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中文
Table of Content
24 April 2003, Volume 24 Issue 4
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Preface
Studies on Effect of Gd(Ⅲ) on Ca(Ⅱ) Species in Human Interstitial Fluid by Mathematical Model Method
WANG Jin Ping, ZHANG Hai Yuan, NIU Chun Ji
2003, 24(4): 565-568.
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The effect of Gd(Ⅲ) on Ca(Ⅱ) species in human interstitial fluid was studied by mathematical model method. Meantime artificial neural network was applied to the estimation of lg β value of some complex. The results show that the variety of concentration of Gd(Ⅲ) has effect on Ca(Ⅱ) species. At the background the concentration of Gd(Ⅲ) in human interstitial fluid, Ca
2+
(71.0%), [Ca(HCO
3
)](9.5 %) and (6.0%) are main species. With the concentration of Gd(Ⅲ) rising, Gd(Ⅲ) firstly competes with Ca(Ⅱ) for PO
4
3-
and CO
3
2-
, then tends to compete for other biological low molecular weight ligands. This leads to Ca(Ⅱ) redistribution with the variety of concentration of Gd(Ⅲ).
Effect of Mutation of Cys33 and Cys34 in the α-Domain of Monkey Metallothionein-1 on the Protein Stability
YU Wen Hao, CAI Bing, GAO Yuan, CHEN Dong, HUANG Zhong Xian
2003, 24(4): 569-575.
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FPLC analysis of the recombinant protein of monkey metallothionein, MT1 and its C33M, C34S and C33M/C34S mutants shows that there were two stable components, f1 and f2. CD study and metal ion analyses indicate that multi components of the mutants relates not only to the binding mode and configuration between cysteins and cadmiun ions, but also to the number of the metal ions. This result also demonstrates that when the Cys33 and Cys34 of α domain of monkey metallothion were mutated into non cystein residues in an attempt of creating a metallothionein with β β domain structure, it led to a protein with multiple structures. It indicates that the α domain plays an important role in the protein stability, and also the distribution of cystein residues affects the formation of metal thiolate clusters and the tertiary structure of the protein significantly.
Structure, Preparation Mechanism and Thermo decomposition Process of LiMn
2
O
4
Precursor Prepared by Low heating Solid state Reaction
TANG Xin Cun, HE Li Ping, CHEN Zong Zhang, JIA Dian Zeng, XIA Xi
2003, 24(4): 576-579.
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The precursors were prepared from lithium hydroxide, manganese acetate and citric acid by the method of low heating solid state reaction with the molar ratio of Li
+
to Mn
2+
as 1∶2. The composition, structure, reaction mechanism and thermo decomposing process of the precursor were studied by using elemental analysis, IR spectrum, MS spectrum and TG/DTA analysis. The results show that the composition of precursor was fitted as LiMn
2
L(Ac)
2
, in which L represents citric acid radical and Ac was acetic acid radical. Spinel LiMn
2
O
4
began to form only at 350 ℃ for 4 h.
Synthesis and Crystal Structure of Anionic Zirconium(Ⅱ) Intermediate for Carbon-carbon Coupling: Li[Cp
2
Zr(C≡CPh)(η
2
∶1,2-PhC
2
C≡CPh)]
ZHAO Jian She, GU Ai Ping, HE Shui Yang, Choukroun Robert, Valade Lydie, Cassoux Patrick
2003, 24(4): 580-583.
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The unexpected anionic Zr(Ⅱ) complex [Cp
2
Zr(C≡CPh)(η
2
: 1,2 PhC
2
C≡CPh)]
-
was isolated from LiC≡CPh and Cp
2
ZrCl
2
in THF, giving clear evidence for a C-C coupling between two alkynyl moieties, one of them being η
2
bonded to the zirconium atom. The complex was characterized by elemental analysis, NMR, IR spectroscopy and X ray diffraction. The synthesis reaction mechanism was discussed.
Studies on Preparation and Properties of Mg
1-x
Ti
x
Ni (0≤x≤0.4) Alloys
YUAN Hua Tang, SONG He Nan, LI Qiu Di, FENG Yan, LI Zhi Yun, WANG Yi Jing
2003, 24(4): 584-587.
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The Mg based hydrogen storage alloys Mg
1- x
Ti
x
Ni(0≤ x ≤0.4) were successfully synthesized by mechanical alloying(MA). The X ray diffraction showed that the amorphous structures of the alloys were different from the diverse components and would be completed with increasing the ball milling time. It was found that the discharge capacity and the cycle life of the alloys were improved with Ti partial substitution. Among the alloys which were prepared by ball milling for 120 h, the discharge capacity of the Mg
0.9
Ti
0.1
Ni alloy electrode was 356.85 mA·h ·g
-1
(100 mA·g
-1
, -0.5 V
vs
. Hg/HgO) in the first charge discharge cycle, and Mg 0.7 Ti 0.3 Ni showed the best cycle life. It was also found that the Ti partial substitution was more effective to improve the anti corrosion behavior.
Chemical Modification of Abzyme with Deiodinase Activity
SUN Li Wei, LIU Li Yan, ZHAO Da Qing
2003, 24(4): 588-590.
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The abzyme with deiodinase activity was modified with diethyl pyrocarbonate(DEPC) and carbodiimide(EDC) respectively. The modified abzymes were dialyzed and their activities were compared with that of the native abzyme. The results indicate that the histidine residue is one of the essential groups in the abzyme, and the modification causes the catalytic activity a loss of 70%. The modification of the residues containing carboxyl group with EDC leads to a loss of 50% activity, indicating that acid amino residues play important roles in the catalytic reaction.
