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Table of Content

    24 April 1981, Volume 2 Issue 2
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    Articles
    PREPARATION OF PHOTOSENSITIVE ELECTRODES BY THE THERMAL OXIDATION ON TITANIUM FOIL
    Su Hongyu, Fu Yilu, Zhuang Shuxian, Xu Shuqian, Chen Congxiang
    1981, 2(2):  131-138. 
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    The condition for the preparation of the electrodes of polycrystalline TiO2 film on Ti foil was studied. It was found that the adhesive problem of the film with the substrate metal during the reaction of thermal oxidation of Ti and reduction of TiO2 film might be solved by adding small amount of water vapor to the fluxional gas. Photosensitive electrodes with different thicknesses of film had been prepared. The relation between the thickness of film and photocurrent had been studied. By means of thermal conductivity detector, we studied the reducing condition of TiO2 in hydrogen ambient. The influences of the different reducing temperature of TiO2 on photocurrent were investigated. Using the TiO2 electrode prepared, we have photoelectrolyzed water by sunlight with an energy conversion efficiency of 1.2%.
    STUDIES ON SYNERGISTIC EXTRACTION SYSTEMS INVOLVING ACYLPYRAZOLONES——Ⅱ——EXTRACTION OF CERIUM (Ⅲ) BY ACYLPYRAZOLONES WITH VARIOUS SUBSTITUTING GROUPS AND THE SYNERGISM WITH DIOCTYLSULFOXIDE
    Gu Yidong(Ku Yih-tong), Song Yuan(Soong Yuan)
    1981, 2(2):  139-147. 
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    Five different acylpyrazolones, with various substituing groups, were used to study the extractibility of Ce(Ⅲ) at pH 3.1 into chloroform. The extractive ability decreases in the following order: (HTTAwas also included for comparison).1-Phenyl, 3-methyl, 4-trifluoroacetyl pyrazolone(5) (HAPZ-8113F)>1-phenyl-3-phenyl, 4-benzoyl pyrazolone(5) (HAPZ-888)>1-phenyl, 3-methyl, 4-benzoyl pyrazolone(5) (HAPZ-818)>1-phenyl, 3-methyl, 4-acetyl pyrazolone(5) (HAPZ-811)>2-thenoyl trifluoroacetone(HTTA)>l-phenyl, 3-methyl, 4-formyl pyrazolone(5) (HAPZ-810)The reasons for introducing the above symbols in the above parentheses to represent the various extractants are explained.From the slope method, although HTTAin HCl gave the extracted species as CeA3, various acyl pyrazolones gave CeA2·Cl·HAin the same experimental conditions. In HNO3 system, HAPZ-8113Fgave CeA3 however.The logarithms of the extraction equilibrium constants calculated from the experimental data are: HAPZ-8113F/Cl-0.08, HAPZ-818/Cl--0.82, HAPZ-811/Cl- -2.57, HTTA/Cl- -9.05, HAPZ-8113F/NO3--4.05. The extraction with HAPZ-810 is very slight.The synergistic effect, when dioctylsulfoxide DOSOwas used in conjunction with various acylpyrazolones, was also studied. The effectiveness of synergism, when expressed as the ratio, Dmax(HA + S): DHA, was in the order,HAPZ-8113F>HTTA>HAPZ-888>HAPZ-818.Radioactive 144Ce as fracer added to natural cerium, was used throughout the experiment.
    A NEW COLORIMETRIC INVESTIGATION IN DETERMINATION OF TWO INTERFERING COMPONENT SYSTEMS——THE EXTRAPOLATION METHOD OF CONSTANT COMPONENT RATIO
    Shih Hueiming, Hoh Siwen, Yang Wanlong
    1981, 2(2):  148-154. 
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    An extrapolation method of constant component ratio has been proposed for the determination of two interfering component systems. The theoretical fundament of the method has been discussed finally, in applying the method for investigation of two interfering component systems is desired.
    ON THE FORMATION OF THE TERNARY COMPLEX OF Mo(Ⅵ)-NH2OH-5-Br-PADAP AND ITS APPLICATION IN SPECTROPHOTOMETRIC DETERMINATION OF MOLYBDENUM
    Chen Yushou, Huang Zexing, Lu Jintong, Zhang Lulian
    1981, 2(2):  155-162. 
