Table of Content

10 May 2011, Volume 32 Issue 5

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Contents

Cover and Content of Chemical Journal of Chinese Universities Vol.32 No.5(2011)

2011, 32(5):  0. 

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Review

Developments in Microfluidics-based Immunoassays

CHEN Zhao-Na, LIU Bao-Hong, WU Hui-Ling*, YANG Peng-Yuan*

2011, 32(5):  1001-1007. 

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Microfluidics\|based immunoassays have become an increasing research field in recent years owing to their advantages of miniaturization, high throughput, fast detection and low consumption. Detection is an important part in microfluidics-based immunoassays. Recent advances in the studies of micro-systems and detection methods, including electrochemical detection, fluorescence spectrometry, ultraviolet\|visible spectrometry, chemiluminescence and bioluminescence, surface-enhanced Raman scattering, fiber-optic sensor, surface plasmon resonance, thermal lens microscopy, colorimetry and other new detection methods applied in microfluidics-based immunoassays, were summarized and reviewed in this paper. The prospects of the detection methods for microfluidics-based immunoassays were presented.



Letters

A Novel Interfacial Potential Sensor

NIE Fu-Qiang, GAO Yi, SUN Jie-Juan, GUO Xiao-Xia, GAO Wei, SONG Jun-Feng*

2011, 32(5):  1008-1009. 

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A novel electrochemically interfacial potential sensor was developed. The setup of the sensor was to connect a conducting material between two clips of working and count electrodes of a three-electrode potentiostat to be Ohmic circuit. Experimental procedure included immersing the conducting material in aqueous solution containing some species of interest, applying a linear sweep potential(with respect of reference electrode) to the conducting material and recording the I-E curve. Owing to the distribution, adsorption, reaction and others of the species at the conducting material-solution interface, interfacial potential changed and offseted applied potential partially, resulted in the shift of the recorded I-E curve along potential axis. The shift of the I-E curve was marked with so-called zero current potential where circuit current is zero in the I-E curve. With the dependence of zero current potential on interfacial potential in various interfacial conditions, the sensor has wide application field not only in the study of interfacial phenomena but also in the analytical determination.



Letter

Galactose Substituted Phthalocyanines for Tumor Imaging as Near-infrared Fluorescence Probe

Lü Feng, LI Yan-Zhou, WU Li, LIU Tian-Jun*

2011, 32(5):  1010-1012. 

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Abstract Phthalocyanine conjugation with galactose was synthesized as Near-infrared fluorescent probes. In vivo fluorescence imaging effect and organ distribution of probe was conducted with nude mice bearing liver cancer as model , result shows that galactose modified phthalocyanine have obvious near-infrared imaging effect in vivo and a certain tumor targeting ability. So the near infrared optical probe can be potentially applied in the diagnosis of cancer in future.



Preparation of Novel Trolox-chitosan Nanoparticles and  Its Anti\|oxidation Activity

HAN Lu, DU Li-Bo, JIA Hong-Ying, TIAN Qiu, LIU Yang*

2011, 32(5):  1013-1015. 

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Trolox, an analogue of vitamin E, was firstly encapsulated into chitosan nanoparticles(20～40nm). In this way, the solubility of Trolox in water was increased about 27 times. Moreover, Trolox-chitosan nanoparticles showed better ability of protecting RAW264.7 cells from oxidative stress induced by t-BHP than Trolox alone at the same concentration. More importantly, the present study demonstrated a new strategy for elevating the solubility of antioxidants or drugs and improving their bioavailability by virtue of encapsulating them into nanoparticles.



Preparation and Standard Molar Formation Enthalpy of Weed-like ZnO Nanostructures

FAN Gao-Chao, HUANG Zai-Yin*, JIANG Jun-Ying, LI Yan-Fen, SUN Li

2011, 32(5):  1016-1018. 

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Weed-like ZnO nanostructures with uniformity in size were prepared by inverse microemulsion. The characterization results revealed that each weed consisted of several nanowires which were about 1 μm in length, 40 nm in diameter. On the basis of the known standard molar formation enthalpy of the bulk ZnO, the relationship of standard molar formation enthalpy between nano ZnO and bulk ZnO was obtained by designing a thermochemical cycle according to thermodynamic potential function method. Combined with the microcalorimetry, the standard molar formation enthalpy of the as-achieved weed-like ZnO nanostructures at 298.15 K was calculated as (-315.15±4.99) kJ/mol.



Synthesis and Properties of Poly(aryl ether)s with Pendent Multi\|sulfonic Acid Groups on Side Chain

LI Xue-Feng, XING Yan, DENG Hai-Dong, PANG Jin-Hui, JIANG Zhen-Hua*

2011, 32(5):  1019-1021. 

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poly(arylene ether ketone) carring multi-sulfonated side chain was prepared via graft polymerization reaction. The obtained soluble sulfonated polymer SP-I and SP-II have high viscosity (ηinh >1.72dL/g). The transparence and tough sulfonated polymer film was obtained by solution casting method and exhibited good thermochemical stability, high proton conductivity（>0.90 S/cm）and good dimensional stability.



Synthesis and Properties of SPEEK/PES Block Polymers

LI Xue-Feng, GUO Mei-Mei, LIU Bai-Jun*, JIANG Zhen-Hua

2011, 32(5):  1022-1024. 

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Two block SPEEK/PES copolymers were prepared via the postsulfonation reaction of the well designed precursors. The influence of microstructure/sequence distribution on the properties of the membranes was investigated. The block copolymers always had higher water uptake and proton conductivity in comparison with their random analogue. At 80 oC, the proton conductivities of the block copolymers were above 0.2 S/cm. The membranes of the block polymers exhibited obvious phase-separation microstructure. The study suggested that some properties could be improved by rational designing of the chemical architecture.



Preface

Synthesis, Structure and Mimic Catalytic Activity of Novel Vanadium Haloperoxidase Model Complexes

CAO Yun-Zhu, LI Zhang-Peng, XING Yong-Heng*, WEI Dong-Ming, PU Zhi-Feng, GE Mao-Fa, SHI Zhan

2011, 32(5):  1025-1032. 

