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中文
Table of Content
24 September 1989, Volume 10 Issue 9
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Articles
Diaryl Boron Chelates of Thioproline
Yuan Guozheng, Huang Junjie, Zhang Guomin
1989, 10(9): 881-885.
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Thioproline which can induce the cancer cells to lose the characteristics of tumoral transformation unites with diaryl boron group, forming pseudometal-chelated compound.The structures of nine compounds were confirmed by elemental analysis,and IR,MSand NMRspectrometries.
Synthesis and Spectroscopic Properties of Tetrakis(triphenylphosphine oxide)dichlorolanthanide-Cupric Trichlorides
Wang Xukun, Zhang Mingjie, Wang Zhefu, Jing Xuying, Wang Jitao, Lin Chuai
1989, 10(9): 886-889.
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Aseries of new complexes [LnCl
2
(Ph
3
PO)
4
][CuCl
3
] were prepared (Ln = La, Ce,Pr,Nd, Sm,Eu, Gd, Tb, Dy, Ho, Er, Y).X-ray diffraction crystallographic structural analysis for [GdCl
2
(Ph
3
PO)
4
] [CuCl
3
] reveals Gd(Ⅲ) is of hexa-coordinated distorted octahedral configuration and Cu(Ⅱ) is of tri-coordinated trigonal planar configuration.All the complexes are characterized by IR,
31
P NMR,and ESR.The conditions for the synthesis of the title complexes are discussed.
The Principle of Expansion-Contraction and Position Shift of Oscillopolarogram
Xu Weijian, Gao Hong
1989, 10(9): 890-893.
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Using expansion (contraction) and position shift of the whole oscillopolarogram to indicate the end-point of titration is a new technique which is a very useful oscillopolarographic titration method.This paper reports the principle of this method.The theoretical predictions consist with the experimental results.Expansion (contraction) of oscillopolarogram is due to the variation of electrode impedance and the position shift comes from the differences between kinetic factors at two electrodes.
1.5th and 2.5th Order Differential Polarographies with Multistep Reversible Charge Transfer
Xue Yongjun, Yuan Zhuobin
1989, 10(9): 894-896.
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The theories of 1.5th and 2.5th order differential polarographies for (n
1
= n
2
) multistep reversible charge transfer are proposed and the theoretical polarograms were drawn with a computer.The effect of both the standard potential separation (△E
0
) and the number of electrons (n) on polarograms is carefully discussed.The reduction of Cu(Ⅱ) in 0.10 mol/L NH
4
+
Cl
-
NH
4
+
OH
-
was selected to test the theories and the experimental results were in agreement with the theories.
Studies on A Micro-Sample Introduction System for MIPAES
Que Hong, Zhang Hanqi, Jin Qinhan
1989, 10(9): 897-900.
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In order to overcome the problem of low sample tolerance of MIPwith a high excitation capability, a new microsample introduction system based on the combination of microelectrothermal vaporization (ETV) and desolvation with concentrated sulfuric acid was developed.Acomparison between the new system and the conventional desolvation system with a condensor was made.It was shown that the water vapor was better removed by the new system and the stability and the excitation capability were therefore improved.The new sample introduction system is of practical usage.The spectroscopic behavior of Ar MIPand He MIPand the effects of easily ionized elements were studied.
Studies on the Chemical Components of Oxytropis Ochrocephala Bunge(Ⅲ)
Sun Rongqi, Jia Zhongjian, Cheng Dongliang, zhu Ziqing
1989, 10(9): 901-904.
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Two triterpenoid sapogenols Ⅰ and Ⅱ were obtained from the acidic hydrolysis products of the total saponin mixture of oxytropis ochrocephala bunge.Compound Ⅰ, the genuine sapogenol of the total saponin mixture, was identified as soyasapogenol B; compound Ⅱ, a new type artifact sapogenol, was determined to be olean-13(18)-ene-22a-chloro-33, 24-diol.We also isolated a minor saponin Ⅲ which was identified as 3-O-[β-D-glucopyranosyl(1→2)-β-D-glucuronopyranosyl] soyasapogenol B.This paper deals with the identification of compound Ⅰ, Ⅱ and Ⅲ, as well as the chemical transformations between them.The
13
C NMRsignals of compound Ⅰ and Ⅱ were also assigned by using
13
C,
1
Hspin couplings and PRFT-
13
C NMRtechnique.
Studies on Reaction System of Iron Carbonyl-Thiol (Thiophenol)-Triethylamine ——Synthesis and Structure of Some σ,π-μ-Vinyl Fe-S Complexes
Song Licheng, Liu Jinting, Wang Jitao
1989, 10(9): 905-908.
