© ISO 2016 Air quality — Bulk materials — Part 3 Quantitative determination of asbestos by X ray diffraction method Qualité de l’air — Matériaux solides — Partie 3 Dosage quantitatif de l’amiante par[.]
INTERNATIONAL STANDARD ISO 22262-3 First edition 2016-10-01 Air quality — Bulk materials — Part 3: Quantitative determination of asbestos by X-ray diffraction method Qualité de l’air — Matériaux solides — Partie 3: Dosage quantitatif de l’amiante par la méthode de diffraction des rayons X Reference number ISO 22262-3:2016(E) © ISO 2016 ISO 2 62 -3 : 01 6(E) COPYRIGHT PROTECTED DOCUMENT © ISO 2016, Published in Switzerland All rights reserved Unless otherwise specified, no part o f 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 o f the requester ISO copyright o ffice Ch de Blandonnet • CP 401 CH-1214 Vernier, Geneva, Switzerland Tel +41 22 749 01 11 Fax +41 22 749 09 47 copyright@iso.org www.iso.org ii © ISO 2016 – All rights reserved ISO 22262-3:2016(E) Contents Page Foreword v Introduction vi Scope Normative references Terms and definitions Range Limit o f quantification Symbols and abbreviated terms Requirements for quantification Apparatus and reagents 8.1 Apparatus 8.2 Reagents Quantitative XRD method and principle 9.1 Quantitative XRD methods using an external standard f 9.3 Preparation of working curve and measurement 9.4 Interference minerals 10 Preparation of comminuted sample 10.1 Preparation of comminuted sample from original sample 10.2 Heat treatment of comminuted samples that contain organic constituents 10.3 Pretreatment for preparation of residual samples 10 10.4 Preparation of sub-residual samples 11 11 Diffraction peaks for analysis of asbestos and of interference materials 11 ff f f 11 11.2 Interference minerals 15 11.2.1 Possible interference minerals 15 11.2.2 Mass reduction treatments for dissolving interference minerals 16 12 Quantitative analysis by XRD employing substrate standard mass absorption correction 16 12.1 General 16 12.2 Preparation of working curve 17 12.2.1 Preparation of working curve I 17 12.2.2 Preparation of working curve II 17 f 18 12.4 Calculation of asbestos mass fraction 18 12.4.1 Calculation of asbestos mass fraction from a residual sample 18 12.4.2 Calculation of the asbestos mass fraction from a sub-residual sample 19 12.5 Lower limits of detection and quantitative determination for the working curve 19 f f 20 13 Test report 20 Annex A (normative) X-ray diffractometer parameters for quantitative analysis of asbestos 22 Annex B (normative) Substrate standard mass absorption correction for asbestos quantification 26 Annex C (informative) Types of commercial asbestos-containing materials and optimum analytical procedures 27 Annex D (informative) Effects of matrix reduction methods 38 9.2 S ummary o the quantitative metho d 1 Di Pro cedure Evaluatio n o ractio n p eaks o r quantitative analys is o as b es to s o r quantitative analys is © ISO 2016 – All rights reserved uncertainty o XRD meas urement iii ISO 22262-3:2016(E) Annex E (informative) Range of typical detection limits and evaluation of uncertainty of quantitative XRD measurements by XRD method 41 Bibliography 45 iv © ISO 2016 – All rights reserved ISO 22262-3:2016(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies) The work o f 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 o f electrotechnical standardization The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part In particular the different approval criteria needed for the di fferent types o f ISO documents should be noted This document was dra fted in accordance with the editorial rules of the ISO/IEC Directives, Part (see www.iso.org/directives) Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f patent rights ISO shall not be held responsible for identi fying any or all such patent rights Details o f any patent rights identified during the development o f 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 in formation given for the convenience o f users and does not constitute an endorsement For an explanation on the meaning o f ISO specific terms and expressions related to formity assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary in formation The committee responsible for this document is 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 — Part 2: Quantitative determination of asbestos by gravimetric and microscopical methods — Part 3: Quantitative determination of asbestos by X-ray diffraction method © ISO 2016 – All rights reserved v ISO 2 62 -3 : 01 6(E) Introduction In the past, asbestos was used in a wide range of products Materials containing high proportions o f asbestos were used in buildings and in industry for fireproofing, thermal insulation and acoustic insulation Asbestos was also used to reinforce materials and to improve fracture and bending characteristics A large proportion of the asbestos produced was used in asbestos-cement products These include flat sheets, tiles and corrugated sheets for roofing, pipes and open troughs for collection o f rainwater and pressure pipes for supply o f potable water Asbestos was also incorporated into products such as decorative coatings and plasters, glues, sealants