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A practical guide to pharmaceutical analyses using X-ray powder diffraction

Published online by Cambridge University Press:  15 April 2019

T. G. Fawcett*
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
S. Gates-Rector
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
A. M. Gindhart
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
M. Rost
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
S. N. Kabekkodu
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
J. R. Blanton
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
T. N. Blanton
Affiliation:
International Centre for Diffraction Data, Newtown Square, Pennsylvania 19073
*
a)Author to whom correspondence should be addressed. Electronic mail: dxcfawcett@outlook.com

Abstract

Advances in instrumentation, software applications, and database content have all contributed to improvements in pharmaceutical analyses by powder diffraction methods in the 21st century. When compared to the globally harmonized United States Pharmacopeia General Chapter <941>, “Characterization of Crystalline and Partially Crystalline Solids by X-ray Powder Diffraction”, many historic problems in pharmaceutical analysis have been addressed by combinations of improved methods and instrumentation. Major changes in the last 20 years include (i) a dramatic lowering in detection capability and detection limits, (ii) enhanced capabilities for dynamic measurements such as in situ analyses under a variety of conditions, and (iii) the ability to identify and characterize nanomaterials, non-crystalline, and amorphous materials by both coherent and incoherent scattering profiles.

Type
Review Article
Copyright
Copyright © International Centre for Diffraction Data 2019 

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References

Arakcheeva, A., Pattison, P., Bauer-Brandl, A., Birkedal, H., and Chapuis, G. (2013). “Cimetidine, C10H16N6S, form C: crystal structure and modeling of polytypes using the superspace approach,” J. Appl. Crystallogr. 46, 99107.Google Scholar
Bates, S. (2013). “An Investigation of Non-Crystalline Materials Using X-ray Powder Diffraction,” presented at PPXRD-12 Beijing, China. Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/12/P15-Simon-Bates-ppxrd-12.pdf.Google Scholar
Beckers, D. (2015). “Quantification of traces -pushing the limits with laboratory instrumentation,” presented at PPXRD-13 - 18–21 May 2015, Bad Herrenalb, Germany Full presentation available for free download at http://www.icdd.com/ppxrd/13/presentations/PPXRD-13-Beckers-Quantification.pdf.Google Scholar
Beckers, D. and Bethke, K. (2011). “In situ Measurement and Characterization of Crystal Growth by X-ray Diffraction,” presented at PPXRD-10 - 16–19 May 2011 Lyon, France, Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/10/PPXRD-10_Detlef-Beckers.pdf.Google Scholar
Beckers, D., Gteshki, M., and Adibhatla, A. (2017). “Atomic Pair Distribution Function (PDF) and X-ray Scattering Methods to Assess Amorphous Organic Compounds,” presented at PPXRD-15, 18–20 August, 2017, Hyderabad, India. Full presentation available for free download at: http://www.icdd.com/assets/ppxrd/presentations/15/P22-Beckers.pdf.Google Scholar
Berzins, A., Actins, A., and Skarbulis, E. (2010). “Stability and desolvation kinetics of Droperidol hydrates and an ethanol solvate, studied by powder X-ray diffractometry and differential thermal analysis/thermogravimetry,” presented at PPXRD-10 - 16–19 May 2011 Lyon, France, Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/10/PPXRD-10_Agris_Berzins.pdf.Google Scholar
