Table of Content

24 January 1988, Volume 4 Issue 1

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Articles

The Synthesis and Structure of Tris-nitrato-Aqua-(2,6-Diacetyl-Pyridine) Bis (semicarbazone)lanthanum(III)

Yao Xinkan, Wang Honggen, Wang Ruji, Pan Xiangyang, Yan Sniping, Wang Genglin

1988, 4(1):  1-8. 

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The complex of (La(DAPSC)(NO₃)₃ H₂O) · H₂O was prepared. Its crystal data are: triclinic, space group P₁, a =8.736(1), b = 12.108(3), c =12.412(3)Å, α=110.35(2)°, β =94.88(1)°, γ = 95.35(2)°, v =1215.78(ų, Z =2.It was found that two arms of the ligand DAPSC can be opened to accept the La(Ⅲ). This is obviously different from the complex of Sm(Ⅲ) with DAPSC. DAPSC can be expanded easily, but it is hard to be compressed.

The Synthesis and Structure of Silica-Sodalite from Nonaqueous Systems

Feng Shouhua, Xu Jianing, Xu Ruren, Yang Guangdi, Chen Zhonggou, Li Genpei

1988, 4(1):  9-16. 

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A silica polymorph, silica-sodalite was synthesized from a nonaqueous system NaOH-SiO₂-C₂H₄(OH)₂ and its chemical compositionwas determined to be Si₁₂O₂₄,2C₂H₄(OH)₂ by the X-fluorescence,thermogravimetric and organic elemental analyses. The single crystal X-ray diffraction structure determination of the silica-sodaliteshowed that the silica-sodalite is cubic, spacing group I23 and unitcell parameter a= 8.8354Å. The IF and solid state high resolution ²⁹Si and ¹³C NMR spectra of the silica-sodalite were measured and discussed.

Separation of Nine Metal Tetrekis (M-Bromic)phenylporphyrin Complexes by High-performance Liquid Chromatography

Cheng Jieke(Cheng Jai-Kai), Xu Xuejun, Zhang Huashan, Zhang Chuanyou

1988, 4(1):  17-22. 

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A series of compounds of meso-tetraphenylporphyrin (TPP) derivatives of fluorine, chlorine and bromine was synthesized. The sub-stituent of meta-Br has a great effect on the retention strength of TPP. The reversed-phase HPLC for the separation of some metal complexes of meso-tetrakis (m -bromic) phenylporphyrin (m-BrTPP) was studied. The resolution(R_s) of the metal complexes increases significantly. A combination of an octadecyl-bonded stationary phase with a mobile phase such as methanol-acetone mixture has been proved tobe effective for the separation. The nine m-BrTPP complexes of Sn, Mg, Cd, Fe, Pb, Zn, Ni, Cu and Ag and m-BrTPP free acid were completely separated within 20min on a RP-C18 column (YQG-C₁₈, China, 5μm, 150×5mm i.d.) with a 65:35 (V/V) mixture of mefhanol and acetone. The detection limits are in the range of from 6 to 100ppt (pg/mL) for each metal except Pb. The recoveries of the eight trace metals in the synthetical mixture samples were in the range of 93-108%.

Synthesis of Fluoro-Contained Bisazo Chromotropic Acid Derivants and studies on Their Color Reactions with Rare Earth Elements

Yang Yi, Yu Ximao, Cai Ruxiou, Zeng Yun'e

1988, 4(1):  23-29. 

