ASTM D5755-2009 1875 Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Surface Loading《用.pdf

1、Designation: D5755 09Standard 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 designation indicates the ye

2、ar 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.1. Scope1.1 This test method covers a procedure to (a) identifyasb

3、estos 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 mass is to be determined,the user is referred to Test Method D5756.1.2 This test method d

4、escribes 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 membranecassette from the sampling of a surface area for dust which maycontain asbestos.1.2.1 T

5、his 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, adhesiveness, electro-static properties and other factors.1.3 Asbestos identified by t

6、ransmission 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 This test method is generally applicable for an estimateof the surface loading of asbestos

7、 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 disperseaggregated asbestos into fundamental fibrils, fiber bundles,clusters, or matrices that can

8、 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 theasbestos as sampled. More specifically, the procedure de-scribed neither creates nor dest

9、roys 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 standard does not purport to address all of thesafety concerns, if any, associated with its use

10、. 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 Standards:2D1193 Specification for Reagent WaterD3195 Practice for Rotameter Calibratio

11、nD3670 Guide for Determination of Precision and Bias ofMethods of Committee D22D5756 Test Method for Microvacuum Sampling and Indi-rect Analysis of Dust by Transmission Electron Micros-copy for Asbestos Mass Surface LoadingD6620 Practice for Asbestos Detection Limit Based onCountsE177 Practice for U

12、se 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 fibrous habit in whichthe fibers are separable into thinner fibers and ultimately int

13、ofibrils. 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 andAnalysis of Asbestos.Current edition approved Dec. 1, 2009. Published December 2009.

14、Originallyapproved in 1995. Last previous edition approved in 2003 as D5755 - 03. DOI:10.1520/D5755-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards

15、 Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.tensile strength than other habits of the same mineral. For moreinformation on asbestiform mineralogy, see Refs (1),3(2) and(3).3.1.2 asbestosa

16、 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 DiscussionIncluded in the definition are the as-bestiform varieties of: serpentine (chr

17、ysotile); riebeckite (cro-cidolite); grunerite (grunerite asbestos); anthophyllite (antho-phyllite asbestos); tremolite (tremolite asbestos); and actinolite(actinolite asbestos). The amphibole mineral compositions aredefined according to nomenclature of the International Miner-alogical Association (

18、3).Asbestos Chemical Abstract Service No.4Chrysotile 12001-29-5Crocidolite 12001-28-4Grunerite Asbestos 12172-73-5Anthophyllite Asbestos 77536-67-5Tremolite Asbestos 77536-68-6Actinolite Asbestos 77536-66-43.1.3 fibrila single fiber that cannot be separated intosmaller components without losing its

19、fibrous properties orappearance.3.2 Definitions of Terms Specific to This Standard:3.2.1 aspect ratiothe 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 ea

20、ch other.3.2.3 clustera structure with fibers in a random arrange-ment such that all fibers are intermixed 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 dia

21、meter) that can be visuallyidentified as to their source.3.2.5 dustany material composed of particles in 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,

22、radiating,or interlaced aggregates of fibers, from which the fibers aresometimes separable. That is, the crystalline aggregate may bereferred to as fibrous even if it is not composed of separablefibers, but has that distinct appearance.The term fibrous is usedin a general mineralogical way to descri

23、be aggregates of grainsthat crystallize in a needle-like habit and appear to be com-posed of fibers. Fibrous has a much more general meaning thanasbestos. While it is correct that all asbestos minerals arefibrous, not all minerals having fibrous habits are asbestos.3.2.8 indirect preparationa method

24、 in which a samplepasses through one or more intermediate steps prior to finalfiltration.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. The exposed fiber

25、must meet the fiberdefinition (see 3.2.6).3.2.10 structuresa term that is used to categorize all thetypes of asbestos particles which are recorded during theanalysis (such as fibers, bundles, clusters, and matrices). Finalresults of the test are always expressed in asbestos structuresper square cent

26、imetre.4. Summary of Test Method4.1 The sample is collected 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 o

27、f known volume. Aliquots of thesuspension are then filtered 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

28、20 000X.5. Significance and Use5.1 This microvacuum sampling 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 compo

29、nents, duct work, carpet, etc.This test method provides an 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

30、 ofbuildings with asbestos-containing materials, or compliancewith 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

31、potential human exposure to airborne asbestos. Accord-ingly, the users should consider other available information intheir interpretation of the data obtained from this test method.5.2 This definition of dust accepts all particles small enoughto pass througha1mm(No. 18) screen. Thus, a single, large

32、asbestos containing particle(s) (from the large end of 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

33、the same area, and that a minimum of three samples beanalyzed by the entire procedure.6. Interferences6.1 The following minerals have properties (that is, chemi-cal or crystalline structure) which are very similar to asbestosminerals and may interfere with the analysis by causing a falsepositive to

34、be recorded during the test. Therefore, literaturereferences for these materials must be maintained in the3The boldface numbers in parentheses refer to the list of references at the end ofthis test method.4The non-asbestiform variations of the minerals indicated in 5.1.3 have differentChemical Abstr

35、act Service (CAS) numbers.D5755 092laboratory for comparison to asbestos minerals so that they arenot misidentified as asbestos minerals.6.1.1 Antigorite.6.1.2 Palygorskite (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 an

36、d 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,must be avoided.7. Materials and Equipment7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwi

37、se indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available. Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to per

38、mit its use without lessening the accuracy ofthe determination.57.2 Transmission Electron Microscope (TEM),an80to120kV TEM, capable of performing electron diffraction, with afluorescent screen inscribed with calibrated gradations, isrequired. The TEM must be equipped with energy dispersiveX-ray spec

39、troscopy (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 crossover.7.3 Energy Dispersive X-ray System (EDXA).7.4 High Vacuum Carbon Evaporator, with rotating stage.7.5 High Effciency Particul

40、ate 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 Sample Containers, with wide mouth screw cap(200 mL) or equivalent sealable container (height of the glasssample container should b

41、e 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 mL sizes), glass orplastic.7.14 Filter Funnel, either 25 mm or 47 mm, glass ordisposable. Filter funnel assemblies, either glass or

42、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,25or47 mm diameter, #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

43、 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 low temperature dryingoven.7.22 Chloroform, reagent grade.7.23 Acetone, reagent grade.7.24 Dimethylformamide (DMF).7.25 Glacial Ace

44、tic 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 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

45、.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 Tygon6Tubing, or equivalent.7.36 Small Vacuum Pump, that can maintain a pressure of 92kPa.7.37 Petri Dishes, large glass, approximately 90 mm indiameter.7.38 Jaffe Washe

46、r, 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.7.40 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.

47、45 Reagent Alcohol, 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 enviro

48、nments, commercially available cassettesmust be used.Air monitoring cassettes containing 25 mm or 37mm 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 collecteddepends upon the specific

49、circumstances of the study.8.2 Maintain a log of all pertinent sampling information andsampling locations.5Reagent Chemicals, American Chemical 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. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.6Tygon is a registered trademark of the DuPont Co.D5755 0938.3 Sampling pum