Billinge, S. J. L. (2011). “Total Scattering Pair Distribution Functions (TSPDF) for Fingerprinting Amorphous Pharmaceuticals,” presented at PPXRD-10, 16–19 May 2011, Lyon, France. Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/10/PPXRD-10_Simon_Billinge.pdf.Google Scholar
Blanton, T. (2013). Eastman Kodak Co., Rochester, NY, USA. Private Communication Three PDF references containing full digital experimental patterns of various commercial gelatins.Google Scholar
Blanton, T. (2016). International Centre for Diffraction Data, Newt.own Square, PA, USA. ICDD Data Collect. Two PDF references containing full digital experimental patterns of commercial polyethylene glycols.Google Scholar
Brittain, H. G. (2000a). “X-ray diffraction I: on the diffraction of X-rays by crystalline solids,” Spectroscopy 15, 4449.Google Scholar
Brittain, H. G. (2000b). “X-ray diffraction II: using single-crystal X-ray diffraction to study polymorphism and solvatomorphism,” Spectroscopy 15, 3439.Google Scholar
Brittain, H. G. (2001). “X-ray diffraction III, pharmaceutical applications,” Spectroscopy 16, 3439.Google Scholar
Chandrappa, R. K., Ochsenbein, P., Martineau, C., Bonin, M., Althoff, G., Engelke, F., Malandrini, H., Castro, B., El Hajii, M., and Taulette, F. (2013). “Polymorphism in xaliproden: an X-ray diffraction and solid-state NMR investigation,” Cryst. Growth Des. 13, 46784687.Google Scholar
Clearfield, A. B., Reibenspies, J. H., and Bhuvanesh, N. S. P. (Eds.) (2008). Principles and Applications of Powder Diffraction (Wiley & Sons, Oxford, United Kingdom).Google Scholar
Chernyshev, V. V., Yatsenko, A. V., Fitch, A. N., Sonneveld, E. J., Makarov, V. A., and Shenk, H. (2000). “Molecular crystal structures from powder diffraction data: applications to pharmaceutical analysis and to the chemistry of dyes,” Adv. X-ray Anal. 43, 299.Google Scholar
Das, P. P. (2015). “Crystal Structure Determination of Pharmaceuticals with Electron Diffraction,” presented at PPXRD-13, 18–21 May 2015, Bad Herranalb, Germany.Google Scholar
Das, P. P. (2017). “TEM 3D precession electron diffraction to solve pharmaceutical API structures,” presented at PPXRD-15, 18–20 August 2017, Hyderabad, India http://www.icdd.com/assets/ppxrd/presentations/14/Das_PPXRD14_FLORIDA.pdf.Google Scholar
Debye, P. (1915). “Zerstreuung von Röntgenstrahlen,” Ann. Phys. 351, 809823.Google Scholar
Drathen, C., Kern, A., and Evans, M. (2017). “Fast PDF Screening of Amorphous Pharmacueticals,” presented at PPXRD-15, 18–20 August, 2017, Hyderabad, India http://www.icdd.com/assets/ppxrd/presentations/15/P14-Evans.pdf.Google Scholar
Egami, T. and Billinge, S. J. L. (2012). Under the Bragg Peaks, Structural Analysis of Complex Materials (Pergamon Materials Series, Elsevier Publishers, London, UK), 2nd ed.Google Scholar
Elton, N. J. and Salt, P. D. (1996). “Particle statistics in quantitative X-ray diffractometry,” Powder Diffr. 11, 218229.Google Scholar
Faber, J. and Blanton, J. (2008). “Full pattern comparisons of experimental and calculated powder patterns using the integral index method in PDF-4 +,” Adv. X-ray Anal. 51, 183189. (These same two authors developed a normalization of the integral index (normalized R-index) that was published in PDF database products starting with Release 2011).Google Scholar
Faber, J., Crowder, C. E., Blanton, J., Kabekkodu, S. N., Blanton, T. N., Fawcett, T. G., and Gourdon, O. (2014). “New neutron diffraction data capability in the ICDD PDF-4 + 2014 relational database,” Adv. X-ray Anal. 57, 7789.Google Scholar
Faber, J., Kabekkodu, S., Blanton, J., Blanton, T., and Fawcett, T. (2017). “New neutron time-of-flight (TOF) capability in PDF-4 + relational databases: digitized diffraction patterns and I/Ic for quantitative phase analysis,” Powder Diffr. 32, 107111.Google Scholar
