Phase composition and morphological analysis of human gallstones using IR spectroscopy, scanning electron microscopy and X-ray Rietveld analysis

Author(s):  
Samiran Pramanik ◽  
Soumen Ghosh ◽  
Arkaprovo Roy ◽  
Ramanuj Mukherjee ◽  
Alok Kumar Mukherjee

AbstractQuantitative phase composition and morphological characterization of 12 human gallbladder stones (GS1–GS12) retrieved from patients of eastern India have been carried out using IR-spectroscopy, powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). The FTIR spectra indicated that the primary composition of gallstones studied was cholesterol. X-ray powder diffraction study revealed cholesterol monohydrate (CHM) as the major crystalline phase in GS1–GS12. The Rietveld analysis showed that nine of the gallstones were composed exclusively of CHM, while the remaining three stones contained in addition to CHM, small amounts (4.2–10.6 wt%) of calcium carbonate as aragonite and vaterite. The crystallite size of CHM in GS1–GS12 varied between 82(6) and 249(3) nm. The SEM images of gallstones showed different crystal habits of CHM such as plates, thin rods, rectangular and hexagonal blocks, which resulted into different levels of agglomeration at the mesoscopic scale. Presence of numerous parasitic eggs with a typical muskmelon surface in three gallstones (GS2, GS7 and GS9) suggests possible association between the liver fluke infection and biliary stone formation in these patients. To the best of our knowledge, the study constitutes the first report of X-ray quantitative phase analysis of gallstones using the Rietveld methodology.

2009 ◽  
Vol 42 (4) ◽  
pp. 629-635 ◽  
Author(s):  
Soumen Ghosh ◽  
Sharmila Basu ◽  
Santu Chakraborty ◽  
Alok K. Mukherjee

Structural and microstructural characterizations of eight human kidney stones (KS1–KS8) from eastern India have been carried out using IR spectroscopy, X-ray powder diffraction, scanning electron microscopy and thermogravimetric methods. An X-ray diffraction phase quantification revealed that three of the renal stones (KS1–KS3) were composed exclusively of calcium oxalate monohydrate (COM) and the remaining five (KS4–KS8) contained varying amounts of calcium oxalate dihydrate (40.1–53.0 wt%) and hydroxyapatite (1.3–17.3 wt%), in addition to the COM phase. The crystalline structure of COM (whewellite) at the atomic scale was redetermined through an X-ray powder diffraction study at room temperature using Rietveld analysis. Thermogravimetric analysis of KS1 reveals that COM (whewellite) is stable up to around 439 K, above which temperature anhydrous calcium oxalate is formed. The oxalate transforms to calcium carbonate at 751 K and finally to calcium oxide above 969 K. It should be emphasized that meaningful statistics in total number or gender specificity cannot be achieved with eight kidney stones.


2017 ◽  
Vol 12 (1) ◽  
pp. 63-77 ◽  
Author(s):  
Siriporn Sirikingkaew ◽  
Nuta Supakata

This study presents the development of geopolymer bricks synthetized from industrial waste, including fly ash mixed with concrete residue containing aluminosilicate compound. The above two ingredients are mixed according to five ratios: 100:0, 95:5, 90:10, 85:15, and 80:20. The mixture's physico-mechanical properties, in terms of water absorption and the compressive strength of the geopolymer bricks, are investigated according to the TIS 168-2546 standard. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses are used to investigate the microstructure and the elemental and phase composition of the brick specimens. The results indicate that the combination of fly ash and concrete residue represents a suitable approach to brick production, as required by the TIS 168–2546 standard.


Materials ◽  
2019 ◽  
Vol 12 (24) ◽  
pp. 4171 ◽  
Author(s):  
Paweł Rutkowski ◽  
Jan Huebner ◽  
Adrian Graboś ◽  
Dariusz Kata ◽  
Dariusz Grzybek ◽  
...  

In this study, the influence of the addition of rare earth oxides on the phase composition and density of KNN piezoelectric ceramics was investigated. The initial powders of Na2CO3 and K2CO3 were dried at 150 °C for 2 h. Then, a powder mixture for synthesis was prepared by adding a stoichiometric amount of Nb2O5 and 5 and 10 wt % overabundance of Na2CO3. All powders were mixed by ball-milling for 24 h and synthesized at 950 °C. The phase composition of the reaction bed was checked by means of X-ray diffraction (XRD). It had an appearance of tetragonal and monoclinic K0.5Na0.5NbO3 (KNN) phases. Then, 1 and 2 wt % of Er2O3 and Yb2O3, were added to the mixture. Green samples of 25 mm diameter and 3 mm thickness were prepared and sintered by hot pressing at 1000 °C for 2 h under 25 MPa pressure. The final samples were investigated via scanning electron microscopy (SEM)-energy-dispersive X-ray spectroscopy (EDS), XRD, Rietveld, and ultrasonic methods. Phase analysis showed tetragonal and orthorhombic KNN phases, and a contamination of (K2CO3·1.5H2O) was present. The obtained KNN polycrystals had a relative density above 95%. Texturing of the material was confirmed as a result of hot pressing.


2008 ◽  
Vol 368-372 ◽  
pp. 977-979
Author(s):  
Sheng Li Jin ◽  
Ya Wei Li ◽  
Jing Liu ◽  
Yuan Bing Li ◽  
Lei Zhao ◽  
...  

