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     

New amperometric glucose biosensor by entrapping glucose oxidase into chitosan/nanoporous ZrO2/multiwalled carbon nanotubes nanocomposite film

A new nanocomposite material for construction of glucose biosensor was prepared. The biosensor was formed by entrapping glucose oxidase(Gox) into chitosan/nanoporous ZrO2/multiwalled carbon nanotubes nanocomposite film. In this biosensing thin film, the multiwalled carbon nanotubes can effectively catalyze hydrogen peroxide and nanoporous ZrO2 can enhance the stability of the immobilized enzyme. The resulting biosensor provides a very effective matrix for the immobilization of glucose oxidase and exhibits a wide linear response range from 8 μmol/L to 3 mmol/L with a correlation coefficient of 0.994 for the detection of glucose. And the response time and detection limit of the biosensor are determined to be 6 s and 3.5 μmol/L, respectively. Another attractive characteristic is that the biosensor is inexpensive, stable and reliable.     

Interaction of 4-aminosalicylic acid and surfactants in aqueous solutions using UV-Vis spectra and steady-state fluorescence spectroscopy

The interactions of 4-aminosalicylic acid (4-ASA) and surfactants in aqueous solutions were investigated by using UV-Vis spectra and steady-state fluorescence spectroscopy.The results showed that the strongest peak at UV-vis spectra of 4-ASA aqueous solution in the presence of cationic surfactant and cetyltrimethyl ammonium bromide (CTAB) appeared at 206 nm and took a red shift from 206 nm to 221 nm with the increase of 4-ASA concentrations from 0.8×10-5 to 4.4×10-4 mol/L.Similarly,the strongest peak at UV-vis spectra of 4-ASA aqueous solution in the presence of nonionic surfactant and polyvinylpyrrolidone (PVP) appeared at 206 nm and took a red shift from 206 nm to 219 nm with the increase of 4-ASA concentrations from 0.8×10-5 to 4.4×10-4 mol/L.However,the similar phenomena did not appeared in the presence of anion surfactant,sodium dodecyl sulfate (SDS),the UV-vis spectra of 4-ASA aqueous solution remained the same peak position and the peak value increased with the 4-ASA concentration increase.The results could be attributed to the electrostatic attraction between 4-ASA and CTAB or PVP,as well as the electrostatic repulsion between 4-ASA and SDS.Furthermore,the value of critical micelle concentration (CMC) of surfactants in the presence of 4-ASA was determined with Fluorescence method.The first and second CMC of CTAB was 1.2×10-4 M and 2.4×10-4 M,respectively.The first and second CMC of PVP was 1.2×10-4 M and 2.8×10-4 M.SDS realized the multiple micellizations to form multiple CMC.     

Electrochemical behavior of magnolol on FeWO<Subscript>4</Subscript> nanoflower modified carbon paste electrode

In order to establish a simple, sensitive, and fast reliable detection method to determine the magnolol, FeWO₄ nanoflower was synthesised through a solvothermal technique and FeWO₄ nanoflower modified carbon paste electrode (CPE) was developed. The voltammetric behavior of magnolol on the modified electrodes was studied using cyclic voltammetry (CV), linear sweep voltammetry (LSV), and differential pulse voltammetry (DPV). The experimental results showed that the modified electrode remarkably enhanced the electrochemical response of the magnolol and exhibited a wide linear range for determination of the magnolol from 1.0×10^-7 to 1.0×10^-4 mol/L with a low detection limit of 5.0×10^-8 mol/L.     

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.     

Adsorption of Pb^2＋ on macroporous weak acid adsorbent resin from aqueous solutions： Batch and column studies

The adsorption properties of a novel macroporous weak acid resin (D152) for Pb²⁺ were investigated with chemical methods. The optimal adsorption condition of D152 resin for Pb²⁺ is at pH 6.00 in HAc-NaAc medium. The statically saturated adsorption capacity is 527 mg/g at 298 K. Pb²⁺ adsorbed on D152 resin can be eluted with 0.05 mol/L HCl quantitatively. The adsorption rate constants determined under various temperatures are k _{288 K}=2.22×10⁻⁵ s^t-1, k _{298 K}=2.51×10⁻⁵ s⁻¹, and k _{308 K}= 2.95×10⁻⁵ s⁻¹, respectively. The apparent activation energy, E _a is 10.5 kJ/mol, and the adsorption parameters of thermodynamics are ΔH ^Θ=13.3 kJ/mol, ΔS ^Θ=119 J/(mol·K), and ΔG ^Θ 298 K =−22.2 kJ/mol, respectively. The adsorption behavior of D152 resin for Pb²⁺ follows Langmuir model. Foundation item: Project(2008F70059) supported by the Scientific and Technological Research Planning of Zhejiang Province, China     