A Novel γ- Aminobutyric Acid Monolayer Modified Glassy Carbon Electrode for Simultaneous Determination of Dopamine, Uric Acid and Ascorbic Acid
ZHANG Lei, LIN Xiang Qin
2003, 24(4): 591-594.
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A novel monolayer γ aminobutyric acid covalently modified glassy carbon electrode has been fabricated via electrochemical oxidation procedure and was characterized with X ray photoelectron spectra(XPS) and cyclic voltammetry. The modified electrode was not only used to electrocatalyze the oxidation of dopamine(DA), uric acid(UA) and ascorbic acid(AA), but also gave rise to three well defined square wave voltammetric peaks, which can be used for simultaneous determination of these species in a mixture. The modified electrode shows good sensitivity, selectivity, stability and anti fouling effects.
A Novel Method for Determining the Principal Factor Number Based on Immune Recognition
SHAO Li Min, SHAO Xue Guang, LIN Xiang Qin
2003, 24(4): 595-598.
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Based on the idea of the immune algorithm, an immune recognition(IR) method was proposed to obtain the principal factor number of a data matrix. The original matrix is input to the algorithm as antigens, a number of antibodies are generated by means of PCA, elimination of antigens is performed in a recurrence procedure. An equation for the calculation of the affinity value is defined. In each elimination, an affinity value is calculated. According to the series of the calculated affinity values, the principal factor number of the matrix can be obtained. By the tests of both simulated and experimental HPLC DAD data, the IR method showed the superiority over the imbedded error(IE), the factor indicator function(IND) and the cross validation(CV). In treating experimental HPLC DAD data, due to the interference of the nonlinearity and the heteroscedastic noise, only IR can obtain the correct factor number, none of IE, IND or CV succeeded.
Studies on Both Voltammetric Behavior and Polarographic Catalytic Wave of Antitumor Irisquinone
SONG Jun Feng, HE Ping, GUO Wei
2003, 24(4): 599-604.
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The voltammetric behavior and the production mechanism of polarographic catalytic wave of irisquinone were studied by linear potential scan polarography, cyclic voltammetry, UV spectroscopy and constant potential electrolysis in both aqueous and N,N dimethyl formamide(DMF) media. In Na
2
B
4
O
7
KH
2
PO
4
(pH=7.7) buffer, the quinonyl group of irisquinone was first reduced in a 1e
-
, 1H
+
process to produce an intermediate free radical semiquinone, and the further reduction of the free radical semiquinone to the corresponding hydroquinone anion in the same way was accompanied by its chemical reaction. In DMF tetraethyl ammonium bromide(TEAB) media, the reduction of irisquinone was two successive single electron processes without the chemical reaction of the free radical semiquinone. All these processes yield the reversible reduction wave of irisquinone. When S
2
O
8
2-
was present, the free radical semiquinone of irisquinone was oxidized to regenerate the original quinonyl group, which resulted in the production of a polarographic catalytic wave. The apparent first order rate constant k
f
of the oxidation reaction of the free radical semiquinone of irisquinone with S
2
O
8
2-
was 3.3×10
6
L·mol
-1
·s
-1
.
Studies on the Detection of Weak Chemical Signal by Using a StochasticResonance Algorithm Based on Periodic Modulation
PAN Zhong Xiao, WU Xiao Jing, GUO Wei Min, CAI Wen Sheng, SHAO Xue Guang
2003, 24(4): 605-608.
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A new stochastic resonance algorithm for detection of weak chemical signal was proposed. The algorithm was achieved through periodic modulation to realize the system resonance. After a detailed discussion of the parameters in the system, a simulated signal and experimental noisy signals of a set of CCl
4
sample were analyzed by the method. It was proven that the proposed algorithm is very efficient in improving the signal to noise ratio of weak signals and a good performance of detection of weak signals with different S/N ratio can be ensured under the optimized conditions.
Studies on Labeling of Papain with Quantum DotsSynthesized in Aqueous Solution
LIN Zhang Bi, ZHANG Hao, CHEN Qi Dan, WAN Yi, YANG Bai, SU Xing Guang, ZHANG Jia Hua, JIN Qin Han
2003, 24(4): 609-611.
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The feasibility of the mercaptopropyl acid modified CdTe nanoparticles synthesized in aqueous solution to the labeling of biomoleculespapain via electrostatic interaction was studied in this paper. The absorption spectrum of CdTe papain solution became more flat than that of CdTe nanoparticles in the wavelength range from 400 to 600 nm. While the emission peak of CdTe papain solution underwent a red shift, the intrinsic emission band width was unchanged. The TEM images of monodisperse mercaptopropyl acid stabilized CdTe nanoparticles and CdTe papain solution were compared and the effect of pH of buffer solution was studied. It was proved that the red shift of the emission peak was the result of the electrostatic interaction between CdTe nanoparticles and papain.
Fluorescence Enhancing Method for the Determination of Human Serum Albumin with Functionalized CdS Nanoparticles as Fluorescence Probes
WANG Le Yu, ZHOU Yun You, ZHU Chang Qing, ZHANG Ming Cui, TAO Hai Sheng, WANG Lun
2003, 24(4): 612-614.
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CdS nanoparticles were prepared and modified with mercaptoacetic acid. The functionalized nanoparticles were water soluble and biocompatible and used as fluorescence probe in the determination of Human serum albumin(HSA) and γ globulin(γ G). Under the optimal conditions, linear relationships were found between the enhanced intensity of fluorescence and the concentration of protein in the range of 0.2 and 3.5 μg/mL for HSA and 0.2 and 11.0 μg/mL for γ G. The limits of detection were 0.09 μg/mL for HSA and 0.18 μg/mL for γ G.
