scholarly journals Synthesis of Zeolite A from Iraqi Natural Kaolin Using a Conventional Hydrothermal Synthesis Technique

2020 ◽  
Vol 4 (2) ◽  
pp. 11-23
Author(s):  
Ali Salih ◽  
Craig Williams ◽  
Polla Khanaqa
Keyword(s):  
Sodium Hydroxide Solution ◽  
Analytical Techniques ◽  
Crystal Habit ◽  
Zeolite A ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chemical Treatments ◽  
Zeolite Type ◽  
Hydrothermal Transformation ◽  
Lower Temperature

The synthesis of zeolite materials by hydrothermal transformation of kaolin using a conventional hydrothermal method was investigated. Different analytical techniques were used to characterize the starting kaolin and produced zeolite A samples, including scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), x-ray diffraction (XRD), x-ray fluorescence (XRF), thermogravimetric analysis (TGA), and Fourier transform infrared (FT-IR) spectroscopy. The synthetic zeolite type A was obtained after activation of kaolin and metakaolin followed by different thermal and chemical treatments. The metakaolinization phase was achieved by calcining the kaolin in air at 600°C for 3 hours, a much lower temperature than previously reported in the literature. Metakaolin was treated with 3 M sodium hydroxide solution at a ratio of 1:5 and, using stainless steel autoclaves with teflon liners, heated the mixture to 200°C in a microwave for 24 hours. The results from this synthesis route showed that zeolite A with a cubic crystal habit has been successfully synthesized.

The effect of calcination temperature on metakaolin structure for the synthesis of zeolites

Clay Minerals ◽  
2018 ◽  
Vol 53 (4) ◽  
pp. 657-663 ◽  
Author(s):  
Magdalena Król ◽  
Piotr Rożek
Keyword(s):  
Electron Microscopy ◽  
Sodium Hydroxide Solution ◽  
Alkali Activation ◽  
Zeolite A ◽  
Optimal Temperature ◽  
X Ray Diffraction ◽  
Activation Temperature ◽  
X Ray ◽  
Naoh Solution ◽  
Scanning Electron

ABSTRACTThe aim of this research was to determine the temperature of kaolin calcination in order to obtain an intermediate product (metakaolin) for the synthesis of geopolymers with potential application as self-supporting zeolitic membranes. The products obtained were analysed with X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The structural analysis of the metakaolins obtained suggested that the optimal temperature for the proposed application is 700°C. After alkali activation of metakaolin, it is possible to obtain zeolite A and hydroxysodalite. The factors analysed, determining the type and quantity of crystalline phases, were activation temperature and concentration of sodium hydroxide solution (activator). The largest amounts of zeolites were obtained by alkali activation with 9 mol/dm3 NaOH solution at 70°C.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

scholarly journals First Report on the Geologic Occurrence of Natural Na–A Zeolite and Associated Minerals in Cretaceous Mudstones of the Paja Formation of Vélez (Santander), Colombia

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Carlos Alberto Ríos-Reyes ◽  
German Alfonso Reyes-Mendoza ◽  
José Antonio Henao-Martínez ◽  
Craig Williams ◽  
Alan Dyer
Keyword(s):  
Natural Zeolite ◽  
Scanning Electron Micrographs ◽  
Total Sulfur ◽  
Zeolite A ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mineral Phases ◽  
The World ◽  
Porosity And Permeability ◽  
First Time

This study reports for the first time the geologic occurrence of natural zeolite A and associated minerals in mudstones from the Cretaceous Paja Formation in the urban area of the municipality of Vélez (Santander), Colombia. These rocks are mainly composed of quartz, muscovite, pyrophyllite, kaolinite and chlorite group minerals, framboidal and cubic pyrite, as well as marcasite, with minor feldspar, sulphates, and phosphates. Total organic carbon (TOC), total sulfur (TS), and millimeter fragments of algae are high, whereas few centimeters and not biodiverse small ammonite fossils, and other allochemical components are subordinated. Na–A zeolite and associated mineral phases as sodalite occur just beside the interparticle micropores (honeycomb from framboidal, cube molds, and amorphous cavities). It is facilitated by petrophysical properties alterations, due to processes of high diagenesis, temperatures up to 80–100 °C, with weathering contributions, which increase the porosity and permeability, as well as the transmissivity (fluid flow), allowing the geochemistry remobilization and/or recrystallization of pre-existing silica, muscovite, kaolinite minerals group, salts, carbonates, oxides and peroxides. X-ray diffraction analyses reveal the mineral composition of the mudstones and scanning electron micrographs show the typical cubic morphology of Na–A zeolite of approximately 0.45 mμ in particle size. Our data show that the sequence of the transformation of phases is: Poorly crystalline aluminosilicate → sodalite → Na–A zeolite. A literature review shows that this is an unusual example of the occurrence of natural zeolites in sedimentary marine rocks recognized around the world.