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In this paper three σ,π-μ-vinyl Fe-Scomplexes(μ-RS) (μ-PhCH = CH)Fe
2
(CO)
6
(R=Et, t-Bu, Ph) and six σ, π-μ-vinyl Fe-Scomplexes (μ-RS) (μ-ZCOCH = CH)Fe
2
(CO)
6
(R = Et, t-Bu; Z=Me, Ph, p-MeC
6
H
4
) have been synthesized through the reaction of the intermediates Et
3
NH[(μ-CO)(μ-RS)Fe
2
(CO)
6
](formed from Fe
3
(CO)
12
, RSHor PhSHand Et
3
N)with β-bromostyrene or β-chlorovinyl ketones.The structures for the new complexes prepared were well characterized all by C/ Hanalysis, IRand
1
H NMRspectroscopy and partly by
13
C NMRspectroscopy.
Study on the Components of Saussurea Involucrata Kar. et kin (V)
Li Yu, Jia Zhongjian, Zhu Ziqing
1989, 10(9): 909-912.
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Two sesquiterpenoids were obtained from the extract of 70% aqueous ethanol of Saussurea involucrata kar.et kin.by means of silica gel column chromatography.Their chemical structures are elucidated on the basis of spectral analysis (IR, UV,
1
H NMR,
13
C NMR, MS-EI, MS-FAB, HRMS), chemical transformations and comparison with authentic samples.Crystal I: m.p.244-245℃, C
21
H
30
O
9
, 3a-OH, 11β, 13-dihydrodehydrocostuslactone-β-D-glucoside.Crystal Ⅱ m.p.> 300℃.C
20
H
27
NO
4
; Mayer reagent test: positive, Dragendorff reagent test: positive.It is a novel sesquiterpene lactone alkaloid named as Involucratine.
Study on the Reaction of Aqueous Titanium Trichloride with α-or β-Aminoketones in Basic Media
Chen Weixing, Zhou Zhaolin, Feng Juncai
1989, 10(9): 913-906.
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α-and β-aminoketones are reduced to corresponding diaminopinacols by aqueous titanium trichloride in basic media under an argon atmosphere at room temperature.The dl-and meso-isomers were separated and identified.
Studies on the Characteristics of Metastable Zone of the Aqueous K
2
SO
4
Solution (Ⅰ)——Nucleation Characteristics
Wang Zichen, Zhao Qiugang, Yang Yonghua, Zhao Muyu
1989, 10(9): 917-921.
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Some characteristics of the nucleation kinetics can be obtained by measuring the width of metastable zone during the crystallization of aqueous salt solution.According to the theory of crystal growth, the method of calculation of the nucleation characteristic parameters, including the order of nucleation n, the radius of the critical nucleus r
*
, the number of particles in a critical nucleus N
*
and the specific surface energy σ
12
etc from the experimental data is improved in this article.Using an apparatus equipped with a temperature-programmed digital controller and laser detector of the particle appearance, the widths of metastable zone of aqueous K
2
SO
4
solution were measured and the nucleation characteristic parameters were calculated.The data obtained are very satisfactory by comparison with the values in the literatures.
Theoretical Study on the Spectra of HeNa and HeNa
+
Chen Demian, Huang Mingbao, Xin Houwen, Gao Yuming
1989, 10(9): 922-924.
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In this article we calculate the curves of the ground state
2
∑3s, the excited state
2
Π3p of the molecule HeNa and the states of
1
Π2p,
3
∑3s and
1
∑3s of the cation HeNa+ by using the db initio Molecule-UHFprogram.Furthermore, we calculate the Franck-Condon factors of the excitation from state to state by using the program made by us.The results show that the ground state of HeNa is unstable, the state
2
Π3p has a shallow potential well as well as the state
1
Π2p of HeNa+ and the states of
3
∑3s and
1
∑3s of the cation have very deep potential wells.
The Surface Films of Aliphatic Acid Vapours on the Silica Gel
Zhao Zhenguo
1989, 10(9): 925-929.
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The relationships between the surface pressure(π) and the area(σ) occupied by each adsorbed molecule on the silica gel were calculated by the Gibbs adsorption equation from the adsorption isotherms of vapours of formic, acetic and propionic acid (at 20℃).The resulting π-σ curves were similar to those of the insoluble films on the sarface of solution, there also exist "the liquid-expanded state", "the liquid-condensed state" and "the intermediate state".The surface films are monomolecu-lar layer on water, but become multimolecular layer on the silica gel at a higher vapour pressure.When the monolayer turns to the multilayer, the liquid-expanded state becomes the intermediate.The enthalpy and entropy of adsorption were culculated from the adsorption isotherms at 20℃ and 30℃.The results show that △Hand △Sgo through a minimum at or near monolayer capacity.Near the minimum the state of the film shows a marked change.
