1、Designation: D6602 03b (Reapproved 2010)1D6602 13Standard 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
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 () indicates an editorial change since the last revision or reapproval.1 NOTEEditorially corrected Annex A1 in May 2010.1. Scope1.1 Thi
3、s practice covers sampling and testing for distinguishing ASTM type carbon black, in the N100 to N900 series, fromother environmental particulates.1.2 This practice requires some degree of expertise on the part of the microscopist. For this reason, the microscopist must haveadequate training and sub
4、stantial on-the-job experience in identifying the morphological parameters of carbon black. black andgeneral knowledge of other particles that may be found in the environment. In support of this analysis, Donnets book2 is highlyrecommended to be used as a technical reference for recognizing and unde
5、rstanding the microstructure of carbon black.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address allof the
6、 safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriatesafety and health practices and determine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D1619 Test Methods for Carbon
7、 BlackSulfur ContentD3053 Terminology Relating to Carbon BlackD3849 Test Method for Carbon BlackMorphological Characterization of Carbon Black Using Electron Microscopy3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aciniformshaped like a cluster of grapes.3.1.1.1 DiscussionTh
8、e spheroidal primary particles of carbon black are fused into aggregates of colloidal dimension forming an acinoformmorphology.3.1.2 aciniform carboncolloidal carbon having a morphology consisting of spheroidal primary particles (nodules) fusedtogether in aggregates of colloidal dimension in a shape
9、 having grape-like clusters or open branch-like structures3.1.3 carbon black, nan engineered material, primarily composed of elemental carbon, obtained from the partial combustionor thermal decomposition of hydrocarbons, existing in the form of aggregates of aciniform morphology which are composed o
10、fspheroidal primary particles characterized by uniformity of primary particle sizes within a given aggregate and turbostratic layeringwithin the primary particles.1 This practice is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.66 o
11、n Environment, Health, andSafety.Current edition approved Jan. 1, 2010Nov. 1, 2013. Published May 2010December 2013. Originally approved in 2000. Last previous edition approved in 20032010 asD6602 03b (2010)1. DOI: 10.1520/D660203BR10E01.10.1520/D6602-13.2 Hess, W.M. and Herd, C.R., Carbon Black Sci
12、ence and Technology, Edited by Donnet, J.B., Bansal, R.C., and Wang, M.J., Marcel Dekker, Inc., New York, NY, 1993,pp. 89173.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, r
13、efer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all
14、changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959
15、. United States13.1.3.1 DiscussionParticle size and aggregate size (number of particles per aggregate) are distributional properties and vary depending on the carbonblack grade. Transmission electron micrographs shown inAnnexAnnexA2 1 of Practice D6602demonstrate that while particle andaggregate siz
16、es vary greatly within a given grade of carbon black, the primary particle size is essentially uniform within anindividual aggregate.3.1.4 chain of custodya document describing the condition of a sample during its collection, analysis, and disposal.3.1.5 chara particulate larger than 1 m made by inc
17、omplete 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 dusttransitory, fleeting material comprised of particulates for
18、eign to the surface of deposition.3.1.7 fungus, sooty mold, mildewmildew, biofilmparticulates from a superficial growth that grows on living and decayingorganic matter.3.1.8 mineral and urban dustairborne, naturally occurring inorganic particulates inherent to the area.area such as soilminerals.3.1.
19、9 pollenparticulates from a mass of microspores in a seed plant.3.1.10 rubber dustfinely divided soft particulates abraded from rubber.3.1.11 samplea small fractional part of a material or a specified number of objects that are selected for testing, inspection, orspecific observations of particular
20、characteristics.3.1.12 soota submicron black powder generally produced as an unwanted by-product of combustion or pyrolysis. It consistsof various quantities of carbonaceous and inorganic solids in conjunction with adsorbed and occluded organic tars and resins.3.1.12.1 DiscussionThe carbonaceous por
21、tion also is colloidal and often has the aciniform morphology. Soot may have several carbon morphologies.Examples of soot are carbon residues 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, solvent-solub
22、le adhesive used in the collection of particles from surfaces.3.1.14 surfacethe outer surface, facing, or exterior boundary of an object capable of supporting carbon and other fugitive andnatural occurring dusts and particulates.3.1.15 turbostratica type of graphitic crystallographic structure in wh
23、ich there is no symmetry along the z-axis.3.2 Acronyms:3.2.1 EDSenergy dispersive spectroscopy associated with SEM 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 TEMtransmission electro
24、n microscope.3.2.6 TEMWDStransmission electron microscope.wavelength dispersive spectroscopy associated with SEM and TEM forthe identification of elemental composition.NOTE 1Standard terminology relating to carbon black can be found in Terminology D3053.4. Summary of PracticePractices4.1 This practi
25、ce describes the procedures and protocols to follow in order to collect fugitive emission/environmental samplesand identify if these samples contain the classes of particulate present including materials consistent or inconsistent withmanufactured carbon black (referred to simply as carbon black). A
26、 semi-quantitative estimate of the percentage of each type ofsurface particulate component is determined using polarized light microscopy (PLM). However, PLM analysis cannot differentiatebetween carbon black and soots (black carbons) that may come from many sources in the environment. Therefore, tra
27、nsmissionelectron microscopy (TEM) analysis is mandatory in determining whether a sample contains carbon black. Because the preparationsteps for the TEM analysis eliminates certain types of particles and concentrates only the fine (small) particles from the sample,the TEM analysis alone cannot be us
