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    24 November 1989, Volume 10 Issue 11
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    Articles
    Synthesis, Molecular Structure and ESR Spectra of r,r'-Bipyridyl Bridged Cu-Rh Complex
    Chen Dong, Tang Wenxia, Dai Anbang, Wang Ming, Wang Boyi, Zheng Peiju
    1989, 10(11):  1071-1076. 
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    The systhesis, characterization and molecular structure of [(dien)Cu(H2O) (β-r,r'-bpy) Rh(NH3)5](ClO4)5.H2Owere studied.The title compound crystallized in space group Pbca, with unit cell constants, a = 14.425(1) Å,b=29.589(2) Å,c=16.893(6) Å,a=β=r=90°,Z=8.R= 0.065.In the molecule Cu2+and Rh3+are separately in square-pyramidal and octahedral configurations, bridged by r,r'-bipyridyl.The angle of two planes of pyridines in r,r'-bipyridyl of title compound is about 51°, more than that of r,r'-bipyridyls in other compounds.From obtained ESRspectra the bond parameters of Cu2+ in the title compound were calculated and bonding characters of the compound were discussed.
    Studies on Preparation and Carrying Oxygen of A New Tailed Porphyrincobalt(Ⅱ)
    Cao Xizhang, Wang Qingmin, Shi Tongsun
    1989, 10(11):  1077-1080. 
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    Anew tailed porphyrincobalt complex, meso-mono-[o-(4-diethylamino) butyramidophenyl] triphenal porphyrin cobalt (Ⅱ), meso-MDBPTPP Co(Ⅱ), was prepared and the formation of it was monitored by electronic spectrum.IRspectrum exhibits vCo-Nband at 310cm-1, and 1001 cm-1 peak attributable to the porphyrin ring' s vibration.EPRspectrum and Ⅱeff demonstrate that the central ion is cobaltous.Mass spectrum demonstrates that the molecular weight of meso-MDBPTPP Co(Ⅱ) is 828.The results of axial reactions demonstrate that meso-MDBPTPP Co(Ⅱ) complex has as ability reyer sibly to carry O2 at low temperature.
    Calibration Model Testing and Background Correction in Multivariate SoectroDhotometrv
    Liang Yizeng, Xie Yulong, Yu Ruqin
    1989, 10(11):  1081-1085. 
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    The calibration model of a multivariate spectrophotometric system is said to be incorrect, if some interferent impurity component is present in the system and not included in the calibration model.Amethod based on the matrix projection procedure is developed in this paper for testing the calibration model for such system.If the test shows that the analytical system contains an interfering component, the projection vectors of possibly existing in the system are compared with that of the sample mixture to find out the existing interfering species.The experimental data of three analytical samples were analyzed by the proposed method, and satisfactory results were obtained.
    On the Equilibrium Among the Determined Atoms Inside Graphite Tube During Atomization
    Zhou Nangen, Yan Qingyuan
    1989, 10(11):  1086-1089. 
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    The equilibrium among those determined atoms is studied.The coefficient β between numbers of ground-state atoms and the absorbance was derived theoretically, and the characteristic amount for the number of elements was calculated.Comparing with the value presented by Varian Company, it was shown that the atomization efficiency for GTA-95 atomizer was over 80% calculated with peak height for the more volatile elements such as Zn and Cd.20%～50% for those medium volatile elements such as Cu, Ni, Mg, Ag, Cr etc.and 10% below for less volatile elements Al, Ti and Vetc.
    Studies on the Chemical Constituents of Saussurea Hieracioides Hook.F
    Lin Zimin, Jia Zhongjian, Chu Tse-tsin
    1989, 10(11):  1090-1094. 
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    From the aerial parts of Saussurea Hieracioides Hook.F (Compositate), a new sesquilignan, saussol(E5), and eight previously reported compounds, scopoletin(E1), umbelliferone(E2), chrysoeri-ol(E3), luteolin(E4), arctiin(B1), skimmin(B2), luteolin-7-O-β-D-glucoside(B4) and syringin(B5) were isolated.Their structures were elucidated on the basis of the spectral data, MS (EI, CIand FD), 1H NMR, 13C NMR, DEPT, IR, UV, and comparison with the authentic samples.Skimmin and sy-ringin are reported for the first time from Saussurea genus.
    Studies on the [4+2] Cycloaddition Reaction of α,β-Unsaturated Thiocarbonyl System
    Zhang Mingzhe, Zhang Yongliang
    1989, 10(11):  1095-1099. 