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In order to mimicking the active center of the VHPO, we designed and synthesized a series of oxovanadium complexes containing poly(pyrazolyl)borate ligands: VO(HB(3,5-Me2pz)3)(3,5-Me2pz)(HOOCCH2CH2COO) and VO(HB(3,5-Me2pz)3)(3,5-Me2pz)(C5H4N-COO), and they have been characterized by X-ray single crystal diffraction. Based on vanadium(V) complexes catalyzing the visible conversion of phenol red to bromophenol blue under weak-acid conditions, we investigated the role of the oxovanadium complexes in the bromide oxidation reaction. It is found that the oxovanadium (IV) complexes can be considered as potential functional model of vanadium-dependent haloperoxidases. And the mechanism of the catalytic reaction is analyzed by molecular orbital theory.



Antibacterial Activities of Polyoxometalates Containing Silicon

CHEN Bing-Nian, FENG Zhen-Ge, WANG Li*

2011, 32(5):  1033-1036. 

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The polyoxometalates α-1,2,3-K6H[SiW9V3O40], α-1,2-K6[SiW10V2O40] and α-K5[SiW11VO40] (abbreviated as α- SiW9V3, α-SiW10V2, α-SiW11V, respectively) were synthesized and characterized by UV-Vis and FT–IR spectrums. The antibacterial activity of four polyoxometalates against common bacteria（Escherichia coli, Bacillus subtilis, yeast, Aspergillus niger and Penicillium） was studied by disk diffusion method. The results indicated that four compounds showed different antibacterial effects on Escherichia coli, Bacillus subtilis, yeast, Aspergillus niger, and the antibacterial activity of Penicillium was relatively worse. This study should give theoretical support for polyoxometalate used as a fruit and vegetable preservative agent.



Preparation and Characterization of NaGdF₄∶Eu³⁺/AAO Thin Films

WANG Meng, YANG Zhi*, WANG Yu-Fei, TAO Ye

2011, 32(5):  1037-1042. 

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NaGdF4:Eu3+/AAO thin films were prepared on porous anodic aluminum oxide (AAO) template surface via a hydrothermal process and the effects of some processing variables such as preparing method, the amount of NaGdF4:Eu3+, annealing temperature, were investigated. The crystal structure, morphology and luminescent properties of the as-prepared NaGdF4:Eu3+/AAO thin films were characterized by X–ray powder diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence (PL) spectra. XRD results show that the phase transition of NaGdF4:Eu3+/AAO thin films from the hexagonal phase to the cubic phase occurs at about 500℃ in air. SEM images indicate that the preparing method influences obviously the morphology of NaGdF4:Eu3+/AAO thin films, NaGdF4:Eu3+/AAO thin films with the rectangle morphology were prepared by a two-step hydrothermal process, and however the one-step hydrothermal process was employed to prepare NaGdF4:Eu3+/AAO thin films without any special morphology. The amount of NaGdF4:Eu3+ in the solution and the annealing temperature do not obviously affect the morphology of NaGdF4:Eu3+/AAO thin films. PL results show that the characteristic emission of NaGdF4:Eu3+/AAO thin films with hexagonal or cubic NaGdF4 structure is Eu3+ 5D0→7F2 transition.



One\|pot Synthesis of CdS Quantum  Dots and Their Quantum Yields

WANG Li, WANG Jin, CHEN Yan, ZHONG Hong-Hai, JIANG Yang*

2011, 32(5):  1043-1048. 

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CdS QDs were synthesized via one-pot method, with ODE as the solvent and oleic acid as capping ligands. The influences of reaction time, reaction temperature and Cd/S molar ratio on optical properties of CdS QDs were studied. The zinc-blende, monodisperse and high-crystalline structures of CdS QDs were characterized by means of XRD and HRTEM. The good monodisperse size distribution and optical properties were also confirmed by UV-vis and PL. The PL spectra are symmetrical, and their full-width at half-maximum (FWHM) is samll. The first absorption peak is very sharp. The growth temperature and the initial Cd/S molar ratio have important influences on the size and photoluminescence quantum yields (PLQY) of CdS QDs. It has been demonstrated that high photoluminescence quantum yields with nearly monodisperse CdS nanocrystals can be obtained by a judicious choice of the Cd:S molar ratio (3:1) and the growth temperature (240℃), and the PLQY is about 30%.



Dielectric Properties of a Series  of  Perovskite La_1-x-yCa_xK_yMnO₃ Manganites

2011, 32(5):  1049-1053. 

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A series of perovskite manganese oxides La1-x-yCaxKyMnO3 are synthesized from hydrothermal redox reaction, and they have La3+, Ca2+ and K+ three kinds of cations with different valences occupied at A site. The obtained samples are ground and pressed in discs, and the discs are then sintered to form a parallel-plate capacitor. At room temperature, the capacitance, the loss tangent and the resistance are measured as a function of frequency. We find that the real part of the complex relative dielectric permittivity varies considerably in different samples with the A-site cation size mismatch. The comparison of the resistance derived from experiment and calculation respectively indicates the equivalent circuit in intrinsic samples.



Matrix Solid Phase Dispersion for the Extraction of Podophyllotoxin Glucoside and Isopicropodophyllone from Roots of Sinopodophyllum emodi(Wall.)

JIN Yong-Ri, SHI Xiao-Lei, LI Xu-Wen, ZHAO Xue-Zhong*, ZHANG Mu-Chun*

2011, 32(5):  1054-1057. 

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A fast and simple extraction procedure based on the matrix solid-phase dispersion was proposed for the extraction of two kinds of lignans including Podophyllotoxin gluoside and isopicropodophylloneas from the dried roots of Sinopodophyllum emodi wall.. The compounds were determined by High performance liquid chromatography. The main parameters that affect extraction yields, such as type of dispersant, type of clean-up absorbent, were examined and optimized. Compared with reflux extraction, the proposed method is simpler, faster and more efficient.



