Mineralogical characterization of a highly-weathered soil by the Rietveld Method

The mineralogical characterization through mineral quantification of Brazilian soils by X-ray diffraction data using the Rietveld Method is not common. A mineralogical quantification of an Acric Ferralsol from the Ponta Grossa region, state of Paraná, Brazil, was carried out using this Method with X-Ray Diffraction data to verify if this method was suitable for mineral quantification of a highly-weathered soil. The A, AB and B3 horizons were fractioned to separate the different particle sizes: clay, silt, fine sand (by Stokes Law) and coarse sand fractions (by sieving), with the procedure free of chemical treatments. X-ray Fluorescence, Inductively Coupled Plasma Atomic Emission Spectrometry, Infrared Spectroscopy and Mössbauer Spectroscopy were used in order to assist the mineral identification and quantification. The Rietveld Method enabled the quantification of the present minerals. In a general way, the quantitative mineralogical characterization by the Rietveld Method revealed that quartz, gibbsite, rutile, hematite, goethite, kaolinite and halloysite were present in the clay and silt fractions of all horizons. The silt fractions of the deeper horizons were different from the more superficial ones due to the presence of large amounts of quartz. The fine and the coarse sand fractions are constituted mainly by quartz. Therefore, a mineralogical quantification of the finer fraction (clay and silt) by the Rietveld Method was successful.

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Synthesis and characterization of Na-P1 (GIS) zeolite using a kaolinitic rock

10.21203/rs.3.rs-111813/v1 ◽

2020 ◽

Author(s):

Daniela Novembre ◽

Domingo Gimeno ◽

Alessandro Del Vecchio

Keyword(s):

Inductively Coupled Plasma ◽

Rietveld Method ◽

Ambient Pressure ◽

Optical Emission ◽

Emission Spectrometry ◽

Quantitative Phase Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Cell Parameters ◽

Inductively Coupled

Abstract This work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 ° and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods.The results make the experimental protocol very promising for an industrial transfer.

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Microstructure and Electrochemical Properties of a LaMgAlMnCoNi Based Alloy for Ni/MH Batteries

Materials Science Forum ◽

10.4028/www.scientific.net/msf.727-728.80 ◽

2012 ◽

Vol 727-728 ◽

pp. 80-84 ◽

Cited By ~ 4

Author(s):

Eliner Affonso Ferreira ◽

J.M. Serra ◽

Julio César Serafim Casini ◽

Hidetoshi Takiishi ◽

Rubens Nunes de Faria Jr.

Keyword(s):

Electrochemical Properties ◽

Inductively Coupled Plasma ◽

Atomic Emission ◽

Emission Spectrometry ◽

X Ray Diffraction ◽

Cast State ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Inductively Coupled ◽

Type Test

The microstructure and electrochemical properties of a La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 hydrogen storage alloy have been studied. The anode was prepared using a mixture of the ingot alloy in the as-cast state with carbon black and polytetrafluoroethylene (PTFE) as a binder. A Ni (OH)2 electrode was used as the cathode of the square-type test cell. A separator was used together with a 6M KOH electrolyte. Microstructure and phase composition of the alloy have been investigated using inductively coupled plasma atomic emission spectrometry (ICP-AES), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction analysis (XRD). A niobium-containing alloy has also been included for a comparison.

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Synthesis and characterization of Na-P1 (GIS) zeolite using a kaolinitic rock

Scientific Reports ◽

10.1038/s41598-021-84383-7 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Daniela Novembre ◽

Domingo Gimeno ◽

Alessandro Del Vecchio

Keyword(s):

Inductively Coupled Plasma ◽

Rietveld Method ◽

Ambient Pressure ◽

Optical Emission ◽

Emission Spectrometry ◽

Quantitative Phase Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Cell Parameters ◽

Inductively Coupled

AbstractThis work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The results make the experimental protocol very promising for an industrial transfer.

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Heat Treatment and Microstructural Studies of LaNi-Type Battery Electrode Alloys

Materials Science Forum ◽

10.4028/www.scientific.net/msf.899.366 ◽

2017 ◽

Vol 899 ◽

pp. 366-370

Author(s):

Eliner Affonso Ferreira ◽

Lusinete Pereira Barbosa ◽

Rubens Nunes de Faria Jr.