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    In order to study the behavior of α,β-unsaturated thiocarbonyl system in [4 + 2] cycloaddi-tion reaction, some 5-arylidenethiazolidine-2,4-dithiones were reacted with several dienophiles such as N-phenylmaleimide, ethyl acrylate, acrylonitrile and maleic anhydride.Twelve 5,6-disubstituted-4-aryl-5,6-dihydrothiapyrano[2, 3-d]-thiazoline-2-thiones were given.Ahigher regioselectivity is shown in this kind of reaction.The reaction conditions and the reactivities of the reactants are discussed.
    The Studies on the Conversion of μ-Oxo-bis(meso-tetraphenylporphinato) iron(Ⅲ) to Chloro(meso-tetraphenylporphinato) iron (Ⅲ) in CH2Cl2 with Oxidant
    Zhu Shenjie, Gui Mingde, Guo Cancheng
    1989, 10(11):  1100-1104. 
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    The kinetic study on the conversion of (TPPFe)2Oto TPPFeCl is reported in this paper.In the presence of oxidant PhIOor H2O2 this conversion is first order for (TPPFe)2O, but in the presence of air this conversion is zero order for (TPPFe)2O.The temperature dependence of the rate constant is consistant with Arrhenius equation.Based on these results the probable mechanisms for this conversionare suggested.
    Vibrational Spectra of Triphenylphosphine Oxide and Some Complexes
    Liang Yingqiu, Xu Weiqing, Huang Chunhui
    1989, 10(11):  1105-1109. 
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    FT-IRand Raman spectra(4000～100 cm-1) of PhsPO, Nd(NCS)3.4Ph3PO, [Nd(ClO4)2·4Ph3PO]+ClO4-·2CH3COCH3 and Nd (NO3)3·2Ph3PO·C2H5OHare measured.The properties of bands and the structure of complexes are analyzed and discussed.
    Electrochemiluminescence of ABEI in Aqueous Alkaline Solution
    An Jingru, Chen Xi
    1989, 10(11):  1110-1113. 
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    6-[N-(4-aminobutyl-N-ethyl)-N-ethyl]-amino-2,3-dihydrophthalazine 1,4-dione (ABEI) is a kind of common labelled compounds in luminescence immunodiagnosis.We have made a study of the various conditions of electrochemiluminescence of ABEIand found that the optimal rectangular electric pulse parameters are: pulse space 0.45, pulse length 20 ms, pulse amptitude +1.6 V(vs.SCE), and that the medium condition is: 0.12 mol/L KOH-0.080 mol/L H3BO3-0.080 mol/LKCl (pH 12.0).Under these conditions, the range of the linear relationship between light intensity and concentration of ABEIis 1.0×10-8 mol/Lto 9.0×10-5 mol/L.Our study also shows that Cl- in the solution was oxidized to ClO-, and ClO- acts on ABEIand then gives out luminescence.
    The Potential Energy Surface and Mechanism of Intramolecular Excited-State Proton Transfer of 3-Hydroxychromone
    Feng Jikang
    1989, 10(11):  1114-1118. 
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    With the use of MNDOand.INDO-SCF-CImethods, the potential energy surface and the mechanism of intramolecular excited-state proton transfer of 3-hydroxychromone were studied.The corresponding energy barriers and the fluorescence shift were obtained.
    The Surface Properties of the Silanized Active Carbon
    Zhao Zhenguo, Shen Zhong, Chen Lite, Shao Changsheng
    1989, 10(11):  1119-1123. 
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    The specific surface area, specific pore volume and the average pore radius of the silanized active carbon were determined.The wetting and adsorption properties of the same active carbon were studied.The results indicate.(1) with the lapse of the time of the reaction between the active carbon and ClSi(CH3)3 vapor, the specific surface area and specific pore volume decrease greatly, but the average pore radius and pore size distribution are nearly unchanged; (2) the hydrophobicity of the silanized active carbon is stronger than that of the original carbon; (3) the adsorption of butanol from water onto the active carbon increases with the silanization.The above-mentioned results can be explained by the surface reaction between the surface oxygenated groups of the active carbon and the ClSi(CH3)3 vapor.
    On the Polycondensation Reaction of Aa-Bb,Cc,Dd Type
    Sun Jiazhong, Li Zesheng, Tang Xinyi, Tang Aoqing
    1989, 10(11):  1124-1128. 
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    The curing theory for poly condensation reaction of Aa-Bb,Cc,Dd type is investigated in detail to give sol fraction for post-gel and gelation condition explicitly.Furthermore, a recursion formula for evaluating the polymer moments is obtained.This formula is suitable for both pre-gel and post-gel.
