Fe-loaded zeolites as catalysts in the formation of humic substance-like darkcoloured polymers in polycondensation reactions of humic precursors

Clay Minerals ◽  
2012 ◽  
Vol 47 (3) ◽  
pp. 355-364 ◽  
Author(s):  
S. Fukuchi ◽  
M. Fukushima ◽  
R. Nishimoto ◽  
G. Qi ◽  
T. Sato

AbstractTo enhance the catalytic activities of zeolites for the polycondensation reactions of humic precursors, Fe was loaded into a zeolite via an ion-exchange reaction and the resulting product was subjected to calcination at 773 K. Two types iron-loaded zeolites were prepared using one equivalent (Fe-Z-1) and 10-equivalents (Fe-Z-10) of Fe2+ to the cation-exchange capacity of a natural zeolite from Niki town (Hokkaido, Japan). X-ray diffraction (XRD) patterns and X-ray photoelectron spectroscopy (XPS) spectra showed that the Fe(II) that was originally loaded into the cation-exchange sites in the zeolite became oxidized to a Fe(III) ionic species during the preparation. The catalytic activities of each zeolite were evaluated, based on the degree of darkening for reaction mixtures containing catechol, glycine and glucose as model humic precursors. The catalytic activities of Fe-Z-1 and Fe-Z-10 were higher than that for an untreated zeolite, and increased with the amount of Fe in the zeolite.

Materials ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1173
Author(s):  
Fotini Martsouka ◽  
Konstantinos Papagiannopoulos ◽  
Sophia Hatziantoniou ◽  
Martin Barlog ◽  
Giorgos Lagiopoulos ◽  
...  

Six pharmaceutical pastes were prepared using chemically modified kaolin and talc powders. Tests were conducted to determine their structural and chemical characteristics as well as their antimicrobial protection, thus rendering them suitable for cosmetic and pharmaceutical uses. Kaolin and talc were treated chemically via the cation exchange method to load the clay particles with copper and zinc ions, two cations well known for their antimicrobial properties. Mineralogical analyses were conducted by using X-ray diffraction (XRD) before and after the modification, confirming the mineralogical purity of the samples. Scanning electron microscopy was also used in conjunction with energy dispersed spectroscopy (SEM-EDS) to obtain chemical mapping images, revealing the dispersion of the added metals upon the clay minerals surfaces. Moreover, chemical analysis has been performed (XRF) to validate the enrichment of the clays with each metal utilizing the cation exchange capacity. All modified samples showed the expected elevated concentration in copper or zinc in comparison to their unmodified versions. From the X-ray photoelectron spectroscopy (XPS), the chemical state of the samples’ surfaces was investigated, revealing the presence of salt compounds and indicating the oxidation state of adsorbed metals. Finally, the resistance of pastes in microbial growth when challenged with bacteria, molds, and yeasts was assessed. The evaluation is based on the European Pharmacopeia (EP) criteria.


2009 ◽  
Vol 2009 ◽  
pp. 1-8 ◽  
Author(s):  
Valentina Krylova ◽  
Mindaugas Andrulevičius

Copper sulfide layers were formed on polyamide PA 6 surface using the sorption-diffusion method. Polymer samples were immersed for 4 and 5 h in 0.15 mol⋅  solutions and acidified with HCl (0.1 mol⋅) at . After washing and drying, the samples were treated with Cu(I) salt solution. The samples were studied by UV/VIS, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) methods. All methods confirmed that on the surface of the polyamide film a layer of copper sulfide was formed. The copper sulfide layers are indirect band-gap semiconductors. The values of are 1.25 and 1.3 eV for 4 h and 5 h sulfured PA 6 respectively. Copper XPS spectra analyses showed Cu(I) bonds only in deeper layers of the formed film, while in sulfur XPS S 2p spectra dominating sulfide bonds were found after cleaning the surface with ions. It has been established by the XRD method that, beside , the layer contains as well. For PA 6 initially sulfured 4 h, grain size forchalcocite, , was  nm and fordjurleite, , it was 54.17 nm. The sheet resistance of the obtained layer varies from 6300 to 102 .


Nanomaterials ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 1440 ◽  
Author(s):  
Sanjeev K. Sharma ◽  
Ashish R. Sharma ◽  
Sudheer D. V. N. Pamidimarri ◽  
Jyotshana Gaur ◽  
Beer Pal Singh ◽  
...  

