Table of Content

23 November 2005, Volume 21 Issue 6

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Articles

[Ce(H₂ O)₇ Al(OH)₆ Mo₆O₁₈]·4H₂ O: A New One-dimensional Zigzag Chainlike Structure of Anderson Cluster Linked by Cerium Ions

JIN Hua, QI Yan-fei, QIN Chao, WANG Xin-long, WANG En-bo, XU Lin

2005, 21(6):  637-640. 

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A new cerium polyoxomolybdate {[Ce(H₂O)₇Al(OH)₆Mo₆O₁₈]·4H₂O} (compound 1) was synthesized and characterized by X-ray diffraction analysis, elemental analysis, TG analysis and IR spectrometry.Compound 1 exhibits a zigzag chain-like structure, which is constructed from an Anderson type anion and rare earth metal, Ce (Ⅲ).These 1-D chains are further extended into a 3-D network by the aid of multipoint hydrogen-bonding interactions.

Synthesis of Tin Oxide Through Thermal Decomposition of Sn₂ (NH₄)₂ (C₂ O₄)₃ and Its Gas Sensing Property

SHI Juan, WU Shi-hua, WANG Shu-rong

2005, 21(6):  641-645. 

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Nanocrystalline tin oxide samples were prepared by using Sn₂ (NH₄)₂ (C₂O₄)₃ as the precursor.The thermal decompositions were respectively conducted at 250,450 and 650 ℃.TG-DTA, XRD, TEM, FTIR were used to characterize the samples.The indirect heating sensors by using these materials as sensitive bodies were fabricated on an alumina tube with Au electrodes and platinum wires.Sensing properties of these sensors were investigated.It was found that the tin oxide sample obtained by thermal decomposition at 450 ℃ has a higher sensitivity to C₂ H₅ OH and a higher selectivity to hexane and ammonia than those obtained via the conventional precipitate method and the working temperatures needed were greatly decreased.

Controlled Fabrication of Cd-Bi Nanoparticles via Sonochemical Method

CHEN Hong-jie, LI Sheng, LA Zhi-wei, WU Zhi-shen, ZHANG Ping-yu, ZHANG Zhi-jun

2005, 21(6):  646-649. 

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A sonochemical method for the direct controlled synthesis of Cd-Bi nanoparticles from a bulk Cd-Bi alloy is introduced.The nanoparticles were found to be monodispersed and the size distribution can be easily controlled by adjusting the ultrasonic power.The formation and the constituent of the as-prepared Cd-Bi nanoparticles were revealed by means of X-ray diffraction, differential thermal analysis and thermogravimetry, transmission electron microscopy, and electron diffraction.It was found that the Cd-Bi eutectic alloy nanoparticles are made of the hexagonal phase of metal cadmium and the rhombohedral phase of metal bismuth.In addition, we also found through tribological tests that the powder has an excellent antiwear property.

Determination of Vitamin B1 in Pharmaceutical Preparations by Flow-injection Analysis with Biamperometric Detection

LI Li-jun, CHENG Hao, ZHAO Chuan, HU Xiao-ge

2005, 21(6):  650-653. 

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A new electrochemical method for the on-line determination of vitamin B₁ is presented.Based on dead-stop endpoint biamperometry by using two platinum foil electrodes with an applied potential difference of 150 mV, vitamin B₁ can be oxidized by hexacyanoferrate (Ⅲ) in a sodium hydroxide medium via a reversible indicating couple Fe(CN)₆^4-/Fe(CN)₆^3-.The cell current is linear with the concentration of vitamin B₁ in the concentration range of 4.0×10^-6—1.0 × 10^-3 mol/L with a detection limit of 8.0×10^-7 mol/L(0.27 μg/mL).Most familiar excipients,ions and vitamins do not interfere with the determination of vitamin B₁.The method displays the advantages of simplicity, high efficiency(180 samples/h), and high selectivity, and is suitable for the determination of vitamin B₁ in pharmaceutical preparations.

Preliminary Research on Cd²⁺ Removal from Wastewater by Sphaerotilus Natans

QIN Yu-chun, GUAN Xiao-hui, YIN Rong, WANG Li-wen, WEI De-zhou

2005, 21(6):  654-657. 