Fawcett, T. G. (2018). private communications. Fawcett has chaired or co-chaired the new instrumentation session of the Denver X-Ray Conference from 2009–2018, advances in detectors and sources are common annual topics, specifications are frequently presented but not always published. Over 150 abstracts on sources and detectors from 2003–2017 are available at http://www.dxcicdd.com/search_dxc/search_dxc.asp.Google Scholar
Fawcett, T. G., Martin, E. J., Crowder, C. E., Kincaid, P. J., Strandjord, A. J., and Blazy, J. A. (1986). “Analysis of multi-phase pharmaceuticals using simultaneous differential Scanning calorimetry and X-ray diffraction,” Adv. X-ray Anal 29, 323332.Google Scholar
Fawcett, T. G., Goralski, C. T., and Ziettlow, D. W. (1988). “Preparation of polymorphically pure terfenadine,” USP 4, 742–175.Google Scholar
Fawcett, T. G., Kabekkodu, S. N., Faber, J., and Needham, F. (2004). “Evaluating experimental methods and techniques in X-ray diffraction using 280 000 data sets in the Powder Diffraction File,” Powder Diffr. 19, 2025.Google Scholar
Fawcett, T. G., Faber, J., Needham, F., Kabekkodu, S. N., Hubbard, C. R., and Kaduk, J. A. (2006). “Developments in formulation analyses by powder diffraction analysis,” Powder Diffr. 21, 105110.Google Scholar
Fawcett, T. G., Needham, F., Faber, J. N., and Crowder, C. E. (2010). “International centre for diffraction data round robin on quantitative rietveld phase analysis of pharmaceuticals,” Powder Diffr. 25, 18.Google Scholar
Fawcett, T. G., Crowder, C. E., Kabekkodu, S. N., and Kaduk, J. A. (2011). “Improved material identification methods through targeted data mining,” Adv. X-ray Anal. 54, 149161.Google Scholar
Fawcett, T. G., Crowder, C. E., Kabekkodu, S. N., Needham, F., Kaduk, J. A., Blanton, T. N., Petkov, V., Bucher, E., and Shpanchenko, R. (2013). “Reference materials for the study of polymorphism and crystallinity in cellulosics,” Powder Diffr. 28, 1831.Google Scholar
Fawcett, T. G., Kabekkodu, S. N., Zhong, K., Gindhart, A. M., Blanton, J. R., and Blanton, T. N. (2015). “Analyzing amorphous and nanocrystalline materials by full pattern analysis,” presented at PPXRD-13, 18–21 May 2015, Bad Herranalb, Germany. Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/13/PPXRD-13-Fawcett.pdf.Google Scholar
Fawcett, T. G., Kabekkodu, S. N., Gates-Rector, S., Gindhart, A. M., Blanton, J. R., and Blanton, T. N. (2016). “The analysis of noncrystalline materials in pharmaceutical formulations,” presented at PPXRD-14, 6–9 June 2016, Ft. Myers, FL. Full presentation available for free download at http://www.icdd.com/assets/ppxrd/presentations/14/NON-CRYSTALLINE%20MATERIALSLong.pdf.Google Scholar
Fawcett, T. G., Kabekkodu, S. N., Blanton, J. R., and Blanton, T. N. (2017). “Chemical analysis by diffraction: the powder diffraction file™,” Powder Diffr. 32, 6371.Google Scholar
Fawcett, T. G., Gates-Rector, S., Gindhart, A., Rost, M., Kabekkodu, S. N. M., Blanton, J. R., and Blanton, T. N. (2019). “Formulation Analyses of High Volume Prescription Drugs,” Powder Diffr. (in press).Google Scholar
Gates, S. D., Blanton, T. N., and Fawcett, T. G. (2014). “A new “chain” of events: polymers in the Powder Diffraction File™ (PDF ®)”, Powder Diffr. 29, 102107.Google Scholar
Gozzo, F. (2013). “Advances in Synchrotron XRPD for the Enhanced Characterization of Pharmaceuticals,” presented at PPXRD-12, 20–24 May, 2013 Beijing, China. Full presentation available for free download at http://www.icdd.com/ppxrd/12/presentations/P13-Fabia-Gozzo-ppxrd-12.pdf.Google Scholar
Hashimoto, T., Hanajiri, R., Yasuda, N., Nakamura, Y., Mizuno, N., Honda, S., Hayakawa, S., Nishiwaki, Y., and Kimua, S. (2017). “Single crystal structure analysis of designer drugs circulating in the Japanese drug market by the synchrotron radiation X-Ray diffraction,” Adv. X-Ray Anal., 60. and Powder Diffr. 32, 112117.Google Scholar
