International Tables for Crystallography (2019). Vol. H. ch. 2.10, pp. 200-222
https://doi.org/10.1107/97809553602060000945

Chapter 2.10. Specimen preparation

Contents

  • 2.10. Specimen preparation  (pp. 200-222) | html | pdf | chapter contents |
    P. S. Whitfield, A. Huq and J. A. Kaduk
    • 2.10.1. X-ray powder diffraction  (pp. 200-218) | html | pdf |
      • 2.10.1.1. Powders and particle statistics (granularity)  (pp. 201-206) | html | pdf |
      • 2.10.1.2. Preferred orientation  (pp. 206-209) | html | pdf |
      • 2.10.1.3. Absorption (surface roughness), microabsorption and extinction  (pp. 209-211) | html | pdf |
        • 2.10.1.3.1. Absorption (surface roughness)  (pp. 209-210) | html | pdf |
        • 2.10.1.3.2. Microabsorption  (p. 210) | html | pdf |
        • 2.10.1.3.3. Extinction  (pp. 210-211) | html | pdf |
      • 2.10.1.4. Holders  (pp. 211-218) | html | pdf |
        • 2.10.1.4.1. Reflection sample holders  (pp. 211-213) | html | pdf |
        • 2.10.1.4.2. Transmission sample holders  (pp. 213-218) | html | pdf |
          • 2.10.1.4.2.1. Flat foils  (pp. 213-215) | html | pdf |
          • 2.10.1.4.2.2. Capillaries  (pp. 215-218) | html | pdf |
    • 2.10.2. Neutron powder diffraction  (pp. 218-221) | html | pdf |
      • 2.10.2.1. Specimen form  (p. 218) | html | pdf |
      • 2.10.2.2. Sample size  (p. 218) | html | pdf |
      • 2.10.2.3. Specimen containment  (pp. 218-219) | html | pdf |
      • 2.10.2.4. Isotopes, absorption and activation  (pp. 219-221) | html | pdf |
    • 2.10.3. Conclusions  (p. 221) | html | pdf |
    • References | html | pdf |
    • Figures
      • Fig. 2.10.1. Calculated corundum powder patterns using the structure of Lewis et al  (p. 200) | html | pdf |
      • Fig. 2.10.2. 2D images of the spotty Debye rings of a coarse (~35 µm) cement powder using a Co Kα radiation 1 mm point source  (p. 201) | html | pdf |
      • Fig. 2.10.3. 2D image from the same sample after reducing the crystallites down to a few µm, together with the properly averaged integrated data  (p. 201) | html | pdf |
      • Fig. 2.10.4. 2D image showing the Debye rings when the unmilled sample from Fig  (p. 201) | html | pdf |
      • Fig. 2.10.5. The appearance of specimen granularity in a hand-ground specimen of a railroad tank car corrosion deposit  (p. 202) | html | pdf |
      • Fig. 2.10.6. An extreme example of granularity  (p. 202) | html | pdf |
      • Fig. 2.10.7. Optical microscope images of the surfaces of the hand-ground and micronized specimens of Scott's Moss Control Granules  (p. 203) | html | pdf |
      • Fig. 2.10.8. Rietveld refinement plot for micronized Scott's Moss Control Granules  (p. 203) | html | pdf |
      • Fig. 2.10.9. A rocking curve (φ scan) of (Ba0.7Sr1.3)TiO4, with the detector fixed at 9.647° 2θ, the top of a strong peak in the synchrotron pattern  (p. 203) | html | pdf |
      • Fig. 2.10.10. Rietveld plot of a mixture of β-17α-estradiol hemihydrate and α-17α-estradiol  (p. 204) | html | pdf |
      • Fig. 2.10.11. The main 101 reflection in data collected from a very coarse (~100 µm) highly crystalline quartz  (p. 204) | html | pdf |
      • Fig. 2.10.12. Comparison between capillary (0.3 mm, 0.8265 Å) and rocking flat-plate (strip heater, 1.2386 Å, ω ±2°) data from the Australian Synchrotron  (p. 204) | html | pdf |
      • Fig. 2.10.13. φ scans of the five fingers of quartz for (a) <38 µm, (b) <15 µm and (c) micronized samples  (p. 205) | html | pdf |
      • Fig. 2.10.14. Optical micrographs of (a) -400 mesh quartz at 100× magnification and (b) quartz milled in a McCrone micronizer for 15 min in isopropyl alcohol at 150× magnification  (p. 206) | html | pdf |
      • Fig. 2.10.15. Diagram showing the source of improved particle statistics in reflection geometry using a 1D position sensitive detector (PSD) versus a point detector  (p. 206) | html | pdf |
      • Fig. 2.10.16. Top: diffraction pattern of top-loaded 400 mesh phlogopite mica  (p. 207) | html | pdf |
      • Fig. 2.10.17. Diffraction pattern of top-loaded miconized phlogopite mica  (p. 207) | html | pdf |
      • Fig. 2.10.18. Diffraction pattern of miconized phlogopite mica when back-loaded onto a smooth surface  (p. 207) | html | pdf |
      • Fig. 2.10.19. 20× optical micrograph of a cross section of the 400-grit carborundum paper used for back-loaded mica  (p. 207) | html | pdf |
      • Fig. 2.10.20. Diffraction pattern of micronized phlogopite mica when back-loaded onto 400-grit carborundum paper  (p. 208) | html | pdf |
      • Fig. 2.10.21. Diffraction pattern of top-loaded spray-dried phlogopite mica  (p. 208) | html | pdf |
      • Fig. 2.10.22. SEM micrograph of spray-dried micronized phlogopite mica (courtesy of M  (p. 208) | html | pdf |
      • Fig. 2.10.23. View through the alignment scope of the spherical spray-dried mica inside a 0.5 mm capillary  (p. 208) | html | pdf |
