Simultaneous determination of chromium and manganese in alumina by slurry sampling graphite furnace atomic absorption spectrometry using NbC and NaF as modifiers

This paper reports a method for the direct and simultaneous determination of Cr and Mn in alumina by slurry sampling graphite furnace atomic absorption spectrometry (SiS-SIMAAS) using niobium carbide (NbC) as a graphite platform modifier and sodium fluoride (NaF) as a matrix modifier. 350 mu g of Nb were thermally deposited on the platform surface allowing the formation of NbC (mp 3500 degrees C) to minimize the reaction between aluminium and carbon of the pyrolytic platform, improving the graphite tube lifetime up to 150 heating cycles. A solution of 0.2 mol L(-1) NaF was used as matrix modifier for alumina dissolution as cryolite-based melt, allowing volatilization during pyrolysis step. Masses (c.a. 50 mg) of sample were suspended in 30 ml of 2.0% (v/v) of HNO(3). Slurry was manually homogenized before sampling. Aliquots of 20 mu l of analytical solutions and slurry samples were co-injected into the graphite tube with 20 mu l of the matrix modifier. In the best conditions of the heating program, pyrolysis and atomization temperatures were 1300 degrees C and 2400 degrees C, respectively. A step of 1000 degrees C was optimized allowing the alumina dissolution to form cryolite. The accuracy of the proposed method has been evaluated by the analysis of standard reference materials. The found concentrations presented no statistical differences compared to the certified values at 95% of the confidence level. Limits of detection were 66 ng g(-1) for Cr and 102 ng g(-1) for Mn and the characteristic masses were 10 and 13 pg for Cr and Mn, respectively.

A hybrid material assembled by anthocyanins from acai fruit intercalated between niobium lamellar oxide

Organic-inorganic hybrid materials can be prepared dispersing organic species into well-defined inorganic nanoblocks. This paper describes the immobilization of natural dyes from the extract of the Brazilian acai-fruit into two types of layered hexaniobate precursors derived from H(2)K(2)Nb(6)O(17): (i) colloidal dispersion of niobate exfoliated nanoparticles and (ii) niobate pre-intercalated with tetraethylammonium cations (TEA(+)). The restacking of exfoliated particles in the presence of acai anthocyanins promotes their intercalation and produces stacked layers showing large basal spacing (ca. 50 angstrom). The TEA(+) pre-intercalated niobate provides particles with lower content of dye species than the exfoliated precursor but with higher degree of organization and regularity according to X-ray diffraction data and images obtained by electron microscopies. Vibrational (FTIR and Raman) and (13)C NMR spectroscopies indicate the presence of flavylium cations in the hybrid materials and spectral profiles characteristic of glycosylated anthocyanidins. According to thermal analysis results, the purplish hybrids materials are more stable than the free acai-dyes. One hybrid sample was heated under air up to 170 degrees C and maintained at this temperature for 240 min. No weight loss events were observed and the sample retained its original color, indicating that the intercalation of anthocyanin into hexaniobate increases its thermal stability. Considering the structural, chemical, optical and thermal properties of the synthesized hybrid materials, they might be good candidates to be investigated for future specialized applications.

An investigation of phosphate adsorption from aqueous solution onto hydrous niobium oxide prepared by co-precipitation method

The synthetic hydrous niobium oxide has been used for phosphate removal from the aqueous solutions. The kinetic data correspond very well to the pseudo second-order equation The phosphate removal tended. to increase with a decrease of pH. The equilibrium data describe very well the Langmuir isotherm. The peak appearing at 1050 cm(-1) in IR spectra after adsorption was attributed to the bending vibration of adsorbed phosphate. The adsorption capacities are high, and increased with increasing temperature. The evaluated Delta G degrees and Delta H degrees indicate the spontaneous and endothermic nature of the reactions. The adsorptions occur with increase in entropy (Delta S positive) value suggest increase in randomness at the solid-liquid interface during the adsorption. A phosphate desorbability of approximately 60% was observed with water at pH 12, which indicated a relatively strong bonding between the adsorbed phosphate and the sorptive sites on the surface of the adsorbent. (C) 2008 Elsevier B.V. All rights reserved.

