powder diffraction


Summary: Method of using a polycrystalline powder and Rietveld refinement (LEAST SQUARES ANALYSIS) of X-RAY DIFFRACTION or NEUTRON DIFFRACTION. It circumvents the difficulties of producing single large crystals.

Top Publications

  1. Shameli K, Ahmad M, Yunus W, Rustaiyan A, Ibrahim N, Zargar M, et al. Green synthesis of silver/montmorillonite/chitosan bionanocomposites using the UV irradiation method and evaluation of antibacterial activity. Int J Nanomedicine. 2010;5:875-87 pubmed publisher
    ..These results show that Ag/MMT/Cts BNCs can be useful in different biologic research and biomedical applications, such as surgical devices and drug delivery vehicles...
  2. Futterer S, Andrusenko I, Kolb U, Hofmeister W, Langguth P. Structural characterization of iron oxide/hydroxide nanoparticles in nine different parenteral drugs for the treatment of iron deficiency anaemia by electron diffraction (ED) and X-ray powder diffraction (XRPD). J Pharm Biomed Anal. 2013;86:151-60 pubmed publisher
    ..X-ray powder diffraction (XRPD) and electron diffraction (ED) methods were used in order to investigate the nine different parenteral ..
  3. He W, Lu Y, Qi J, Chen L, Hu F, Wu W. Nanoemulsion-templated shell-crosslinked nanocapsules as drug delivery systems. Int J Pharm. 2013;445:69-78 pubmed publisher
    ..Furthermore, the presence of surface food proteins introduces carboxyl and amine moieties, which enables the nanocapsules to anchor ligands, suggesting its potential application in targeting drug delivery, bioimaging and therapeutics. ..
  4. Hussein Al Ali S, Al Qubaisi M, Hussein M, Ismail M, Zainal Z, Hakim M. Controlled release and angiotensin-converting enzyme inhibition properties of an antihypertensive drug based on a perindopril erbumine-layered double hydroxide nanocomposite. Int J Nanomedicine. 2012;7:2129-41 pubmed publisher
    ..Intercalated perindopril showed better thermal stability than its free counterpart. The resulting material showed sustained-release properties and can therefore be used as a controlled-release formulation. ..
  5. Leventouri T, Bunaciu C, Perdikatsis V. Neutron powder diffraction studies of silicon-substituted hydroxyapatite. Biomaterials. 2003;24:4205-11 pubmed
    ..4wt% silicon-substituted HAp prepared by an aqueous precipitation method. High-resolution neutron powder diffraction and Rietveld refinement methods were used to investigate the effect of silicon substitution on the crystal ..
  6. Shameli K, Ahmad M, Zargar M, Yunus W, Ibrahim N. Fabrication of silver nanoparticles doped in the zeolite framework and antibacterial activity. Int J Nanomedicine. 2011;6:331-41 pubmed publisher
    ..All of the synthesized Ag/zeolite NCs were found to have antibacterial activity. These results show that Ag NPs in the zeolite framework can be useful in different biological research and biomedical applications...
  7. Shameli K, Ahmad M, Yunus W, Ibrahim N, Darroudi M. Synthesis and characterization of silver/talc nanocomposites using the wet chemical reduction method. Int J Nanomedicine. 2010;5:743-51 pubmed publisher
    ..These Ag/talc-NCs may have potential applications in the chemical and biological industries. ..
  8. Desigaux L, Belkacem M, Richard P, Cellier J, Leone P, Cario L, et al. Self-assembly and characterization of layered double hydroxide/DNA hybrids. Nano Lett. 2006;6:199-204 pubmed
    ..96 nm. Our results indicate that labile complexes resulting from the association of nucleic acids and inorganic materials can be obtained not only by anion exchange but also by a direct self-assembly route...
  9. Zhang Y, Xue C, Xue Y, Gao R, Zhang X. Determination of the degree of deacetylation of chitin and chitosan by X-ray powder diffraction. Carbohydr Res. 2005;340:1914-7 pubmed
    ..the degree of deacetylation (DD) of alpha-chitin and chitosan in the range of 17-94% DD using X-ray powder diffraction (XRD) is proposed...

