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Table of Content

    24 January 1988, Volume 9 Issue 1
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    Articles
    The Structure of ZSM-39 Single Crystal Grown in CH3NH2- SiO2-H2O Gel Solution
    Zheng Peiju, Wang Boyi, Wu Guang, Long Yingcai
    1988, 9(1):  1-3. 
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    ZSM-39 single crystals were hydrothermally grown from CH3NH2-SiO2-H2Ogel system. Its structure was determined on an Enraf-Nonius CAD4 diffractometer.The space group is Fd3m, with α= 19.403(3)Å. Final Rfactor is 0.055. The. methylamine molecules are located in the 16-hedra(hexakaidecahedra) in disorder.The carbon atom is sited on center of 16-hedron. The system is stabilized.
    Study on Vapor-Solid Replacement and Properties of Hetero-atom Aluminoslicate Molecular Sieve
    Pang Wenqin, Zuo Lihua, Qiu Shilun
    1988, 9(1):  4-8. 
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    Si-Al-Y, Ti-Si-Al-Y, Ti-ZSM-5, Ti-Silicalite-Ihetero-atom aluminosilicate molecular sieve have been synthesized by vapour-solid phase reaction. Their crystal morphology, ability of adsorption, thermal stability and the structure have been also researched by means of IR,ESR,XPS,XEPand XRD.The results showed that the introduction of 4-coordinated titanium has occurred.
    Preface
    Determination of Thermodynamic Parameters of Adduct Reaction of Nic(O8H17O)2PS2]2 and (C2H5)3N by GLC Method
    Yu Yunpeng, Xu Zheng, You Xiaozeng
    1988, 9(1):  9-12. 
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    It is reported that the equilibrium constants of acid-base interaction between Ni(C8H17O)2PS2]2, and (C2H5)3Nforming 1:1 adduct were determined by GLCmethod at variable temperature. Thermodynamic parameters △Hand △Swere found. The experimental data fit the equation:lgK=-5.196(±0.328)+[1.6503(0.1144)/T]×103。
    Articles
    A Study on the Ternary Systems MCl-M'Cl-HOAc (25℃)(M,M/=K,Rb,Cs;M ≠M')
    Ran Xinquan, Li Chuanbin, Chen Yunsheng
    1988, 9(1):  13-16. 
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    The systems KCl-RbCl-HOAc, KCl-CsCl-HOAc and RbCl-CsCl-HOAc have been studied isothermally at 25±0.05℃. Solubilities of the systems were measured and the corresponding equilibrium diagrams and the distribution curves were constructed.In the first system, there is only one solid phase, the system belongs to Rpozeboom type Ⅰ. The later ones belong to Roozeboom type Ⅳ, but the mutual solubility in solid state is obviously larger than that in water systems.
    An Investigation on the Complex of Vanadium(Ⅴ) with Benzilic Acid and Pyridine (Ⅱ)——The Preparation of Single Crystal and Determination of Crystal Strucutre.
    Fan.Yuguo, Du Yaoguo, Ding Yoagsheng, Wang Xiaoxia, Xiu Zhengkun
    1988, 9(1):  17-22. 
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    The vanadium(Ⅴ) complex, PyH[VO(Bz)2Py]Py, has been prepared from NaVO3, H2Bz and Py. The single crystal belongs to triclinic in space group, P1, with unit cell constants, α=12.400(5)Å, b= 14.042(5)Å, c= 10.441(4)Å, α=91.92(3)°,β= 93.57(3)°, γ=74.41(3)°, V=1874.7(1,2)Å3, Z = 2.Least-spuare refinement has led to a final Rvalue of 0.0450.The coordination number of vanadium is equal to 6, and it is constructed as a distored octahedral form by one Natom and five Oatoms. That complex is a cis-isomer.
    The Rf Graph of Metallic Ions and Extraction of Palladium by Ethyl n-Laurylthioacetate
    Lu Zhong'e, Liu Guoxing
    1988, 9(1):  23-26. 
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    By means of reversed-phase paper chromatography with ethyl n-iaurylthioace-tate (ELTA) as stational phase, the Rf graph of more than 40 metallic ions was obtained. From the Rf graph it can be found that ELTA is an excellent extrac-tant for Palladium. The extraction of Palladium with ELTA was then studied by the method liquid-liquid extraction. The effects of different diluents and concentrations of hydrochloric acid are discussed. The composition of the extracted complex is PdCl2(ELTA)2.The mechanism of the extraction of Palladium by ELTA was also studied.
