[Ca (2,2′-Bipyridine)3]2+-Intercalated Montmorillonite: An Application as Potentiometric Sensor

2012 ◽  
Vol 428 ◽  
pp. 7-13 ◽  
Author(s):  
S. Payungsak ◽  
Atchana Wongchaisuwat ◽  
Ladda Meesuk
Keyword(s):  
Interlayer Space ◽  
C:N Ratio ◽  
Potentiometric Sensor ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Solid Reaction ◽  
X Ray ◽  
Artificial Graphite ◽  
Higher Sensitivity

This article involves the use of [Ca (2,2′-bipyridine)3]2+-intercalated montmorillonite as a potentiometric sensor to measure anions in aqueous solution. The [Ca (2,2′-bipyridine)3]2+-intercalated montmorillonite was prepared by modification of an in situ solid-solid reaction, between natural Ca (II)-montmorillonite and 2,2′-bipyridine at a molar ratio 1:3. The formation of [Ca (2,2′-bipyridine)3]2+- in the interlayer space of montmorillonite was confirmed by powder X-ray diffraction (XRD) and the existence of 2,2′-bipyridine was confirmed by the C:N ratio of the product compared with that of the 2,2′-bipyridine molecule. The potentiometric sensor was constructed by mixing [Ca (2,2′-bipyridine)3]2+-intercalated montmorillonite with artificial graphite, polytetrafluoroethylene (PTFE) and carboxymethylcellulose (CMC) in an appropriate ratio. It was found that the sensor had higher sensitivity to S2- rather than other anions, graphs of log [S2-] vs voltage (mv) gave a slope 30.0 which was closed to theoretical value, 29.5. Activity of the [Ca (2,2′-bipyridine)3]2+ sensor was verified by using sensor made from Ca (II)-montmorillonite as a reference. Reproducibility and precision of the electrode were also determined.

A Sulfide Ion Sensor from Commercial Bentonite

2014 ◽  
Vol 894 ◽  
pp. 412-415
Author(s):  
Duangsamorn Morawong ◽  
Atchana Wongchaisuwat ◽  
Ladda Meesuk
Keyword(s):  
Interlayer Space ◽  
Intercalation Compound ◽  
X Ray Diffraction ◽  
Solid Reaction ◽  
X Ray ◽  
Sulfide Ion ◽  
Best Response ◽  
Percent Recovery ◽  
Synonymous Term ◽  
Nernstian Slope

Bentonite is a synonymous term of montmorillonite which is a clay mineral consisting of 2 : 1 aluminosilicate layered structure. In this work, a commercial bentonite was used to prepare an intercalation compound [Ca (2,2-bipyridine)3]2+in the interlayer space, by solid-solid reaction, which formation was confirmed by the expansion of the interlayer space of bentonite from 1.5 to 1.8 nm, by powder X-Ray Diffraction technique. The intercalation compound [Ca (2,2-bipyridine)3]2+-bentonite was then used as a sensor to assemble a potentiometric electrode. The electrode gave best response to sulfide ion in terms of Nernstian slope. Precision of measurement, reproducibility and percent recovery were also studied. The electrode could be used to measure sulfide ion in real water samples and gave satisfactory results.

pH-Controlled Assembly of 3D and 2D Zinc-based Metal-Organic Frameworks with Tetrazole Ligands

2017 ◽  
Author(s):  
Felipe Herrera ◽  
Ignacio Chi-Duran ◽  
Javier Enriquez ◽  
Carolina Manquian ◽  
Kerry Wrighton-Araneda ◽  
...  
Keyword(s):  
Structural Diversity ◽  
Molar Ratio ◽  
Aqua Complex ◽  
Initial Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Metal Organic ◽  
Metal Ligand

<div> <div> <div> <p>We report the synthesis and structural diversity of Zn(II) MOF with in situ formation of tetrazole ligand 3-ptz [3-ptz = 5-(3-pyridyl)tetrazolate], as a function pH. By varying the initial reaction pH, we obtain high-quality crystals of the non-centrosymmetric 3D MOF Zn(3-ptz)2, mixed phases involving the zinc-aqua complex [Zn(H2O)4(3-ptz)2]·4H2O, and 2D MOF crystals Zn(OH)(3-ptz) with a tunable micro-rod morphology, keeping reaction time, temperature and metal-ligand molar ratio constants. Structures are characterized by X-ray diffraction, scanning electron microscopy, FTIR and UV-Vis spectroscopy. We discuss the observed structural diversity in terms of the relative abundance of hydroxo-zinc species in solution for different values of pH. </p> </div> </div> </div>

Effects of In-Situ DC-Bias on the Composition, Microstructures and Dielectric Properties of RF Magnetron Reactive Sputtered (Ba,Sr)TiO3 Films

1999 ◽  
Vol 596 ◽  
Author(s):  
Wen-Hao Chan ◽  
Hui-Ling Shen ◽  
Lih-Hsin Chou ◽  
Jinn-Lung Wang ◽  
Jyi-Ching Tsai
Keyword(s):  
Dielectric Constant ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grain Sizes ◽  
Alloy Target ◽  
Bst Films ◽  
Dc Bias ◽  
Diffraction Patterns

