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Archive By Volume
Acta Chimica Sinica 2002 Vol.60
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Original Articles
Transition from precipitation to vesicle and formation of aqueous two-phase in the system of catanionic surfactants within short chain fatty alcohol/water
TANG SHIHUA;HUANG JIANBIN;DAI LERONG;WANG CHUANZHONG;FU HONGLAN
Acta Chimica Sinica 2002, 60 (1): 1-3.
Published: 15 January 2002
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1652
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In this work a way of transition from precipitation to vesicle through addition of short chain fatty alcohol was developed. By adding 7%~14%(V/V) of 1-propanol or 10%~21%(V/V) of ethanol at 30℃ the precipitation of catanionic surfactant was dissolved to give a two liquid-phase system. The photography of TEM demonstrated that vesicles exist in the lower phase. The phenomenon of double refraction was found in the upper phase.
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Cited: Baidu(
18
) CSCD(
9
)
Original Articles
Design and properties of a novel electrically bistable organic material
WU FANGHUI;ZHOU ZHENGRONG;WANG QUANRUI;DING ZONGBIAO;TAO FENGGANG;XIA ;XU WEI;HUA ZHONGYI
Acta Chimica Sinica 2002, 60 (1): 4-6.
Published: 15 January 2002
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1581
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A novel spiro-annulated compound 3, 9-di(dicyanomethylene)-2, 4, 8, 10-tetrathiaspiro [5, 5] undecane (SCN) has been designed and synthesized as an organic electrically bistable material. The crystal structure of SCN has been studied. Silver/copper-SCN charge transfer complexes were obtained and both of them show good bistable states and thermal stability.
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Cited: Baidu(
9
) CSCD(
2
)
Original Articles
Theoretical study of the pyridine-BH~3 interaction complex
MENG FANCUI;BU YUXIANG;LIU CHENGBU
Acta Chimica Sinica 2002, 60 (1): 7-12.
Published: 15 January 2002
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1541
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Geometries and dissociation energies are predicated at MP2-/6-31+G^* and B3LYP/6-31+G^* levels respectively. Single point energy calculations using CCSD method at 6-31+G^* level are also carried out on the four obtained conformers to confirm the results. Then vibrational analysis are made using B3LYP/6-31+G^* method. Single point energy calculations at much larger basis sets and natural bond orbital analysis have been also carried out on th eoptimized conformers. The outcome indicates that the conformer with the boron atom directly connected to the nitrogen atom is the most stable one with a dissociation energy of 141.50 kJ/mol. The results for the conformer with the nitrogen atom close to one of the hydrogen atom in BH~3 differ from each other at MP2 and B3LYP levels. The stability of the other two conformers (with boron atom lying on one of the pyridine carbons) is between that of the aforementioned two conformers and their dissociation energies are 15.18 and 14.06 kJ/mol (MP2/6-31+G^*), respectively.
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Original Articles
Effects of temperature on the kinetic performance of hydrogen storage alloy MINi~3~.~7~5Co~0~.~6~5Mn~0~.~4Al~0~.~2
YUAN XIANXIA;XU NAIXIN
Acta Chimica Sinica 2002, 60 (1): 13-18.
Published: 15 January 2002
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1410
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Effects of temperature on the kinetic performance of hydrogen storage alloy MINi~3~.~7~5Co~0~.~6~5Mn~0~.~4Al~0~.~2 have been systematically investigated in the temperature range from -20℃ to 85℃. The results show that temperature has pronounced effects on the characteristics of the electrode. With the increase of temperature, the polarization resistance R~t, the ohmic resistance R~0, the cathodic polarization overpotential, the anodic polarization overpotential, and the activation overpotential η~a and the concentration overpotential η~c under anodic polarization decrease, while the exchange current density i~0, the symmetry factor β, and the hydrogen diffusion coefficient D increase. At lower discharge current densities, charge-transfer is the rate-determining step of the electrode reaction, at higher discharge current densities, the diffusion of hydrogen in the bulk of the alloy is the rate-controlling step, whereas at medium discharge current densities, the electrode reaction is under mixed control of charge-transfer and hydrogen-diffusion. The activation energy for charge-transfer and for hydrogen-diffusion in the electrode are calculated to be 28.1 kJ.mol^-^1 and 19.9 kJ.mol^-^1 respectively.
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Original Articles
Thermokinetic reduced parameter method for slower opposing reactions
CHEN YONG;YAN HUA;ZHANG BIN;ZENG XIANCHENG
Acta Chimica Sinica 2002, 60 (1): 19-23.
Published: 15 January 2002
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According to the theoretical basis of thermokinetics, the thermokinetic reduced parameter equation of opposing reaction has been derived, and the mathematical models of the reduced parameter method for opposing reaction have been established. Only needing the thermoanalytical data at the characteristic time parameter t~m and 2t~m from a single thermoanalytical curve, both the reduced energy and the reduced time parameter can be easily obtained, and then the rate constants and the equilibrium constant of slower opposing reaction can be easily obtained, and then the rate constants and the equilibrium constant of slower opposing reaction can be calculated conveniently. In order to test the validity of this method, the thermokinetics for the proton-transfer reaction of nitroethane with ammonia at 15 and 25℃, and with Tris at 15 and 30℃ have been studied, respectively. The experimental results indicate that the theory and method of the reduced parameter method for slower opposing reactions are correct.
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Original Articles
Copper cluster structural stablity and energetic-calculations and simulations
TAN KAI;LIN MENGHAI;WANG NANQIN;ZHANG QIANER
Acta Chimica Sinica 2002, 60 (1): 24-29.
