In Situ Diffraction Studies: Thermal Decomposition of a Natural Plumbojarosite and the Development of Rietveld-Based Data Analysis Techniques

2010 ◽  
Vol 651 ◽  
pp. 37-64 ◽  
Author(s):  
Ian C. Madsen ◽  
Ian E. Grey ◽  
Stuart J. Mills
Keyword(s):  
Thermal Decomposition ◽  
Amorphous Material ◽  
Data Sets ◽  
X Ray Diffraction ◽  
Data Set ◽  
X Ray ◽  
Analysis Techniques ◽  
Path Lengths ◽  
Instrument Configuration

A study of the thermal decomposition sequence of a sample of natural arsenian plumbojarosite has been undertaken using in situ X-ray diffraction. The sample was heated to 900°C using an Anton-Paar heating stage fitted to an INEL CPS120 diffractometer. The data were analysed using a whole-pattern, Rietveld based approach for the extraction of quantitative phase abundances. The instrument configuration used required the development and application of algorithms to correct for aberrations in the (i) peak intensities due to differing path lengths of incident and diffracted beams in the sample and (ii) peak positions due to sample displacement. Details of the structural models used were refined at selected steps in the pattern and then fixed for subsequent analysis. The data sequence consists of some 110 individual data sets which were analysed sequentially with the output of each run forming the input for analysis of the next data set. The results of the analysis show a complex breakdown and recrystallisation sequence including the formation of a major amount of amorphous material after initial breakdown of the plumbojarosite.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

Accelerated Thermal Decomposition of Graphene Oxide Films in Air via in Situ X-ray Diffraction Analysis

2016 ◽  
Vol 120 (27) ◽  
pp. 14984-14990 ◽  
Author(s):  
Qin Pan ◽  
Ching-Chang Chung ◽  
Nanfei He ◽  
Jacob L. Jones ◽  
Wei Gao
Keyword(s):  
Thermal Decomposition ◽  
Graphene Oxide ◽  
Diffraction Analysis ◽  
Oxide Films ◽  
X Ray Diffraction ◽  
X Ray

Probing the thermal decomposition process of layered double hydroxides through in situ 57Fe Mössbauer and in situ X-ray diffraction experiments

2006 ◽  
Vol 42 (2) ◽  
pp. 534-538 ◽  
Author(s):  
Daniel X. Gouveia ◽  
Odair P. Ferreira ◽  
Antonio G. Souza Filho ◽  
M. G. da Silva ◽  
J. A. C. de Paiva ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Layered Double Hydroxides ◽  
Decomposition Process ◽  
X Ray Diffraction ◽  
Thermal Decomposition Process ◽  
X Ray ◽  
57Fe Mössbauer ◽  
Double Hydroxides

Synthesis and characterization of the barium oxalates BaC2O4·0.5H2O, α-BaC2O4 and β-BaC2O4

2002 ◽  
Vol 58 (5) ◽  
pp. 808-814 ◽  
Author(s):  
Axel Nørlund Christensen ◽  
Rita Grønbæk Hazell ◽  
Ian Charles Madsen
Keyword(s):  
Thermal Decomposition ◽  
Ammonium Oxalate ◽  
Barium Chloride ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Weak Hydrogen Bonds ◽  
Made In

The synthesis of BaC2O4·0.5H2O and its thermal decomposition to α-BaC2O4 and β-BaC2O4 was investigated. BaC2O4·0.5H2O is precipitated at room temperature from aqueous solutions of barium chloride and ammonium oxalate. The deuterated compound BaC2O4·0.5D2O was made in analogy with D2O as the solvent. The compounds were characterized by X-ray and neutron diffraction analysis. Single-crystal X-ray diffraction of BaC2O4·0.5H2O measured at 120 K gave the triclinic cell a = 8.692 (1), b = 9.216 (1), c = 6.146 (1) Å, α = 95.094 (3), β = 95.492 (3), γ = 64.500 (3)°, space group P\bar 1, Z = 4. Two independent Ba atoms are each coordinated to nine O atoms at distances from 2.73 (1) to 2.99 (1) Å. One of the two oxalate ions deviates significantly from planarity. The water molecule does form weak hydrogen bonds. In situ X-ray powder diffraction was used to study the thermal decomposition of BaC2O4·0.5H2O and the formation of α-BaC2O4. The X-ray powder pattern of α-BaC2O4 measured at 473 K was indexed on a triclinic cell with a = 5.137 (3), b = 8.764 (6), c = 9.006 (4) Å, α = 83.57 (4), β = 98.68 (5), γ = 99.53 (5)°, and the space group P\bar 1 with Z = 4.

scholarly journals In situ X-ray diffraction investigation of thermal decomposition of wood cellulose

2007 ◽  
Vol 80 (1) ◽  
pp. 134-140 ◽  
Author(s):  
Gerald A. Zickler ◽  
Wolfgang Wagermaier ◽  
Sérgio S. Funari ◽  
Manfred Burghammer ◽  
Oskar Paris
Keyword(s):  
Thermal Decomposition ◽  
X Ray Diffraction ◽  
Wood Cellulose ◽  
X Ray

scholarly journals Progress in Microanalysis

2013 ◽  
Vol 21 (3) ◽  
pp. 7-7
Author(s):  
Charles Lyman
Keyword(s):  
Light Microscopy ◽  
Spatial Resolution ◽  
Equilibrium Phase ◽  
X Ray Diffraction ◽  
Bulk Analysis ◽  
X Ray ◽  
Analysis Techniques ◽  
Composition And Structure

Many researchers view microanalysis as the determination of composition and structure of individual phases at a spatial resolution of 1 μm or better. It is remarkable to me that much of what we know about the phases shown in equilibrium phase diagrams was determined using bulk analysis techniques like powder X-ray diffraction in combination with light microscopy of flat-polished sections of materials. The identities and amounts of phases were deduced from systematic experiments because there was no way to analyze micrometer-sized phases in situ.

scholarly journals MeshAndCollect: an automated multi-crystal data-collection workflow for synchrotron macromolecular crystallography beamlines

2015 ◽  
Vol 71 (11) ◽  
pp. 2328-2343 ◽  
Author(s):  
Ulrich Zander ◽  
Gleb Bourenkov ◽  
Alexander N. Popov ◽  
Daniele de Sanctis ◽  
Olof Svensson ◽  
...  
Keyword(s):  
Hierarchical Cluster ◽  
Data Sets ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
Data Set ◽  
X Ray ◽  
Partial Data ◽  
Final Data ◽  
Dispersion Technique

Here, an automated procedure is described to identify the positions of many cryocooled crystals mounted on the same sample holder, to rapidly predict and rank their relative diffraction strengths and to collect partial X-ray diffraction data sets from as many of the crystals as desired. Subsequent hierarchical cluster analysis then allows the best combination of partial data sets, optimizing the quality of the final data set obtained. The results of applying the method developed to various systems and scenarios including the compilation of a complete data set from tiny crystals of the membrane protein bacteriorhodopsin and the collection of data sets for successful structure determination using the single-wavelength anomalous dispersion technique are also presented.

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