28、ed to estimate the amount of carbon black or other particle type in the whole sample. Eitherthe PLM or TEM analysis may be done first.4.2 Section 6 provides guidelines for proper sampling and handling of fugitive emission/environmental samples. SectionSec-tions 78 describesand 9 describe the analysi
29、s of the sample using polarized light microscopy (PLM) and transmission electronmicroscopy (TEM). This The TEM analysis is critical in determining if the collected sample is consistent or inconsistent with theD6602 132morphology of carbon black. Use of this the TEM analysis is mandatory in applying
30、this practice. determining whether a sampleis positive for carbon black. The use of the PLM analysis is not mandatory when the TEM analysis finds no aciniform aggregatesresembling carbon black. Section 89 describes additional ancillary techniques that may be included in a sample analysis forpurposes
31、 of providing supporting information as to the nature of the sample material. These are situation-dependent methods andcan provide critical identification information in certain cases.4.3 A block diagram is presented in Fig. 1 to give a possible scheme to follow in performing this analysis. However,
32、 it shouldbe noted that this schemediagram is a suggestion, not a requirement. Either the PLM or TEM analysis may be performed first.5. Significance and Use5.1 Particulate emissions are major contributors to air contamination in industrial and urban environments. There are a varietyof darkening agen
33、ts that contribute to air and surface contamination in industrial, urban and rural environments. Biofilms (fungaland algal), soil minerals, plant fragments, rubber fragments, metal corrosion and soot are common darkening agents. Soot is formedas an unwanted by-product of combustion and consequently
34、varies widely with the type of fuel and combustion conditions. Carbonblack, on the other hand, is purposely produced under a controlled set of conditions. Therefore, it is important to be able todistinguish carbon black from soot, as well as other environmental contaminants.6. Sampling6.1 The area t
35、o be sampled mustshould be representative of the contaminated area. For sampling, choose an area that appearsto contain black particulates. The In some situations, the same general surface shouldcan be used for gathering all test samples foreach property site location.location or area.6.2 Equipment:
36、6.2.1 Polyester/Cotton BallsPolyester Wipes or Glass Fiber Pads.(Texwipe Alphasat syntheic fiber wipes in 70 % alcohol/30 %DI water or equivalent).6.2.2 Sticky tape (Scotch Crystal Clear Tape, No. 25 or equivalent).FIG. 1 Block Diagram of Suggested Analysis Scheme for SamplesD6602 1336.2.3 Petri Dis
37、hes or Polyethylene Polyethylene Ziploc Bags.6.2.4 Standard Glass Microscope Slides.6.3 Samples are to be collected by the following two techniques (wipe and tape) in accordance with 6.3.1 and 6.3.2. Precautionsshould be taken to carefully collect, handle, and transport samples in a manner that will
38、 not cause further contamination.6.3.1 Technique I: Wipe SamplingCollect the wipe sample by rubbingwiping the surface to be sampled with a pre-weighed polyester ball or glass fiber filter pad witha light back-and-forth motion polyester wipe to remove surface particulates and solids. Do not try to re
39、move “old” or agedcontaminants from the surface. Light pressure on the ball or pad wipe should be sufficient. Make sure that enough of an area hasbeen wiped to load the surface of the wipe. Place the exposed ball or pad wipe in a plasticziploc bag and label.6.3.2 Technique II: Tape SamplingPrepare a
40、 tape-lift slide by applying an appropriate length of tape to a clean glass microscope slide, leaving a tab for easy removalof the tape. Remove particulates and solids from surfaces by placing an appropriate length of sticky tape on the removing the tapefrom the prepared slide and applying it to the
41、 surface to be sampled. Carefully remove the tape and place across a petri dish openingor in a polyethylene bag. All samples collected must be clearly identified at the time of collection. This technique may be usedfor samples intended for further examination via light microscopy or X-ray spectrosco
42、py or both. back across the glass microscopeslide. Take care not to overload the tape.6.3.3 All collected samples must be clearly identified at the time of collection. Measure the surface area sampled to the nearest60.25 cm2 (each measurement has to be taken to the nearest 60.5 cm) and record the me
43、asurement in Table 1. These samples maybe used for microscopy and TGA analysis. Please note that if TGA analysis is a possibility, the samples should be collected onthe fiber pad instead of the polyester ball.6.4 At the time of sample collection, complete a sampling and meteorology record (Table 21)
44、 and also complete a chain ofcustody record (Table 12).6.5 This practice does not preclude examination of samples collected by other means than the preceding, such as polyethyleneglove wipes, filter paper, samples of clothing, material scraped directly from the surface of interest, and so forth, or
45、a large sampletaken in other containers at a spill site. However, these samples always require thorough identification taken at the time of samplecollection.6.6 It is advisable in the case of repeated incidents to clean the surface between sampling.7. Examination by Light Microscopy7.1 Summary of Te
46、st MethodThis method of examination is a screening test method that provides an overview of the bulkcomposition of the sample through examination under a light microscope. This portion of the method is mandatory except in caseswhere TEM examination gives no positive results for aciniform aggregates
47、resembling carbon black and there is no request for asemi-quantitative analysis of the other components in the sample. In addition, there are special situations where other informationsuch as a torn bag near a carbon black manufacturing site strongly suggests that the black particulate being sampled
48、 is carbon black.In this case, a TEM analysis may be sufficient to confirm the presence of carbon black without the mandatory PLM analysis. Itis important to note that the results obtained by the light microscopy technique cannot be considered as conclusive for identifyingthe presence of carbon blac
49、k.7.2 Apparatus:7.2.1 Light Stereomicroscope, capable of at least 40 magnification.7.2.2 Polarized Light Microscope, equipped with objectives at least in the 10 to 40 range of magnification.7.2.3 Refractive Index Liquids including Meltmount, 1.662 or 1.55 RI Cargille liquid or equivalent.TABLE 1 Example Sampling RecordSample Identification Number: _Sample Location: _Date of Sampling: _