Published: 15 January 2002
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Equilibrium geometries and electronic properties of Cu~n(n=2, 3, 4, 6) clusters are determined via DFT calculations. We construct potential function with parameters fitted to ab initio potential energy surfaces, and use a global minima"basin-hopping" algorithm to obtain minimum-energy structures of Cu clusters for n=13~56. The results are in good agreement with experiments and other calculations.
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Original Articles
Semiconducting properties of passive film formed on stainless steel by using A. V. passivation
ZHANG JUNQING;QIAO YINAN;CAO CHUNAN;ZHANG JIANQING;ZHOU GUODING
Acta Chimica Sinica 2002, 60 (1): 30-36.
Published: 15 January 2002
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1875
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Passive film formed on 304 stainless steel in 2.5 mol/L H~2SO~4 solution by using alternating voltage (A. V. ) passivation have been investigated by measuring capacitance and photoelectrochemical parameters. The investigation of the effect of measure frequency on the slope of Mott-Schottky curve has been carried out. The photoelectrochemical measurements were consistent with the capacitance measurement. Analysis of the experimental results showed that the passive film formed 304 stainless steel by using A. V. passivation exhibits semiconducting properties. Using the simple model of semiconductor rather than the multi-donor level model can explain satisfactorily the semiconducting behavior of the film formed on 304 stainless steel by using A. V. passivation.
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Cited: Baidu(
31
) CSCD(
6
)
Original Articles
Study of molecule-exchanging energy of surfactants in binary mixed surfactant spherical micelles of gleditsin sapinin in aqueous solutions with the dimensional crystal model
WANG ZHENGWU;LI GANZUO;LIU JUNCHENG;GUAN DAREN;LIAO LILING;LOU ANJING
Acta Chimica Sinica 2002, 60 (1): 37-42.
Published: 15 January 2002
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1748
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By using the dimensional crystal model and the regular solution theory, the relationship between the super chemical potential of component A(μ^E~m~,~A) and the surfactant molecule-exchanging energy (ε~m) of spherical micelles in binary surfactant aqueous solution, μ^E~m~,~A=ε~m~gN~0(1-x~A)^2, has been firstly established. Then with the help of the micellar separated phase model, the relationship between the parameter of molecule interaction in spherical micelles (β~m), which cabtained from the surface tension vs. the logarithm curves (γ~logc), and the surfactant molecule-exchanging energy, ε~m=gRTβ~m/N~0, has secondly been deduced. By using this equation for practical calculation of ε~m, the synergism of binary surfactant ixtures of gleditsin saponin (GS) (C~3~0H~3~8O~3) with C~1~2H~2~5SO~3Na (AS), C~1~2H~2~5(OC~2H~4)~3SO~4Na (AES), C~7F~1~5CO~2Na (OBS), C~1~6H~3~3NMe~3Br (CTAB), C~8H~1~7Ph(EO)~1~0OH (Tritonx 100) and C~1~2H~2~5(EO)~9OH (AEO~9) in spherical micelles of aqueous solutions has been studied from the view of energy at 25℃. The results show that all the surfactant molecule-exchanging energies of the binary systems of GS in micelles are smaller than zero, which means that GS can produce remarkable synergism when mixed with other surfactants.
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Cited: CSCD(
2
)
Original Articles
Molecular docking studies of the 4-anilinoquinazoline inhibitors with EGFR
ZHU LILI;HOU TINGJUN;CHEN LIRONG;XU XIAOJIE
Acta Chimica Sinica 2002, 60 (1): 43-48.
Published: 15 January 2002
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The interaction pattern between the epidermal growth factor receptor (EGFR) with a group of 4-anilinoquinazoline inhibitors has been investigated. The 3D structure of EGFR was constructed using homology modeling, and the complex structures between receptor and ligands were predicted by using molecular mechanics and molecular dynamics. From the calculations, it can be found that the van der Waals interactions, the hydrophobic interactions, as well as the H-bonding interactions are crucial for the ligand binding. The 4-phenylamino group can produce strong van der Waals adn hydrophobic interactions with the nonpolar side chains of the residues deep in the binding cleft. The R^1 and R^2 substituents on the bicyclic chromophore can also produce strong van der Waals and hydrophobic interactions with the residues located at the exterior part of the binding pocket. Moreover, the two N atoms of the quinazoline can form H-bonds with EGFR, which will produce significant contribution to biological activities. The calculated nonbonded interactions between anilinoquinazolines and EGFR, as well as the information obtained from the predicted complexes, can interpret the structure-activities of the inhibitors well, which can afford us important information for structure-based drug design.
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Cited: Baidu(
28
)
Original Articles
The structures, relative stability, and potential energy surface of HAsO~2 isomers
YU HAITAO;CHI YUJUAN;FU HONGGANG;HUANG XURI;LI ZESHENG;SUN JIAZHONG
Acta Chimica Sinica 2002, 60 (1): 49-54.
Published: 15 January 2002
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The potential energy surface (PES) of HAsO~2 system including nine isomers and ten transition states is predicated at MP2/6-311+ +G(d, p) and QCISD(T)/6-311+ +G(3df, 2p) (single-point) levels of theory. On the PES, cis-HOAsO(E1) is found to be thermodynamically the most stable isomer followed by trans-HOAsO(E2) and HAsO(O)(C~2~V, E3) at 13.15 and 192.74 kJ/mol. Based on the PES, E1, E3, cis-HOOAs(E6) and trans-HOOAs(E5) are thermodynamically and kinetically stable isomers, and should be experimentally observable. The products in the first-step reaction of HAs with O~2 can isomerize into isomer E3 that has higher thermodynamical stability. The reaction of OH with AsO will directly lead to the formation of isomer E1. The comparison of the calculated results with the PESs of HPO~2, HPS~2, HNO~2, HNS~2(analogs of HAsO~2) is also made.
