Preparation and Characterization of Nanotitanium Dioxide Coating Film Doped with Fe^3＋ Ions on Porous Ceramic

The nanotitanium dioxide （TiO2） photocatalytic and porous ceramic filtering technique is one of the advanced methods to effectively treat organic wastewater. The TiO2 sol doped with Fe^3＋ ions was prepared by sol-gel processing. The influences of the process conditions of coating nanophotocatalytic material- Fe^3＋-TiO2 film on the surface of porous ceramic filter by dipping-lift method on the performance of porous ceramic filter were studied. The porous ceramic filters have two functions at the same time, filtration and photocatalytic degradation. The results of this study showed that the pH and viscosity of the sol, amount of Fe^3＋ ions doped as well as the coating times greatly affect the quality of coating film, the performance parameters and the photocatalytic activity of the porous ceramic filter. When the pH of the sol is 3-4, the viscosity is about 6 mPa.S, the amount of doped Fe^3＋ ions is about 2.0 g/L, the porous ceramic filter has been shown to have the best filtering performance and photocatalytic activity. In this condition, the porosity of porous ceramic is about 42.5%, the pore diameter is 8-10μm. The degradation of methyl-orange is 74.76% under lighting for 120 rain.     

Preparation and practical application of spinel pigment Co0.46Zn0.55(Ti0.064Cr0.91)2O4

Synthesis of the green spinel pigment Co_0.46Zn_0.55(Ti_0.064Cr_0.91)₂O₄ by a novel two-step method of preparation have been investigated. Inorganic pigments are almost always prepared by a solid state reaction. It is classical ceramic method which used oxides, hydroxides or carbonates as precursors. The reaction is performed at temperature higher than 1300°C and an agent of mineralization is usually present. The presented novel method of preparation decreases the calcining temperature necessary for reaching of bright and clear hue of the pigments prepared. Main attention was focused on the influence of two types of titanium raw materials on the temperature region of the spinel structure formation and on the colour properties of the pigments. The mixture of precursors with TiO₂ gives a one-phase system when calcining at 1100°C but the colour properties are more interesting at 1150°C. Thermal stability of this pigment is limited by temperature 1300°C. This temperature is connected with partial oxidation of Cr(III) to Cr(VI). Thermal analysis provided the first information about the temperature region of the pigment formation and determined the thermal stability of pigment.     

Modification of carbon ceramic electrode prepared with sol-gel technique by a thin film of chlorogenic acid: application to amperometric detection of NADH

The carbon ceramic electrode prepared with sol-gel technique is modified by a thin film of chlorogenic acid (CGA). By immersing the carbon ceramic electrode in aqueous solution of chlorogenic acid at less than 2 s a thin film of chlorogenic acid adsorbed strongly and irreversibly on the surface of electrode. The cyclic voltammetry of the resulting modified CCE prepared at optimum conditions shows a well-defined stable reversible redox couple due to hydroquinone/quinone system in both acidic and basic solutions. The modified electrode showed excellent electrocatalytic activity toward NADH oxidation and it also showed a high analytical performance for amperometric detection of NADH. The catalytic rate constant of the modified carbon ceramic electrode for the oxidation of NADH is determined by cyclic voltammetry measurement. Under the optimised conditions the calibration curve is linear in the concentration range 1-120 μm. The detection limit (S/N = 3) and sensitivity are 0.2 μM and 25 nA μM⁻¹.The results of six successive measurement-regeneration cycles show relative standard deviations of 2.5% for electrolyte solution containing 1 mM NADH, indicating that the electrode renewal gives a good reproducible and antifouling surface. The advantages of this amperometric detector are: high sensitivity, excellent catalytic activity, short response time t < 2 s, remarkable long-term stability, simplicity of preparation at short time and good reproducibility.     

Preparation, Electrochemical Behavior and Electrocatalytic Activity of a Copper Hexacyanoferrate Modified Ceramic Carbon Electrode

A copper hexacyanoferrate modified ceramic carbon electrode （CuHCF/CCE） had been prepared by two-step sol-gel technique and characterized using electrochemical methods. The resulting modified electrode showed a pair of well-defined surface waves in the potential range of 0.40 to 1.0 V with the formal potential of 0.682 V （vs. SCE） in 0.050 mol·dm^-3 HOAc-NaOAc buffer containing 0.30 mol·dm^-3 KCl. The charge transfer coefficient （a） and charge transfer rate constant （ks） for the modified electrode were calculated. The electrocatalytic activity of this modified electrode to hydrazine was also investigated, and chronoamperometry was exploited to conveniently determine the diffusion coefficient （D） of hydrazine in solution and the catalytic rate constant （kcat）. Finally, hydrazine was determined with amperometry using the resulting modified electrode. The calibration plot for hydrazine determination was linear in 3.0 × 10^-6--7.5 × 10^-4 mol·dm^-3 with the detection limit of 8.0 × 10^-7 molodm^-3. This modified electrode had some advantages over the modified film electrodes constructed by the conventional methods, such as renewable surface, good long-term stability, excellent catalytic activity and short response time to hydrazine.     

