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中文
Table of Content
24 June 1985, Volume 6 Issue 6
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Articles
The Studies of Three Organic Salts of Hexachloroceric Acid
Zhao Jizhou, Lu Yiqiang
1985, 6(6): 473-478.
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Adding the alcoholic solution of the organic bases directly into the alcoholic solution of hexachloroceric acid and leading dry HCl into the mixture, three new snlts of hexachloroceric acid, 2, 6-dimethyl-r-pyrone oxonium hexachlorocerate,imida-zolium hexachlorocerate, pyrrolidinium hexachlorocerate, were prepared. By elementary analysis method, the formulas of these compounds were determined as follows. (C
7
H
8
O
2
H)
2
CeCl
6
, (C
3
H
4
N
2
H)
2
CeCl
6
and (C
4
H
9
NH)
4
CeCl
8
. The physical and chemical properties of these new compounds were studied with IR, UV, X-ray diffraction, differential thermal analysis, thermogravity and conductivity method.
Thermodynamic Studies of Extraction(Ⅰ) --PMBP-DPSO-Er (ClO
4
)
3
-C
6
H
5
CH
3
Systems
Chen Jinbang, Peng Lie, Liang Liyuan
1985, 6(6): 479-483.
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The extraction of Europium (Ⅲ) from perchloric acid solution with mixtures of l-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (PMBPor HA) and diphenyl sulfoxide (DPSOor B) in toluene has been investigated.The formulas of the extracted species have been shown to be ErA
3
·HA, ErA
3
·Band ErA
3
·2B. Their extraction equilibrium constants and thermodynamic parameters of the enthalpy change (ΔH) Gibbs free energy change (ΔG) and entropy change (ΔS) have been calculated at 298.2K.
Study of pH-Potentiometric Method Determination of Stability Constants of Complexes --A New Method of Treatment of Experimental Data
Guan Luxiong, Chen Keying
1985, 6(6): 484-486.
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An improved method for the determination of the stability constants of complexes has been presented by combining the principles of pH-potentiometric method and the method of simultaneous measurement of pH-pMvalues. Only pHvalues have to be measured during the titration, but the volumes of the titrant added be recorded. The method has been applied to complex system Cd(Ⅱ)-Citric acid at 25±0.5℃ and the ionic strength 1.0. The results arc practically consistent with the values obtained by previous works.
The Principle of Compressed Mapping of Double Standard Addition Method in Ion-Selective Electrode Potentiometry
Wan Jirong, Zhang Maosen, Wu Haibin
1985, 6(6): 487-492.
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The principle of a double standard addition method is strictly demonstrated. Four lemmas and two theorems are given and proved. On the basis of them, two simple and rapid algorithms and programs are recommended. Some results of computation are listed to show the accuracy of the two algorithms furthem.
The Frontier Orbital Energy Level and Spectra of Some Unsymmetrical Bisazo Derivatives of ChromotropicAcid Containing Halogen Groups
Chen Qiong, Luo Mingdao, Cai Ruxiu, Chen Shukang, Lin Zhixin
1985, 6(6): 493-498.
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In the paper the Π electron molecular orbital energy level and electron spectra of some unsymme-trical bisazo derivatives of chromotropic acid containing halogen group are studied with HMOmethod. The results of calculation show that the maximum peak value is about smaller 8 nm than the experimental value. The substituting position of electrophilic group accord with experimental value. According to these results the red shift of electron spectra and the substituting position of electrophilic group are discussed.
Determination of Trace Molybdenum Using 2nd Order Derivative Convolution Voltammetry of Catalytic Wave
Cai Pcixiang, Mo Jinyuan, Liang Hongjian
1985, 6(6): 499-501.
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Ahighly sensitive method has been described for the determination of the trace molybdenum by the 2nd order derivative convolution voltammetry to determination of catalytic current in molybdenum-sulfur acid-mandelic acid-chlorate, in which the 2nd order derivative convolution, e', of the catalytic current,i, is measured as a function of electrode potential at a thin mercury film glass carbon electrode formed in situ. The peak height is directly proportional 10 the concentration of the molybdenum at the range of 10
-12
-10
-8
M. Samples of sea water, river water, well water and tapwater etc. can be determined directly without need of collection and separation.
