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Table of Content

    24 December 1991, Volume 12 Issue 12
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    Articles
    Synthesis and Properties of Cobalt Tetraphenyloxyphthalocyanine and Its Complexes with Derivatives of Pyridine
    Wu Xing, Liu Chang-qing, Zhang Guo-lin, Huang Ming-chang, Zhu Xun-zhi
    1991, 12(12):  1563-1567. 
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    2,2', 2",2''' -Tetraphenyloxyphthalocyanine cobalt [TPhOPcCo(Ⅱ)] and its complexes with derivatives of pyridine [TPhOPcCo(Ⅱ)(L)2] (L=pyridine, 4-methylpyridine, 2-aminopyridine) were synthesized. Their IR, UV-Vis, half-wave potentials (E1/2) and electron transfer rate constants of the redox reactions for the complexes in DMF were measured. The change of UV-Vis spectra for the complexes was studied when electrolysed at different voltages.
    Preparation of Bi-Pb-Sr-Ca-Cu-O Micro-powder by Sol-Gel Method
    Xu Qin-lun, Peng Ding-kun, Meng Guang-yao, Yu Dong, Bie Li-jian, Wei Zheng-hui, Yang Li
    1991, 12(12):  1568-1571. 
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    This paper reports the preparation processes of Bi-Pb-Sr-Ca-Cu-Omicro-powder by Sol-Gel method, using metal acetates as starting materials. Wanalyzed the mechanisms of decomposition of synthesized powders and their crystallization behavior by means of thermo-gravimetric analysis, differential thermal analysis, infrared spectra and X-ray diffraction. Also we determined the sizes of powder decomposed at different temperatures by using transmission electron microscope. Meanwhile a high -Tcceramic superconductor which has 2223 as the main phase and zero resistance 105Kwas fabricated by using these micro-powders.
    Studies on the Cobalt Clusters(Ⅳ)--The Syntheses and Characterization of Sulfuro-Trinuclear Cobalt Carbonyl Clusters Containing Bridging Heterocyclic Thioamide and Heterocyclic Carbene
    Liu Shu-tang, Jin Zhen-xing, Hu Xiang
    1991, 12(12):  1572-1575. 
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    The preparation of two kinds including six new Co3-carbonyl clusters with chiral tetra-hedral Co3S frameworks, containing bridging heterocyclic thioamide and heterocyclic carbene lig-ands is described. The reaction of Co2(CO)8with heterocyclic thioamides SCXCH2CH2NH(X= NH,S,O) yielded products Co3(CO)7(μ3-S)(μ-SCXCH2CH2N)(Ⅰ)and Co3(CO)6(μ3-S) (2CXCH2CH2NH) (μ--SCXCH2CH2N) (Ⅱ), in which μ-SCXCH2CH2N is a three-electron bridging ligand linked by Sand Nto two cobalts, and: CXCH2CH2NH is a heterocyclic carbene ligand. These six clusters have been characterized by IR, 1HNMR spectra and MS.
    Studies on the Syntheses and Properties of Heteropoly Tungstoborate Complexes of Lanthanide Elements
    Wang En-bo, Liu Lian-li, Shen En-hong, Wang Zuo-ping
    1991, 12(12):  1576-1578. 
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    In the paper the preparation of eleven heteropoly compounds was reported, which are K15[Ln(BW11O39)2]·xH2O(Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Yb). They were systematically studied and characterized by TG-DTA.IR, UV, XPS, polarography and elemental analysis.
    Syntheses and Characterization of Some New Complexes of Cu(Ⅰ) with Substituted Alkenes
    Liu Yun-shan, Xiao Ya-ping, Bei Mei-zhi
    1991, 12(12):  1579-1580. 
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    Four new complexes of Cu(Ⅰ) with substituted alkenes were synthesized successfully in N2atmosphere. The structures of the four complexes were characterized by microanalysis and IR. It was found that the complexes were moderately stable in an inert atmosphere at room temperature.
    Mechanism of Enhancement of Surfactants on Manganese in Flame Atomic Absorption Spectrometry
    Wang Fu-yi, Wan Jia-liang, Lu Han-bing, Xia Wang
    1991, 12(12):  1581-1584. 
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    Anew enhancing mechanism of surfactants in FAASis proposed. This paper narrates that below the cmc of surfactants, the enhancement results primarily from enrichment of analyte in small droplets of aerasols because of the surface effect of surfactants, and above the cmc, the enrichment is getting less and less, and the new enhancement results from the binding of analyte to micellae in bulk. And in flame, amplifying of reductive environment because of the incomplete burning of surfactants is always one of the enhancing factors.
