ISO 10312:2019
Ambient air — Determination of asbestos fibres — Direct transfer transmission electron microscopy method
This document specifies a reference method using transmission electron microscopy for the determination of airborne asbestos fibres and structures in in a wide range of ambient air situations, including the interior atmospheres of buildings, and for a detailed evaluation for asbestos structures in any atmosphere. The method allows determination of the type(s) of asbestos fibres present and also includes measurement of the lengths, widths and aspect ratios of the asbestos structures. The method cannot discriminate between individual fibres of asbestos and elongate fragments (cleavage fragments and acicular particles) from non-asbestos analogues of the same amphibole mineral[13].
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Symbols and abbreviated terms
5 Type of sample
6 Range
7 Limit of detection
8 Principle
9 Reagents
10 Apparatus
10.1 Air sampling — Equipment and consumable supplies
10.1.1 Filter cassette
10.1.2 Sampling pump
10.1.3 Stand
10.1.4 Personal sampling
10.1.5 Flowmeter
10.2 Specimen preparation laboratory
10.3 Equipment for analysis
10.3.1 Transmission electron microscope
10.3.2 Energy dispersive X-ray analyser
10.3.3 Plasma asher
10.3.4 Vacuum coating unit
10.3.5 Sputter coater
10.3.6 Solvent washer (Jaffe washer)
10.3.7 Condensation washer
10.3.8 Slide warmer or oven
10.3.9 Ultrasonic bath
10.3.10 Carbon grating replica
10.3.11 Calibration specimen grids for EDXA
10.3.12 Carbon rod sharpener
10.3.13 Disposable tip micropipettes
10.4 Consumable supplies
10.4.1 Copper or nickel electron microscope grids
10.4.2 Gold or nickel electron microscope grids
10.4.3 Carbon rod electrodes
10.4.4 Routine electron microscopy tools and supplies
10.4.5 Reference asbestos samples
10.4.6 Reference samples of mineral fibres other than asbestos
11 Air sample collection
12 Procedure for analysis
12.1 General
12.2 Cleaning of sample cassettes
12.3 Direct preparation of TEM specimens from polycarbonate filters
12.3.1 Selection of filter area for carbon coating
12.3.2 Carbon coating of filter portions
12.3.3 Preparation of the Jaffe washer
12.3.4 Placing of specimens in the Jaffe washer
12.4 Direct preparation of TEM specimens from cellulose ester filters
12.4.1 Selection of area of filter for preparation
12.4.2 Preparation of solution for collapsing cellulose ester filters
12.4.3 Filter collapsing procedure
12.4.4 Plasma etching of the filter surfaces
12.4.5 Carbon coating
12.4.6 Preparation of the Jaffe washer
12.4.7 Placing of specimens in the Jaffe washer
12.5 Criteria for acceptable TEM specimen grids
12.6 Procedure for structure counting by TEM
12.6.1 General
12.6.2 Measurement of mean opening area
12.6.3 TEM alignment and calibration procedures
12.6.4 Determination of criterion for termination of TEM examination
12.6.5 General procedure for structure counting and size analysis
12.6.6 Magnification requirements
12.7 Blank and quality control determinations
12.8 Calculation of results
13 Performance characteristics
13.1 General
13.2 Interferences and limitations of fibre identification
13.3 Precision and accuracy
13.3.1 Precision
13.3.2 Accuracy
13.3.3 Inter-laboratory and intra-laboratory analyses
13.4 Limit of detection
14 Test report
Annex A (normative) Determination of operating conditions for plasma asher
Annex B (normative) Calibration procedures
Annex C (normative) Structure counting criteria
Annex D (normative) Fibre identification procedure
Annex E (normative) Determination of the concentration of asbestos fibres and bundles longer than 5 µm, and PCM equivalent asbestos fibres
Annex F (normative) Calculation of results
Annex G (informative) Strategies for collection of air samples
Annex H (informative) Methods for removal of gypsum fibres
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Symbols and abbreviated terms
5 Type of sample
6 Range
7 Limit of detection
8 Principle
9 Reagents
10 Apparatus
10.1 Air sampling — Equipment and consumable supplies
10.1.1 Filter cassette
10.1.2 Sampling pump
10.1.3 Stand
10.1.4 Personal sampling
10.1.5 Flowmeter
10.2 Specimen preparation laboratory
10.3 Equipment for analysis
10.3.1 Transmission electron microscope
10.3.2 Energy dispersive X-ray analyser
10.3.3 Plasma asher
10.3.4 Vacuum coating unit
10.3.5 Sputter coater
10.3.6 Solvent washer (Jaffe washer)
10.3.7 Condensation washer
10.3.8 Slide warmer or oven
10.3.9 Ultrasonic bath
10.3.10 Carbon grating replica
10.3.11 Calibration specimen grids for EDXA
10.3.12 Carbon rod sharpener
10.3.13 Disposable tip micropipettes
10.4 Consumable supplies
10.4.1 Copper or nickel electron microscope grids
10.4.2 Gold or nickel electron microscope grids
10.4.3 Carbon rod electrodes
10.4.4 Routine electron microscopy tools and supplies
10.4.5 Reference asbestos samples
10.4.6 Reference samples of mineral fibres other than asbestos
11 Air sample collection
12 Procedure for analysis
12.1 General
12.2 Cleaning of sample cassettes
12.3 Direct preparation of TEM specimens from polycarbonate filters
12.3.1 Selection of filter area for carbon coating
12.3.2 Carbon coating of filter portions
12.3.3 Preparation of the Jaffe washer
12.3.4 Placing of specimens in the Jaffe washer
12.4 Direct preparation of TEM specimens from cellulose ester filters
12.4.1 Selection of area of filter for preparation
12.4.2 Preparation of solution for collapsing cellulose ester filters
12.4.3 Filter collapsing procedure
12.4.4 Plasma etching of the filter surfaces
12.4.5 Carbon coating
12.4.6 Preparation of the Jaffe washer
12.4.7 Placing of specimens in the Jaffe washer
12.5 Criteria for acceptable TEM specimen grids
12.6 Procedure for structure counting by TEM
12.6.1 General
12.6.2 Measurement of mean opening area
12.6.3 TEM alignment and calibration procedures
12.6.4 Determination of criterion for termination of TEM examination
12.6.5 General procedure for structure counting and size analysis
12.6.6 Magnification requirements
12.7 Blank and quality control determinations
12.8 Calculation of results
13 Performance characteristics
13.1 General
13.2 Interferences and limitations of fibre identification
13.3 Precision and accuracy
13.3.1 Precision
13.3.2 Accuracy
13.3.3 Inter-laboratory and intra-laboratory analyses
13.4 Limit of detection
14 Test report
Annex A (normative) Determination of operating conditions for plasma asher
Annex B (normative) Calibration procedures
Annex C (normative) Structure counting criteria
Annex D (normative) Fibre identification procedure
Annex E (normative) Determination of the concentration of asbestos fibres and bundles longer than 5 µm, and PCM equivalent asbestos fibres
Annex F (normative) Calculation of results
Annex G (informative) Strategies for collection of air samples
Annex H (informative) Methods for removal of gypsum fibres
Bibliography