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    When the solution containing Mo(Ⅵ) is boiled in the presence of NH2OH, Mo(Ⅵ) can react with 5-Br-PADAP, forming a water insoluble blue ternary complex Mo(Ⅵ)-NH2OH-5-Br-PADAP. However, in the presence of OPthe complex does not precipitate. The molar ratio of the three components in the complex is estimated to be Mo(Ⅵ):NH2OH:5-Br-PADAP =1:1:1. The wavelength of maximum absorbance for the complex is 605 nm. The molar absorptivity is 48000 at 605 nm. The calibration curve follows Beer's law in the range from o to 30μg of Mo (Ⅵ) in 10ml solution. As contrary to the usual practice masking agent is added after the colour development, and then the solution is boiled again to eliminate the effect of interfering ions. It is found that the method proposed in this work has very high selectivity.
    STUDIES OF LIQUID CRYSTALS AS STATIONARY PHASES IN GAS-LIQUID CHROMATOGRAPHY——I——CHROMATOGRAPHIC SEPARATION OF TOLUIC ACID ISOMERS ON KIESEL GUHR-LINED GLASS CAPILLARY COLUMN COATED WITH NEMATIC LIQUID CRYSTAL
    Chen Yaozu, Ma Xueyi, Wu Linyou
    1981, 2(2):  163-168. 
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    Arapid and effective chromatographic separation of toluic acid (methyl ester) isomers on a kieselguhr-lined glass capillary column of 30m length and 0.32mm. i. d. coated with a nematic liquid crystal has been established.
    THE RESEARCH ON THE LASER INTRA-CAVITY ABSORPTION SPECTROMETRY OF NEODYMIUM
    Zhu Guiyun, Yang Jinghe
    1981, 2(2):  169-175. 
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    The laser intra-cavity absorption method is of a newly developed technique used for the determination of weakly absorbed substance, it has the merits of high sensitivity and simple operation. This paper has, studied the effects of various laser parameters(including resonant cavity length, pump energy, the transmittance of output mirror, pulse repetition frequency, etc.) on sensitivity. Apreliminary theoretical exploration is presented. An important reason why the formula proposed by Horlick does not coincide with the result of this experiment is due to the fact that two reflective mirrors of the resonant cavity can not be strictly parallel. The corresponding formula is deduced.Experimental results showedn that Beer's law is obeyed in the range of Neodymium ion concentration of 2 ×10-3-1×10-2 M, the sensitivity increases by a factor of 27, as compared with that of the conventional absorption spectrometry, some rare-earth elements like La, Ce, Pr, Sm, Yetc. do not interfere. This method can be used for the determination of Neodymium in light rare-earth mixtures.
    STUDY OF GEOMETRIC ISOMERS OF SOME VINYLPHOSPHATE INSECTICIDES——II——THE STEREOSPECIFIC SYNTHESIS OF THE O,O-DIMETHYL-O-(1-ETHOXYCARBONYL-1-PROPEN-2-YL) PHOSPHATE INSECTICIDE (MIE-YA-JING) AND ITS ANALOGUES
    Shao Ruilian, Dong Xiyang, Zhang Chunzao
    1981, 2(2):  176-182. 
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    The present report deals with the stereospecific synthesis of the O, O-dimethyl-O-(1-ethoxycarbonyl-1-propen-2-yl) phosphate, an insecticide named Mie-Ya-jing in Chinese. The reaction of phosphorus oxychloride with ethyl acetoacetate in the presence of tributylamine yeilded specifically the E-stereoisomer as the key intermediate, from which E-stereoisomer "Mie-Ya-jing" was prepared by treating with excess of methyl alcohol. It seems that there is a relationship between the steric factors of the base and the E/Zratio obtained. The Z-stereoisomer was synthesized by the action of dimethyl phosphoryl Chloride on ethyl sodioacetoacetate. The other two Mie-Ya-jing derivatives were similarly prepared. The E-isomer proved to be more toxic to insects than the corresponding Z-isomers.
    SYNTHESIS OF N-ETHYLPERHEXILINE MALEATE AND PERHEXILINE MALEATE
    Li Liangzhu
    1981, 2(2):  183-187. 
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    Anew compound N-ethylperhexiline maleate (Ⅱ) is isolated duringthe synthesis of perhexiline maleate (I), which has been known as an effective drug in the treatment of coronary atherosclerosis. Studies of its m. s., IR. and element analysis prove that it has the structure as indicated by (Ⅱ). (Ⅱ) was also prepared by alkylation of the free base of perhexiline maleate. Its pharmocologic test is shown to be more effective than (I) when it is used as an anti-arrhythmic agent.The new route of synthesis is by condensing of benzophenone with 2-methylpyridine in the presence of sodamide giving-1,1-diphenyl-2- (2-pyri-dyl) ethanol (Ⅲ), which is dehydrated to yield 1 ,1-diphenyl-2-(2-pyridyl) ethene (Ⅳ), followed by complete hydrogenation in ethanol and then treated with maleic acid to form perhexiline maleate (I) and N-ethylperhexiline maleate (Ⅱ). The yields of (I) and (II) are 43% and 11% repectively.
