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    24 June 1988, Volume 9 Issue 6
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    Articles
    Syntheses and Properties of Ternary Complexes of Rare Earth Elements with 1-Amino-2-Naphthol-4-Sulfonic Acid and Phenanthroline
    Wang Liufang, Wu Jigui, Ma Xianxian, Ren Yanping, Yan Guohong
    1988, 9(6):  535-540. 
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    In this paper, syntheses and properties of solid tertiary coordination compounds of the title compound (1-2-4-acid, ANSH) with rare earths and o-phenanthro-line (Phen) were studied.The four coordination compounds obtained were confirmed as [RE(ANS)2· Phen] Cl·xH2O, for La and Nd, x= 1, for Eu, x = 2, for Ho, x = 5. Comparison of their IRspectra with that of ANSH, three conclusions can be drawn:1) intermolecular H-bond of ligand ANSH is ruptured accompanying formation of coordination compound, 2) proton dissociation of sulfonic acid group occurred,3) OHgroup probably participated in coordination.The characteristic 1H NMRshifts belonging to Phen shifted to high field in the coordination compounds. This shows the participation of N-atom in Phen in coordination with REion, which in turn decreases both the aromaticity of Phen and descreening action of π-electron cloud in benzene ring. The fluorescence spectra showed the decreasing of aromaticity of Phen after coordination. The thermogram shows the higher thermal stability of coordination compounds. Different 2θ and I/I0 values in the X-ray diffraction pattern show the formation and the similarity of new coordination compounds. The coordination compounds obey activation type electric conduction pattern, so that they are a good class of semiconducting materials.
    Synthesis of Fe(Ⅲ), Co(Ⅲ), Ni(Ⅱ),Cu(Ⅱ),Zn(Ⅱ) Complexes of Sulphur Containing Schiff Bases
    An Xingmin, Zhao Jishou
    1988, 9(6):  541-546. 
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    Five sulphur containing, schiff bases and eight complexes have been prepared and characterized by elemental analysis, IR, 1H NMRand MS. Some of the structures determinded are shown as follows.
    The Gathodic Reduction of Carbon from LiCl-KCl-NaGl Molten Salts
    Mo Wenjing, Duan Shuzhen, D. Inman
    1988, 9(6):  547-550. 
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    The electrochemical behaviour of carbon in diluted carbonate solution of LiGl-KCl-NaCl eutectic melt at 723K was studied by using cyclic, voltamme try arid chronoamperometry.
    Studies on Wet Chemical Synthesis of Y2O3 Stabilized ZrO2
    Fu Peiihen, Zhou Feng, Yang Pinghua, Meng Guangyao, Peng Dingkun
    1988, 9(6):  551-555. 
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    The fine powder of Y2O3 stabilized ZrO2 with fec structure was. synthesized by a wet chemical method. Thermal analysis techniques(DTA, TGand DSC),X-ray diffraction and electron microscope (TEMand SEM) etc. were applied to study the formation of fcc phase and the sintering behaviour of the powder. ACimpedance measurement showed that the sintered YSZsamples exhibited higher conductivity than that reported in literature in lower temperature range(<750℃) . The formation mechanism of YSZfcc phase and temperature dependance of conductivity were discussed.
    Photoacoustic Spectrometry Investigation, and Determination of Rare Earth Ions Ho3+ arid Nd3+ in Liquid
    Yan Hongtao, Deng Yanzhuo, Zeng Yun'e
    1988, 9(6):  556-559. 
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    The applications of the pulsed laser photoacoustic spectroscopy. to the rare earth spectra and trace analysis are presented. Ahome-made high sensitive photoacoustic transducer was used to. detect the photoacoustic signal in liquid. The high resolution photoacoustic spectra of Ho3+ ion in different, solvents, were mea-sured and compared with its absorption spectrum. It also discusses how the phqto-acoustic sensitivity is affected by laser pulse energy, temperature of measurement and the organic solvents which can be mixed with water. The trivalent rare earth ions Ho3+ and Nd3+ in aqueous acetonitrile solution had been determined. The detection limit is 5×10-8mol/Lfor Ho3+,1.0×10-7mol/Lfor Nd3+, and corresponds to the absor.bance of 1.5×10-7 and 6.3×10-7, respectively.
    Investigation of Simultaneous Spectrophotometric Determination of Multielement——Calculation of Zirconium and Hafnium Amounts in a Mixed System by CPA-Matrix Methed
    Zhou Zheren, Wang Zhenqing
    1988, 9(6):  560-563. 