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Influencing factors, such as the biomass concentration, pH value, tem perature and time of adsorption on the removal of Cd²⁺ were investigated when Sphaerotilus natans was used as a biosorbent.The results show that Sphaerotilus natans has a significant effect on the adsorption of Cd²⁺.The process of adsorption will reach the equilibrium in 20 min.Temperature has no significant effect on the adsorption.The removal rate of Cd²⁺ can approach to 90% under the conditions of pH 5.5, the biomass mass concentration 0.6 g/L and the initial mass concentration of cadmium ≤20 mg/L.The maximum specific uptake is 1.9 mmol/g dry biomass .The adsorption was fitted with the Freundlich isotherm adsorption equation when the concentration of Cd²⁺ is in a range of 0-100 mg/L.HCl and EDTA can desorb Cd²⁺ from biomass effectively.

Analysis of Essential Oils from Flower-buds, Leaves and Stems of Filipendula palmata (Pall.) Maxim.

WU Yin, MENG Xiang-ying, LIU Xiao-hua, BAO Yong-li, WANG Shu-ping, LI Yu-xin

2005, 21(6):  658-662. 

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The essential oils of the flower-buds, leaves and stems of Filipendula palmata (Pall.) Maxim.were analyzed by GC and GC-MS.Thirty-three, forty-seven and forty-seven compounds in the flower-buds, leaves and stems were identified, respectively.Methyl salicylate exists in a great amount which is up to 70.10% in the flower-buds.Its amount is also high in other two parts.The data obtained show that it may be one of the main natural mosquito-expelling and pain-alleviating components in the three parts.The flower-buds are the main active part with the mosquito-expelling function.

Facile Syntheses of New Pyrazolo[1,5-a] pyrimidines Derivatives via Reactions of Enaminones with Aminopyrazole

LI Ming, WANG Shu-wen, WEN Li-rong, KE Zi-qin

2005, 21(6):  663-667. 

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Ethyl 7-aryl-2-benzylthiopyrazolo [1,5-a] pyrimidine-3-carboxylates (3a-3f) were conveniently synthesized through the reactions of enaminones with 5-amino-3-benzylthio-4-ethoxycarbonyl-1H-pyrazole in good yields and high regioselectivity.The structures of the new compounds were fully characterized by spectroscopic measurments, elemental analysis and X-ray diffraction analysis.A plausible reaction mechanism for the formation of the title compounds was also presented.

Preparation and Identification of Angelica sinensis Polysaccharide-iron Complex

WANG Kai-ping, ZHANG Yu, DAI Li-quan

2005, 21(6):  668-672. 

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Angelica sinensis polysaccharide(ASP) was extracted from Angelica sinensis by boiling water.An Angelica sinensis polysaccharide-iron complex(APC) was prepared under the alkaline condition by adding a ferric chloride solution to the ASP solution.Then some identifiable properties of the complex were studied.The content of iron (Ⅲ) in the complex was determined with iodometry.The thermal property, the microscopic structure, the spectral characteristics, and N, C, H contents of the complex were examined by a variety of techniques including DSC, TEM, IR,NMR, and elemental analysis.The content of iron (Ⅲ) in the complex ranges from 10% to 40%.The DSC result shows that the melting point of the complex is about 450 ℃.The TEM result shows that the complex has an iron(Ⅲ)core(β-FeOOH core) linked by hydroxy and oxy bridges, with the polysaccharide chains attached to the surface of the core.The IR and NMR results also show that there is aβ-FeOOH core in the complex.The elemental analysis shows that the contents of N, C, H in the complex are, respectively, lower than those of N, C, H in ASP.All our studies indicate that the APC consists of aβ-FeOOH core surrounded by ASP.

Synthesis, Crystal Structure and Biological Activities of 2-(4-Fluorophenyl)-2-oxo-1-(1H-1, 2,4-triazol-1-yl) ethyl morpholine-4-carbodithioate

XU Liang-zhong, ZHU Chong-yi, YU Chen-long, LI Kai, SI Guo-dong

2005, 21(6):  673-676. 

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The title compound, 2-(4-fluorophenyl)-2-oxo-1-(1H-1, 2,4-triazol-1-yl) ethyl morpholine-4-carbodithioate,was synthesized and its structure was confirmed by means of IR, MS, ¹H NMR and elemental analysis.The single crystal structure of the title compound was determined by X-ray diffraction.The preliminary biological test showed that the synthesized compound possesses some biological activities.