and resins, floor tiles, gaskets and road paving In some products, asbestos was incorporated to modi fy rheological properties, for example in the manufacture of ceiling tile panels and oil drilling muds While the asbestos concentration in some products can be very high and in some cases approaches 100 %, in other products the concentrations o f asbestos used were significantly lower and o ften between % and 15 % In some ceiling tile panels, the concentration of asbestos used was close to % There are only a few known materials in which the asbestos concentration used was less than % Some adhesives, sealing compounds and fillers were manu factured in which asbestos concentrations were lower than % There are no known commercially manu factured materials in which any one o f the common asbestos varieties (chrysotile, amosite, crocidolite or anthophyllite) was intentionally added at concentrations lower than 0,1 % ISO 22262-1 specifies the procedures for collection o f samples and qualitative analysis o f asbestos in commercial bulk materials using microscopical methods such as polarized light microscopy (PLM) ISO 22262-2 specifies the procedures for the determination o f asbestos mass fractions in bulk materials by microscopical methods This part o f ISO 22262 specifies the analytical procedures for the quantitative determination o f asbestos by X-ray powder di ffraction (XRD) The procedure employs a substrate standard mass absorption correction method to quanti fy asbestos that was previously identified by the microscopical method in ISO 22262-1 While the XRD method is use ful for qualitative analysis o f crystalline substances in powder samples by measurement o f di ffraction patterns that can be related to crystal structure, XRD analysis cannot distinguish between di fferent morphological habits o f the same mineral Thus, XRD cannot discriminate between the asbestiform and non-asbestiform analogues of serpentine and the amphiboles Furthermore, the primary di ffraction peaks for di fferent amphiboles lie within a very narrow range and it is not possible to quanti fy individual amphiboles when a mixture o f amphiboles is present Diffraction peaks appearing in XRD patterns of the asbestos-forming minerals are considered to be “possible peaks o f asbestos”, assumed to represent the asbestos detected during analysis in ISO 22262-1 However, if non-asbestiform serpentine or non-asbestiform amphibole minerals are present in the sample matrix, the “possible peaks o f asbestos” will represent them Accordingly, this method is not intended for application to samples in which non-asbestiform serpentine or nonasbestiform amphibole minerals are present A conventional XRD method, which employs a powder sample mounted in a powder specimen holder and a scintillation counter, can quanti fy a crystalline material at a concentration o f approximately % The XRD method using a substrate standard mass absorption correction method employed in this part o f ISO 22262 can detect the di ffraction peaks o f chrysotile asbestos from quantities as low as 0,01 mg on a membrane filter o f cm area [0,01 mg/filter (2 cm )] as shown in References [13] and [14] The amount o f sample on the filter is limited to 15 mg due to the limit o f the X-ray absorption correction In this method, gravimetric matrix reduction procedures are used to reduce the matrix constituents and interference minerals in a 100 mg comminuted sample When the matrix reduction achieves a residual ratio of 10 % or lower, the XRD method can provide a limit of detection of 0,01 wt% and the limit of quantification can be as low as 0,03 wt% When the matrix reduction is less e ffective and the residual ratio is over 10 % of the initial 100 mg sample, a sub-divided 10 mg to 15 mg sample is taken from the residual sample In the case where none or very little o f the matrix is reduced, the limit o f detection can increase up to approximately 0,1 % and the limit o f quantification can increase up to approximately 0,3 % When matrix reduction achieves a residual ratio o f approximately 30 % o f the original weight, the limit o f quantification is approximately 0,1 % These limits o f detection and quantification are further vi © ISO 2016 – All rights reserved ISO 2 62 -3 : 01 6(E) de grade d i f i nter ference X-ray p e a ks or h igh b ackgrou nd X-ray i nten s itie s present T he XRD me tho d s p e c i fie d in th i s part of ISO 2 62 7500-1/10 [17] , EPA/600/R-93/116[18] and JIS A 1481-3 [19] © ISO 2016 – All rights reserved is b as e d on from NIOSH matri x materi a l s are 0 -1 /7 [16] , NIOSH vii INTERNATIONAL STANDARD ISO 22262-3:2016(E) Air quality — Bulk materials — Part 3: Quantitative determination of asbestos by X-ray diffraction method Scope T h i s p ar t o f I S O 2 62 i s pri ma ri ly i ntende d b e en identi fie d at e s ti mate d mas s frac tion s for qua ntitative ana lys i s o f s ample s i n wh ich asb e s to s s lower than approxi mately % b y weight T h i s p a r t o f I S O 2 62 e xtend s the appl ic abi l ity a nd l i m it o f de te c tion o f quantitative ana lys i s b y the u s e o f s i mple pro ce du re s o f as h i ng and/or acid tre atment prior to