International Tables for Crystallography
Volume H: Powder diffraction

First online edition (2019)   ISBN: 978-1-118-41628-0   doi: 10.1107/97809553602060000115  

Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

Contents

• Preface  (p. xxviii) | html | pdf |
  C. J. Gilmore, J. A. Kaduk and H. Schenk

• Introduction
  • 1.1. Overview and principles of powder diffraction  (pp. 2-23) | html | pdf | chapter contents |
    R. E. Dinnebier and S. J. L. Billinge
    • 1.1.1. Information content of a powder pattern  (p. 2) | html | pdf |
    • 1.1.2. The peak position  (pp. 2-9) | html | pdf |
    • 1.1.3. The peak intensity  (pp. 9-11) | html | pdf |
    • 1.1.4. The peak profile  (pp. 11-15) | html | pdf |
    • 1.1.5. The background  (pp. 15-19) | html | pdf |
    • 1.1.6. Local and global optimization of crystal structures from powder diffraction data  (pp. 19-22) | html | pdf |
    • 1.1.7. Outlook  (pp. 22-23) | html | pdf |
    • References | html | pdf |

• Instrumentation and sample preparation
  • 2.1. Instrumentation for laboratory X-ray scattering techniques  (pp. 26-50) | html | pdf | chapter contents |
    A. Kern
    • 2.1.1. Introduction  (p. 26) | html | pdf |
    • 2.1.2. Scope and terminology  (p. 26) | html | pdf |
    • 2.1.3. Historical overview  (pp. 26-28) | html | pdf |
    • 2.1.4. The platform concept – fitting the instrument to the need  (pp. 28-32) | html | pdf |
    • 2.1.5. Goniometer designs  (pp. 32-36) | html | pdf |
    • 2.1.6. X-ray sources and optics  (pp. 36-45) | html | pdf |
    • 2.1.7. X-ray detectors  (pp. 45-49) | html | pdf |
    • References | html | pdf |
  • 2.2. Synchrotron radiation and powder diffraction  (pp. 51-65) | html | pdf | chapter contents |
    A. Fitch
    • 2.2.1. Introduction  (p. 51) | html | pdf |
    • 2.2.2. Production of synchrotron radiation  (pp. 51-54) | html | pdf |
    • 2.2.3. Optics  (pp. 54-56) | html | pdf |
    • 2.2.4. Diffractometers  (pp. 56-60) | html | pdf |
    • 2.2.5. Considerations for powder-diffraction experiments  (pp. 60-63) | html | pdf |
    • References | html | pdf |
  • 2.3. Neutron powder diffraction  (pp. 66-101) | html | pdf | chapter contents |
    C. J. Howard and E. H. Kisi
    • 2.3.1. Introduction to the diffraction of thermal neutrons  (pp. 66-67) | html | pdf |
    • 2.3.2. Neutrons and neutron diffraction – pertinent details  (pp. 67-70) | html | pdf |
    • 2.3.3. Neutron sources  (pp. 70-80) | html | pdf |
    • 2.3.4. Diffractometers  (pp. 80-92) | html | pdf |
    • 2.3.5. Experimental considerations  (pp. 92-98) | html | pdf |
    • 2.3.6. Concluding remarks  (p. 98) | html | pdf |
    • References | html | pdf |
  • 2.4. Electron powder diffraction  (pp. 102-117) | html | pdf | chapter contents |
    J.-M. Zuo, J. L. Lábár, J. Zhang, T. E. Gorelik and U. Kolb
    • 2.4.1. Introduction  (pp. 102-103) | html | pdf |
    • 2.4.2. Electron powder diffraction pattern geometry and intensity  (pp. 103-104) | html | pdf |
      J.-M. Zuo and J. L. Lábár
    • 2.4.3. Electron powder diffraction techniques  (pp. 105-108) | html | pdf |
      J.-M. Zuo and J. Zhang
    • 2.4.4. Phase identification and phase analysis  (pp. 108-110) | html | pdf |
      J. L. Lábár
    • 2.4.5. Texture analysis  (pp. 110-111) | html | pdf |
      J. L. Lábár
    • 2.4.6. Rietveld refinement with electron diffraction data  (pp. 111-113) | html | pdf |
      T. E. Gorelik and U. Kolb
    • 2.4.7. The pair distribution function from electron diffraction data  (pp. 113-114) | html | pdf |
      T. E. Gorelik and U. Kolb
    • 2.4.8. Summary  (p. 114) | html | pdf |
    • Appendix 2.4.1. Computer programs for electron powder diffraction  (pp. 114-115) | html | pdf |
    • References | html | pdf |
  • 2.5. Two-dimensional powder diffraction  (pp. 118-149) | html | pdf | chapter contents |
    B. B. He
    • 2.5.1. Introduction  (pp. 118-119) | html | pdf |
    • 2.5.2. Fundamentals  (pp. 119-123) | html | pdf |
    • 2.5.3. Instrumentation  (pp. 123-132) | html | pdf |
    • 2.5.4. Applications  (pp. 132-147) | html | pdf |
    • References | html | pdf |
  • 2.6. Non-ambient-temperature powder diffraction  (pp. 150-155) | html | pdf | chapter contents |
    C. A. Reiss
    • 2.6.1. Introduction  (p. 150) | html | pdf |
    • 2.6.2. In situ powder diffraction  (p. 150) | html | pdf |
    • 2.6.3. Processes of interest  (p. 150) | html | pdf |
    • 2.6.4. General system setup of non-ambient chambers  (pp. 150-151) | html | pdf |
    • 2.6.5. Specimen properties  (p. 151) | html | pdf |
    • 2.6.6. High-temperature sample stages  (pp. 151-153) | html | pdf |
    • 2.6.7. Low-temperature sample stages  (pp. 153-154) | html | pdf |