Antibody Phage Library Screening Efficiency Measured by KD Values

WANG Hui-tang, SHAN Ya-ming, TANG Li-li, GAO Li-zeng, WANG Li-ping, LI Wei, LI Yu-xin

2005, 21(6):  677-679. 

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An antibody phage library was screened with two target molecules, IFNα-2a and FGFR-GST, and the KD value of each round of panning was measured.It was found that the apparent KD values decreased along with each additional panning round, which indicates the increase of the binding affinity between the phage and the target molecules.This result shows that the KD value is a reliable intrinsic parameter and a new method for screening efficiency detection is thus provided.

Performance of HZSM-5 as Catalyst for Alkylation of Methyl naphthalene with Methanol in Supercritical Phase

BAI Xue-feng, WU Wei, HU Hao-quan

2005, 21(6):  680-683. 

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The alkylation of methylnaphthalene(MN) with methanol in the presence of HZSM-5 is a promising route for producing 2,6-dimetylnaphthalene(2,6-DMN) with a high selectivity.However, the conversion of MN is very low and the catalyst will be deactivated rapidly with increasing time on stream.In this study, the effects of the reaction pressure on the reactivity, selectivity and life of the catalyst of alkylation of MN over HZSM-5 modified by BaO were investigated.It was observed that with the enhancement of pressure, the conversion of MN increased, but the selectivity of 2,6-DMN kept unchanged, which was about 40%-42%.When the alkylation was carried out under a supercritical condition, the conversion of MN was 3-6 times higher and the life of catalyst was 25-30 times longer than those at an ambient pressure.The thermogravimetric analyses of the deactivated catalysts at different reaction pressures indicate that the amount of coke deposited on the catalysts was about 10% to 12 %, and the coke-burning reactions mainly took place in a temperature range from 720 to 860 K, and the apparent activation energies of the coke-burning catalysts at 0.1 MPa(10 h) and 7.6 MPa(108 h) were, respectively, 65.90 and 84.72 kJ/mol.It is concluded from the results that the supercritical condition is advantageous to enhancing the conversion of alkylation and extraction in situ, and to transporting those high molecular-weight poly-aromatic compounds so as to extend the catalyst life successively.

Catalytic Synthesis of Hexyl-naphthalene over H-type Zeolites

WEI Chang-ping, SUN Xiao-fei, JIANG Xin-hua, ZHEN Kai-ji

2005, 21(6):  684-686. 

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H-type zeolites(HY, Hβ, and HM) were synthesized and characterized by XRD, NH₃-TPD, and Py-IR.Selectively catalytic alkylation of naphthalene with n-hexanol to hexyl-naphthalene over the zeolites was carried out.The experimental results show that the catalytic activities of the zeolites are mainly determined by their acid properties and pore structures.The larger the pore diameter is, the higher the catalytic activity is.NH₃-TPD profiles show that Hβand HM have lower acid strengths than HY.HY has both the highest activity and highest selectivity for the hexylnaphthalene.Higher reaction temperatures and longer reaction time are beneficial to the production of β-hexyl-naphthalene over the HY zeolite.

Determination of Critical Parameters of Carbon Dioxide+ Butyraldehyde System with Different Compositions

ZHANG Jing-chang, GAO Xi-xin, CAO Wei-liang

2005, 21(6):  687-691. 

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Supercritical carbon dioxide(SC-CO₂) is considered in green chemistry as a substitute for conventional solvents in chemical reactions due to its environmentally benign character.Recently we have reported the homogeneous hydroformylation of propylene in supercritical carbon dioxide(SC-CO₂), which is an example of this kind of application of carbon dioxide.The determination for the critical parameters of carbon dioxide + butyraldehyde mixtures is necessary for this reaction design which is the focus of the present paper.The critical parameters of the binary systems were determined via the static visual method at a constant volume with the molar fraction of butyraldehyde ranging from 1.0%to 2.2% and the pressure ranging from 5 to 10 MPa.The experimental results show that the critical pressure and temperature increased with increasing the molar fraction of butyraldehyde.The bubble(dew) temperatures and the bubble (dew) pressures for the binary systems were also determined experimentally.The p-T Figures at different compositions of the binary systems were described.In addition, the critical compressibility factors Z_c of the binary systems at different concentrations of n-butyraldehyde were calculated.It was found that the critical compressibility factor values of the binary systems decreased with increasing the molar fraction of n-butyraldehyde in the experimental range.