Biogenic silica (b-SiO2) nanopowders from rice husk ash (RHA) were prepared by chemical method and their bacterial compatibility/toxicity was analyzed. The X-ray diffractometry (XRD) patterns of the b-SiO2 nanopowders indicated an amorphous feature due to the absence of any sharp peaks. Micrographs of the b-SiO2 revealed that sticky RHA synthesized SiO2 nanopowder (S1) had clustered spherical nanoparticles (70 nm diameter), while b-SiO2 nanopowder synthesized from red RHA (S2) and b-SiO2 nanopowder synthesized from brown RHA (S3) were purely spherical (20 nm and 10 nm diameter, respectively). Compared to the S1 (11.36 m2g−1) and S2 (234.93 m2g−1) nanopowders, the S3 nanopowders showed the highest surface area (280.16 m2g−1) due to the small particle size and high porosity. The core level of the X-ray photoelectron spectroscopy (XPS) spectra showed that Si was constituted by two components, Si 2p (102.2 eV) and Si 2s (153.8 eV), while Oxygen 1s was observed at 531.8 eV, confirming the formation of SiO2. The anti-bacterial activity of the b-SiO2 nanopowders was investigated using both gram-positive (Escherichia coli) and gram-negative (Staphylococcus aureus) microorganisms. Compared to S2 and S3 silica nanopowders, S1 demonstrated enhanced antibacterial activity. This study signifies the medical, biomedical, clinical, and biological importance and application of RHA-mediated synthesized b-SiO2.


2019 ◽  
Vol 9 (6) ◽  
pp. 1100 ◽  
Author(s):  
Xiangfeng Guan ◽  
Peihui Luo ◽  
Yunlong Yu ◽  
Xiaoyan Li ◽  
Dagui Chen

In this paper, we prepared mesoporous nickel cobaltite (NiCo2O4) nanostructures with multi-morphologies by simple solvothermal and subsequent heat treatment. By adjusting the solvent type, mesoporous NiCo2O4 nanoparticles, nanorods, nanowires, and microspheres were easily prepared. The as-prepared products were systematically characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Brunauer–Emmett–Teller (BET) method. Furthermore, the catalytic activities towards the thermal decomposition of ammonium perchlorate (AP) of as-prepared NiCo2O4 nanostructures were investigated.


1994 ◽  
Vol 344 ◽  
Author(s):  
T. Sano ◽  
K. Akanuma ◽  
M. Tsuji ◽  
Y. Tamaura

AbstractOxygen-deficient magnetite (ODM; Fe3O4-δ, δ>0) synthesized by reduction of magnetite with H2 at 300°C decomposed CO2 to carbon with an efficiency of nearly 100% at 300°C. In this reaction, two oxygen ions of the CO2 were incorporated into the spinel structure of ODM and carbon was deposited on the surface of ODM with zero valence to form visible particles. The particles of carbon separated from ODM were studied by Raman, energy-dispersive X-ray and wave-dispersive X-ray spectroscopies. The carbon which had been deposited on the ODM was found to be a mixture of graphite and amorphous carbon in at least two levels of crystallization. X-ray photoelectron spectroscopy and X-ray diffraction patterns of the carbon-bearing magnetite (CBM) showed no indication of carbide (Fe3C) or metallic iron (α-Fe) phase formation. In the C 1s XPS spectra of the CBM, no peaks were observed which could be assigned to CO2 or CO. X-ray diffractometry, chemical analysis and TG-MS measurement showed that the carbon-bearing Ni(II)-ferrite (CBNF) (Ni(II)/Fetotal = 0.15) synthesized by the carbon deposition reaction from CO2 with the H2-reduced Ni(II)-ferrite was represented by (Ni0.28Fe2.72O4.00)1-δ (Ni2+06.9Fe2+2.31O3.00)δCτ (δ= 0.27, τ= 0.17). The carbon of the CBNF gave the CIOlayer-like oxide containing some Ni2+ ions.


2015 ◽  
Vol 804 ◽  
pp. 97-103 ◽  
Author(s):  
Panakamon Deeyai ◽  
Thanapong Sareein ◽  
Bundit Putasaeng ◽  
Naphat Chathirat

Bulk Y2NiMnO6 samples were prepared by thermal decomposition technique at 800 °C for 6 hours. The effects of temperature on the structure of ceramics were investigated for different sintering temperatures in the range of 1000-1300 °C, while kept constant the sintering time of 12 hours. Structural characterization had been investigated via X-ray diffraction (XRD) on samples of different sintering temperatures. Results from the experiment had revealed that high temperature affected oxide in ceramic materials. Further analysis with X-ray photoelectron spectroscopy (XPS) technique had revealed an outstanding point of ceramics by investigating the Ni 2p, 2p3/2, Mn 2p1/2, 2p3/2, and Y 3d3/2, 3d5/2 at the surface of Y2NiMnO6 ceramics. The changes in relative intensity of XPS peaks and the shifts in their binding energy (eV) were observed in the results, while the effect of temperature on oxide in ceramics may be investigated with dielectric property in the future.