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In this paper, a series of f1uoro-contained bisazo chromotropic acid derivants has been designed and synthesized. They are easily soluble in water, alcohol and acetone but insoluble in benzene, ether and chloroform. Some regularities of the effects of their molecular structure on the color reaction have also been studied. The result shows that in this series of reagents, DCF-chlorophosphonazo and DBF-chlorophosphonazo are excellent color reagents for the determination of the total amount of rare earth elements. The molar absor-ptivities of light and heavy rare earth elements are approach to each other. The tolerant quantity of Bi (Ⅲ) and Pb (Ⅱ), Sn(Ⅳ) are larger than that of the other arsenazo or chlorophosphonazo type of color reagents. We also discover that p-fluorochlorophosphonazo can form β-type complexes with heavy rare earth elements, and p -fluoro-carboxyazo with light rare earth elements. If the reaction time is controlled, p -fluoro-carboxyao can form β-type complex only with La, and the other light or heavy rare earth elements have no this type of reaction.

1,3,2-Oxazaphospholidine Derivatives(I)——The Synthessa of 2 - Diethylamino- 3-arylsulfonyl- 1,3,2-Oxazaphospholidine and Its 2-thiono Deiativea and Their Properties

Yang Huazheng, Cui Shuhua, Zhang Zhengpu, Chen Ruyu

1988, 4(1):  30-37. 

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A series of new 2-diethylamino-3-substituted phenylsulfonyl-1,3,2-oxazaphospholidine derivatives (Ⅰ) has been synthesized by the reaction of tris(diethylamino) phosphine with N-(β-hydroxyethyl) substitutedphenylsulfonamides. When was refluxed with sulfur in benzene, the 2-thiono derivatives (Ⅱ) was obtained conveniently.(Ⅰ) was easily oxidized in air and the diethylamino group could be substituted by phenoxy or other amino group giving the corresponding derivatives. Their ¹H NMR and MS spectra have been discussed. Some of compounds (Ⅱ) have herbicidal activities.

Studies on Nucleophilic Ring-Opning Reaction of Ethylene Epoxide by (μ- CH₃S)(μ-IMIgS) Fe₂ (CO)₆——Syntheais and Crystal Structure of (μ-Methylthio)- (μ- R -Hydroxylethylthio)hexacarbonyldiiron

Song Licheng, Wang Ruji, Hu Qingmei, Wang Honggen

1988, 4(1):  38-44. 

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A new type of Fe-S complex (C), (μ -CH₃S) (μ-HOCH₂CH₂S) Fe₂(CO)₆ which contains μ-β-hydroxyethyl, has been synthesized in high yield through ring-opening reaction of ethylene epoxide under uncleophilic attack of active complex (A), (μ-CH₃S)(μ-IMgS) Fe₂(CO)₆, followed byan alcoholysis of the intermediate (B). The crystal structure of (C) was determined by an X-ray diffraction technique. The crystal belongs to monoclinic system with space group of C₂/c. Cell parameters a= 15.784(3), b = 22.172(3), c=9.774(2)Å, β=119.53(2)°, V=2976.3ų. D_c = 1.80g cm^-3, Z=8, F(000)=1616 and final R=0.077.

The modef ication of Spectrophotometric Method for Coordinetion Nucleophilic Systems

Wang Kezhi, Han Weiping

1988, 4(1):  45-52. 

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A modified spectrophotometric method for coordination nucleo-philic substitution reactions between two kinds of ligands of mono-nuclear complexes MZ#em/em#, MLj is proposed, which introduces a simpler formula for calculation and may be applied to complex systems and the hydrolysis of metal ions.As an illustration of the proposed method, we determined the spectrophotometric data of seven competitive systems in the solutions of various pH and calculated the successive stability constants and molar extinction coefficients, and the results are in good agreement with each other. The effect of the hydrolysis of metal ions on determined results depends on (1 + Σβ_a^* H^-a) and (ΣβⁱC_zⁱ)

Study of Resolution of dl-Amino Acids with Acrylate Type of LigandE Exchange Ghiral Resins

He Binglin(Ho Pinglun), Jin Renhua

1988, 4(1):  53-59. 