Effect Factors in Synthesis of Nicotinic Acid by Electrooxidation of 3-Picoline

SUN Xiu-yun, ZHANG Yu-min, CAO Xue-jing, ZHANG Heng-bin, LI Fei, XU Yu-ling

2005, 21(6):  692-696. 

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In an electrolytic cell with a proton exchange membrane, nicotinic acid was synthesized at the PbO₂ anode.The relationship between the current density and the potential at different concentrations of 3-picoline and sulfuric acid as well as at different temperatures was studied with polarization curves.The effects of the concentrations of sulfuric acid and 3-picoline, the anode potential and the reaction temperature on the selectivity and the current efficiency were explored.The optimum conditions were determined by orthogonal experiments.Under optimum conditions the selectivity and the current efficiency for the synthesis of nicotinic acid might reach 89% and 65%, respectively.The concentrations of 3-picoline and nicotinic acid were analyzed with high performance liquid chromatography and the product was characterized with elemental analysis, chromatography-mass spectrometry and IR spectrometry.

Heat Capacity and Enthalpy of Fusion of Crystalline Pyrimethanil Decylate (C₂₂H₃₃N₃O₂)

SUN Xiao-hong, LIU Yuan-fa, TAN Zhi-cheng, WANG Mei-han, JIA Ying-qi

2005, 21(6):  697-701. 

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Low-temperature heat capacities of pyrimethanil decylate (C₂₂H₃₃N₃O₂) were precisely measured with an automated adiabatic calorimeter over the temperature range from 78 to 373 K.The sample was observed to melt at(311.04 ±0.06) K.The molar enthalpy and entropy of fusion as well as the chemical purity of the compound were determined The extrapolated melting temperature for the absolutely pure compound obtained from fractional melting experiments is (311.204±0.035) K.

Resting Study of Tracer Experiment on Catalytic Wet Oxidation Reactor under Micro-gravity and Earth Gravity Conditions

YANG Ji, JIA Jin-ping

2005, 21(6):  702-706. 

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The International Space Station(ISS) employs catalytic wet oxidation carried out in a Volatile Reactor Assembly (VRA) for water recycling.Previous earth gravity experiments show that the VRA is very effective at removing polar,low molecular weight organics.To compare the reactor performance under micro-gravity and Earth gravity conditions,a tracer study was performed on a space shuttle in 1999 by using 0.2% potassium carbonate as the chemical tracer.In this paper, the experimental data were analyzed and it is indicated that the reactor can be considered as a plug flow one under both micro-gravity and earth gravity experimental conditions.It has also been proved that dispersion is not important in the VRA reactor under the experimental conditions.Tracer retardation was observed in the experiments and it is most likely caused by catalyst adsorption.It is concluded that the following reasons may also have influence on the retardation of mean residence time: (1) the liquid can be held by appurtenances, which will retard the mean residence time; (2) the pores can hold the tracer, which can also retard the mean residence time.

Phase Separation and Transport Behavior in La_0.67-xSm_xSr_0.33MnO₃ System

LIU Ning, YAN Guo-qing, XU Su-jun

2005, 21(6):  707-713. 

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The magnetic behavior and the transport behavior of La_0.67-xSm_xSr_0.33MnO₃ (x=0.00, 0.10, 0.20, 0.30,0.40, 0.50 and 0.60) systems were studied through measuring the M-T curves, electron spin resonance (ESR)curves and ρ-T curves.The samples exhibit a long-range ferromagnetic order when x = 0.00, 0.10, a cluster-spin glass state when x = 0.20 and 0.30, and an anti-ferromagnetic state at low temperatures when x = 0.40, 0.50 and 0.60.The samples of x = 0.30 and 0.40 show phase separation at temperatures above T_c.The transport behavior of the sample of x = 0.60 becomes abnormal when the doping is high, and an insulator-metal transition occurs near T_c and then a metal-insulator transition occurs, which rarely appears in an ABO₃ structure.It is concludedthat the magnetic and electric behavior changes of the systems depend on the extra magnetism and lattice distortion effect induced by Sm doping.