Preparation and Investigation of a Solid-phase Microextraction Fiber Coated with Open Chain Crown Ether Containing Vinyl Group
YANG Min, ZENG Zhao Rui, QIU Wen Li, HUANG Zai Fu
2003, 24(4): 615-617.
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A novel solid phase microextraction(SPME) fiber coated with open chain crown ether(α,ω diallyltriethlene glycol, DATEG)/hydroxy terminated silicone oil(OH TSO) was prepared by sol gel approach and cross linking step. The adsorption and desorption properties of the new SPME fiber to polar compounds such as aromatic amines, non polar compounds such as benzene homologue and high boiling compound such as phthalate esters were investigated by SPME coupled with GC FID, and the results were compared with those of commercially available fibers. The new coating provided a better extraction efficiency and possessed a significantly stable performance at a high temperature(>300 ℃) in solvents, as well as long life span(>200 times). Under the experimental conditions used, the detection limits were 0.1-1.5 μg/L for aromatic amines and 0.03-0.3 μg/L for benzene homologue, and the precisions were below 8%(n =5).
Determination of Urapidil by Flow Injection Chemiluminescence
LANG Hui Yun, LI Ya Rong, ZHANG Wei Ping, ZHANG Xiu Jun, SHEN Yie Hua
2003, 24(4): 618-620.
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A reverse flow injection chemiluminescence(CL) method for the determination of urapidil was firstly described. It was found that the CL intensity from the Luminol ClO
-
system could be enhanced in the presence of urapidil. The increase of CL emission was correlated with urapidil mass concentration in the range from 0.2 to 100 μg/mL, the detection limit was 0.01 μg/mL and the relative standard deviation was 1.3%(ρ =4 μg/mL, n =11), a sampling frequency of 150 h
-1
was attained. The method was applied to the determination of leucoge in pharmaceutical preparations with recovery of 101.0% and 101.3%.
Determination of Fat soluble Components in Danshen by High-ResolutionElectrospray Ionization Time-of-flight Mass Spectrometry
YU Wen Jia, HE Jian, SHEN Jin Can, WANG Xiao Ru
2003, 24(4): 621-623.
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An excellent analytical tool for the separation and analysis of TCM(Traditional Chinese Medicine) by using HR ESI TOF MS(High Resolution Electrospray Ionization Time of flight Mass Spectrometry) was developed. A home built HR ESI TOF MS was applied to detect fat soluble components in Danshen(Salvia miltiorrhiza Bage) directly. Compared with the method of HPLC ESI MS(High Performance Liquid Chromatograph Electrospray ionization Mass Spectrometry) method, HR ESI TOF MS method is more accurate, quick, simple and reliable, so the method can become an effective tool for the quality control of TCM.
Studies on Antibody Immobilization Based on o-Phenylenediamine Electropolymerized Films for Immunosensors
LI Ji Shan, WU Zhao Yang, WANG Hua, SHEN Guo Li, YU Ru Qin
2003, 24(4): 624-626.
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A novel method based on electropolymerized films(Eps) is proposed for immobilizing antibodies(antigens) through a polyelectrolyte mediated layer. The o phenylenediamine Eps are deposited on the surfaces of quartz crystal microbalance(QCM) with an electropolymerized method using o phenylenediamine as the precursor. After self assembling a polystyrenesulfonate(PSS) layer on the Eps, the immobilization of goat anti IgG antibody, as an example, is investigated. The effects of experimental conditions about PSS self assembly, IgG antibody immobilization and immunoreaction et al. on the performances of immunosensor were discussed respectively. The QCM immunosensor can be used to quantitatively determine NHIgG in the range of 1.67-196.08 μg/mL. Moreover, the PSS and protein layer can easily be removed by shifting the pH, making the immunosensor regenerable.
Structure Characterization and Resolution of Spiro cyclopropane Compounds Containing Multiple Chiral Centers
FU Yu Qin, ZHANG Xi Yun, CHEN Qing Hua
2003, 24(4): 627-631.
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The functionalized spiro cyclopropane compounds containing multiple stereogenic centers 1a-1g were obtained in good yields with e.e.≥98%. The chemical structure of the interesting compounds 1 was established on the basis of their spectroscopic data, such as UV, IR,
1
HNMR,
13
CNMR and MS. The spectroscopic characteristics of these title compounds are reported in detail. This result can provide an important and valuable value to recognize the structure of some complex molecules containing spiro cyclopropane skeleton with multiple chiral centers.
A Facile Syntheses of (Z)-2-Phenoxy(THIO)methylene-γ-pentanolide and (Z)-2-Phenoxy(THIO)methyl-2-penten-γ- lactone
LIU Li Jun, LUO Fen Tair
2003, 24(4): 632-635.
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Starting from 3 phenoxy(thio) 1 propyne 1a(1b), 5 phenoxy(thio)
3
pentyn 2 ol 2a(2b) were obtained by Grignard reaction. After treating 2a(2b) with Jones reagent, hydroiodination of 3a(3b) with a reagent system of TMSCl/NaI/H
2
O in CH 3CN, the conjugated product (Z) 5 phenoxy(thio) 4 iodo 3 pentene 2 one 4a(4b) and de conjugated product (Z) 5 phenoxy(thio) 4 iodo 3 pentene 2 one 5a(5b) were generated. In the presence of Pd(PPh
3
)
4
, Et 3N, and CO in toluene, the intramolecular cyclization of reducing products of 4a(4b) and 5a(5b) afforded the target compounds (Z)
2
phenoxy(thio) methylene γ pentanolide 9a(9b) and (Z)
2
phenoxy(thio) methyl 2 penten γ lactone 8a(8b) respectively in good yields. All compounds have been fully characterized by
1
H and
13
CNMR, IR and MS spectroscopy. The one pot deconjugation and hydroiodination of 3a(3b) with a reagent system of TMSCl/NaI/H
2
O in CH
3
CN was the key step.