Keyword(s):

Heat Treatment ◽

Inductively Coupled Plasma ◽

Atomic Emission ◽

Emission Spectrometry ◽

Electrochemical Characteristics ◽

X Ray Diffraction ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Inductively Coupled ◽

Battery Electrode

The effects of annealing on the microstructures and electrochemical characteristics of a La0.7Mg0.3Al0.3Mn0.4Co0.5Ni3.8 hydrogen storage alloy have been studied. The heat treatment by vacuum annealing was carried out at 700 °C, 800 °C, 900 °C and 1000 °C. The microstructure and phase composition of the alloy have been investigated using inductively coupled plasma - atomic emission spectrometry (ICP-AES), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction analysis (XRD). The battery anode was prepared using a mixture of the pulverized alloy with carbon black and polytetrafluoroethylene as a binder.

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Characterization and identification of mixed-metal phosphates in soils: the application of Raman spectroscopy

Mineralogical Magazine ◽

10.1180/0026461036760166 ◽

2003 ◽

Vol 67 (6) ◽

pp. 1299-1316 ◽

Cited By ~ 25

Author(s):

A. M. Lanfranco ◽

P. F. Schofield ◽

P. J. Murphy ◽

M. E. Hodson ◽

J. F. W. Mosselmans ◽

...

Keyword(s):

Raman Spectroscopy ◽

Inductively Coupled Plasma ◽

Emission Spectrometry ◽

X Ray Diffraction ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Mixed Metal ◽

Synthesis Conditions ◽

Metal Phosphates ◽

Cell Parameters

AbstractThe development of protocols for the identification of metal phosphates in phosphate-treated, metalcontaminated soils is a necessary yet problematical step in the validation of remediation schemes involving immobilization of metals as phosphate phases. The potential for Raman spectroscopy to be applied to the identification of these phosphates in soils has yet to be fully explored. With this in mind, a range of synthetic mixed-metal hydroxylapatites has been characterized and added to soils at known concentrations for analysis using both bulk X-ray powder diffraction (XRD) and Raman spectroscopy.Mixed-metal hydroxylapatites in the binary series Ca –Cd, Ca –Pb, Ca –Sr and Cd –Pb synthesized in the presence of acetate and carbonate ions, were characterized using a range of analytical techniques including XRD, analytical scanning electron microscopy (SEM), infrared spectroscopy (IR), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and Raman spectroscopy. Only the Ca –Cd series displays complete solid solution, although under the synthesis conditions of this study the Cd5(PO4)3OH end member could not be synthesized as a pure phase. Within the Ca –Cd series the cell parameters, IR active modes and Raman active bands vary linearly as a function of Cd content. X-ray diffraction and extended X-ray absorption fine structure spectroscopy (EXAFS) suggest that the Cd is distributed across both the Ca(1) and Ca(2) sites, even at low Cd concentrations.In order to explore the likely detection limits for mixed-metal phosphates in soils for XRD and Raman spectroscopy, soils doped with mixed-metal hydroxylapatites at concentrations of 5, 1 and 0.5 wt.% were then studied. X-ray diffraction could not confirm unambiguously the presence or identity of mixed-metal phosphates in soils at concentrations below 5 wt.%. Raman spectroscopy proved a far more sensitive method for the identification of mixed-metal hydroxylapatites in soils, which could positively identify the presence of such phases in soils at all the dopant concentrations used in this study. Moreover, Raman spectroscopy could also provide an accurate assessment of the degree of chemical substitution in the hydroxylapatites even when present in soils at concentrations as low as 0.1%.

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Distribution and Mode of Occurrence of Co, Ni, Cu, Zn, As, Ag, Cd, Sb, Pb in the Feed Coal, Fly Ash, Slag, in the Topsoil and in the Roots of Trees and Undergrowth Downwind of Three Power Stations in Poland

Minerals ◽

10.3390/min11020133 ◽

2021 ◽

Vol 11 (2) ◽

pp. 133

Author(s):

Henryk R. Parzentny ◽

Leokadia Róg

Keyword(s):

Inductively Coupled Plasma ◽

Coal Fly Ash ◽

Atomic Emission ◽

Emission Spectrometry ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Inductively Coupled ◽