    Studies on Chemical Constituent of Euphorbia soongarica Boiss(I)——The Structure of a New Triterpene
    Ding Yili, Jia Zhongjian, Zhu Ziqing
    1989, 10(11):  1129-1130. 
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    Anew triterpene C32H54O, m.p.86-87℃, was isolated from the petroleum ether extract of the roots of E.Soongarica Boiss by using silica gel column chromatography.Its structure was determined as 26,26-dimethyl-25-ene cycloartanol by means of IR, MS, 13C NMRspectrometry and the DEPTtechnique.
    The Esterification Catalyzed by Niobic Acid in Gas-phase
    Sun Zhongqi, Wagn Xu, Cui Shengfan, Wen Lingsheng, Zou Lehui, Guo Canxiong, Qian Zaihu
    1989, 10(11):  1131-1132. 
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    Gas-phase esterifications of six kinds of carboxylic acid with ethyl alcohol catalyzed by nio-bic acid at normal pressure were studied.The results show that the conversion of ethanol is very high in each esterification here, it is up to 92% for esterification of acetic acid with ethanol, and that, especially, the selectivities for all the esterification are up to 100%.
    Studies on Schiff Base Complexes (V)——Reaction of Fe(Salen)NO3 with Nitrite
    Lu Lude, Wang Xin, Song Qize, Yang Xujie
    1989, 10(11):  1133-1135. 
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    The reaction of Fe(Salen)NO3 with nitrite in DMFwas studied by UV-visible,1H NMR, and cyclic yoltammetry.The UV-visible results show that there are no isosbestic points in all the range of nitrite concentrations, indicating that more than two species are present at equilibrium.The NMRspectrum gives a feature of high-spin property.The E1/2 values depended on the concentration of nitrite, shifting slightly to more negative potentials as the nitrite concentration was increased.When the scanning rate was increased, the Fe3+/Fe2+ reduction wave split into two waves, also indicating that more than two different species are present at eauilibrium.
    The Synthesis of 7 Meso-Tetrasubstituted Porphyrins
    Zhang Zhoupeng, Xu Deyu, Wang Shaoyin
    1989, 10(11):  1136-1138. 
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    In this paper, the synthesis of 7 meso-tetrasubstituted porphyrins is reported, five of which are new compounds.These new compounds are-mesa-tetrakis(3-methoxy-4-carboxymethoxyphenyl) porphyrin(B), meso-tetrakis(3-morpholinomethyl-4-methoxyphenyl)porphyrin(C), meso-tetrakis[3-(N,N-diethylaminomethyl)-4-methoxyphenyl] porphyrin (D), meso-tetrakis (3-piperidinomethyl-4-methoxyphenyl) porphyrin (E) and meso-tetrakis (3-pyrrolidinomethyl-4-methoxyphenyl) porphyrin (F).Four new substituted benzaldehydes with morpholino-,diethylamino-, piperidino-and pyrrolidi-no-groups are also prepared.
    Studies on the Different Matrix Modifier for the Determinationof Se in Human Hair by ETAAS
    He Jinlan, Liang Feng, He Huilan
    1989, 10(11):  1139-1141. 
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    The trace element Se in human hair was determined by ETAAS.The effect of the different matrix modifiers is discussed.The mechanism of the matrix modifier in the graphite furnace was studied by means of surface analysis of the graphite cup by X-ray photbelectron spectroscopy.
    The Determination of Trace Germanium by Adsorptive Stripping Catalytic Voltammetry
    Sun Changqing, Gao Qian, Xi Jubai, Xu Hongding
    1989, 10(11):  1142-1143. 
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    Anew method for determination of trace germanium by adsorptive stripping catalytic voltammetry has been established.In a supporting electrolyte containing 1.5 × 10-3 mol/L DHB, 2.5 ×10-3 mol/L EDTAand 1 × 10-4 mol/L V(V), a sensitive adsorptive stripping catalytic peak of germanium-DHBcomplex was obtained by DPSat pH=2.1.The change of peak height with the concentration of germanium is linar in the range of 1.2× 10-10～8× 10-8 mol/L.
    Interaction Between Triphenylmethane Acidic Dyes and Non-ionic Surfactant Studied by NMR
    Zhu Jinjing, Tao Jiaxun, Zheng Yongxi
    1989, 10(11):  1144-1146. 
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    Interactions between triton X-100 and chrome azurol Sor eriochrome azurol Bare studied by 1H NMRtechnique.The variant behavior of triphenylmethane acidic dyes in these reactions were due to the difference of hydrophilic-lyophobic equilibrium values.