    Studies on Gas Ghromatography/Surfatron Microwave Plasma Emission Spectrometry
    Yang Guangde, Yu Aimin, Xu Hanying, Li Guoyou, Lu Jun, Jin Qinhan(Q. Jin)
    1988, 9(1):  27-30. 
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    Asimple instrumentation of gas chromatography-microwave plasma emission spectrometry was set up. The plasma was sustained in a lab-made surfatron with argon operated at atmospheric pressure. The effect of plasma operating parameters on the performance of the set-up was studied. It was shown that the set-up could be successfully used to determine the C/Pratio of various species.
    Tartaric Acid Modified Electrode and Studies on Its Application for the Anodic Stripping Voltammetric Determination of Cu(Ⅱ)
    Fang Yuzhi, Li Yuansheng, Jin Litong
    1988, 9(1):  31-35. 
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    We studied the preparation and performance of the tartaric acid modified electrodes, and found the conditions for determining trace copper (Ⅱ). These electrodes have good reproducibilily and the sensitivity is increased by one order of magnitude. There is a good linear relationship between peak height and concentration in the range of 1 to 20 ng/mLof Cu(Ⅱ). At the concentration of 10ng/mL of Cu(Ⅱ), the variation coefficient of six parallel determinations was 1.6%. Moreover, the reaction mechanism of Cu(Ⅱ) at the tartaric acid modified electrodes is discussed. The modified electrodes can increase the number of activated sites, and promote the exchange of electrons, so that both the enrichment efficiency and sensitivity are raised. The stripping process of copper at the modified electrodes is the same as that at glassy carbon electrodes.
    Fragmentation Reaction of Aryl Tertiary Phosphines Under Ultrasonic Irradiation
    Xu Linxiao, Tao Fenggang, Yu Tongyin
    1988, 9(1):  36-40. 
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    The fragmentation reaction of aryl tertiary phosphines in the presence of lithium can be promoted effectively by use of ultrasonic irradiation. The reactions under various conditions are compared and a discussion on the action of ultrasoundis also given hereof. Some organophosphine ligands have been prepared by use of this method.
    Research on 1,2-Bis(2'-(5'-Phenyloxadiazol-1',3',4'-yl)) Ethylene and Its Derivatives with Substi-tuents on 5'-Phenyl Groups
    Pan Jiaxing, Wang Changsheng, Gao Zhenheng
    1988, 9(1):  41-46. 
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    By dehydration of fumaric dihydrazide and benzoic acid as well as substituted benzoic acids respectively, in polyphosphoric acid, trans-l,2-bis ( 2′-(5′-phenyl-oxadiazol-1′,3′,4′-yl))ethylene and twenty of its derivatives with substituents on 5′-phenyl groups were synthesized, of which, the melting points, infrared spectra, ultraviolet spectra, fluorescence emission spectra, laser conversion efficiencies were determined. Their fluorescence quantum yields were obtained by the relative method as well.
    Studies on Glycosides (Ⅰ)——Synthesis of Gastrodin and its Derivatives
    Peng Shiqi, Li Lipu, Wu Jianwei, Zheng Xiaomin, Cheng Tieming, Cai Mengshen
    1988, 9(1):  47-51. 
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    In this paper 1′-O-(potionally substituted formyl phonyl)-2′, 3′, 4′, 6′-tetra-O-acetyl-β-D-glucopyranoside(Ⅱ) were prepared by reacting 1-Br-2′,3′,4′, 6′-tetra-O-α-D-glucopyranose and optionally substituted hydroxybenzaldehyde.After successively treating compound Ⅱ with sodium borohydride and acetic anhydride, the products of thoroughly acetylatd(Ⅲ) were obtained.Alternatively, compound Ⅱ was treated with sodium borohydride, sodium hydroxide and ion exchange resin and the products of deprotected (Ⅳ) were obtained. Their 13CNMR and assigned 1H NMRwere also studied and the anomeric configurations of them were as β configuration indicated by NMR data.
    Ladder-Like Polymers of Polycyclic Conjugated Hydrocarbon and its Stability
    Li Qianshu, Shen Liangjun, Zhang Xingchen
    1988, 9(1):  52-56. 
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    In this paper,according to the results of CNDO/2 quantum chemistry calculation, we have discussed the possibility on a set of novel conjugated shown that, hydrocarbons, ladder-like polymers of polycyclic conjugated hydrocabons. It is when n is a even number the molecules of chain ladder-like polymers of polycyclic conjugated hydrocabons with three menbered ring-five menbered ring or four menbered ring-four menbered ring as repeated unit, H2-(-C3C5H2) or H2-(-C4HC4H-)-nH2, might be stable, which enables us to believe that the aformentioned molecules are possible potential synthesized objects.