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    The previous method with m-NPFand CTMABas reagents for spe-ctrophotometric determination of microamount of zirconium has been developed for simultaneous determination of microamount of zirconium and hafnium in this work. The determination is based on the calculation by CPA-M-atrix method. The optimum experimental conditions for the determination have been established and ten mixed samples with arbitrary proportions of Zr and Hf wereexamined by this method with very satisfactory results.Meantime the problem of selecting wavelengths which is the key to the determination is discussed thoroughly and concepts of "correlation wavelengths" and "correlation components" are proposed in this paper.
    Investigation on Triangular-wave AC Oscillopolarography(Ⅰ)——Properties of Triangular-wave AC Oscillopolarogram
    Qi Hong, Ma Xinsheng, Gao Hong(H. Kao)
    1988, 9(6):  564-567. 
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    Triangular-wave current sweeping was used in ACoscillopolarography instead of sine-wave current. The oscillopolarogram obtained is similar to that obtained with sine-wave current. The appearance or disappearance of incision on the oscillopolarogram can be used to indicate the end-point of titration. The relationship of incision height hi to the concentration of depolarizer and current sweeping rate Vare respectively as follows.hi(mV) = -0.02300 + 4.702×10-4C0*(-2/3) hi(mV)= -0.02807 +950.68V(2/3) When Vis very lower 5.0×10-9mol/L Tl+ ion can be determined by this method
    Electrochemical Behavior of Multilayer ISE Connected in Series and Effect of Nernst Multiplication
    Yao Shouzhuo, Xiao Jun, Nie Lihua
    1988, 9(6):  568-573. 
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    Multilayer ISEconnected in series was designed and it has been proved both theoretically and experimentally that the response slope, sensitivity and precision in the potentiometric determination can be raised by n-times by using the proposed multilayer ISE (n = 4) connected in series in comparison to the usual ISE, while the response time, electrode selectivity and detection limit remain the same as the usual ISE.
    The Synthesis of Poly(Vinyl-Ethylenediamine-Propaneamideoxime) Macroporous Chelate Resin and Its Application to Enriching and Separating Some Trace Elements
    Chang Xijun, Luo Xinyin, Su Zhixing, Zhao Xibai, Lu Yihong
    1988, 9(6):  574-579. 
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    Poly(vinyl-ethylenediamine-propaneamideqxime) chelate resin was synthesized' by using macroporous polyvinyl chloride as an original material.The ICPclcmical spectrum method was established for enriching and separating' 20 kinds of trace elements with, the chelate resin. Its performance and mechanism for enriching some trace elements are discussed.The structural analysis of chelate resin was performed by SEMand infrared spectrum et al. The trace elements in samples were enriched and determined with satisfactory results.
    Studies on the Adsorption Voltammetry of Germanium(Ⅳ)-Pyrogallol System with Differential Pulse Polarography
    Sun Changqing, Gao Qian, Liu Liling
    1988, 9(6):  580-583. 
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    The characteristics of adsorption voltammetry of the germanium complex with pyrogallol at the mercury electrode were investigated in detail.Generally applicable condition for this method are given. When . the accumulative time is 4 min the limit of determination for germanium is 1.2×10-10mol/L
    Syntheses of Aryl Aryloxyacetates and Phenyl Aryloxythioacetates Using Liquid-Liquid Phase Transfer Catalysis
    Li Yingjun, Dai Yujia, Chen Jichou
    1988, 9(6):  584-589. 
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    Thirty-five aryl aryloxyacetates and five phenyl aryloxythioacetates have been synthesized using liquid-liquid phase transfer [catalysis. All the compounds are new. Compared to the classical methods, phase-transfer catalysis has the advantages of good yields, easy preparations and mild conditions.
    Eister-Containirig Porous Polymeric Beads as GC Stationary Phase
    Zuo Yumin, Wang Busen, Xie Mengxia, Luo Zhiqiang, Wei Junfu
    1988, 9(6):  590-595. 
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    Two series of polymeric beads from methyl methacrylate or methyl-acrylate and divinylbenzehe were synthesized. The physico-chemical and gas chromatographic properties of these ester-containing polymers have been determined and the polarities have been evaluated by means of McReynolds polarity scale. The use of these beads for the separation of various mixtures was; well documented through several examples. It was shown.that they were better than Porapak Tand some other commercial, ayailable polymers with close polarity for the shorter retention time, lower column temperature, and higher selectivity.
    Investigation of Methyl Tri-Hydrogen Group
    Huang Changhua, Wan Yanzhong, Lu Liangde, Liu Jingjiang
    1988, 9(6):  596-600. 
