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Table of Content
24 May 1988, Volume 9 Issue 5
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Articles
An Investigation on the Phase Diagram of Ternary System NdCl
3
-BaCl
2
-NaCl
Zheng Chaogui, Ye Yupu
1988, 9(5): 423-426.
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The phase diagram of ternary system NdCl
3
-BaCl
2
-NaCl was investigated by means of DTAand X-ray diffraction analysis. It was found that there are 5 surfaces corresponding to the primary crystallization of NdCl
3
,α-BaCl
2
,β-BaCl
2
, NaCl and Ba3NdCl9 respectively, and 6 univariant lines related to the secondary crystallization in this system. The temperature of the ternary eutectic, composed of 74.0wt%NdCl
3
, 24.4wt%NaCl, 1.6wt% BaCl
2
, was determined to be 430℃. The temperature of the ternary peritectic, composed of 57.0wt. %NdCl
3
, 23.9wt% NaCl,19.1wt%BaCl
2
, was observed to be 508℃. Acompound, formed in the solid state, is found, and decomposed occurs at 420℃.
Preface
The Synthesis, Spectra and Magnetic Properties of Dibenzoyl-Bis-(Thiosemicarbazone)Copper(Ⅱ)
Bai Lingjun, Huang Ling, Wang Genglin
1988, 9(5): 427-431.
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Dibenzoyl-bis-(thiosemicarbazone) C
16
H
16
N
6
S
2
and a complex with copper(Ⅱ) Cu(C
16
H
14
NaS
2
), were synthesized. The measurements of elemental analysis,electrical conductivity, 1Rspectra, electronic spectra, ESRspectra and magnetic susceptibility curve with temperatures (1.5~300°K) were carried out. The magnetic susceptibility data fit the modified Bleaney-Bowers dimer equation yielding J = -2.88cm
-1
and g = 2.07. The coordinated bond of the complex is strongly covalent bond and α
2
=0.64, P
N
= 0.114, which have been suggested from ESRspectra.
Articles
Synthesis and Crystal Structure of Tri-(O,O' -Diethyldithiophosphato) Cobalt(Ⅲ)
Xu Zheng, Yu Yunpeng, Lin Jianhua, Xu lie, You Xiaozeng, Lin Chichang, Liu Shixiong
1988, 9(5): 432-437.
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Oxidation process of CoC(C
2
H
5
O)
2
PS
2
]
2
was studied by UV-Vis method to get the title compound. The rate of oxidation reaction is very slow and seems depending on alkyl group in the ligand molecule. The oxidation product CoC(C
2
H
5
O)
2
PS
2
]
3
·1/2 H
2
Owas characterized by UV-Vis, MS, TG-DTand PES.The crystal of CoC(C
2
H
5
O)
2
PS
2
]
3
· 1/2 H
2
O belongs to Iriclinic, space group P1, parameters of unit cell are:α= 8.805(1)Å, b=9.812(2)Å, c = 14.271(2)Å, α = 89.46(2)°, β=89.42(1)°, γ=86.95(2)°, F=1370.9Å
3
, Z=2, D
c
= 1.509g·cm
-3
, F(000) = 645e, final R= 0.080 for 4279 reflections with I≥3σ(Ⅰ) bond lengths of Co-Sare 2.319 + 0.004Å. Bond angles of cobalt atom and two sulphur atoms in the same dithiophosphate group are 85.07~85.35°. Bond angles of cobalt atom and any two neighbour sulphur atoms which are not in same dithiophosphate group are 89.35 - 95.35 °.There have three oxygen atoms of crystal water with 1/6 possibility for each in unsymmetry unit. Nonbonding distances between these oxygen and sulphur atoms are 2.12~2,27Å, which are much less than the sum of the van der Waals radii. It shows that some kinds of hydrogen bonds such as O—H...S are present.
Investigations on Oscillopolarographic Titrations(XXXⅦ)——Principle of Oscillopolarographic Titrations at Two Micro Pt-Electrodes
Yang Zhaoliang, Gao Hong(H. Kao)
1988, 9(5): 438-443.
