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    24 August 1989, Volume 10 Issue 8
    Articles
    Synthesis, Properties and Structure of Mixed Ligand Complex of Iron(Ⅲ) with 2-[(o-Hydroxybenzylidene)amino] Phenol and Pyridine
    Liu Dexin, Cui Xuegui, Geng Fangdong, Li Fengling, Kong Qingchi
    1989, 10(8):  787-791. 
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    The mixed ligand complex of Fe(Ⅱ) with 2[(o-hydroxybenzylidene)amino] phenol and pyridine was prepared.Its structure was determined by means of four cycle diffractometer.It was found that the crystal belongs to the monoclinic system with space group C2/c, and the unit cell parameters are:a= 10.109(4)Å.6=23.403(7)Å.c= 18.417(3)Å, β=102.20(2)°, V = 4258.8 Å3,Z=4, Dc=1.41 g/cm3,μ=7.4 cm-1 (Mo Ka), F(000) = 1872.The process of its thermal decomposition was investigated by means of DTAand TGtechniques.
    Principle of A. C. Oscillo-Bipotentiometric Titrations(Ⅱ) ——Verification of the Theoretical Equation of the Fluorescent Potential Line
    Xu Weijian, Gao Hong
    1989, 10(8):  792-795. 
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    The theoretical equation of the fluorescent potential line was derived in previous paper.The experimental verification of the equation is given in this paper.The results obtained from theoretical calculation consist well with the experimental results.The properties of some parameters, e.g.E10,E20, ω, Cd, i0, in the equation and the sensitivity of this method are discussed.
    Studies on Adsorptive Voltammetry for the Nickel (Ⅱ)-Thiosemicarbazide System
    Hu Naifei, Li Qilong
    1989, 10(8):  796-799. 
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    In a supporting electrolyte containing 0.025 mol/Lpotassium hydrogen phthalate, a sensitive adsorptive peak of Ni(Ⅱ)-TSCsystem at the Hg electrode was found.The mechanism of the peak was studied by chronocoulometry.The study shows that in the presence of TSCthe adsorption of Ni(Ⅱ) at the surface of Hg electrode is direct adsorption of Ni(Ⅱ)-TSCcomplex and the adsorbed species is Ni(Ⅱ)(TSC)22+.The detection limits are 1×10-8 mol/Land 4×10-9mol/Lby linear sweep adsorptive stripping voltammetry and differential pulse adsorptive stripping voltammetry, respectively.
    Studies on the Colour Reactions of Vanadium (V)-Thiocyanate-Basic Triarylmethane Dyes
    Liu Shaopu, Liu Zhongfang
    1989, 10(8):  800-803. 
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    The colour reactions of the vanadium (V) with thiocyanate and basic triarylmethane dyes such as crystal violet, malachite green, brilliant green, methyl violet and victoria blue 4Rin the presence of some surface active agents in aqueous solution were investigated.The reaction conditions and analytical characteristics of the system of vanadium (V)-thiocyanate-Crystal violet-arabic gum were studied in detail.This colour reaction has a very high sensitivity (ε530=2.55 × 105 L·mol-1.cm-1) and a favourable selectivity and so can be applied to spectrophotometric determination of micro amounts of vanadium in aluminium alloy.
    Study on Chemical Constituents of Volatile Oil of Fresh Flowers of Elaeagnus Angustifolia L
    Li Zhaolin, Chen Ning, Xue Dunyuan, Li Haiquan, Chen Yaozu
    1989, 10(8):  804-808. 
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    In this paper, the volatile oil of fresh flowers of Elaeagnus angustifolia Lwas extracted bymeans of the device of simultaneous steam distillation-solvent extraction made in our laboratory.The yield of the oil is 0.1 % of fresh flowers (W/W).By using capillary gas chromatography-mass spec-trometry, 85 constituents were separated, of which 47 compounds constituting 96.51 % of the oil were identified.The major ingredient is trans-ethyl cinnamate, contents of which reach to 78.88 %.The fact that the major constituent was trans-ethyl cinnamate was also supported by the infrared and NMRdata.
    Nickel Carbonyl Complex Containing Bidentate Ligand 2-(Diphenylphosphino)pyridine——Synthesis and Molecular Structure of (Ph2PPy)2Ni(CO)2
    Wang Honggen, Wang Ruji, Zhang Zhengzhi, Wang Xukun, Zhang Weijun, Yang Limei
    1989, 10(8):  809-811. 