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Original Articles
A novel calorimeter for the determination of the heat sink of endothermic hydrocarbon fuels
GUO YONGSHENG;JIANG WU;LIN RUISEN
Acta Chimica Sinica 2002, 60 (1): 55-59.
Published: 15 January 2002
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1432
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A novel high-temperature flow calorimetric system of conduction type was designed, with a built in chromatograph suitable for on-line analysis. The thermal and time constants at 700℃ of the calorimeter were calibrated by a sample electric energy method. The accuracy of the equipment was also validated with standard samples such as heptane and N~2. The heat sink values of endothermic hydrocarbon fuels S-1 and R-1 at 700℃ were determined to be 2.99 MJ/kg and 2.82 MJ/kg, respectively.
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Cited: Baidu(
18
) CSCD(
12
)
Original Articles
Solid state synthesis at lower heating temperature of Zn(p-DMABA)~2Cl~2 and its X-ray powder diffraction data
CHEN JINXI;PAN TAO;LIU MINGGUANG;LIN SHAOFAN;XIN XINQUAN
Acta Chimica Sinica 2002, 60 (1): 60-64.
Published: 15 January 2002
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1708
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The coordination complex of a weak ligand, p-dimethylaminobenzaldehyde (p-DMABA), with ZnCl~2 was prepared by a solid state reaction at low temperature (60℃). The final product was characterized by elemental analysis, TGA-DTA, FT-IR, Raman, fluorescence spectroscopy and XRD. The C=O stretching frequency of the title compounds shifted to lower wavenumber upon addition of Zn^+ indicating the formation of a covalent bond between the carbonyl oxygen and the zinc cation. 25 lines (5°<2θ<60°) were indexed to give the unit cell parameters: a=1.5897(2)nm, b=0.7560(4)nm, c=1.0373(1) nm, β=95.23(3)°, V=1.241(2) nm^3. Extinction conditions indicate that the space group is P2~1 11(4).
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Cited: Baidu(
3
)
Original Articles
Syntheses, characterization and third-order nonlinear optical properties of ruthenium(Ⅱ) polypyridine complexes
JIANG CAIWU;CHAO HUI;LI RUNHUA;LI HONG;JI LIANGNIAN
Acta Chimica Sinica 2002, 60 (1): 65-70.
Published: 15 January 2002
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1767
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Three ruthenium (Ⅱ) complexes containing imidazo[4, 5-f][1, 10] phenanthroline (IP) have been synthesized and characterized by EA, FAB-MS, ^1H NMR, UV-vis and electrochemistry. The cubic nonlinear refraction index n~2 and the nonlinear absorption coefficient α~2 of the ruthenium (Ⅱ) complexes are measured by Z-scan techniques and the third-order nonlinear susceptibility χ^(^3^), and hyperpolarizability γ of the complexes are calculated. The effects of molecular structure on the third- order nonlinear optical properties are discussed.
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Original Articles
Synthesis of Al-MCM-41 with high content of framework aluminum
WAN YING;WANG ZHENG;MA JIANXIN;JIN XINGMEI;ZHOU WEI
Acta Chimica Sinica 2002, 60 (1): 71-75.
Published: 15 January 2002
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1453
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Mesoporous molecular sieves MCM-41 with incorporated structural aluminum (Al-MCM-41) of different Si/Al ratios (ranging from 3 to 100) were prepared using a modified hydrothermal method. Characterization using X-ray powder diffraction and nitrogen adsorption measurement showed that all these samples had typical XRD diffractogram of MCM-41, the adsorption isotherm of type Ⅳ and an uniform pore size distribution. The last feature reflects a highly ordered structure of pore arrays. Solid state ^2^7Al MAS NMR investigation showed further that even at high level of aluminum (x~A~l=0.303), the Al atoms could still be incorporated tetrahedrally in the MCM-41 structure. Based on the experimental results, the effects of aluminium content on the pore structure and the formation mechanism of Al-MCM-41 were discussed.
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Cited: Baidu(
22
) CSCD(
13
)
Original Articles
Study on the special properties of manganese oxide nanoclusters confined in the ordered porous zirconium oxide
CHEN HANGRONG;SHI JIANLIN;YAN JINA;CHEN HONGGUANG;RUAN MEILING;YAN DONGSHENG
Acta Chimica Sinica 2002, 60 (1): 76-80.
Published: 15 January 2002
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1734
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Manganese oxide nanoclusters were synthesized within ordered porous ZrO~2 by using wet impregnation technique. X-ray powder diffraction, HRTEM, XPS, UV-vis spectroscopy, Electron paramagnetic resonance (EPR) spectroscopy and O~2-TPD measurement were adopted for the characterization of the synthesized materials. The results showed that the nanoclusters of manganese oxide could be successfully confined and randomly distributed into the pores of ZrO~2. The size of the MnO~2 nanoclusters was better confined by the dimension of the pore channels with increasing the heating temperature. EPR measurement revealed that decreasing of the particles' sizes led to a significant chagne in the magnetic property. The excellent oxygen adsorption properties of the clusters of manganese oxide confined into the pore channels were demonstrated by the O~2-TPD analysis.
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Cited: Baidu(
3
) CSCD(
3
)
Original Articles
Effect of ultrasound on aluminium trihydroxide crystallization from sodium aluminate solution
ZHAO JIHUA
Acta Chimica Sinica 2002, 60 (1): 81-86.
Published: 15 January 2002
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1690
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Compared with crystallization of aluminium trihydroxide without treatment of ultrasound, the time of precipitation was reduced from 30 h to 15 h when the precipitation ratio was 45% under 20 kHz and 33 kHz ultrasound irradiation. The enhancement effects of two frequencies are not the same. Irradiation with 33 kHz ultrasound could shorten the induction time, increase the secondary nucleation and enhance the agglomeration. Use of 20 kHz ultrasound, however, led to prolong induction time, increase agglomeration and enhance the growth of aluminium trihydroxide. As a result, the average diameter of aluminium trihydroxide product was increased 3.7 μm. But the autoprecipitation of sodium aluminate solution was not enhanced under ultrasound irradiation.