    • 2.6.8. Temperature accuracy  (pp. 154-155) | html | pdf |
    • 2.6.9. Future  (p. 155) | html | pdf |
    • References | html | pdf |
  • 2.7. High-pressure devices  (pp. 156-173) | html | pdf | chapter contents |
    A. Katrusiak
    • 2.7.1. Introduction  (p. 156) | html | pdf |
    • 2.7.2. Historical perspective  (pp. 156-157) | html | pdf |
    • 2.7.3. Main types of high-pressure environments  (pp. 157-159) | html | pdf |
    • 2.7.4. The diamond-anvil cell (DAC)  (pp. 159-160) | html | pdf |
    • 2.7.5. Variable-temperature high-pressure devices  (pp. 160-161) | html | pdf |
    • 2.7.6. Soft and biomaterials under pressure  (p. 161) | html | pdf |
    • 2.7.7. Completeness of data  (pp. 161-162) | html | pdf |
    • 2.7.8. Single-crystal data collection  (pp. 162-163) | html | pdf |
    • 2.7.9. Powder diffraction with the DAC  (pp. 163-164) | html | pdf |
    • 2.7.10. Sample preparation  (p. 164) | html | pdf |
    • 2.7.11. Hydrostatic conditions  (pp. 164-165) | html | pdf |
    • 2.7.12. High-pressure chamber and gasket in the DAC  (pp. 165-166) | html | pdf |
    • 2.7.13. High-pressure neutron diffraction  (p. 166) | html | pdf |
    • 2.7.14. Pressure determination  (pp. 166-167) | html | pdf |
    • 2.7.15. High-pressure diffraction data corrections  (pp. 167-168) | html | pdf |
    • 2.7.16. Final remarks  (p. 168) | html | pdf |
    • References | html | pdf |
  • 2.8. Powder diffraction in external electric and magnetic fields  (pp. 174-188) | html | pdf | chapter contents |
    H. Ehrenberg, M. Hinterstein, A. Senyshyn and H. Fuess
    • 2.8.1. Introduction  (p. 174) | html | pdf |
    • 2.8.2. Experimental conditions  (pp. 174-177) | html | pdf |
    • 2.8.3. Examples  (pp. 177-186) | html | pdf |
    • 2.8.4. Summary  (p. 186) | html | pdf |
    • References | html | pdf |
  • 2.9. Cells for in situ powder-diffraction investigation of chemical reactions  (pp. 189-199) | html | pdf | chapter contents |
    W. van Beek and P. Pattison
    • 2.9.1. Introduction  (p. 189) | html | pdf |
    • 2.9.2. Historical perspective  (p. 189) | html | pdf |
    • 2.9.3. Main types of reaction cells  (pp. 189-197) | html | pdf |
    • 2.9.4. Complementary methods and future developments  (p. 197) | html | pdf |
    • References | html | pdf |
  • 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 |
    • 2.10.2. Neutron powder diffraction  (pp. 218-221) | html | pdf |
    • 2.10.3. Conclusions  (p. 221) | html | pdf |
    • References | html | pdf |

• Methodology
  • 3.1. The optics and alignment of the divergent-beam laboratory X-ray powder diffractometer and its calibration using NIST standard reference materials  (pp. 224-251) | html | pdf | chapter contents |
    J. P. Cline, M. H. Mendenhall, D. Black, D. Windover and A. Henins
    • 3.1.1. Introduction  (p. 224) | html | pdf |
    • 3.1.2. The instrument profile function  (pp. 224-230) | html | pdf |
    • 3.1.3. Instrument alignment  (pp. 230-235) | html | pdf |
    • 3.1.4. SRMs, instrumentation and data-collection procedures  (pp. 235-238) | html | pdf |
    • 3.1.5. Data-analysis methods  (pp. 238-241) | html | pdf |
    • 3.1.6. Instrument calibration  (pp. 241-250) | html | pdf |
    • 3.1.7. Conclusions  (p. 250) | html | pdf |
    • References | html | pdf |
  • 3.2. The physics of diffraction from powders  (pp. 252-262) | html | pdf | chapter contents |
    P. W. Stephens
    • 3.2.1. Introduction  (p. 252) | html | pdf |
    • 3.2.2. Idealized diffraction from powders  (pp. 252-257) | html | pdf |
    • 3.2.3. Complications due to non-ideal sample or instrument properties  (pp. 257-261) | html | pdf |
    • 3.2.4. The Debye scattering equation  (p. 261) | html | pdf |
    • 3.2.5. Summary  (p. 261) | html | pdf |
    • References | html | pdf |
  • 3.3. Powder diffraction peak profiles  (pp. 263-269) | html | pdf | chapter contents |
    R. B. Von Dreele
    • 3.3.1. Introduction  (p. 263) | html | pdf |
    • 3.3.2. Peak profiles for constant-wavelength radiation (X-rays and neutrons)  (pp. 263-265) | html | pdf |
    • 3.3.3. Peak profiles for neutron time-of-flight experiments  (pp. 265-266) | html | pdf |
    • 3.3.4. Peak profiles for X-ray energy-dispersive experiments  (pp. 266-267) | html | pdf |
    • 3.3.5. Sample broadening  (pp. 267-268) | html | pdf |
    • References | html | pdf |
  • 3.4. Indexing a powder diffraction pattern  (pp. 270-281) | html | pdf | chapter contents |
    A. Altomare, C. Cuocci, A. Moliterni and R. Rizzi
    • 3.4.1. Introduction  (p. 270) | html | pdf |
    • 3.4.2. The basic concepts of indexing  (pp. 270-272) | html | pdf |
    • 3.4.3. Indexing methods  (pp. 272-275) | html | pdf |