AlN/Al ceramic composite was fabricated by directed melt nitridation of pure Al block covered with 10wt% Mg powder at 1300°C in a high purity flowing N2. Microstructure and phase composition of the composite were investigated by scanning electron microscopy with energy dispersive spectroscopy and X-ray diffraction. Results showed that AlN is the main phase in the composite and its lattice parameters of a and c are 3.1110Å and 4.9806Å, respectively. The phase composition of the composite changes along the growth direction and a gradient sandwich structure forms. The surface of the composite is made up of a dense and thin nodular AlN layer, underneath which an AlN/Al layer appears, followed by an AlN/Al/MgAl2O4 layer. Thermodynamic calculations predicted the formation of possible phases with the addition of Mg. It suggested that the content of Mg at the reaction frontier of nitridation is considerably lower to 0.15wt% where MgAl2O4 was stable, because of escape and reaction exhaustion of Mg. Once Mg is lower than 0.05wt%, only a dense AlN layer can exist, which prevents the further nitridation of Al melt.


2009 ◽  
Vol 66 ◽  
pp. 171-174
Author(s):  
Zhao Deng ◽  
Ying Dai ◽  
Wen Chen

Single-crystalline BaTiO3 nanoparticles and BaCO3 nanowires were synthesized respectively through the use of a reverse micelle as a medium in the same Oleic acid/n-octane/H2O system, by changing the H2O2 dosage. Both the phase composition and the morphology can be controled. The samples derived were characterized with X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The formation mechanism has been fully discussed.


2010 ◽  
Vol 152-153 ◽  
pp. 1683-1686
Author(s):  
Qing Wang ◽  
Ya Hui Zhang

Biomorphic silicon carbide (bioSiC) was prepared by high temperature pyrolysis and sol-gel and carbothermal reduction processing at 1600 oC. The morphology and microstructure of carbon-silica composites and purified bioSiC samples were characterized by scanning electron microscopy. The phase composition of the resulting sample was analyzed by X-ray diffraction. The results suggest that the bioSiC mainly consists of cubic ß-SiC, and principally replicates the shape and microstructure of the carbon template.


Cerâmica ◽  
2016 ◽  
Vol 62 (361) ◽  
pp. 1-8 ◽  
Author(s):  
J. L. Alves ◽  
A. E. Zanini ◽  
M. E. de Souza ◽  
M. L. F. Nascimento

Abstract Clays obtained from nature have a lot of impurities. Therefore, for best using of these materials, it is necessary its selection and purification. Thus, the aim of this work is to separate and to purify the smectite fractions using water as a solvent at a low flux mixed with a bentonite clay extracted from a mine in Vitória da Conquista - Bahia / Brazil. For this a separation method of fractions of expandable clays based on the Stokes' Law was applied - this process is called elutriation, in order to ensure and to expand possible industrial applications of this material. The samples were characterized by analysis of X-ray diffraction, X-ray fluorescence and scanning electron microscopy. The Rietveld method enabled the quantification of main phase minerals: montmorillonite, kaolinite, nontronite and quartz, reaching 85% in mass of montmorillonite phase at the end of the process. Results showed that the method used was efficient to remove almost all quartz, carbonates and organic matter from the sample. It was also observed a monomodal grain size distribution of elutriated materials with thinner grains, around (18.1 ± 1.8) μm at the end of the process. It has been concluded that the method developed and applied showed promising characters to be applied to elutriate kilograms of clays and could be used in industrial scale.


2012 ◽  
Vol 602-604 ◽  
pp. 526-529
Author(s):  
Qing Wang ◽  
Lin Zhang ◽  
Ya Hui Zhang

Biomorphic TiO2 was prepared by high temperature pyrolysis and a modified sol-gel route. The morphology and microstructure of TiO2 samples were characterized by scanning electron microscopy. The phase composition of the resulting sample was analyzed by X-ray diffraction. The results suggest that the biomorphic TiO2 mainly consists of rutile TiO2, and replicates the shape and part microstructure of the carbon template.


Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1515
Author(s):  
Halyna Klym ◽  
Ivan Karbovnyk ◽  
Andriy Luchechko ◽  
Yuriy Kostiv ◽  
Viktorija Pankratova ◽  
...  

BaGa2O4 ceramics doped with Eu3+ ions (1, 3 and 4 mol.%) were obtained by solid-phase sintering. The phase composition and microstructural features of ceramics were investigated using X-ray diffraction and scanning electron microscopy in comparison with energy-dispersive methods. Here, it is shown that undoped and Eu3+-doped BaGa2O4 ceramics are characterized by a developed structure of grains, grain boundaries and pores. Additional phases are mainly localized near grain boundaries creating additional defects. The evolution of defect-related extended free volumes in BaGa2O4 ceramics due to the increase in the content of Eu3+ ions was studied using the positron annihilation lifetime spectroscopy technique. It is established that the increase in the number of Eu3+ ions in the basic BaGa2O4 matrix leads to the agglomeration of free-volume defects with their subsequent fragmentation. The presence of Eu3+ ions results in the expansion of nanosized pores and an increase in their number with their future fragmentation.


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