He, B. (2013). “New Instrumentation For Pharmaceutical XRD/SAXS,” presented at PPXRD-12, 20–24 May, 2013 Beijing, China. Full presentation available for free download at http://www.icdd.com/ppxrd/12/presentations/P31-Bob-He-ppxrd-12.pdf.Google Scholar
Hiramatsu, T., Kitamura, M., Matsumoto, K., and Watanabe, K. (1998). EP1020454A1, “Polymorphic modifications of 2-(3-cyano-4-isobutyloxyphenyl)-4-methyl-5-thiazole-carboxylic acid and processes for the preparation thereof,” assigned to Teijin Pharma Ltd.Google Scholar
International Centre for Diffraction Data (2014a). “Technical Bulletin, PDF-4/Organics,” published by the ICDD. Nano material examples for apatite and Lipitor given in the case histories. Available for free download at http://www.icdd.com//wp-content/uploads/2018/03/PDF-4_Organics_Technical_Bulletin.pdf.Google Scholar
International Centre for Diffraction Data (2014b). “Technical Bulletin, Search and Identify with SIeve/SIeve + ,” published by the ICDD. Available for free download at http://www.icdd.com//wp-content/uploads/2018/03/SIeve-Technical-Bulletin.pdf.Google Scholar
International Centre for Diffraction Data (2016) “Technical Bulletin, How to Measure Thermal Expansion and Thermal Expansion Coefficients Using the Powder Diffraction File™,” published by the ICDD. Nano material examples for apatite and Lipitor given in the case histories. Available for free download at http://www.icdd.com//wp-content/uploads/2018/03/Nanomaterials_Technical_Bulletin.pdf.Google Scholar
International Centre for Diffraction Data (2017). PDF-4/Organics 2018 (Database), edited by Dr. Soorya Kabekkodu published by the ICDD, Newtown Square, PA, USA.Google Scholar
International Centre for Diffraction Data (2018). PDF-4/Organics 2019 (Database), edited by Dr. Soorya Kabekkodu, published by the ICDD, Newtown Square, PA, USA.Google Scholar
International Pharmaceutical Excipients Councils – Americas (2018). “FAQs About Excipients” most commonly used excipients in U.S.-manufactured drug products, https://ipecamericas.org/what-ipec-americas/faqs#question4.Google Scholar
Jenkins, R. and Snyder, R. L. (1996). Introduction to X-ray Powder Diffractometry (John Wiley & Sons, New York).Google Scholar
Kabekkodu, S. N. and Fawcett, T. (2013). The Powder Diffraction File: Recent Developments in Quality Control, presented at Accuracy in Powder Diffraction, APD-IV, April 22nd, NIST, Gaithersburg, MD.Google Scholar
Kaduk, J. A. (2005). “The crystal structure of cellulose Iβ,” BP Chemical, Naperville, IL, USA. Private Communication. This is the source for PDF 00-056-1718.Google Scholar
Kaduk, J. A. (2019). Chapter 3.7, “Crystallographic databases and powder diffraction,” in International Tables for Crystallography, Volume H, Powder Diffraction, edited by C. Gilmore, J. A. Kaduk, and H. Schenk (John Wiley & Sons, New York), Wiley IUCr series, pp. 304324.Google Scholar
Kaduk, J. A. and Reid, J. (2011). “Typical values of rietveld instrument profile coefficients,” Powder Diffr. 26, 8893.Google Scholar
Kaduk, J. A., Crowder, C. E., Zhong, K., Fawcett, T. G., and Suchomel, M. R. (2014). “Crystal structure of dusteride (Avodart), C27H20F6N2O2,” Powder Diffr. 29, 264279.Google Scholar
Kern, A., Madsen, I. C., and Scarlett, N. V. Y. (2012). “Quantifying Amorphous Phases” in Uniting Electron Crystallography and Powder Diffraction, edited by Kolb, U., Shankland, K., Meshi, L., Avilov, A. and David, W. (Springer, Dordrecht), NATO Science for Peace and Security Series B: Physics and Biophysics, pp. 219–231.Google Scholar