Porous ceramic bed supports for fused silica packed capillary columns used in liquid chromatography

Porous ceramic bed supports for fused silica packed capillary columns utilized in liquid chromatography were prepared by polymerizing solutions containing potassium silicate in-situ within a column to create a mechanically stable, rugged, and easily constructed termination. The effect of the bed support length on efficiency, and comparisons to glass wool bed supports, were considered in terms of column efficiencies and hydrodynamic variables. Results obtained indicate better performance for the ceramic bed support.     

Electroanalytical Study of the Composition of the Raw Pigment Mixtures that Yield the Metallic Lustre on Ceramics. A Link Between Composition and Final Result

Voltammetry of immobilized microparticles was used to study the electrochemistry of the raw pigments that produce the metallic lustre on ceramics after a successful firing. To study this influence of the mixture components on the reduction properties to achieve the metallic lustre, 14 mixtures of illitic clay, Fe₂O₃, HgS, CuO and AgNO₃ were prepared and studied in different media. Iron oxide improves the yield of the reduction of the metals and cinnabar helps a closer reduction of silver to copper reduction and prevents the Ag? Cu alloying because of the formation of silver–mercury adducts. The presence of one of the metals influences the peak position of the other metal. The use of vinegar as diluting agent is not casual, because in this media the reduction of silver takes place at a potential closer to the copper. This electroanalytical technique allowed to distinguish between powders of different composition and offered some information about the role of the components in the reduction of copper and silver and the selection of vinegar to prepare the raw pigment suspensions.     

Topical Problems in Elemental Analysis of Advanced Ceramic Materials

Selected prominent problems in the analysis of advanced ceramic materials are surveyed. The importance of reliability of results is discussed in the field of elemental trace- and microanalysis in view of its interaction with economy, power of detection, local resolution and speciation selectivity. Particular problems in the analysis of major constituents, trace components and microlocal distributions are based on the striking propertics of ceramics; they are exemplified. Analytical assistance must start from the beginning of the production processing, in the preparation of the powdered base materials. Determination of the stoichiometry requires high accuracy and differentiation of chemical species in bulk and surface analysis of ceramic base powders. Element trace determination by direct instrumental methods requires standard reference materials for calibration; these are currently inavailable in a sufficient variety. For optimum reliability and power of detection, element traces must be prepared in isolated form in a small excitation volume for analysis. A review on the state-of-the-art of wet-chemical combined procedures is presented. Decomposition position procedures are emphasized, due to their risk of contributing severe systematic error. Combustion in elementary fluorine is presented for decomposition of refractory materials. The performance of some direct procedures is discussed. Very efficient methods are available for element trace determinations in ceramic materials, offering high detection power. Several approaches for high-resolution local microanalysis in non-conductive ceramic materials are identified as the most promising development in the analysis of sintered compact ceramic products and devices.     

Oxidation at a sol-gel composite electrode doped with a dirhodium-substituted polyoxometalate for amperometric detection of peptides separated by HPLC

Oxidation of a variety of compounds, including methionine (Met), using a complex formed between dirhodium(II) acetate and the lacunary form of phosphotungstic acid as the catalyst is effective over a wide range of conditions, including pH 2–10. Thus, amperometric detection at a composite in which this complex is immobilized in a sol–gel material does not place restrictions on selection of conditions for separations by reverse-phase HPLC. A demonstration of this point is shown by a study of Met, Met–Phe, Phe–Met, Met–Met, and Gly–Met–Gly (Phe, phenylalanine; Gly, glycine). Using a 0.05 M phosphate buffer at pH 6.7, a C18 column, and a flow rate of 1 ml min⁻¹, capacity factors for Met, Gly–Met–Gly, Met–Met, and Phe–Met were 1.4, 2.1, 5.6, and 34, respectively. Phe–Met and Met–Phe co-eluted.     

Microporous SiO2 and SiO2/MOx (M=Ti,Zr, Al) for ceramic membrane applications: A microstructural study of the sol-stage and the consolidated state

Microporous SiO₂ and SiO₂/MO₂ (M=Ti, Zr, Al; 10 mol% MO_x) materials for gas separation membrane applications have been prepared from polymeric sols. Characterization of these sols with SAXS showed that the mean fractal dimension of the SiO₂ sols is 1.3–1.4 with a radius of gyration of approximately 2.5 nm. The dried and calcined films are microporous and the pore size distribution was bimodal with maxima at diameters of 0.5 nm and 0.75 nm. For the SiO₂/TiO₂, SiO₂/ZrO₂ and SiO₂/Al₂O₃ systems, much milder reaction conditions proved to be necessary to obtain sols with comparable fractal dimensions due to the high reactivity of the Ti/Zr/Al-alkoxides. Microporous supported membranes with molecular sieve-like gas transport properties can be prepared from a relatively wide range of sol structures: from polymers too small to characterize with SAXS to structures with fractal dimensions: 1<d _f<2.04.