Acute Toxicity of Venenum Bufonis and Compatibility of Heart Musk Protecting Pills by Microarray Expression Analysis

YANG Ai-Wen, FAN Xue-Mei, LI Xue, LIANG Qiong-Lin, WANG Yi-Ming, LUO Guo-An*

2011, 32(5):  1058-1064. 

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The differentially expressed genes involved in acute toxicity and compatibility of Heart Musk Protecting Pills(HMP) via cDNA microarray were investigated in this paper. Then the GO and KEGG Pathway enrichment analysis were carried as well as the functional analysis and real time RT-PCR validation of two important genes. Results indicated that the ion homeostasis and actin organization were affected in the low dosage group for Venenum Bufonis, Meanwhile, regulation of anti-apoptosis and fatty acid metabolism could be induced within two hours; the myocardial contraction was finally disturbed. The ion homeostasis and actin organization could also be disturbed more quickly in the high dosage group. In addition, the iron accumulation could lead to oxidation reduction and cardiomyocyte apoptosis. For HMP, there were some clinical functions, such as blood pressure regulation and myocardial structure organization. However, the related acute toxicity of Venenum Bufonis was not shown. This paper could provide a novel research strategy in the compatibility study of Traditional Chinese Medicine (TCM).



Detection of Ochratoxin A by Label\|Free Liquid Crystal Immunosensor

YANG Sheng-Yuan, TAN Hui, LIU Yan-Mei, WU Zhao-Yang*, SHEN Guo-Li, YU Ru-Qin

2011, 32(5):  1065-1069. 

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A novel liquid crystal immunosensor based on the indirect competitive assay format was developed for the detection of ochratoxin A (OTA). In this method, the OTA was tethered onto the self-assembled film surface on a glass slide via a cross-linker glutaradehyde. The specific binding event of anti-OTA antibody and ochratoxin A induced the homeotropic-to-tilted transition of LCs, resulting in the corresponding changes of opitical images under the crossed polarized light. The LC-based imaging method has a good signal-to-noise ratio and a clear distinction between positive and negative results. When the concentration of analyte OTA exceeds a critical value (0.01 ng/mL) , the opitical images gives a very sharp response. The opitical images changes with the concentration of OTA in a dynamic range of 0.01–10 ng/mL .The fabricated sensor is show to exhibit high sensitivity, desirable selectivity, label free and ease in operation。



Preparation and Properties of High-Density HBsAg-Conjugated Magnetic Probes

ZHANG Bao-Liang, ZHANG Qiu-Yu*, ZHANG He-Peng, LIU Yu, FAN Xin-Long, XU Hai-Long

2011, 32(5):  1070-1076. 

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The preparation of magnetic beads loaded with high-density Hepatitis B Surface Antigen (HBsAg) detection probes was introduced in this paper, and the properties of the beads for HBsAg detection were also studied. The immunomagnetic beads coupled with HBsAb were firstly prepared by chemical bond. Then, immunomagnetic beads were used for detecting HBsAg and were obtained a favorable effect. In order to improve the accuracy and sensitivity of detection, the preparation process of immunomagnetic beads was optimized, including amination and coupling process. Through the optimization, the amino content of magnetic beads was 2.71mmol/g, unit magnetic beads bonded 108.36 ug/mg antibodies and the coupling efficiency was 77.40%. The activity of HBsAb on magnetic beads was detected by the method similar to Enzyme-Linked Immunosorbent Assay (ELISA). Compared with common ELISA technology, magnetic beads loaded with high-density HBsAb have higher sensitivity.



Photoconversion of p-Chlorphenol in Photo-Fe³⁺-oxalic Acid System in Ice

XUE Hong-Hai, PENG Fei, ZHAO Xu-Hui, KANG Chun-Li*, LI Lin-Lin, LI Zhe, LIU Han-Fei

2011, 32(5):  1077-1082. 

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This work investigated the photoconversion of para-chlorphenol (4-CP) in simulated sunlight - Fe3+ - oxalic acid system in ice using self-made low temperature device. The results showed that in the presence of Fe3+ and oxalic acid, the photoconversion of 4-CP was accelerated in ice. The initial concentration of Fe3+ and oxalic acid, the ratio of the initial concentration of Fe3+ and oxalic acid, and the initial pH value had significant influence on the photoconversion of 4-CP. The photoconversion rate of 4-CP reached 39.1% after irradiation for 7.5 h when the initial pH value was 6.5, the ratio of the initial concentration of Fe3+ and oxalic acid was 1/5, and the initial concentration of oxalic acid was 0.8mmol/L. During irradiation, the conversion rate of TOC was lower than that of 4-CP. The photoconversion of 4-CP obeyed the first order kinetics equation. The photoproduct of 4-CP were enriched through direct extraction and derivatization respectively, and then analyzed by GC-MS. Accroding to the outcome, the photoconversion mechanism was deduced in the simulated sunlight - Fe3+ - oxalic acid system in ice.



Synthesis and Cytotoxic Activities of Ferrocene Schiff Bases

TAN Ping, YU Ai-He, YAN Jing, MI Yong-Sheng, LI Jun-Zi, XIANG Jian-Nan*

2011, 32(5):  1083-1087. 

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Ferrocene derives have many special properties. In order to evaluate cytotoxic activity of ferrocene Schiff base, six novel ferrocene Schiff bases were synthesized through the reaction of ferrocene carboxaldehyde with 3-substituted-4-amino-1,2,4-triazole-5-thione and four new ferrocene acylhydrazone Schiff bases were also synthesized with ferrocenecarboxaldehyde or acetylferrocene with acylhydrazine. Its structure were characterized by 1H NMR，IR , MS and Element analysis. their cytotoxic activities were determined in vitro by an 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay using human cervical cancer cells (Hela). The results indicated that these compounds exhibited some cytotoxic activities against cancer cells. The mechanism of this useful property of these compounds should be conformed in the future.



