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1998, Vol.14 No.2   
刊出日期: 1998-04-24

本期栏目: Articles |
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WANG Xing-qiao, GAO Shuang, CA Chang-sheng, YU Lian-xiang, GUO Jing-fu, SHUN Shu-ju, CAO Xi-zhang
A Study of Synthesis, Immobilization and Catalytic Capability of Metalloporphyrin
1998 Vol. 14 (2): 111-115 [摘要] ( 840 ) [HTML 1KB] [PDF 1935KB] ( 323 )   

A stepwise-synthesis method was used to immobilize tetrachloro-tetramethyl porphyrins in the supercages of NaCoX molecular sieve. The immobilized porphyrin was characterized by means of UV-Vis, IR, DTA, SEM and EPR. A comparision was made for the activities among tetrachloro-tetramethyl porphyrins, its cobalt(Ⅱ) complex, NaCoX molecular sieve and the immobilized porphyrin as catalysts in the oxidation reaction of styrene and p-cresol. The stability and catalytic capability of the metalloporphyrin is increased after the combination of porphyrin with molecular sieve. In addition, this new type of catalyst tetrachloro tetramethyl porphyrin immobilized in the supercages of NaCoX molecular sieve not only possesses the advantages of both porphyrin and molecular sieve, but also makes up for their respective deficiencies. The experimental results confirmed that both the stability and catalytic capability of metalloporphyrin immobilized in the supercages of molecular sieve are increased.

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ZHU Zhi-ping, ZHOU De-feng, LIU Jing-fu
Heteropolyacids Catalysis in Synthesizing Butylacrylate
1998 Vol. 14 (2): 116-119 [摘要] ( 941 ) [HTML 1KB] [PDF 591KB] ( 163 )   

The catalytic activities of some heteropolyacids(HPAs) in synthesizing butyl-acrylate are reported. It has been demonstrated that 12-tungstophosphoric acid is the most effective catalyst among more than 20 HPA(salts). Various factors concerned in this reaction have been investigated. The optimum conditions have been found, that is, the molar ratio of alcohol to acid is 1.2∶1.0 , the catalyst concentration 1%(mass fraction), the reaction time 2 h, the temperature 98—124 ℃ and a certain amount of polymerization inhibitor exists.

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QIANG Liang-sheng, FU Hong-gang, XU Chong-quan
The Solgel Preparation and Electric Properties of MnO2-doped PbTiO3 Ceramics
1998 Vol. 14 (2): 120-124 [摘要] ( 820 ) [HTML 1KB] [PDF 775KB] ( 336 )   

MnO2-doped PbTiO3 ceramics was prepared by means of sol-gel method, its density and some electric properties were investigated. The results showed that it was feasible to prepare multicomponent PbTiO3 sol-gel series with the aid of sol-gel method, the obtained MnO2-doped PbTiO3 ceramics showed a high-purity, uniform component, better dense structure, hardly crack, and had good dielectric, piezoelectric, ferroelectric and pyroelectric properties.

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ZHANG Jing-wen, ZHAO Jian-zhang, ZHANG Xiao-long, JIANG Yu-lin, MA Xiu-li, SUN Yun-xiu, JIANG Wen-pu, LI Yao-xian, XU Zhi-luo
Chemoselective Catalytic Hydrogenation of α,β-Unsaturated Ketones and α,β-Unsaturated Carboxylic Esters
1998 Vol. 14 (2): 125-130 [摘要] ( 1099 ) [HTML 1KB] [PDF 1664KB] ( 407 )   

The effect of catalysts P-2.00-Ni(Nickel boride) and P-2.00-Ni-M(M: Co, Fe, Cu, Sn), prepared by adopting a modified recipe, on the chemoselective hydrogenation of carbon-carbon double bonds in α,β- unsaturated ketones, and the activity of catalysts P 1.80 Ni, P-2.00-Ni or P-1.80(2 00)-Ni-M(M: Pd, Co, Cu) in the selective hydrogenation of carbon-carbon double bonds in α,β-unsaturated carboxylic esters, were investigated systematically. According to the experimental results, the selectivities of these catalysts toward the hydrogenation of the carbon carbon double bonds of α,β-unsaturated keones or α,β-unsaturated carboxylic esters are 96%—100% or 100%, respectively.

