Direct and Simultaneous Determination of Several Impurity Elements in Manganese Tetroxide using ICP-AES

1 IntroductionManganic mine resource is Chinese particular re-source,only fewcountries have manganic mine resourceinthe world. Manganese tetroxide whichis made of puremanganese is an important high-tech product that hasbeenregarded as a kind of combat readiness material inseveral countries[1 ,2]. Manganese tetroxide with a highpure and high specific surface area has been ranked inproject of high tech industrialization with preferential de-velopment andsupportinspecial purpose electron material…     

Determination of Trace Selenium in Electrolytic Manganese by Graphite Furnace Atomic Absorption Spectrometry

1　IntroductionBecauseofitsadvantagesofhigh purity ,electrolyticmanganeseismainlyusedinproducingspecialsteel,nonferrousmetalsalloyandasthecrudematerialforpro ducinghighlypuremanganesecarborate ,mangano mana ganicoxide ,electricweldingrodcoatingandartificialdi amondaccelerant.Electrolyticmanganese ,oneofthemostimportantproductsinXiangxiautonomousregion ,isthemainexportproduct.However,thecontentofimpuri tyinelectrolyticmanganeseofXiangxiismuchhigher,whichgreatlyimpairsthequalityoftheproduct .Fo…     

Preparation of magnetic chitosan nanoparticles and immobilization of laccase

The magnetic chitosan nanoparticles were prepared by reversed-phase suspension method using Span-80 as an emulsifier, glutaraldehyde as cross-linking reagent. And the nanoparticles were characterized by TEM, FT-IR and hysteresis loop. The results show that the nanoparticles are spherical and almost superparamagnetic. The laccase was immobilized on nanoparticles by adsorption and subsequently by cross-linking with glutaraldehyde. The immobilization conditions and characterizations of the immobilized laccase were investigated. The optimal immobilization conditions were as follows: 10 mL of phosphate buffer (0.1 M, pH 7.0) containing 50 mg of magnetic chitosan nanoparticles, 1.0 mg · mL⁻1 of laccase and 1% (v/v) glutaraldehyde, immobilization temperature of 4°C and immobilization time of 4 h. The immobilized laccase exhibited an appreciable catalytic capability (480 units · g⁻¹ support) and had good storage stability and operation stability. The K _m of immobilized and free laccase for ABTS were 140.6 and 31.1 μM in phosphate buffer (0.1 M, pH 3.0) at 37 °C, respectively. The immobilized laccase is a good candidate for the research and development of biosensors based on laccase catalysis. Funded by Key Project of National Science Foundation of China (No. 60537050) and the National Science Foundation of China (No. 60377032)     

Novel fluorescence sensor based on covalent immobilization of 3-amino-9-ethylcarbazole via electrostatically assembled gold nanoparticle layer

A novel technique of immobilizing indicator dyes by electrostatic adsorption and covalent bonding to fabricate optical sensors was developed. 3-Amino-9-ethylcarbazole (AEC) was attached to the outmost surface of quartz glass slide via aminosilanizing the slide, crosslinking chitosan, adsorbing Au nanoparticle, self-assembling HS(CH₂)₁₁OH, and coupling AEC. Thus, an AEC-immobilized optical sensor was obtained. The sensor exhibits a wide linear response range from 7.0×10⁻⁷ to 1.0×10⁻⁴ mol/L and a correlation coefficient of 0.995 9 for the detection of 2-nitrophenol. The detection limit and response time of the sensor are 1.0×10⁻⁷ mol/L and less than 10 s, respectively. The fluorescence intensity of the used sensor can be restored to the blank value by simply rinsing with blank buffer. A very effective matrix for immobilizing indicator dye is provided by the proposed technique, which is adaptable to other indicator dyes with amino groups besides AEC. Foundation item: Project(20775010) supported by the National Natural Science Foundation of China; Project(208095) supported by the Key Project of Ministry of Education, China; Project(07A006) supported by the Scientific Research Fund of Hunan Provincial Education Department, China; Project(07JJ3020) supported by Hunan Provincial Natural Science Foundation of China     