    Electrochemical Study on the Transfer of Proton Across the Water/ Nitrobenzene Interface Facilitated by Neutral Carrier
    Cai Zhen, Li Jian-wei, Wu Ya-ying, Qi De-yao
    1991, 12(12):  1585-1587. 
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    Facilitated transfer of proton across the water/nitrobenzen interface was studied with cyclic voltammetry in the presence of N, N' -diheptyl-N, N' dimethylsuccinic acid diamide (ETH1117) in the nitrobenzene phase. The neutral carrier acts as the carrier, the complex formation makes the translocation of the ion across the water/nitrobenzene interface. The transfer of proton across the interface is a reversible process controlled by diffusion. The complex ratio of the complex of proton and ETH1117 in nitrobenzene is 1: 1 and the stability constant is 2.9× 107. The diffusion coefficient of ETH1117 in nitrobenzene is 4. 2×106cm/s.
    A Simple UV-Visible, Circular Dichroism Thin-layer Spectroelectro-chemical Cell with Long Optical Path
    Zhu Yong-chun, Cheng Guang-jin, Dong Shao-jun
    1991, 12(12):  1588-1591. 
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    Asimple UV-visible, circular dichroism thin-layer spectroelectrochemical cell with long optical path has been designed and characterized. The cell with 10 mm quartz cuvette as the optical window, two pieces of 5 mm×10 mm×15 mm teflon as the electrode supporters and a glassy carbon slide as the working electrode has an adjustable thickness of thin-layer. We have carried out the optical and electrochemical experiments of characterization with K3Fe(CN)s and tyrosine working system, which show the cell has a very good thin-layer electrochemistry character and fast spectroelectrochemistry response. The cell can also be used in circular dichroism electrochemistry study.
    Separation of Overlapping Incisions of A.C.Oscillopolarogram Using Kalman Filter
    Bi Shu-ping, Du Si-dan, Wang Zhong, Gao Hong(H. Kao)
    1991, 12(12):  1592-1594. 
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    Kalman filter technique for the separation of overlapping incisions of a. c. oscillopo-larogram is presented. The experimental verifications were carried out in various systems with the ions of Pb2+, Tl+, In3+and Cd2+. The results show that the concentration of depolarizer can be determined directly and easily with this technique while other interference elements exist.
    An Investigation of the Chemiluminescence Reaction Between Luminol and Reductants(Ⅱ)--The Chemiluminescence Reaction of the V(Ⅰ)-Luminol System
    Lu Jiu-ru, Zhang Xin-rong, Zhu Zhi-jia, Zhang Zhu-jun, Li Mei-qing
    1991, 12(12):  1595-1597. 
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    The chemiluminescence(CL) reaction of the V(Ⅱ)-luminol system was examined by the flow injection system with the Jones reductor. Anew method for the determination of Von the basis of this reaction is reported. The detection limit is 8 × 10-11g/mL V. The relative standard deviation is less than 2%(1.0×10-8g/mL V, n=11). The method has been applied to the determination of Vin water samples.The mechanism of V(Ⅱ)-luminol reaction is as follows:
    The Determination of Oxalate in Urine by the Tissue-Based Membrane Sensor of Banana Skin Acetone Pulp as Biocatalyst
    Fang Yao, Cai Rong-hui, Deng Jia-qi, Wang Ping, You Da-heng
    1991, 12(12):  1598-1599. 
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    Coupling of acetone-precipitated pulp from the banana skin to an oxygen electrode, an amperometric tissue-based sensor for oxalate is prepared. The linear response range of this sensor is 0. 01 -0. 5 mmol/Lwith a detection limit of 2.5 ×10-6mol/L. It has a response time less than two minutes and an useful lifetime of thirty days.
    Studies on the Polysaccharides from the Pollen of Codonopsis Pilosula (Franch.) Nannf.
    Liu Zhan-zhu, Zhu Guo-fen, Jin Sheng
    1991, 12(12):  1600-1604. 