    Effects of Polymerization Degree of Polyglycols on Their Adsorption and Inhibition of Cu2+ Discharge
    Cai Jiale, Zhang Aiqiang, Zhou Shaomin
    1988, 9(1):  57-61. 
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    Effects of polymerization degree of polyglycols on their adsorption on Hg and inhibition of Cu2+ discharge were studied. It follows that increasing polymerization degree with widen the potential region of adsorption and enhance the inhibiting effect upon Cu2+ discharge, but a little further effect is made when the polymerization degree is more than 100; as a result, the polyglycol with polymerization degree about 120 is suggested to be used as the additive in acidic copper-plating. In this paper the models for the adsorption of polyglycol molecules and the mechanism of inhibition of Cu2+ discharge are discussed,by which the regularity on the effects of the polymerization degree can be satisfactorily explained.
    Electrocatalysis of Electrodes Coated with Conducting Polypyrrole Films——Electrocatalytic Oxidation of Ascorbic Acid
    Zhong Chuanjian, Wang Zhongquan, Tian Zhaowu
    1988, 9(1):  62-66. 
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    Electrocatalytic oxidation of ascorbic acid(AH2) in acidic solutions was studied at electrodes coated with conducting polypyrrole(PP) films. Shifts of 200-300mVfor the oxidation potential of AH2 at the polymer-coated electrodes were observed by cyclic voltammetry. Through measurements of Tafel plots, the mechanism of electrocatalytic oxidation of AH2 was discussed. With the help of XPSand in-situ ESRspectrum, interactions between electrochemically oxidized PPand AH2 surface species were also discussed.Acoupling of electron-transfer-mediated catalysis and chemical catalysis on PPwas believed.
    Synthesis of Cis-Polyacetylene with New Catalysts Consisting of Ferric Phosphates and Naphthenate
    Wang-Zheng, Wu Jian. Qiao-Yinan, Wang Youwen, Shen Zhiquan
    1988, 9(1):  67-72. 
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    The high cis-polyacetylene filmis with metallic appearance were synthesized by new coordination catalysts composed of Fe(naph), or Fe(P204)3 or Fe(P507)3 and aluminum trialkyl at room temperature.The resultant polyacetylene was charac-terized by IR, ESR, X-ray diffraction, SEM, TEM, electrical resistivity measurement and elemental analysis. The higher activity of polymerization and direct forming films of polyacetylene having rich cis-content were obtained with these catalysts.The single crystal and spot diagram from electron diffraction of polyaCetyl-ene prepared with the Fe(P507)3 system were found. Electrochemistry and batteryof polyacetylene were studied too.
    The Absorbance Effect in Photopolymerization——0-Acyl-α-Oximinoketone Initiator System
    Li Tong, Sun Meng, Tong Weida, Yu Tongyin
    1988, 9(1):  73-77. 
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    The photopolymerization of acrylonitrile and methyl methacrylate initiated by O-acyl-α-oximinoketones was studied under the irradiation at 313 and 365nm. The kinetic behavior was quite different in high absorbance and low absorbance systems. In higher absorbance the rate of polymerization and the molecular weights of the polymers were all independent of the initiator concentrations. The greater the extinction coefficient of the initiator,the lower the concentration with initiator exponent being zero power.
    Conductivity Measurements in a Conjugated-Polymer Single Crystal at Lower Temperatures
    He Pingsheng, Peng Jianbang, Lu Zhihui, Chen Baozhu, Li Yuejin
    1988, 9(1):  78-81. 
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    The conductivity in bis-(p-toluene sulfonate) of 2,4-hexadiyne-l,6-diol(TS) and its polymer PTSsingle crystal was measured by means of a special device at a range of temperature from 77Kto 373K (353Kfor TS). Anomalies of conductivity of TSand PTSalong c-axes which are the directions of polymer chains of PTSat the temperature corresponding to their low temperature phase transition were observed.The temperatures of phase transition in TSobtained from anomalies of conductivity are 163Kand 208K.
    Catalytic Spectrophotometric Determination of Trace Manganese in Food
    Yang Zhibin, Huang Lan, Gao Yemu
    1988, 9(1):  82-84. 
