Micellar sensitized catalytic kinetic spectrophotometry for highly accurate and reproducible determination of Ⅴ(Ⅳ) and Ⅴ(Ⅴ)

A highly accurate and reproducible micellar sensitized kinetic method was proposed for determination of V(VI). The method is based on its catalytic effect on the oxidation of Coomassie brilliant blue R 250(CBB?) by bromate at pH 2.0. The reaction was monitored spectrophotometrically by measuring absorbance change with a fixed-time method of 5 min at 594 and 552 nm with and without surfactant. The variables influencing the calibration sensitivity were extensively investigated, and the optimal conditions were established. The linear calibration range was 10–1,600 lg L-1with a relative SD ranging from 0.35 % to 3.35 %(for five replicate measurements of75, 500, 1,000, and 1,500 lg L-1) and a detection limit of3.8 lg L-1. The selectivity was also investigated, and greatly enhanced by suitable masking agents. The method was successfully applied to the analysis of V(IV) in presence of excess V(V) up to 25 fold in environmental waters with the recoveries of 100.0 %–102.8 % for V(IV) and95.7 %–99.7 % for total V. Its accuracy was validated by analysis of certified reference material via the present kinetic method and standard flame atomic absorption spectrometric method after extractive preconcentration with good agreement between certified and found values.     

Solid-phase extraction of trace Au（Ⅲ） with SDG and determination by the catalytic spectrophotometric method

The new catalytic kinetic spectrophotometric method for Au(III) determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate ((NH4)2S2O8) with nitrilo triacetic acid as an activator in mi- croemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au(III) at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel (SDG) as a solid-phase extractant has been developed for the preconcentration and separation of Au(III) ions. The method has been applied to the determination of trace gold with satisfactory results.     

Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide (TiO2) as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry (CVAAS). Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg2 on the dithizone-modified nanoparticles was investigated in detail. It was found that excellent adsorption ratio for Hg2 could be obtained in the pH range of 7-8 with an oscillation time of 15 min, and a 5 mL of 3.5 mol·L-1 HCl solution could quantitatively elute Hg2 from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit (3σ) for Hg2 was calculated to be 5 ng·L-1. The proposed method was applied to the determination of Hg2 in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD (n = 5) of 2.9%-3.5%.     

Thermal decomposition kinetics and lifetime of the complex of Tb2（BA）6（PHEN）2

The thermal behavior of Tb2(BA)6(PHEN)2 (BA: benzoate, and PHEN: 1,10-phenanthroline) in a static air atmospbere was investigated by TG-DTG, SEM and IR techniques. By the kinetic method of processing thermal analysis data put forward by Malek et al., it is defined that the kinetic model for the first-step thermal decomposition is SB(m, n). The activation energy E for this step reaction is 99.07 kJ/mol, the entropy of activation ΔS^≠ is -84.72 J/mol, the enthalpy of activation ΔH^≠ is 94.26 kJ/mol, the free energy of activation ΔG^≠ is 144.77 kJ/mol and the pre-exponential factor lnA is 20.93.The lifetime equation at mass-loss of 10% was deduced as lnτ = -29.0312 19760.83/T by isothermal thermogravimetric analysis.     

Solid-phase extraction of trace Au(Ⅲ) with SDG and determination by the catalytic spectrophotometric method

The new catalytic kinetic spectrophotometric method for Au(Ⅲ) determination was developed and validated.It was based on the catalytic effect of gold on the oxidation of sudan red Ⅲ by ammonium peroxodisulfate ((NH4)2S2O8) with nitrilo triaeetic acid as an activator in microemulsion and H2SO4 medium.Under optimum conditions,there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au(Ⅲ) at 520 nm.The relative standard deviation was 3.0% with a correlation coefficient of 0.9986.The detection limit achieved was 9.75×10-5 μg/mL.A new method using a column packed with sulfhydryl dextrose gel (SDG) as a solid-phase extraetant has been developed for the preeoncentration and separation of Au(Ⅲ) ions.The method has been applied to the determination of trace gold with satisfactory results.     