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The paper discribes the resolution of dl-Phe, dl-Phser, dl-Tyr, dl-Tryp, dl-His etc. by ligand exchange chromatography using L-Pro grafted resins coordinated with copper (Ⅱ) as stationary phase. Except dl-His, the other amino acids mentioned above could be completely resolved and D-amino acids were eluated before L-amino acids. Through determination of IR spectra of L-Pro-PGMA-Cu resin, its possible coordinated model of structure of resin and mechanism of resolution are presented.

Conductivity Measurements of a Con jugated-Polymer Single crystal at Lower Temperature

He Pingsheng, Peng Jianbang, Lu Zhihui, Chen Baozhu, Li Yuejin

1988, 4(1):  60-66. 

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The conductivities in bis-(p-toluene sulfonate) or 2,4-hexa-diyne-1,6-diol(TS) and its polymer PTS single crystal were measured by means of a special device at a range of temperature from 77K to 373K (353K for TS). Anomalies of the conductivity of TS and PTS along c-axes which are the directions of PTS at the temperature corresponding to their low temperature phase transition were observed. The temperature of phase transition in TS obtained from anomalies of conductivity are 163K and 208K.

Studies on the Copolymerization of Propylene and Butadiene with Supported Titanium Catalysts (I)——Copolymerizat ion and Characterizat ion of the Products

Wu Qing, Lu Zejian, Lu Yun, Lin Shangan

1988, 4(1):  67-73. 

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Copolymerizations of propylene and butadiene in various ratios with two kinds of supported catalysts, i.e. TiCl₄/MgCl₂/AlEt₃ and TiCl₄/MgCl₂/AlEt₃/ethyl Bonzoate(EB). have been investigated. The results show that these two catalysts are quite effective for propylene-butadiene copolymerization but behave in different features. Characterizations of the copolymerization products by solvent extraction, IR, ¹³C NMR, X-ray diffraction and DTA show that blocked propylene-propylene and butadiene-butadiene sequences exist in polymer chain and the butadiene units are exclusively in trans-1,4 configuration.

The Immobilization of Glucose Oxidase and its Improved Method

Li Lixia, Lu Ge, Chen Changzhi, Yu Yaoting

1988, 4(1):  74-82. 

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The best conditions of immobilizing glucose oxidase using different supports and different methods were studied and compared. An improved method of glucose oxidase immobilization by glutar aldehyde was studied. One end of a glutaraldehyde molecule was first protected by die thanolamine and the other end was linked to the carrier. Then the protected end was hydrolysed and glucose oxidase was linked to it. Glucose oxidase immobilized according to the above method has the highest activity. The enzyme activity was two fold higher than the polyacrylamide and 10% higher than the diazo method.

The Absorbance Effect in photopolymerization——O-Acyl - α -Oximinoketone Initiator System

Li Tong, Sun Meng, Tong Weida, Yu Tongyin

1988, 4(1):  83-88. 

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The photopolymerization of acrylonitrile and methyl methacrylate initiated by O-acyl-α-oximinoketone was studied under irradiation at 365nm and 313nm. The kinetic behavior was quite different in high absorbance and in low absorbance systems. In low absorbance, the initiator exponent measured was 0.5, while in high absorbance, the rate of polymerization and molecular weights of the polymers were all independent of the initiator concentrations. The greater the extinction coefficient of the initiator, the lower the concentration at which initiator exponent is zero power.

Kinetics of the Ziegler-Natta Polymerization of 1-Octene——The Kinetics and Mechanism of the Induction period

Fan Zhiqiang, Feng Linxian, Yang Shilin

1988, 4(1):  89-96. 

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The kinetics of the induction period in the polymerization of 1-octene catalyzed by Solvay TiCl₃-alkyl aluminium was studied with a dilatometer. The induction period decreases as [TiCl₃] and [M]₀ increase and temperature rises. It was observed through a microscope that large catalyst particles broke up into small particles in the induction period. So a kinetic model was proposed which ascribes the induction period to the breaking up of catalyst particles under the effect of polymer, and the most of the experimental results can be explained on the basis of the model.