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Cited: Baidu(
7
) CSCD(
3
)
Original Articles
Synthesis of nanophase PbO~2 by solid state reaction and its influence on MnO~2 electrode
XIA XI;GONG LIANGYU
Acta Chimica Sinica 2002, 60 (1): 87-92.
Published: 15 January 2002
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1577
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Nanophase PbO~2 was prepared successfully by solid-phase redox reaction and characterized by XRD, TEM and CV techniques. The synthesis conditions of nanophase materials were discussed. PbO~2 modified MnO~2 electrodes were fabricated and their electrochemical properties were studied by means of constant current discharge and CV experiments. The results indicated that the optimum ratio of PbO~2 additives were 1.25%~5.00%. The charge-discharge mechanism of MnO~2 changed because the Pb(X)(X=0, Ⅱ) and Mn(Y)(Y=Ⅳ,Ⅲ,Ⅱ) atoms formed stable complexes. These complexes could be cooxidized and coreduced and thus restrained the formation of electrochemically inactive Mn~3O~4. The rechargeability of the MnO~2 electrode could be improved. Discharge mechanism of MnO~2 doped with nanophase sample was similar to that doped with conventional sample(S). But the nanophase sample was more effective in modifying MnO~2 electrode than the conventional sample. The discharge capacity of the nanophase PbO~2 modified MnO~2 electrodes were in average 30% higher than that of the conventional PbO~2 modified ones.
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Cited: Baidu(
37
)
Original Articles
Separation of enantiomers on bonded cellulose trisphenylcarbamate stationary phase by high-performance liquid chromatography
CHEN XIAOMING;MAO XIQIN;ZHANG ZENGZI;LUO QUANZHOU;ZOU HANFA
Acta Chimica Sinica 2002, 60 (1): 93-97.
Published: 15 January 2002
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1523
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708
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Cellulose trisphenylcarbamate was regioselectively bonded to 3-aminopropyl silica gel at 6-position of the primary hydroxyl group on the glucose unit of cellulose with 4, 4'-diphenylmethane diisocyanate as a spacer. Nine racemates were resolved on the prepared stationary phase under normal-HPLC mobile phases. It was observed that enantioseparations on the bonded-phase showed higher efficiency by using tetrahydrofuran as a component of the mobile phase, and the structure of the derivative agent reacted with the amino acids played a role for the enantioseparation. Chiral separation on the bonded phase under reversed-HPLC mobile phase was also performed successfully. It has been shown that the retention factors of the racemates decreased appreciably with the increment of the concentration of acetonitrile in the mobile phase, while no significant change was observed for the enantioselectivity. Separation of enantiomer for the acidic racemate could be improved with a lower pH value of the mobile phase since the dissociation of acidic compound was impressed, but it did not affect significantly the resolution of neutral compounds.
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Cited: Baidu(
8
) CSCD(
3
)
Original Articles
Study on the conformational change of DNA in surfactant
LI LAISHENG;HUANG WEIDONG;WANG LIPING;YAN YUAN
Acta Chimica Sinica 2002, 60 (1): 98-104.
Published: 15 January 2002
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1690
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Study on the DNA behavior in surfactant solutions show that various surfactants could greatly affect the DNA conformations in solutions in the sequence of cationic surfactant (e. g. cetyltrimethylammonium bromide, CTMAB)>anionic surfactants (e. g. sodium dodecyl sulfate, SDS)> neutral surfactants (e. g. Triton X-100). CTMAB interacts with DNA by Coulombic forces and hydrophobicity. The interaction between anionic surfactants and DNA is relatively weak, while the effect of Triton X-100 on DNA is similar to that of solvent, which means that both of them affect DNA conformations by polarity and dielectric constant. The results indicate that Coulombic forces and hydrophobicity play an important role in the interaction between DNA and surfactant molecules.
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Cited: Baidu(
33
) CSCD(
19
)
Original Articles
Study on the interaction mechanism between Ge-132 and DNA by spectral methods
LI WENYOU;ZHU SHOUTIAN;HE XIWEN;LIANG HONG
Acta Chimica Sinica 2002, 60 (1): 105-108.
Published: 15 January 2002
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1563
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The interaction between Ge-132 and DNA was investigated using absorption spectra, DNA alkaline denaturation and fluorescence spectra. Based on the measurements of A~2~6~0 in different pH media, the alkaline denaturation curves of CT DNA in the absence of and in the presence of Ge-132 were obtained. The results showed that the alkaline denaturation for Ge-132-DNA complex occurred at a higher pH than for DNA alone and the hyperchromicity of Ge-132-DNA complex was smaller than that of DNA, which suggested the intercalation mechanism of Ge-132 into DNA bases. All the exprimental results indicated that the intercalative binding was the major mode for the interaction of Ge-132 with DNA.
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Cited: Baidu(
36
) CSCD(
12
)
Original Articles
Study on the structure and reactivity of the geometric isomers of [Co(2, 3-tri)(amp)Cl]^2^+
TAO ZHU;ZHU QIANJIANG
Acta Chimica Sinica 2002, 60 (1): 109-120.