Effectiveness Factor of Deep Oxidation of Butane, Trans-2-butene and Cis-2-butene over Pt/Al
2
O
3
Catalyst
Jin Yun, Yu Qiquan, Zhang Ruiqin
1989, 10(9): 930-934.
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The effect of intraparticle diffusion on the deep oxidation of butane, traus-2-butene and cis-2-butene over Pt/Al
2
O
3
was investigated by the flow recirculation reactor.The effectiveness factor of catalyst η was determined experimentally.The values of η are 0.42～1.27, and decrease with the rise of the reaction temperature.The pressure profile of oxygen in the pore of catalyst was calculated by Runge-Kutta method.The partial pressure of oxygen in the pore decreases with the increasing effect of intraparticle diffusion and it tends to zero at 420 ℃.
Studies on the Synthesis and Antitumor Activity of Polyphosphates Containing Both Nitrogen Mustard and Lipophilic Groups
Zhou Nianen, Zhuo Rcnxi
1989, 10(9): 935-938.
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11 New poly phosphates containing both nitrogen mustard and lipophilic groups were synthesized by the polycondensation of N,N'-bis(2-chloroethyl)phosphoramido dichloride with 3-alkoxy-1, 2-propanediol in bezene and in the presence of triethylamine.The polyphosphates were structurally characterized by
1
H NMR, IRspectra and elemental analysis.All of the polymers obtained are insoluble in water, but soluble in common organic solvents.The antitumor activity of some of these polymers were tested against Sarcoma 180 in mice.Polymer Ⅲe exhibits an inhibition ratio of 54.5%.
A Study on the Structures of Polyvinylpyridine-Poly (Styrene-Maleic Acid)-Palladium Catalysts Supported on Silica
Yang Shiyong, Sun Juntan, Li Hong, He Binglin
1989, 10(9): 939-943.
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The Poly(4-vinylpyridine)(P4VP) or Poly(2-vinylpyridine) (P2VP)-Poly(styrene-maleic acid) (PSM)-palladium catalysts supported on silica were prepared.The structures of these catalysts were investigated with X-ray photoelectron spectroscopy, ultraviolet-visible spectroscopy and transmission and scanning electron microscopy etc.It is found that the catalysts were composed of both Pd(0) and Pd(Ⅱ) complexes, and the ratio of Pd(Ⅱ)/Pd(0) was affected by the presence of PSM.The palladium particles in the catalysts are well distributed on the carrier surface.
The Relationships Between Empirical and Theoretical Molecular Weight Distributions of Polymers (Ⅰ)——Guan, Distribution and Poisson Distribution
Yang Meilin, Shen Jiacong
1989, 10(9): 944-947.
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The relationship between Guan distribution and Poisson distribution of molecular weight of polymers has been given by moment analysis, which is the first step for inferring the polymerization mechanism from molecular weight distribution of addition polymer.
NMR Study of Isomers Characteristics of 1-Phenyl-3-methyl-4-benzoylpyrazolone-(5) in Solvents
Feng Anchun, Song Yuan, Wan Guojiang, Gu Yidong
1989, 10(9): 948-950.
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The presence of enol form of l-phenyl-3-methyJ-4-benzoylpyrazolone(5) (PMBP) with an endocyclic intramolecular hydrogen bond elucidated by NMRstudy in Cl
4
or CHCl
3
was established.No reaction of the chelate-proton of enol form with water was shown,but exchange ability was quite active.
Study on the Synthesis and Structure of Zr-ZSM-5 Type Molecular Sieves from Weak Acid System in the Presence of F-Ions
Pang Wenqin, Yu Long, Wu Yaping
1989, 10(9): 951-952.
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Zr-ZSM-5 type molecular sieves were reported in alkali system.In this paper, we crystallized Zr-ZSM-5 type molecular sieves from weak acid system in the presence of F-ions.We verified that Zr replaces Si and enters into the framework of molecular sieves by unit cell determination, IRspectrometry and X-ray electron probe.
Synthesis and Properties of Rare Earth Nitrates with 1,2-Cyclohexyl-12-crown-4 Ether
Yang Ruina, Zhu Wenxiang, Zhao Jizhou
1989, 10(9): 953-955.
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Aseries of complexes of rare earth nitrates with 1, 2-cyclohexyl-12-crown-4 ether were prepared.Elementary analysis data show that they have the same formula of RE(NO
3
)
3
C
12
H
22
O
4
(RE = La-Eu,Gd-Er,Y).The prope.ties of the complexes have also been studied with the IRspectrome-try, differential thermal analysis and molar conductivity techniques.
Separation of Metal Ions by Ion-interaction Chromatography
Lei Zhihong, Tian Shizhong, Cheng Jieke
1989, 10(9): 956-958.