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ZHU Yi-qiang, TANG Hui-tong, ZHANG Pang
Formation of Pyrrolidin-1-ylcyclopentadienes via Cyclization of Alkyl-2-Dimethoxyacetyl and 2-Ethoxalyl-4-oxopentanoates
1998 Vol. 14 (2): 131-137 [摘要] ( 877 ) [HTML 1KB] [PDF 684KB] ( 249 )   

The cyclizations of alkyl 2-dimethoxyacetyl and 2-ethoxalyl-4-oxopentanoates were only effected by means of pyrrolidine with the formation of appropriately substituted 1-pyrrolidin-1-ylcyclopentadienes.

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LI Ye-zhi, GUO Chun-xiao, ZHANG Li, HUANG Hua-min
Synthesis and Quantum Chemistry Studies of (R)-N-(Propionylthiazolidine-2-thione-4-methoxycarbonyl)germanium Sesquioxide
1998 Vol. 14 (2): 138-142 [摘要] ( 836 ) [HTML 1KB] [PDF 684KB] ( 255 )   

(R)-N-(β-Trichlorogermyl propionyl)thiazolidine-2-thione-4-carboxylic methyl ether(1) and its sesquioxide(2) were synthesized. The crystal structure of 1 was determined by means of X-ray diffraction analysis, which shown that the >C=O and >C=S groups are located in the opposite sides of C(4)—N—C(3) bond with trans configuration. The electronic structures and optimized configurations of compounds 1 and 2 were studied with MNDO method.

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MA Xiu-li, HAO Chun-yan, LU Shi-xiang, SUN Yun-xiu, LIU Ju-zheng, LIU Shu-ying
Isolation and Characterization of a Bioactive Polysaccharide from Panax Quinquefolium L.
1998 Vol. 14 (2): 143-146 [摘要] ( 961 ) [HTML 1KB] [PDF 601KB] ( 226 )   

Inactivity guided experiments, awater soluble polysaccharide PPQ5-2, which shows lymphocite stimulation and interleukin induction activieties, from Panax quinquefolium L. was isolated and characterized. It is composed of D-arabinose and D-galactose in amolar ratio of 1∶1.1 in alditol acetate derivatives analyzed by means of GC. Galacturonic acid was detected with GC. The elementary analysis showed about 8% of protein in it. The molecular weight is about 21 000 determined by matrix-assisted laser desorption/ionization mass spectrometry.

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YANG Chun-he, DONG Shao-jun
The Phenomenon of Mutual Media in Polypyrrole with Electroactive Ions
1998 Vol. 14 (2): 147-152 [摘要] ( 849 ) [HTML 1KB] [PDF 1383KB] ( 308 )   

The dependence of the differential capacitance of polypyrrole doped with several typical dopants on potential is presented, which shows that the differential capacitance varies with the potential, the doped polypyrroles with electroactive ions give the largest capacitance near their formal potentials, which is attributed to the mutual media for electron transfer between polypyrrole and electroactive dopants. The existence of two conducting phases was observed in the complex capacitance plots. The electroactive anions act as an intra-conducting-phase medium for electron transfer, the electroactive cations act as an inter-conducting phase medium for electron transfer. The mutual media between polypyrrole and redox dopants lead to the increase of the discharging time.

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ZHU Yi-min, WANG Jin-cheng, LI Jing-hong, DONG Shao-jun
Electrochemical Probe of Hydroxylation of 4-Nitrophenol by Cytochrome C with Hydrogen Peroxide
1998 Vol. 14 (2): 153-159 [摘要] ( 881 ) [HTML 1KB] [PDF 997KB] ( 271 )   

The reaction of hydrogen peroxide with cytochrome c makes them coupled to lead to the hydroxylation of 4-nitrophenol. In situ electrochemical probe was used to detect the hydroxylation of 4-nitrophenol, which can avoid the tedious extraction procedure, the loss of the active species and the interference of some colored substances in the detection of 4-nitrocatechol by spectroscopic method. The hydroxyl radical scavengers mannitol and sodium benzoate did not eliminate hydroxylation, but the inhibitory effect of uric acid on the hydroxylation lead to the formation of the ferryl species of the protein during the reaction. These studies suggest that the electrochemical probe might efficiently detect the trace 4-nitrocatechol from the onset of the hydroxylation reaction and thus provides a more sensitive tool.