scholarly journals Transport and Dielectric Properties of Mechanosynthesized La2/3Cu3Ti4O12 Ceramics

Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 313
Author(s):  
Mohamad M. Ahmad ◽  
Hicham Mahfoz Kotb ◽  
Celin Joseph ◽  
Shalendra Kumar ◽  
Adil Alshoaibi
Keyword(s):  
Dielectric Constant ◽  
Sintering Temperature ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Boundary Conductivity ◽  
X Ray ◽  
Giant Dielectric ◽  
Mechanochemical Milling ◽  
Giant Dielectric Constant ◽  
Lower Temperature

La2/3Cu3Ti4O12 (LCTO) powder has been synthesized by the mechanochemical milling technique. The pelletized powder was conventionally sintered for 10 h at a temperature range of 975–1025 °C, which is a lower temperature process compared to the standard solid-state reaction. X-ray diffraction analysis revealed a cubic phase for the current LCTO ceramics. The grain size of the sintered ceramics was found to increase from 1.5 ± 0.5 to 2.3 ± 0.5 μm with an increase in sintering temperature from 975 to 1025 °C. The impedance results show that the grain conductivity is more than three orders of magnitude larger than the grain boundary conductivity for LCTO ceramics. All the samples showed a giant dielectric constant (1.7 × 103–3.4 × 103) and dielectric loss (0.09–0.17) at 300 K and 10 kHz. The giant dielectric constant of the current samples was attributed to the effect of internal barrier layer capacitances due to their electrically inhomogeneous structure.

scholarly journals Analytical study of Buddha sculptures in Jingyin temple of Taiyuan, China

2021 ◽  
Vol 9 (1) ◽  
Author(s):  
Xiaojian Bai ◽  
Chen Jia ◽  
Zhigen Chen ◽  
Yuxuan Gong ◽  
Huwei Cheng ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Analytical Study ◽  
Energy Dispersive Spectrometry ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Ancient China ◽  
X Ray ◽  
Unique Style ◽  
Scanning Electron

AbstractWith exquisite design and unique style, the painted sculptures of Tutang Buddha and two attendants Buddha in Jingyin Temple are precious cultural heritages of China. The sculpture of Tutang Buddha, which was carved from a mound and painted by ancient craftsmen, was rarely found in ancient China. However, due to natural and human factors, the sculptures were severely damaged. Obviously, they require urgent and appropriate protection and restoration. In this study, samples taken from the sculptures were analysed through multiple analytical techniques, including scanning electron microscopy with energy dispersive spectrometry (SEM–EDS), Raman spectroscopy, X-ray diffraction (XRD), optical microscopy (OM) and granulometry. The analysis results enable us to infer the techniques used by the craftsmen in making the sculptures and provide a reliable evidence for the conservation and future protection of these and similar sculptures.

scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Xrd Analysis ◽  
Crystal Habit ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Evaluation ◽  
Rational Understanding ◽  
Structural Inspection

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

scholarly journals Assay and physicochemical characterization of the antiparasitic albendazole

2012 ◽  
Vol 48 (2) ◽  
pp. 281-290 ◽  
Author(s):  
Noely Camila Tavares Cavalcanti ◽  
Giovana Damasceno Sousa ◽  
Maria Alice Maciel Tabosa ◽  
José Lamartine Soares Sobrinho ◽  
Leila Bastos Leal ◽  
...  
Keyword(s):  
Physicochemical Characterization ◽  
Analytical Techniques ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
X Ray Diffraction ◽  
Melting Points ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Complementary Techniques

The aim of this study was to characterize three batches of albendazole by pharmacopeial and complementary analytical techniques in order to establish more detailed specifications for the development of pharmaceutical forms. The ABZ01, ABZ02, and ABZ03 batches had melting points of 208 ºC, 208 ºC, and 209 ºC, respectively. X-ray diffraction revealed that all three batches showed crystalline behavior and the absence of polymorphism. Scanning electron microscopy showed that all the samples were crystals of different sizes with a strong tendency to aggregate. The samples were insoluble in water (5.07, 4.27, and 4.52 mg mL-1, respectively) and very slightly soluble in 0.1 M HCl (55.10, 56.90, and 61.70 mg mL-1, respectively) and additionally showed purities within the range specified by the Brazilian Pharmacopoeia 5th edition (F. Bras. V; 98% to 102%). The pharmacopeial assay method was not reproducible and some changes were necessary. The method was validated and showed to be selective, specific, linear, robust, precise, and accurate. From this characterization, we concluded that pharmacopeial techniques alone are not able to detect subtle differences in active pharmaceutical ingredients; therefore, the use of other complementary techniques is required to ensure strict quality control in the pharmaceutical industry.