    Studies on Adsorption Behaviour and Application of Noble Metal Group Reagent Polythioether
    Li Lingying, Xu Xiaowen, An Yan, Ma Jinqiu
    1989, 10(11):  1147-1149. 
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    Anew adsorbent polythioether(PTE) synthesised by us for simultaneously adsorbing and determining all noble metals was represented and studied.The effects of temperature, heating time, acidity, different acid mediums, base metals were investigated intensively.Nearly all base metals did not interfere.The adsorption capacity of PTEfor noble metals was very high (e.g.750 mg Au/g dry adsorbent).The possible mechanism of adsorption was suggested.Areasonable PTEadsorption process followed by ICP-AESmethod for simultaneous determination of all noble metals was represented.The results found in the synthesized samples were satisfactory.
    Studies on Hydrolysis and Polarographic Behavior of Amygdalin
    Li Cang, Yuan Zhoubin
    1989, 10(11):  1150-1152. 
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    Amygdalin is a non-active material.The polarographic study is based on the β-glucosidase-catalyzed hydrolysis of amygdalin to benzaldehyde.In a basic solution of injectio natrii chloridi the hy-drolysate of amygdalin exhibited a well defined reduction peak in a 2.5th differential polarogram, the peak potential was-1.340V (Vs.Ag/AgCl).The current was proportional to amygdalin concentration in the range of 5.9× 10-7 to 1.4× 10-4mol/L.With increasing pHin the basic solution, peak potential negatively shifted.Scanning rate, surfactant temperature and cyclic polarogram show that the reduction wave is a irreversible process controlled by difusion.Specific activity of β-glucosidase was first determined by polarography.The effect of various enzyme concentration on peak current was observed.
    The Reaction Model for the Esterification of Acetic Acid with Propene in Gas-Liquid System Catalyzed by Heteropolyacid
    Huang He, Liu Jinlong, He Min, Cai Tianxi
    1989, 10(11):  1153-1155. 
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    According to the experimental results, a reaction model for the gas-liquid addition esterifica-tion catalyzed by heteropolyacid was proposed.The existence of optimum temperature and its shift regularly with change of the reaction conditions, e.g., the species or concentration of catalyst, pressure and the water content are explained by proposed reaction model.
    AOM Analysis on Ligand Field Spectra of the Pyrazole Species Complexes of Pseudo-Tetrahedral Co(Ⅱ) (C2υ)
    Dou Yusheng, Ren Youxian, Zhao Jianshe, Liu Yuanfa
    1989, 10(11):  1156-1159. 
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    The ligand field spectra of the complexes with formulae CoL2'X2 (L' = 1-methyl-3, 4-diphenylpyrazole, X=Cl-, Br-, I-, NCS-) and CoL2Cl2(L=1-methyl-3,5-diphenylpyrazole) have been fitted by means of Angular Overlap Model (AOM).The fitting results are comparatively satisfactory.The effects of varying the angle, the angle between the C2 axis and the metal-ligand bond directions, on the energy levels of quartet states for the complex CoL2Cl2 were interpreted by means of AOMcalculations.The AOMparameters for each ligand were obtained.The fitting and calculating results has been discussed.
    Studies on Syntheses of Macrocyclic Polyether Compounds (Ⅲ)——Syntheses of 6-Alkoxy-dibenzo-16-crown-5
    Niu Changrong, Wu Chengtai, Qu Hexin
    1989, 10(11):  1160-1162. 
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    This paper reports the syntheses of a new groups of 6-alkoxy-dibenzo-16-crown-5 compounds Ⅲa-h.The reaction of 6-hydroxy-dibenzo-16-crown-5 with metal sodium produced a sodium alkoxide in anhydrous benzene and anhydrous 1,4-dioxane.When the sodium salt underwent condensation reaction with dimethyl sulfate, bromoethane, i-butyl iodide, 1-bromobutane, 1-bromopentane, 1-bromoheptane, 1-bromohexadecane and benzyl bromide, respectively, eight kinds of corresponding crown ether compounds were obtained.
    Studies on a Liquid Crystal Forming Polymethacrylate with Laterally Substituted Mesogens
    Zhou Qifeng, Zhou Hongbing
    1989, 10(11):  1163-1165. 
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    Apolymethacrylate with laterally substituted mesogens as side groups was synthesized.It v/as found that the polymer was noncrystailine with a glass transition temperature of 170℃, above which a liquid crystalline state was formed.The stiffening effect that the mesogenic side groups have upon the molecules is considered responsible for both the high Tg value and the liquid crystal forming properties of the polymer.
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