      • Fig. 2.10.24. Plot of the ratio of the integrated intensities of the 001/200 reflections of the mica using different sample-preparation techniques  (p. 208) | html | pdf |
      • Fig. 2.10.25. SEM micrograph of wollastonite needles  (p. 208) | html | pdf |
      • Fig. 2.10.26. Effect of preferential orientation on data from top-loaded wollastonite compared with the calculated pattern from the literature wollastonite-1A structure (Ohashi, 1984)  (p. 209) | html | pdf |
      • Fig. 2.10.27. Rietveld refinement fit to the literature wollastonite-1A structure (Ohashi, 1984) with data from a 0.3 mm capillary with no orientation corrections  (p. 209) | html | pdf |
      • Fig. 2.10.28. Rietveld refinement fit to the literature wollastonite-1A structure (Ohashi, 1984) with data from a 0.2 mm capillary with no orientation corrections  (p. 209) | html | pdf |
      • Fig. 2.10.29. The effect of surface roughness on the intensity compared to that of a bulk copper specimen  (p. 209) | html | pdf |
      • Fig. 2.10.30. Powder patterns of a commercial cobalt silicate sample, measured from a (rough) slurry-mounted specimen (red) and from a (flat) conventional front-packed specimen (green)  (p. 210) | html | pdf |
      • Fig. 2.10.31. Derivation of the equation relating peak displacement to sample displacement (s) in parafocusing geometry  (p. 211) | html | pdf |
      • Fig. 2.10.32. A home-made top-loading zero-background silicon holder with a 0.5 mm deep cavity  (p. 211) | html | pdf |
      • Fig. 2.10.33. Commercial holder for air-sensitive samples  (p. 212) | html | pdf |
      • Fig. 2.10.34. Filling a commercial back-loading sample holder  (p. 212) | html | pdf |
      • Fig. 2.10.35. Data from powdered sucrose on a Bragg–Brentano instrument, with the peak intensities normalized to the first reflection  (p. 212) | html | pdf |
      • Fig. 2.10.36. Diffraction pattern from a silicon-wafer zero-background holder, smears of Vaseline and Corning high-vacuum grease, and the surface treated with hairspray  (p. 213) | html | pdf |
      • Fig. 2.10.37. Parts prior to assembly of a transmission foil sample in the holder  (p. 214) | html | pdf |
      • Fig. 2.10.38. Transmission data from double layers (as used for powder samples) of different polymer substrate films  (p. 214) | html | pdf |
      • Fig. 2.10.39. Diffraction pattern from loose SRM640c powder between two 50 µm Kapton foils  (p. 214) | html | pdf |
      • Fig. 2.10.40. Transmitted light view of a micronized quartz sample through 50 µm Kapton foils  (p. 214) | html | pdf |
      • Fig. 2.10.41. Comparison of data from micronized 40S mica taken in reflection and transmission geometry, and spray-dried material in reflection geometry  (p. 214) | html | pdf |
      • Fig. 2.10.42. Comparison of the diffraction patterns of pure SnO2 from a 0.3 mm quartz capillary in transmission and reflection geometries with Cu Kα radiation  (p. 216) | html | pdf |
      • Fig. 2.10.43. Raw diffraction data from 0.3 mm capillaries of SnO2 diluted with 8000 grit diamond powder and carbon black  (p. 216) | html | pdf |
      • Fig. 2.10.44. Rietveld refinement of the diamond-diluted data with the SnO2 cassiterite structure  (p. 216) | html | pdf |
      • Fig. 2.10.45. Comparison of data from SnO2 when diluted with diamond inside a 0.3 mm capillary and pure SnO2 coated on the outside of a 0.3 mm capillary  (p. 217) | html | pdf |
      • Fig. 2.10.46. Comparison of the background from four different 0.5 mm-diameter capillaries  (p. 217) | html | pdf |
      • Fig. 2.10.47. Platform and pin mounts for capillary samples  (p. 217) | html | pdf |
      • Fig. 2.10.48. A 0.5mm capillary secured into a standard brass capillary pin using dental wax at both ends of the pin  (p. 217) | html | pdf |
      • Fig. 2.10.49. Goniometer head position in relation to the goniometer-mounted alignment scope  (p. 218) | html | pdf |
      • Fig. 2.10.50. Two examples of sample holders used in neutron powder diffraction  (p. 218) | html | pdf |
      • Fig. 2.10.51. Two sample holders used for high-temperature studies  (p. 219) | html | pdf |
      • Fig. 2.10.52. Aerodynamic levitation system to suspend melts at temperatures to 2773 K and beyond for neutron diffraction measurements  (p. 219) | html | pdf |
      • Fig. 2.10.53. Calculation of the penetration of neutrons into Li3N using the online tool at https://www.ncnr.nist.gov/resources/activation/   (p. 220) | html | pdf |
    • Tables
      • Table 2.10.1. Intensity (counts) and mean deviation in intensity of the main quartz 101 reflection with a stationary sample of -325 mesh quartz powder  (p. 205) | html | pdf |
      • Table 2.10.2. Theoretical behaviour of different crystallite sizes of quartz in a volume of 20 mm3  (p. 205) | html | pdf |
      • Table 2.10.3. Absorption and physical characteristics of the capillaries whose data are shown in Fig. 2.10.46  (p. 215) | html | pdf |