    RESEARCH ON O,O-DIALKYL-S- [N-(2-THIAZOLYL OR SUBSTITUTED THIAZOLYL) CARBAMOYLMETHYL ] MONO-OR DITHIOPHOSPHATES AS INSECTICIDES OR FUNGICIDES
    Yang Shih-hsien, Tsai I-Chiang
    1981, 2(2):  188-194. 
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    1. Aseries of sodium thio- or dithiophosphates and derivatives of 2-aminothiazole were prepared.Three among the derivatives of 2-aminothiazole are new compounds which have never been reported.
    THE CLEAVAGE OF ARYL-SILICON BONDS
    Zhou Xiuzhong, Zhang Zengyou, Liang Ge, Guo Congyuan, Me Qiangzhong, Xie Qinglan, Xu Shansheng
    1981, 2(2):  195-200. 
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    By means of equimolecular competing reaction we investigated the cleavage of five aryl trimethyl silanes by hydrogen chloride.The cleavage products were quantitatively analyzed by gas cbromato-graphy. The selective yield of every cleavage product showed that the reactive sequance was in accordance with the result of corresponding homogeneous cleavage.
    THE RELATION BETWEEN THE NEIGHBORING PHASE REGIONS AND THEIR BOUNDARIES IN PHASE DIAGRAMS-Ⅱ
    Zhao Muyu
    1981, 2(2):  201-210. 
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    The theorem of corresponding relation between the neighbouring phase regions (expressed by N. P. Rs) and their phase boundaries and six corollaries of this theorem were derived from the principle of phase equilibria. According to them, there are definite relations between the dimension of phase boundary (set of equilibrium phase points) R1,the total number of different phases in the two N. P. Rs Φ, the number of the common phases existing in the both N. P. Rs, △φ, and the dimension of common boundary (set of system points), R1. Applying this theorem and its corollaries, the following results may be obtained. Both of the boundary rule and Palatnik-Landau's contact rule of phase regions in phase diagrams may be deduced. The ten empirical rules, concluded by F, N. Rhines and followed for constructing the complex ternary phase diagrams, may be put on a theoretical basis. The relations between the N. P. Rs and their boundaries in the phase diagrams of one-、two-、three-and four- components of different types may be explained without applying any supplementary conceptions.
    A NEW NUMERICAL METHOD FOR THE SOLUTION OF RADIAL HARTREE-FOCK-SLATER EQUATION
    Liu Xuezhong, Li Lemin
    1981, 2(2):  211-224. 
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    In this paper, a new numerical method for the solution of radial Hartree-Fock-Slater equation is proposed. The discretized form of the HFSequation, using second-order or 4th-order finite differences, results in a set of quasi-linear algebraic eigenvalue problems. The coefficient-matrices are dependent on the solutions. After linearizing the coefficient-matrices, we can solve the eigenvalue problems by the Newton's method to obtain the eigenvalues and the corresponding eigenvectors simultaneously. We solve he linear system therein by the double sweep method. Then we can correct the coefficient-matrices by the simple weighting iterate method or by the Newton's method. This numerical method has been programmed for computer. The results of trial calculations of Cu+ and Mn2+ are consistent with those in published literature. Actual calculation shows that the stability of this numerical method is good.
    THE CHROMATOGRAPHIC INVESTIGATION ON ADSORPTION OF ETHYLENE ON Pd-V SYSTEM CATALYSTS
    Wu Zhiyun, Guo Heichen, Li Minxue, Zhao Zhongqing
    1981, 2(2):  225-232. 