More Information


  1. Basso S, Fitch A, Fox G, Margiolaki I, Wright J. High-throughput phase-diagram mapping via powder diffraction: a case study of HEWL versus pH. Acta Crystallogr D Biol Crystallogr. 2005;61:1612-25 pubmed
    ..The Rietveld analysis gave an average structural model with excellent goodness of fit and stereochemistry. ..
  2. Margiolaki I, Wright J, Wilmanns M, Fitch A, Pinotsis N. Second SH3 domain of ponsin solved from powder diffraction. J Am Chem Soc. 2007;129:11865-71 pubmed
    ..seems to be no fundamental reason, except the sheer size and complexity of the structures involved, why powder diffraction should not be employed to solve structures of small proteins...
  3. Margiolaki I, Wright J. Powder crystallography on macromolecules. Acta Crystallogr A. 2008;64:169-80 pubmed
    ..A wide range of small proteins have been found to give synchrotron powder diffraction profiles where the peak widths are essentially limited only by the instrumental resolution...
  4. Park J, Choy Y, Oh J, Kim J, Hwang S, Choy J. Controlled release of donepezil intercalated in smectite clays. Int J Pharm. 2008;359:198-204 pubmed publisher
    ..Therefore, to formulate a complete drug delivery system, the hybrids were coated with Eudragit E-100 using a spray dryer, which also showed great enhancement in the release rate during a short period of time (180min)...
  5. Zhang X, Wu D, Lai J, Lu Y, Yin Z, Wu W. Piroxicam/2-hydroxypropyl-beta-cyclodextrin inclusion complex prepared by a new fluid-bed coating technique. J Pharm Sci. 2009;98:665-75 pubmed publisher
    ..Solid-state (13)C NMR spectrometry indicated possible inclusion of PIX through the pyridine ring. It is concluded that fluid-bed coating has potential to be used as a new technique to prepare cyclodextrin inclusion complex. ..
  6. Choy J, Shin J, Lim S, Oh J, Oh M, Oh S. Characterization and stability analysis of zinc oxide nanoencapsulated conjugated linoleic acid. J Food Sci. 2010;75:N63-8 pubmed publisher
    ..Nanoencapsulation improved the thermal stability of CLA by about 25%, compared to pristine CLA. Practical Application: This system can be used for protection of encapsulated negatively-charged food ingredients from thermal processing...
  7. Thangadurai S, Shukla S, Srivastava A, Anjaneyulu Y. X-ray powder diffraction patterns for certain fluoroquinolone antibiotic drugs. Acta Pharm. 2003;53:295-303 pubmed
    X-ray powder diffraction (XRD) data for six pure fluoroquinolone antibiotic drugs, ciprofloxacin, norfloxacin, enrofloxacin, ofloxacin, pefloxacin and sparfloxacin have been obtained using a powder diffractometer...
  8. Lei Y, Lu Y, Qi J, Nie S, Hu F, Pan W, et al. Solid self-nanoemulsifying cyclosporin A pellets prepared by fluid-bed coating: preparation, characterization and in vitro redispersibility. Int J Nanomedicine. 2011;6:795-805 pubmed publisher
    ..It is concluded that fluid-bed coating is a new technique with considerable potential for preparation of pellet-based solid SNEDDS formulations. ..
  9. Margiolaki I, Wright J, Fitch A, Fox G, Von Dreele R. Synchrotron X-ray powder diffraction study of hexagonal turkey egg-white lysozyme. Acta Crystallogr D Biol Crystallogr. 2005;61:423-32 pubmed
    The structure of turkey egg-white lysozyme (TEWL) has been refined from high-resolution X-ray powder diffraction data. The sample was rapidly obtained as a polycrystalline precipitate at high protein concentration using 0...
  10. Huq A, Stephens P. Subtleties in crystal structure solution from powder diffraction data using simulated annealing: ranitidine hydrochloride. J Pharm Sci. 2003;92:244-9 pubmed
    ..We redetermine the structure from powder data using simulated annealing and show that the conformational disorder is clearly revealed by this method. ..