2012 ◽  
Vol 531-532 ◽  
pp. 512-518 ◽  
Author(s):  
Ye Qing Chen ◽  
Joo Hyun Lee ◽  
Sung Wook Park ◽  
Byung Kee Moon ◽  
Byung Chun Choi ◽  
...  

In this paper, we report a successful synthesis of CaWO4:Eu3+ phosphor via an ethanol assisted hydrothermal process. X-ray diffraction (XRD) patterns, X-ray photoelectron spectroscopy (XPS) and field emission scanning electron microscope (FE-SEM) were used to investigate the growth of the products. The water and ethanol volume ratio is found to have extraordinary effect on the particle size and morphological appearance. Flower like ~ 1µm superstructures can be obtained with mixed solution of w/e of 50/50 at 120 °C hydrothermal sysnthesis for 12 h. High concentration of ethanol in aqueous solution was discovered to have a tendency in limiting the interaction between the small particles for crystallization. Temperature and time experiments were also performed to further investigate the growth mechanism of the ethanol assisted hydrothermal process. The photoluminescence properties of flower like CaWO4:Eu3+ has also been investigated.


Clay Minerals ◽  
2005 ◽  
Vol 40 (1) ◽  
pp. 15-24 ◽  
Author(s):  
S. Ramirez ◽  
D. Righi ◽  
S. Petit

AbstractHydrolytic exchange was performed experimentally on four smectitic clays to evaluate the extent of clay alteration induced by this process and the associated ‘auto-transformation’ of H+ clays. Clay samples were Na-saturated and submitted to 10, 50 and 100 wetting-drying (WD) cycles and characterized after treatment using X-ray diffraction (XRD), infrared spectroscopy (FTIR) and cation exchange capacity analysis. Evidence for hydrolytic exchange was given by increasing amounts of exchangeable Mg2+ and precipitation of Na soluble salts for samples subjected to 100 WD cycles. Results indicated a decrease in the interlayer charge after 10 WD cycles but no further decrease was observed after 50 and 100 WD cycles. For one sample, XRD data indicated a decrease in the proportion of the smectite phase and a relative increase in the concentration of illite-smectite mixed layers also present in the sample. The results suggested that the reaction induces first a decrease in the layer charge and then a partial dissolution of some smectite layers.


2021 ◽  
Vol 4 (3) ◽  
pp. 234-244
Author(s):  
Amelia Olivas Sarabia ◽  
Marlene N Cardoza-Contreras ◽  
Gonzalo Lastra Medina ◽  
Marcos Alan Cota Leal ◽  
Selene Sepúlveda Guzmán

In this work, nanowires and nanorods of WOx have been synthesized by the solvothermal method. The effect of reaction time and acetic acid as solvent were studied. X-ray diffraction (XRD) patterns showed the monoclinic WO2.72, WO2.79, and orthorhombic WO3 crystalline structures. Scanning Electron Microscopy (SEM) and High-Resolution Transmission Electronic Microscopy (HRTEM) images presented nanostructures such as nanowires and nanorods at different sizes. Band gap energies were supplied by Ultra Violet visible (UV-vis) absorption spectra. The Photoluminescence (PL) spectra exhibited three emission peaks in the blue zone at 440, 460, and 484 nm. X-ray Photoelectron Spectroscopy (XPS) was used to calculate W6+, W5+, and W4+ oxidation states. The results showed that increasing the reaction time from 10 h to 24 h affected the crystalline structure from monoclinic to orthorhombic. Moreover, with the addition of acetic acid as solvent, the crystal structure is not affected but stabilizes the monoclinic phase in the course of time.


2019 ◽  
Vol 59 ◽  
pp. 166-179 ◽  
Author(s):  
Betül Gürünlü ◽  
Mahmut Bayramoğlu

Graphene is one of the most promising materials discovered in last years. It is usually synthesized by Hummers’ method requiring the usage of many chemicals. As an alternative to traditional methods, in this study a bottom-up synthesis method was developed from various saccharides such as starch, mannose, cellulose, fructose, arabinose, and xylose by carbonization at 600 °C to 800 °C in LiCl/KCl molten salt system. The proposed method is environmental friendly and economic. Graphene yields at 600 °C are higher than at 800 °C. Graphene products give peak at 2θ = 23° on the X-Ray Diffraction (XRD) patterns. As the temperature is increased, amorph structure is observed on the XRD patterns. Raman spectroscopy results show that intensity of D band peak over intensity of G band peak (ID/IG) values of graphene products synthesized from arabinose and cellulose at 600 °C, graphene from arabinose synthesized at 800 °C are 0.76, 0.65 and 0.85 respectively, which show that these products are few-layered. According to X-ray photoelectron spectroscopy (XPS) results, graphene products synthesized at 600 °C have higher carbon content than those synthesized at 800 °C.


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