AbstractThin films of (Ba,Sr)TiO3 (BST) have been prepared by rf magnetron reactive sputtering using single alloy target, and in-situ negative DC-bias. Post annealing was applied to the asdeposited films at 620°C for 2 hours in 1 atm oxygen atmosphere. Thin film microstructures and grain sizes were studied and calculated by means of X-ray diffraction, while the film composition was analyzed by Electron Probe X-ray Microanalyzer (EPMA). The dielectric constant of the films was also studied. As the applied DC-bias increased, the dielectric constant increased from 176 to 912, the x-ray diffraction patterns became more intense and narrower, and the (Ba+Sr)/Ti molar ratio increased from 0.70 to 0.83. In-situ DC-bias was observed to be a feasible fabrication process to increase the grain size and relative permittivity of sputtered BST films.

Preparation of Composites by In Situ Polimerisation of PET-Hydrotalcite Using Dodecylsulphate

2008 ◽  
Vol 587-588 ◽  
pp. 568-571 ◽  
Author(s):  
S. Martínez-Gallegos ◽  
Maria Herrero ◽  
Vicente Rives
Keyword(s):  
Thermal Stability ◽  
Interlayer Space ◽  
Polymeric Matrix ◽  
Inorganic Component ◽  
X Ray Diffraction ◽  
Tg Analysis ◽  
X Ray ◽  
Thermal Stability Of

A polyethylenterephthalate-hydrotalcite (PET-HT) composite was prepared by in situ polymerisation, using polyethylenterephthalate (PET) and different amounts of a hydrotalcite with dodecylsulphate in the interlayer space (DS-HT). The resulting material has been characterised by powder X-ray diffraction (PXRD) and thermogravimetric (TG) analysis. The thermal stability of PET is not greatly enhanced upon incorporation of the inorganic component, despite PXRD shows that the HT is exfoliated in the composite. Thus with 2-10% shows a complete dispersion of the layered component in the polymeric matrix, while if the inorganic loading is between 20-50 % (larger loadings were not tested) no complete dispersion is achieved and PXRD-detectable agglomerates are formed.

The Characterization and Gas Sensing Properties of Polythiophene Coated V2O5 Nanotubes

2010 ◽  
Vol 654-656 ◽  
pp. 1154-1157 ◽  
Author(s):  
Yu Lu ◽  
Wei Jin ◽  
Wen Chen
Keyword(s):  
Electron Microscopy ◽  
Gas Sensing ◽  
In Situ Polymerization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sensing Properties ◽  
Transmission Electron ◽  
Gas Sensing Properties ◽  
Higher Sensitivity

Polythiophene (PTP) coated V2O5 nanotubes were prepared by an in-situ polymerization of thiophene monomers in the presence of prepared V2O5 nanotubes. The nanotubes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), which proved the polymerization of thiophene monomer and the strong interaction between polythiophene and V2O5 nanotubes (VONTs). The gas sensing properties of PTP coated V2O5 nanotubes were studied at room temperature, which was found that PTP coated V2O5 nanotubes could detect ethanol with much higher sensitivity than pure VONTs. The sensing mechanism of PTP coated V2O5 nanotubes to ethanol is presumed to be the synergetic interaction between polythiophene (PTP) and V2O5 nanotubes.

Synthesis and Electrical Conductivity Measurement of Polyaniline / Vermiculite Nanocomposites

2010 ◽  
Vol 96 ◽  
pp. 221-226
Author(s):  
Hong Juan Sun ◽  
Ying Liu ◽  
Tong Jiang Peng ◽  
Hai Feng Liu ◽  
Jin Mei Sun
Keyword(s):  
Electrical Conductivity ◽  
Interlayer Space ◽  
In Situ Polymerization ◽  
Conductivity Measurement ◽  
Ammonium Bromide ◽  
X Ray Diffraction ◽  
Electrical Conductivity Measurement ◽  
X Ray ◽  
Dimethyl Ammonium

A series of polyaniline/vermiculite nanocomposites was synthesized. The interlayer space of vermiculite was initially increased by the insertion of dioctadecyl dimethyl ammonium bromide, and then the aniline monomers were inserted into the interlayer space of vermiculite replacing dioctadecyl dimethyl ammonium cations. The polyaniline/vermiculite nanocomposites materials were prepared via in situ polymerization of the aniline monomers in the interlayer space of vermiculite. The as-synthesized polyaniline/vermiculite nanocomposite materials were characterized by X-ray diffraction analysis, infrared spectroscopy, and electrical conductivity measurement. The results indicated that the vermiculite was peeled off into the polyaniline. The introduction of vermiculite nanosheets showed a beneficial effect on the electrical conductivity of polyaniline.

