Structural and microstructural characterization of human kidney stones from eastern India using IR spectroscopy, scanning electron microscopy, thermal study and X-ray Rietveld analysis

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.

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.


Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts

Calcium is an important element in the growth and development of plants and one form of calcium is calcium oxalate. Calcium oxalate has been found in leaf seed, stem material plant tissue culture, fungi and lichen using one or more of the following methods—polarized light microscopy (PLM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction.Two methods are presented here for qualitatively estimating calcium oxalate in dried or fixed tobacco (Nicotiana) leaf from different stalk positions using PLM. SEM, coupled with energy dispersive x-ray spectrometry (EDS), and powder x-ray diffraction were used to verify that the crystals observed in the dried leaf with PLM were calcium oxalate.


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.


2015 ◽  
Vol 48 (6) ◽  
pp. 1794-1804 ◽  
Author(s):  
Paramita Chatterjee ◽  
Samiran Pramanik ◽  
Alok Kumar Mukherjee

A combination of IR spectroscopy, scanning electron microscopy (SEM) and powder X-ray diffraction has been used to analyze the compositional and architectural variation across the different parts (core, middle and outer layers) of five human urinary calculi (KS1–KS5) from eastern India. Rietveld quantitative phase analysis using X-ray powder diffraction revealed that the composition of the core regions in KS1–KS3 and KS5 is exclusively whewellite, whereas in KS4 it is a mixture of whewellite (84.5 wt%) and carbonated hydroxyapatite (15.5 wt%). While one of the renal stones, KS1, is composed of only whewellite in all three regions, a distinct variation in phase composition from the core towards the periphery has been observed in KS2–KS5. A drastic change in phase composition has been noted in KS5, with the major constituent phases in the core, middle and outer layers as whewellite (100.0 wt%), anhydrous uric acid (60.7 wt%) and carbonated hydroxyapatite (69.6 wt%), respectively. The crystallite size of whewellite in different parts of the kidney stones varies between 91 (1) and 167 (1) nm, while the corresponding sizes of the anhydrous uric acid in KS5 and carbonated hydroxyapatite in KS3 are 107 (1) and 18 (1)–20 (1) nm, respectively. SEM images of the kidney stones showed different levels of organization, resulting from an agglomeration of crystallites with diverse shapes and sizes.


2003 ◽  
Vol 58 (11-12) ◽  
pp. 812-816 ◽  
Author(s):  
Mohamed E. Malainine ◽  
Alain Dufresne ◽  
Danielle Dupeyre ◽  
Michel R. Vignon ◽  
Mostafa Mahrouz

Abstract Calcium oxalate crystallites occur very often in the plants tissues and their role is still poorly known. We report here the experimental protocol leading to the isolation of two forms of calcium oxalate crystallites differing in their hydration level in the parenchymal tissues of Opuntia ficus indica (Miller). Whereas the whewellite crystallites are habitual in all Opuntia species, the weddellite form has never been isolated from these species before, which is probably due to their small size (about 1 μm). We have identified these forms using X-ray diffraction and scanning electron microscopy.


1977 ◽  
Vol 55 (13) ◽  
pp. 1807-1819 ◽  
Author(s):  
Jean D. Schoknecht ◽  
Harold W. Keller

The nature of the peridial deposits in the genus Perichaena and in a species of Dianema has been defined by a combination of scanning electron microscopy, x-ray microanalysis, and various chemical techniques. These crystalline deposits in the peridium have proven to be primarily calcium oxalate. Some species of Perichaena and the Dianema also incoiporate silicon crystals on the peridium. The white and non-white phases of different species of Perichaena were compared and found to have similar elemental composition of peridia.


2009 ◽  
Vol 12 (3) ◽  
pp. 77-84
Author(s):  
Thao Tien Nguyen ◽  
Ngoan Thi Nguyen ◽  
Long Van Dang

All TiO2/SiO2 samples were prepared by the impregnation of Ti(i-PrO)4 in isopropanol at room temperature followed drying and calcination. The solids were characterized by several techniques including X- ray diffraction (XRD), IR spectroscopy, Scanning Electron Microscopy (SEM). No reflection lines of TiO2 are detected at a low content of TiO2 (< 7%), but are more visible at a higher concentration. The catalysts are tested in the liquid oxidation of styrene under mild conditions, producing mainly benzaldehyde. The effects of variables on the catalytic activity are also investigated.


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