A Modified Matrix Approach to Multicomponent Spectroscopic Analysis
Yin Longbiao, Liu Yiying
1985, 6(6): 502-504.
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Amodified matrix approach to multicomponent spectroscopic analysis has been described. This matrix is used for simultaneous determination of Aspirin, Phenacetin, and Caffeine with the ultraviolet spectrophotometry. Calibration with standard mixtures incorporates molecular interactions and nonzero intercept in the analysis matrix. This method, the Linear Programming, and the Coordinate Rotation are compared and discussed.
NMR Study of β-(3 -Methyl- 2, 4 -Dioxocyclohexyl) Propionic Acid and Its Derivatives
Zhao Chengzhi, Ren Zhongjiao, Li Ying, Huang Huamin
1985, 6(6): 505-508.
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13
Cand
1
H NMRspectra of five congeners of β-(3-methyl-2,4-dioxocyc-lohexyl) propionic acid were determined in this work. Ketone-enol tautomerism was observed. The structures of these compounds were discussed.
Synthesis and Some Properties of Co(Ⅱ) Meso-Nitrooctaethylporphyrins
Gong Liangchu, Zhang Taisen
1985, 6(6): 509-512.
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The synthesis of four types of Co (Ⅱ) meso-nitrooctaethylporphyrins are described; the data of their electronic absorption spectra, half wave potentials of redox and equillibrium constants of axial coordination with several ligands are reported. The more meso-nitro grouos the porphyrin has, the stronger the coordinating ability of the central cobalt ion achieves except with Ps, which shows some steric effect. The half wave potentials of both oxidation and reduction are increased by electron withdrawing nitro groups. The cyclic voltammograms of these porphyrins show quasi reversible processes for oxidation and first ring reduction, only the latter being a two electron process.
Synthesis and Propertion of Polysubstitution Pyrrole
Li Bao, Zhang Shuwpn
1985, 6(6): 513-514.
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Acetylacetones were treated by m-nitro-ω-bromoacetophenones to give l-(m-nitrophenyl) -3-acetyl-1, 4-pentandiketone(1). 9 new 1-aryl-2-methyl-3-acetyl-5-(m-nitrophenyl)pyrroles (2)-(10) have been synthesized by reaction of (1)with various primary amines. Semicarbazoncs were prepared from (2)-(10).Compounds(1)-(10) and the Semicarbazoncs were reported for the first time.
Synthesis of 4,4'-Biphenylenediphosphine and Related Compounds
Liu Shutang, U. Honrath
1985, 6(6): 515-517.
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The 4,4'-biphcnylenediphosphine H
3
PC
6
H
4
-C
6
H
4
PH
2
as well as p, p,p',p'-tclrakis (diethylamino)-4,4'-biphenylenddiphosphine (Et
2
N)
2
PC
6
H
4
-C
6
H
4
P(NEt
2
)
2
and p,p,p',p'-tetrachloro-4,4'-biphenylenediphosphine Cl
2
PC
6
H
4
-C
6
H
4
PCl
2
have been prepared firstly. Their molecular formulae and structures were deduced from their IR, NMRspectroscopic data and elemental analysis.
A New Synthetic Route for β-(3,4-Diaminophenyl)-Alanine Dihydrochloride
Ken Youda, Yuan Yunchcng, Yang Conggui, Zhang Yucying
1985, 6(6): 518-520.
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Anew synthetic route for β-(3,4-diaminophenyl)-alaninc dihydrochloride by using P-nitrobenzaldehydc and N-benzoylglycine as starting substrates is reported. Some of the intermediates in this route are new compounds.Our method,compared with that of V.G.Pesin ct al.[1], has the advantages that the starting substrates are easily available, the reacting conditions are moderate and the operations are simple.
