ASTM D5755-2009(2014)e1 8653 Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Surface L.pdf

1、Designation: D5755 09 (Reapproved 2014)1Standard Test Method forMicrovacuum Sampling and Indirect Analysis of Dust byTransmission Electron Microscopy for Asbestos StructureNumber Surface Loading1This standard is issued under the fixed designation D5755; the number immediately following the designati

2、on indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEWarning notes were editorially updated thr

3、oughout in April 2014.1. Scope1.1 This test method covers a procedure to (a) identifyasbestos in dust and (b) provide an estimate of the surfaceloading of asbestos in the sampled dust reported as the numberof asbestos structures per unit area of sampled surface.1.1.1 If an estimate of the asbestos m

4、ass is to be determined,the user is referred to Test Method D5756.1.2 This test method describes the equipment and proce-dures necessary for sampling, by a microvacuum technique,non-airborne dust for levels of asbestos structures. The non-airborne sample is collected inside a standard filter membran

5、ecassette from the sampling of a surface area for dust which maycontain asbestos.1.2.1 This procedure uses a microvacuuming sampling tech-nique. The collection efficiency of this technique is unknownand will vary among substrates. Properties influencing collec-tion efficiency include surface texture

6、, adhesiveness, electro-static properties and other factors.1.3 Asbestos identified by transmission electron microscopy(TEM) is based on morphology, selected area electron diffrac-tion (SAED), and energy dispersive X-ray analysis (EDXA).Some information about structure size is also determined.1.4 Th

7、is test method is generally applicable for an estimateof the surface loading of asbestos structures starting fromapproximately 1000 asbestos structures per square centimetre.1.4.1 The procedure outlined in this test method employs anindirect sample preparation technique. It is intended to disperseag

8、gregated asbestos into fundamental fibrils, fiber bundles,clusters, or matrices that can be more accurately quantified bytransmission electron microscopy. However, as with all indi-rect sample preparation techniques, the asbestos observed forquantification may not represent the physical form of thea

9、sbestos as sampled. More specifically, the procedure de-scribed neither creates nor destroys asbestos, but it may alterthe physical form of the mineral fibers.1.5 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.6 This standar

10、d does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM

11、 Standards:2D1193 Specification for Reagent WaterD3195 Practice for Rotameter CalibrationD3670 Guide for Determination of Precision and Bias ofMethods of Committee D22D5756 Test Method for Microvacuum Sampling and IndirectAnalysis of Dust by Transmission Electron Microscopyfor Asbestos Mass Surface

12、LoadingD6620 Practice for Asbestos Detection Limit Based onCountsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 asbestiforma special type of f

13、ibrous habit in whichthe fibers are separable into thinner fibers and ultimately intofibrils. This habit accounts for greater flexibility and higher1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.07 on Sampling andA

14、nalysis of Asbestos.Current edition approved April 1, 2014. Published May 2014. Originallyapproved in 1995. Last previous edition approved in 2009 as D5755 09. DOI:10.1520/D5755-09R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm

15、.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1tensile strength than other habits of the same mineral. For mor

16、einformation on asbestiform mineralogy, see Refs (1-3).33.1.2 asbestosa collective term that describes a group ofnaturally occurring, inorganic, highly fibrous, silicate domi-nated minerals, which are easily separated into long, thin,flexible fibers when crushed or processed.3.1.2.1 DiscussionInclud

17、ed in the definition are the as-bestiform varieties of: serpentine (chrysotile); riebeckite (cro-cidolite); grunerite (grunerite asbestos); anthophyllite (an-thophyllite asbestos); tremolite (tremolite asbestos); andactinolite (actinolite asbestos). The amphibole mineral compo-sitions are defined ac

18、cording to nomenclature of the Interna-tional Mineralogical Association (3).Asbestos Chemical Abstract Service No.AChrysotile 12001-29-5Crocidolite 12001-28-4Grunerite Asbestos 12172-73-5Anthophyllite Asbestos 77536-67-5Tremolite Asbestos 77536-68-6Actinolite Asbestos 77536-66-4AThe non-asbestiform

19、variations of the minerals indicated in 3.1.2.1 have differentChemical Abstract Service (CAS) numbers.3.1.3 fibrila single fiber that cannot be separated intosmaller components without losing its fibrous properties orappearance.3.2 Definitions of Terms Specific to This Standard:3.2.1 aspect ratiothe