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WANG Tsong-hui, CHEN T. F., Barofsky D. F.
FAB MS of Permethylated L-β-Aspartamido-Carbohydrates
1998 Vol. 14 (2): 160-166 [摘要] ( 957 ) [HTML 1KB] [PDF 2191KB] ( 215 )   

Native glycopeptides are suitable to FAB mass spectrometric analysis due to their high polarity, low volatility and large molecular size. The deficiency in the FAB spectra of glycopeptides is the limited number of peaks and the low abundances of fragments. In order to obtain the information of carbohydrate sequence the permethylation of carbohydrate, a well known method, is recommended here. The L-β-aspartamido-carbohydrate from chicken egg albumin was chosen as the model compound of glycopeptides. Our experiments showed obvious carbohydrate-sequence in the spectra of permethylated aspartamido carbohydrates. The key conditions to perform the method are the methylation reagent and purification process for the permethylated derivatives.

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CHEN Song-ming, ZHANG Xue-zhong, CHAI Xiang-dong, LI Tie-jin
Studies on the Conformation of Poly(1-naphthol) Assembled by Horseradish Peroxidase in Aqueous Micelle
1998 Vol. 14 (2): 167-170 [摘要] ( 1122 ) [HTML 1KB] [PDF 721KB] ( 191 )   

FTIR, UV-visible , fluorescence spectra and calculation of CPK model indicated that poly(1-naphthol) synthesized and assembled by horseradish peroxidase(HRP) in aqueous micelle was constructed with orderly helical conformation, which was the lowest energy conformation of the polymer under this condition and resulted in an advanced π-conjugated system.

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SHE Yi-min, SUN Yu-quan, JI Yi-ping, LIU Shu-ying
Sites of Protonation and Unimolecular Fragmentation of Protonated N-Hydroxyphthalimide in the Gas Phase
1998 Vol. 14 (2): 171-175 [摘要] ( 918 ) [HTML 1KB] [PDF 644KB] ( 257 )   

The low energy collision induced dissociation, linked scan techniques and isotopic labeling experiment were used to investigate the unimolecular fragmentation of protonated N-hydroxyphthalimide under electron impact and chemical ionization conditions. It was found that this compound shows an unusual reactivity towards protonation. Two possible sites of protonation have been proposed to explain the corresponding fragmentation processes, one is that the protonation takes place on the oxygen atom of hydroxyl group, resulting in the loss of water and the other is the formation of an intermediary proton-bound complex in the fragmentation process, giving rise to the fragment ions of m/z 133 and m/z 135. The results show both cases are coexistence in the fragmentations of protonated N-hydroxyphthalimide, and the unimolecular fragmentation pathways are available.

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GUO Jun, LI Yun-lun, JIAO Qing-ze, JIANG Da-zhen, MIN En-ze
Pillaring of Zn2Al Layered Double Hydroxide by Dawson Polyoxometalate Anions
1998 Vol. 14 (2): 176-178 [摘要] ( 869 ) [HTML 1KB] [PDF 613KB] ( 222 )   

Zn2Al layered double hydroxide pillared with Dawson polyoxometalates, P2W17ZO618-(Z=Mn2+, Co 2+, Ni2+, Cu2+, Zn2+) was prepared. A basal space of ca. 16 nm indicates the intercalated Dawson ions to be oriented with their C2 axis perpendicular to the double hydroxide layers(with the exception of P2W17Zn-LDH). The IR and13P MASNMR spectral reveal that the Dawson ions retain their integrity in the interlayer space of LDH. A preliminary study shows that these compounds are highly active catalysts for the oxidation of cyclohexene with molecular oxygen.

