ASTM D5187 Standard Test Method for Determination of Crystallite Size (Lc) of Calcined Petroleum Coke by X-Ray Diffraction
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° per minute or incrementally step scanning at 0.2° per step.
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 10 000 psi (69 MPa).
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).
7.4 Binding Agent - Prepare a 15 mass % solution of polyethylene glycol and acetone by adding 15 g of polyethylene glycol to 85 g of acetone.