Direct rapid determination of traces of sulfide in environment samples

An improved ethylene blue method for determination of sulfide is developed. It has been adapted to a direct determination of sulfide by both common spectrophotometric method and total differential spectrophotometric method. In common spectrophotometric method, the calibration curve is A=1.69ρ+0.006 and the correlation coefficient is 0.9994.The apparent molar absorptivity is 5.42×104 L*mol-1*cm-1 and calibration curve is liner when ρ is in the range of 0-0.9 mg*L-1. In total differential spectrophotometric method, the calibration curve is A=9.25ρ+0.004 and the correlation coefficient is 0.9996. The apparent molar absorptivity is 2.96×105 L*mol-1*cm-1and calibration curve is liner when ρ is in the range of 0-0.10 mg*L-1. The sensitivity of this method is increased significantly compared with the former ethylene blue method. The speed of reaction is also faster than the former one. The limit of detection is found to be 1.0 ng*mL-1 by both common spectrophotometric method and total differential spectrophotometric method. Ten replicate analyses of a sample solution containing 100 ng*mL-1sulfide give a relative standard deviation of 1.8%. The effects of various cations and anions on the determination of sulfide are studied and procedures for removal of interference is described. The method is used for the determination of sulfide in environment samples with satisfactory results.     

High temperature plastic deformation behavior of non-oriented electrical steel

High temperature plastic deformation behavior of non-orientated electrical steel was investigated by Gleeble 1500 thermo-mechanical simulator at strain rate of 0.01−10 s⁻¹ and high temperature of 500–1 200 °C. The stress level factor (a), stress exponent (n), structural factor (A) and activation energy (Q) of high temperature plastic deformation process of non-orientated electrical steel in different temperature ranges were calculated by the Arrhenius model. The results show that, with dynamic elevation of deformation temperature, phase transformation from α-Fe to γ-Fe takes place simultaneously during plastic deformation, dynamic recovery and dynamic recrystallization process, leading to an irregular change of the steady flow stress. For high temperature plastic deformation between 500 and 800°C, the calculated values of a, n, A, and Q are 0.039 0 MPa⁻¹, 7.93, 1.9×10¹⁸ s⁻¹, and 334.8 kJ/mol, respectively, and for high temperature plastic deformation between 1 050 and 1 200 °C, the calculated values of a, n, A, and Q are 0.125 8 MPa⁻¹, 5.29, 1.0×10²⁸ s⁻¹, and 769.9 kJ/mol, respectively. Foundation item: Project(2005038560) supported by the Postdoctoral Foundation of China; Project(05GK1002-2) supported by Key Program of Hunan Province     

Adsorption of Macroporous Phosphonic Acid Resin for Nickel

1Introduction Thesynthesischaracterizationandadsorptionproper tyofpolymericmaterialshavebeenresearchedinrecent years[110].Macroporousphosphonicacidresin[11](PAR)isanovelpolymericmaterialwhichcontainsafunctional groupof[PO(OH)2].Ithasalotofadvantagessuchas…     

Preparation and reaction mechanism of red mud based ceramic simple bricks

In order to utilize solid wastes,ceramic simple bricks with high performances were made from industrial solid wastes such as red mud,fly ash and poor clay shale as main raw materials in this paper.The phase compositions and microstructures were tested by XRD,SEM and EPMA.The experimental results show that the water absorption is 45.64%,the porosity is 58.91%,bulk density is 1.29 g·cm-3,compressive strength is 54.91 MPa,bending strength is 29.52 MPa,freeze-thaw resistance is 29.28 MPa,specific heat capacity at constant pressure is 1.31 J·g-1·K-1,thermal diffusivity is 5.89×10-3 cm2·s-1,and thermal conductivity is 1.15×10-2 W·cm-1·K-1.These effects of additives and preparation process to the properties and microstructures were discussed in detail.The reaction mechanism was also discussed.The results of the reaction mechanism show that there has wollastonite and feldspar generated during the process of firing while Ca gathered around the feldspar,and then Ca would displace K and generated cacoclasite.     