20、 ratio of the length of a fibrousparticle to its average width.3.2.2 bundlea structure composed of three or more fibersin a parallel arrangement with the fibers closer than one fiberdiameter to each other.3.2.3 clustera structure with fibers in a random arrange-ment such that all fibers are intermix

21、ed and no single fiber isisolated from the group; groupings of fibers must have morethan two points touching.3.2.4 debrismaterials that are of an amount and size(particles greater than 1 mm in diameter) that can be visuallyidentified as to their source.3.2.5 dustany material composed of particles in

22、 a sizerange of 1 mm.3.2.6 fibera structure having a minimum length of 0.5 m,an aspect ratio of 5:1 or greater, and substantially parallel sides(4).3.2.7 fibrousof a mineral composed of parallel, radiating,or interlaced aggregates of fibers, from which the fibers aresometimes separable: that is, the

23、 crystalline aggregate may bereferred to as fibrous even if it is not composed of separablefibers, but has that distinct appearance.3.2.7.1 DiscussionThe term fibrous is used in a generalmineralogical way to describe aggregates of grains that crys-tallize in a needle-like habit and appear to be comp

24、osed offibers. Fibrous has a much more general meaning than asbes-tos. While it is correct that all asbestos minerals are fibrous, notall minerals having fibrous habits are asbestos.3.2.8 indirect preparationa method in which a samplepasses through one or more intermediate steps prior to finalfiltra

25、tion.3.2.9 matrixa structure in which one or more fibers, orfiber bundles that are touching, are attached to, or partiallyconcealed by a single particle or connected group of non-fibrous particles in which the exposed fiber must meet the fiberdefinition (see 3.2.6).3.2.10 structuresa term that is us

26、ed to categorize all thetypes of asbestos particles which are recorded during theanalysis (such as fibers, bundles, clusters, and matrices).3.2.10.1 DiscussionFinal results of the test are alwaysexpressed in asbestos structures per square centimetre.4. Summary of Test Method4.1 The sample is collect

27、ed by vacuuming a known surfacearea with a standard 25 or 37-mm air sampling cassette usinga plastic tube that is attached to the inlet orifice which acts asa nozzle. The sample is transferred from inside the cassette toan aqueous suspension of known volume. Aliquots of thesuspension are then filter

28、ed through a membrane. A section ofthe membrane is prepared and transferred to a TEM grid usingthe direct transfer method. The asbestiform structures areidentified, sized, and counted by TEM, using SAED andEDXA at a magnification of 15 000 to 20 000.5. Significance and Use5.1 This microvacuum sampli

29、ng and indirect analysismethod is used for the general testing of non-airborne dustsamples for asbestos. It is used to assist in the evaluation ofdust that may be found on surfaces in buildings such as ceilingtiles, shelving, electrical components, duct work, carpet, etc.This test method provides an

30、 index of the surface loading ofasbestos structures in the dust per unit area analyzed as derivedfrom a quantitative TEM analysis.5.1.1 This test method does not describe procedures ortechniques required to evaluate the safety or habitability ofbuildings with asbestos-containing materials, or compli

31、ancewith federal, state, or local regulations or statutes. It is theusers responsibility to make these determinations.5.1.2 At present, no relationship has been established be-tween asbestos-containing dust as measured by this test methodand potential human exposure to airborne asbestos.Accordingly,

32、 the users should consider other available infor-mation in their interpretation of the data obtained from this testmethod.5.2 This definition of dust accepts all particles small enoughto pass through a 1-mm (No. 18) screen. Thus, a single, largeasbestos containing particle(s) (from the large end of

33、theparticle size distribution) dispersed during sample preparationmay result in anomalously large asbestos surface loadingresults in the TEM analyses of that sample. It is, therefore,recommended that multiple independent samples are securedfrom the same area, and that a minimum of three samples bean

34、alyzed by the entire procedure.3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.D5755 09 (2014)126. Interferences6.1 The following minerals have properties (that is, chemi-cal or crystalline structure) which are very similar to asbestosminerals and may in

35、terfere with the analysis by causing a falsepositive to be recorded during the test. Therefore, literaturereferences for these materials must be maintained in thelaboratory for comparison to asbestos minerals so that they arenot misidentified as asbestos minerals.6.1.1 Antigorite.6.1.2 Palygorskite

36、(Attapulgite).6.1.3 Halloysite.6.1.4 Pyroxenes.6.1.5 Sepiolite.6.1.6 Vermiculite scrolls.6.1.7 Fibrous talc.6.1.8 Hornblende and other amphiboles other than thoselisted in 3.1.2.6.2 Collecting any dust particles greater than 1 mm in sizein this test method may cause an interference and, therefore,mu