    • 3.4.4. Software packages for indexing and examples of their use  (pp. 275-280) | html | pdf |
    • 3.4.5. Conclusion  (p. 280) | html | pdf |
    • References | html | pdf |
  • 3.5. Data reduction to |F_hkl| values  (pp. 282-287) | html | pdf | chapter contents |
    A. Le Bail
    • 3.5.1. Introduction  (p. 282) | html | pdf |
    • 3.5.2. Algorithms  (pp. 282-284) | html | pdf |
    • 3.5.3. Pitfalls in the extraction of accurate |F_hkl| values using the Pawley and Le Bail methods  (pp. 284-285) | html | pdf |
    • 3.5.4. Applications and by-products  (pp. 285-286) | html | pdf |
    • 3.5.5. Conclusion  (p. 286) | html | pdf |
    • References | html | pdf |
  • 3.6. Whole powder pattern modelling: microstructure determination from powder diffraction data  (pp. 288-303) | html | pdf | chapter contents |
    M. Leoni
    • 3.6.1. Introduction  (pp. 288-289) | html | pdf |
    • 3.6.2. Fourier methods  (pp. 289-298) | html | pdf |
    • 3.6.3. Examples of WPPM analysis  (pp. 298-301) | html | pdf |
    • Appendix 3.6.1. Functions for profile shapes  (p. 301) | html | pdf |
    • References | html | pdf |
  • 3.7. Crystallographic databases and powder diffraction  (pp. 304-324) | html | pdf | chapter contents |
    J. A. Kaduk
    • 3.7.1. Introduction  (pp. 304-305) | html | pdf |
    • 3.7.2. Powder Diffraction File (PDF)  (pp. 305-313) | html | pdf |
    • 3.7.3. Cambridge Structural Database (CSD)  (pp. 313-314) | html | pdf |
    • 3.7.4. Inorganic Crystal Structure Database (ICSD)  (pp. 314-316) | html | pdf |
    • 3.7.5. Pearson's Crystal Data (PCD/LPF) (with Pierre Villars and Karen Cenzual)  (pp. 316-318) | html | pdf |
    • 3.7.6. Metals data file (CRYSTMET)  (p. 318) | html | pdf |
    • 3.7.7. Protein Data Bank (PDB)  (pp. 318-319) | html | pdf |
    • 3.7.8. Crystallography Open Database (COD) (with Saulius Gražulis)  (pp. 319-321) | html | pdf |
    • 3.7.9. Other internet databases  (p. 321) | html | pdf |
    • References | html | pdf |
  • 3.8. Clustering and visualization of powder-diffraction data  (pp. 325-343) | html | pdf | chapter contents |
    C. J. Gilmore, G. Barr and W. Dong
    • 3.8.1. Introduction  (p. 325) | html | pdf |
    • 3.8.2. Comparing 1D diffraction patterns  (pp. 325-327) | html | pdf |
    • 3.8.3. Cluster analysis  (pp. 327-329) | html | pdf |
    • 3.8.4. Data visualization  (pp. 329-331) | html | pdf |
    • 3.8.5. Further validating and visualizing clusters: silhouettes and fuzzy clustering  (pp. 331-333) | html | pdf |
    • 3.8.6. Examples  (pp. 333-337) | html | pdf |
    • 3.8.7. Quantitative analysis with high-throughput PXRD data without Rietveld refinement  (pp. 337-339) | html | pdf |
    • 3.8.8. Using spectroscopic data  (pp. 339-340) | html | pdf |
    • 3.8.9. Combining data types: the INDSCAL method  (pp. 340-342) | html | pdf |
    • 3.8.10. Quality control  (p. 342) | html | pdf |
    • 3.8.11. Computer software  (p. 342) | html | pdf |
    • References | html | pdf |
  • 3.9. Quantitative phase analysis  (pp. 344-373) | html | pdf | chapter contents |
    I. C. Madsen, N. V. Y. Scarlett, R. Kleeberg and K. Knorr
    • 3.9.1. Introduction  (p. 344) | html | pdf |
    • 3.9.2. Phase analysis  (pp. 344-345) | html | pdf |
    • 3.9.3. QPA methodology  (pp. 345-350) | html | pdf |
    • 3.9.4. Demonstration of methods  (pp. 350-353) | html | pdf |
    • 3.9.5. Alternative methods for determination of calibration constants  (pp. 353-356) | html | pdf |
    • 3.9.6. Quantification of phases with partial or no known crystal structures  (pp. 356-360) | html | pdf |
    • 3.9.7. QPA from in situ experimentation  (pp. 361-362) | html | pdf |
    • 3.9.8. QPA using neutron diffraction data  (p. 362) | html | pdf |
    • 3.9.9. QPA using energy-dispersive diffraction data  (pp. 362-364) | html | pdf |
    • 3.9.10. Improving accuracy  (pp. 364-370) | html | pdf |
    • 3.9.11. Summary  (p. 370) | html | pdf |
    • References | html | pdf |
  • 3.10. Accuracy in Rietveld quantitative phase analysis with strictly monochromatic Mo and Cu radiations  (pp. 374-384) | html | pdf | chapter contents |
    L. León-Reina, A. Cuesta, M. García-Maté, G. Álvarez-Pinazo, I. Santacruz, O. Vallcorba, A. G. De la Torre and M. A. G. Aranda
    • 3.10.1. Introduction  (pp. 374-375) | html | pdf |
    • 3.10.2. Compounds and series  (pp. 375-376) | html | pdf |
    • 3.10.3. Analytical techniques  (pp. 376-377) | html | pdf |
    • 3.10.4. Powder-diffraction data analysis  (p. 377) | html | pdf |
    • 3.10.5. Crystalline single phases  (pp. 377-379) | html | pdf |
    • 3.10.6. Limits of detection and quantification  (pp. 379-381) | html | pdf |
    • 3.10.7. Increasing inorganic crystalline phase content series  (p. 381) | html | pdf |