3D\|QSAR Study of Rocaglamide Analogues

ZHOU Yi-Hui, DUAN Hong-Xia*, FU Bin, MA Yong-Qiang, DU Feng-Pei, WANG Ming-An, QIN Zhao-Hai*

2011, 32(5):  1088-1093. 

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The research on the three dimensional quantitative structure activity relationship (3D-QSAR) of 26 rocaglamide analogues in the training set, was carried with comparative molecular field analysis (CoMFA) and comparative molecular similarity indices analysis (CoMSIA). The cross validated coefficient(q2) is 0.593 and 0.656 respectively in the resulting CoMFA and CoMSIA models, which was used to predict the activities of the traning set and 5 analogues in the testing set, showing a favorable predictive ability. Dimensional contour maps of CoMFA and CoMSIA can not only show the visualized interpretation between the important R1, R2 and R5 groups in the structures with activities, but also provide a guidance to changed the structures for prominent biological activities.



Synthesis of Fulleropyrrolidine Derivatives with Aromatic Substituted Imidazoles and Their Application in CdSe-Quantum Dot Solar Cells

ZHAO Ai-Ting, XIONG Yan-Ling, ZENG He-Ping*

2011, 32(5):  1094-1099. 

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Two aromatic substituted imidazole compounds including 4-(4,5-bis(3- nitrophenyl)- 1H-imidazole-2-yl)-3,6-biacetyl-9-ethyl-carbazole(5) and 4-(1-benzyl-4,5-bis(3-nitrophenyl)- imidazol-2-yl) 3,6-biacetyl-9-ethyl-carbazole (6) have been synthesized by the optimized Debus’ method. Fulleropyrrolidine derivatives (7) and (8) were successfully synthesized by 1,3-dipolar cycloaddition. The structure of these moleculars were identified by MS, NMR and IR. Seven solar cells were fabricated: FTO/TiO2/CdSe/Pt, FTO/TiO2/C60/Pt, FTO/TiO2/Im-C60/Pt, FTO/TiO2/Bn-Im-C60/Pt, FTO/TiO2/C60-CdSe/Pt, FTO/TiO2/Im-C60-CdSe /Pt and FTO/TiO2/Bn-Im-C60-CdSe/Pt. The result showed that the observed energy conversion efficiency of Im-C60-CdSe based solar cell and Bn-Im-C60-CdSe based solar cell are 5.28% and 40.08% respectively which were compared with CdSe QDs sensitized solar cell.



Immobilization of Trypsin on Amino Acid-modified SiO₂ Porous Materials

LI Ye*, ZHANG Heng-Jian, LIAO Ming-Xia, LIU Tao

2011, 32(5):  1100-1105. 

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To improve the biocompatibility and hydrophobicity of silica carrier material, and maintain the biological activity of embedded biological molecules, the synthetic routes of hydrolysis precursor 3-aminopropyl trimethoxysilane modified by amino acids are reported. The SiO2 porous material precursor modified by amino acid was prepared by a acryl chloride method. To be specific, the N-(9-Fluorenylmethoxycarbonyl)-L-valine reacted with thionyl chloride. The obtained compounds further react 3-aminopropyl trimethoxysilane. The valine modified precursor is obtained after removaling Fomc group. All obtained compounds were characterized by IR、MS、1H-NMR.. Using amino acids modified APTMS for silicon source, immobilized trypsin was prepared on a mild sol-gel process. When the molar ratio of amino acid modified 3-aminopropyl trimethoxysilane in hydrolysis precursor was 15 mol%, the immobilized trypsin shows the highest activity. The enzyme activity of immobilized trypsin by amino acid modified 3-aminopropyl trimethoxysilane is 2 times of that of free enzyme. The enzyme activity of immobilized trypsin by hybrid materials is 5 times of that of enzyme immobilized by tetramethoxysilane. The synthesized hybrid materials show a good biocompatibility.



Observed Kinetics Study of Methylene Diphenyl Dicarbamate Thermo-decomposition to Diphenylmethane Diisocyanate

ZHANG Qin-Hua, LI Hui-Quan*, LIU Hai-Tao, PEI Yi-Xia

2011, 32(5):  1106-1111. 

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The observed kinetics study of Methylene diphenyl dicarbamate decomposition was investigated in the presence of diisooctyl sebacate. A consecutive reaction model was established by simplifying the decomposition process and the two steps were conformed to be the first-order by integral test model and numerical differential method, respectively. The results showed that the activation energies of the two steps are 138.82 kJ/mol and 167.78 kJ/mol, while the frequency factors are 1.51×1012 and 5.33×1014, respectively. Base on the obtained kinetic model, the reaction proceeding can be calculated in given conditions.



Controllable Fabrication of SnO₂ Nanomaterials with Three Kinds of Morphologies and Their Application as Cataluminescence Sensor

LIU Ming-Yang*, ZHAO Jing-Hong, ZOU Ming-Qiang, LIU Da

2011, 32(5):  1112-1117. 

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SnO2 nanomaterials with three kinds of morphologies like nanoparticles, nanorods and SnO2-CNT nanocomposites were controllable synthesized using CNT as a template. Cataluminescence (catalytic chemiluminescence, CTL) characteristic of ethyl acetate catalyzed on nanosized SnO2 with 3 kinds of morphologies was studied. Nanostructure and BET　surface area of the SnO2 nanomaterial was very important for the CTL. A relationship between SnO2 nanomaterial with 3 kinds of morphologies and CTL of ethyl acetate was established. Three new kinds of gas sensors have been invented based on the spectrum mentioned above.



Study on Photosensitized Oxidative Desulfurization of Dibenzothiophene by Riboflavin

ZHANG Juan, ZHAO Di-Shun*, YANG Jie, YANG Li-Yan

2011, 32(5):  1118-1122. 

