1、Designation: D6602 13 (Reapproved 2018)Standard Practice forSampling and Testing of Possible Carbon Black FugitiveEmissions or Other Environmental Particulate, or Both1This standard is issued under the fixed designation D6602; the number immediately following the designation indicates the year ofori
2、ginal 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 practice covers sampling and testing for distin-guishingA
3、STM type carbon black, in the N100 to N900 series,from other environmental particulates.1.2 This practice requires some degree of expertise on thepart of the microscopist. For this reason, the microscopist musthave adequate training and on-the-job experience in identifyingthe morphological parameter
4、s of carbon black and generalknowledge of other particles that may be found in the envi-ronment. In support of this analysis, Donnets book2is highlyrecommended to be used as a technical reference for recogniz-ing and understanding the microstructure of carbon black.1.3 The values stated in SI units
5、are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard may involve hazardous materials,operations, and equipment. This standard does not purport toaddress all of the safety concerns, if any, associated with itsuse. It is the responsibility of the
6、user of this standard toestablish appropriate safety, health, and environmental prac-tices and determine the applicability of regulatory limitationsprior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in
7、the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D1619 Test Methods for Carbon BlackSulfur ContentD3053 Terminology Relati
8、ng to Carbon BlackD3849 Test Method for Carbon BlackMorphologicalCharacterization of Carbon Black Using Electron Micros-copy3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aciniformshaped like a cluster of grapes.3.1.1.1 DiscussionThe spheroidal primary particles ofcarbon blac
9、k are fused into aggregates of colloidal dimensionforming an acinoform morphology.3.1.2 aciniform carboncolloidal carbon having a mor-phology consisting of spheroidal primary particles (nodules)fused together in aggregates of colloidal dimension in a shapehaving grape-like clusters or open branch-li
10、ke structures3.1.3 carbon black, nan engineered material, primarilycomposed of elemental carbon, obtained from the partialcombustion or thermal decomposition of hydrocarbons, exist-ing in the form of aggregates of aciniform morphology whichare composed of spheroidal primary particles characterized b
11、yuniformity of primary particle sizes within a given aggregateand turbostratic layering within the primary particles.3.1.3.1 DiscussionParticle size and aggregate size (num-ber of particles per aggregate) are distributional properties andvary depending on the carbon black grade. Transmissionelectron
12、 micrographs shown in Annex A2 demonstrate thatwhile particle and aggregate sizes vary greatly within a givengrade of carbon black, the primary particle size is essentiallyuniform within an individual aggregate.1This practice is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the
13、direct responsibility of Subcommittee D24.66 on Environment,Health, and Safety.Current edition approved June 1, 2018. Published August 2018. Originallyapproved in 2000. Last previous edition approved in 2013 as D6602 13. DOI:10.1520/D6602-13R18.2Hess, W.M. and Herd, C.R., Carbon Black Science and Te
14、chnology, Edited byDonnet, J.B., Bansal, R.C., and Wang, M.J., Marcel Dekker, Inc., New York, NY,1993, pp. 89173.3For 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
15、 standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in th
16、e Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.4 chain of custodya document describing the condi-tion of a sample during its collection, analysis, and disposal.
