ASTM D5061-2016 Standard Test Method for Microscopical Determination of the Textural Components of Metallurgical Coke《冶金焦炭结构部件显微测定的标准试验方法》.pdf

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1、Designation: D5061 07D5061 16Standard Test Method forMicroscopical Determination of the Textural Components ofMetallurgical Coke1This standard is issued under the fixed designation D5061; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis

2、ion, 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 the equipment and procedures used for determining the types and amounts of co

3、ke carbon formsand associated recognizable coal- and process-derived textural components in metallurgical coke in terms of volume percent. Thistest method does not include coke structural components such as coke pores, coke wall dimensions, or other structural associations.1.2 The values stated in S

4、I units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and heal

5、th practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD3997D3997/D3997M Practice for Preparing Coke Samples for Microscopical Analysis by Reflected Light3. Terminology3.1 DefinitionsFor additiona

6、l definitions of terms used in this test method, refer to Terminology D121.3.2 Definitions of Terms Specific to This Standard:3.2.1 anisotropic, adjexhibiting optical properties of different values when viewed with an optical microscope havingmutually exclusive polarized light, for example, crossed

7、nicols.3.2.2 binder phase, na continuous solid carbon matrix formed during the thermoplastic deformation of those coal maceralsthat become plastic during carbonization.3.2.2.1 DiscussionThe binder phase material is formed from the thermoplastic deformation of reactive (vitrinite and liptinite) and s

8、emi-inert(semifusinite) coal macerals of metallurgical bituminous coals. During thermoplasticity, the inert coal maceral and mineral arepartly or wholly incorporated into the binder phase. Also, most of the coke pores are located in the binder phase.3.2.3 carbon form, nmicroscopically distinguishabl

9、e carbonaceous textural components of coke, but excluding mineralcarbonates.3.2.3.1 DiscussionCarbon forms are recognized on the basis of their reflectance, anisotropy, and morphology. They are derived from the organicportion of coal and can be anisotropic or isotropic.1 This test method is under th

10、e jurisdiction ofASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.28 on PetrographicAnalysisof Coal and Coke.Current edition approved Oct. 1, 2007April 1, 2016. Published Ocotber 2007April 2016. Originally approved in 1992. Last previous edition approved in 20

11、052007 asD5061 - 05.D5061 - 07. DOI: 10.1520/D5061-07.10.1520/D5061-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the AST

12、M 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 changes accurately, ASTM recommends that users consult

13、 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. United States13.2.4 circular anisotropic phase, na g

14、roup of binder-phase anisotropic carbon textures that are distinguished by approximatelycircular domains (that is length equals width) and composed of fine circular (0.5 to 1.0-m), medium circular (1.0 to 1.5-m), andcoarse circular (1.5 to 2.0-m) size categories.3.2.5 coke pore, na microscopically d

15、istinguishable void that is a structural element of coke.3.2.5.1 DiscussionCoke pores are considered to be nearly spherical-shaped voids created by the entrapment of gaseous volatiles during thesolidification of thermoplastic coal. However, other types of voids can be distinguished in coke that incl

16、ude fractures or cracks,interconnected and elongated pores, and the open cell lumens of fusinite and semifusinite. The size and shape of the voids are coalrank and grade, and to some degree, process dependent. Pore sizes vary from tens of angstroms to tens of millimetres in any givencoke.3.2.6 coke

17、reactivity, na measure of the mass loss when coke, held at a designated temperature, is contacted with gaseouscarbon dioxide over a specific time interval.3.2.7 coke wall, na predominantly carbonaceous layer that encloses a coke pore and which is a structural element and essenceof coke.3.2.8 deposit

18、ional carbon, na group of carbon forms that are formed from cracking and nucleation of gas-phase hydrocarbonmolecules during coal carbonization.3.2.8.1 pyrolytic carbon, nan anisotropic carbon form that is formed by the deposition of carbon parallel to an inert substratecausing the resulting texture

19、 to appear ribbon-like.3.2.8.2 sooty carbon, nan isotropic carbon form comprised of approximately spherical particles of less than 1-m diametersometimes referred to as combustion black.3.2.8.3 spherulitic carbon, na spherical anisotropic carbon form sometimes referred to as thermal black that is for