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Photosensitized oxidative desulfurization of dibenzothiophene（DBT） in n-octane/water extraction system was studied with riboflavin as photosensitizer and O2 in air as oxidant. A 15W UV lamp was used as the light source for irradiation and air was introduced by a gas pump for supplying O2. The result showed DBT was photooxidized successfully. The optimal reaction condition is, riboflavin concentration at 20mg/L and the air flow a t 80～100mL /min. Under optimal condition, the removal rario of DBT is up to 60% for 2 hours. Riboflavin sensitized DBT by 1O2 mechanism, the kinetics of photosensitized oxidation of DBT is fist-order.



Reaction Class Isodesmic Reaction Method and Calculation of Thermokinetic Parameters for Reactions in a Class

WANG Hai-Xia, WANG Bi-Yao, ZHANG Jun-Ling, LI Ze-Rong*, LI Xiang-Yuan

2011, 32(5):  1123-1128. 

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Reaction class isodesmic reaction method, which is the extension of the isodesmic reaction method usually used for the calculation of the thermodynamic properties to calculate the reaction barrier and reaction enthalpy for reactions in a class, is proposed. The pyrolysis of β alkyl hydrogen peroxide generating olefin and HO2 radical, an important class of reactions in the combustion of the hydrocarbon in low-temperature phase, is studied. Calculations for five representative reactions in this reaction class using reaction class isodesmic reaction method and direct calculation method respectively, at HF、DFT、MP2、CCSD(T) level reveal that a low-level ab initio method such as B3LYP method using reaction class isodesmic reaction method can reproduce reaction barriers by high-level ab initio methods such as CCSD(T). In this study, reaction barriers and the reaction enthalpies for 16 reactions of this class at B3LYP/6-311G(d,p) level using reaction class isodesmic reaction method are calculated and a linear free energy relationship between the reaction barrier and the reaction energy is obtained: delta V=71.02+0.41?delta E.



Theoretical Comparison for the Excited States of Chlorophyll-a by Quantum-chemical Calculations

YANG Jia-Yu, YIN Shi-Wei*, YANG Yong-Mei, LI Lan-Lan

2011, 32(5):  1129-1137. 

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The four lowest excited states of chlorophyll-a are calculated by SAC-CI (symmetry adapted cluster coupled configuration interaction), ZINDO (Zerner’s intermediate neglect of differential overlap) and various time-dependant DFT methods. The influences of the side group and nstate on the excite state of Chl-a are discussed. The orientation of three-dimensional transition dipole moment of the Qy band is assigned by different method, these means that is not exactly towards the y direction as Renger’s DFT calculation mentioned. Among of different DFT methods, CAM-B3lyp is the best method to describe the four lowest excited states of Chl-a.



Sulfonic Acid-functionalized MCM-41 for Transesterification of Triacetin with Methanol

CAO Ying-Yu, WANG Ya-Quan*, HAO Jin-Ku

2011, 32(5):  1138-1143. 

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A series of sulfonic acid-functionalized MCM-41 catalysts have been synthesized through coating and polymerization of the furfuryl alcohol on the pore walls, and then sulfonated in the presence of sulfuric acid at different temperatures. The catalysts are characterized by Nitrogen adsorption measurements using the procedure according to Brunauer, Emmet and Taller (BET), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier transform Infrared resonance spectroscopy (FTIR), and studied for the transesteri?cation of triacetin with methanol as a model reaction for biodiesel production. The results show that a number of sulfonic groups attach on the pore walls with the mesopores of MCM-41 not being damaged; the catalysts show very high activity and selectivity in the transesteri?cation reaction, and the SO3H-MCM-41(200 oC) exhibits the highest triacetin conversion(99.4%)after 300 min which has the same activity as H2SO4, the selectivity of methy acetate and glycerol is 71.5% and 17.4% after 180 min, respectively.



Preparation of Pd/Pt Bimetallic Electrodes and Its Activity Toward Oxygen Reduction Reaction

FANG Lan-Lan, LIAO Ling-Wen, LIU Shao-Xiong, CAI Jun, LI Ming-Fang, CHEN Yan-Xia*

2011, 32(5):  1144-1149. 

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Pd/Pt bimetallic electrodes are prepared using under-potential deposition (UPD) of Cu following with galvanic displacement of Cu by Pt(denoted as Pd/Ptx, here x denoted the cycle No. of UPD Cu and the subsequent Pd-Cu displacement processes). The atomic ratios of Pt:Pd in the surface region can be tuned by holding the low potential limit for Cu UPD at 0.34 V, and tuning the cycle No. of UPD Cu and Pd-Cu displacement processes. The surface composition of Pd/Pt bimetallic electrodes were examined by x-ray photon-electron spectroscopy (XPS) and electrochemical infrared spectroscopy (EC-IRS) using CO as a probe. And the activity of Pd/Ptx bimetallic electrodes toward oxygen reduction reaction (ORR) have been studied using cyclic voltammetry (CV) in a flow cell. XPS and EC-IRS demonstrate that the atomic ratios of Pt:Pd increase monotonically with the cycle No. of Cu-upd and Pt-Cu displacement. For Pd/Pt4 electrode, the atomic ratios of Pt:Pd in the region of ca. 2~3 nm from the surface is 1:4, while Pt:Pd ratio at the surface is ca. 5:1. With the increase in Pt ratio at the surface, Pd/Ptx electrodes become more and more oxidation resistant. The ORR activity increase with x up to 4 and it remains unchanged at x?4. For Pd/Ptx electrode (with x>3), its ORR activity is higher than that of polycrystalline(pc) Pt. Under otherwise identical condition, the half wave potential for ORR at Pd/Pt4 electrode is about 25 mV more positive than that at pc-Pt electrode. The enhancement in ORR activity of Pd/Ptx bimetallic electrodes is attributed to the reduction of adsorption energy of O containing species on Pt atoms induced by adjacent Pd atoms at the surface or by Pd atoms under the surface Pt layer.



