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.     

Microwave digestion polarography for determining seven trace elements in Salvia Miltiorrhiza Root and compound Salvia Miltiorrhiza Root injection simultaneously

The sensitive second derivative waves of Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ),Ni(Ⅱ),Zn(Ⅱ),Fe(Ⅱ)and Mn(Ⅱ),forming in the substrate solution(pH=9.26)consisting of ammonia,ammonium chlorid,gelatin and ascorbic acid were researched.The peak potentials of the polarographic waves of the seven ions are at about 0.48,0.63,0.79,1.04,1.28,1.44 and 1.60 V respectively.Combining with microwave technique,a new method for the simultaneous determination of the seven trace elements in Chinese traditional medicine was developed.The method is easy to operate,rapid,simple and convenient.When the signal-to-noise rate equals 3,the detection limits of Cu,Pb,Cd,Ni,Zn,Fe and Mn are 4.2×10 3,5.3×10 3,2.1×10 3,5.8×10 4,3.0×10 3,7.7×10 4 and 1.1×10 3 μg/mL respectively.Well linear relationships exist between the concentrations and the peak currents when Cu,Pb,Cd,Ni,Zn,Fe and Mn concentrations are within 8.5×10 3 10,9.7×10 3 10,4.5×10 3 10,1.2×10 3 10,6.4×10 3 10,1.5×10 3 10 and 2.8×10 3 10 μg/mL,respectively.The method has been used to the simultaneous determination of the seven trace elements in Salvia Miltiorrhiza Root and compound Salvia Miltiorrhiza Root injection,the relative standard deviations(RSDs)of the Cu,Pb,Cd,Ni,Zn,Fe and Mn in the two medicines are 3.9% and 5.8%,4.0% and 4.1%,4.3% and 5.7%,4.9% and 5.3%,4.4% and 4.7%,3.5% and 4.0%,0.51% and 2.8%,respectively;the comparisons of the determination results with the values obtained by the standard method indicate that the presented method has very well veracity.     

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%.     

High Efficieney Synthesis of Isotaetie Polypropylene and Linear Polyethylene Using a New C2-symmetrie Carbon-bridged Zireonoeene Catalyst

Ansa-Cyclohexyl-bis（4,5,6,7-tertrahydro-l-indenyl） zirconium dichloride （5） was used as catalyst for propylene and ethylene polymerization together with methyl aluminoxane （MAO） as the cocatalyst. Isotactic polypropylene （PP） was obtained with the highest activity of 6.37× 107g PP （molZr）^-1h^-1. The mesomeso （mmmmm） pentads sequence content of PP was determined by 13C NMR spectroscopy. The dependence of the microstructure on the reaction temperature and the AI/Zr molar ratio was examined and the catalytic activity of complex 5 was compared with that of the similar ansa-zirconocene 3. The high activity of the new zirconocene 5 for propylene isospectic polymerization at high temperature （60℃） is the result of its unique bridged-group structure. Complex 5/MAO displays also high catalytic activity of 0.46× 10^6 to 9.87× 10^6g PE（molZr）^-h^-in the homo-polymerization of ethylene, The visometric molecular weight of PE ranges from 0.97×10^4 to 11.16×10^4 g.mol^- under the given conditions.^13C NMR spectroscopy analysis proves the PE to be linear polyethylene （LPE）.     

Drag reduction of flow boiling with polymer additives

Ｓｏｍｅｓｔｕｄｉｅｓｗｅｒｅｄｏｎｅｏｎｐｏｏｌｂｏｉｌｉｎｇｈｅａｔｔｒａｎｓｆｅｒｏｆａｄｄｉｔｉｖｅａｑｕｅｏｕｓｓｏｌｕｔｉｏｎ ,ｂｕｔｌｉｔｔｌｅｏｎｆｌｏｗｂｏｉｌｉｎｇ[1 3] .Ｔｈｅｕｓｅｄａｄｄｉｔｉｖｅｓａｒｅｓｕｒｆａｃｔａｎｔａｄｄｉｔｉｖｅｓａｎｄｐｏｌｙｍｅｒａｄｄｉｔｉｖｅｓ[1 4] .Ｉｎｖｅｓｔｉｇａｔｉｏｎｓｏｎｔｈｅｄｒａｇｒｅｄｕｃｔｉｏｎｏｆａｄｄｉｔｉｖｅｓａｒｅｕｓｕａｌｌｙｃｏｎ ｃｅｎｔｒａｔｅｄｏｎｓｉｎｇｌｅｐｈａｓｅｆｌｏｗ[5 ] ,ｏｒｒａｔｈｅｒ,…     

Mechanism of zinc electroplating in alkaline zincate solution

The cathodic deposition properties and mechanism of Zn in alkaline zincate solution were studied by electrochemical techniques. The results show that Zn2 exists in the alkaline solution in the form of Zn(OH)42-. The apparent activation energy of the electrode reaction is 38.93 kJ/mol, which indicates that the discharge of Zn(OH)42- on cathode is controlled by electrochemical polarization, and accompanied by a preceding chemical reaction. The diffusion coefficient of Zn(OH)42- is 2.452×10-6 cm2/s. Zn(OH)2 is the species directly discharged on the cathode surface. Based on the above results the mechanism of zinc electroplating in alkaline zincate solution was put forward. The discharged species is Zn(OH)2 formed from the preceding chemical reaction, which becomes Zn(OH)ad when gaining one electron, and then gaining the second electron to become Zn. The first electron gaining step is rate determining one.     