37、st be avoided.7. Materials and Equipment7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications

38、 are available. Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.47.2 Transmission Electron Microscope (TEM), an 80 to 120kV TEM, capable of performing electron diffraction, w

39、ith afluorescent screen inscribed with calibrated gradations, isrequired. The TEM must be equipped with energy dispersiveX-ray spectroscopy (EDXA) and it must have a scanningtransmission electron microscopy (STEM) attachment or becapable of producing a spot size of less than 250 nm indiameter in cro

40、ssover.7.3 Energy Dispersive X-ray System (EDXA).7.4 High Vacuum Carbon Evaporator, with rotating stage.7.5 High Effciency Particulate Air (HEPA), filtered nega-tive flow hood.7.6 Exhaust or Fume Hood.7.7 Particle-free Water (ASTM Type II, see SpecificationD1193).7.8 Glass Beakers (50 mL).7.9 Glass

41、Sample Containers, with wide mouth screw cap(200 mL) or equivalent sealable container (height of the glasssample container should be approximately 13 cm high by 6 cmwide).7.10 Waterproof Markers.7.11 Forceps (tweezers).7.12 Ultrasonic Bath, table top model (100 W).7.13 Graduated Pipettes (1, 5, 10-m

42、L sizes), glass orplastic.7.14 Filter Funnel, either 25 mm or 47 mm, glass ordisposable. Filter funnel assemblies, either glass or disposableplastic, and using either a 25-mm or 47-mm diameter filter.7.15 Side Arm Filter Flask, 1000 mL.7.16 Mixed Cellulose Ester (MCE) Membrane Filters, 25 or47-mm di

43、ameter, 0.22-m and 5-m pore size.7.17 Polycarbonate (PC) Filters, 25 or 47-mm diameter,0.2-m pore size.7.18 Storage Containers, for the 25 or 47-mm filters (forarchiving).7.19 Glass Slides, approximately 76 by 25 mm in size.7.20 Scalpel Blades, No. 10, or equivalent.7.21 Cabinet-type Desiccator, or

44、low temperature dryingoven.7.22 Chloroform, reagent grade.7.23 Acetone, reagent grade.7.24 Dimethylformamide (DMF).7.25 Glacial Acetic Acid.7.26 1-methyl-2-pyrrolidone.7.27 Plasma Asher, low temperature.7.28 pH Paper.7.29 Air Sampling Pump, low volume personal-type, ca-pable of achieving a flow rate

45、 of 1 to 5 L/min.7.30 Rotameter.7.31 Air Sampling Cassettes, 25 mm or 37 mm, containing0.8 m or smaller pore size MCE or PC filters.7.32 Cork Borer, 7 mm.7.33 Non-Asbestos Mineral, references as outlined in 6.1.7.34 Asbestos Standards, as outlined in 3.1.2.7.35 Tygon5Tubing, or equivalent.7.36 Small

46、 Vacuum Pump, that can maintain a pressure of 92kPa.7.37 Petri Dishes, large glass, approximately 90 mm indiameter.7.38 Jaffe Washer, stainless steel or aluminum mesh screen,30 to 40 mesh, and approximately 75 mm by 50 mm in size.7.39 Copper TEM Finder Grids, 200 mesh.4Reagent Chemicals, American Ch

47、emical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S.

48、Pharmaceutical Convention, Inc. (USPC), Rockville,MD.5Tygon is a registered trademark of the DuPont Co.D5755 09 (2014)137.40 Carbon Evaporator Rods.7.41 Lens Tissue.7.42 Ashless Filter Paper Filters, 90-mm diameter.7.43 Gummed Paper Reinforcement Rings.7.44 Wash Bottles, plastic.7.45 Reagent Alcohol

49、, HPLC Grade (FisherA995 or equiva-lent).7.46 Opening Mesh Screen, plastic, 1.0 by 1.0 mm,(Spectra-Mesh #146410 or equivalent).7.47 Diffraction Grating Replica.8. Sampling Procedure for Microvacuum Technique8.1 For sampling asbestos-containing dust in either indooror outdoor environments, commercially available cassettesmust be used. Air monitoring cassettes containing 25-mm or37-mm diameter mixed cellulose ester (MCE) or polycarbonate(PC) filter membranes with a pore size less than or equal to 0.8m are required (7.31). The number of samples collec