    • 3.10.8. Increasing crystalline organic phase content series  (pp. 381-382) | html | pdf |
    • 3.10.9. Increasing amorphous content series within an inorganic crystalline phase matrix  (pp. 382-383) | html | pdf |
    • 3.10.10. Conclusions  (pp. 383-384) | html | pdf |
    • References | html | pdf |

• Structure determination
  • 4.1. An overview of currently used structure determination methods for powder diffraction data  (pp. 386-394) | html | pdf | chapter contents |
    K. Shankland
    • 4.1.1. Introduction  (p. 386) | html | pdf |
    • 4.1.2. Methods used in SDPD  (pp. 386-387) | html | pdf |
    • 4.1.3. Conventional direct methods of structure determination  (pp. 387-388) | html | pdf |
    • 4.1.4. Modified direct methods of structure determination  (p. 388) | html | pdf |
    • 4.1.5. The direct-methods sum function  (p. 388) | html | pdf |
    • 4.1.6. The Patterson function  (p. 388) | html | pdf |
    • 4.1.7. Resonant (anomalous) scattering  (pp. 388-389) | html | pdf |
    • 4.1.8. Isomorphous replacement  (p. 389) | html | pdf |
    • 4.1.9. Maximum-entropy methods  (p. 389) | html | pdf |
    • 4.1.10. Charge flipping  (pp. 389-390) | html | pdf |
    • 4.1.11. Molecular envelopes  (p. 390) | html | pdf |
    • 4.1.12. Model building  (p. 390) | html | pdf |
    • 4.1.13. Molecular replacement  (p. 390) | html | pdf |
    • 4.1.14. Global optimization  (pp. 390-391) | html | pdf |
    • 4.1.15. Maximum-likelihood methods  (p. 391) | html | pdf |
    • 4.1.16. Local minimization  (p. 391) | html | pdf |
    • 4.1.17. Active use of prior information for particular structural classes  (pp. 391-392) | html | pdf |
    • 4.1.18. Combined figures of merit  (p. 392) | html | pdf |
    • References | html | pdf |
  • 4.2. Solving crystal structures using reciprocal-space methods  (pp. 395-413) | html | pdf | chapter contents |
    A. Altomare, C. Cuocci, A. Moliterni and R. Rizzi
    • 4.2.1. Introduction  (p. 395) | html | pdf |
    • 4.2.2. Intensity extraction for RS methods  (p. 395) | html | pdf |
    • 4.2.3. Direct methods  (pp. 395-399) | html | pdf |
    • 4.2.4. Improving data normalization  (pp. 399-400) | html | pdf |
    • 4.2.5. Patterson methods  (pp. 400-401) | html | pdf |
    • 4.2.6. Charge flipping  (pp. 401-403) | html | pdf |
    • 4.2.7. Maximum-entropy methods  (pp. 403-404) | html | pdf |
    • 4.2.8. Optimization of the structure model  (pp. 404-406) | html | pdf |
    • 4.2.9. Software packages for powder solution  (pp. 406-410) | html | pdf |
    • 4.2.10. Conclusions  (p. 410) | html | pdf |
    • References | html | pdf |
  • 4.3. Real-space methods for structure solution from powder-diffraction data: application to molecular structures  (pp. 414-432) | html | pdf | chapter contents |
    W. I. F. David
    • 4.3.1. Introduction  (pp. 414-416) | html | pdf |
    • 4.3.2. Real-space structure determination: a global-optimization extension of the Rietveld method  (p. 416) | html | pdf |
    • 4.3.3. Optimizing the process of real-space structure determination from powder-diffraction data  (pp. 416-418) | html | pdf |
    • 4.3.4. The nature and magnitude of the global-optimization challenge  (pp. 418-424) | html | pdf |
    • 4.3.5. Global-optimization algorithms  (pp. 424-430) | html | pdf |
    • 4.3.6. Using maximum-likelihood techniques to tackle incomplete structural models  (pp. 430-431) | html | pdf |
    • References | html | pdf |
  • 4.4. The use of supplementary information to solve crystal structures from powder diffraction  (pp. 433-441) | html | pdf | chapter contents |
    A. J. Florence
    • 4.4.1. General remarks  (p. 433) | html | pdf |
    • 4.4.2. Molecular models  (pp. 433-439) | html | pdf |
    • 4.4.3. Concluding remarks  (p. 439) | html | pdf |
    • References | html | pdf |
  • 4.5. Solving and refining inorganic structures  (pp. 442-451) | html | pdf | chapter contents |
    R. Černý and V. Favre-Nicolin
    • 4.5.1. The molecular/non-molecular and the organic/inorganic boundaries  (p. 442) | html | pdf |
    • 4.5.2. Modelling of non-molecular compounds  (p. 442) | html | pdf |
    • 4.5.3. Solving, refining and completing inorganic structures  (pp. 445-448) | html | pdf |
    • 4.5.4. Examples  (pp. 448-450) | html | pdf |
    • References | html | pdf |
  • 4.6. Zeolites  (pp. 452-464) | html | pdf | chapter contents |
    L. B. McCusker and Ch. Baerlocher
    • 4.6.1. Introduction  (p. 452) | html | pdf |
    • 4.6.2. Framework structure determination  (pp. 452-458) | html | pdf |
    • 4.6.3. Structure refinement  (pp. 458-462) | html | pdf |
    • 4.6.4. Conclusions  (pp. 462-463) | html | pdf |