Kern, A., Beckers, D., Gozzo, F., and Dinnebier, R. (2015). “PPXRD-13 Workshop - Quantitative phase analysis by XRPD,” presented at PPXRD-13 18-21 May 2015, Bad Herrenalb, Germany. All authors presentations available at http://www.icdd.com/index.php/ppxrd/ppxrd-13-presentations/.Google Scholar
Kern, A., Gozzo, F., and Reinle-Schmitt, M. (2016). “PPXRD-14 Workshop - Quantitative phase analysis by XRPD,” presented at PPXRD-14 −6–9 June 2016, Fort Myers, Florida, U.S.A. All authors presentations available at http://www.icdd.com/index.php/ppxrd/ppxrd-14-presentations/.Google Scholar
Kishi, A., and Toraya, H. (2004). “Simultaneous measurements of X-ray diffraction (XRD) and differential scanning calorimetry (DSC) data under controlled humidity conditions: instrumentation and application to studies of hydration, dehydration and re-hydration processes of pharmaceutical compounds,” Adv. X-ray Anal. 47, 240.Google Scholar
Kitamura, S., Miyamae, A., Koda, S., and Morimoto, Y. (1989). “Effect of grinding on the solid-state stability of cefixime trihydrate,” Int. J. Pharm. 56, 125134.Google Scholar
Klug, H. P. and Alexander, L. E. (1974). X-ray Diffraction Procedures (Wiley InterScience, John Wiley & Sons Ltd., New York), 2nd ed.Google Scholar
Kolb, U., Shankland, K., Meshi, L., Avilov, A., and David, W. (2012). Chapter 3, “organic compounds” in Uniting Electron Crystallography and Powder Diffraction edited by Shankland, K. (Springer, Dordrecht, Germany), pp. 4552.Google Scholar
Madsen, I. C., Scarlett, N. V. Y., and Kern, A. (2011). “Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction,” Z. Krist. 226, 944–955.Google Scholar
Madsen, I. C., Scarlett, N. V. Y., Cranswick, L. M. D., and Lwin, T. (2001). “Outcomes of the International Union of Crystallography Commission on powder diffraction round robin on quantitative phase analysis, samples 1a to 1 h,” J. Appl. Crystallogr. 34, 409426.Google Scholar
Madsen, I., Scarlett, N., Kleeberg, R., and Knorr, K. (2019). Chapter 3.9, “Quantitative Phase Analysis,” in International Tables for Crystallography, Volume H, Powder Diffraction, edited by Gilmore, C., Kaduk, J. A., and Schenk, H. (John Wiley & Sons, New York), Wiley IUCr series, pp. 344372.Google Scholar
Madsen, I. C., Scarlett, N. V. Y., Riley, D. P., and Raven, M. D. (2012). “Quantitative phase analysis using the Rietveld method,” in Modern Diffraction Methods, edited by Mittemeijer, E. J. and Welzel, U. (Wiley-VCH, Weinheim, Germany), pp. 219231.Google Scholar
Masciocchi, N. and Artioli, G. (1996). “Lattice parameters determination from powder diffraction data: results from a round robin project,” Powder Diffr. 11, 253258.Google Scholar
Petkov, V., Ren, Y., Kabekkodu, S., and Murphy, D. (2013). “Atomic pair distribution functions analysis of disordered low-Z materials,” P. Chem. Chem. Physi. 22, 85448554.Google Scholar
Qiu, J-B., Li, G., Sheng, Y., and Zhu, M-R. (2015). “Quantification of febuxostat polymorphs using X-ray diffraction technique,” J. Pharm. Biomed. Anal. 107, 298303.Google Scholar
Reid, J., Crane, D., Blanton, J., Crowder, C., Kabekkodu, S., and Fawcett, T. (2011). “Tools for Electron Diffraction Pattern Simulation for the Powder Diffraction File,” Microscopy Today, 19, 3237.Google Scholar
Rietveld, H. M. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Crystallogr. 2, 6571.Google Scholar
Scardi, P., Leoni, M., Lamas, D. G., and Cabanillas, E. D. (2005). “Grain size distribution of nanocrystalline systems,” Powder Diffr. 20, 353358.Google Scholar
Scardi, P., Leoni, M., and Faber, J. (2006). “Diffraction line profile from a disperse system: a simple alternative to Voightian profiles,” Powder Diffr. 21, 270.Google Scholar
Schreiner, W. N. and Fawcett, T. (1984). “Results of a round robin study of systematic errors found in routine X-ray diffraction Raw data,” Adv. X-ray Anal. 28, 309314.Google Scholar