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    Five water-soluble polysaccharides, CPA, CPB, CPC, CPDand CPE,were isolated and purified from the pollen of Codonopsis Pilosula. Their purity was identified by gel-filtration and electrophoresis. The average molecular weights were estimated by gel-filtration. Hydrolysis, methylation, periodate oxidation and Smith degradation methods were used in the structural studies of CPA. The absolute configurations of the monosaccharides of CPAwere identified by measuring the optical rotation of the mixture of the monosaccharides. IR, 1H NMR, 13C NMRand 1H, 13Ccoupled NMRspectra of CPAwere analysed. The transmission electron microscopy (TEM) investigation of CPAshowed a clear secondary structural picture. Some information was attained about the structural feature through analysing the micrograph of CPA.
    Syntheses of 2,5-Diphenyl-3,3-disubstituted-2,3-dihydro-1,4,2-oxazaphosphole-2-oxides by Mannich Reaction
    Chen Ru-yu, Feng Ke-sheng
    1991, 12(12):  1605-1608. 
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    By using Mannich reaction with benzamide, aldehydes (or ketones) and phenyldi-chlorophosphine as the starting materials and with the product being partially hydrolysed, α-(N-benzoyl) aminoalkyl phenylphosphinic acids (Ⅰ) were synthesized. The products (Ⅰ) were cy-clized to 2, 5-diphenyl-3, 3-disubstituted-2, 3-dihydro-1, 4. 2-oxazaphosphole-2-oxides (Ⅱ) by dehydrating with SOCl2and Et3N. The structures of Ⅰ and Ⅲ are confirmed by 1H NMR and elementary analysis. The mechanism of the Mannich reaction is also discussed.
    Studies on the Concentration Effects on Ultraviolet Spectra of Organic Iron-Sulfur Cluster Complexes
    Li Song-lan, Yang Xue-jin, Yu Mei, Liang Shu-sen, Song Li-cheng, Hu Qing-mei
    1991, 12(12):  1609-1612. 
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    The ultraviolet spectra of organic iron-sulfur cluster complexes in dichloromethane in the range of 190-400 nm have been studied. It was found that the ultraviolet absorption peaks (λmax)of these compounds showed noticeable bathochromic shifts due to π-π*transition with increasing the solution concentration. But the compounds containing isolated C-Sbond or C=Obond did not show such shifts. We also studied some π-π or n-π conjugated compounds and discovered that their ultraviolet obsorption peaks (λmax) showed bathochromic and hypsochromic shifts due to π-π*and n-π*transion, respectively, with increasing the solution concentration.
    Studies on the Chemical Constituents of Saussurea Gossypiphora D.Don
    Zheng Sheng-zhen, Yu Jian-hua, Shen Xu-Wei
    1991, 12(12):  1613-1616. 
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    Sixteen compounds have been isolated in the first time from the aerial parts of saus-surea Gossypiphora D. Don. On the basis of IR, UV, 1H NMR, 13C NMR, MS and chemical methods as well as comparison with authentic samples. Fourteen compounds were identified as follows; Tritriacontance(1),1-Tetrocontene(2), Dotriacontanoic acid (3),Ergostan-3,24-diol (4), β-Sitostercol(5), Stigmast-7-en-3-ol(6), Aretigenin(7), 2-Hydroxylappaol B(8), Api-genin (9), Quercetin(10),Arctin(11), Apigenin-7-O-β-D-glucoside(12), Chrysoeriol-7-O-β-D-glucoside(13), Apigenin-7-O-β-D-neonesperidoside(14). Among them (4) and (8) are two new compounds. (2), (6) and (14) are reported for the first time in the genus of this plant.
    Studies on the Self-Oxidation of Metal loporphyrins
    Guo Can-cheng, Liu Xiao-yu, Yang Ming-sheng, Zhu Shen-jie, Gui Ming-de
    1991, 12(12):  1617-1619. 
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    We synthesized 9 kinds of metalloporphyrins and studied systematically the kinetic properties of their self-oxidation during the biomimetic oxidation of hydrocarbons. It has been proved that the kinetic properties of the self-oxidation of the metalloporphyrins depend on the metal ions bonded with the porphyrins. The reaction is second order for ironporphyrins or chro-moporphyrins, and first order for manganoporphyrins. It is shown from the results that the rateof the reaction is much related to the structure of the porphyrins--the substituents on the por-phyrin ring and the axial ligandsr the properties of the oxidants and the reaction mediums, and is abated by adding some neutral organic ligands to the reaction system.
    Synthesis of 2-Isopropyl-1,3-Dihydro-4(1H) Isoquinolone and Its Derivatives
    Qian Jian-hua, Jiang Gui-ji
    1991, 12(12):  1620-1622. 