Researches on the Complex Reactions of Dithioacetylacetone with Some Metal Ions
Huang Jianquan, Huang Jinling, Zhuang Honghui, Lin Xianti, Wu Dingming, Shang Maoyu, Zheng Jianji
1985, 6(6): 521-526.
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This paper reports the research on the reactions of a variety of metal ions with dithioacetylacetone in a ethanol medium saturated with HCl The products of the reactions have been characterized by X-ray crystal structure analysis.The result shows that the complex types formed for different metal ions can be classified into three categories which are in coincidence with the division of metal ions according to their Z
2
/r as a function of (x
s
+ X
M
/(X
s
- X
M
). In addition,it is found that among the ions used in the examination,the molybdenum is the only one element capable to form the cluster compound under such a specific reaction condition.
A Study of the Theory of Ligand Field for the Rare Earth Compounds --The Transformation of SO(3)-D
n
Wang Zhexin, Tang Auchin
1985, 6(6): 527-533.
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A few rare earth compounds have the structure of point group Dn symmetry. The link-up of the group chain from SO(3)to D
n
is a matter of importance. In this paper, theoretical method of the Ligand Field theory proposed by Tang and his coworkers is used as a startling point. The transformation propety of SO(3)-D
n
, is discussed. The concept of the characteristic Mof the irreducible representation of Dn is introduced. The phase factors [-1]
Γ
, [-1]
γ
the V-coefficients, the symmetrized [Γ
2
] and anisymmetrized (Γ
2
) squares of irreducible representation, factors(-1)
Γ
, θ(Γ
M
Γ
M
Γ
M
) for D
n
and S
mFr
i
parameter of SO(3)-D
n
are given.
A Study on the Behaviors of Terbium (Ⅳ) Oxide Hydrate in Various Acid Solution (Ⅰ) --In HCI, HNO
3
, HClO
4
and HAc Solutions
Liu Jianmin, Ma Tairu, Yang Rudong, Li Tougshuang
1985, 6(6): 534-538.
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In this paper we have studied the existing state of terbium (Ⅳ) oxide hydrate in HCl, HNO
3
, HClO
4
and HAc solutions. Through the investigations of the optical and electrical properties and coagulation values it is showed that the Terbium (Ⅳ) oxide hydrate exists as a sol with positive charges in these solutions. The UVand visible absorption spectra and kinetics of reduction of the sols have also been studied.
Optimal Scheme of Fm(z) Integral Sequence Calculations in ab initio Method --Combination of Upward with Downward Recurrence Method
Liao Muzhen, Wu Guoshi, Chen Kaixian, Liu Honglin, Chen Nianyi
1985, 6(6): 539-543.
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In this paper the quantitative rules of error transfer and change of Gaussian integral function Fm(z) sequence calculation by recurrence formula in ab initio method are expounded. The optimal scheme of Fm(z) integral sequence calculations by conbination of upward with downward recurrence is proposed. This method assures that the absolute derivations only decrease without increasing in recurrence process, and hence the subsidiary precision prescrible is not need for the recurrence founda-tional term. As a result it can be applied to improvement of the exsitent serious Fm(z) computer programs. Combination of this method with Schaad's formula being used to p,d,f type Gaussian function calculations, the additive operation and the multiplication and exponential operation decrease by above 40% and above 60% specifically.
Studies on Synthesis, Structure and Properties of a Model Compound of “J” System Chemistry of Active Center of Nitrogenase
Zhang Zhigui, Wang Fengshan, Lin Yongqi, Fan Ynguo
1985, 6(6): 544-548.
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The crystal of [(C
2
H
5
)
4
N]
3
{[(SCH
2
CH
2
S)MoSs]
2
Fe} was obtained by the reaction of [(C
2
H
5
)
4
N]
2
MoS
4
, FeCls and ethane-1, 2-dithiol in MeOH-MeONa. The crystal structure of the compound was measured by X-ray.The crystal belongs to the monoclinic system, it crystallizes in space group Cc with a =14.0030Å, b=18.3970Å, c=17.5705Å, β = 96.458°, V=4497.6Å
3
and z = 4. The structure was refined by least-squares. The value of Rwas 0.052. The compound possesses activity of acetylene reduction with KBH
4
as reductant, it displays good activity of acetylene reduction with reconstitution of uw45. The characters of IRuv-visible,
1
H NMR, EPR, Mossbauer spectra and magnetic susceptibility of the compound have been investigated.