Characterization and Electrochemical Properties of LiMn2O4 Thin Films Prepared by Solution Deposition

1 IntroductionThin-filmlithium-ion batteries have attracted greatattention of researchfor possible use inimplantable medi-cal devices , CMOS-based integrated circuits ,radio fre-quency (RF) identification tags for inventory control andanti-theft protection[1],etc. Li Mn2O4thin films , aspromising cathode materials for thin-filmlithium-ion bat-teries, have been prepared by a few methods such aspulsedlaser deposition[2 ,3],electrospraying[4-9],RF mag-netron sputtering[10], laser ablation[11]…     

Electrochemical kinetics of gold dissolving in alkaline thiourea solution

1 INTRODUCTIONEssentially , determination of electrode reac-tion mechanism is just the determination of thecourse of electrode reaction and the rate-determi-ning step[1 5]. Based on the previous results[6 11],gold dissolution mechanism undergoes the follow-ing courses in alkaline thiourea solution: adsorp-tion of thiourea on active points of electrode sur-face and formation of Au[SC(NH2)2]ads; chargetransfer fromactive gold atomto thiourea moleculeand formation of Au[SC(NH2)2]a+ds; Au-…     

Electrochemical behaviors of gold and its associated elements in various complex agent solutions

1　INTRODUCTIONGoldisquitestableanddifficulttodissolveinacommonmineralacid .However ,becausethereisadelectroniclayerunfilledingoldatomicstructure ,goldcanbecombinedwithmanychemicalagentstoformstablecomplexions,causingthepotentialofgoldinasolutiontodecreaseandgoldtodissolveinthesolutioneasily .Basedonthisprinciple ,cyanideisanefficientlixiviatingagentofgold ,andhasbeenwidelyusedtoextractgoldfrom primaryandsecondaryresources .However ,itisthemosttoxicandnotbeneficialtoen vironmentprotection…     

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)     

Synthesis and characterization of arsenate antimonic acid AAAc(1 : 1)

The AAAc(1 : 1) was synthesized in water by As₂O₃ and Sb₂O₃ with molar ratio of 1 : 1. AAAc(1 : 1) was characterized by Raman, IR, TG/DTG, DSC, XPS and XRD. The results show that there are four peaks to v _s of As-OH, As-O-Sb, Sb-OH and Sb-O-Sb in Raman spectra of AAAc(1 : 1) at 100 – 1 000 cm⁻¹. The solution of AAAc(1 : 1) was also titrated with KOH solution. The titration results show that AAAc(1 : 1) is a hexabasic acid with dissociation constants of k ₁=3.62 × 10⁻², k ₂=3.05 × 10⁻³, k ₃=6.43 × 10⁻⁶, k ₄ =9.78 × 10⁻⁸, k ₅=1.32 × 10⁻¹¹, k ₆=3.87 × 10⁻¹². AAAc(1 : 1) has a good solubility and stability in water, its solid obtained by free volatilizing water from its solution under air at ambient temperature is amorphous. Chemical and thermal analysis show that the composition of AAAc(1 : 1) is As₂O₅ · Sb₂O₅ · 8H₂O in air at 25 °C. AAAc(1 : 1) has the structure of AsO(OH)₂-OH-Sb(OH)₄-O-Sb(OH)₄-OH-AsO(OH)₂ or As(OH)₃-O-Sb(OH)₄-O-Sb(OH)₄-O-As(OH)₃ (isomerism) through experimental determination and geometry optimization. Foundation item: Project(50274075) supported by the National Natural Science Foundation of China     

Separation of xylo-oligosaccharides from enzymatic hydrolytes using membrane reactor

1　INTRODUCTIONMembranereactorsrepresentapromisingtech nologyforproductionandprocessinginthepharma ceuticalandfoodindustry .Theincreasingattentionto“natural like” productsandenviron mentalpro cessesmakesthemembranereactorsparticularlyat tractive,becausetheydonotrequirechemicaladdi tives ,areabletoworkundermildconditionsofpH ,temperature,and pressure ,andcanreducethefor mationofby products[1] .Thecatalyticactionofen zymesisextremelyefficientandselectivecomparedwithordinarychemicalcatalys…     