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    Compound (2) was synthesized through condensation of ethyl N-isoproyl-N-(2-car-boethoxy benzyDglycinate. Compound (1) was obtained from the hydrolysis and decarboxylation of (2) in the presence of 18% HCl.Derivatives of (1), (3a-6e) were produced by condensation of (1) with benzaldehyde and p-substituted benzaldehyde, phenylhydrazines and oxime or (4) with benzoyl chlorides, respectively. Benzodiazepinone (7) was prepared by Beckmann rearrangement of (4) or reaction of (1) with NaN3. Pyrazolo-isoquinolones(8a-d) were synthesized through the condensation of (2) with hydrazine or substituted hydrazine, respectively. The structures of 20 new compounds have been confirmed by element analysis, IR and 1HNMR.
    Synthesis of Diethyl 2,3-dicyano-2,3-Bi(p-substituted phenyl)-succinates and Its Decompositions in Styrene
    Yang Di-lun, Qi Chen-ze, Li Zhao-long, Liu You-cheng
    1991, 12(12):  1623-1626. 
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    Diethyl 2,3-dicyano- 2,3-bi(p-Xphenyl)specinates(X=OCH3, CH3,Cl, NO2) were synthesized and meso and dl-isomers were separated for the each diester by fractional recrystal-lization, of which the structures were determined by means of elemental analysis, 1H NMR,IR, MS and X-ray crystallogram analysis. The rate constants of the thermal decomposition of these compounds in styrene at 100℃ were observed by use of dilatometry. The results indicated that kt of meso-isomers with the exception of compound 1 are larger than kd of dl-isomers, and the influence of the p-substituents in benzene ring on kd is in the following order: OCH3>CH3>Cl>H.
    Studies on the 1H NMR Spectra of meso and dl diethyl 2,3-dicyano-2,3-bis(p-substituted phenyl)succinates
    Yang Di-lun, Qi Chen-ze, Cui Yu-xin, Dang Hai-shan, Liu You-cheng
    1991, 12(12):  1627-1630. 
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    The 1H NMR spectra of mesa and dl diethyl 2,3-dicyano-2,3-di(p-Xphenyl)succi-nates(X=OCH3, CH3, H, Cl, NO2) and 1H Noesy spectra of meso and dl isomers of the diethyl ester with X=CH3were determined by using Bruker Am 400 MHz superconducting NMR spectrometry. The corresponding proton of the substituent groups attached to the two central carbon atoms in the molecules are chemical shift equivalence. The average difference between o -1Habsorptions of phenyl in the dl-isomers and that in meso-isomers was found to be △δdl-meso= -120. 1 ± 6.1 Hz. All of the meso-isomers, then, have, methylene (ABX3system) and methyl in the ethoxy at upfield positions, and all of the dl-isorners have that at downfield positions, △δdl-meso= 53. 3 ± 5. 9 Hz and △δdl-meso= 53. 5 ± 5. 4 Hz for Aand Bprotons in the methyienes, and △δdl-meso=39. 3+3. 5 Hz for protons in the methyls. △δdl-meso is the mark of influence of molecular configuration on the chemical shift.
    Catalytic Behaviour of Synthetic SMM and Pillared SMM in the Animation of Ethanol
    Ren Bei-yuan, Liu Zi-yang, Jiang Da-zhen, Min En-ze, He Ming-yuan
    1991, 12(12):  1631-1634. 
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    Synthetic mica-montmoriilonite (SMM) was synthesized by using the hydrothertnal method. Pillared synthetic dioctahedral clays(Al-CLS) were prepared by crosslinking SMMwith hydroxyl aluminium oligomer between the layers. The results obtained by DTA and IRindicate that the dehydroxylation of octahedral hydroxyl group is easier at a high temperature calcination because of pillar introduced. The surface acidity of SMM and Al-CLSmeasured by NH3-TPDand pyridine adsorption showed that Al-CLSpresents even more sites of weaker and stronger acid than SMM. The dehydration-amination of ethanol with ammonia was studied over SMM and Al-CLSat 400℃ under ambient pressure. It is found that the weak acid sites on the surface favour the dehydration of ethanol and the NH3molecular adsorpted on the strong acid sites favour the amination of ethanol. The results from NH3-TPD, C2H5OH-TPD and estimation test showed that the reaction between NH3adsorpted on the strong acid sites and gas state C2H5OH perhaps occur in the amination of ethanol.