Shankland, K., Broder, C., Ibberson, R., and David, W. (2006). “Neutron Powder Diffraction without resort to deuteration: use in molecular structure refinement,” presented at PPXRD-05 14–16 February 2006 Somerset, New Jersey, USA.Google Scholar
Smith, D. K. (1963). “A FORTRAN Program for Calculating X-ray Powder Diffraction Patterns,” Lawrence Radiation Laboratory, Livermore, CA, UCRL-7 193.Google Scholar
Smith, D. K. (2001). “Particle statistics and whole-pattern methods in quantitative X-ray powder diffraction analysis,” Powder Diffr. 16, 186191.Google Scholar
Smith, D. K., Johnson, G. G., Scheible, A., Wims, A. M., Johnson, J. L., and Ullmann, G. (1987). “Quantitative X-ray powder diffraction method using the full diffraction pattern,” Powder Diffr. 2, 7377.Google Scholar
Sun, M., Hu, X., Zhou, X., and Gu, J. (2017). “Determination of minor quantities of linezolid polymorphs in drug substance and tablet formulation by powder X-ray diffraction,” Powder Diffr. 32, 78.Google Scholar
Takahashi, Y., Nakashima, K., Nakagawa, H., and Sugimoto, I. (1984). “Effects of grinding and drying on the solid-state stability of ampicillin trihydrate,” Chem. Pharm. Bull. 32, 49634970.Google Scholar
Teng, J., Bates, S., Engers, D., Leach, K., Schields, P., and Yang, Y. (2010). “Effect of water vapor sorption on local structure of poly(vinylpyrrolidone),” J. Pharm. Sci. 99, 38153825.Google Scholar
Thakral, N. K., Zanon, R. I., Kelly, R. C., and Thakral, S. (2018). “Applications of powder X-ray diffraction in small molecule pharmacueticals: achievements and aspirations,” J. Pharm. Sci. 107, 29692982.Google Scholar
Ungar, T., Leoni, M., and Scardi, P. (1999). “The dislocation model of strain anisotropy in whole powder-pattern fitting: the case of an Li-Mn cubic spinel,” J. Appl. Crystallogr. 32, 290295.Google Scholar
United States Pharmacopea (USP) (1995) “X-ray Diffraction,” General Chapter 941, USP 23/NF 18 (The United States Pharmacopoeial Convention, Rockville, MD), pp. 18431844.Google Scholar
United States Pharmacopea (USP) (2000) “X-ray Diffraction,” General Chapter 941, USP 24/ NF 19 (United States Pharmacopoeial Convention, Rockville, MD), pp. 20052007.Google Scholar
Van Gendersen, E., Clabbers, M. T. B., Das, P. P., Stewart, A., Nederlof, I., Barentsen, K. C., Portillo, Q., Pannu, N. S., Nicopoulos, S., Gruene, T., and Abrahams, J. P. (2016). “Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area electron detector,” Acta Crystallogr. A72, 236242.Google Scholar
Veron, M., Rauch, E. F., Nicolopoulos, S., Ling, W. L., and Otero, J. M. (2011) “Novel Electron Diffraction Technique for Texture Analysis (Orientation & Phase Mapping) of Organic Nanocrystals”, presented at PPXRD-10, 16–19 May 2011, Lyon France Full presentation available http://www.icdd.com/assets/ppxrd/presentations/10/PPXRD-10_Stavros_Nikolopoulos.pdf.Google Scholar
Whitfield, P. S., Huq, A., and Kaduk, J. A. (2019). Chapter 2.10, “Specimen preparation,” in International Tables for Crystallography, Volume H, Powder Diffraction, edited by Gilmore, C., Kaduk, J. A., and Schenk, H. (John Wiley & Sons, New York), Wiley IUCr series, pp. 200222.Google Scholar
Wong-Ng, W. and Hubbard, C. R. (1987). “Standard reference materials for X-ray diffraction part II. Calibration using d-spacing standards,” Powder Diffr. 2, 242248.Google Scholar
Wu, D., Li, S., Xu, K., Zhang, L., Wu, X., and Li, H. (2014) “X-Ray powder diffraction data for loratadine (C22H23ClN202),” Powder Diffr. 29, 193195.Google Scholar
Zvirgzdina, A., Mishnev, A., and Actins, A. (2014). “Structure determination of three polymorphs of xylazine from laboratory diffraction data,” Acta Crystallogr. B70, 342346.Google Scholar