  11. Hussein M, Al Ali S, Zainal Z, Hakim M. Development of antiproliferative nanohybrid compound with controlled release property using ellagic acid as the active agent. Int J Nanomedicine. 2011;6:1373-83 pubmed publisher
    ..In vitro bioassay study showed that the EAN has a mild effect on the hepatocytes cells, similar to its counterpart, free EA. ..
  12. Chen X, Griesser U, Te R, Pfeiffer R, Morris K, Stowell J, et al. Analysis of the acid-base reaction between solid indomethacin and sodium bicarbonate using infrared spectroscopy, X-ray powder diffraction, and solid-state nuclear magnetic resonance spectroscopy. J Pharm Biomed Anal. 2005;38:670-7 pubmed
    ..The reaction was monitored by IR spectroscopy, X-ray powder diffraction, and solid-state NMR. At 40 degrees C and 80% RH, the reaction is nearly complete after 300 h...
  13. Ma M, Zhu Y, Chang J. Monetite formed in mixed solvents of water and ethylene glycol and its transformation to hydroxyapatite. J Phys Chem B. 2006;110:14226-30 pubmed
    ..The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform ..
  14. Presciutti F, Capitani D, Sgamellotti A, Brunetti B, Costantino F, Viel S, et al. Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays. J Phys Chem B. 2005;109:22147-58 pubmed
    ..paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR...
  15. Ayenew Z, Paudel A, Rombaut P, Van den Mooter G. Effect of compression on non-isothermal crystallization behaviour of amorphous indomethacin. Pharm Res. 2012;29:2489-98 pubmed publisher
    ..Compression affects the physical stability of amorphous indomethacin. Structural changes originated from tablet compression should be duly investigated for the stable amorphous formulation development. ..
  16. Giri T, Kumar K, Alexander A, Ajazuddin -, Badwaik H, Tripathy M, et al. Novel controlled release solid dispersion for the delivery of diclofenac sodium. Curr Drug Deliv. 2013;10:435-43 pubmed
    ..Moreover, combined carriers of EE 100-ES 100 exhibited more dissolution retarding effect than any of the carriers. The release of drug followed anomalous transport in artificial intestinal juice (pH 6.8). ..
  17. Kanagathara N, Marchewka M, Drozd M, Renganathan N, Gunasekaran S, Anbalagan G. FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate. Spectrochim Acta A Mol Biomol Spectrosc. 2013;112:343-50 pubmed publisher
    ..The chemical structure of the compound has been established by (1)H and (13)C NMR spectra. No detectable signal was observed during powder test for second harmonic generation. ..
  18. Cuervo C, Gonzalez J, Rives V, Vicente M. Characterization of a sulfadiazine-induced lithiasis calculus by physicochemical techniques. AAPS PharmSciTech. 2013;14:128-32 pubmed publisher
    ..Analytical techniques widely used in laboratories of Materials Chemistry have proven to be useful tools for characterizing the chemical nature of unusual urolithiasis. ..
  19. Tomić Z, Ašanin D, Đurović R, Đorđević A, Makreski P. Near-infrared spectroscopy study for determination of adsorbed acetochlor in the organic and inorganic bentonites. Spectrochim Acta A Mol Biomol Spectrosc. 2012;98:47-52 pubmed publisher
    ..to acetochlor adsorbed to organo-montmorillonite and Na-montmorillonite, which is confirmed by X-ray powder diffraction (XRPD). Greater quantity of acetochlor is adsorbed to organo-clays compared to non-modified montmorillonite...
  20. Aldawsari H, Altaf A, Banjar Z, Iohara D, Nakabayashi M, Anraku M, et al. Crystallization of a new polymorph of acetohexamide from 2-hydroxybutyl-?-cyclodextrin solution: form VI with a high aqueous solubility. Int J Pharm. 2013;453:315-21 pubmed publisher
    ..Crystalline Form VI was highly soluble in water and dissolved more rapidly than the other known polymorphs. This property was reflected in the blood concentrations of the drug after oral administration to rats. ..
  21. Zha S, Zhou Y, Jin X, Chen Z. The removal of amoxicillin from wastewater using organobentonite. J Environ Manage. 2013;129:569-76 pubmed publisher
    ..DK1 was characterized by scanning electronic microscopy (SEM), Specific Surface Area (SSA), X-ray powder diffraction (XRD) and Fourier Transform Infrared (FTIR) spectrometer...