Mechanistic Studies on Radical Dynamics of Daidzein and Genistein upon Photooxidation

CHEN Chang-Hui, LIANG Ran, HAN Rui-Min*, AI Xi-Cheng, ZHANG Jian-Ping

2011, 32(5):  1150-1156. 

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As natural antioxidants, flavonoids, containing polyphenolic hydroxyls and conjugated electronic structures, can inhibit chain oxidation reaction by scavenging radicals. The antioxidation active sites of flavonoids and the stabilities of product radicals are the basically factors on affecting their antioxidant reactivities. This work compares the dynamics of radicals formed from photooxidation on anionic daidzein and genistein, respectively, as revealed by the use of time-resolved spectroscopies combined with quantum chemical analyses. It is found that direct photooxidation of mono- and di-anionic daidzein both formed an intermediate radical which transformed into a relatively more stable radical via intramolecular electron trasfer. Photooxidation of anionic genistein, an isoflavone with one more 5-hydroxyl than daidzein, including mono-, di- and tri-anions, results in the formation of a stable radical with electronic spin density delocalizing on the whole molecular backbone. The antioxidant reactivity of 4’-hydroxyl for mono-anion is enhanced by the presence of 5-hydroxyl, which is ascribed to the key structural factor for the higher antioxidant activity of genistein than daidzein in physiological condition.



Construction and Catalytic Properties of Molecular Imprinting Microreactor on Multiwalled Carbon Nanotubes for Diels-Alder Reaction

XU Zhi-Feng*, WEN Ge, KUANG Dai-Zhi, ZHANG Fu-Xing, WANG Jian-Qiu, LI Jun-Hua

2011, 32(5):  1157-1162. 

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The applications of molecularly imprinted polymers (MIPs) in synthesis and catalysis are being increasingly investigated. Conventional bulk polymerization often produce the polymer materials exhibiting low binding capacity, binding sites heterogeneity, and poor site accessibility. The use of nano-sized MIPs is expected to overcome these problems because nano-sized materials have a small dimension with high surface-to-volume ratio. The objective of this study is to construction molecular imprinting microreactor (MIM) in nanomaterials. In the first step, alkenyl multiwalled carbon nanotubes (MWNTs) were prepared by esterification reaction of hydroxyl group of MWNTs and methacryloyl chloride. Then, the molecular imprinted catalyst for Diels-Alder cycloaddition was fabricated on MWNTs by using alkenyl-MWNTs as matrix, Diels-Alder cycloaddition product of anthracene and maleic acid as template molecule, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EDMA) as functional monomer and cross-linker, respectively. The molecular imprinted catalyst exhibited catalytic activity for the cycloaddition reaction of anthracene and maleic acid. Compared with the uncatalyzed reaction, a rate enhancement of 1.77 fold was obtained. Plots of initial velocities of the cycloaddition versus substrate concentration showed typical Michaelis-Menten kinetics. In addition, the Michaelis constant (KM) and maximal rate (vmax) were calculated from Lineweaver-Burk plots to be 17735.24 umolL-1 and 0.713 umolL-1S-1, respectively.



Amount and Mechanism of HF Production in Fire Extinguishing Process Using CF₃H

ZHOU Biao, ZHOU Xiao-Meng*, CHEN Tao, ZHOU Jun-Xue, HU Li-Ming

2011, 32(5):  1163-1168. 

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Trifluoromethane (CF3H, HFC-23), as one of important perfluoroalkanes, is used commonly in now fire extinguishing agent market. However, when CF3H is discharged into the fire protection place, HF will be produced by the interaction between the flame and CF3H. HF not only has severe erosion to the metal apparatus, but also makes serious harm to the people in fire scene, so the production amount of HF in fire extinguishing protection is an important problem when CF3H is applied. At present, there is lacking of in-depth insight of HF production in fire extinguishing process with CF3H. So the amount and mechanism of HF production in fire extinguishing process using CF3H is studied in this paper. Firstly, the decomposition of CF3H under different temperature is calculated by Ab initio method at B3LYP/6-311 + + G (d, p) level. And then, the model for predicting HF amount is proposed on the base of calculation. Thirdly, the production amount of HF is measured real-timely by in-situ spectral diagnostics method when CF3H is discharged into Cup-burner with steady alcohol flame. Conclusion: By comparing the calculated results with experimental results, it shows that the HF production predicting theory model was reliable; When the temperature is lower than 100℃, there little HF；The fastest HF production rate between 100℃ and 400℃；after 400℃, it has nearly no change; The main pathway for HF production is CF3H+?H reaction.



Stability of the Complexes Combined by Metal Ions and Adenine Base Isomers

CHEN Jin-Peng, QI Zhong-Nan, YANG Ai-Bin, AI Hong-Qi*

2011, 32(5):  1169-1174. 

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132 stable complexes formed by metal ions(Na+，K+，Ca2+，Mg2+) and fourteen stable adenine tautomers in gas and aqueous phases were optimized at the B3LYP/6-311++G**//6-31+G* level in combination with the PCM models. By comparison, the stabilization ordering of all these stable complexes in aqueous phase is first obtained and the optimal binding site for a metal ion in a specific adenine tautomer is identified. Meanwhile, the differences of the ordering in the two different phases are analyzed systematically. Results indicate that it is solvent effect to induce different solute-solvent interaction and, as a result, lead to the stabilization ordering change from that in gas phase. It is the different metal ion effect to result in the different ordering of relative stability of a complex formed by different metal ion and identical adenine tautomer. For these changes, this article makes detailed analysis based on gas-phase binding energies (EBE) and aqueous phase polarized solute-solvent energies (Epol).



Superhydrophobicity of Lotus-leaf-like Fluorinated Ethylene Propylene Copolymer Surface

LIU Chuan-Sheng, JIANG Wen-Qu, GUAN Zi-Sheng*

2011, 32(5):  1175-1180. 