In vitro Studies on the Immunoadsorbent for Removal of IgA in IgA-Nephropathy (Ⅱ)
CHU Jia Qiang, YU Yao Ting, ZHANG Wei Hua, CHEN Jian Jun, ZHU Bo Ru, LIU Jing Duo
2003, 24(4): 636-638.
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Bead type agarose as a carrier was prepared and activated by glycidyl 1,4 butanediol which could easily couple with human IgG because it has a long spacer, thus reducing the hinderence effect of IgG coupling reaction. In vitro experiments showed that the immunoadsorbent could adsorb 60% of IgA in plasma which is much higher than the CDI coupling method of 35%.
Selective Reductions of Steroidal Ketones with Keto-groups in the Nucleus and Side-chain
CUI Jian Guo, ZENG Long Mei, SU Jing Yu
2003, 24(4): 639-642.
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On the study of reduction of some steroidal ketones with keto groups in the nucleus and side chain, it was found that the reduction with NaBH
4
CH
3
OH, in the presence of different kind of metal ions such as Cd
2+
, Co
2+
, Ce
3+
etc., may lead to different regio and stereo selective results and obtain different products.
Combined Removal of Arsenic(Ⅴ) and Fluoride from Drinking Water by Fe(Ⅲ)-loading Ligand Exchange Cotton Adsorbent
ZHAO Ya Ping, WANG Jun Feng, CHEN Fu Hua
2003, 24(4): 643-647.
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The concentration effects of combined removal of arsenate and fluoride(F) were studied by novel bead Fe(Ⅲ) loading ligand exchange cotton cellulose adsorbent in batch and column experiments. As(Ⅴ) and F could be simultaneously removed by the adsorbent from drinking water highly and selectively after three adsorption regeneration readsorption cycles. The saturation adsorption capacity of As(Ⅴ) and F reached up to 15 mg/g. Indexes of effluent were in good agreement with the living drinking water health standard of China, especially the arsenic concentrations below 0.01 mg/L and satisfy WHO stringent drinking water standards. It shows that the adsorbent may be a promising adsorbent in the region of arsenic and fluoride coexisting.
A Novel Method for the Synthesis of 1,3,5-Triarylpyrazoles
WANG Bing Xiang, LIU Wei Wei, HU Hong Wen
2003, 24(4): 648-650.
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A novel and one pot procedure was developed to prepare the derivatives of 1,3,5 triarylpyrazoles(3a-3g) by tetrakispyridine cobalt(Ⅱ) dichromate (TPCD) promoted dehydrogenation of 1,3,5 triarylpyrazolines to their aromatic forms. Advantageously, the intermediates 1,3,5 triarylpyrazolines were generated by the reaction of chalcones with phenyl hydrazine need not to be separated and can be further converted to 1,3,5 triarylpyrazoles. It is worth noting that 1,3 diphenyl 5 [2 (4 bromophenyl)ethenyl] pyrazoline(2h), which contains a double bond, afforded the corresponding compound 3h in a yield of 68%. This general method features cheap reagents, simple working procedure and gives the products in moderate and high yields(65%-93%).
Novel Synthesis of Bis(4-bromophenyl)phosphine Oxide and Its Application in the Preparation of Water-soluble Phosphine Precursors
ZHANG Tian Zhu, XU Li Jin, CHEN Yong, MO Jun, SUN Wen Hua
2003, 24(4): 651-653.
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A more convenient and economic method has been developed for synthesizing bis (4 bromophenyl)phosphine oxide in a high yield, which was introduced to prepare three water soluble phosphine precursors successfully. All new compounds were fully characterized by IR,
1
HNMR,
13
CNMR,
31
PNMR, MALDI TOFMS and elemental analyses.
Synthesis and Insecticidal/Acaricidal Activities of New Pyrethroid Esters Containing Pyridine Ring
MA Jun An, HUANG Run Qiu
2003, 24(4): 654-656.
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Preparations of new pyrethroid esters(5, 6) containing a pyridine ring in the acid moiety were described. The α and β form of α cyano 3 phenoxybenzyl esters 6 were separated chromato graphically. These compounds were screened for insecticidal activities against Mythimna separata(W.) and Aphis fabae and for miticidal activity against Tetranychus urticae. Compound 5 showed 85% mortality against Mythimna separata(W.) at 250 mg/L, and 6 β had more miticidal activity on Tetranychus urticae than fenvalerate at a mass fraction of 200 mg/L.
Studies on Recognition and Dynamic Analysis of Polydiacetylene Langmuir-Schaefer Films Functionalized with Glycolipid
FAN Yi, ZHANG Li Gong, HOU Fang Yu, MA Bao Liang, SHEN De Zhen, LI Ya Jun
2003, 24(4): 657-661.
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As a potential materials for optic biosensor, the surface properties of the polydiacetylene films fuctionalized with glycolipid on pure water are interesting and important. Pressure area isotherms of mixed α D mannoside hexadecyl(MC
16
) and 10,12 pentacosadiynoic acid(PDA) monolayers were studied. The interfacial behavior at the air/water interface show that MC
16
/PDA monolayers on the water surface have a good miscibility. The interactions of MC
16
with Escherichia coli(E.coli) jm 109 were studied by rapid colorimetric transitions on the MC
16
/PDA Langmuir Schaefer (LS) films. This colorimetric transition can be quantified by UV Vis absorption spectra. The kinetic experiments show that the color change induced by the addition of E.coli reaches a plateau after 15 min, although the change becomes apparent within 3 min. Kinetics of the process was discussed. We estimate that one Escherichia coli can only bind two MC
16
molecules.
