ASTM D5187-21

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it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
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Designation: D5187 − 10 (Reapproved 2015) D5187 − 21
Standard Test Method for
Determination of Crystallite Size (L ) of Calcined Petroleum
c
Coke by X-Ray Diffraction
This standard is issued under the fixed designation D5187; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial changes were made throughout in December 2015.
1. Scope Scope*
1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined
petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.
1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average
thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (L )
a
is not determined by this test method.
1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are
provided for information purposes only.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D346D6969 Practice for Collection and Preparation of Calcined Petroleum Coke Samples for Laboratory Analysis
D2013D6970 Practice for Preparing Coal Collection of Calcined Petroleum Coke Samples for Analysis
D2234/D2234M Practice for Collection of a Gross Sample of Coal
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Oct. 1, 2015Jan. 1, 2021. Published December 2015January 2021. Originally published in 1991. Last previous edition approved in 20102015
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as D5187 – 10.D5187 – 10 (2015) . DOI: 10.1520/D5187-10R15E01.10.1520/D5187-21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5187 − 21
3.1.1 crystallites, n—stacks of graphitic carbon platelets located parallel to one another.
3.1.2 L , n—the mean or average thickness of crystallites in a sample. It is expressed as a linear dimension in angstrom units, A˚
c
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(10 nm).
3.1.3 hkl(002), n—the Miller indices of the crystalline planes of graphite corresponding to a lattice spacing (d) of 3.35 Å.
3.1.4 Theta angle, Θ, n—the glancing angle produced when a parallel beam of uniform X-rays impinges upon a crystalline lattice.
This angle is measured by the X-ray goniometer and is usually expressed in degrees TwoTheta ° (2Θ).
4. Summary of Test Method
4.1 A packed sample pulverized to less than 75 μm is subjected to a monochromatic X-ray beam and rotated to produce a
diffraction pattern under specific conditions. The location and shape of the peak with hkl = (002) at d = 3.35 A˚ is used to
calculate the L by manual interpretation of the peak or by computer simulation.
c
5. Significance and Use
5.1 The crystallinity of petroleum coke, as reflected by the L value, is a general measure of quality affecting suitability for end
c
use and is a function of the heat treatment.
5.2 The crystallite thickness is used to determine the extent of such heat treatment, for example, during calcination. The value of
the L determined is not affected by coke microporosity or the presence of foreign, non-crystalline materials such as dedust oil.
c
6. Apparatus
6.1 X-Ray Powder Diffractometer, equipped with an X-ray source, a monochromator or filter for restricting the wavelength range,
a sample holder, a radiation detector, a signal processor, and readout (chart or computer memory). The diffractometer must be
capable of rate scanning at 1 °2Θ ⁄min or incrementally step scanning at 0.2 °2Θ steps.
6.2 Sample Holders, as specified by the manufacturer of the diffractometer that enables packing of a pulverized sample of
sufficient thickness to expose a level, smooth surface to the X-ray beam.
6.3 Briquetting Press, capable of generating pressures up to 69 MPa (10 000 psi).
6.4 Compressible Aluminum Caps, used as a support for producing a briquetted sample.
6.5 Silicon or Quartz Sample, available from National Institute of Standards and Technology (NIST).
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. It is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available.
Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without
lessening the accuracy of the determination.
7.2 Acetone.
7.3 Polyethylene Glycol, (approximate molecular weight of 200 AU).
“Reagent Chemicals, American Chemical Society Specification.” American Chemical ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington, D.C.DC. For suggestions on the testing of reagents not listed by the American Chemical
Society, see “AnalarAnalar Standards for Laboratory U.K.Chemicals, Chemicals,” BDH Ltd., Poole, Dorset, U.K., and the “United States Pharamacopeia.”United States
Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D5187 − 21
7.4 Binding Agent—Prepare a 15 % by mass solution of polyethylene glycol and acetone by adding 15 g of polyethylene glycol
to 85 g of acetone.
8. Sample Preparation
8.1 For recommended practices for obtaining, handling and preparing coke samples, refer to Test Methods D2013 and
D2234/D2234M and Practices D346D6969 and D4057D6970. The equipment and procedures for crushing and dividing are also
described in these test methods.practices.
8.2 Reduce and divide the gross sample to obtain a laboratory analysis sample.
8.3 Divide, by riffling, a minimum of 100 g from the laboratory analysis sample.
8.4 Crush 100 g of the test sample such that 98 % will pass through a 75 μm (No. 200) sieve.
8.5 Techniques—Any of the following techniques can be used for packing the sample into the X-ray diffractometer specimen
holder:
8.5.1 Back Fill Technique—Put the window on a glass slide (Slide 1) and transfer sufficient quantities of sample into the window.
Work the sample towards the corners of the holder by use of a glass slide or spatula. Press down using a flat glass slide and scrape
off any excess material. Place a glass slide (Slide 2) on top of the sample and secure with tape. Remove Slide 1 to expose a flat,
smooth surface before inserting into the diffractometer for analysis.
8.5.2 Front Fill Technique—Place a confining ring over the round sample holder and fill the holder cavity and ring with sample.
The ring will initially over
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