    In-Situ FTIR Reflective Spectroscopic Study of Electrochemical Activation of Glassy Carbon Electrode
    Dai Hong-ping, Sun Shi-gang, Wu Hui-huang, Zhou Shao-min
    1991, 12(12):  1635-1639. 
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    In-situ FTIR reflective spectrometry was used to study the formation and the changes of oxygen-containing functional groups on the GCelectrode surface during its electrochemical activation. The surface functional groups were formed during the high-potential oxidation of GCelectrode, some of which were further oxidized to CO2Parts of the quinone-like groups were reduced during the cyclic voltammetric process thereafter, and stable surface redox couples were formed at the end. In the differential FTIR reflective spectra in these cycling processes appeared positive peaks at 1669 cm-1and 1690 cm-1, corresponding to quinone-like groups and a wide negative peak at 1590 cm-1, corresponding to the stretching vibration of carboxylic anion and aromatic ring. The potential difference spectra showed a pair of bipolar peaks at 1705 cm-1and 1750 cm-1and peaks at 1605 cm-1and 1580 cm-1. These results are explained by supposing hydrogen-bonding between quinone-like groups and carboxylic groups and the chemical and electrochemical processes of the surface functional groups.
    The Electronic Spectra of [M2(η5-C5H5)2(CO)4] with Weak Metal-Metal Bond and M(η5-C5H5)(CO)2Cl(M=Fe,Ru)
    Li Zhi-ru, Wang Hai-tao, Li Qian-shu, Li Jun, Feng Ji-kang, Zheng Zhi-ren
    1991, 12(12):  1640-1643. 
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    The Electronic Spectra of CMCP(CO)2]2and MCp(CO)2Cl(M=Fe,Ru) are studied by means of INDO/CI method. The calculated values of wave number and transition intensity of the spectra correspond with the experimental results. The bands are assiged and the nature of their charge trasfer is discussed. The blue shift of the same label band with M-Fe,Ru are explained. In addition, the reactions of isomerization and photochemistry are discussed.
    Anion Negative Adsorption by Montmorillonite Colloid Surface with Overlapping Electric Double Layers
    Jiang Xin, Yin Da-qiang, Xue Jia-hua
    1991, 12(12):  1644-1646. 
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    Anion negative adsorption by montmorillonite colloid surface with overlapping flat double layers was determined and the influence of the overlappping degree of the flat double layers and the electrolyte concentration on the anion negative adsorption is discussed. The experimental results are concluded as following: (1) the overlapping degree of the flat double layers can be described by the variation of the ratio of the electric potential at the midplane,φd, to the electric potential at the Outer Helmhotz Plane(OHP), φδ; (2) the overlapping degree of the flat double layers, φd/φδ, raises with the increase of the applied pressure; (3) the anion negative adsorption decreases with the increase of the overlapping degree of the flat double layers and the increase of the electrolyte concentration.
    Studies on Ruthenium Used as the Promoter of Co-Mo/Al2O3Catalyst in Hydrodesulfurization
    Xiao Feng-shou, Xin Qin, Guo Xie-Xian
    1991, 12(12):  1647-1650. 
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    Catalytic performance of Ru-Co-Mo/Al2O3and Co-Mo/Al2O3catalysts in thiophene conversion as a model reaction of hydrodesulfurization has been performed, and it is shown that the conversion of thiophene on Ru-Co-Mo/Al2O3catalyst is 2 times of that/on Co-Mo/Al2O3.The infrared adsorption of COand NOon the catalysts reveals that the frequencies of COand NOadsorbed on Co, Mo sites of Ru-Co-Mo/Al2O3were shifted to low wavenumbers and their intensities were increased, in contrast to those on Co-Mo/Al2O3catalyst. It is suggested that some d electrons of ruthenium in Ru-Co-Mo/Al2Os were transferred into Co, Mo sites, leading to an increase of COand NOadsorption abilities.
    Studies of Properties of Salt of 10,12-Tricosadiynoic Acid LB Films
    Bai Yu-bai, Li Li-hua, Wang Ya-ru, Tang Xin-yi, Li Tie-jin, Tang Da-xin, Dong Xi-juan, Wang Hui
    1991, 12(12):  1651-1654. 