Preparation of Stable Fluorescence CdTe Material by Hydrothermal Method
ZHANG Gang, YU Yi, ZHANG Hao, HAN Yu, DI Yan, ZOU Yong Cun, XIAO Feng Shou, YANG Bai
2003, 24(4): 661-665.
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A kind of stable fluorescence CdTe nanostructure material encapsulated by silica has been synthesized hydrothermally from the assembling of nanosized CdTe particles, surfactant and silicon source, and this composite nanostructure was characterized by means of a series of techniques(such as TG DTA, EDX, TEM, fluorescence spectra and N
2
adsorption). Furthermore, the surfactant was removed by calcinations, metal oxide was removed by nitric acid and porous silica material was obtained.
Photoacoustic Spectroscopy Study of the Co-luminescence Effect of Lanthanide-dibenzoylmethane, Phenanthroline Complex Powders and Their Doped Silica Gels
YANG Yue Tao, ZHANG Shu Yi
2003, 24(4): 662-670.
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Eu(Dbm)
3
·Phen and Eu
0.8
Ln
0.2
(Dbm)
3
·Phen(Ln: Er
3+
, Y
3+
; Dbm: dibenzoylmethane; Phen: phenanthroline) complex powders and their doped silica gels have been prepared. Their photoacoustic(PA) spectra have been detected and interpreted for the first time. In the region of ligand absorption, the PA intensity decreases for Eu
0.8
Er
0.2
(Dbm)
3
·Phen, Eu(Dbm)
3
·Phen and Eu
0.8
Y
0.2
(Dbm)
3
·Phen respectively. While for Eu(Dbm)
3
·Phen and Eu
0.8
Y
0.2
(Dbm)
3
·Phen doped silica gels, the reverse is true. It is found that the PA intensity bears a correlation with the energy transfer processes of the complexes. The additions of Er
3+
, Y
3+
ion change the relaxation processes of the complexes and the relaxation processes of ternary complexes are different in the two kinds of solid states. The changes of fluorescence spectra turn out to be complementary to the PA spectra. The luminescence properties of the complex powders and their doped silica gels are interpreted in depth from two aspects: nonradiative process and radiative process.
Multiphoton Ionization and Dissociation of Acetone Clustersand the Strucure Calculation
HU Zhan, JIN Ming Xing, XU Xue Song, LIU Hang, DING Da Jun
2003, 24(4): 671-674.
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Clusters and their fragments contain up to 12 acetone molecules, produced by supersonic expansion jet, are observed in the time of flight mass spectrum under 355 nm laser irradiation. The calculations using density functional theory give structures and the energies of the ground state acetone clusters for n =2-5. The results show that a near perpendicular structure is steady for 2 acetone cluster, while a circle structure is more steady for the clusters contain 3 to 5 acetone molecules.
Ab initio Study on the Nonlinear Optical Properties of (H
2
O)
2
and (HCl)
2
WANG Yi, LI Zhi Ru, WU Di, HAO Xi Yun, ZHANG Man, CHU San Yang, SUN Chia Chung
2003, 24(4): 675-677.
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The static dipole moments(μ
0
), polarizabilities(α
0
) and first hyperpolarizabilities (β
0
) of (H
2
O)
2
and (HCl)
2
dimers are investigated by means of ab initio methods with various basis sets, ADZ, ADZ+BF, ATZ, and ATZ+BF at MP2 level. Through analysis and comparison, we found that the results of the dimers are convergent when the basis sets are not less than ATZ and the electron correlation is important. In order to show the contributions from intermolecular interactions to nonlinear optical properties, the counterpoise method is applied. The calculated results show that the μ
z
and β
0
values of hydrogen bonding dimers (H
2
O)
2
and (HCl)
2
are smaller than those of the sums of the values of subsystems. In addition, for μ
z
and β
0
, the ratios of contribution from π type H bond to that of the total intermolecular interactions in the β
0
properties are small.
Density Functional Theory Study of Structures and Spectroscopic Properties of Cu
n
-
and Cu
n
CO
-
(n=2-7)
WANG Yan Jin, CAO Ze Xing, ZHANG Qian Er
2003, 24(4): 678-681.
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Equilibrium geometries, stabilities, preferred fragmentation channels, CO adsorption features and spectroscopic properties of Cu
n
-
and Cu
n
CO
-
were investigated by the density functional theory(DFT) combined with the relativistic effective core potentials. The calculated results show that the odd numbered copper cluster generally has a relatively higher ionization potential than the even numbered species, and CO dissociation from the odd Cu
5
CO
-
requires the largest energy of 1.21 eV among such copper cluster monocarbonyls here. Such high stabilities of the odd copper cluster anions and Cu
5
CO
-
are consistent with the closed shell effect within the jellium shell model approximation. B3LYP fragmentation energies reveal that the preferred dissociation channel of the odd numbered copper cluster anion is the loss of copper dimer Cu
2
, while the loss of Cu is favored in energy for the even numbered copper cluster anion. On the basis of current DFT calculations, the size dependences of static polarizabilities and the features of CO adsorption on copper clusters were discussed.
Ab initio Investigation of the Rearrangement Between the Isomers of C
36
Fullerene Derivative(C
36
OH)
+
──Intramolecular OH shift
XU Xiu Fang, YANG Zuo Yin, WANG Gui Chang, SHANG Zhen Feng, WU Ben Xiang, PAN Yin Ming, ZHAO Xue Zhuang
2003, 24(4): 682-685.