    • References | html | pdf |
  • 4.7. Rietveld refinement  (pp. 465-472) | html | pdf | chapter contents |
    B. H. Toby
    • 4.7.1. History  (pp. 465-466) | html | pdf |
    • 4.7.2. Rietveld versus single-crystal refinements  (p. 466) | html | pdf |
    • 4.7.3. Multiphase and multiple data set fitting  (pp. 466-467) | html | pdf |
    • 4.7.4. The mechanism of Rietveld fitting  (p. 467) | html | pdf |
    • 4.7.5. Types of profile functions  (p. 467) | html | pdf |
    • 4.7.6. Observed structure-factor estimates  (pp. 467-468) | html | pdf |
    • 4.7.7. Estimating observed structure factors without a structure  (p. 468) | html | pdf |
    • 4.7.8. Agreement factors  (pp. 468-469) | html | pdf |
    • 4.7.9. Restraints and constraints in Rietveld refinement  (pp. 469-470) | html | pdf |
    • 4.7.10. The order in which to introduce parameters in a fit  (pp. 470-471) | html | pdf |
    • 4.7.11. Examples  (p. 471) | html | pdf |
    • 4.7.12. Conclusions  (p. 471) | html | pdf |
    • References | html | pdf |
  • 4.8. Application of the maximum-entropy method to powder-diffraction data  (pp. 473-488) | html | pdf | chapter contents |
    O. V. Magdysyuk, S. van Smaalen and R. E. Dinnebier
    • 4.8.1. Introduction  (pp. 473-474) | html | pdf |
    • 4.8.2. The principle of maximum entropy  (pp. 474-475) | html | pdf |
    • 4.8.3. Prior densities in MEM calculations  (pp. 475-476) | html | pdf |
    • 4.8.4. Crystallographic MEM equations  (p. 476) | html | pdf |
    • 4.8.5. MEM algorithms  (pp. 476-477) | html | pdf |
    • 4.8.6. Constraints in the MEM based on the measured intensities from powder-diffraction data  (pp. 477-480) | html | pdf |
    • 4.8.7. Analysis of the electron-density distribution from powder-diffraction data  (pp. 480-485) | html | pdf |
    • 4.8.8. Extensions of the MEM  (pp. 485-486) | html | pdf |
    • References | html | pdf |
  • 4.9. Structure validation  (pp. 489-514) | html | pdf | chapter contents |
    J. A. Kaduk
    • 4.9.1. Introduction  (p. 489) | html | pdf |
    • 4.9.2. Statistical measures (with contributions from B. H. Toby)  (pp. 489-490) | html | pdf |
    • 4.9.3. Graphical measures (with contributions from B. H. Toby and J. K. Stalick)  (pp. 490-496) | html | pdf |
    • 4.9.4. Chemical reasonableness  (pp. 496-508) | html | pdf |
    • 4.9.5. Working by analogy  (p. 508) | html | pdf |
    • 4.9.6. Structure validation in general  (pp. 508-509) | html | pdf |
    • 4.9.7. CheckCIF/PLATON  (pp. 509-512) | html | pdf |
    • References | html | pdf |
  • 4.10. Use of CIF for powder diffraction data  (pp. 515-521) | html | pdf | chapter contents |
    B. H. Toby
    • 4.10.1. Background  (p. 515) | html | pdf |
    • 4.10.2. A brief introduction to CIF  (pp. 515-516) | html | pdf |
    • 4.10.3. CIF usage for powder diffraction  (pp. 516-517) | html | pdf |
    • 4.10.4. Creation of pdCIF data files  (pp. 517-518) | html | pdf |
    • 4.10.5. Creating readers for pdCIF data files  (p. 518) | html | pdf |
    • 4.10.6. CIF software for powder diffraction  (pp. 518-521) | html | pdf |
    • 4.10.7. Conclusions  (p. 521) | html | pdf |
    • References | html | pdf |

• Defects, texture and microstructure
  • 5.1. Domain size and domain-size distributions  (pp. 524-537) | html | pdf | chapter contents |
    M. Leoni
    • 5.1.1. Introduction  (p. 524) | html | pdf |
    • 5.1.2. The Scherrer formula and integral-breadth methods  (p. 524) | html | pdf |
    • 5.1.3. Fourier methods  (p. 526) | html | pdf |
    • 5.1.4. The peak profile and the common volume function (`ghost')  (pp. 526-528) | html | pdf |
    • 5.1.5. Common volume function for simple shapes  (pp. 528-530) | html | pdf |
    • 5.1.6. Calculation of the intensity profile for simple shapes  (pp. 530-531) | html | pdf |
    • 5.1.7. Meaning of the size Fourier coefficients: mean size and column-length distribution  (p. 531) | html | pdf |
    • 5.1.8. Extension of the Fourier approach to a size distribution  (pp. 531-533) | html | pdf |
    • 5.1.9. Analytical distributions  (p. 533) | html | pdf |
    • 5.1.10. Histogram (arbitrary) distributions  (pp. 533-534) | html | pdf |
    • 5.1.11. Example  (pp. 534-536) | html | pdf |
    • References | html | pdf |
  • 5.2. Stress and strain  (pp. 538-554) | html | pdf | chapter contents |
    N. C. Popa
    • 5.2.1. The importance of determining stress and the diffraction method  (p. 538) | html | pdf |
    • 5.2.2. Strain and stress in single crystals, elastic constants and transformations  (p. 538) | html | pdf |
    • 5.2.3. Strain and stress in polycrystalline samples  (pp. 540-542) | html | pdf |
    • 5.2.4. Determining the strain/stress by diffraction  (pp. 542-543) | html | pdf |