  22. Sivaramakrishna D, Swamy M. Synthesis, characterization and thermotropic phase behavior of a homologous series of N-acyl-L-alaninols and interaction of N-myristoyl L-alaninol with dimyristoylphosphatidylcholine. Chem Phys Lipids. 2016;196:5-12 pubmed publisher
    ..Transmission electron microscopic studies show that the NMAOH:DMPC (45:55, mol/mol) mixture forms unilamellar vesicles of about 120-150 nm in diameter. ..
  23. Kramer S, Celestian A. Effects of hydration during strontium exchange into nanoporous hydrogen niobium titanium silicate. Inorg Chem. 2012;51:6251-8 pubmed publisher
    ..11 fractional occupancy level was passed. Exchange of Sr(2+) into the nanoporous material reached maximum fractional site occupancy of approximately 0.20 using a 10.0 mM SrCl(2) solution...
  24. Takata E, Tsutsumi K, Tsutsumi Y, Tabata K. Production of monosaccharides from napier grass by hydrothermal process with phosphoric acid. Bioresour Technol. 2013;143:53-8 pubmed publisher
    ..phosphoric acid at 200 °C for 8 min. Consequently, 77.2% yield of xylose and 50.0% yield of glucose were obtained from the combined process. ..
  25. Sunitha D, Nagabhushana H, Singh F, Sharma S, Dhananjaya N, Nagabhushana B, et al. Ion beam induced amorphization and bond breaking in Zn2SiO4:Eu3+ nanocrystalline phosphor. Spectrochim Acta A Mol Biomol Spectrosc. 2012;90:18-21 pubmed publisher
    ..These results show degradation of SiO (2?(3)) bonds present on the surface of the sample and/or due to lattice disorder produced by dense electronic excitation under heavy ion irradiation. These results are discussed in detail. ..
  26. Miyasaka K, Hano H, Kubota Y, Lin Y, Ryoo R, Takata M, et al. A stand-alone mesoporous crystal structure model from in situ X-ray diffraction: nitrogen adsorption on 3D cagelike mesoporous silica SBA-16. Chemistry. 2012;18:10300-11 pubmed publisher
    ..The present method is readily extendable to any ordered mesopores wrapped by the wall matrix containing a certain intrawall porosity. ..
  27. Li D, Wang M, Yang C, Wang J, Ren G. Solid state characterizations and analysis of stability in azelnidipine polymorphs. Chem Pharm Bull (Tokyo). 2012;60:995-1002 pubmed
    ..The kinetics of the solid-state decomposition, studied using DSC analysis, showed that the activation energies of decomposition of the polymorphs ? and ? at high temperatures were 148.67 and 151.93 kJ·mol(-1). ..
  28. Chen R, Christiansen M, Anikeeva P. Maximizing hysteretic losses in magnetic ferrite nanoparticles via model-driven synthesis and materials optimization. ACS Nano. 2013;7:8990-9000 pubmed publisher
  29. Ruz V, Froeyen M, Busson R, González M, Baudemprez L, Van den Mooter G. Characterization and molecular modeling of the inclusion complexes of 2-(2-nitrovinyl) furan (G-0) with cyclodextrines. Int J Pharm. 2012;439:275-85 pubmed publisher
    ..The latter results were in agreement with the experimental data. Inclusion complexes of G-0 with HP-?-CD contributed to improve the chemical stability of the drug in the presence of other commonly used pharmaceutical excipients. ..
  30. Youngren S, Mulik R, Jun B, Hoffmann P, Morris K, Chougule M. Freeze-dried targeted mannosylated selenium-loaded nanoliposomes: development and evaluation. AAPS PharmSciTech. 2013;14:1012-24 pubmed
  31. Margiolaki I, Giannopoulou A, Wright J, Knight L, Norrman M, Schluckebier G, et al. High-resolution powder X-ray data reveal the T(6) hexameric form of bovine insulin. Acta Crystallogr D Biol Crystallogr. 2013;69:978-90 pubmed publisher
    ..A novel approach for refining protein structures using powder diffraction data is presented. In this approach, each amino acid is represented by a flexible rigid body (FRB)...