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    10,12-Tricosadiynoic acid was synthesized and its LBfilm was deposited onto quartz, CaF2and silicon substrates. The polymerization behaviour of LBfilm of 10,12-tricosadiynoic acid under UV-radiation was monitored. The molecular orientation of the 10,12-tricosadiynoic acid Cd2+salt LB film was analyzed by linear dichroic behaviour of FTIRspectrometry. The results of small angle X-ray diffraction showed that the layer structure of LB film was not destroyed after polymerization, and the equal period, 4. 26 nm, has slightly changed, but the line intensity of X-ray diffraction decreased.
    Diffusion Kinetics of Rare Earth Ion in Bidispersed Porous Cation Exchange Resins
    Ling Da-ren, Zheng Zu-ying, Chang Sheng-dong, Dan Gui-ping
    1991, 12(12):  1655-1658. 
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    Experiments for determining cerium isotope ion exchange rates with macroporous resins Amberlyst 15, D001 and XN1010 are discribed. The kinetics of the isotope ion exchange reaction has been examined by a simple theoretical equation of intraparticle effective diffusivity De in a porous ion exchanger. The ion exchange proceeds by diffusion within the macropores and the solid phase of the resin. De of cerium was affected by the concentration of the bulk solution C. and was separated into a macropore diffusivity Dp and a solid phase diffusivity D by the equation. The diffusion coefficients of the exchanging ion are shown to have the values in the macro-pores comparable with their valuse in the bulk solution and to have the values in the solid phase comparable with their values in gel resin with the same crosslinkage as the resins used for the experiments.
    Spectroscopic Analysis of a Series of Fe4S4Clusters
    Niu Shu-yun, Li Shu-qin, Nan Yu-ming, Xu Ji-qing, Cai Hui, Wang Tie-gang
    1991, 12(12):  1659-1662. 
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    The data of electronic and infrared spectra are reported for the following four Fe4S4clusters: (Ⅰ) [Et4N][Fe4S4(Et2dtc)4], (Ⅱ) [Et4N],[Fe4S4(Et2dtc)4], (Ⅲ)[Et4N]3[Fe4S4(Et2dtc)4],(W)[Bu4N]2[Fe4S4(Ph-S)4]. According to the weak-ligand-field theory and the structure informations provided by X-ray diffraction, all the spectra were analyzed, assigned and listed in this paper. Comparing the individual spectra with each other, the following regulations can be drawn: (1) If the geometric structures of coordination anions are the same, the change of valence state of the central ion causes the apparent shifts of d-d bands in the electronic spectra and maintains infrared spectra principally. (2) In the coordination anions, the increase of oxidation state of the central ion results in the red-shift of M←L charge transfer bands. (3) If electron-pushing ability of the groups connected with the coordinating atom increases, the vibration bands of M-L bond move to the higher frequencies. These regulations above just show that our assignment to the spectra is reasonable.
    Thermodynamic Studies of Hydrochloric Acid in HAc-H2O Systems
    Song Wen-yu, Wang Feng-yun
    1991, 12(12):  1663-1665. 
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    By using a glass electrode and a numerical ionometer, an EMF measurement for the cellglass (H+)|HCl(m), HAc+H2O|AgCl-Agwas performed in a series of HAc-H2O mixed solvents with the concentration of HCl as 0. 020, 0. 040, 0. 060, 0. 080 and 0. 100 mol/kg-solvent. The average activity coefficients for HC1in the mixed solvents and the standard transfer free energy for the electrolyte from water to the mixed solvents are evaluated, and a discussion about the results is given briefly.
    The Electrocatalytic Activity of Nickel and Molybdenum Implanted in Titanium Substrates
    Wu Zhong-da, Li Song-mei, Lin Wen-lian, Ding Xiao-ji
    1991, 12(12):  1666-1668. 
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    The catalyst was prepared by implanting Ni and Mo into Ti substrates. Ti was implanted with 1×1016ions·cm-2of Ni and 1×1016-1×1017ions·cm-2of Mo. The concentration profiles of Ni and Mo implanted were measured by XPS. The quantitative measurements show that the concentration profiles of Ni and Mo in Ti are approximately Gauss profiles. The current density potential curves of the cathodic hydrogen evolution reaction show that Ni and Mo implanted into Ti electrode exhibit a low hydrogen overvoltage (110-180 mV at 25℃, 200-400 mA· cm-2, in 30 wt% KOH) and an excellent stability. The observed electrocatalytic activity is explained provisionally by an interaction between the ions implanted in Ti.