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The mechanism of the rearrangement between the isomers of (C
36
OH)
+
, one of C 36 fullerene derivatives, has been investigated by ab initio calculation at HF/STO-3G level. The result shows that isomer 2 is thermodynamically the most stable, and kinetically it is much easier to convert isomers 1 and 3 into 2 than to convert 2 into 1 and 3 judging from the calculated energy barriers. On the other hand, the distribution of the charges on the cage of the (C
36
OH)
+
isomers implies relatively more probability for the addition of OH group to the 1,4 sites in the six membered ring locating at the equatorial belt of the C 36 cage than to the other sites, which agrees with the themodynamic stability of the C
36
(OH)
2
isomers.
Theoretical Studies for the Potential Energy Surface and Rovibrational Spectra of Ne-HCl
LI Jiang, ZHU Hua, XIE Dai Qian, YAN Guo Sen
2003, 24(4): 686-689.
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The intermolecular potential energy surface for Ne HCl has been calculated by supermolecule method by using the CCSD(T) approach with a large basis set containing the midpoint bond function set 3
s
3
p
2
d
. Two local potential minima are found to be located at the linear Ne ClH and Ne HCl geometries. The rovibrational energy levels are calculated with Lanczos method. The calculated results show that the ab initio potential support five vibrational bond states for Ne HCl and seven vibrational bond states for Ne DCl, respectively. The calculated vibrational frequencies and rotational transition frequencies are in good agreement with the available observed results.
Effects of Critical Solvation on Hydrolysis Kinetics
YUAN Pei Qing, CHENG Zhen Min, LIU Tao, YUAN Wei Kang
2003, 24(4): 690-693.
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The work presented in this paper focuses on employing Transition State Theory and Kirkwood dielectric model to interpret the solvation effects on hydrolysis of methyl acetate under near or supercritical conditions. The experimental data show that the apparent activation energy of hydrolysis is (23.5±8.29) kJ/mol, which is much lower than that obtained by using the conventional technique, the intricate solvation effects observed in the experiment may cause a minimum activation volume at the temperature near to the critical temperature, and the reaction field shows a good linear relationship with ln
kc
, which can be utilized to correct the effect of pressure on reaction kinetics, also S
N
2 reaction mechanism can be validated from several aspects.
Proton-conducting Polymer Electrolyte Doped with Molybdophosphoric Acidand Ammonium Molybdophosphate
ZHAO Xu, XIONG Huan Ming, DING Hong, XI Chun Yu, CHEN Jie Sheng
2003, 24(4): 694-697.
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Polymer inorganic composite films of PEO-12-NPMA(NPMA: ammonium molybdophosphate; PEO: polyethylene oxide, Aldrich, M
w
=600 000) and PEO-12-PMA(PMA: molybdophosphoric acid) have been prepared through a film casting method. The Keggin anions and the polymer molecules are linked together to form a new composite compound of PEO-12-PMA, which has a gauche conformation of PEO being changed to a certain degree. However, no new phase is observed in the PEO-12-NPMA composite film system. The protons in the composite materials form H bonds with the external oxygens of Keggin anions and the ether oxygens of PEO. The H bonding system of the PEO-12-NPMA film is superior to that of the PEO-12-PMA composite film. As a result, the conductivity of the PEO-12-NPMA film is higher than that of PEO-12-PMA film under the same condition.
Mullite Synthesis at Low Temperature and Its Crystal Structure Characterization
LIU Cong Hua, DENG You Quan, HUANG Quan, LI Qiang, GAO Xiong Hou, TAN Zheng Guo
2003, 24(4): 698-702.
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Vanadium mullite had been surprisingly observed in the phase transition of kaolin in the presence 1%-5% vanadium at about 700 ℃,and quite a pure vanadium mullite could be obtained through the process of acid & base leaching reaction and separation. In addition, unit cell parameters of various mullites were especially determined by XRD and the unit cell volume of vanadium mullite formed at a low temperature was found to be greater than that of the common mullite, which could be deduced that vanadium incorporated into the mullite framework. Furthermore, the reaction process of vanadium mullite formation could be expressed as low melting vanadium kaolin eutectic transition.
A Study on Hydrogen Bond in Coal Macerals with In situ Diffuse Reflectance FTIR by Using a New Experimental Method
LI Dong Tao, LI Wen, SUN Qing Lei, LI Bao Qing
2003, 24(4): 703-706.
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A new method using the small porcelain as the reactor combined with increasing the flow rate of carrier gas was proposed, which has the advantage of excluding the condensation of volatile produced by heated solid samples on the windows during in situ diffuse reflectance FTIR experiment. Moreover, the feasibility of this method was also discussed. Using this method, the distribution and thermal stability of hydrogen bonds in coal macerals obtained from two coals were studied. The results show that the differences between the distribution of hydrogen bonds formed by hydroxyl group in the macerals of two coals were very similar; For the vitrinites, the thermal stability of SH-N, carboxylic acid dimmers and self associated OH is higher than those in inertinites, but for OH-N and hydroxyl tetramers and OH-OR
2
, there is no obvious laws. For OH-π, its content was increased with increasing the temperature until 350-380 ℃, and then decreased with further heating. The variation of hydrogen bonds in macerals reflects the difference in their structure.
Preparation of Silver Colloid by Hydrochlorinated Hydroxy Amine Method and Its Surface Enhanced Raman Substrate
LI Xiao Ling, XU Wei Qing, ZHANG Jun Hu, JIA Hui Ying, ZHAO Bing, YANG Bai
2003, 24(4): 707-710.