Power Stations ◽

Mode Of Occurrence ◽

Feed Coal

It is supposed that the determination of the content and the mode of occurrence of ecotoxic elements (EE) in feed coal play the most significant role in forecasting distribution of EE in the soil and plants in the vicinity of power stations. Hence, the aim of the work was to analyze the properties of the feed coal, the combustion residues, and the topsoil which are reached by EE together with dust from power stations. The mineral and organic phases, which are the main hosts of EE, were identified by microscopy, X-ray powder diffraction, inductively coupled plasma atomic emission spectrometry, and scanning electron microscope with an energy dispersive X-ray methods. The highest content of elements was observed in the Oi and Oe subhorizons of the topsoil. Their hosts are various types of microspheres and char, emitted by power stations. In the areas of long-term industrial activity, there are also sharp-edged grains of magnetite emitted in the past by zinc, lead, and ironworks. The enrichment of the topsoil with these elements resulted in the increase in the content of EE, by between 0.2 times for Co; and 41.0 times for Cd in the roots of Scots pine, common oak and undergrowth, especially in the rhizodermis and the primary cortex and, more seldom, in the axle roller and cortex cells.

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Structure Refinements of the Layered Intergrowth Phases SbIIISbV x A 1−x TiO6 (x≃0, A = Ta, Nb) Using Synchrotron X-ray Powder Diffraction Data

Acta Crystallographica Section B Structural Science ◽

10.1107/s0108768197007787 ◽

1997 ◽

Vol 53 (6) ◽

pp. 861-869 ◽

Cited By ~ 2

Author(s):

C. D. Ling ◽

J. G. Thompson ◽

S. Schmid ◽

D. J. Cookson ◽

R. L. Withers

Keyword(s):

Single Crystal ◽

Powder Diffraction ◽

Diffraction Data ◽

Homologous Series ◽

Rietveld Method ◽

Powder Diffraction Data ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray ◽

The Family

The structures of the layered intergrowth phases SbIIISb^{\rm V}_xAl-xTiO6 (x \simeq 0, A = Ta, Nb) have been refined by the Rietveld method, using X-ray diffraction data obtained using a synchrotron source. The starting models for these structures were derived from those of Sb^{\rm III}_3Sb^{\rm V}_xA 3−xTiO14 (x = 1.26, A = Ta and x = 0.89, A = Nb), previously solved by single-crystal X-ray diffraction. There were no significant differences between the derived models and the final structures, validating the approach used to obtain the models and confirming that the n = 1 and n = 3 members of the family, Sb^{\rm III}_nSb^{\rm V}_xA n−xTiO4n+2 are part of a structurally homologous series.

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Geological Controls on Mineralogy and Geochemistry of the Permian and Jurassic Coals in the Shanbei Coalfield, Shaanxi Province, North China

Minerals ◽

10.3390/min10020138 ◽

2020 ◽

Vol 10 (2) ◽

pp. 138

Author(s):

Yunfei Shangguan ◽

Xinguo Zhuang ◽

Jing Li ◽

Baoqing Li ◽

Xavier Querol ◽

...

Keyword(s):

Inductively Coupled Plasma ◽

North China ◽

Ordos Basin ◽

Source Region ◽

Atomic Emission ◽

Shaanxi Province ◽

Emission Spectrometry ◽

Plasma Atomic Emission Spectrometry ◽

X Ray ◽

Diagenetic Fluid

Coal as the source of critical elements has attracted much attention and the enrichment mechanisms are of significant importance. This paper has an opportunity to investigate the mineralogical and geochemical characteristics of the Permian and Jurassic bituminous coals and associated non-coals from two underground coal mines in the Shanbei Coalfield (Northeast Ordos basin), Shaanxi Province, North China, based on the analysis of X-ray diffraction (XRD), inductively coupled plasma atomic-emission spectrometry (ICP-AES/MS), and scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS). The Jurassic and Permian coals have similar chemical features excluding ash yield, which is significantly higher in the Permian coals. Major mineral matters in the Jurassic coals are quartz, kaolinite, and calcite. By contrast, mineral assemblages of the Permian coals are dominated by kaolinite; and apatite occurring in the middle section’s partings. The Jurassic coals are only enriched in B, whereas the Permian coals are enriched in some trace elements (e.g., Nb, Ta, Th, and REY). Boron has a mixed inorganic and organic association which may be absorbed by organic matter from fluid (or groundwater) or inherited from coal-forming plants. Additionally, climatic variation also plays an important role. As for the Permian coals, kaolinite and apatite as the major carriers of elevated elements; the former were derived from the sedimentary source region (the Yinshan Oldland and the Benxi formation) and later precipitated from Ca-, and P-rich solutions. We deduced that those elevated elements may be controlled by the source rock and diagenetic fluid input. The findings of this work offered new data to figure out the mechanism of trace element enrichment of coal in the Ordos basin.

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