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    Using a new and simple method, under ordinary temperature and pressure (Ph2PPy)2NiCl2 was reduced by zinc powder in the presence of carbon monoxide to give (Ph2PPy)2Ni(CO)2, the structure of which was determined by X-ray diffraction.The complex crystallizes in the orthogonal space group Pcabwith a=12.044(3)Å, b=21.322(5) Å, c=24.925(5)Åand Z=8.The deviation factors R=0.051 and Rw = 0.055 were obtained for 2166 independent reflections.The nickel atom is of tetrahedral configuration.
    Bis-Crown Ether Containing Pyrimidine Ring (Ⅱ)
    Lu Guoyuan, Wang Defen, Hu Hongwen
    1989, 10(8):  812-816. 
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    Six bis-crown ethers containing benzo-12-crown-4(A1,B1), benzo-15-crown-5(A2,B2) and benzo-18-crown-6(A3,B3) moieties bridged by pyrimidine ring were prepared by the reaction of 4,6-dichloro-5-nitropyrimidine, 2, 4-dichloro-5-nitro-6-methylpyrimidine with the 4'-aminoben-zocrown ethers, respectively.Extractions were carried out from aqueous solution of alkali metal pi-crates with these bis-crown ether solutions in chloroform.The extraction equilibrium constants were also evaluated.The results indicate that compound (A1,B1), (A2,B2) and (A3,B3) are effective extracting reagents for sodium, potassium and caesium, respectively.The cation-selectivity is more effective than the corresponding monocyclic crown ethers.
    Titano-hydrogenation of Alkyne Hydrocarbons and Stereoscopic Structure of Products
    Liu Yiyin, Wang Jiabing, Liang Ge, Wang Jitao
    1989, 10(8):  817-820. 
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    The Titano-hydrogenation of Alkyne hydrocarbons was studied by the method of G.C.track.At the early stage the cis-alkene hydrocarbons were obtained with a higher selectivity and a good yield, but trans-ethenes were obtained with a higher selectivity and a good yield at the later stage of the reaction.Controlling the time of the reaction and quenching with ketones,a series of new stere-ospecific allyl alcohols were obtained.
    Stereochemistry and Crystal Structures of Palladium (Ⅱ) Complexes with cis- {meso(race)-1, 2-bis[alkyl(aryl)sulfinyl]ethane}
    Shao Pinxi, Zhu Fuchun, Yang Yukun, Chen Ruisheng, Yao Xinkan, Wang Honggen, Wang Ruji
    1989, 10(8):  821-825. 
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    Six complexes of palladium (Ⅱ) with meso- and race-diastereoisomeric RS(O)CH2CH2-S(O)R(abbr.to meso-, race-BXSE.R = n-C3H7, C6H5, n-C8H17, X = Pr, P, O) were prepared.The crystal structures of PdCl2-meso-BPrSE (I) and PdCl2.race-BPrSE(Ⅱ) were determined.Crystal data: I : P212121, a = 9.3650(9), b=9.747(2), c=19.341(5)Å, Z=4, R=0.044; Ⅱ: Ibca, a = 9.442(1), b=15.386(4), c = 20.095(3)Å, Z=8, R=0.030.The IRspectra indicate that the ligands are bonded to Palladium (Ⅱ) via sulfur atoms to form the cis-chelated complexes, which has been confirmed by the crystal Structures.△vso[vso complex -vso ligand] for different Rgroups varies in the order: meso-BPrSE- race-BPrSE>meso-BOSE- race-BOSE> meso-BPSE- race-BOSE.Ihas a C1 symmetry and Ⅱ has C2 symmetry.The four coordinated atoms around palladium (Ⅱ) form a right square plane for Ⅱ and a only slightly tetrahedrally distorted plane for I.It can be concluded that the higher melting point BPrSEis of meso form and the lower melting point BPrSEis of rac form.
    Localization of Virtual Orbitals
    Tian Anmin, Yuan Gaoqing, Tang Zuohua, Yan Guosen
    1989, 10(8):  826-830. 
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    The Magnesco - Perico' s method of virtual MOspace is performed.Aseries of molecules (including small inorganic molecules, Alkanes, Alcohols, Amines and conjugated hydrocarbons etc.) are calculated at the level in STO-3Gof ab initio.The results show that the similar regularity of distributions of coefficient and energy levels is presented for the localized occupied and the virtual or-bitals.The Localized virtual orbitals and the corresponding Fock matrix elements are transferable.Futhermore the discussion of chemical bond breaking in the free-radical reaction by use of the difference between energies of localized occupied and vertual orbitals is presented.
    Effects of Dopants on the Charge Density Wave in Polyacetylene
    Wang Rongshun, Meng Lingpeng, Zhao Chengda, Sun Yan
    1989, 10(8):  831-835. 