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A new method--hydrochlorinated hydroxy amine method for preparing silver colloid was reported, and the formation process of silver nanoparticles was studied by UV Vis spectroscopy and TEM. From the results, we can see the particle formation process is as follows: small particles were formed at the beginning of the reaction, and then they aggregate to large ones rapidly, then the large particles decomposed to small ones gradually. The TEM images showed directly the same process as the results from the UV Vis spectra, indicating that the particle size distribution became more and more uniform. In addition, we transferred the Ag nanoparticles to the glass slide by electrostatic interaction to produce SERS active substrates. Strong SERS signals can be obtained on such substrates.
Preparation of Polyethylene/Montmorillonite(MMT) Nanocomposite by in situ Polymerization
YANG Feng, ZHAO Hai Chao, ZHANG Xue Quan, HUANG Bao Tong, FENG Zhi Liu
2003, 24(4): 711-714.
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Polyethylene(PE)/montmorillonite(MMT) nanocomposites were prepared by in situ coordination polymerization by using a MMT MgCl
2
TiC
l4
catalyst activated by Al(Et)
3
. The catalyst was prepared by firstly diffusing MgCl
2
into the swollen MMT layers, followed by loading TiC
l4
on the inner/outer layer surfaces of MMT where MgCl
2
already deposited on. The intercalation of MMT layers by MgCl
2
and TiC
l4
was demonstrated by the enlarged spacing between neighboring layers measured from WAXD patterns. The nano scale dispersion of MMT layers in the polyethylene matrix was characterized by WAXD and TEM observation. As consequence, tensile strength and tensile modulus of the nanocomposite materials were significantly improved as compared to virgin polyethylene of comparable molecular weight. The strong interaction between the uniformly dispersed nano dispersed montmorillonite layers and the resin matrix was thought to account for the remarkably enhancement in tensile properties.
Linear Viscoelasticity Calculation of Exfoliated Polymer/Layer Silicate Nanocomposites
YU Wei, WU Zeng Gang, ZHOU Chi Xing, ZHAO De Lu
2003, 24(4): 715-718.
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The linear viscoelasticity of polymer/layer silicate nanocomposites was calculated on the basis of dual constraint model. It was suggested that the increase of elasticity of nanocomposites at a low frequency was due to the long relaxation mode of tethered polymer chain.
Synthesis and Adsorption Properties of New Type Chelating Cellulose Resins Containing Sulfur and Nitrogen
DONG Qi Gong, ZHANG Jun Ping, LI Ya Rong, JIA Ying Qi
2003, 24(4): 719-723.
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Rice husk cellulose was treated by thionyl chloride to give 6 chlorodeoxycellulose(6 CDC), which was treated with anhydrous hydrazine, ethylenediamine, diethylenetriamine, triethylenetetramine, 1,4 diaminobutane and hexamethylenediamine respectively in DMSO at 100 ℃ giving six chelating resins(ADC-1-ADC-6). The cross linking of ADC with chloromethylthiiane in the presence of alkaline gave six new chelating resins(TADC-1TADC-6) which contain sulfur and nitrogen. The conditions of synthesis for CDC, ADC and TADC were studied. The adsorption properties of ADC-resins and TADC resins for metal ions were thoroughly studied. It was found that ADC resins possessed high capacities for Hg
2+
(about 0.5 mmol/g) and TADC resins did for Hg
2+
(1.1 mmol/g) and Ag
+
(1.9 mmol/g). The effect of pH value on adsorption capacities of ADC resins was more remarkable than on TADC resins. The adsorption capacities of ADC resins and TADC resins were in the order Hg
2+
>Cu
2+
>Ni
2+
and Ag
+
>Hg
2+
>Cu
2+
and they can be reused by desorption of 15% ammonia hydroxide.
Synthesis and Characterization of a Novel Azo Polyelectrolyte with Surface Relief Structures
WANG Guo Jie, HE Ya Ning, WANG Xiao Gong
2003, 24(4): 724-727.
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The surface relief gratings(SRG) of azo polymers formed upon irradiation with an interference pattern of coherent light have attracted great attention recently. In this study, a novel photodynamic azo polyelectrolyte was synthesized by incorporating azobenzene units into poly(acrylic acid) backbone. The polymer structure and properties were characterized by
1
HNMR, elemental analysis, GPC, TA, UV Vis and contact angle measurement. The spin coated films on glass substrates were prepared from DMF solutions of the azo polyelectrolyte. The atomic force microscopy image of the films, which were exposed to the interference pattern of p polarized Ar
+
laser beams at 140 mW/cm
2
, showed that the synthesized azo polyelectrolyte possessed a good photodynamic property. Good quality SRG structures were clearly generated(the depth from peak to trough was 100 nm).
Hydrogen-bonding Interaction of Ethylene Vinyl Alcohol Copolymers and Its Relation to the Chain Structures as Studied by VT
1
H NMR Spectroscopy
ZHANG Qiu Jin, CHEN Qun
2003, 24(4): 728-730.
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The hydrogen bonding interaction of ethylene vinyl alcohol copolymer in DMSO solution was studied by variable temperature
1
HNMR spectroscopy. It was found that the signals of the hydroxy protons of vinyl alcohol units shift to the upfield linearly with the increase of temperature, indicating the formation of the hydrogen bonds between the hydroxy groups and the solvent. The shift rates of these signals were found to be dependent on the chain structure and to decrease in the order of EVE>mEVV>rEVV>mmVVV>mrVVV>rrVVV triads, where m and r denote meso and racemic. Such a result indicates that the strength of hydrogen bonds formed by the hydroxy groups is dependent on the comonomer sequence and the stereo chemical structure of the copolymer. Contrary to the behavior of the hydroxy groups, the methine signals of the V unit were found to shift to the downfield linearly with the increase of temperature, demonstrating that the formation of hydrogen bonds also affects the chemical shift of protons on the neighboring group.