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    The adsorption properities of ethlene on Pd-V-Ti-Mo oxide/SiO2 and Pd-Voxide/SiO2, V2O5/SiO2, PdO/SiO2, SiO2 were investigated by pulse chromatography.On both Pd-V-Ti-Mo oxide/SiO2 and pd-Voxide/SiO2 catalysts the irreversible adsorption and reversible adsorption of ethylene were measured respectively. The reversible adsorption in our experimental conditions does not play a direct role in oxidation reaction.No irreversible adsorption of ethylene on PdO/SiO2, V2O5/SiO2 and SiO2 was exhibited. However, the irreversible adsorption of ethylene on Pd-V-Ti-Mo oxide/SiO2 and Pd-Voxide/SiO2 was very obvious. It is also shown that the amount of irreversible adsorbed ethylene on Pd-V-Ti-Mo oxide/SiO2 catalyst containing 0.05% Pd and its correlated activity of oxidation were all the highest. So the authors consider that there is a direct relationship between irreversible adsorption and the reactivity of selective oxidation of etylene, and the active centers are, perhaps, caused by Pd-Vconbination.The active surface area was calculated and the effect of preadsorbed oxygen on chemisorption of ethylone was examined By-product (CO2) does not make catalysts poisoned.
    A STUDY OF THE BIS(TRIPHENYLSILYL)CHROMATE CATALYST AND ITS SURFACE REACTIONS IN THE PREPARING PROCESS
    Qiu Xingyu, Ping Xuezhen
    1981, 2(2):  233-243. 
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    The effects of light and thermal and the hydrolysis of bis(triphenyl-silyl)chromate and the surface reactions in the preparing process of bis (triphenylsilyl)chromate catalyst have been studied. The results show that while the bis(triphenylsilyl)chromate was precipitated on the silica, it was reacted with hydroxyl group of surface of silica, and formed a surface organo-chromium compound, but the valent state of chromium was unchanged. After added triisobutyl aluminium, the surface compounds were reduced to form low-valence surface organo-chromium compounds which contained Cr-Cor Cr-Obond. There was catalytic activity for olefins polymerization. The load mechanism of active component of this catalyst system has also been discussed.
    A CONDUCTION TYPE AUTOMATIC CALORIMETER
    Tian Anming, Qin Ziming, Zeng Xiancheng, Zhan Shuguang, Deng Yu
    1981, 2(2):  244-250. 
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    1. On the basis of our previous works, a conduction type calorimeter, is constructed which is automatized with a photo-pen recorder. It behaves well in a wider temperature range between ambient to 150℃.2. The heat constant of this calorimeter is calibrated with electric energy and the constants at 100℃ and 150℃ are reported in this paper. From these experimental results, this calorimeter is believed to be in conformity with Tian's equation.3. The sensitivity of this calorimeter is high enough for the measurement of the heat evolved by a chemical reaction. The heat of one calorie can be measured with a relative standard devivation of about 0.5% to 1%.
    STUDIES OF THE EXTRACTION OF GALLIUM AND ITS MECHANISM WITH DIMETHYLHEPTYL ACETAMIDE
    Bao Changnian, Zhang Decheng, Niu Shaochong, Liu Zhenrong, Song Qingfang
    1981, 2(2):  251-256. 
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    The extraction behaviour of gallium(Ⅲ) ion and of metal ions from aqueous hydrochloric acid solution or sulfiric acid and sodium chloride solution with substituted amide-type extractant-dimethylheptyl acetamide (N503) has been investigated systematically.The mechanism of extraction of gallium with dimethylheptyl acetamide was discussed by the maximun saturation method, chemical analysis, infrared spectrum, etc.
    Preface
    SPECTROPHOTOMETRIC DETERMINATION OF THE EQUILIBRIUM CONSTANT OF THE MIXED-LIGAND COMPLEX (Cd phen) 2 BPR
    Yang Weida, Jin Jihong
    1981, 2(2):  257-260. 
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    The equilibrium constant of mixed-ligand complex formation in the following reaction  has been evaluated by a new variant of graphical method based on the data of spectrophotometric measurements. The equilibrium constant and the apparent stability constant of the mixed-ligand complex are 6.7×1010 and 2.6×1022 respectively at 25℃, pH8 and ionic strength 0.1.
    Articles
    NEW EXTRACTIVE PHOTOMETRIC METHOD FOR THE MICRODETERMINATION OF TELLURIUM
    Xu Qiheng, Liu Songyu, Liu Jinyao, Peng Youxian, Xu Xiujun
    1981, 2(2):  261-263. 
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    In the present work, the reaction of tellurium(Ⅳ)with malachite green has been investigated. In phosphoric acid solution, Te (Ⅳ) forms ionic associates with KIand malachite green. This complex can be extracted into benzene.The maximum absorbance of the complex is at 635nm. Its molar absorption coefficient is 2.37×105. The mole ratio of tellurium, iodide and malachite green is 1:6:2. The amounts of tellurium in the range 0-6μg per 10ml.of benzene follow Beer's Law. The procedure is simple, rapid and sensitive. The results are satisfactory for the microdetermination of tellurium in alloys.
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