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    In this paper, effects of various dopants on charge density wave in polyacetylene were studied by means of CNDO/2 quantum chemical calculation.There are large charge density on the carbon atoms near the dopant, and the effects of p-type dopants are greater than those of n-type ones.The relationship between charge density wave and conductivity is discussed at last.
    On Extended Definition of Standardized Definite Integral in Neighborhood Theory
    Sun Honglin, Guo Dongyao
    1989, 10(8):  836-840. 
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    In this paper, the necessary discussion and extension are made on the standardized definite integral definition of joint probability of neighborhood theory in direct methods of X-ray crystallography.The extended definition leads to more extensive application for the definite integral theorem.All of the formulas in Hauptman' s papers published in the past are derived again from the new method, and then it is verified that the extended theorem is correct, concise and universally applicable.
    Study on Determination Method and Apparatus for Salt-Containing Vapor Liquid Equilibria
    Zhou Xingfeng, Pan Huanquan, Lan Guiquan, Han Shijun
    1989, 10(8):  841-844. 
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    A New method, based on dynamic method of double phase circulation for measurement of vapor liquid equilibrium data of salt-containing system, is present,and a new apparatus developed.To solve the problems existing in the common determination method for salt-containing vapor liquid equilibrium, our work is based on the principle of double phase circulation method and the determination procedure is divided into two steps.In the first step, the quasi-static method is used to measure the bubble point line data (t,x) which does not require composition analysis,and in the second step, by using the same apparatus CS- Ⅱ multipurpose VLEdetermination apparatus, the dew point line data (t, y) of the same constant salt concentration in equilibrium liquid phase is determined.The new VLBdetermination apparatus with a pump-like stirrer can make the circulation so steady that it can avoid effectively the fluctuation and the rush of the liquid flow which often happens when double phase circulation apparatus are used for salt-containing systems.The error equation of quasi-static method for the bouble point measurement of salt-containing system is deduced from the relationship of material balance concerned,the verification work was done experimentally, including the examination of the applicability of the new apparatus in saturated salt-containing system and the determination of VLEdata of CaCl2-acetone(1)-methanol(2) system at normal pressure and 5% CaCl2 concentration in equilibrium liquid phase.The experimental data agree finely with literature data.
    Effect of Sucrose and Glucose on the Activity of Acetone, Ethanol and Acetonitrile in Water at 2981K
    Lu Dianzhen, Ni Chaoshuo, Li Zhifen, Liu Ruilin
    1989, 10(8):  845-847. 
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    The activity coefficients of acetone, ethanol, and acetonitrile in aqueous solutions of sucrose or glucose were measured by headspace gas chromatograpy at 298.1K.The variations of activity coefficients of three nonaqueous solutes (lnr)with concentration of sugar are explained preliminary in term of the hydration of equatorial OHof sugar molecules, the mixing order of solvents, and the interaction of molecule between solute and sugar.
    Flocculation and Stabilization of PAM to Clay Suspension
    Hou Wanguo, Zhang Chunguang, Wang Guoting
    1989, 10(8):  848-851. 
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    The flocculation kinetics of PAMto kaolinite was investigated.Flocculating ability is maximal when the hydrolysis degree (a) is between 34% and 41%.PAMhas a stabilization for Na-mont-morillonite suspension and the stability is maximal when a is between 20% and 30%.Maximum of Bingham' s yield strength τ0 appears within 30%~40% and maximum of gel strength τ0 appears within 15%~20%.These results were discussed in terms of configuration of polymer and surface properties of clay.It was indicated that PAMwhose a is about 30% may flocculate selectively kaolinite of the mixed suspension of Na-montmorillonite-kaolinite.
    Synthesis and Characterization of Polyvinylene Carbonate and Polyhydroxymethylene
    Huang Jiaxian, Adriaan Bantjes, Leen van der Does
    1989, 10(8):  852-856. 
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    Polymerization of vinylene carbonate gave colourless polymers with high molecular weights.Films and powders of polyhydroxymethylene were obtained by hydrolysis of polyvinylene carbonate.Mechanism of degradation of polyvinylene carbonate in acetone and DMFwas studied.
    Studies on Solvation Effect on Colour Reactionof Multicomponent Complexes (Ⅱ) ——The Effects of Organic Solvents on Distribution Constants of Chrome Azurol S Between Micellar Phase and Water
    Zhu Youyu, Yie Xiaolan
    1989, 10(8):  857-859. 