17、3.1.5 chara particulate larger than 1 m made by incom-plete combustion which may not deagglomerate or disperse byordinary techniques, may contain material which is not black,and may contain some of the original materials cell structure,minerals, ash, cinders, and so forth.3.1.6 fugitive dusttransito
18、ry, fleeting material comprisedof particulates foreign to the surface of deposition.3.1.7 fungus, sooty mold, mildew, biofilmparticulates froma superficial growth that grows on living and decaying organicmatter.3.1.8 mineral dustnaturally occurring inorganic particu-lates inherent to the area such a
19、s soil minerals.3.1.9 pollenparticulates from a mass of microspores in aseed plant.3.1.10 rubber dustfinely divided soft particulates abradedfrom rubber.3.1.11 samplea small fractional part of a material or aspecified number of objects that are selected for testing,inspection, or specific observatio
20、ns of particular characteris-tics.3.1.12 soota submicron black powder generally producedas an unwanted by-product of combustion or pyrolysis. Itconsists of various quantities of carbonaceous and inorganicsolids in conjunction with adsorbed and occluded organic tarsand resins.3.1.12.1 DiscussionThe c
21、arbonaceous portion also is col-loidal and often has the aciniform morphology. Soot may haveseveral carbon morphologies. Examples of soot are carbonresidues from diesel and gasoline engines, industrial flares,sludge pits, burning tires, and so forth.3.1.13 sticky tapea section of tape with a sticky,
22、 solvent-soluble adhesive used in the collection of particles fromsurfaces.3.1.14 surfacethe outer surface, facing, or exterior bound-ary of an object capable of supporting carbon and other fugitiveand natural occurring dusts and particulates.3.1.15 turbostratica type of graphitic crystallographicst
23、ructure in which there is no symmetry along the z-axis.3.2 Acronyms:3.2.1 EDSenergy dispersive spectroscopy associated withSEM and TEM for the identification of elemental composition,3.2.2 LMlight microscope,3.2.3 PLMpolarizing light microscope,3.2.4 SEMscanning electron microscope,3.2.5 TEMtransmis
24、sion electron microscope.3.2.6 WDSwavelength dispersive spectroscopy associatedwith SEM and TEM for the identification of elemental com-position.NOTE 1Standard terminology relating to carbon black can be found inTerminology D3053.4. Summary of Practice4.1 This practice describes the procedures and p
25、rotocols tofollow in order to collect fugitive emission/environmentalsamples and identify the classes of particulate present includ-ing materials consistent or inconsistent with manufacturedcarbon black (referred to simply as carbon black). A semi-quantitative estimate of the percentage of each type
26、 of surfaceparticulate component is determined using polarized lightmicroscopy (PLM). However, PLM analysis cannot differen-tiate between carbon black and soots (black carbons) that maycome from many sources in the environment. Therefore,transmission electron microscopy (TEM) analysis is mandatoryin
27、 determining whether a sample contains carbon black.Because the preparation steps for the TEM analysis eliminatescertain types of particles and concentrates only the fine (small)particles from the sample, the TEM analysis alone cannot beused to estimate the amount of carbon black or other particlety
28、pe in the whole sample. Either the PLM or TEM analysismay be done first.4.2 Section 6 provides guidelines for proper sampling andhandling of fugitive emission/environmental samples. Sections8 and 9 describe the analysis of the sample using polarizedlight microscopy (PLM) and transmission electron mi
29、croscopy(TEM). The TEM analysis is critical in determining if thecollected sample is consistent or inconsistent with carbonblack. Use of the TEM analysis is mandatory in determiningwhether a sample is positive for carbon black. The use of thePLM analysis is not mandatory when the TEM analysis findsn
30、o aciniform aggregates resembling carbon black. Section 9describes additional ancillary techniques that may be includedin a sample analysis for purposes of providing supportinginformation as to the nature of the sample material. These aresituation-dependent methods and can provide critical identifi-
31、cation information in certain cases.4.3 Ablock diagram is presented in Fig. 1 to give a possiblescheme to follow in performing this analysis. However, itshould be noted that this diagram is a suggestion, not arequirement. Either the PLM or TEM analysis may be per-formed first.5. Significance and Use
32、5.1 There are a variety of darkening agents that contribute toair and surface contamination in industrial, urban and ruralenvironments. Biofilms (fungal and algal), soil minerals, plantfragments, rubber fragments, metal corrosion and soot arecommon darkening agents. Soot is formed as an unwantedby-p
33、roduct of combustion and consequently varies widely withthe type of fuel and combustion conditions. Carbon black, onthe other hand, is purposely produced under a controlled set ofconditions. Therefore, it is important to be able to distinguishcarbon black from soot, as well as other environmentalcon