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Some metal ions are separated on a 10 urn bonded column coated with cetylpyridinium by using aminopolycarboxylic acid as the complex reagent.The retention of the metal complexes is due to ion-interaction between the anionic complexes and the sorbed cationic cetylpyridinium.Bi,Co, Pb, Mn, Ni and Cu ions can be completely separated with EDTAas the comoplex reagent,and the detection limits of the metal ions are 0.8, 2, 30, 100, 80 and 50 ng at 230 nm respectively.Co, Bi, Ni, Fe, Cu and Pb ions can be completely separated with DTPAas the complex reagent, and the detection limits of the metal ions are 80, 4, 400, 5, 20 and 100 ng at 254 nm respectively.
Anodic Differential Pulse Voltammetric Determination of 3,4-Dihydro-2-hydroxyquinoxaline
Liu Kuaizhi, Huang Renhe, Li Qiurong
1989, 10(9): 959-961.
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In Methanol-Britton Robinson buffer solution, 3, 4-dihydro-2-hydroxyquinoxaline showed a definite anodic peak at +0.48 V (vs Ag-AgCl electrode) when a glassy carbon electrode was used as the work electrode.The linear relationship between the peak height and the concentration of 3,4-dihy-dro-2-hydroxyquinoxaline was obtained over the range of 2.8×10
-6
～8.0×10
-5
mol/L.The peak potential decreased with decreasing the acidity of the solution.It is proved that the electrode reaction is irreversible.This paper also reports the determination of 3,4-dihydro-2-hydroxyquinoxaline in the intermediate product 2-hydroxyquinoxaline.
Determination of Trace Silver by Catalytic Method with CN Ion Selective Electrode
Yang Shuxun, Ma Wanhong
1989, 10(9): 962-964.
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This paper reports a catalytic method for determing silver (I), using CN-ion selective clectrode which is based on the reaction between potassium ferrocyanide and water with silver(I) ion catalyst and a,a'-bipyridyl as the activator.Taking a fixed time procedure, the potential difference of catalytic and noncatalytic reaction is linearly related to the concentration of silver (I) ion in the range of 2.5×10
-9
～8.0× 10
-8
mol/L.Using the proposed method, we determined the mount of sisver in four standard samples of silicate with satisfactory result.The reaction mechanism is as discussed.
Synthesis and Properties of 10,9-Boroxarophenanthrene Chelates with Intramolecular Nitrogen-Boron Coordinate Bond
Shan Zixing, Zhao Dejie, Wu Feiyue, Zhang Guomin
1989, 10(9): 965-967.
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The reaction of 10-hydroxy-10,9-boroxarophenanthrene with aliphatic β-amino alcohols, substituted 8-hydroxy-quinolines and quinaldic acid affords seven title compounds.The coordination structure of them was demonstrated by IRand
1
H NMRspectra.
Effect of Heat-Treatment on Adsorption of Water Vapor of Hydrophobic Silica Gels
Shen Zhong, Shao Changsheng, Chen Lite, Pu Huiling, Xu Qiuhua
1989, 10(9): 968-970.
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In the present investigation, two samples of hydrophobic silica gel have been prepared, and heated at different temperatures up to 600 or 800 ℃.The water vapor adsorption isotherms, adsorption amount of methylene blue and the TG-DTAcurves were determined.Some conclusions were obtained as follows: (1) In water vapor adsorption, only "free" hydroxyls on silica gel surface interact with water molecules; (2) When temperature is raised to 500 ℃, the methylated surface of hydrophobic silica gel is destroyed partly, and completely destroyed at 600 ℃; (3) The heat stability of silica gel treated with trimethyl-chlorosilane is greater than that treated with dimethyldichlorosilane.
A Calculation Diagram of Standard Addition Applicable to Different Electrode Slopes in Ion-Selective Electrode Analysis
Luo Dengbai
1989, 10(9): 971-972.
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Aquantitative equation of standard addition has been described as(1+V
s
/V
x
)×10
Ape
=(1+C
s
V
s
/C
x
V
x
) According to this equation, a diagram expressing the relationship between △pe and V
s
has distinct advantages in comparison with Gran Plot and other reported methods, the former does not cause errors in the result treatment when non-standard slope electrodes are used.
X-Ray Structural Analysis of Norhendosin
Wang Qiguang, Meng Xianjun, Chen Yaozu
1989, 10(9): 973-975.
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Norhendosin, C
28
H
38
O
10
, colourless parallelepiped, orthorhombic system, space group P2
1
2
1
2
1
with cell dimension a=11.144 (2).b= 14.333(3), c= 17.146(3) Å, Z=4, are studied by X-ray analysis.The result shows that the skeleton of the compound is spirolactonekaurene type diterpene and the crystallographic data has not been reported previously.
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