Characterization of nickel-niobium composite electrocoatings

The electrodeposition of nickel based composites is been performed in order to improve properties of nickel layers, such as hardness, wear resistance, lubrication, corrosion resistance and catalytic activity. In the present work Nb powders (20 mu m average size) and Ni were codeposited on 1020 carbon steel by galvanostatic electrolysis of Watts bath, using 10, 20 and 40 mA/cm(2) cathodic current density and 240, 400 and 550 rpm electrolyte stirring rate. The morphology and texture of the coatings, Nb incorporated volume fraction, microhardness, adhesion to the substrate and corrosion behavior were evaluated. The Ni-Nb composite layers presented a rough morphology with randomly oriented Ni grains, whereas pure Ni coatings were smooth and showed highly preferred orientation in the [110] or [100] direction. The volume fraction of Nb in the composites determined by image analysis ranged from 8.5 to 19%. The 400 rpm stirring rate led to the highest Nb content (16 to 19016) for all current densities investigated The microhardness of the composite layers was higher than that of pure Ni coatings due to refining of Ni grains induced by incoporation of Nb particles. The adhesion of the coatings estimated qualitatively by bend test was found satisfactory. The Ni-Nb composites presented lower corrosion rate than Ni coatings in both 3% NaCl and 20% H2SO4 solutions.

Niobium hydrogenation process Effect of temperature and cooling rate from the hydrogenation temperature

High-purity niobium powder can be produced via the hydrogenation and dehydrogenation processes The present work aimed at the effect of temperature and cooling rate conditions on the niobium hydrogenation process using hydrogen gas The hydrogen contents of the materials were evaluated by weight change and chemical analysis X ray diffraction (XRD) was performed to identify and determine the lattice parameters of the formed hydride phases No hydrogenation took place under isothermal conditions only during cooling of the materials Significant hydrogenation occurred in the 500 C and 700 C experiments leading to the formation of a beta NbH(x) single phase material (C) 2010 Elsevier Ltd All rights reserved

Thermodynamic and kinetic investigations of phosphate adsorption onto hydrous niobium oxide prepared by homogeneous solution method

The adsorption kinetics of phosphate onto Nb(2)O(5)center dot nH(2)O was investigated at initial phosphate concentrations 10 and 50 mg L(-1). The kinetic process was described by a pseudo second-order rate model very well. The adsorption thermodynamics was carried out at 298, 308, 318, 328 and 338 K. The positive values of both Delta H and Delta S suggest an endothermic reaction and increase in randomness at the solid-liquid interface during the adsorption. Delta G values obtained were negative indicating a spontaneous adsorption process. The Langmuir model described the data better than the Freundlich isotherm model. The peak appearing at 1050 cm(-1) in IR spectra after adsorption was attributed to the bending vibration of adsorbed phosphate. The effective desorption could be achieved using water at pH 12. (C) 2010 Elsevier B.V. All rights reserved.

Adsorption kinetic, thermodynamic and desorption studies of phosphate onto hydrous niobium oxide prepared by reverse microemulsion method

A type of Nb(2)O(5)center dot 3H(2)O was synthesized and its phosphate removal potential was investigated in this study. The kinetic study, adsorption isotherm, pH effect, thermodynamic study and desorption were examined in batch experiments. The kinetic process was described by a pseudo-second-order rate model very well. The phosphate adsorption tended to increase with a decrease of pH. The adsorption data fitted well to the Langmuir model with which the maximum P adsorption capacity was estimated to be 18.36 mg-Pg(-1). The peak appearing at 1050 cm(-1) in IR spectra after adsorption was attributed to the bending vibration of adsorbed phosphate. The positive values of both Delta H degrees and Delta S degrees suggest an endothermic reaction and increase in randomness at the solid-liquid interface during the adsorption. Delta G degrees values obtained were negative indicating a spontaneous adsorption process. A phosphate desorbability of approximately 68% was observed with water at pH 12, which indicated a relatively strong bonding between the adsorbed phosphate and the sorptive sites on the surface of the adsorbent. The immobilization of phosphate probably occurs by the mechanisms of ion exchange and physicochemical attraction. Due to its high adsorption capacity, this type of hydrous niobium oxide has the potential for application to control phosphorus pollution.