Published: 15 January 2002
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1527
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Kinetics of basic hydrolysis shows that the cis(N^*) mer-isomers (m1 or m2) are about 100-fold more reactive than the trans(N^*) forms (m3 or m4) due to steric strain caused by the pyridyl residue in the amp. No facial isomers have been found in the experiments. Detailed stereochemical studies using progressive NMR spectroscopy reveal that all mer reactants give a common product distribution in the basic hydrolysis reaction. Four substituted mer-isomers have been observed. Rearrangements of the isomers in DMSO at 100℃ show that the m1-Cl complex is the most reactive one, the cis(N^*) isomers (m1 and m2) yield m3-Cl complex first. A subsequent equilibrium between chloro species of m3 and m4 then takes place. Experiments of deuteration of the active protons in each isomer indicate that reactivity of an isomer is not proportional to the H-D exchange ratio which is observed before hydrolysis and rearrangement of the isomer. Ab initio computational results (RHF/LANL2DZ optimised structure) are well consistent with the crystal structural parameters of four geometric mer-isomers of [Co(2, 3-tri)(amp)Cl]ZnCl~4 with an maximum error of ±3%. The cis-mer isomers (m1 and m2) are calculated to be about 4 kJ/mol less stable than the trans-mer isomers (m3 and m4). However, the facial isomers are calculated to be at least 17 kJ/mol less stable than the mer isomers. Each isomer are calculated to be at least 5 kJ/mol more stable when the effect of solvent (water) is included using the Onsager model within the solvent continuum reaction field method. The distortions for the different isomers from the idealised octahedron are correlated with reactivity. The more severely distorted species is predicted to be more reactive.
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Study on 2D NMR spectra and product distribution of the geometric isomers in [Co(3, 3-tri)(ibn)Cl]^2^+ system
YUAN XUNMO;ZHU QIANJIANG;TAO ZHU;ZHANG JIANXIN
Acta Chimica Sinica 2002, 60 (1): 121-128.
Published: 15 January 2002
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1445
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The configurations of the four geometric mer-isomers in a new [Co(3, 3-tri)(ibn)Cl]^2^+(3, 3-tri=N-(3-aminoethyl)-1, 3-propanediamine; ibn=1, 2-diamino-2-methylpropane) system were assigned by using 2D NMR techniques such as gCOSY and NOESY. Solvent used was Me~2So=d~6 with the central peak of the CD~3 septet as the reference (^1^3C, δ39.37; ^1H, δ2.49 relative to SiMe~4). Comparing to the eluates from the chromatographic column, cation exchange media used was Dowex 50 W×2 (H^+ form, 200~400 mesh; Biorad), the first band contains the m2, the second band contains the m4, the third band contains the m1, the fourth band contains the m3 and the last band contains the f3. An ab initio computational result (RHF/LANL2DZ level) suggests why the facial isomer has been isolated and the distribution of the four mer-isomers is not different from those of [Co(2, 2-tri)(diamine)Cl]^2^+.
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Electronic effect of indolecarboxaldehyde in the condensation with t-butyl bromoacetate promoted by biazaborolidine
WEN SHIJUN;YAO ZHUJUN
Acta Chimica Sinica 2002, 60 (1): 129-133.
Published: 15 January 2002
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1657
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The condensation reaction of indolecarboxaldehydes with t-butyl bromoacetate induced by biazaborolidine was studied. The electronic effect of aldehydes upon the products is discussed.
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Cited: Baidu(
2
)
Original Articles
Three dimentional quantitative structure-activity relationships of novel 2-heteroaryl-4-chromanone derivatives
YANG GUANGFU;JIANG XIAOHUA;DING YU;YANG HUAZHENG
Acta Chimica Sinica 2002, 60 (1): 134-138.
Published: 15 January 2002
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1670
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464
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In order to develop novel fungicides, the structure of flavanane phytoalexins was modified in view of bioisosterism and 23 novel title compounds, 2-heteroaryl-4-chromanones, were designed and synthesized, whose structures were confirmed by ^1H NMR, MS and elemental analyses. The fungicidal IC~5~0 in vitro against rice blast disease of the title compounds were measured and the quantitative relationship between the structures and fungicidal activities was established using the comparative molecular field analysis (CoMFA) approach. The results of 3D-QSAR analysis suggested that the introduction of small steric bulk but strong electronreleasing group onto the 5, 6, 7-position of th ebenzene ring would be favorable to the activity of the compound. The CoMFA analyses about the electronic property requirement of 7-O and 19-O were consistent with those derived from the Hansch-Fujita approach.
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Cited: Baidu(
11
) CSCD(
2
)
Original Articles
Calix[6] arene-bismetalloporphyrins as enzyme models for P-450 Ⅳ. catalytic performance in oxidation of isopropyl benzene
LI DONGHONG;CHEN SHUHUA;ZHAO HUAMING
Acta Chimica Sinica 2002, 60 (1): 139-142.
Published: 15 January 2002
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1418
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The catalytic performance of calix[6] arene-bismetalloporphyrins in oxidation of isopropyl benzene has been studied. The results show that calix[6] arene-bismetalloporphyrins possess much higher catalytic activity than the corresponding metalloporphyrin while displaying the sam eselectivity by giving rise to acetophenone as the ketonic component in excellent yield. This result is different from the usual reactions catalyzed by metallophthalocyanine and other macromolecule such as Schiff base metal chelate, where the ketonic component is acetone. The effects of temperature, axial ligands, amounts of catalyst used, and the variety of central metal etc. on the oxidation are also studied.
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Original Articles
Synthesis and crystal structure of a novel ionic organotin {[Ph~2Sn]~2[2, 6-Py(CO~2)]~3H~2O}^2^-[HNEt~3]^+~2
YIN HANDONG;WANG CHUANHUA;WANG YONG;MA CHUNLIN;SHAO JIANXIN;ZHANG JUNHONG
Acta Chimica Sinica 2002, 60 (1): 143-149.