One-pot Synthesis of Dimethyl Carbonate in the Presence of a Two-component Catalyst

CHEN Xiu-zhi, HU Chang-wen, GAO Zhi-ming

2005, 21(6):  714-717. 

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The one-pot synthesis of dimethyl carbonate (DMC) with co-production of propy-lene carbonate(PC) and propylene glycol(PG) from propylene oxide(PO), carbon dioxide and methanol as the starting materials was investigated.The catalyst adopted here was a mixture of tetrabutyl ammonium bromide and sodium methoxide.It was found that under the reaction conditions of t = 150 ℃, p =3-4 MPa and 2 h, the PO conversion could reach 100%, the DMC,PC and the PG selectivities were 49.7%, 42.7% and 49.8%, respectively, and the selectivity of by-products was below 10%.

Effect of Heat Treatment on Structure and Magnetic Performance of Ni-Fe-P Alloy Obtained by Electroless Plating

WANG Sen-lin, ZHANG Yong

2005, 21(6):  718-722. 

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The electroless deposition of Ni₆₈-Fe_10.5-P_21.5 alloy has been investigated.The crystallization behavior of the deposit was comparatively studied by using differential scanning calorimetry and X-ray diffractometry.The deposit transforms into a square Ni3P phase at 380.0 ℃, then changes into a cubic FeNi₃ phase at 490.0 ℃.The microhardness,the size of the formed grains and the magnetic performance of the deposit increase with the increase of the heat treatment temperature below 500 ℃, then they decrease after this temperature.The effect of heat treatment time at 500 ℃on the surface micromorphology, the structure and the magnetic performance of the deposit were also studied.The resuIts show that with the increase of heat treatment time, the extent of crystallization of the deposit increases and the size of the formed grains becomes uniform.The results also show that the magnetic performance of the deposit under heat treatment for 40 min is maximal and then decreases with the increase of heat treatment time.The property change of the deposit is related to the crystal structure and the size of the formed grains of the deposit.

Covalent Immobilization of Lipase on Poly (acrylonitrile-co-maleic acid) Ultrafiltration Hollow Fiber Membrane

YE Peng, XU Zhi-kang, WU Jian, DENG Hong-tao, SETA Patrick

2005, 21(6):  723-727. 

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Lipase from Candida rugosa was covalently immobilized on the surface of an ultrafiltration hollow fiber membrane fabricated from poly (acrylonitrile-co-maleic acid) (PANCMA) in which the carboxyl groups were activated with 1-ethyl-3-(dimethylaminopropyl) carbodiimide hydrochloride (EDC) and dicyclohexyl carbodiimide (DCC)/N-hydroxyl succinimide(NHS), respectively.The properties of the immobilized lipase were assayed and compared with those of the free enzyme.The maximum activities were observed in a relatively broader pH value range at high temperatures for the immobilized lipase compared to the free one.It was also found that the thermal and pH stabilities of lipase were improved upon immobilization and at 50 ℃ the thermal inactivation rate constant values are 2.1×10^-2 for the free lipase, 3.2×10^-3 for the immobilized lipase on the EDC-activated PANCMA membrane and 3.5×10^-3 for the immobilized lipase on the DCC/NHS-activated PANCMA membrane, respectively.

Preparation of CdSe/ZnSe Core-shell Nanocrystal in One-step Reaction

FEI Xiao-fang, SHAN Gui-ye, KONG Xiang-gui, WANG Xin, ZENG Qing-hui, ZHANG You-lin

2005, 21(6):  728-733. 

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High-quality Zn-doped CdSe core-shell nanocrystals were successfully prepared by incorporating a stoichiometric amount of Zn precursor into the CdSe reaction system, in which the Se precursor was excess and an Se-rich surface was formed.By injecting different amounts of Zn precursor, the core-shell nanocrystals demonstrated by the emission spectra were formed.The obtained Zn-doped CdSe nanocrystals exhibit a photoluminescence efficiency from 30% to 85%, which is comparable to those for the reported CdSe/ZnS, CdSe/CdS in the literature.In particular, a shell ZnSe layer with different thicknesses of ZnSe can be formed in this experiment by only changing the amount of Zn precursor added, which is simple and effective.

