ASTM D5755-2003 Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Surface Loading《用石棉结构值.pdf

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1、Designation: D 5755 03Standard Test Method forMicrovacuum Sampling and Indirect Analysis of Dust byTransmission Electron Microscopy for Asbestos StructureNumber Surface Loading1This standard is issued under the fixed designation D 5755; the number immediately following the designation indicates the

2、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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure to (a) identify

3、asbestos 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 D 5756.1.2 This test meth

4、od 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 membranecassette from the sampling of a surface area for dust which maycontain asbestos.1.2

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

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

7、stos 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

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

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

10、 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 Standards:2D 1193 Specification for Reagent WaterD 3195 Practice for Rotameter Cali

11、brationD 3670 Guide for Determination of Precision and Bias ofMethods of Committee D22D 5756 Test Method for Microvacuum Sampling and Indi-rect Analysis of Dust by Transmission Electron Micros-copy for Asbestos Mass Surface LoadingD 6620 Practice for Determining a Detection Limit forAsbestos Measure

12、ments Based on Counts3. Terminology3.1 Definitions:3.1.1 asbestiforma special type of fibrous 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

13、 onSampling and Analysis of Atmospheres and is the direct responsibility of Subcom-mittee D22.07 on Sampling and Analysis of Asbestos.Current edition approved April 10, 2003. Published June 2003. Originallyapproved in 1995. Last previous edition approved in 2002 as D 5755 - 02.2For referenced ASTM s

14、tandards, 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 Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke

15、n, 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 collective term that describes a group ofnaturally occurring, inorganic, highly fibrous, silicate domi-nated minerals, which

16、 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 (chrysotile); riebeckite (cro-cidolite); grunerite (grunerite asbestos); anthophyllite (antho-phyllite asbestos); tremolite (trem

17、olite asbestos); and actinolite(actinolite asbestos). The amphibole mineral compositions aredefined according to nomenclature of the International Miner-alogical Association (3).Asbestos Chemical Abstract Service No.4Chrysotile 12001-29-5Crocidolite 12001-28-4Grunerite Asbestos 12172-73-5Anthophylli

18、te 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 fibrous properties orappearance.3.2 Definitions of Terms Specific to This Standard:3.2.1 aspect ratiothe ratio of the length

19、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 intermixed and no single fibe

20、r 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 a sizerange of 1 mm.

21、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 crystalline aggregat

22、e 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 describe aggregates of grainsthat crystallize in a needle-like habit and appear to be com-posed of fibers. Fibrous has a much more

23、 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 in which a samplepasses through one or more intermediate steps prior to finalfiltration.3.2.9 matrixa structure in which on

24、e 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 must meet the fiberdefinition (see 3.2.6).3.2.10 structuresa term that is used to categorize all thetypes of asbestos partic

25、les which are recorded during theanalysis (such as fibers, bundles, clusters, and matrices). Finalresults of the test are always expressed in asbestos structuresper square centimetre.4. Summary of Test Method4.1 The sample is collected by vacuuming a known surfacearea with a standard 25 or 37 mm air

26、 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 filtered through a membrane. A section ofthe membrane is prepared and tra

27、nsferred 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 000X.5. Significance and Use5.1 This microvacuum sampling and indirect analysismethod is used for the general testing of

28、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 index of the surface loading ofasbestos structures in the dust pe

29、r 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 compliancewith federal, state, or local regulations or statutes. It is t

30、heusers 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. Accord-ingly, the users should consider other available information intheir i

31、nterpretation 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, largeasbestos containing particle(s) (from the large end of theparticle size distribution) dispersed during sample preparationmay

32、 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 beanalyzed by the entire procedure.6. Interferences6.1 The following mine

33、rals 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 be recorded during the test. Therefore, literaturereferences for these materials must be maintained in the3The boldface numb

34、ers 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 Abstract Service (CAS) numbers.D5755032laboratory for comparison to asbestos minerals so that they arenot misidentified as asbest

35、os 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 and other amphiboles other than thoselisted in 3.1.2.6.2 Collecting any dust particles greater than 1 mm in sizein this test me

36、thod 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 otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the Ame

37、rican Chemical Society, wheresuch specifications 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.57.2 Transmission Electron Microscope (TEM),an80to120kV TEM, c

38、apable of performing electron diffraction, with 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 spo

39、t 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 Particulate Air (HEPA), filtered nega-tive flow hood.7.6 Exhaust or Fume Hood.7.7 Particle-free Water (ASTM Type II, see Specificatio

40、nD 1193).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 be approximately 13 cm high by 6 cmwide).7.10 Waterproof Markers.7.11 Forceps (tweezers).7.12 Ultrasonic Bath, table top mode

41、l (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 disposableplastic, and using either a 25 mm or 47 mm diameter filter.7.15 Side Arm Filter Flask, 1000 mL.7.16 Mixed Cellulos

42、e 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 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

43、 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 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 per

44、sonal-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.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.

45、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 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 Gr

46、ids, 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.7.45 Reagent Alcohol, HPLC Grade (FisherA995 or equiva-lent).7.46 Opening Mesh Screen, plastic, 1.0 by 1.0 mm,(Spectra-Mesh #1

47、46410 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 or 37mm diameter mixed cellul

48、ose 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 circumstances of the study.8.2 Maintain a log of all pertinent sampling information andsampling locations.5Reagent Chemicals

49、, 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.D57550338.3 Sampling pumps and flow indicators shall be calibratedusing a certified standard apparatus or assembly (see PracticeD 3195 and 7.29).8.4 Reco