Published: 15 January 2002
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1552
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A novel ionic organotin compound {[Ph~2Sn]~2[2, 6-Py(CO~2)]~3H~2O}^2^-[HNEt~3]^+~2 was synthesized by the reaction of Ph~3SnCl with 2, 6-pyridine dicarboxylic acid in 1:1 molar ratio in the presence of an organic base Et~3N. The structure was characterized b elemental analysis, IR and ^1H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic with space group P2~1/n, a=1.7073(7) nm, b=1.7447(7) nm, c=2.5333(10) nm, β=109.694(7)°, Z=4, V=6.824(5) nm^3, D~c=1.282 g/cm^3, μ=0.793 mm^-^1, F(000)=2696, R~1=0.0563, WR~2=0.1539. In the crystal structure of the compound, the tin atoms are seven-coordinated in a distorted pengonal bipyramidal geometry. The compound was tested in vitro against human tumour cell lines, MCF-7 and WiDr, and displayed high activity.
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Original Articles
A facile large scale synthesis of the core mannose pentasaccharide of N-linked glycoprotein and its isomer
ZHANG JIANJUN;KONG FANZUO
Acta Chimica Sinica 2002, 60 (1): 150-156.
Published: 15 January 2002
Abstract
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1942
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528
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Condensation with 1, 2-O-ethylidene-4, 6-O-benzylidene-β- D-mannopyranose (2) as the acceptor and 2, 3, 4, 6-tetra-O-benzoyl- α-D-mannopyranosyl trichloroacetimidate (3) as the donor gave 3-O-linked disaccharide (4), subsequent debenzylidenation afforded the disaccharide acceptor5. Coupling of 5 with 3 selectively furnished 6-O-linked trisaccharide 6, then deethylidenation, acetylation, selective 1-O-deacetylation, and trichloroacetimidation yielded the trisaccharide donor 10. Condensation of 10 with 5 afforded 6-O-linked pentasaccharide 11, its deethylidenation followed by acetylation gave the required pentasaccharide 13. Coupling of 10 with 2 gave the tetrasaccharide 14, its debenzylidenation afforded the tetrasaccharide acceptor 15. Condensation of 15 with 3 gave the pentasaccharide isomer.
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Original Articles
Polymerized unsymmetrical iron post-metallocene catalyst for ethylene polymerization
LIU CHANGKUN;JIN GUOXIN
Acta Chimica Sinica 2002, 60 (1): 157-161.
Published: 15 January 2002
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1731
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The unsymmetrical allyl containing post-metallocene complex [ArN=C(Me)][Ar'N=C(Me)]C~5H~3NFeCl~2 [Ar=2, 6-(i-Pr)~2C~6H~3, Ar'=4-allyl-2, 6-(i-Pr)~2C~6H~3](3) has been prepared and characterized. Complex (3) can be co-polymerized with styrene in the presence of radical initiator to produce polymerized post-metallocene catalyst which exhibits high activity for ethylene polymerization (2.5×10^6 g PE/mol Fe.h).
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Cited: Baidu(
16
)
Original Articles
Cyclopropanation of styrene catalyzed by chitosan schiff-base copper (Ⅱ) heterogeneous catalyst
SUN WEI;XIA CHUNGU;WANG AIQIN
Acta Chimica Sinica 2002, 60 (1): 162-165.
Published: 15 January 2002
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1799
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Chitosan Schiff-base copper (Ⅱ) catalyst catalyzed cyclopropanation reaction of styrene with ethyl diazoacetate. The catalyst showed high activity in cyclopropanation. Moderate stereoseletivity (up to 17.1% ee), with the ratio of trans to ics being 66.7:33.3 was obtained at 60℃, Furthermore, the catalyst could be recycled without loss of cyclopropanation activity.
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Cited: Baidu(
29
) CSCD(
14
)
Original Articles
A novel large heteropolyanion Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)^1^9^-~4
XUE GANGLIN
Acta Chimica Sinica 2002, 60 (1): 166-168.
Published: 15 January 2002
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1506
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The heteropolytungstate [Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)~4](NH~4)~1~9.48H~2O is prepared by the reaction of Na~2WO~4.2H~2O with Sb~2O~3 and Ce(NO~3)~3.6H~2O. The structure of heteropolyanion Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)^1^9^-~4 is determined by X-ray diffraction analysis and elemental analysis. The cell parameters of [Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)~4](NH~4)~1~9.48H~2O: a=1.8908(6) nm, b=2.0032(14) nm, c=2.8653(12) nm, α=86.95(6)°, β=75.68(3)°, γ=67.52(5)°, V=9.706(9) nm^3, space group P1. The [Ce~3Sb~4W~2O~8(H~2O)~1~0(SbW~9O~3~3)~4]^1^9^- anion possesses a large center group [Ce~3Sb~4W~2O~8(H~2O)~1~0]^1^7^+ attached by four β-B-(SbW~9O~3~3)^9^-, the center group contains three Ce(Ⅲ), two bridging {WO~2(H~2O)} groups and one {Sb~4O~4} group. The coordination number of all three Ce(Ⅲ) is nine however their coordination circumstances are different: Ce(1) and Ce(3) have the same coordination circumstance in which the cerium atoms are coordinated by four oxygen atoms of two (SbW~9O~3~3)^9^-, one oxygen atom of {Sb~4O~4}, one oxygen atom of one bridging {WO~2(H~2O)} and two oxygen atoms of two water molecules. Four antimony atoms form a tetrahedron in {Sb~4O~4} group. The anion belongs to C~s point group.
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Original Articles
Determination of lanthanum effect on myocardiac potassium channels
XUE SHAOWU;YANG PIN;DU HUIZHI
Acta Chimica Sinica 2002, 60 (1): 169-170.
Published: 15 January 2002
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1524
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Whole-cell patch-clamp recording mode was used to study the action mechanism of La^3^+ on rat ventricular myocytes potassium channels. The Ca^2^+-independent voltage-activated outward K^+ current was activated by the depolarizing pulse in enzymatically isolated rat ventricular myocytes. When 10 μmol/L La^3^+ was added to the bath solution, the Ca^2^+-independent voltage-activated outward K^+ current was distinctly suppressed. It implies that there may exist one or more binding-sites in potassium channels for La^3^+.