34、taminants.6. Sampling6.1 The area to be sampled should be representative of thecontaminated area. For sampling, choose an area that appearsto contain black particulates. In some situations, the sameD6602 13 (2018)2general surface can be used for gathering all test samples foreach property site locat
35、ion or area.6.2 Equipment:6.2.1 Polyester Wipes (Texwipe Alphasat syntheic fiberwipes in 70 % alcohol/30 % DI water or equivalent).6.2.2 Sticky tape (Scotch Crystal Clear Tape, No. 25 orequivalent).6.2.3 Polyethylene Ziploc Bags.6.2.4 Standard Glass Microscope Slides.6.3 Samples are to be collected
36、by the following twotechniques (wipe and tape) in accordance with 6.3.1 and 6.3.2.Precautions should be taken to carefully collect, handle, andtransport samples in a manner that will not cause furthercontamination.6.3.1 Technique I: Wipe SamplingCollect the wipe sampleby wiping the surface to be sam
37、pled with a polyester wipe toremove surface particulates and solids. Light pressure on thewipe should be sufficient. Make sure that enough of an area hasbeen wiped to load the surface of the wipe. Place the exposedwipe in a ziploc bag and label.6.3.2 Technique II: Tape SamplingPrepare a tape-lift sl
38、ideby applying an appropriate length of tape to a clean glassmicroscope slide, leaving a tab for easy removal of the tape.Remove particulates and solids from surfaces by removing thetape from the prepared slide and applying it to the surface to besampled. Carefully remove the tape and place back acr
39、oss theglass microscope slide. Take care not to overload the tape.6.3.3 All collected samples must be clearly identified at thetime of collection.6.4 At the time of sample collection, complete a samplingrecord (Table 1) and also complete a chain of custody record(Table 2).6.5 This practice does not
40、preclude examination of samplescollected by other means than the preceding, such as polyeth-ylene glove wipes, filter paper, samples of clothing, materialscraped directly from the surface of interest, and so forth, or alarge sample taken in other containers at a spill site. However,these samples alw
41、ays require thorough identification taken atthe time of sample collection.6.6 It is advisable in the case of repeated incidents to cleanthe surface between sampling.7. Examination by Light Microscopy7.1 Summary of Test MethodThis method of examinationis a screening test method that provides an overv
42、iew of the bulkcomposition of the sample through examination under a lightmicroscope. This portion of the method is mandatory except incases where TEM examination gives no positive results foraciniform aggregates resembling carbon black and there is noFIG. 1 Block Diagram of Suggested Analysis Schem
43、e forSamplesTABLE 1 Example Sampling RecordSample Identification Number: _Sample Location: _Date of Sampling: _Comments:.D6602 13 (2018)3request for a semi-quantitative analysis of the other compo-nents in the sample. In addition, there are special situationswhere other information such as a torn ba
44、g near a carbon blackmanufacturing site strongly suggests that the black particulatebeing sampled is carbon black. In this case, a TEM analysismay be sufficient to confirm the presence of carbon blackwithout the mandatory PLM analysis. It is important to notethat the results obtained by the light mi
45、croscopy techniquecannot be considered as conclusive for identifying the presenceof carbon black.7.2 Apparatus:7.2.1 Light Stereomicroscope, capable of at least 40 mag-nification.7.2.2 Polarized Light Microscope, equipped with objectivesat least in the 10 to 40 range of magnification.7.2.3 Refractiv
46、e Index Liquids including Meltmount, 1.662or 1.55 RI Cargille liquid or equivalent.7.2.4 Scissors or Safety Razor Blades, or both.7.2.5 Glass Slides.7.2.6 Glass Cover Slips.7.2.7 Microscope Camera (Polaroid, 35 mm, or digital).7.2.8 Tungsten Needles.7.2.9 Forceps.7.2.10 Reference Slides of Particles
47、 Found in Dust Samples.7.2.11 Fiber-Optic Light Source, for reflected light exami-nation.7.3 Procedure:7.3.1 Inspect the tape-lift with a stereobinocular micro-scope. Note regions of interest where either jet black or darkparticles are visible.7.3.2 Inspect the tape-lift with a polarized light micro
48、scopeusing both transmitted and reflected light. The tape lift willpreserve intact colonies of fungal material (biofilm) if present.If the sampled surface is weathered paint, pigment lifted fromthe surface will not obscure or hinder identification of biofilmconstituents, as is often the case with wi
49、pe samples.Aciniformsoot will appear as opaque, jet black aggregates of particlesdisplaying a dull reflection in top light. The tape lift generallypreserves the integrity of the particle aggregates without thesmearing that tends to occur when using the wipe sampler.7.3.3 Inspect the wipe sample with a stereobinocular micro-scope. With a clean razor bla
