — Determination of
numerical concentration of inorganic
fibrous particles — Scanning electron
microscopy method
Air ambiant — Détermination de la concentration en nombre des
particules inorganiques fibreuses — Méthode par microscopie
électronique à balayage
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 4
5 Principle . 4
6 Apparatus and materials. 4
6.1 Air sampling . 4
6.1.1 Sampling head . 4
6.1.2 Sampling train . 5
6.1.3 Sampling pump . 5
6.1.4 Needle valve . 6
6.1.5 Volumetric flowmeter (rotameter) . 6
6.1.6 Timer . 6
6.1.7 Dry type gas meter (optional) . 6
6.1.8 Meteorological instruments (optional) . 6
6.1.9 Instruments for unattended sampling (optional) . 7
6.2 Preparation of filters . 7
6.2.1 Vacuum evaporator . . 7
6.2.2 Plasma asher . 8
6.3 Sample analysis . 8
6.3.1 Scanning electron microscope (SEM) . 8
6.3.2 Energy-dispersive X-ray system . 8
6.3.3 Stereo-microscope . . 9
6.3.4 Gold-coated capillary-pore polycarbonate filters. 9
6.3.5 Backing filters . 9
6.3.6 Disposable plastic field monitors (optional) . 9
6.3.7 Technically pure oxygen . 9
6.3.8 Rubber connecting hoses . 9
6.3.9 Filter containers . 9
6.3.10 Routine electron microscopy tools and supplies . 9
6.3.11 Sample for resolution adjustment . 9
6.3.12 Sample for magnification calibration .10
7 Air sample collection and analysis .10
7.1 Measurement planning .10
7.2 Collection of air samples .10
7.3 SEM specimen preparation .13
7.4 Analysis in the scanning electron microscope .13
7.4.1 General instructions.13
7.4.2 Fibre-counting criteria .14
7.4.3 Fibre classification .19
7.4.4 Analysis using reference spectra and peak height ratios .26
7.4.5 Measurement of fibre dimensions .28
7.4.6 Recording of data on the fibre counting form .28
8 Calculation of results .28
8.1 Calculation of the mean fibre concentration .28
8.2 Calculation of the 95 % confidence interval .30
9 Performance characteristics .30
9.1 General .30
9.2 Measurement uncertainty .30
9.2.1 Systematic errors . . .30
9.2.2 Random errors .30
9.2.3 Errors due to sampling .31
9.2.4 Errors associated with the SEM examination .31
9.2.5 Total error of the measurement.31
9.2.6 Random errors due to fibre counting .32
9.3 Limit of detection .34
10 Test report .35
Annex A (normative) Preparation of filters for air sampling .37
Annex B (normative) Procedures for calibration and adjustment of the SEM .38
Annex C (informative) Characteristics and chemical composition of inorganic fibres .40
Annex D (informative) Poisson variability as a function of fibre density on sampling filter
and area of filter analysed .45
Annex E (informative) Combination of the results from multiple samples .47
Bibliography .48
iv © ISO 2019 – All rights reserved

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organizat
...

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