A novel quantificational assessment method of frothers effect on bubble characteristics

A new visual method for quantitative measurement of frothers effect and flotation efficiency was presented. A self-designed electrolytic cell was chosen as the reaction environment with sodium chloride (NaCl) as the electrolyte. Constant current, supplied by a self-designed power supplier and fixed cathode and anode equipment, guaranteed the constant bubble volume per unit time. Even aperture of the cathode material guaranteed the original bubbles size to be uniform. Bubble generating equipment was connected with a microscopical camera. Statistic data collected by high speed charge-coupled device (CCD) and processed by software Sigmascan and Matlab could reflect bubble characteristics. The efficiency of dipropylene glycol monomethyl ether (DPM) and tripropylene glycol n-butyl ethel (TPnB) were measured at the same condition, and 2×10⁻⁴ mol/L and 5×10⁻² mol/L were found to be the inflexions of bubble size changes.     

The Optimization of Synthesizing Graft Copolymer of Starch with Vinyl Monomers

1Introduction Thechemicallymodifiedstarchesaregainingin creasingimportanceinapplication,becauseoftheirnatu ralabundance,specialstructureandbiodegradablepr operty[1,2].Graftcopolymerizationisthemostattractive methodforthechemicalmodificationofstarch.Andthe graftcopolymerizationofvinylmonomerssuchasacrylam ide(AM)acrylicacid(AA)ontostarchhasbeencur rentlyanactiveresearcharea[37].Thoughmanyeffortshavebeenmadetoimprovethe waterabsorbencyofthegraftcopolymers,thecombined effectsofdifferentreaction…     

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     

磁性纳米Fe_3O_4颗粒掺杂多壁碳纳米管修饰的葡萄糖生物传感器

磁性纳米Fe3O4颗粒掺杂多壁纳米碳管混合分散于壳聚糖中,得到壳聚糖胶质液.将其修饰到玻碳电极表面,通过交联剂戊二醛固定葡萄糖氧化酶,制得一种新型的传感器.该传感器在pH=6.8的磷酸盐缓冲溶液中,对葡萄糖的线性响应范围为1.0×10^-5-2.3×10^-2mol/L,响应时间5.3 s.     

Study on the isothermal oxidation behavior in air of Ti3AlC2 sintered by hot pressing

The isothermal oxidation behavior at 900–1300°C for 20 h in air of bulk Ti₃AlC₂ with 2.8 wt% TiC sintered by means of hot pressing was investigated in the work. The isothermal oxidation behavior generally followed a parabolic rate law. The parabolic rate constants increased from 1.39×10⁻¹⁰ kg²·m⁻⁴·s⁻¹ at 900°C to 5.56×10⁻⁹ kg²·m⁻⁴·s⁻¹ at 1300°C. The calculated activation energy was 136.45 kJ/mol. It was demonstrated that Ti₃AlC₂ had excellent oxidation resistance due to the continuous, dense and adhesive protect scales consisted of a mass of α-Al₂O₃ and a little of TiO₂ and/or Al₂TiO₅. In principle, the oxide scale was grown by the inward diffusion of O²⁻ and the outward diffusion of Ti⁴⁺ and Al³⁺. The rapid outward diffusion of cations usually resulted in the formation of cracks, gaps, and holes.     

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.     

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.     

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）.     

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.     

Effects of h-BN content on properties of Ni-Cr/h-BN composite

Ni-Cr/h-BN self-lubricating composities were prepared by powder metallurgy (P/M) method. The effects of hexagonal boron nitride (h-BN) content on the mechanical and tribological properties of the Ni-Cr/h-BN composites were investigated. The corresponding frictional models were established to analyze the formation of the lubricant h-BN films on the surfaces of the Ni-Cr/h-BN composites. The results show that, when the content of h-BN increases from 5% to 15% (mass fraction), the bending strength of the Ni-Cr/h-BN composite decreases from 96.670 MPa to 17.319 MPa, and the hardness (HB) decreases from 33 to 14. The friction coefficient of the Ni-Cr/h-BN composite decreases firstly from 0.385 to 0.216, and then increases to 0.284, while the wear rate decreases firstly from 4.14×10⁻⁹ kg/(N·m) to 1.35×10⁻⁹ kg/(N·m), then increases to 2.36×10⁻⁹ kg/(N·m). The best comprehensive mechanical and tribological properties can be obtained between 10% and 12% h-BN addition.     