  32. Muehlenfeld C, Kann B, Windbergs M, Thommes M. Solid dispersion prepared by continuous cogrinding in an air jet mill. J Pharm Sci. 2013;102:4132-9 pubmed publisher
    ..Differential scanning calorimetry and X-ray powder diffraction were used to verify the crystalline structure of the coground formulation...
  33. Alhalaweh A, Kaialy W, Buckton G, Gill H, Nokhodchi A, Velaga S. Theophylline cocrystals prepared by spray drying: physicochemical properties and aerosolization performance. AAPS PharmSciTech. 2013;14:265-76 pubmed publisher
    ..Spray drying could be a potential technique for preparing cocrystals with modified physical properties. ..
  34. Ober C, Gupta R. Formation of itraconazole-succinic acid cocrystals by gas antisolvent cocrystallization. AAPS PharmSciTech. 2012;13:1396-406 pubmed publisher
  35. Hu C, Barabanschikov A, Ellison M, Zhao J, Alp E, Sturhahn W, et al. Nuclear resonance vibrational spectra of five-coordinate imidazole-ligated iron(II) porphyrinates. Inorg Chem. 2012;51:1359-70 pubmed publisher
    ..Our study suggests that the Fe motions are coupled with the porphyrin core and peripheral groups motions. Both peripheral groups and their conformations have significant influence on the vibrational spectra (position and shape). ..
  36. Chen Q, Xue W, Lin J, Lin R, Zeng M, Chen X. Highly-connected, porous coordination polymers based on [M4(?3-OH)2] (M = Co(II) and Ni(II)) clusters: different networks, adsorption and magnetic properties. Dalton Trans. 2012;41:4199-206 pubmed publisher
    ..0 and 15.0 K for 1 and 2, respectively. The intra- and inter-tetramer coupling interactions and cooperative magnetic correlation greatly influence the bulk magnetic behaviours in this system. ..
  37. Raula J, Seppälä J, Malm J, Karppinen M, Kauppinen E. Structure and dissolution of L-leucine-coated salbutamol sulphate aerosol particles. AAPS PharmSciTech. 2012;13:707-12 pubmed publisher
    ..The structure of the coated drug particles was studied by means of thermal analysis techniques (DSC and TG), and the dissolution of salbutamol sulphate was studied as an on-line measurement in a diffusion cell. ..
  38. Lee J, Boerrigter S, Jung Y, Byun Y, Yuk S, Byrn S, et al. Organic vapor sorption method of isostructural solvates and polymorph of tenofovir disoproxil fumarate. Eur J Pharm Sci. 2013;50:253-62 pubmed publisher
    ..This study demonstrates an alternative crystallization method to obtain isostructural solvates. ..
  39. Shah B, Mistry C, Shah A. Seizure modeling of Pb(II) and Cd(II) from aqueous solution by chemically modified sugarcane bagasse fly ash: isotherms, kinetics, and column study. Environ Sci Pollut Res Int. 2013;20:2193-209 pubmed publisher
    ..Synthesized zeolitic material (CZBFA and ECZBFA), a low-cost sorbent, was proven as potential sorbent for the uptake of Pb(II) and Cd(II) heavy metal ions. ..
  40. Marinoni N, D Alessio D, Diella V, Pavese A, Francescon F. Effects of soda-lime-silica waste glass on mullite formation kinetics and micro-structures development in vitreous ceramics. J Environ Manage. 2013;124:100-7 pubmed publisher
    ..Measurements have been performed by in situ high temperature X-ray powder diffraction, scanning electron microscopy, thermal dilatometry, water absorption and mechanical testing...
  41. Song X, Boily J. Structural controls on OH site availability and reactivity at iron oxyhydroxide particle surfaces. Phys Chem Chem Phys. 2012;14:2579-86 pubmed publisher
    ..Our findings provide new possibilities for molecular-scale resolution of important gas-phase processes on the surfaces of these important minerals. ..