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    In this paper, compounds containing methyl trihydrogen group (acetone, methyl acetate, dimethyl sulfpxide) are investigated by FT-IR. When dilute them with,inert Solvents, the overtones of stretching model of CO and SO groupsshift to high frequency. At the same time, the C—H stretching model shifts to low frequency. It declares that CH3 interacts with O atom, but the interaction is different, from hydrogenbonding.
    The Kinetics Study on Synthesis of Diacetone Alcohol on Basic Ion Exchange Resin Catalyst
    Fang Yanquan, Zhang Shuji, Xing Xiaodong, Shi Huizban, Zhao Weijun
    1988, 9(6):  601-607. 
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    This paper studies on a basic ion exchange resin catalyst that was used in condensation reaction of acetone to prepare diacetone alcohol and find it having good activity and selectivity. The life time of this catalyst is long,and the method of regeneration of deactivated catalyst is easy. The kinetics experiments on preparation of diacetone alcohol from acetone on this resin catalyst show that the condensation reaction is obviously reversible. The forward and reverse reaction are first-order reaction for concentration of acetone and diacetone res-peptively. This reaction is fond to obey the following rate equation.-dCacetone/dt=k+Cacetone-k_Cdiacetone The apparent activation energy of forward and reverse reaction can be obtained from each rate constant k+ arid k_ and according to this activation energy theheat of the condensation reaction can be given also. It is - 24kJ/mol. On the basis of the kinetics experiments we suggest that acetone was adsorpted onto theactive site of the resin catalyst first and secondly the adsorpted molecular of acetone decompose to form acetonyl. Then the acetonyl reacts with another molecule of acetone forming diacetone and regenerating catalyst again.The second step is the rate-control step. We also estimate the heat of the reaction by calculating the bond energies of the compounds which were involved in. the condensation reaction. The values of the heat of reaction between the calculating . result and kinetics experiment are very close.
    The Influence of Short Range Parameters for a-Si on Its Electronic Structures
    Zhang Rujqin, Dai Guocai, Guan Daren, Cai Zhengting
    1988, 9(6):  608-611. 
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    The real space structural models with short range disorder - for- amorphous silicon have been built by means of pseudo-stochastic data produced in computers. The CRN's (continuous random networks)atomic cluster models, which include 29 silicon atoms, have been presented for a-Si materials. The quantum chemicalCNDOcalculation, which is different from the traditional treatment (in K-space), has-been performed for those cluster models. The influence of the shortrange parameters for the a-Si on its electronic density of states (DOS) has been researched. The calculation results show that both bond angle and dihedral angle are the main parameters determining electronic structure for a-Si under the same RDFcondition as experiments. The bond length has only a little influence on it. The localized states near the top of valence band and the bottom of conduc-tion band might arise from the fluctuation of the bond angles and dihedral angles.
    The Complex Kinetics of Isomertization of Butene-1
    Yu Qiquan, Jin Yun, Huang Wei
    1988, 9(6):  612-617. 
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    The existence of phase of BiPO4 was proved by the X-ray powder patterns of MoBiP1.8/SiO2 catalyst. The acidity of the catalyst was titrated by n-butyl-amine with the method of adsorption of colored indicators.The catalyst exhibited moderate acidity. The, presence of Bronsted and Lewis acids of the catalyst was discriminated by the infrared spectroscopic method of pyridine adsorption on the catalyst. The heats of adsorption of butene-1 and butene-2 were determined by the pulse method. The kinetics of isomerization of butene-1 over MoBiP1.8 /SiO2 catalyst has been investigated by the flowrecirculation glass non-gradientness reactor. The kinetic equations obey the L-Hmechanism of triangular reaction of isomerization of butene. When the parameters of simplified kinetic equation of L-Hmechanism were estimated by the linear least square method, the condition number of coefficient matrix of norm equation was more than 108.
    Isomer Seperation of Dibenzo-18-Crown-6 Nitration and Structure Determination of the Cis Product
    Yang Guangdi, Sun Yunxiu, Zhang Huixiang, Zhang Hui
    1988, 9(6):  618-621. 
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    Under the improved condition, the dibenzo-18-crown-6 can be nitrated with production rate over 90 per cent. In addition, we proposed a method by which the cis-dinitro-dibenzo-18-crown-6 can be easely separated from its trans isomer. By combining elemental analysis, infrared and X-ray diffraction results, the molecular and crystal structure of cis-dinitro-dibenzo-18-crown-6 has been determined. The crystals belong to monoclinic space group P21/n, with a= 15.985(7), 6 = 20.411(9), c = 8.173(4)Å, β=101.09(4)°, Z = 4. The structure was solved by direct methods and refined to convergence with final Rvalue of 0.067.