scholarly journals Synthesis and characterization of apatite silicated powders with wet precipitation method

2021 ◽  
Vol 234 ◽  
pp. 00106
Author(s):  
Houda Labjar ◽  
Hassan Chaair
Keyword(s):  
Electron Microscopy ◽  
Heat Treatment ◽  
Analytical Techniques ◽  
Precipitation Method ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wet Precipitation ◽  
Scanning Electron

The synthesis of apatite silicated Ca10(PO4)6-x(SiO4)x(OH)2-x (SiHA) with 0≤x≤2 was investigated using a wet precipitation method followed by heat treatment using calcium carbonate CaCO3 and phosphoric acid H3PO4 and silicon tetraacetate SiC8H20O4 (TEOS) in medium of water ethanol, with three different silicate concentrations. After drying, the samples are ground and then characterized by different analytical techniques like X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning electron Microscopy (SEM) and chemical analysis.

scholarly journals Characterising the Microstructure of an Additively Built Al-Cu-Li Alloy

Materials ◽  
2020 ◽  
Vol 13 (22) ◽  
pp. 5188
Author(s):  
Iris Raffeis ◽  
Frank Adjei-Kyeremeh ◽  
Uwe Vroomen ◽  
Silvia Richter ◽  
Andreas Bührig-Polaczek
Keyword(s):  
Volume Fraction ◽  
Analytical Techniques ◽  
High Strength ◽  
High Energy ◽  
Phase System ◽  
X Ray Diffraction ◽  
Powder Bed ◽  
X Ray ◽  
Conventional View ◽  
Multi Phase

Al-Cu-Li alloys are famous for their high strength, ductility and weight-saving properties, and have for many years been the aerospace alloy of choice. Depending on the alloy composition, this multi-phase system may give rise to several phases, including the major strengthening T1 (Al2CuLi) phase. Microstructure investigations have extensively been reported for conventionally processed alloys with little focus on their Additive Manufacturing (AM) characterised microstructures. In this work, the Laser Powder Bed Fusion (LPBF) built microstructures of an AA2099 Al-Cu-Li alloy are characterised in the as-built (no preheating) and preheat-treated (320 °C, 500 °C) conditions using various analytical techniques, including Synchrotron High-Energy X-ray Diffraction (S-HEXRD). The observed dislocations in the AM as-built condition with no detected T1 precipitates confirm the conventional view of the difficulty of T1 to nucleate on dislocations without appropriate heat treatments. Two main phases, T1 (Al2CuLi) and TB (Al7.5Cu4Li), were detected using S-HEXRD at both preheat-treated temperatures. Higher volume fraction of T1 measured in the 500 °C (75.2 HV0.1) sample resulted in a higher microhardness compared to the 320 °C (58.7 HV0.1) sample. Higher TB volume fraction measured in the 320 °C sample had a minimal strength effect.

scholarly journals Natural and Activated Allophane Catalytic Activity Based on the Microactivity Test in Astm Norm 3907/D3907M-2019

2020 ◽  
Vol 10 (9) ◽  
pp. 3035
Author(s):  
Edward Henry Jiménez Calderón ◽  
Ana Emperatriz Paucar Tipantuña ◽  
Paulina Fernanda Herrera Mullo ◽  
Daniel Alejandro Hidalgo Cháfuel ◽  
Washington Ruiz ◽  
...  
Keyword(s):  
Analytical Techniques ◽  
Bet Surface Area ◽  
Navier Stokes ◽  
Maximum Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Catalytic Activation ◽  
Atomic Force ◽  
Activating Agent

The optimal conditions of the catalytic activation of allophane were evaluated for possible use as a catalyst within a fluidized bed catalytic cracking unit (FCC). The physicochemical properties of natural allophane and activated allophane were studied by using an alkaline activating agent, followed by a hydrothermal treatment. For the characterization, analytical techniques were used: Fourier transform infrared spectroscopy, particle size, (BET) surface area, thermogravimetry (TGA), X-ray diffraction (XRD), chemisorption, X-ray fluorescence (XRF), atomic force microscopy (AFM), and chromatography. The catalytic evaluation was determined by the (MAT) micro activity test equipment constructed according to ASTM D-3907/D3907M-2019. In addition, the Navier–Stokes 3D equations (nonlinear partial derivatives) were studied, which allow studying molecular dynamics contributing substantively to chemical kinetics describing the process of decomposition of crude oil in thermal cracking, determining the maximum temperature at which it retains its properties through the action of heat.

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