    • 5.2.5. Macrostrain/stress in isotropic samples: classical approximations  (pp. 543-546) | html | pdf |
    • 5.2.6. The hydrostatic state in isotropic polycrystals  (pp. 546-547) | html | pdf |
    • 5.2.7. Calculating the macroscopic strain/stress using spherical harmonics  (pp. 547-552) | html | pdf |
    • 5.2.8. The spherical-harmonics approach to strain broadening  (pp. 552-553) | html | pdf |
    • References | html | pdf |
  • 5.3. Quantitative texture analysis and combined analysis  (pp. 555-580) | html | pdf | chapter contents |
    D. Chateigner, L. Lutterotti and M. Morales
    • 5.3.1. Introduction  (p. 555) | html | pdf |
    • 5.3.2. Crystallographic quantitative texture analysis (QTA)  (pp. 555-567) | html | pdf |
    • 5.3.3. Magnetic quantitative texture analysis (MQTA)  (pp. 567-569) | html | pdf |
    • 5.3.4. Modelling of preferred orientation in the Rietveld method  (pp. 569-571) | html | pdf |
    • 5.3.5. Combined analysis: structure, texture, microstructure, stress, phase, layering and reflectivity analyses in a single approach  (pp. 571-578) | html | pdf |
    • 5.3.6. Conclusions  (p. 578) | html | pdf |
    • References | html | pdf |
  • 5.4. Thin films and multilayers  (pp. 581-600) | html | pdf | chapter contents |
    M. Birkholz
    • 5.4.1. Introduction  (p. 581) | html | pdf |
    • 5.4.2. Effects of absorption  (p. 581) | html | pdf |
    • 5.4.3. Grazing-incidence configurations  (pp. 584-590) | html | pdf |
    • 5.4.4. Thin-film textures and their depth dependence  (pp. 590-593) | html | pdf |
    • 5.4.5. Stress and strain analysis  (pp. 593-594) | html | pdf |
    • 5.4.6. X-ray reflectivity (XRR)  (pp. 594-597) | html | pdf |
    • 5.4.7. Grazing-incidence X-ray scattering (GIXS)  (pp. 597-598) | html | pdf |
    • 5.4.8. Conclusions and perspective  (p. 598) | html | pdf |
    • References | html | pdf |
  • 5.5. Multigrain crystallography and three-dimensional grain mapping  (pp. 601-616) | html | pdf | chapter contents |
    H. F. Poulsen and G. B. M. Vaughan
    • 5.5.1. List of symbols  (p. 601) | html | pdf |
    • 5.5.2. Introduction  (pp. 601-602) | html | pdf |
    • 5.5.3. Experimental setup  (pp. 602-603) | html | pdf |
    • 5.5.4. Diffraction geometry  (pp. 603-605) | html | pdf |
    • 5.5.5. Indexing  (pp. 605-606) | html | pdf |
    • 5.5.6. Multigrain crystallography  (pp. 606-607) | html | pdf |
    • 5.5.7. Centre-of-mass and stress mapping  (pp. 607-608) | html | pdf |
    • 5.5.8. 3D grain and orientation mapping  (pp. 608-609) | html | pdf |
    • 5.5.9. Representation of crystallographic orientation  (pp. 609-613) | html | pdf |
    • 5.5.10. Representation of elastic strain  (p. 613) | html | pdf |
    • 5.5.11. Crystal symmetry in relation to multigrain samples  (pp. 613-614) | html | pdf |
    • 5.5.12. Discussion  (p. 614) | html | pdf |
    • References | html | pdf |
  • 5.6. X-ray diffraction from non-crystalline materials: the Debye model  (pp. 617-648) | html | pdf | chapter contents |
    S. Bates
    • 5.6.1. Outline  (p. 617) | html | pdf |
    • 5.6.2. Crystalline and non-crystalline: an introduction to the Debye model  (pp. 617-619) | html | pdf |
    • 5.6.3. Application of the Debye equation to a single molecule  (pp. 619-621) | html | pdf |
    • 5.6.4. The Debye–Menke equation  (pp. 621-622) | html | pdf |
    • 5.6.5. Verification of the Debye–Menke intensity function  (p. 622) | html | pdf |
    • 5.6.6. Background removal, intensity normalization and choice of X-ray optics  (pp. 622-625) | html | pdf |
    • 5.6.7. Application of the Debye normalization to semi-quantitative analysis  (pp. 625-627) | html | pdf |
    • 5.6.8. Correction for the instrumental intensity response  (pp. 627-631) | html | pdf |
    • 5.6.9. The full Debye normalization procedure  (pp. 631-632) | html | pdf |
    • 5.6.10. Application of the Debye normalization procedure  (pp. 632-635) | html | pdf |
    • 5.6.11. Universal appearance of non-crystalline powder patterns  (pp. 635-638) | html | pdf |
    • 5.6.12. Steps towards an effective lattice model of high-density randomly packed materials  (pp. 638-642) | html | pdf |
    • 5.6.13. Practical application of the effective lattice function determination  (pp. 642-645) | html | pdf |
    • 5.6.14. Debye diffraction models for larger molecular ensembles  (pp. 645-646) | html | pdf |
    • 5.6.15. Conclusions  (pp. 646-647) | html | pdf |
    • References | html | pdf |
  • 5.7. Nanometre-scale structure from powder diffraction: total scattering and atomic pair distribution function analysis  (pp. 649-672) | html | pdf | chapter contents |
    S. J. L. Billinge