Upgrade and separation of Co from solution with low-grade Co

Ｆｉｎｅｌｉｎｎａｅｉｔｅ ,ｕｓｕａｌｌｙｗｉｔｈＣｏｃｏｎｔｅｎｔｆｒｏｍ0 .2 %ｔｏ 0 .3 % ,ｉｓｏｎｅｏｆｔｈｅｉｍｐｏｒｔａｎｔｍａｔｅｒｉａｌｓｕｓｅｄｔｏｕｐｇｒａｄｅＣｏｏｒｅｓ .Ｄｕｅｔｏｌｏｗ ｇｒａｄｅＣｏａｎｄｉｔｓｉｎｔｅｒｇｒｏｗｉｎｇｗｉｔｈｓｅｖｅｒａｌｍａｔｅｒｉａｌｓｓｕｃｈａｓＦｅ ,ＣｕａｎｄＮｉｅｔｃ .,ｉｔｓｕｐｇｒａｄｅａｎｄｓｅｐａｒａｔｉｏｎａｒｅｄｉｆｆｉｃｕｌｔ[1] .ＴｈｅｍｅｔｈｏｄｍａｉｎｌｙｕｓｅｄｉｎＣｈｉｎａａｎｄａｂｒｏａｄｉｓｔｏｒｏａｓ…     

Adsorption of Macroporous Phosphonic Acid Resin for Nickel

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

Synthesis, oxygenation and catalytic performance of manganese complex with p-aminomethyl benzoic acid Schiffbase

The amino acid Schiff base complex (Sal-AMBA-Mn) was prepared with p-amino-methylbenzoic acid, salicylaldehyde and Mn(OAc)2·4H2O. Its structures was characterized with IR and UV spectra. Oxygenation mechanism of the complex in N, N-dimethylformamide solution was investigated. The results show that lower temperature is in favor of the oxygenation, and energy, enthalpy and entropy are -3.8 kJ/mol, -4.2 J/mol and -161.44 J/(mol·K), respectively. In the presence of the manganese complex, dehydroepiandrosterone acetate is effectively oxidized by molecular oxygen and the corresponding enone 7-ketodehydroepiandrosterone acetate is obtained. The yield is 62.1% when the oxidation is carried out under the reaction conditions of 60 ℃, 2 MPa of O2 pressure, C5H5N as a solvent and molar ratio of the substrate to the complex of 1:10.     

Separation of cobalt and nickel by non-equilibrium solvent extraction

Ｓｏｌｖｅｎｔｅｘｔｒａｃｔｉｏｎｉｓｇｅｎｅｒａｌｌｙｂｅｌｉｅｖｅｄｔｏｂｅａｋｉｎｄｏｆｅｑｕｉｌｉｂｒｉｕｍｅｘｔｒａｃｔｉｏｎｏｎｔｈｅｃｏｎｄｉｔｉｏｎｔｈａｔｔｈｅｔｗｏｐｈａｓｅｓａｒｅｍｉｘｅｄｆｏｒｅｎｏｕｇｈｔｉｍｅａｎｄｔｈｅｅｘｔｒａｃｔｉｏｎｐｒｏｃｅｓｓｃａｎｒｅａｃｈｔｈｅｓｔａｔｅｏｆｔｈｅｒ ｍｏｄｙｎａｍｉｃｅｑｕｉｌｉｂｒｉｕｍ .Ｓｏｍｅｔｉｍｅｓ ,ｔｈｉｓｋｉｎｄｏｆｅｑｕｉｌｉｂｒｉｕｍｅｘｔｒａｃｔｉｏｎｃａｎｎｏｔａｃｈｉｅｖｅｓａｔｉｓｆａｃｔｏ…     

On-line Preconcentration of Trace Nickel from Electrolytic Manganese Using Minicolumn Packed Activated Carbon for Electrothermal Atomic Absorption Spectrometry

1　IntroductionElectrolyticmanganeseisanimportantmetallurgicalproductthathasbeenregardedasakindofcombatreadi nessmaterialinseveralcountries[1] .Itisamainindustri alexportproductofXiangxiAutonomousRegionofChina .However,theimpuritycontentintheelectrolyticm…     

Measurement and Analysis of Density of Molten Ni-W Alloys

1IntroductionNi-based heat-resistant superalloys are widely usedto make critical components in gas-turbine engines,suchas bladeetc.But they are very hard and difficult to bemachined,the net-shape machining of these materials isveryimportant.Computer simul…     

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.     

Surface modification of magnesium hydroxide by γ-aminopropyltriethoxysilane

Magnesium hydroxide（MH）,which is commonly used as a halogen-free flame retardant filler in composite materials,was modified by silanization reaction with γ-aminopropyltriethoxysilane （γ-APS） in aqueous solution at different pH values （pH range from 8.0 to 12.0）. The surface properties of grafted γ-APS on MH surface as a function of solution pH value were studied using elemental analysis,Fourier transform infrared spectroscopy and zeta potential measurement. The results show that hydrolysis and condensation of γ-APS are activated in alkaline solution and lead to multilayer adsorption of γ-APS molecules on the surface of MH. The type of adsorption orientation of γ-APS on MH surface is a function of coverage density that is altered by changing solution pH value. At low coverage density （e.g. 55 nm^-2）,γ-APS molecules are preferentially adsorbed to the surface with the silicon moiety towards the surface,and increasing coverage density （e.g. 90 nm^-2） leads to parallel orientation. At an even higher coverage density （e.g. 115 nm^-2）,γ-APS molecules bond to the surface with the amino moiety towards the surface.