XRD quanti fic ation T h i s p ar t o f I S O 2 62 i s appl ic ab le to the asb e s to s - conta i n i ng materia l s identi fie d i n I S O 2 62 -1 T he following are examples of sample matrices: a) a ny bui ld i ng materi a l s i n wh ich asb e s to s wa s de te c te d b y the ana lys i s i n I S O 2 62 -1 ; b) re s i l ient flo or ti le s , a s ph a ltic materi a l s , ro o fi ng felts a nd any o ther materi a l s i n wh ich asb e s to s i s emb e dde d i n an organ ic matri x and i n wh ich a sb e s to s wa s de te c te d when u s i ng I S O 2 62 -1 ; c) wall and ceiling plasters, with or without aggregate, in which asbestos was detected when using ISO 22262-1 If non-asbestiform serpentine or non-asbestiform amphibole minerals are included in the matrix, the XRD peaks that are assumed to be “possible peaks of asbestos” will represent these minerals This me tho d i s no t for appl ic ation to natu l m i nera l s that may contai n asb e s to s or a ny pro duc ts i ncorp orate s uch natu l m i nera l s T h i s me tho d i s i ntende d on ly for that appl ic ation to bu i ld i ng materi a l s ample s th at conta i n del ib erately adde d com merc ia l grade a sb e s to s i nclud i ng tremol ite asb e s to s T h i s p ar t o f I S O 2 62 i s i ntende d for u s e b y a na lys ts who are fa m i l i ar and the o ther ana lytic a l pro ce du re s s p e c i fie d i n the Re ference s [ p a r t o f I S O 2 62 to provide b as ic i n s tr uc tion i n the with X-ray d i ffrac tion me tho d s 5] and [6] It is not the intention of this fu nda menta l ana lytic a l pro ce du re s Normative references T he fol lowi ng i nd i s p en s able c u ments , i n whole or i n p ar t, are normatively re ference d i n th i s c u ment a nd are for its appl ic ation For date d re ference s , on ly the e d ition cite d appl ie s For u ndate d re ference s , the late s t e d ition o f the re ference d c u ment (i nclud i ng any amend ments) appl ie s ISO 22262-1:2012, Air quality — Bulk materials — Part 1: Sampling and qualitative determination of asbestos in commercial bulk materials ISO 22262-2:2014, Air quality — Bulk materials — Part 2: Quantitative determination of asbestos by gravimetric and microscopical methods Terms and definitions For the pu r p o s e o f th i s c u ment, the © ISO 2016 – All rights reserved fol lowi ng term s and defi n ition s apply ISO 2 62 -3 : 01 6(E) asbes tiform specific type o f mineral fibrosity in which the fibres and fibrils possess high tensile strength and flexibility [SOURCE: ISO 13794:1999, 2.6] 3.2 asbes tos term applied to a group of silicate minerals belonging to the serpentine and amphibole groups which have crystallized in the asbesti form habit, causing them to be easily separated into long, thin, flexible, strong fibres when crushed or processed Note to entry: The Chemical Abstracts Service Registry Numbers o f 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) Other varieties of asbestiform amphibole, such as richterite asbestos and winchite asbestos[20] , are also found in some products such as vermiculite and talc [SOURCE: ISO 13794:1999, 2.7, modified] 3.3 comminuted sample analytical sample prepared by comminution and sieving o f the original sample gravimetric matri x reduction procedure in which constituents o f a material are selectively dissolved or otherwise separated, leaving a residue in which any asbestos present in the original material is concentrated [SOURCE: ISO 22262-2:2014, 3.22] 3.5 integral intensity peak area count (integral count) of a designated XRD peak after subtracting the background area limit of detection weight o f asbestos on a filtered sample which produces a detectable XRD peak under the measurement conditions shown in Annex A Note to entry: Expressed as a percentage mass fraction o f the original sample f weight o f asbestos on a filtered sample for which the integral intensity o f the XRD peak can be measured l i m i t o q u a n t i f i c a t i o n Note to entry: Expressed as a percentage mass fraction o f the original sample Limit o f quantification is conventionally expressed as three times the limit o f detection 3.8 matri x materials in a bulk sample within which fibres are dispersed [SOURCE: ISO 22262-1:2012, 2.36, modified] original sample sample taken from a building material product which was analysed using ISO 22262-1 © ISO 2016 – All rights reserved ISO 22262-3:2016(E) Table C.1 (continued) Product Asbestoscontaining troweled-on compositions and putty Examples of application Typical asbestos Analysis in type and mass fraction if asbestos accordance with is present — Grouting of Up to 20 % prefabricated concrete chrysotile components — Sealing of movement joints — Pipe feed-throughs through walls and ceilings — Door casings of floorings Asphalt or vinyl asbestos floor tiles Rubberized asbestos seals — Anti-drumming coatings (car preservation) — Coating of underwater structures — Baseboard coating on house walls — Reinforcement in Chrysotile 10 % to — Rot-resistant chrysotile 80 % to flexible sheets support layer as underlay o f cushion vinyl flooring materials — Reinforcement — Gaskets for pipe flanges An estimate of asbestos mass fraction 