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    The distribution constants (KD) of CAS (HR3-) between micellar (CTMAB) and aqueous phase in the presence of organic solvents (DMSO, MeOH, EtOH, Me2CO, i-PrOH, Dioxane) were determined by spectrophotometric method.The KDof the systems in the presence of organic solvent is higher than that of the systems without the presence of organic solvents.This indicates that the organic solvents increase the effective concentration of CAS (HR3-) on the surface of the micelle, which is beneficial to colour reaction.The relationship between the distribution constant and sensitivity of colour reaction is studied in detail.
    Oscillographic Conductometric Titration
    Bi Shuping, Gao Hong
    1989, 10(8):  860-862. 
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    Acathode-ray oscillograph is directly connected to the electrodes of a conductometric titra-tion cell and the sudden change of the oscillogram is used to indicate the end-point of conductometric titration.The new technique has advantages over the usual conductometric titration methed: (1) The end-point can directly be perceived through the senses, and the graphic method for end-point location is no longer used.(2) The equipment and manipulation are more simple.
    Adsorption Behaviour and Mechanism of 4-Aminopyridine Resin for Gallium
    Wang Naidong, Xu Sujun, Chen Yiyong
    1989, 10(8):  863-865. 
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    4-Aminopyridine resin (4-APR) has a good adsorption ability for the anionic complex of gallium with chloride in 6 mol/L HCl.The anionic gallium complex adsorbed on 4-APRcan be eluted by water quantitatively.The static adsorption capacity is 351.2 mg Ga(Ⅲ)/g 4-APR.The basic adsorption parameters of 4-APRfor gallium (Ⅲ) are calculated from the data of chemical analysis and IR-spectra.The adsorption mechanism is discussed.
    Studies on the Flavonoids of Elsholtzia Ciliata Hyland
    Zheng Shangzhen, LU Runhai, Shen Xuwei
    1989, 10(8):  866-868. 
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    The isolation and identification of five flavonoids of Elsholtzia ciliata Hyland, a Chinese herb medicine, are reported.The structure of compound V, a new compound, is elucidated by means of spectral as well as chemical methods as 5-hydroxy-6-methylflavanone-7-O-α-D-galactopyanoside.
    Study on Indirubin and Indigo by ESR Spectrometry
    Chen Kunyuan, Wang Zhefu, Li Chuanyong, Li Weixiang
    1989, 10(8):  869-871. 
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    The parameters of the ESRspectra indirubin and indigo were measured in this paper.For indirubin g = 2.0038, △Hpp=406Am-1.For indigo g = 2.0032, △Hpp=528Am-1.The indirubin ESRspectrum intensity is 36 times weaker than that of indigo in the same weight of the samples.As the temperature increases from room temperature to 60℃, the spectral intensity of indirubin is increased, the indigo spectral intensity is decreased and follows the Boltzman' s law of temperature effect.
    Relationship Between Solvating Power and Dielectric Constants for the Dehydration of Tertiary Alcohol to Alkenes
    Zhang Jingwen, Xu Zhiluo, Zhou Xiumei, Liu Ying, Li Yuexian, Liu Fuan, Zhu Shaoxian
    1989, 10(8):  872-874. 
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    Solvent effects on the dehydration of 2-methyl-2-hexanol to corresponding alkenes, catal-lyzed by Fe2(SO4)3.xH2O, were determined in different solvents.The relationship between solvating power and dielectric constants was derived from these experimental data.
    Studies on Shrinkage-Compensating Effect of Unsaturated Polyester (Ⅱ) ——Shrinkage-Compensating Effect of Several Saturated Polyesters
    Gao Shanjuan, Wu Xuemei
    1989, 10(8):  875-877. 
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    Seven low molecular weight saturated polyesters were synthesized and their shrinkage-compensation effects were estimated.It has been found that aromatic saturated polyesters as low-shrinkage agents are more effective than aliphatic ones.Some sheet-molding compounds and hulkmolding compounds were prepared, and the volume and linear shrinkage of these products as well as mechanicaland thermal properties were determined.The properties of these modified low-shrinkage unsaturated polyesters are found excellent.
    Studies on Addition Reaction of Melamine and Formaldehyde
    Liu Fengqi, Tang Xinyi
    1989, 10(8):  878-880. 
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    The addition reaction between melamine and formaldehyde involves the conversion of melamine into nine different methylol melamines.The reaction mechanism of the complex system can be summarized in a simple reaction model as below:(这里有图片19890824-878-1.gif)The rate equations of above reactions are evaluated by using Runge-Kutta method, and the rate constants are determined by means of fitting them to reaction species concentrations at various times.The molecular distribution formula of methylol derivatives of polyamine, which we developed previously, is used to form simultaneous equations with reaction rate equations and the contents of various meth-ylol-melamine are calculated.The results are good in agreement with the experiment data.