Catalytic spectrophotometric determination of trace vanadium in fly ash and coal gangue by Triton X-100 enhancing effect

Trace V(V) catalyzes mightily the decolorization reaction of arsenazo Ⅲ(AsA Ⅲ) by oxidizing with H2O2 in a pH 4.0 HAc-NaAc buffer solution, and the addition of Triton X-100 can further increase the sensitivity of the reaction and its catalytic extent is linear with the content of V(V). A catalytic spectrophotometric procedure for determining trace V(V)was developed. The results show that the maximun absorption of the color solution is at 560 nm and the detection limit of the method for V(V) is 0.014 mg.L-1. Beer's law is obeyed for V(V) in the range of 0.00-0.20 mg.L-1. The recoveries are 99.0%-104.6%, and the relative standard deviations (RSD) are 2.7%-3.7%. Combined with ion-exchange resin, the method has been applied to the determination of trace vanadium in fly ash and coal gangue with satisfactory results.     

Catalytic-kinetic spectrophotometric determination of vanadium （V） based on the Celestine blue-bromate-vanadium （V）-citric acid reaction

A novel sensitive and relatively selective kinetic method is presented for the determination of V(V) based on its catalytic effect on the oxidation reaction of Celestine blue by potassium bromate in the presence of citric acid as an activator.The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of Celestine blue at a maximum absorption wavelength of 540 nm between 0.5 and 9 min(the fixed-time method) in an H3PO4 medium at 45°C.The effect of various parameters such as con...     

Processing and mechanical properties of porous 316L stainless steel for biomedical applications

Highly porous 316L stainless steel parts were produced by using a powder metallurgy process, which includes the selective laser sintering（SLS） and traditional sintering. Porous 316L stainless steel suitable for medical applications was successfully fabricated in the porosity range of 40%-50% （volume fraction） by controlling the SLS parameters and sintering behaviour. The porosity of the sintered compacts was investigated as a function of the SLS parameters and the furnace cycle. Compressive stress and elastic modulus of the 316L stainless steel material were determined. The compressive strength was found to be ranging from 21 to 32 MPa and corresponding elastic modulus ranging from 26 to 43 GPa. The present parts are promising for biomedical applications since the optimal porosity of implant materials for ingrowths of new-bone tissues is in the range of 20%-59% （volume fraction） and mechanical properties are matching with human bone.     

Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities in high-purity sodium tungstate. Six elements(Co,Cu,Fe,Mn,Ni,and Pb) were coprecipitated by lanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of some factors on the recoveries of the analytes and on the residual amount of sodium tungstate were investigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matching calibration curve method was used for the analysis. It is shown that the elements mentioned above can be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4, 0.2, 0.1, 0.6, and 1.3 μg.g^-1, respectively. The recoveries vary from 92.5% to 108%, and the relative standard deviations (RSDs) are in the range of 3.1%-5.5%.     

A novel indicator system for catalytic spectrophotometric determination and speciation of inorganic selenium species (Se(Ⅳ), Se(Ⅵ)) at trace levels in natural lake and river water samples

A novel catalytic kinetic method is proposed for the determination of Se(Ⅳ), Se(Ⅵ), and total inorganic selenium in water based on the catalytic effect of Se(Ⅳ) on the reduction of Celestine blue by sodium sulfide at pH 7.0 phosphate buffer. The fixed-time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the two calibration graphs are linear with a good correlation coefficient in the range 2-20 and 20-200 μg·L-1 of Se(Ⅳ) for the fixed-time method a...     

Influence of hydrogenation on microstructures and microhardness of Ti6A14V alloy

The microstructures of Ti6A14V alloy after hydrogenation were investigated by optical microscopy（OM）, X-ray diffraction（XRD） and transmission electron microscopy（TEM）. The influence of hydrogenation on the hardness of α and β phases was analysed by microhardness testing. The influence of hydrogenation on alloying elements diffusion was studied by electron probe microanalysis（EPMA）. The microstructural observation reveals that hydride δ （FCC structure） as well as large number of dislocations precipitate in the specimens with 0.278% and 0.514% hydrogen, and a lot of twins are found in the specimen with 0.514% hydrogen, simultaneously. The result of microhardness testing shows that the hardness of a and β phases increases synchronously with the increase of hydrogen and the hardness increment of β is larger than that of a. According to analysis of EPMA, the diffusion ability of alloy elements Al and V increases after hydrogenation. It is considered that hydrogen solution strengthening and V element diffusion are the main factors causing the hardness of a phase increase with the increase of hydrogen, and the formation of δ hydrides, lattice defects, hydrogen solution strengthening and Al element diffusion jointly cause the hardness of β phase increase with the increasing hydrogen.     