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WU Zhi-jian, MENG Qing-bo, ZHANG Si-yuan
Structures and Vibrational Spectra of C2 and LaC2+ Clusters
1998 Vol. 14 (2): 179-183 [摘要] ( 869 ) [HTML 1KB] [PDF 707KB] ( 184 )   

C2 and LaC2+ were studied using Hartree Fock(HF), B3LYP (Becke 3-paremeter-Lee-Yang-Parr) density functional method, second order M φller-Plesset perturbation(MP2) and coupled cluster singles and doubles with non-iterative triples(CCSD(T)) methods. The basis set employed was LANL1DZ. Geometries, vibrational frequencies and other quantities were reported. The results showed that for C2, all the methods performed well for low spin state(singlet), while only HF and B3LYP remained so for high spin state(triplet). For LaC2+, four isomers were presented and fully optimized. The results suggested that linear isomers with C∞v and D∞h symmetries were predicted to be saddle points on the energy surface for all the methods, while for isomers with C2v and Cs symmetries, they were local minima except C2v at B3LYP level, and were isoenergetic at HF, MP2 and CCSD(T) levels, near isoenergetic at B3LYP level. From the differences between HOMO and LUMO, it is also known that the isomers with C2v and Cs symmetries offer the largest values and therefore correspond to the most stable structure. ForLa—C bond lengths, B3LYP gives the shortest, the order is B3LYP<HF<MP2<CCSD(T) for all the methods.

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CUI Ai-li, GE Xu-dong, HU Yong-qi, JIN Yong, WANG Xiao-hui
Studies on the Lanthanum-Modified Lead Titanate Ultrafine Particles by Raman Spectroscopy
1998 Vol. 14 (2): 184-187 [摘要] ( 927 ) [HTML 1KB] [PDF 559KB] ( 278 )   

Lanthanum-modified lead titanate(PLT14) ultrafine particles were synthesized by means of stearic acid gel method. The structure of the samples was characterized using X-ray diffraction(XRD) and TEM. The crystal graphic parameters of the samples were calculated. The Raman spectra of PLT14 powders at a high pressure as well as a high temperature reveal that the phase transition pressure or temperature shifts to a lower pressure or temperature with the decrease of grain size.

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FAN Hong-Jun, ZHONG Shi-Jun, LIU Chun-Wan
Ab Initio Studies on the Structure and Binding Interaction of M+CO2(M=Sc, Ti…Zn)
1998 Vol. 14 (2): 188-193 [摘要] ( 942 ) [HTML 1KB] [PDF 976KB] ( 146 )   

The geometry and binding interaction of M+CO2(M represents the first row transition metals) were studied using ab initio methods. In some cases the frequency calculations and basis set superposition error corrections were included. For all the complexes under the study, the linear structures were found to be the equilibrium structure. The distances of M+—O in R(M+—O) in which M has 4s electrons are obvious longer than those in which M has no 4s electrons, and from Sc to Zn the change trend is decreased, accompanied with some oscillation. The binding energy has an opposite change trend to that of the R(M+—O). Linear M+CO2 has the same spin as M+, while T-shape structures may have different spins. The static electronic interaction was found to be about 80% of the total binding energy.

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WU Cheng-pei, PAN Cai-yuan, Toshiyuki-Uryu
Syntheses of Cellulose-Type Polysaccharide by Means of Ring-Opening Copolymerization of Anhydroriboses ABRP and AIRP
1998 Vol. 14 (2): 194-198 [摘要] ( 1193 ) [HTML 1KB] [PDF 722KB] ( 225 )   

Two kinds of 1,4-anhydroribose derivatives, 1,4-anhydro 2,3-O-benzylidene-α-D-ribopyranose (ABRP) and 1,4-anhydro 2,3-O-isopropylidene α D ribopyranose (AIRP) were prepared from D-ribose. The ring-opening copolymerizations of ABRP and AIRP in various feed ratios were carried out with SbCl5 and BF3OEt2 as catalyst at low temperatures. The copolymer structure was characterized by means of 1H,13C NMR spectroscopy and specific rotation. When SbCl5 was used as catalyst, the copolymer obtained had completely 1,4-β-pyranosidic structure, i.e., cellulose type structure. However, when BF3OEt2 was used as catalyst, the copolymer had a mixed structure of furanosidic and pyranosidic units.