Application of Lorenz Function Model of Refractive Index Distribution in Gradient-index Polymer Optical Fiber Rod
CHU Jiu Rong, WEN Xu Ming, DING Wen, XU Chuan Xiang
2003, 24(4): 731-734.
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Refractive index distribution of gradient index polymer optical fiber(GI POF) was simulated by Lorenz function and model of refractive index distribution was found firstly, which included three basic parameters: initial concentration, molecule bulk of dopant monomer and polymerization temperature. The refractive index distribution of GI POF adulterated by kinds of high refractive index dopant monomer in PMMA was predicted by the Lorenz function model. It was found that effect of dopant monomers refractive index on gradient index was larger than that of molecule bulk; adulterate efficiency of diphenyl sulfide(DPS) was the highest in kinds of inertia dopant monomers; and adulterate efficiency of vinyl benzoate(VB) was the highest in kinds of co polymerization dopant monomers.
Studies on the Photosensitivity of Cationic Polymerization Photoinitiator [Cp-Fe-arene]BF
4
WANG Tao, HUANG Yu Li, SHI Shu Jian
2003, 24(4): 735-738.
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The photosensitivity in the expoxide system of several arene cyclopentadienyl iron tetroflouroborate salts with different structures was studied. Among them, [C
5
H
5
Fe
2
,5 (CH
3
)
2
CO
-
C
6
H
3
]BF
4
and [CH
3
CO
-
C
5
H
4
Fe
2
,4 (CH
3
)
2
C
6
H
4
]BF
4
are new compounds. The study shows that all the salts have two main absorptions near 370 and 450 nm. It also shows that those with CC group and CO group have a stronger absorption and higher photosensitivity, and can be suitable for the light cured reaction irradiated by high pressure mercury lamp. Meanwhile, the study also shows that some kinds of organic expoxides including multifunctional epoxy resins, cycloaliphatic epoxides and glycidylethers can be initiated by these salts. Heating or adding BPO could prompt the rate of polymerization significantly.
Concentrated Emulsion Polymerization of the Styrene Initiated by Redox Initiator System at Lower Temperature
ZHANG Hong Tao, CAO Jian Hua, WANG An Lin
2003, 24(4): 739-744.
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Polystyrene latex particles were prepared by concentrated emulsion polymerization by using (CHPO) TEPA as the redox initiator system and SDS CA as the surfactants. The effects of polymerization condition on the polymerization process were investigated. The effects of surfactant, initiator, temperature and monomers volume fraction on the stability of emulsion, the kinetic process of polymerization and the average size of PS latex particles were discussed. The morphology and size of PS particles were obtained by TEM. The kinetic equation Rp=K[M]
0.36
[I]
0.49
[E]
0.72
and apparent activation energy Ea=19.72 kJ/mol at 30 ℃. The molecular weight was measured by viscosity method in the range of 2×10
6
-4×10
6
.
Dynamic Wettability of Superhydrophilic TiO
2
and TiO
2
SiO
2
Surfaces
FENG Wen Hui, GUAN Zi Sheng, JIANG Feng Zhi, ZHANG Jin Biao, SONG Yan Lin, JIANG Lei
2003, 24(4): 745-747.
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The dynamic wetting of water spreading on TiO
2
and TiO
2
SiO
2
films prepared by sol gel method and subsequently treated by air plasma and UV irradiation was investigated. Water completely spread on TiO
2
surface within 3 s and its dynamic contact angles can be expressed by a power law θ
d
= k(t+a)
-n
with the n value 0.98. Less than 50%(molar fraction) SiO
2
addition can accelerate the dynamic water spreading rate on the TiO
2
SiO
2
films and the optimum molar fraction of SiO
2
amount corresponding to as annealed, air plasma, and UV irradiation treatment process is 15%, 10% and 20%, respectively.
Studies on Optically Active Poly(menthyl methacrylate) by Anionic, GTP and Radical Polymerization Methods
XU Yong An, XUE Hong, ZHANG Suo Bo, GAO Lian Xun, DING Meng Xian
2003, 24(4): 748-750.
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The optically active polymers of (-) menthyl methacrylate were obtained by anionic, group transfer polymerization(GTP) and radical polymerization methods. The influences of different polymerization methods on specific rotation, yield and stereoregularity of polymers were studied. In the fluorene lithium and (S,S) (+)
2
,3 dimethoxy 1,4 bis(dimethylamino)butane complex initiative system, the specific rotation values rise slightly with the increase of molecular weight. There is no obvious difference in the specific rotation values of PMnMAs obtained by different polymerization methods, but there is an obvious variation in stereoregularity of the polymers. And the change of the optical activity of PMnMA is slight as compared with the variation of the stereoregularity. The tacticity of polymers is mainly syndiotactic.
Prediction of the Contribution of Internal Energy to the Elastic Force
SUN Juan, YANG Xiao Zhen
2003, 24(4): 751-752.
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Conformational elasticity theory of chain molecule" proposed by our group was used to explore the contribution of internal energy to elastic force(f
e
/ f). 1,4 Polybutadiene(cis and tran) were studied. The calculated f
e
/ f for cis polymer is consistent with experimental data, while a little difference for the trans polymer, which needs more experimental data to support. The results also show that f
e
/ f is dependent on chemical structure and strain.
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