Purification mechanism of copper electrolyte by As（Ⅲ）

A new kind of precipitate, antimony arsantimonate, was found during the precipitation reactions in acidic solution containing As（Ⅲ）, Sb（Ⅲ） and Sb（ Ⅴ ） by means of chemical analysis, SEM, XRD and IR spectrometry. The results show that the As content in antimony arsantimonate increases with the increase of n（As（Ⅲ）/n（Sb） in solution and the content of component Sb（Ⅲ） and Sb（Ⅴ） remains almost constant with the variation of n（Sb（Ⅲ））/n（Sb（Ⅴ）） in solution. The antimony arsantimonate is a kind of floccules with size of 1-5 μm. The crystal performance of the compound gets better with the decrease of n（As（Ⅲ））/n（Sb）, the cell parameter of which is near to 10.33×10^-10m under different n（As（Ⅲ））/n（Sb） and As atom locates on the surface, not in the inner of the grain. The chemical bonds of As--OH, Sb---OH, As---O--Sb, Sb--O---Sb and O---H of the precipitate are included in the precipitate. The chemical structure of precipitate is described as Sb（OH）2---O--[Sb（OH）3--（O---As（OH）--O---Sb（OH）3）3]----O--- Sb（OH）2·xH2O. The structure analysis shows that the copper electrolyte can be purified by As（Ⅲ） because the antimony arsantimonate precipitate forms.     

Adsorption behavior of gel-type weak acid resin （110-H） for Pb^2＋

The adsorption properties of a novel gel-type weak acid resin （110-H） for Pb^2＋ were investigated using chemical methods and IR spectrometry. The optimal adsorption condition of 110-H for Pb^2＋ is at pH=6.49 in HAc-NaAc medium and the statically saturated adsorption capacity is 485 mg/g at 298 K. Pb^2＋ adsorbed on 110-H resin can be eluted with 0.025 mol/L HCl quantificationally. The adsorption rate constants determined under the temperatures of 288, 298, 308 and 318 K are 2.46×10^-5, 3.82×10^-5, 4.46×10^-5 and 5.71×10^-5 s^-1, respectively. The apparent activation energy, Ea, is 18.1 kJ/mol and the thermodynamic parameters of adsorption, △H=20.9 kJ/mol, △S=-161 J/（mol·K） and △G298 K =-48.0 kJ/mol, respectively. The adsorption behavior of 110-H resin for Pb^2＋ accords with the Langmuir isotherm. Infrared spectra show that the oxygen atoms of the functional group of resin coordinate with Pb^2＋ to form the coordination bands.     

Effect of Isothermal Temperature on Microstructure and Mechanical Properties of High AI-Low Si TRIP Steel

In this study, the effect of isothermal temperature on microstructure and mechanical properties of a high Al-low Si TRIP steel was investigated using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, electron back scattered diffraction, and tensile test. The results show that typical microstructure containing ferrite, bainite, and retained austenite can be obtained when two-stage heat treatment process was utilized. When annealing temperature is 840 ℃ and austempering temperature is 400 ℃, the tensile strength is 542 MPa and the product of strength and elongation is 17,685 MPa%. The morphologies and stability of the retained austenite in low silicon/high aluminum TRIP steel were finally discussed.     