    The Theoretically Thermodynamic and Kinetic Studies on the Scission and Rearrangement of NH2NO2
    Ju Guan-zhi, Ju Quan
    1991, 12(12):  1669-1671. 
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    Using the computational results of quantum chemistry at CI4d level, this paper has finished the thermodynamic and kinetic calculations theoretically for the reactions NH2+NO2←NH2NO2←NHONO←NH2O+NO The results show, the rate of NH2O-NO scission is much larger than that of the rearrangement of NH2NO2for the direction of nitro-nitrite rearrangement, while the N-NO2bond scission and the rearrangement should be competed quite evenly. It is expected that factor A of them is larger The above results are all in agreement with Golden' s experiment on DMNA[(CH3)2NNO2] basically, showing the thermodynamic and kinetic calculations on the system are successful. In addition, a set of thermodynamic functions of the reactions is given. All the results have never been found in literatures.
    1HNMR Studies on 2,6-Bis(benzoimidazol-2' -yl)pyridine and Its Ru(Ⅱ) Complex
    Xiao Xiao-ming, Masa-aki Haga, Takeko Matsumura-Inoue
    1991, 12(12):  1672-1674. 
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    1HNMR spectra of 2, 6-bis(benzoimidazal-2'-yl)pyridine and its Ru(I) complex were assigned by HOMO decoupling method. For the complex, H1, H2and H2' have a small downfield shift in comparison with the free ligand because of theσ-effect, while H9, H9' have a larger upfield shift because of the ring current effect of the phenyl groups.
    Studies on [Pt]-Ni(Ⅱ) Electrode
    Chai Li-fen, Ghen Yan-zhen, Gao Yuan-zhong
    1991, 12(12):  1675-1676. 
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    When Pt is immersed in a nickel salt solution, Ni(I) ion can be attached to the Pt substrates owing to specific adsorption for anion and thus [Pt]-Ni(I) electrode is formed. The electrode has a redox peak in NaOH electrolyte(0. 1 mol/L) obviously.
    Studies on the Ringed SpheruHtes of Nylon 1010
    Zhu Cheng-shen, Li Xiou-dao, Li Hua-guang, Pu Shuai-tian
    1991, 12(12):  1677-1680. 
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    The morphology and optical property of ringed spherulites of nylon1010and its formation conditions have been studied by a polarizing microscope. In isothermal crystalization process, only positive ringed spherulites can be formed. In cooling process, positive, negative and mixed ringed spherulites are formed from the nonringed spherulites with the same optical property. In heating process, mixed and positive ringed spherulites can be transformed into 6-sectional and assymmetric 4-sectional ringed spherulites, and negative nonringed ones are changed into another kind of negative ringed spherulites.
    Plurality of Active Centers on Heterogeneous Ziegler-Natta Catalysts(Ⅰ)--Studies on the Molecular-Weight Distribution of Polymer Synthesized by Titanium Catalysts
    Fan Zhi-qiang, Feng Lin-xian, Yang Shi-lin
    1991, 12(12):  1681-1685. 
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    The molecular-weight distribution (MWD) graphs of polyoctene-1 synthesized by TiCl3or TiCl4/MgCl2with A1(C2H5)3, A1G-C4H9)3or A1(C2H5)2Cl were accurately fitted with 3-5 Schulz-Flory "the most probable" distributions of different position and area, and the position and area of the theoretical distributions change regularly with the catalyst and polymerization conditions, showing that each of the "the most probable" peaks corresponds to a certain kind of active center, and the broad MWD (Mw/qn=3-12) of the studied polymer is the results of 3-5 kinds of active centers. The plurality of active centers was also evidenced by measuring thenumber of active centers in the polymer fractions of different molecular-weight. The characteristics of different active centers as well as the polymerization mechanism are discussed based on the results of MWD fitting.
    Hydrogenation Properties of Palladium Catalyst Dispersed on Poly N-Vinyl Pyrrolidone
    Chen Chun-fu, Sun Jun-tan, Li Hong, He Bing-lin
    1991, 12(12):  1686-1688. 
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    The palladium catalyst dispersed on poly N-vinyl pyrrolidone was prepared. The rate for the hydrogenation of olefins, nitrobenzene and methyl acrylate in different solvents over the catalyst was examined. The experimental results indicate that both the hydrogenation rate and the reaction order of different substrates are different dramatically from each other. The rate for the hydrogenation of methyl acrylate is greatly affected by the solvent. Kinetics for the hydrogenation of methyl acrylate in methanol was also studied.
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