Carbide lime and industrial hydrated lime characterization

This paper focuses on the characterization of carbide lime (CL) - a by-product of acetylene production, composed mainly of calcium hydroxide with minor parts of carbonate - and compares its features to those of ""dry"" hydrated lime (HL) commonly used as a building material. Chemical, thermogravimetric and X-ray diffraction analyses indicated that the limes are similar in chemical and mineralogical compositions. except for the presence of carbon in the waste. Morphological and elemental chemical analyses by SEM and EDS revealed that CL particles differ from HL ones in their morphology and by the presence of carbon formations, Physical characterization included density and BET surface area of the materials. as well as, their particle size distributions in deionized water at diverse time periods. CL underwent agglomeration after approximately 60 min in water, whereas HL progressively became finer with time as determined by laser diffraction. In addition, water retention and squeeze flow tests were used to assess the pastes` fresh properties. (c) 2009 Elsevier B.V. All rights reserved.

Fast and efficient synthesis of pyrano[3,2-c]quinolines catalyzed by niobium(V) chloride

A highly efficient two-step method for the synthesis of pyranoquinoline derivatives from imino-Diels-Alder reactions between aldimines and 3,4-dihydro-2H-pyran using niobium(V) chloride as catalyst under mild conditions is described.

Niobium to alcohol mol ratio control of the concurring esterification and etherification reactions promoted by NbCl5 and Al2O3 catalysts under microwave irradiation

Alcohols and acids can be switched to produce ethers or esters by varying the alcohol to catalyst mol ratio, in a new etherification and esterification method using NbCl5/Al2O3 catalyst under ""solvent free"" conditions and promoted by MW (microwave) irradiation. A ""two sites"" mechanism for the reaction is proposed, in an attempt to clarify the tendency of the catalyst to be dependent on the alcohol alone during the esterification process. (c) 2008 Elsevier B.V. All rights reserved.

Ultrasonic Chemical Vapor Deposition-coated Tip versus High- and Low-speed Carbide Burs for Apicoectomy: Time Required for Resection and Scanning Electron Microscopy Analysis of the Root-end Surfaces

This study compared ultrasonic chemical vapor deposition (CVD)-coated tip (CVDentus #8.1117-1; Clorovale Diamantes Ind. e Com. Ltda Epp, Sao Jose dos Campos, SP, Brazil) versus high-speed (#FG700L) and low-speed (#699) carbide burs for apicoectomy, evaluating the time required for resection and analyzing the root-end surfaces by scanning electron microscopy. Thirty extracted human premolars had the canals instrumented and obturated and were randomly assigned to 3 groups (n = 10), according to the instrument used for root-end resection. The time required for resection of the apical 2 mm of each root was recorded. The resected apical segments were dried, sputter coated with gold, and examined with a scanning electron microscope at X 350 magnification. A four-point (0-3) scoring system was used to evaluate the apical surface smoothness. The results were analyzed statistically by the Kruskal-Wallis test and two-by-two comparisons analyses were performed using the Miller test. The significance level was set at 5%. Root-end resection with the high-speed bur was significantly faster (p < 0.05) compared with the low-speed bur and CVD tip. The carbide burs produced significantly smoother root-end surfaces than the CVD tip (p < 0.05). The low-speed bur produced the smoothest root-end surfaces, whereas the roughest and most irregular root ends (p < 0.05) were obtained with the CVD tip. However, no statistically significant difference (p > 0.05) was found between the high- and low-speed burs regarding the surface roughness of the resected root ends (p > 0.05). In conclusion, under the tested conditions, ultrasonic root-end resection took a longer time and resulted in rougher surfaces compared with the use of carbide burs at both high and low speed. (J Endod 2009;35:265-268)

On-line mass spectrometry of the electro-oxidation of methanol in acidic media on tungsten carbide

The electro-oxidation of methanol at supported tungsten carbide (WC) nanoparticles in sulfuric acid solution was studied using cyclic voltammetry, potentiostatic measurements, and differential electrochemical mass spectroscopy (DEMS). The catalyst was prepared by a sonochemical method and characterized by X-ray diffraction. Over the WC catalyst, the oxidation of methanol (1 M in a sulfuric acid electrolyte) begins at a potential below 0.5 V/RHE during the anodic sweep. During potentiostatic measurements, a maximum current of 0.8 mA mg(-1) was obtained at 0.4 V. Measurements of DEMS showed that the methanol oxidation reaction over tungsten carbide produces CO2 (m/z=44); no methylformate (m/z=60) was detected. These results are discussed in the context of the continued search for alternative materials for the anode catalyst of direct methanol fuel cells.