Adsorption of D113 resin for dysprosium(III)

The adsorption behavior and mechanism of D113 resin for Dy(III) was investigated by using the method of resin adsorption. Experimental results show that the optimum medium pH of adsorption of D113 resin for Dy³⁺ is pH=6.00 in the HAc-NaAc medium. The static adsorption capacity of D113 resin for Dy³⁺ is 292.7 mg·g⁻¹. The optimum eluant is 0.5 mol·L⁻¹ HCl. The adsorption rate constant is k ₂₉₈=6.8×10⁻⁶s⁻¹. The apparent activation energy of D113 resin for Dy(III) is 14.79 kJ·mol⁻¹. The adsorption behavior of D113 resin for Dy(III) obeys the Freundlich isotherm. The adsorption parameters of thermodynamic are ΔH=14.48 kJ·mol⁻¹, ΔS=54.69 J·mol⁻¹·K⁻¹, ΔG=−1.82 kJ·mol⁻¹.The adsorption mechanism of D113 resin for Dy³⁺ was confirmed by chemical analysis and IR spectra. Funded by the Natural Science Foundation of Zhejiang Province (No.201027), Foundation of Zhejiang Provincial Education Bureau (No.20040551) and Zhoushan Science Technology Bureau (No.04114)     

Preparation of ITO nano-powders by hydrothermal-calcining process

1 INTRODUCTIONSn-doped In2O3(ITO) is one kind of n-typesemiconductor material[1].It has excellent electro-optical properties , such as electrical conductivityand high transparency under visible light[2],andiswidely used in electronic , transparent electrode ,solar cells and electro-irradiance , especially inscreen display[3 ,4].Recently nearly half of the met-al indium has been used to prepare ITO materialsin the developed countries[5], such as Japan, A-merica ,France and so on.So the…     

Experiments and reaction characteristics of liquid phase simultaneous removal of SO<Subscript>2</Subscript> and NO

Experiments of simultaneous removal of SO₂ and NO from simulated flue gas, using NaClO₂ solution as the absorbent, were carried out in a self-designed bubble reactor, and high simultaneous removal efficiencies of SO₂ and NO were obtained under the optimal experimental conditions. The mechanism of simultaneous removal based on NaClO₂ acid solutions was proposed by analyzing the removal products. Possibility and limitation of the desulfurization and denitrification using NaClO₂ acid solutions were calculated by thermodynamic methods. Experimental results of reaction kinetics for simultaneous desulfurization and denitrification indicated that the oxidation-absorption processes of SO₂ and NO were divided into two zones, namely the fast and slow reaction zones. In the slow reaction zones both were zero order reactions, and in the fast reaction zones, the reaction order, rate constant and activation energy of SO₂ reaction with absorbent were 1.4, 1.22 (mol·L⁻¹)^−0.4·s⁻¹ and 66.25 kJ·mol⁻¹, respectively, and 2, 3.15×10³ (mol·L⁻¹) ⁻¹·s⁻¹, and 42.50 kJ·mol⁻¹ for NO reaction, respectively. Supported by the National High-Tech Research and Development Program of China (“863” Project) (Grant No. 2007AA061803)     

Electrochemical behavior of diverse vanadium ions at modified graphite felt electrode in sulphuric solution