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Cited: Baidu(
18
) CSCD(
4
)
Original Articles
Primary study for intermittent electrospray
LIU HANQING;GUO YINLONG;YU TIAN;YANG YUAN
Acta Chimica Sinica 2002, 60 (1): 171-175.
Published: 15 January 2002
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1469
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We designed a new method-intermittent electrospray for mass spectrometry. In this paper, the primary principle for intermittent electrospray, the high sensitivity property of intermittent electrospray and advantages for protein analysis is described. Because of its high-sensitivity, this method may find extensive applications in analysis of proteins. The instrumental parameters can be controlled during intermittent electrospray if thesoftware of the instrument is reprogrammed. The parameters can be optimized to give better data. The parameters that can be controlled include tip potential, nozzle potential, flow rate, nebulizer gas flow, curtain gas flow and so on. The instrumental parameters can be changed during different electrospray process in this program. Each process has its own parameters. Then this program runs in cycle to electrospray intermittently. Intermittent electrospray has many advantages for mass spectrometry, which continuous electrospray doesn't have. For example, biological samples are always so little in quantity and the concentration of these samples is so low that many problems are encountered in the determination. But now this kind of samples can be analyzed by intermittent electrospray. Sample solutions are condensed at tip during nonionization time when the solvent is evaporated. After that the condensed sample solution is sprayed in a short time. Because the concentration of the solution is increased, the sensitivity is also improved. So satisfied results from the biological sample can be obtained. Some factors (such as tip potential, sample solution flow) that may influence sensitivity were studied.
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Cited: Baidu(
4
)
Original Articles
Structural changes of lignins caused by oxidative ammonolysis
LIN LU;ZHOU XIANTAO;ZHAO DESHENG;QIU YUGUI
Acta Chimica Sinica 2002, 60 (1): 176-179.
Published: 15 January 2002
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1388
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524
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Nitrogen-modified lignins was produced from the reaction of ammonia and lignins under proper conditions. ^1^3C and ^1H-^1^3C 2D-NMR HMQC spectroscopy was applied to detect the changes of lignin molecule during oxidative ammonolysis. Results showed that fragmentation of lignins molecule was highly drastic during oxidative ammonolysis. Probably oxidative modifications of moieties on the surface of lignin molecule (such as formation of CHO and COOH from CH~3 or CH~2) took place. Then nitrogen was incorporated into the lignin. However, no obvious changes was found in the highly-condensed lignin inner structures.
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Cited: Baidu(
5
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Original Articles
Influence of sedimentation on perikinetic coagulation of different size of polystyrene spheres
DAI GUOLIANG;DONG XIANGQUN;QIAO RUNLONG;SUN ZHIWEI;HU WENRUI
Acta Chimica Sinica 2002, 60 (1): 180-182.
Published: 15 January 2002
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1574
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426
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R. Folkersma et al. had reported that the perikinetic coagulation rate of 2 μm polystyrene(PS) spheres increased remarkably under microgravity conditions. Otherwise, Z. W. Sun et al. had provided their evidence showing that it was only appreciably faster under microgravity than under normal gravity. In order to test the influence of sedimentation on different size of PS spheres, on the basis of Sun's experiments, we have studied the coagulation rates of 1 μm, 2 μm, 3 μm and the mixture of 1 μm and 2 μm PS spheres. Turbidity versus time was employed to monitor the salt-induced coagulation process of PS dispersions. 0.5 mol.L^-^1 MgCl~2 was used to induce fast aggregation. The results show that there is no difference in perikinetic coagulation rate under normal gravity and microgravity for 1 μm, 2 μm, 3 μm and 1 μm+2 μm PS. The authors assumed the surface properties of PS spheres and experimental method might account for the different results.
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Cited: Baidu(
1
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Original Articles
Synthesis and Electrical Properties of BaCe_(0.8)Y_(0.2)O_(3-α)
Jia Dingxian;Ma Guilin;Shi Hui
Acta Chimica Sinica 2002, 60 (10): 1737-1741.
Published: 15 October 2002
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1820
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463
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A precursor of BaCe_(0.8)Y_(0.2)O_(3-α) electrolyte was synthesized by the sol-gel method and sintered at 1400~1500 ℃, which was 150~250 ℃ lower than that used by traditional high temperature solid state reaction. Using the sintered samples as solid electrolyte and porous platinum as electrodes, hydrogen and oxygen concentration cells as well as hydrogen-air fuel cells were constructed. Proton and oxide-ion transport numbers as well as fuel cell peformance of the BaCe_(0.8)Y_(0.2)O_(3-α) sinter were compared with the corresponding values of the BaCe_(0.8)Y_(0.2)O_(3-α) prepared by high temperature solid state reaction. The results indicated that the proton transport number and fuel cell performance of BaCe_(0.8)Y_(0.2)O_(3-α) synthesized by sol-gel method could be obviously affected by sintering temperature. When the sintering temperature was ≥ 1450 ℃, the proton transport number was approximately 1 and the fuel cell performance was good. However, when the sintering temperature was < 1450 ℃, the proton transport number was smaller than 1 and the fuel cell performance was poor. Among the samples sintered at 1400~1500 ℃, the sample sintered at 1450 ℃ exhibited the optimal fuel cell performance, which was close to that of the sample prepared by high temperature solid state reaction.
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Cited: Baidu(
10
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Original Articles
Synthesis, Structure and Electrochemical Behavior of LiNi_(0.85)Co_ (0.15)O_2
Zhu Xianjun;Zhan Hui;Zhou Yunhong
Acta Chimica Sinica 2002, 60 (10): 1742-1746.