In Situ Deposition of CuBiS2 on Mesoporous TiO2 Film for Light Absorber in Solar Cells

2020 ◽  
Vol 20 (12) ◽  
pp. 7748-7752
Author(s):  
Peng-Cheng Wang ◽  
Feng-Zhu Li ◽  
Yu Zhang ◽  
Hao-Chen Fan ◽  
Xue-Qin Zhou ◽  
...  
Keyword(s):  
Energy Gap ◽  
Spectral Absorption ◽  
X Ray Diffraction ◽  
Solid Reaction ◽  
X Ray ◽  
In Situ Deposition ◽  
Light Absorber ◽  
Pure Phase ◽  
First Time

In this report, emplectite (CuBiS2) semiconductor has been deposited on mesoporous TiO2 using gas–solid reaction method. For the first time, CuCl2 and BiCl3 are solution-coated on mesoporous TiO2 films, and thereafter reacted with H2S gas in an H2S atmosphere. The CuBiS2 film is further confirmed using X-ray diffraction; thus, demonstrating the pure phase of CuBiS2. CuBiS2 film shows high spectral absorption with an energy gap (Eg) of 2.18 eV. Furthermore, devices have a structure consisting of FTO/compact-TiO2/mesoporous-TiO2/CuBiS2/P3HT/Ag have been fabricated and hence exhibit high photoresponse performance.

pH-Controlled Assembly of 3D and 2D Zinc-based Metal-Organic Frameworks with Tetrazole Ligands

2017 ◽  
Author(s):  
Felipe Herrera ◽  
Ignacio Chi-Duran ◽  
Javier Enriquez ◽  
Carolina Manquian ◽  
Kerry Wrighton-Araneda ◽  
...  
Keyword(s):  
Structural Diversity ◽  
Molar Ratio ◽  
Aqua Complex ◽  
Initial Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Metal Organic ◽  
Metal Ligand

<div> <div> <div> <p>We report the synthesis and structural diversity of Zn(II) MOF with in situ formation of tetrazole ligand 3-ptz [3-ptz = 5-(3-pyridyl)tetrazolate], as a function pH. By varying the initial reaction pH, we obtain high-quality crystals of the non-centrosymmetric 3D MOF Zn(3-ptz)2, mixed phases involving the zinc-aqua complex [Zn(H2O)4(3-ptz)2]·4H2O, and 2D MOF crystals Zn(OH)(3-ptz) with a tunable micro-rod morphology, keeping reaction time, temperature and metal-ligand molar ratio constants. Structures are characterized by X-ray diffraction, scanning electron microscopy, FTIR and UV-Vis spectroscopy. We discuss the observed structural diversity in terms of the relative abundance of hydroxo-zinc species in solution for different values of pH. </p> </div> </div> </div>

NCO-Chelated organoantimony(III) and organobismuth(III) dichlorides: Syntheses and structures

2010 ◽  
Vol 75 (10) ◽  
pp. 1041-1050 ◽  
Author(s):  
Jan Vrána ◽  
Roman Jambor ◽  
Aleš Růžička ◽  
Jaroslav Holeček ◽  
Libor Dostál
Keyword(s):  
Solid State ◽  
Good Yield ◽  
Solution Nmr ◽  
Molar Ratio ◽  
Organolithium Compound ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chelating Ligand

The novel NCO chelating ligand L, 1-CH2N(CH3)2-3-CH2OCH3-C6H4, was prepared in four steps from commercially available m-tolunitrile in a good yield. Successful lithiation of this ligand was achieved by the reaction with n-BuLi in hexane. Using of this in situ prepared organolithium compound LLi in the reactions with MCl3 (M = Sb, Bi) in 1:1 molar ratio led to isolation of the desired mono-organocompounds MLCl2 (M = Sb (1), Bi (2)). Their structures were studied both in solution (NMR) and in the solid state (X-ray diffraction), and were compared with those of the NCN- and OCO-chelating analogues.

In-situ Synthesis of Zirconium Oxycarbide by Electroreduction of ZrO2/C in Molten Salt

2021 ◽  
Author(s):  
Xianwei Su ◽  
Xiaojia Shang ◽  
Yusi Che ◽  
Shaolong Li ◽  
Jianxun Song ◽  
...  
Keyword(s):  
Molten Salt ◽  
Composite Electrode ◽  
Cell Voltage ◽  
In Situ Synthesis ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lower Molar ◽  
Scanning Electron

Abstract Homogenous ZrCxOy powders have been successfully synthesized by in-situ electro-reduction of solid ZrO2-C composite precursors in molten CaCl2. The effect of applied cell voltage and molar ratio of ZrO2 to C on preparation of ZrCxOy were investigated. The reduction pathway of the composite electrode was studied based on the analysis of intermediate products using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that ZrO2 is firstly converted to CaZrO3. The resulting CaZrO3 is then reduced to ZrCxOy. The ZrCxOy formation is dramatically influenced by electrolysis voltage and molar ratio of ZrO2 to C: a higher cell voltage and lower molar ratio of the ZrO2 to C are more preferable for the formation of ZrCxOy powder. Homogenous ZrCxOy powders with particle size of ~100 nm are synthesized by ZrO2 /C starting elemental powders in CaCl2 molten salt at 1123 K for more than 3 h, when the cell voltage is 3.0 V and the molar ratio of the ZrO2 to carbon starting materials is 1:1.0.

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