Kinetics of the Catalyzed Polymerization for Concentrated Aqueous Solution of Formaldehyde
Liu Xinpeng, Liu Yuming, Xia Shaowu
1985, 6(6): 549-551.
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The kinetics of polymerization for concontratcd aqueous solutions of formaldehyde catalyzed by tin tctrachloride has been investigated. It is demonstrated that the reaction is a first order reaction both for the monomer and the calalyst. Its total activation energy is -2.1 Kcal/moic.It can be concluded that the polymerization of formaldehyde in the aqueous solutions is a reaction of ionic polymerization, which is catalyzed by Lewis acid produced in the presence of tin telrachloride; a reaction mechanism is suggested, and the rate equation Y
M
= k[C][M] in good agreement with the experimental results is derived.
Coil Properties of Ring Shaped Polymer Chains in Good Solvent --Theoretical Calculation and Experimental Determination of r
dgu·ring
-r
ctu·open
and f
ring
-f
open
Huang Jiaxian, Li Chunrong, Wang Linfu, He Binglin
1985, 6(6): 552-556.
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Two correlation equation r
epu
·r
ing
/r
epu·opcn
= 1/([η])
opcn
/[η]
ring
)
3
and f
ring
/f
opcn
=1/([η])
opce
/[V]
ring
)
1
/3 of the ring shaped and linear shaped polymercoils with both same monomer and molecular weight in dilute solution have been derived. When there isn't excluded volume effect, r
equ. ring
/r
equ.opcn
=f
ring
/f
opcn
=2-
1/3
≈ 0.7937 and 〈S
2
〉
ring
/〈S
2
〉
open
= (2-
1/3
)
2
≈0.63.
The Study of Porous Silica Gel for Aqueous Size Exclusion Ghromatographic Use
Wang Qinwei, Duan Xiaoqing, Jing Zhicheng, Ha Huirong
1985, 6(6): 557-561.
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The preparation of a silica-based packing for the aqueous size Exclusion Chro-matography (SEC) is described. The process involved the hydrogen-bonding of a coupling reagent with the silica gel surface followed by ring-openning reactions of the epoxy groups on the coupling reagent molecules by polyethylene glycols. The results show that this modified packing can be used for the SECanalysis of polyvinyl acetate, gelatins, proteins and dextran systems.
The Structral Effect of Electron Donors on the Photo-Polymerization of Acrylonitrile
Cao Weixiao, Han Ping, He Xia, Feng Xinde
1985, 6(6): 562-564.
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The photopolymerization of acrylonitrile (AN) using the triphenyl compounds of N, P, As, Sb, Bi elements (represented as (C
6
H
5
)
3
D) and the diphenyl compounds of O, Selements (represented as (C
6
H
5
)
2
D) as initiators and some relationship between the centre atom Dof the donor compounds and their situations in the periodic table were suggested.
Empirical Correlations Between intrinsic Viscosity and Number-Average Molecular Weight for Aqueous Solution of PSSHMA
Chen Zhusheng, Go Haiqing, He Yuankang, Chen Weiying
1985, 6(6): 565-567.
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The sodium salt of poly-6-sulfohexyl methacrylate (PSSHMA) has been synthesized. In 0.15M NaCl,refractionation and triangle fractionation by precipitation from a solvent-nonsolvent mixture was carried out by adding alcohol to a dilute aqueous solution of the PSSHMA. M
n
and [η] were measured by means of osmometry and viscometry. Empirical correlation between intrinsic viscosity and molecular weight was obtained as follows [η] =3.06×10
-3
M
n
0.82.
The reasonable conditions of measurement of osmometry and viscometry were also discussed.
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