Synthesis of 1,4-benzenedicarbonyl thiourea resins and their adsorption properties for Ag（I）

Several 1,4-benzenedicarbonyl thiourea resins (BTR) were synthesized through interfacial polymerization between 1,4-benzenedicarbonyl diisothiocyanate and polyamine. Their structures were confirmed by FT-IR. The adsorption properties (including the effect of adsorption time, pH, initial concentrations and temperature) of BTR-1, BTR-2 and BTR-3 for Ag(I) were investigated by batch tests. The results show that the adsorption equilibria of BTR-1, BTR-2, BTR-3 for Ag(I) are achieved after about 10 h. Their equilibrium adsorption capacities are 7.11, 6.75 and 6.23, respectively, and the adsorption process accords with G. E. Boyd equation and Langmuir adsorption isotherm as well. The adsorption capacities increase with the increase of pH (the highest uptake values are observed at pH being about 6–7). The thermodynamic parameters of BTR-1 were calculated. The results show that ΔH ^Θ; and ΔS ^Θ are 6 958.8 J/mol and 64.28 J/(mol·K), respectively, and ΔG ^Θ at 20, 30, 40 and 50 °C are −11.79, −12.52, −13.16 and −13.8 kJ/mol, respectively. The silver-loaded resins can be quantitatively eluted by a solution containing 6% thiourea in 1 mol/L HNO₃.     

Evaluation of protective quality of prestressed concrete containment buildings of nuclear power plants

The permeability and sorptivity properties of the two prestressed concrete containment buildings(PCCBs) of a nuclear power plant in South China,which had been under operation for 5 years,were measured by using the autoclam permeability system.The air permeability,sorptivity and water permeability indexes of No.1 PCCB are smaller than or equal to 0.11 ln(102 Pa)/min,0.98×10-7 m3/min1/2 and 1.93×10-7 m3/min1/2,respectively,and the air permeability,sorptivity and water permeability indexes of No.2 PCCB are sma...     

Electrical conductivity of （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts

The effects of contents of AlF3 and Al2O3, and temperature on electrical conductivity of （Na3AlF6-40%K3AlF6）- AlF3-Al2O3 were studied by continuously varying cell censtant （CVCC） technique. The results show that the conductivities of melts increase with the increase of temperature, but by different extents. Every increasing 10 ℃ results in an increase of 1.85 × 10^-2, 1.86× 10^-2, 1.89 × 10^-2 and 2.20 × 10^-2 S/cm in conductivity for the （Na3AlF6-40%K3AlF6）-AlF3 melts containing 0%, 20%, 24%, and 30% AlF3, respectively. An increase of every 10 ℃ in temperature results an increase about 1.89× 10^-2, 1.94 × 10^-2, 1.95 × 10^-2, 1.99× 10^-2 and 2.10× 10^-2 S/cm for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts containing 0%, 1%, 2%, 3% and 4% Al2O3, respectively. The activation energy of conductance was calculated based on Arrhenius equation. Every increasing 1% of AlF3 results in a decrease of 0.019 and 0.020 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3 melts at 900 and 1 000 ℃, respectively. Every increase of 1% Al2O3 results in a decrease of 0.07 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts. The activation energy of conductance increases with the increase in content of AlF3 and Al2O3.     

Preparation of nano-structured Ag solid materials and application to surface-enhanced Raman scattering

Silver nano-particles with average diameter of about 60 nm were compacted in a high-strength mold under different pressures at 523 K to produce nano-structured Ag solid materials. The structure and characteristic of the nano-structured Ag solid materials (NSS-Ag) were studied using X-ray diffraction (XRD), scanning electron microscope (SEM) and Raman spectrometer. The NSS-Ag could be used as highly efficient surface-enhanced Raman scattering (SERS) active substrates. The common probe molecules Rhodamine 6G (R6G, 1×10⁻¹⁰ mol/L) were used to test the SERS activity on these substrates at very low concentrations. It is found that the SERS enhancement ability is dependent on the density of NSS-Ag. When the relative density of NSS-Ag is 83.87%, the materials reveal great SERS signal.