    • 5.7.1. Introduction  (p. 649) | html | pdf |
    • 5.7.2. Scattering from nanostructures  (pp. 649-659) | html | pdf |
    • 5.7.3. Collecting data for total-scattering and PDF measurements  (pp. 659-663) | html | pdf |
    • 5.7.4. Data reduction  (pp. 663-664) | html | pdf |
    • 5.7.5. Extracting structural information  (pp. 664-669) | html | pdf |
    • References | html | pdf |
  • 5.8. Scattering methods for disordered heterogeneous materials  (pp. 673-696) | html | pdf | chapter contents |
    A. J. Allen
    • 5.8.1. Introduction and overview  (pp. 673-675) | html | pdf |
    • 5.8.2. Recommended measurement tools  (pp. 675-683) | html | pdf |
    • 5.8.3. Quantitative analysis of disordered heterogeneous materials  (pp. 683-692) | html | pdf |
    • 5.8.4. Prospects for future development and recommended further reading  (pp. 692-693) | html | pdf |
    • References | html | pdf |

• Software
  • 6.1. Survey of computer programs for powder diffraction  (pp. 698-715) | html | pdf | chapter contents |
    C. J. Gilmore, J. A. Kaduk and H. Schenk
    • References | html | pdf |

• Applications
  • 7.1. Macromolecular powder diffraction  (pp. 718-736) | html | pdf | chapter contents |
    I. Margiolaki
    • 7.1.1. Introduction  (p. 718) | html | pdf |
    • 7.1.2. Sample preparation and handling  (pp. 718-720) | html | pdf |
    • 7.1.3. Data collection  (pp. 720-721) | html | pdf |
    • 7.1.4. Cryo-cooling protein powder samples and microstructural effects  (pp. 721-723) | html | pdf |
    • 7.1.5. Crystal screening  (pp. 723-725) | html | pdf |
    • 7.1.6. Improvements in data quality via the use of multiple profiles  (pp. 725-726) | html | pdf |
    • 7.1.7. Structure solution  (pp. 726-729) | html | pdf |
    • 7.1.8. Structure refinement  (pp. 729-731) | html | pdf |
    • 7.1.9. Related developments  (pp. 731-732) | html | pdf |
    • 7.1.10. Concluding remarks  (p. 732) | html | pdf |
    • References | html | pdf |
  • 7.2. Forensic applications of X-ray powder diffraction  (pp. 737-751) | html | pdf | chapter contents |
    D. F. Rendle
    • 7.2.1. Introduction  (pp. 737-742) | html | pdf |
    • 7.2.2. Instrumentation  (p. 742) | html | pdf |
    • 7.2.3. Technical procedures  (pp. 742-745) | html | pdf |
    • 7.2.4. Examples of forensic casework involving the use of XRPD  (pp. 745-747) | html | pdf |
    • 7.2.5. Summary  (pp. 747-748) | html | pdf |
    • References | html | pdf |
  • 7.3. Materials for energy storage and conversion  (pp. 752-758) | html | pdf | chapter contents |
    M. A. Rodriguez
    • 7.3.1. Introduction  (p. 752) | html | pdf |
    • 7.3.2. Fossil fuel  (p. 752) | html | pdf |
    • 7.3.3. Hydrogen storage  (p. 752) | html | pdf |
    • 7.3.4. Wind  (p. 753) | html | pdf |
    • 7.3.5. Solar  (pp. 753-755) | html | pdf |
    • 7.3.6. Battery technology  (pp. 755-757) | html | pdf |
    • References | html | pdf |
  • 7.4. Powder diffraction in art and archaeology  (pp. 759-766) | html | pdf | chapter contents |
    G. Artioli
    • 7.4.1. Introduction  (p. 759) | html | pdf |
    • 7.4.2. The information provided by diffraction  (p. 759) | html | pdf |
    • 7.4.3. Phase identification and quantification  (pp. 760-761) | html | pdf |
    • 7.4.4. Crystal structure analysis  (pp. 761-762) | html | pdf |
    • 7.4.5. Texture analysis  (p. 762) | html | pdf |
    • 7.4.6. Microstructural analysis  (pp. 762-763) | html | pdf |
    • 7.4.7. Present trends  (pp. 763-764) | html | pdf |
    • References | html | pdf |
  • 7.5. Powder diffraction and pharmaceuticals  (pp. 767-781) | html | pdf | chapter contents |
    J. Bernstein and S. M. Reutzel-Edens
    • 7.5.1. Introduction  (p. 767) | html | pdf |
    • 7.5.2. Some basic background and references  (p. 767) | html | pdf |
    • 7.5.3. Identification and characterization  (p. 767) | html | pdf |
    • 7.5.4. Quantitation of mixtures by traditional and Rietveld methods  (pp. 769-771) | html | pdf |
    • 7.5.5. Characterization of amorphous materials  (pp. 771-773) | html | pdf |
    • 7.5.6. Quality control and regulatory aspects  (p. 773) | html | pdf |
    • 7.5.7. Creating and protecting intellectual property  (pp. 773-777) | html | pdf |
    • 7.5.8. Counterfeit medicines  (pp. 777-778) | html | pdf |
    • 7.5.9. Concluding remarks  (p. 778) | html | pdf |
    • References | html | pdf |
  • 7.6. Selected applications of Rietveld analysis in the aluminium industry  (pp. 782-792) | html | pdf | chapter contents |
    F. R. Feret
    • 7.6.1. Introduction  (p. 782) | html | pdf |
    • 7.6.2. Bauxite  (pp. 782-784) | html | pdf |
    • 7.6.3. Quantification of quartz in bauxite  (pp. 784-785) | html | pdf |