PAN-based graphite felt (PGF) treated in 98% sulphuric acid for 5 h and then kept at 450 ℃ for 2 h was evaluated for their electrochemical performance as electrodes of vanadium redox battery (VRB). Structure and characteristic of treated PAN-based graphite felt (TPGF) were determined by means of Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, Brunauer-Emmett-Teller surface area analysis and VRB test system. The results show that the acid and heat synergistic effect increase the number of —COOH functional groups on the PGF surface, and the PGF is eroded by sulphuric acid oxidation, resulting in the surface area increases from 0.31 m2/g to 0.45 m2/g. The V(Ⅱ)/V(Ⅲ) redox reaction is electrochemically reversible on the TPGF electrode, while the V(Ⅳ)/V(Ⅴ) couple is a quasi reversible process. The diffusion coefficients of the oxidation for V(Ⅳ)/V(Ⅴ) obtained from the scope of peak current Ip vs scan rate v1/2 is 4.4×10-5 cm2/s. The improvement of electrochemical activity for the electrode is mainly ascribed to the increase of the number of —COOH groups on the TPGF, which behaves as active sites catalyzing the vanadium species reactions and accelerating electron transfer reaction and oxygen transfer.     

Sulfonic acid modified hollow silica spheres and its application in proton exchange membranes

In order to improve the proton conductivity of hollow silica spheres (HSS)/perfluorosulfonic acid ion-exchange (PFSA) composite membranes as proton exchange membrane, sulfonic acid groups were grafted onto the surfaces of HSS via post grafting methods. TEM images and FT-IR spectra of the obtained sulfonic acid groups modified hollow silica spheres (SAMHSS) illustrated that the sulfonic acid groups were successfully grafted onto the surfaces of HSS. Water uptake and swelling degree of SAMHSS/PFSA composite membranes were found much higher than those of HSS/PFSA membranes due to the introduction of hydrophilic sulfonic acid groups. In a range from 50 °C to 130 °C, the highest conductivity of composite membranes was obtained when 5 wt% SAMHSS was loaded. The maximum conductivity reached 7.5×10⁻² S·cm⁻¹ at 100 °C and 100% relative humidity, even the temperature increased to 130 °C, the conductivity of composite membranes with 5 wt% SAMHSS could reach 3.7×10⁻² S·cm⁻¹ at 100 % relative humidity, while the conductivity of the recast PFSA was only 2.2×10⁻³ S·cm⁻¹.     

Synthesis of 3D ordered macroporous indium tin oxide using polymer colloidal crystal template

Three-dimensional (3D) ordered macroporous indium tin oxide (ITO) is pre- pared using a polymer colloidal crystal template that is formed by self-assembly of the monodisperse poly(methyl methacrylate) (PMMA) microspheres. The morphologies and BET surface area of the macroporous material is examined by scanning electron micro- scope, transmission electron microscopy and N2 adsorption/desorption. Results indicate that the macroporous material has highly ordered arrays of the uniform pores replicated from the PMMA colloidal crystal template when the polymer colloidal crystal template is removed by calcinations at 500℃. The pore diameter (about 450 nm) of macroporous ITO slightly shrank to the PMMA microspheres. The BET surface area and pore volume of the macroporous material are 389 m2·g-1 and 0.36 cm3·g-1, respectively. Moreover, the macroporous ITO, containing 5 mol% Sn and after annealing under vacuum, shows the minimum resistivity of ρ = 8.2×10-3 Ω· cm. The conductive mechanism of macroporous ITO is discussed, and it is believed that the oxygen vacancies are the major factor for excellent electrical properties.     