Published: 15 October 2002
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1814
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565
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LiNi_(0.85)Co_(0.15)O_2 compounds were synthesized under various conditions by heating a mixture of lithium hydroxide (LiOH·H_2O), nickel oxide (Ni_2O_3) and cobalt oxide (Co_2O_3). The products of LiNi_(0.85)Co_(0.15)O_2 were characterized by XRD and electrochemical tests. Based on the experimental results, the influence of synthetic conditions, including temperature and Li/Ni/Co molar ratio on the structure of the products, and the relationship between structure and electrochemical behavior are discussed. It is important to control synthetic conditions in order to obtain layered and highly crystallized product. By Rietveld refinement, the asprepared product shows a = 0.2874 nm, c = 1.4229 nm, and maximum cell volume V = 0. 10180 nm~3 and it also shows a high initial discharge capacity of 197 mA·h/g and retention of over 180 mA·h/g after 15 cycles.
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Cited: Baidu(
14
)
Original Articles
~1H NMR Studies of DMF-H_2O Association System
Lei Yi;Li Haoran;Zhu Longhua;Han Shijun
Acta Chimica Sinica 2002, 60 (10): 1747-1753.
Published: 15 October 2002
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1793
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Dimethylformamide (DMF) aqueous solution is a kind of simple biochemical model of biological molecular aqueous solutions. In this paper, ~1H NMR of DMF-H_2O system was measured at different temperatures to discuss molecular interactions in the mixtures. The association system was modeled on the equilibrium among H_2O, H_2O· DMF, (H_2O)_2 and (DMF)_2·H_2O and calculated by nonlinear least- square fitting. Association equilibrium constant K and the corresponding ΔH and ΔS were obtained by combined GA and levenberg- marquardt algorithm. In addition, DMF-CCl_4 and DMF-BuOH systems were also studied in order to further understand the nature of interactions in DMF-water mixture. Some peculiar phenomena were found and considered to be mainly caused by the special structure of liquid water, the hydrogen-bonding interactions and the conjugate system of amide.
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Cited: Baidu(
33
)
Original Articles
Study of Cracking Catalysts of Mixed Zeolites Modified by Ag and La to Endothermic Hydrocarbon Fuels
Zhang Bo;Lin Ruisen;Wang Bincheng;Xian Chunlei
Acta Chimica Sinica 2002, 60 (10): 1754-1759.
Published: 15 October 2002
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1788
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389
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In order to improve endothermic ability of endothermic hydrocarbon fuel, the endothermic hydrocarbon fuel NNJ-150 and the catalysts mixed with USY and ZSM-5 which have been modified by La~(3+) and Ag~+ were prepared. NNJ-150 cracked on USHY, HZSM-5, their mixture and mixed zeolite catalysts modified by Ag~+ and La~(3+) was studied. Results show that the selectivity of light olefins is high (600 ℃, 47.92%), the lifetime of catalyst is long (above 35 min, 500 ℃), and the performance of catalyst is stable when NNJ-150 is cracked on Ag-LaUSY + Ag-LaZSM-5 (75:25). It can satisfy the need of cooling high supersonic craft.
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Cited: CSCD(
6
)
Original Articles
Theoretical Study on the Reaction of Fluorine Atoms with ·CH_2SH Radical
Hu Zhengfa;Feng Xia;Wang Zhenya;Zhou Shikang
Acta Chimica Sinica 2002, 60 (10): 1760-1767.
Published: 15 October 2002
Abstract
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1930
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428
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The reaction of F atoms with ·CH_2SH radical has been studied by using quantum chemistry ab initio and density function theory (DFT) calculations along the potential energy surface. The optimized geometrical parameters, vibrational frequencies ad zero-point vibrational energies (ZPVE) of all species were obtained at the B3LYP/6-311G theoretical level. The total energies were worked out using the B3LYP/6-311 + G(2df, pd)//B3LYP/6-311G method. In addition, the G3 energies of reactants and products were also obtained. The results indicate that the reaction proceeds through addition of a F atom to CH_2SH by either F-C or F-S combination to form initial complexes, followed by H(4) migration to form methyl radical CH_3·, which rotates around main C-S bond to result in combination of H(4) and F. Formation of HF and CH_2S is the most probable reaction chanel with the exothermic heats of 396.94 kJ/mol (G3) and 370.7 kJ/mol (DFT) respectively. Furthermore, the enthalpy of formation of CH_2SH was deduced to be 146.44 kJ/mol (DFT) and 167.36 kJ/mol (G3), which are in agreement with existing experimental and theoretical values.
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Cited: Baidu(
13
) CSCD(
11
)
Original Articles
High Pressure Effects on the Photophysical Properties of a New Type of Hyperbranched Conjugated Copolymer
Zhong Bo;Li Shayu;Li Hong;He Liming;Bai Fenglian;He Qingguo;Yang Guoqiang
Acta Chimica Sinica 2002, 60 (10): 1768-1772.
Published: 15 October 2002
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1894
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Photophysical properties of a new hyperbranched conjugated copolymer, poly(2-methoxy-5-(2'-ethylhexoxy)-p-phenylene vinylene)-alt- (3,5-bisvinylicbenzene) (MEH-PPV-HS_1), have been investigated. MEH-PPV- HS_1 shows two adjacent absorption bands in UV region, and similar fluorescence emission spectra are obtained when it is excited selectively by these two bands. Effects of pressure on these two absorption bands are quite different and the emission intensity may change with pressure in a different way for excitation at different band. All these results indicate that these two absorption bands are attributed to different effective conjugated structures in MEH-PPV- HS_1 respectively and the selective excitation of MEH-PPV-HS_1 generates different excited states, which transit to the same luminescent excited state by different relaxation pathway.
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Cited: Baidu(
10
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