20、med by thedeposition of carbon concentrically around a nucleus.3.2.9 domain, na region of anisotropy in a carbon form that is distinctively marked by its isochromatic boundary and cleavage.3.2.10 filler phase, na discontinuous solid formed from coal macerals and minerals that do not deform thermopla

21、sticallyduring carbonization.3.2.10.1 DiscussionThe filler phase material is formed from coal macerals that are inert with respect to development of thermoplasticity (inertinite),the inorganic components of coal (minerals), as well as normally reactive coal entities that are noncoking or have been r

22、enderedinert by thermal oxidation, natural weathering or brecciation. These inert materials possess their original morphologies, but theirreflectance and chemical properties have been altered prior to or during carbonization.3.2.11 green coke, ncarbonaceous binder or filler phase material that has e

23、xceeded the temperature of thermoplasticity, buthas not obtained the temperature of metallurgical coke.3.2.11.1 DiscussionGreen coke is recognized on the basis of relative reflectance in comparison to fully carbonized coke. Green coke exhibits varyingdegrees of lower reflectance than fully carbonize

24、d coke.3.2.12 incipient anisotropic phase, na binder-phase carbon texture having a domain size (less than 0.5 m) that is near themeasuring resolution of the light microscope.3.2.13 isotropic phase, na binder-phase carbon texture that exhibits optical properties that are the same in all directions wh

25、enviewed with an optical microscope having mutually exclusive polarized light, for example, crossed nicols.3.2.14 lenticular anisotropic phase, na group of binder-phase anisotropic carbon textures distinguished by their lens-shapeddomains (that is, length (L) to width (W) ratio of 2W 4W), and subdiv

26、ided based on domain width as fine ribbon (2.0 to 12.0-m),medium ribbon (12.0 to 25.0-m), and coarse ribbon (25.0-m) size categories.3.2.16 textural component, nthe collective term used to describe carbon forms and recognizable coal- and process-derivedcomponents (binder-phase, filler-phase, and mis

27、cellaneous material) in coke.3.2.17 vitrinite type, nreflectance classes of vitrinite which span 0.1 % reflectance intervals.D5061 1623.2.17.1 DiscussionThis term is commonly referred to as V-Type. For example, V-type 6 includes vitrinite reflectance values from 0.6 through 0.69 %.4. Summary of Test

28、 Method4.1 The textural components of coke (coke carbon forms and associated coal- and process-related components) in arepresentative crushed particulate coke sample, prepared in the form of a briquetted, polished specimen as described in PracticeD3997D3997/D3997M, are identified under a microscope

29、according to their degree of anisotropism, carbon form domain sizes,boundary size, color of individual isochromatic domains, their morphology, relative reflectance, and other optical properties. Theproportions of these textural components in a sample are determined by observing a statistically adequ

30、ate number of points, andsumming those representative of each component. Only area proportions of components are observed on the briquette surface.However, the area and volume proportions are the same when the components are randomly distributed throughout the sample.4.1.1 Color photomicrographs of

31、the textural components of metallurgical coke illustrating their microscopic features areavailable from various publications and websites.3,45. Significance and Use5.1 The determination of the volume percent of the textural components in coke is useful to characterize the optical propertiesof coke a

32、s it relates to utilization. Specifically, the technique has been used as an aid in determining coal blend proportions (aftercorrecting for coke yield), proportions, and recognition of features present in the coke that can be responsible for coke quality orproduction problems such as reduced coke st

33、rength or difficulty in removing coke from commercial coke ovens, or both. The studyof coke textures is also useful in promoting a better understanding of coke reactivity, and the relationship between coal petrographyand its conversion to coke.45.2 This test method is used in scientific and industri

34、al research, but not for compliance or referee tests.6. Apparatus6.1 MicroscopeA high quality reflected-light microscope with a vertical illuminator and rotating mechanical stage is used,provided that the objective and eyepiece lenses permit resolution of objects on the order of 0.5 m. The objective

35、 lens shall be ofsuch construction that samples can be studied in oil with plane-polarized light. A minimum total magnification of approximately500 diameters is recommended. Use of an accessory plate (quartz, gypsum, or mica), an analyzer, and polarizer combination isrecommended to achieve optimum o