Microstructure and Properties of In Situ Si and Fe-rich Particles Reinforced AI Matrix Composites Assisted with Ultrasonic Vibration

In this research, the in situ Si and Fe-rich particles reinforced Al matrix composites were fabricated by rheocasting （RC） process assisted with ultrasonic vibration （USV）. After USV treatment, the polygonal primary Si crystals were refined into particles with average diameter of about 15-23 μm, and the fraction of primary Si declined to about 5.4-6.5 vol%. The coarse plate-like δ-Al4（Fe,Mn）Si2 phase was transformed into fine particles with average diameter of about 17-20 μm, and the fraction of particle-like Fe-bearing particles is about 3.6-5.3 vol%. The ultimate tensile strength of the RC composites increases with the increase of Fe content at 350 ℃. The increase of the elevated temperature strength of the composites is mainly attributed to the refinement of δ-Al4（（Fe,Mn）Si2 phase and the increase of the volume fraction of the Fe-bearing compounds. Compared with the composites without USV, the RC composites assisted with USV have thinner mechanical mixing layer in wear test, which corresponds to smaller wear rate.     

Microstructure and properties of 7A52 A1 alloy welded joint

7A52 A1 alloy plate aged at 105℃ for 8 h and then at 130℃ for 24 h was welded by means of TIG using A1- 6.3Mg-0.35Sc-0.1Zr-0.1Cr solder wire. Mechanical properties and microstructures of welded joint were studied. There are two obviously soft areas in the welded joint, welding seam and over-aging zone. The mechanical properties of welded joint are that σb is 358 MPa, σ0.2 is 238 MPa and δ5 is 6.6%. 75.6% of welding coefficient can be achieved. The addition of scandium leads to very significant grain refinement in the fusion zone, which results in a reduction in solidification cracking tendency. The solidification cracking isn＇t observed.     

Microstructure and Mechanical Ultra-High Strength Hot-Rolled Refuge Chamber Properties of 1,000 MPa Plate Steel for Coal Mine

The 1,000 MPa ultra-high strength hot-rolled plate steel with low-carbon bainitic microstructure was developed in the laboratory for coal mine refuge chamber. The static recrystallization behavior, microstructure evolution, and mechanical properties of this hot-rolled plate steel were investigated by the hot compression, continuous cooling trans- formation, and tensile deformation test. The results show that the developed steel has excellent mechanical properties at both room and elevated temperature, and its microstructure mainly consists of lath bainite, granular bainite, and ferrite after thermal-mechanical control process （TMCP）. The ultra-high strength plate steel is obtained by the TMCP process in hot rolling, strengthened by bainitic transformation, microstructure refinement, and precipitation of alloying elements such as Nb, Ti, Mo, and Cu. The experimental steel has relatively low welding crack sensitivity index and high atmospheric corrosion resistance index. Therefore, the developed steel has a good balance of strength and ductility both at room and elevated temperature, weldability and corrosion resistance, and it can suffice for the basic demands for materials in the manufacture of coal mine refuge chamber.     

Shape Memory Alloy-Reinforced Metal-Matrix Composites:A Review

Metal-matrix composites reinforced with shape memory alloys(SMA, including long fiber, short fiber, and particle) are ‘‘intelligent materials' ' with many special physical and mechanical properties, such as high damping property,high tensile strength, and fatigue resistance. In this review article, the fabrication method, microstructure, interface reaction, modeling, and physical and mechanical properties of the composites are addressed. Particular emphasis has been given to(a) fabrication and microstructure of aluminum matrix composites reinforced with SMAs, and(b) shape memory effect on the physical and mechanical properties of the composites. While the bulk of the information is related to aluminum matrix composites, important results are now available for other metal-matrix composites.     

Pulse-plating electrodeposition and annealing treatment of CulnSe2 films

CuInSe2 （CIS） thin film was prepared on molybdenum substrate using pulse-plating electrodeposition in aqueous solution. The most suitable pulse potential range for co-deposition is found to be from -0.55 to -0.75 V （vs SCE） from linear potential scanning curve. The electrodeposited films were characterized by X-ray diffractometry （XRD）, scanning electron microscopy（SEM） and energy dispersive X-ray analysis （EDS）. The annealing effects on electrodeposited precursors were investigated. And the influence of pulse parameters on film quality was studied. The chalcopyrite phase CulnSe2 films with smooth surface and stoichiometric composition are obtained at a pulse potential from -0.65 to -0.7 V （vs SCE）, a pulse period of 1-9 ms with a duty cycle of 33% and annealing treatment.