    • 7.6.4. Occurrence and characterization of Zn and Mn in bauxite  (p. 785) | html | pdf |
    • 7.6.5. Red mud (bauxite residue)  (pp. 785-787) | html | pdf |
    • 7.6.6. Alumina  (pp. 787-788) | html | pdf |
    • 7.6.7. Scrubber alumina  (p. 788) | html | pdf |
    • 7.6.8. Electrolytic bath  (pp. 788-790) | html | pdf |
    • 7.6.9. Spent potlining (SPL)  (p. 790) | html | pdf |
    • 7.6.10. Dross  (pp. 790-791) | html | pdf |
    • 7.6.11. Discussion  (p. 791) | html | pdf |
    • References | html | pdf |
  • 7.7. Mining and mineral processing  (pp. 793-803) | html | pdf | chapter contents |
    N. V. Y. Scarlett and D. L. Bish
    • 7.7.1. Introduction  (p. 793) | html | pdf |
    • 7.7.2. Use of powder diffraction in mining and mineral processing  (pp. 793-794) | html | pdf |
    • 7.7.3. Powder-diffraction methodology  (pp. 794-798) | html | pdf |
    • 7.7.4. Examples  (pp. 798-801) | html | pdf |
    • 7.7.5. Conclusions  (p. 801) | html | pdf |
    • References | html | pdf |
  • 7.8. Ceramic materials  (pp. 804-827) | html | pdf | chapter contents |
    W. Wong-Ng
    • 7.8.1. Introduction  (pp. 804-805) | html | pdf |
    • 7.8.2. Categories of ceramics  (pp. 805-810) | html | pdf |
    • 7.8.3. Applications of powder X-ray diffraction to the studies of ceramics  (pp. 810-825) | html | pdf |
    • 7.8.4. Summary  (p. 825) | html | pdf |
    • References | html | pdf |
  • 7.9. Applications in glass-ceramics  (pp. 828-833) | html | pdf | chapter contents |
    S. T. Misture
    • 7.9.1. Introduction  (pp. 828-829) | html | pdf |
    • 7.9.2. Methods  (p. 829) | html | pdf |
    • 7.9.3. Qualitative analysis of devitrification  (pp. 829-830) | html | pdf |
    • 7.9.4. Kinetics analysis  (pp. 830-833) | html | pdf |
    • 7.9.5. Remnant glass compositions via quantitative analysis  (p. 833) | html | pdf |
    • 7.9.6. Summary  (p. 833) | html | pdf |
    • References | html | pdf |
  • 7.10. Industrial organic pigments  (pp. 834-842) | html | pdf | chapter contents |
    M. U. Schmidt
    • 7.10.1. On organic pigments  (pp. 834-835) | html | pdf |
    • 7.10.2. Main applications of X-ray powder diffraction to organic pigments (and other organic compounds)  (pp. 835-841) | html | pdf |
    • References | html | pdf |
  • 7.11. Powder diffraction in the petroleum and petrochemical industries  (pp. 843-854) | html | pdf | chapter contents |
    J. A. Kaduk
    • 7.11.1. Introduction  (p. 843) | html | pdf |
    • 7.11.2. Exploration and production  (pp. 843-844) | html | pdf |
    • 7.11.3. Refining and petrochemicals  (pp. 844-852) | html | pdf |
    • 7.11.4. In situ studies  (pp. 852-853) | html | pdf |
    • References | html | pdf |
  • 7.12. Powder-diffraction characterization of cements  (pp. 855-867) | html | pdf | chapter contents |
    M. A. G. Aranda, A. G. De la Torre and L. León-Reina
    • 7.12.1. An introduction to cements and types of cements  (p. 855) | html | pdf |
    • 7.12.2. Rietveld quantitative phase analysis of cements  (pp. 855-856) | html | pdf |
    • 7.12.3. Phase quantification of Portland cements  (pp. 856-859) | html | pdf |
    • 7.12.4. Quantification of other cementitious materials  (pp. 859-861) | html | pdf |
    • 7.12.5. Powder-diffraction studies on the hydration of cements  (pp. 861-863) | html | pdf |
    • 7.12.6. The use of synchrotron and neutron powder diffraction for studying cements  (pp. 863-864) | html | pdf |
    • 7.12.7. Conclusions and outlook  (p. 864) | html | pdf |
    • References | html | pdf |
  • 7.13. Powder diffraction of superconductors  (pp. 868-884) | html | pdf | chapter contents |
    Qingzhen Huang
    • 7.13.1. Introduction  (pp. 868-870) | html | pdf |
    • 7.13.2. Advantages of structure analysis from powder diffraction  (pp. 870-872) | html | pdf |
    • 7.13.3. Analysis of the chemical and structural features of nonstoichiometric superconductors  (pp. 872-878) | html | pdf |
    • 7.13.4. Magnetic order in superconductors and parent compounds  (pp. 878-879) | html | pdf |
    • 7.13.5. Conclusions  (p. 879) | html | pdf |
    • Appendix 7.13.1. The study of long-range magnetic order in superconductors  (pp. 879-882) | html | pdf |
    • References | html | pdf |
  • 7.14. Powder diffraction by minerals  (pp. 885-892) | html | pdf | chapter contents |
    R. Arletti, G. Cruciani and G. Ferraris
    • 7.14.1. Powder diffraction and characterization of new mineral species  (pp. 885-886) | html | pdf |
    • 7.14.2. Mineral physics through in situ powder-diffraction experiments  (pp. 886-889) | html | pdf |
    • 7.14.3. Minerals related to human health, the biosphere and planetary exploration  (pp. 889-890) | html | pdf |
    • References | html | pdf |