36、ptical effect for discriminating among the various textural components. Either a prism or apartially reflecting glass plate may be employed in the illuminator. One eyepiece of the microscope must be fitted with a specialruled graticule disc.6.1.1 Eyepiece DiscThe eyepiece shall contain a ruled grati

37、cule disc to enable size estimations and to provide a field-of-viewgrid for point counting. The design may be a squared pattern (10 by 10 squares) containing a bolder crosshair with one of thesquares near the center crosshair intersection divided into 25 subsquares. The ruled portion of the disc sha

38、ll cover at least one thirdof the field of view.6.1.2 Mechanical StageThe mechanical stage shall be of such type that the specimen can be quickly advanced by definitefixed increments in two perpendicular directions (referred to as the X and Y directions).6.2 CounterThe counter shall be capable of re

39、cording counts for at least eight components (preferably twelve or more)equipped with a totalizer. The counter design can either be mechanical or electrical.6.3 Immersion OilThe oil shall be a nondrying, noncorrosive, noncarcinogenic type having similar properties as used for coalmicroscopic techniq

40、ues.7. Organization of Analysis47.1 Textural components are grouped into three major categories; (1) binder phase carbon forms, (2) filler phase carbon forms(including coal-related inorganic material), and (3) miscellaneous materials. These categories are shown in summary form in Table1. Volume perc

41、ent of the various types of binder phase carbon forms should be determined during the first microscopic analyses.The volume percent of the filler phase (including coal-related inorganic material) should be determined as a second analysis. Themiscellaneous materials are commonly determined during ana

42、lysis of the filler phase.7.1.1 Binder Phase Carbon Form DeterminationsThe components counted and kept separate shall be the following: isotropic,incipient, circular anisotropic (fine), circular anisotropic (medium), circular anisotropic (coarse), lenticular anisotropic (fine),lenticular anisotropic

43、 (medium), lenticular anisotropic (coarse), ribbon anisotropic (fine), ribbon anisotropic (medium), ribbon3 Crelling, J.C., and Rimmer, S.M., 2015, Crellings Petrographic Atlas of Coals, Cokes, Char, Carbons, and Graphites available from http:/mccoy.lib.siu.edu/projects/crelling2/atlas/. Coals and C

44、arbons, Southern Illinois University Carbondale, http:/www.coalandcarbonatlas.siu.edu/.4 Gray, R. J., and DeVanney, K. F., “Coke Carbon Forms: Microscopic ClassificationAndand IndustrialApplications,” International Journal of Coal Geology, Vol 6, 1986,pp. 277297.D5061 163anisotropic (coarse). These

45、binder phase categories relate to parent coal rank. When other components (filler phase, includingcoal-related inorganic material, and miscellaneous materials) are encountered, they are to be allocated to the appropriate binderphase category within which they are incorporated.7.1.2 Filler Phase Carb

46、on Form Determinations (Including Coal-Related Inorganic Material)The components counted andkept separate shall be the following: one category for all binder phase carbons (no discrimination to specific binder phasecomponents is necessary), organic inerts (fine), organic inerts (coarse), inorganic i

47、nerts (fine), inorganic inerts (coarse),miscellaneous inerts (by type, such as noncoking vitrinite, coked oxidized coal, coked brecciated coal, etc.), and others. Filler phasematerials relate back to the parent coal type.7.1.3 Miscellaneous Materials DeterminationThe components counted and kept sepa

48、rate shall be the following: depositionalcarbons (by type, that is, sooty, spherulitic, or pyrolytic) and any other observations such as additives (breeze, anthracite, petroleumcoke, etc.), coal, and green coke (by relative degree). Due to the normally small occurrences or absence of these component

49、s, theyare commonly counted during the filler phase counting procedure described in 7.1.2.These miscellaneous materials generally relateto coke plant processes and operational practices not directly related to parent coal rank or type.NOTE 1The degree of detail necessary will dictate the specific components quantified. The specified components to be counted in this test methodassume that the operator is generating a detailed analysis. It may be practical to lump some components together.This is up to the discretion of the operatoror