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Superhydrophobic fluorinated ethylene propylene (FEP) copolymer surface with lotus-leaf-like structure was prepared by thermoforming FEP powder at the condition of 0.3 N/cm2 , 280 ℃ and -0.1Mpa vacuum on the polydimethylsiloxane (PDMS) templates, which replicated the lotus leaf surface. SEM results indicate that the FEP surface shows great similar lotus-leaf-like structures with superhydrophobic, corresponding water contact angle and tilt angle are 168° and 3°, respectively. The superhydrophobic lotus-leaf-like FEP surface also exhibits good stability in water, acohol, acid and alkaline solution after duration of decads-hours immersion. Furthermore, once the hydrophobicity of FEP surface decreased, it?s recoverable via an immersion process in piranha solution for several decades minutes. Differential scanning calorimetry (DSC) results indicate the mass loss of the PDMS templates is very low means that it can be used repeatedly during the therm forming process. Therefore, our methods combine the very good acid resistant, alkaline resistant and corrosion resistant of the FEP with lotus-leaf-like structure to fabrication of superhydropobic surface may be applied in preparation of anti-adhension and self-cleaning vessels, etc.



Preparation and Osteogenesis Activities of  Electroactive Biodegradable Nanocomposites PAP/op-HA/PLGA

WU Hai-Tao, YU Ting, ZHU Qing-San*, JIAO Zi-Xue, WEI Yan, ZHANG Pei-Biao*, CHEN Xue-Si

2011, 32(5):  1181-1187. 

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We prepared the electroactive biodegradable nanocomposites PAP/ op-HA/PLGA by blending a triblock copolymer PLA-b-AP-b-PLA (PAP) of polylactide (PLA) and aniline pentamer (AP) with oligomeric lactic acid-surface grafted hydroxyapatite (op-HA)/poly(lactide-co-glycolide)(PLGA). The electrochemical properties and conductivity were characterized using UV-Vis spectroscopy, cyclic voltammetry and standard four-probe method. Film’s surface morphology was displayed by ESEM and contact angle was measured to evaluate the film’s hydrophilicity. Rabbit’s osteoblasts were cultured in vitro on the film surface. For comprehensively evaluating surface properties and biological activity of the new electroactive nanocomposites PAP/op-HA/PLGA for bone repair, cell adhesion and cell spreading (cell area fraction) were determined using fluorescein isothiocyanate dyeing and NIH Image J software analysis, and gene expression levels were detected using Real-time PCR. The results show that PAP/op-HA/PLGA had good electrochemical redox property and low conductivity (~ 5 ? 10-6 S/cm). With the content of 0.1 wt% PAP, the hydrophilicity of composites was improved, the adhesion and expansion of osteoblasts were enhanced, and bone morphogenetic protein-2 (BMP-2) and bone junction protein (osteonectin) gene expression levels were increased, significantly. In conclusion, PAP/op-HA/PLGA composites have good biocompatibility and osteogenic activity.



Oxidation Resistance and Dielectrical Properties of Boron Nitride by Pyrolysis of Poly(isopropylamino)borazine

LEI Yong-Peng, WANG Ying-De*, SONG Yong-Cai, LI Yi-He, WANG Hao, DENG Cheng, XIE Zheng-Fang

2011, 32(5):  1188-1193. 

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Poly[tri(isopropylamino)borazine] (PTPiAB), a soluble and fusible precursor to hexagonal-BN (h-BN), was synthesized under mild conditions using isopropylamine and trichloroborazine (TCB) as starting materials. h-BN was obtained by pyrolysis of PTPiAB in NH3 and then in Ar. The composition, structure and properties of PTPiAB and pyrolytic product were investigated by using elemental analysis, FT-IR, XRD, TGA and Network Analyzer. The results indicate that N-H, C-H, C-N bonds and B3N3 units exist in the structure of PTPiAB. The melting point is 70 oC. The weight loss mainly occurs below 800 oC and ceramic yields for the precursor in NH3 and Ar are 45.9 % and 52.8 % at 1000 oC, separately. Crystallization occurs at around 1000 oC and the (002) interlayer spacing and density are 0.334 nm and 2.03 g·cm-3 at 1800 oC, respectively. Furthermore, the BN illustrates superior oxidation resistance with weight increase lower than 0.3% below 900 oC in air. The BN also displays low dielectric constants with real part of 2.45 and loss tangent of 0.03 at 10 GHz at ambient temperature, respectively.



Synthesis of Degradable Poly(polyamidoamine-methacrylamide-g-anhydride) Photocrosslinked Gels and Their Controlled Drug Release Behavior

CHEN Yang-Juan, ZHONG Shi-An*, SHI Qiong

2011, 32(5):  1194-1199. 

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Polyamidoamine(PAMAM) dendrimers were methacylated by Methacryloyl chloride and photopolymerized with Methacrylated Sebacic Anhydride(MSA) to obtain degradable gels.Structures of the polymers were characterized by FT-IR and1H NMR. In order to study the effects of polyamidoamine double bond (PAMAM-DB):MSA ratio on the polymer degradation behavior, local pH, water uptake, mass loss and surface morphology in the course of degradation were explored.It is found that the gels containing 50-60wt% anhydride were good surface erosion materials. Degradation time and pH of degradable medium range from 45 to 60 days, and from 6.5 to 8.06, respectively.Sample with 50wt% anhydride was choosed as the bead of ofloxacin based on the degradation experiment.The result shows the drug-released time and content of drug could be controlled by varing the mass fraction of MSA.



Synthesis and Characterization of α-Diimine Nickel(Ⅱ) Catalyst Containing Br Groups for Ethylene Polymerization

YUAN Jian-Chao*, MEI Tong-Jian, WANG Xue-Hu, LIU Yu-Feng

2011, 32(5):  1200-1204. 