  42. Goud N, Gangavaram S, Suresh K, Pal S, Manjunatha S, Nambiar S, et al. Novel furosemide cocrystals and selection of high solubility drug forms. J Pharm Sci. 2012;101:664-80 pubmed publisher
    ..The dissolution rates of furosemide cocrystals were about two times faster than the pure drug. Three novel furosemide compounds of higher solubility and good phase stability were identified in a solid form screen. ..
  43. Distefano G, Suzuki H, Tsujimoto M, Isoda S, Bracco S, Comotti A, et al. Highly ordered alignment of a vinyl polymer by host-guest cross-polymerization. Nat Chem. 2013;5:335-41 pubmed publisher
    ..Indeed, the resulting material exhibits long-range order and is stable to thermal and solvent treatments, as demonstrated by X-ray powder diffraction and transmission electron microscopy.
  44. Langham Z, Booth J, Hughes L, Reynolds G, Wren S. Mechanistic insights into the dissolution of spray-dried amorphous solid dispersions. J Pharm Sci. 2012;101:2798-810 pubmed publisher
    ..This was found to accurately describe the bell-shaped dissolution profiles observed for the compacts containing a low felodipine loading. ..
  45. Cavallari C, Santos B, Fini A. Olanzapine solvates. J Pharm Sci. 2013;102:4046-56 pubmed publisher
  46. Rahman Z, Zidan A, Berendt R, Khan M. Tannate complexes of antihistaminic drug: sustained release and taste masking approaches. Int J Pharm. 2012;422:91-100 pubmed publisher
    ..NMR (SSNMR), thermally by differential scanning calorimetry (DSC), for crystallinity by powder X-ray powder diffraction (PXRD), for organoleptic evaluation by electronic tongue (e-tongue), and for solubility in 0...
  47. Chen T, Shao M, Xu H, Wen C, Lee S. Control over the crystal phase, crystallinity, morphology of AgVO3 via protein inducing process. J Colloid Interface Sci. 2012;366:80-7 pubmed publisher
  48. Frost J, Walsh A. What Is Moving in Hybrid Halide Perovskite Solar Cells?. Acc Chem Res. 2016;49:528-35 pubmed publisher
    ..Herein, we critically discuss the atomistic origin of the dynamic processes and the associated chemical disorder intrinsic to crystalline hybrid perovskite semiconductors. ..
  49. Ali M, Fule R, Sav A, Amin P. Porous starch: a novel carrier for solubility enhancement of carbamazepine. AAPS PharmSciTech. 2013;14:919-26 pubmed publisher
    ..PS-CBZ was found to follow a Fickian behavior during dissolution. In vivo studies conducted in mice displayed a superior performance of CBZ-PS as compared to neat CBZ. ..
  50. van de Streek J. Reinterpretation of the monohydrate of clarithromycin from X-ray powder diffraction data as a trihydrate. Acta Crystallogr C. 2012;68:o369-72 pubmed publisher
    ..E68, o667-o668] recently reported the crystal structure of clarithromycin monohydrate from synchrotron X-ray powder diffraction data. Voids in the crystal structure suggested the possible presence of two more water molecules...
  51. Du J, Lu J, Wu Q, Jing C. Reduction and immobilization of chromate in chromite ore processing residue with nanoscale zero-valent iron. J Hazard Mater. 2012;215-216:152-8 pubmed publisher
    ..Multiple complementary analysis methods including leaching tests, X-ray powder diffraction, X-ray absorption near edge structure (XANES) spectroscopy, and X-ray photoelectron spectroscopy (XPS) were ..
  52. Lin X, Gao W, Li C, Chen J, Yang C, Wu H. Nano-sized flake carboxymethyl cassava starch as excipient for solid dispersions. Int J Pharm. 2012;423:435-9 pubmed publisher
    ..And the dissolution rate of SD2 was considerably higher than that of pure drug. These results indicated that the nanoscale CMCS was a kind of good carrier for solid dispersion to improve the solubility of poorly water-soluble drugs. ..
  53. Tamura N, Gilbert P. X-ray microdiffraction of biominerals. Methods Enzymol. 2013;532:501-31 pubmed publisher
    ..We present some of the most relevant discoveries made in the field of biomineralization using these approaches. ..