    Preparation and Blood Compatibility of Adsorption Resin Coated by Diacetylchitin
    Yan Jun, Xu Rongnan, Xia Yan, Lu Zhaonian, Cai Zhuhui, Wu Xinhua, Wu Zhaoguang
    1988, 9(6):  622-626. 
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    Diacetylchitin(DAC) was used for coating adsorption resin to produce a blood compatible adsorbent. The methods of coating adsorption resin with DACwere investigated, and the DAC-coated resin obtained was studied for their blood compatibility and adsorption capacities for toxic substances. Based on these studies, the DACis believed to be full of promise as a blood compatible material for coating resin used as a hepatic support.
    Determination of Trace Amount of Fluoride by Gas Chromatography
    Ma Mings heng, Chen Weijie
    1988, 9(6):  627-629. 
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    A new method for the determination of fluoride ions is proposed. Under acidic condition, trimethylfluorosilane was produced from hexamethyl disilazane and hydrofluoride, and then separated by gas chromatography using a 15% OV-3 column at 100℃. The detective limit is 5 ng/g. Aluminum ion or silicate ion have no interference with the determination even its content is as high as 2000:1 or 400:1 respectively to the fluoride ion.
    Studies on C-Glycosides(Ⅵ)——Fast-Atom-Bombardment Mass Spectrometry of 1-D-Glucopyranosyl Benzene and Its Derivatives
    Liang Weisheng, Qiu Dongxu, Cai Mengshen
    1988, 9(6):  630-633. 
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    Fast-Atom-Bombardment Mass Spectra (FAB-MS) of four 1-D-glucopyranosyl benzene and their derivatives were reported. Accurate molecular weights of the compounds and the rules of cleavage of glucopyranose ring, which had been proved by the FAB-CA-MJKES, were obtained. But, FAB-MSof α,β-isomers of C-glucosides had no obvious differences.
    A Study on the Kinetics of Oxygen Reduction on Vibrational Ball Milled Graphite
    Zhou Yunhong, Wu Zhiyuan, Gao Rong
    1988, 9(6):  634-636. 
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    Oxygen reduction on rotating ground ultrafine graphite ring-disk electrode has been investigated in alkaline solution. The results show that ultrafine graphite is a good catalyst for O2 reduction to hydrogen peroxide. The peroxide ion not only isn't reduced further but also isn't decomposed by catalysis on the ground graphite.
    Amphoteric Terramycin Sensitive Electrodes and Selectivities
    Yao Shouzhuo, Shiao Jun, Nie Lihua
    1988, 9(6):  637-639. 
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    Electrodes sensitive to cationic or anionic terramycin were constructed using, terramycinium silicotungstate, TPB, DPAand cetyltribctylammonium terramycina-te as electroactive materials. The terramycinium (terramycinate) sensitive elec-trode responds to terramycinium (terramycinate) down to 10 (40) μnol/Lover pHrange 1.6-3.2 (8.0-11.0) with a slope of ca, 57.2(-58)mV/lgC. The electrode selectivities toward quaternary ammoniums and inorganic cations are described in terms of ionic potential Z/Rand induction index I:lgKij = 9.87I-31.94Z/R + 290.44(R = 0.999) and lgKij =1.422 (Z/R)-1-3.363. (R= 0.942).
    The Relation of the Antifoaming Effects of the Polyoxyalkylene Ether Block Polymers and Their Stearate to the Content Percent of the Hydrophilic Group and Hydrophilic-Lipo-Philic Balance
    Shi Mingli, Wang Diangang, Wang Huayuan, Sun Xunyun
    1988, 9(6):  640-642. 
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    The antifoaming effects of some polyoxyalkylene glycerol ethers (GPE) and their distearate (GPES-2) are studied. The best results are achieved by GPEwith hydrophibic groups of mol. Wt. 3500~4000 and 10% hydrophilic group content and HLB 0.8~1.5.The antifoaming effects of GPES-2 is higher than those of GPE. GPES-2 with 15~20% hydrophilic group content results in the highest antifoaming effects.
    The Investigation on Polyurethane and Epoxyresin Interpenetrating Polymer Networks
    Zhao Yaniun, Li Yuwei, Wang Jingyuan, Tang Xinyi, Yu Min, Yang Yuhua
    1988, 9(6):  643-645. 
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    In this paper, the synthesis of interpenetrating polymer nelworks(IPN) based on polyurethane and epoxide by simultaneous polymerization, the influence of various component on their morphology, gh-ss transition behavior,mechanical properties and thermostability are reported. The results show that PU/EP = 25/75 exhibited the best, mechanical properties and thermostability due to the high degree of interpenetration among the networks. PU/Ep = 50/50 exhibited obvious phase separation and the poorest mechnical properties.
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