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A new Br-substituted alpha-diimine compound and its corresponding Ni(II) complex, {bis[N,N’-(3-bromo-2,4,6-trimethylphenyl)imino]acenaphthene}dibromonickel was successfully synthesized, and characterized by 1H NMR, 13C NMR, elemental analysis, FT-IR and XPS. The pre-catalyst 2 activated by methylaluminoxane (MAO) was tested in the polymerization of ethylene, showed to be highly active (5.50×106gPE/ (molNi.h.bar)). The catalyst system 2/MAO showed the highest activity with the 800 of Al/Ni molar ratio at 25 ?C. It was found that the catalyst containing electron-withdrawing groups Br showed better thermal stability and almost the same catalytic activity. At same time, branching degrees was increased in the presence of electron-withdrawing groups Br. The polymer were characterized by 1H NMR, 13C NMR, GPC、TG、DSC.



Fabrication and Characterization of Chemical Vapor-actuated PANI/PU Bilayer

DING Chun-Mei, WANG Liang, ZHU Ying*, WAN Mei-Xiang, JIANG Lei*

2011, 32(5):  1205-1209. 

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Polyaniline/polyurethane (PANI/PU) bilayer actuators are fabricated using PANI nanofibers as active material and electrospun polyurethane (PU) fibers as substrate. It is found that the PANI/PU bilayer actuators undergo bending-recovery movement induced by hydrochloride vapor. The deformation mechanism of the bilayer actuators might result from asymmetric volume expansion/contraction because of doping/dedoping and sorption/desorption of chemical vapors. Moreover, the PANI/PU bilayer actuator can carry over 9 times its own weight due to the high toughness of PU fibers, displaying the well load-bearing capacity. Because the PANI/PU actuator is ultra-lightweight, low cost and simple operation, it is advantageous for practical applications in the future.



NMR Diffusion Studies of n-Hexane Inside Silica/Poly(styrene-co-acrylic acid) Core-shell Composite Particles

DU Li-Jun , WANG Jing-Dai, YANG Yong-Rong, JIANG Bin-Bo*

2011, 32(5):  1210-1215. 

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The diffusion of n-hexane in SiO2 particles and SiO2/poly(styrene-co-acrylic acid) (SiO2/PSA) core-shell particles, prepared by phase inversion method, was investigated by constant gradient field NMR (CFG-NMR). According to the two-site modal and molecular exchange theory, 1H CFG echo decay curves of n-hexane could be fit as biexponentials, implying that two different diffusion coefficients were existed in the diffusion system. The diffusion coefficients of n-hexane in the SiO2/PSA core-shell particles were much lower than in the SiO2 particles, indicating that the poly(styrene-acrylic acid) shell played as a barrier on the diffusion of n-hexane. By varying the diffusion time in the pulsed sequence, we found that the diffusion coefficients of n-hexane in the core-shell particles were strongly depended on the diffusion time.



Synthesis, Structure and Thermal Properties of Bisphenol Fluorene Diamine Benzoxazine

SUN Jian-Xin, SHI Tie-Jun*, XU Hui, WU Xing-Lin

2011, 32(5):  1216-1220. 

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9,9-bis(4-hydroxyphenyl)-fluorene (Bisphenol Fluorene，BHPF) was synthesized from phenol and 9-fluorenone using 98% sulfuric acid as catalyst and 2-mercaptopropionic as promoter, and then a liner BHPF-diamine benzoxazine (BF-eda resin) was synthesized using BHPF, ethylenediamine and paraformaldehyde. Chemical structure of the BF-eda resin were verified by Fourier transform infrared spectroscopy (FT-IR), 1H and 13C nuclear magnetic resonance spectroscopies(NMR). The GPC analysis presents the number average molecular weight of BF-eda resin is 4690，and the polydispersity index (PDI) is 2.93. The curing behavior of BF-eda resin was studied by differential scanning calorimetry (DSC) and the thermal stabilization of polybenzoxazine was evaluated with thermogravimetric analysis (TGA).The ring-opening polymerization temperature of BF-eda resin is about 253℃, the thermal decomposition temperature of polybenzoxazine is 344℃, the temperature at 5% weight loss is 357℃, and the char yield ratio is 51% at 900℃.



Construction of Rhodamine B and Gene Co-delivery Nanoparticles

WANG You-Xiang*, SHEN Xiao-Bo, XU Zhi-Xue, HU Qiao-Ling

2011, 32(5):  1221-1224. 

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The preparation of drug and gene co-delivery nanoparticles was the key scientific problem in tumor multi-combined therapy. In this research, the hydrophobic fluorescent dye rhodamine B was chosen as a model drug. PEI-g-cholesterol amphiphilic polymer was synthesized as drug carrier. By selecting proper conditions, rhodamine B and gene co-delivery nanoparticles were successfully constructed via supramolecular assembly. The co-delivery particles with diameter about 150 nm and ξ-potential about 33 mV could effectively condense DNA. The in-vitro cell culture experiments indicated that the positive co-delivery nanoparticles was easily uptaked by HEK293 cells and showed effective transfection efficiency.



Drawing-induced Crystallization Behavior and Brill Transition of Nylon 1010

WANG Ji-Ku*, ZHAO Guo-Sheng, ZHOU Yun-Chun

2011, 32(5):  1225-1230. 

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Abstract : The crystal transitions and crystal orientations of Nylon 1010 drawing-induced at different drawing temperatures (Td) and drawing ratios (λ) were carefully studied by Differential Scanning Calorimetry (DSC), Wide-Angle X-ray Diffraction (WAXD) and Two Dimensional (2D) Wide-Angle X-ray Scattering (WAXS) experiments. Results show that drawing is favorable to the transition of δˊform from αform of Nylon 1010 and so-called Brill transition became more obviously with drawing ratio increasing under the same temperature. New relationship of crystal form versus temperature was first discovered in which δˊform of Nylon 1010 could be gradually transformed into αform when drawn at higher drawing temperature. This is distict from the crystallization performance of Nylon 1010 under thermal effect without drawing. The measurements of orientation degrees, based on 2D WAXS experiments, showed that crystal orientations were solely decided by the drawing ratios. Furthermore, the d spacing of (002) reflections increased with the drawing ratios, which also showed the dependence of long axis increasment on the drawing orientation.