Influence of sodium hypochlorite and edta on the microtensile bond strength of a self-etching adhesive system

Chemical substances used during biomechanical preparation of root canals can alter the composition of dentin surface and affect the interaction with restorative materials. OBJECTIVE: The purpose of this study was to evaluate the microtensile bond strength (µTBS) of a self-etching adhesive system to dentin irrigated with sodium hypochlorite (NaOCl) and ethylenediaminetetraacetic acid (EDTA). MATERIAL AND METHODS: Thirty human third molars were sectioned 3 mm below the occlusal surface, polished with 600- to 1200-grit silicon carbide papers, and randomly divided into 3 groups: G1 (control): no irrigating solution; G2: 1% NaOCl; and G3: 1% NaOCl followed by the application of 17% EDTA. The specimens received the self-etching adhesive system (XENO III - Dentsply), restored with microhybrid composite resin (Z250 - 3M ESPE), sectioned and trimmed to create 4 hourglass-shaped slabs of each tooth. The slabs were tested in microtensile strength in a universal testing machine (Emic DL 2000) at a crosshead speed of 0.5 mm/min until fracture. The results were analyzed statistically by ANOVA and Newman-Keuls test. RESULTS: Mean µTBS values and standard deviations in MPa were: G1 = 11.89 ± 4.22; G2 = 19.41 ± 5.32; G3 = 11.34 ± 4.73. 1% NaOCl increased the adhesive resistance significantly (p<0.001/F=22.5763). The application of 1% NaOCl/17% EDTA resulted in statistically similar µTBS to the control group. CONCLUSIONS: None of the irrigants affected negatively the µTBS of XENO III to dentin. The use of 1% NaOCl alone resulted in higher bond strength than the other treatments. The combination of 1% NaOCl and 17% EDTA produced similar bond strength to that of untreated dentin.

Influence of Annealing Heat Treatment and Cr, Mg, and Ti Alloying on the Mechanical Properties of High-Silicon Cast Iron

The influence of annealing on the mechanical properties of high-silicon cast iron for three alloys with distinct chromium levels was investigated. Each alloy was melted either with or without the addition of Ti and Mg. These changes in the chemical composition and heat treatment aimed to improve the material's mechanical properties by inhibiting the formation of large columnar crystals, netlike laminae, precipitation of coarse packs of graphite, changing the length and morphology of graphite, and rounding the extremities of the flakes to minimize the stress concentration. For alloys with 0.07 wt.% Cr, the annealing reduced the impact resistance and tensile strength due to an enhanced precipitation of refined carbides and the formation of interdendritic complex nets. Annealing the alloys containing Ti and Mg led to a decrease in the mechanical strength and an increase in the toughness. Alloys containing approximately 2 wt.% Cr achieved better mechanical properties as compared to the original alloy. However, with the addition of Ti and Mg to alloys containing 2% Cr, the chromium carbide formation was inhibited, impairing the mechanical properties. In the third alloy, with 3.5 wt.% of Cr additions, the mechanical strength improved. The annealing promoted a decrease in both hardness and amount of iron and silicon complex carbides. However, it led to a chromium carbide formation, which influenced the mechanical characteristics of the matrix of the studied material.

Production, microstructural characterization and mechanical properties of as-cast Ti-10Mo-xNb alloys

Beta titanium (Ti) alloys are one of the most promising groups of Ti alloys for biomedical applications. This work presents the production, microstructural characterization, and mechanical properties of as-cast Ti-10Mo-xNb (x = 0, 3, 6, 9, 20, and 30) alloys. They were produced via arc melting and characterized by scanning electron microscopy and X-ray diffraction. The density of each alloy was measured by the Archimedes method and the mechanical characterization was carried out by using the Vickers microhardness test and Young`s modulus measurements. The results show a near beta microstructure for niobium (Nb) contents lower or equal to 9 wt% while beta single-phase microstructure was obtained for higher Nb additions. The microhardness values decreased with the increase of Nb content in the alloys. The elastic modulus values of Ti-10Mo-3Nb and Ti-10Mo-20Nb alloys were lower than those of cp Ti and Ti-6Al-4V.