Influence of Temperature on Electrochemical Performances of Rare Earth Based Hydrogen Storage Material

1 IntroductionRare earth-based hydrogenstorage alloys ofAB5typehave beenthe most major electrode material for small-sizeNi/MHbatteries because of their high discharge capacity,superior highrate capability andfavorable ratio of pricetoperformance. But their electrochemical performances be-come worse when the alloys are applied to large-size Ni/MHbatteries of electric vehicles .Thisfact may be due tothe rising of temperature inside the large batteries causedbythe high electric current of char…     

Effect of metallic phase species on the corrosion resistance of 17M/（10NiO-NiFe2O4） cermet inert anode of aluminum electrolysis

1 INTRODUCTIONThere are many disadvantages in the presentaluminumelectrolysis with carbon anode ,such assevere energy consumption,carbon wasting,envi-ronmental pollution and so on.Inert electrode sys-tem can overcome these disadvantages[1 3]. Re-cently ,the researches of the inert anode materialshave mainly been concentrated on alloys[4]and cer-met materials[5 ,6]. NiFe2O4based cermets , whichpossess not only high electrical conductivity ofmetal but also good corrosion resistance of cera…     

Simultaneous determination of adenine, uridine and adenosine in cordyceps sinensis and its substitutes by LC／ESI-MS

A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and uridine was developed. The analytical column is a 2.0 mm× 150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is 86.5 %water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0. 062X 0. 005 and 2.0 - 140.0μg · mL 1for adenine, Y=0. 049X 0. 004 and 4. 0 - 115.0 μg · mL-1 for uridine, Y=0. 154X 0. 014 and 1.0 - 125.0 μg · mL 1 for adenosine. The limits of detection are 0.6 μg · mL 1 for adenine, 1.0μg · mL-1 for uri dine and 0.2 μg · mL 1 for adenosine.The recoveries of the three constituents are from 96.6% to 103.2%.     

Strength and elastic properties of sandstone under different testing conditions

A laboratory experimental program performed on Wuhan sandstones was presented under monotonic loading, partial cyclic loading during loading path and sine wave cyclic loading with different strain rates to compare uniaxial compression strength and elastic properties （elastic modulus and Poisson ratio） under different conditions and influence of pore fluid on them. When the loading strain rates are 10^-5, 10^-4 and 10^-3/s, uniaxial compression strengths of dry sandstones are 82.3, 126.6 and 141.6 MPa, respectively, and that of water saturated sandstones are 70.5, 108.3 and 124.1 MPa, respectively. The above results show that the uniaxial compression strength increases with the increase of strain rate, however, variation of softening coefficient is insignificant. Under monotonic loading condition, tangent modulus increases with an increment of stress （strain） to a maximum value at a certain stress level, beyond which it starts to decline. Under the partial cyclic loading during loading path condition, unloading or reloading modulus is larger than loading modulus, and unloading and reloading moduli are almost constants with respect to stress level, especially unloading modulus. Under the sine wave cyclic loading condition, tangent modulus and Poisson ratio display asymmetric ‘X＇ shape with various strain, and the average unloading modulus is larger than the average loading modulus.     

Catalytic wave of cobalt and its analytical application in rapid determination of trace cobalt in complex zinc electrolyte solution

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Spectra and DNA-binding properties of two novel mixed-ligand complexes containing organosulfonate

Two novel mixed-ligand complexes, [M(phen)₂(ans)₂]·H₂O (M = Cd(II) 1, Zn(II) 2; phen is 1, 10-phenanthroline, and ans is 4-aminonaphthalene-1-sulfonate), were obtained from the reaction of 1, 10-phenanthroline, sodium 4-aminonaphthalene-1-sulfonate tetrahydrate and acetate in mixed solvents. Interaction of the complexes with calf thymus DNA (ctDNA) were investigated using UV-vis absorption spectra, luminescence titrations, steady-state emission quenching by [Fe(CN)₆]⁴⁻, DNA competitive binding with ethidium bromide (EB) and viscosity measurements. The experimental results indicate that there exist two interaction modes between the complexes and DNA, namely the electrostatic interaction and intercalation, with the binding constants of 1.82 × 10⁵ M⁻¹ for 1 and 4.78 × 10⁴ M⁻¹ for 2 in buffer of 50 mM NaCl and 5 mM Tris-HCl (pH 7.0). Funded by Key Project of the National Natural Science Foundation of China (No. 60537050)