20 % rom analysis according to ISO 22262-1 is usually su fficient, since in these types o f material, asbestos f 100 % Asphalt tiles up to 35 % chrysotile, vinyl tiles up to 20 % chrysotile ISO 22262-1 is either present at mass fractions significantly exceeding legislated control limits or asbestos is not present in the formulation In some floor tiles, ISO 22262-2 ISO 22262-3 Chrysotile 50 % to 90 % ISO 22262-1 32 Ashing and treatment with mol/l hydrochloric acid are the optimum procedures PLM examination of the residue is usually su fficient In some cases, PLM point counting may be necessary Absence of asbestos is most demonstrated ISO 22262-2 ebyffectively TEM examination o f ISO 22262-3 the residue using the drop mounting technique fire-resistant doors Asbestoscontaining Optimum analytical procedure substantial asbestos can be observed at a fracture sur face and identified according to ISO 22262-1 Most floor tiles are best analysed by ashing and treatment with concentrated (11,3 mol/l) hydrochlo ric acid, followed by SEM or TEM examination using the drop mount technique An estimate of asbestos mass fraction from analysis according to ISO 22262-1 is usually su fficient, since in these types o f material asbestos is either present at mass fractions significantly exceeding legislated control limits or asbestos is not present in the formulation © ISO 2016 – All rights reserved ISO 22262-3:2016(E) Table C.1 (continued) Product Asbestoscontaining friction products Examples of application — Brake linings — Brake bands — Clutch linings Acid-resistant containers — Lead-acid battery Filter media — Air filters — Liquid filters boxes — Drums for acid — Sterile and aseptic filters — Clari fying sheets — Diaphragms for chloralkali electrolysis process © ISO 2016 – All rights reserved Typical asbestos Analysis in type and mass fraction if asbestos accordance with is present Chrysotile 10 % to 70 % Optimum analytical procedure An estimate of asbestos mass fraction rom analysis according to ISO 22262-1 is usually su fficient, since in these types o f material, asbestos f ISO 22262-1 is either present at mass fractions significantly exceeding legislated control limits or asbestos is not present in the formulation Crocidolite 10 % to Substantial asbestos can 50 % often be observed at a fracture surface and identified according to ISO 22262-1 ISO 22262-1 Otherwise, ashing of a sub-sample is the optimum procedure, followed by examination according to ISO 22262-1 95 % chrysotile, An estimate of rarely asbestos mass fraction from analysis according amosite to ISO 22262-1 is usually su fficient, since in these types o f material, asbestos ISO 22262-1 is either present at mass fractions significantly exceeding legislated control limits or asbestos is not present in the formulation 33 ISO 22262-3:2016(E) Table C.1 (continued) Product Talc (asbestos content dependent on deposit) Examples of application Typical asbestos Analysis in type and mass fraction if asbestos accordance with is present Chrysotile and/or — Release agents for electric cables, rubber actinolite/tremolite products — Release agents in the fectionery industry — Tailor’s chalk — Paper manufacture — Medicine, cosmetics Optimum analytical procedure Talc is not amenable to gravimetric matrix reduction methods For chrysotile, preparation of TEM specimens from the untreated material is the optimum procedure, ollowed by examination by the mass counting f procedure amphibole, either ISO 22262-2 For centri fugation in heavy liquid, followed by evaluation of the centri fugate by microscopy, or Vermiculite (exfoliated) — Loose-fill attic and wall cavity insulation — Supply to horticultural applications 34 Depends on the source of the vermiculite Vermiculite that originated from a former mine in Montana, USA may contain up to % of a mixture of asbestiform preparation of TEM specimens from the untreated material is the optimum procedure, followed by examination using the mass counting procedure Remove the vermiculite by flotation on water Manually pick out any asbestiform amphibole from the sediment, identi fy it according to ISO 22262-1, and weigh to obtain the weight percentage If manual removal of asbestiform amphibole amphibole types is not feasible because the particle sizes are too Current sources of small, use the heavy liquid vermiculite may centrifugation technique to contain no ISO 22262-2 separate the amphibole detectable amphibole or low Alternatively, sequential concentrations of refluxing in mol/l amphibole hydrochloric acid and mol/l sodium hydroxide Depending on may be used to dissolve the source of the most of the vermiculite vermiculite, some Examine the residue by o f any amphibole PLM, SEM or TEM that is present may according to ISO 22262-1 have asbestiform Further morphology quantification may be carried out using the SEM or TEM mass counting procedure © ISO 2016 – All rights reserved ISO 22262-3:2016(E) Table C.1 (continued) Product Examples of application Typical asbestos Analysis in type and mass fraction if asbestos accordance with is present Vermiculite concentrate — Supply to ex folia - Vermiculitecontaining gypsum wallboard — Fire-resistant Amphibole