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XING Pei-xiang, TIAN Yan-qing, WANG Jun-zuo, NA Hui, TANG Xin-yi, JIANG Bing-zheng
Studies on Liquid Crystalline Bis[4-(p-phenoxy)-phenylbenzoate]-Alkyldicarboxylate
1998 Vol. 14 (2): 199-203 [摘要] ( 929 ) [HTML 1KB] [PDF 555KB] ( 223 )   

A new series of liquid crystals of bis[4-(p-phenoxy)-phenylbenzoate]-alkyldicarboxylate which contain two rigid groups connected by a flexible spacer was synthesized. These liquid crystals show nematic phase and were found to show odd even effect in isotropization temperature and entropy change.

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YUAN Yi, ZHAO Shi-hong, YANG Shou, CUI Ya-nan, ZHANG Rei-xue
Studies on Free Radical EPR, Superoxide Dismutase Water-soluble Lipidperoxide in Tears
1998 Vol. 14 (2): 204-209 [摘要] ( 1068 ) [HTML 1KB] [PDF 1948KB] ( 275 )   

By means of electron paramagnetic resonance(EPR), chemistry luminescence and fluorescent spectroscopy, the free radical, superoxide dismutase and water soluble lipid peroxide in tears of normal eyes(150 eyes, 100 cases), Moorens ulcer(9 eyes), coreal grafts rejection(16 eyes) were studied. The results showed that the spin density of the free radical was 3.6(±0.58)×1012 spins/mL tear, the content of the superoxide dismutase(SOD) was 3.84(±1.45) ng/mL tear, the opposite fluorescent density of the water soluble lipid peroxide was 12.912(±1.691) U/mL tear in normal tears. The normal values are 2.5—4.8×1012 spins/mL tear for free radical, 2.39—5.29 ng/mL tear for SOD, 9.598—16.225 U/mL tear for water soluble lipid peroxide. There are significant differences in different eyes, different sexes and different ages. The free radical and lipid peroxide are higher obviously in the tears of patients with Moorens ulcer and rejected corneal grafts, compared with those of the normal control subjects(P<0.01), SOD is lower evidently(P<0.01). The above fact shows the pathogenic mechanism of Moorens ulcer and keractoplasty rejection is significantly related to toxicities injuring effect of the free radical. These results have provided important experimental data for studying lacrimalogy and new methods for clinical diagnosis and treatrment.

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LIU Wei, SHI Tong-shun
Synthesis and Characterization of Liquid Crystal of meso-Tetra(4-n-octanoyloxyphenyl)porphyrin
1998 Vol. 14 (2): 210-212 [摘要] ( 886 ) [HTML 1KB] [PDF 530KB] ( 159 )   

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ZHOU Jian, HU Yue-fei, HU Hong-wen
Preparation of Indolizine by Intramolecular 1,5-Dipolar Cycloaddition of Pyridinium N-Allylides
1998 Vol. 14 (2): 213-214 [摘要] ( 788 ) [HTML 1KB] [PDF 342KB] ( 321 )   

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LU Xin, XU Xin, WANG Nan-qin, ZHANG Qian-er
A Molecular Orbital Study of No Adsorption on Magnesium Oxide
1998 Vol. 14 (2): 215-217 [摘要] ( 861 ) [HTML 1KB] [PDF 469KB] ( 154 )   

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LIU Mo-xiang, ZHENG Yi-nan, LIU Xiao-feng, LI Xiang-gao, XIANG Lan
Isolation and Identification of Flavone Type of Two Compounds from Salix matsudana
1998 Vol. 14 (2): 218-220 [摘要] ( 868 ) [HTML 1KB] [PDF 487KB] ( 289 )   

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WANG Ben-zhong, ZHAO Fang-hai, PENG Yu-heng, JIN Zhi, LI Yu-dong, YANG Shu-ren, LIU Shi-yong
Formation of Self-organization InAs Quantum Dots on (001) InP Substrate by As/P Exchange Reaction in MOCVD
1998 Vol. 14 (2): 221-224 [摘要] ( 1019 ) [HTML 1KB] [PDF 495KB] ( 357 )   

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