Studies on Rate Enhancement of Polymerization in NMRP

HUANG Jian-ying, XU Miao-qing, YAN Ming-fa, CHEN Yi-hong, CHU Jia-yan, ZHUANG Jia-ming, DAI Li-zong, ZOU You-si

2005, 21(6):  734-736. 

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In NMRP, the polymerization of MMA, the polymerization of St and the copolymerization of MMA with St were distinctly accelerated by the addition of a small amount of MN.The polymerization proceeds in a living fashion as indicated by the increase in molecular weight with the increase of time and conversion and a relatively low polydispersity.It has been found that the addition of MN results in a nearly one hundred times higher rate of the polymerization of MMA, a nearly twenty times higher rate of the polymerization of St and a nearly fifteen times higher rate of the copolymerization of St and MMA.

Controlled Radical Polymerization of Methyl Methacrylate Catalyzed by Hybrid Supported Iron Catalyst

LI Zhong-hui, ZHANG Yong-ming, XUE Min-zhao, ZHOU Lei, LIU Yan-gang

2005, 21(6):  737-739. 

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A supported iron catalyst, which was prepared by anchoring FeCl₂/FeCl₃ on the cross-linking macroporous polyacrylate ion exchange resin, was evaluated via the controlled radical polymerization.When a small amount of CuCl₂/Me₆TREN was added, the controllability of the polymerization over the iron-mediated catalyst was significantly improved(M_w/M_n=1.23-1.73), affording a polymer with a low residual metal via a simple catalyst separation procedure.After suitable regeneration, the supported iron catalyst could also be recycled.UV-Vis analysis showed that the additional copper catalyst could facilitate the radical deactivation process.

Thermosensitive Particles with Unusual Morphology Prepared by Dispersion Copolymerization

CHEN Ming-qing, YUAN Yan-hua, LIU Xiao-ya, YANG Cheng, KANEKO Tatsuo, AKASHI Mitsuru

2005, 21(6):  740-742. 

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The monodispersed polymeric particles with an unusual structure were prepared by the dispersion copolymerization of acrylonitrile/styrene(AN/St) in mixed solvents of ethanol/water by using the poly(N-isopropylacrylamide)(PNIPAAm) macromonomer as a reaction stabilizer.It was found that the AN monomer plays a key role in the formation of the particles with special morphology analyzed via scanning electron microscopy(SEM).The reaction parameters have remarkable influences on the particle size and morphology.The particles possess a thermosensitive property according to the result of laser light scattering(LLS).

Synthesis and Electrochemical Characterization of Azomethine Containing N-Ethylcarbazole Group

LI Ya-peng, SUN Li-min, SUN Ming-hao, LI Hong-tu, ZHANG Hong-wen, WANG Jing-yuan

2005, 21(6):  743-748. 

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Conjugated aromatic azomethines containing a carbazole group were synthesized.Their structures have been confirmed by IR, MS and UV spectrometries.When iodine was used as the dope to the conjugated compounds, the electrical conductivities (EC) of the doped conjugated compounds were increased by several orders of magnitude.The thermal stability of these two compounds investigated by TGA shows a good result, which guarantees the correct result of EC when the compounds are heated.As can be seen from the CV characterization of the electrochemical properties .of these two compounds, the azomethine diamine and p-aminophenyl-9-ethylcarbazolyl azomethine possess electrochemical activity, which arises from the heteroatom of molecules.

Inclusion Complex of Paclitaxel in Hydroxypropyl-β-cyclodextrin

CHEN Yue, ZHOU Yu-lai, REN Yong, YAN Wei-qun

2005, 21(6):  749-752. 

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Inductively Coupled Plasma(ICP) Mass Spectrometry(MS) Hyphenated with Atomic Emission Spectrometry(AES) for Simultaneous Determination of Major, Minor and Micro Amounts of Elements in Geochemical Samples

HUANG Zhen-yu, ZHANG Qin, HU Ke, WU Jian-ling, YANG Peng-yuan

2005, 21(6):  753-756. 

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Supercritical Fluid Extraction of Saponins from Ginseng

LIU Chun-ming, ZHAO Xue-liang, LI Hong-mei, LIU Zhi-qiang, XING Jun-peng

2005, 21(6):  757-760. 

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Solvent Effect of DMSO-d6 on 1,2-Diols in ¹H NMR

LI Ting-you, JIANG Shui-shi, WANG Zong-mu

2005, 21(6):  761-762. 

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