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    In this paper a new catalytic-spectrophotomelric method is proposed for the determination of trace amounts of manganese(Ⅱ) in food. The method is based on the manganese-catalysed oxidation of xylene cyanole FFby potassium periodate with the use of 1,10-phenanthroline as an activator. If the sample solution is warmed in a thermostat at 60℃ and pHranging from 3.8 to 4.2, the method is of the best determinable sansilivity. The working curve is linear in the range 1.85~11ng·ml-1 of manganese.
    Indirect Spectrophotometric Determination of Trace Sulfide With Mercury(Ⅱ)-Tetrakis(4-Trime-thylammoniumphenyl)Porphyrin
    Pan Zuting, Xu Mianyi, Chen Wanhua
    1988, 9(1):  85-87. 
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    The choice of suitable conditions is first reported for the indirect spectropho-tometric determination of trace sulfide with the colour reaction of mercury ( Ⅱ)-Tetrakis(4-trimethylammoniumphenyl) porphyrin (TAPP). Common anions such as Cl-,Br-,I-,SO42-,NO3- and SCN- do not interfere in it, and CN- can be masked by formaldehyde. This method was used for the analysis of some industrial waste water and coal-gas with satisfactory results.
    Carbon-13 NMR Study on Qomplex of Some Transition Metal Ions with Sudan I (1-Phenylazo-2-Naphthol)
    Chen Liang, Hu Yuxian, Lu Yun, Wang Baojun
    1988, 9(1):  88-90. 
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    The carbon-13 NMRspectra, UV-VISspectra and IRspectra of the coordina-tion system of transition metal ions Hg2+, Zn2+, Cr3+, Mn2+ and Ni2+ etc.With sudan 1 were determined.The results show that 13C chemical shifts of various carbon atoms in sudan 1 regularly change with the transition metal ions gradually added. IRspectra and UV-VISspectra have confirmed this regularity, too.
    Catalytic Hydrogenation of CO2 over Pd/SiO2 and La-Pd/SiO2 Catalysts
    Jiang Xuanzhen, Bao Jianbin, Zhou Tao, Chen Yang
    1988, 9(1):  91-93. 
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    The catalytic hydrogenalion of CO2 over lanthana promoted and unpromoted Pd/SiO2 was studied. The marked differences can be observed in catalytic activities of formation of methane and methanol.The turnover frequency of production of methane arid methanol are higher on lanthana promoted catalyst than that on unpro-moted one. These differences may be attributed to lanthana promotion effect by which the palladium particles may redispersed on the surface, meanwhile the function of the promoter probably create a number of basic active sites to modify the catalytic behavior of supported palladium catalysts on CO2 hydrogenationreactions.
    Determinations of Dehydration Processes and Their Enthalpy Changes for LaAc3·1.5H2O and LaAc3·5H2O
    Wu Shurong, Xiong Weimiao, Tang Hongcai
    1988, 9(1):  94-96. 
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    LaAc3·1.5H2O(Ⅰ)and LaAc3·5H2O (Ⅱ) have been prepared ,by new synthesis methods and characterized by elemental analysis, thermogravimetry and vacuum dehydration over P2O5. Their dehydration processes and enthalpy changes have been also determined by means of DTA-TG-DTG and DSC techniques respectively.
    Synthesis of 9-Imine-Dibenzocycloiodonium Salts
    Tu Yongqiang, Hou Zijie, Li Yulin, Huang Wenkui
    1988, 9(1):  97-99. 
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    2-Iodo-4,4′-dinitrodiphenyl amine 3 and 2,2′-diiodo-4,4′- dinitrodiphenyl amine 6 were prepared by direct iodination with SbCl5/I2, from 4,4′-dinitrodiphenyl amine. Cyclization of 3 and 6 with K2S2O8/H2SO4 results in 4 and 7, respectively. 4 was reduced and acetylated to give 5. Reduction of 7 obtained 8. 8 was convened into 9,10,11, respectively, by diazotization and halogenation. compounds 4,5 and 7-11 are new 9-imine-dibenzocycloiodonium salts. Their structures were confirmed by IR, NMRand MS.
    Studies on Flavonoids (Ⅳ)——Synthesis of 2′-Hydroxy-4′-Substituted-Chalcones and 4′-Hydroxy-7-Substituted-Flavonols
    Sun Hngqin, Liu Luwei, Cai Mengshen
    1988, 9(1):  100-103. 
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    Eight new 2′-hydroxy-4′-substituted-chalcones and five new 4′-hydroxy-7-substituted-flavonols were synthesized. Their structures were proved by UV,1HNMR, MSand elemental analysis.
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