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The symmetrical incisions occurring on oscillopolarograms obtained at two polarized micro Pt-electrodes when EDTAis present in solutions are not due to redox reaction of EDTAat Pt-electrodes. They mainly come from the adsorption of EDTAat Pt-electrodes which hinders the formation of an oxygen layer at Pt-electrodes. EDTAchanges the E
i
~t curve of each Pt-electrode by shifting the upper left part of the curve to right and lower left part to left. The E~t curve obtained at two polarized micro Pt-electrodes is the superposition of E
a
~t and-E
b
~t EDTAshift gives sharp time lags on the final E~t curve and sharp incisions on dE/dt~E curve.
Studies on Electrochemical Methods of Controlled Convolution(Ⅰ)——Simple Electron Transfer Reactions
Xie Naixian, Huang Yixiang
1988, 9(5): 444-449.
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Three kinds of controlled convolution experimenlal methods, constant sc-mi-integral (CSI), linear semi-integral svveep(LSIS) and linear semi-differential sweep (LSDS), have been developed.
Studies on C-glycosides (Ⅳ)——The Reactions of 1-α-Chloro-,1-α-Bromo-,1-α-lodo-,and 1-α-Tosyloxy-2,3,4,6,-tetra-O-benzoyl-D-gluco-pyranose with Substituted Phenylmagnesium Bromides
Cai Mengshen, Dong Lingjiao, Gao Yigong
1988, 9(5): 450-455.
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Acyl glucopyranosyl halides with different leaving groups attached to C-1, including-OTs, reacted with aryl magnesium bromides in ether or THFto give C-glycosides in 30-80% yield. Acetyl glucopyranosyl halides gave better yields than benzoyl derivatives. The reaction products were affected by the solvent used in the reaction, thus THFfavored the formation of C-2 aryl substituted by-product and lowered the yield of C-glucosides. The ratio of the anomers formed in the reaction mixture was affected by the activity of different leaving groups. More α-anomer was obtained from glucopyranosyl halides with leaving group of higher activity. More β-anomer was formed from Grignard reagents with higher nucleophilicity, but more a-anomer from Grignard reagents with higher steric hindrance. The ratio of theα- and β-anomers in C-glucoside mixtures was calculated from the areas of
1
HNMR peaks.
Syntheses and Properties of Some New Spirochelate 1,3,2-Benzodihetero (S,O) Borole 2-β-Diketonates
Shan Zixing, Zhao Dejie, Huang Guoping, Zhang Guomin, Tan Zhongjia, Wu Xuanjie
1988, 9(5): 456-460.
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Aseries of 1,3,2-benzodihetero (S,O) borole 2-β-diketonates have been synthesized by reacting 2-chloro-5-methy-1,3,2-benzodithioborole or 2-chloro-1,3,2-benzodioxaborole with β-diketones (acetylacetone, acetoacetylferrocene, benzoylacetone, and dibenzoylmethane). Five of them are reported for the first time. All these compounds are colourful solids and the stability of benzodithio-borole derivatives is less than that of benzodioxaborole derivatives. The IRand
1
H NMR data indicate that they have similar chelate structure and the framework π electrons of β-diketones are extensively delocalized in these molecules.
The Use of TTT Active Amide Method in Solid-phase Peptide Synthesis——The Synthesis of the Growth Hormone Releasing Peptide and Its Biological Activity
Xue Chubiao, Li Chongxi, Xing Qiyi, Dong Minghui
1988, 9(5): 461-465.
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The use of tetrahydrothiazole-2-thione (TTT) active amide method in solid-phase peptide synthesis has been studied through the synthesis of the growth hormone releasing peptide using chloromethylated copoly (styrene-2% divinylben-zene) resin as polymeric support. It was found that the coupling reaction was fast, the yield in each coupling step was nearly quantitative, and the purity of the final crude peptide was satisfactory. The biological activity of the synthetic peptide is also presented.
Studies on Organosilicon Compounds with Biological Activity(Ⅷ)——Synthesis of 1-Alkylsilatranes and Study of Antitumour
Wang Jitao, Xie Qinglan, Liao Renan, Li Jing, Li Baoyuan, Wang Shixian
1988, 9(5): 466-469.
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l-Alkylacyloxy-2,8,9-trioxa-5-aza-l-silatricyclo[3,3, 3, 0
1,5
] undecanes (1-alkylacyloxysilatranes) were synthesized by the reaction of 1-brornosilatrane with organic acids. Compare with the method using 1-ethoxysilatrane reagent, this reaction gave higher yields and simpler process of treatment. The influence of reaction conditions was discussed. The
1
H NMRand 1Rof the title compounds were determined.The antitumour activity of some acyloxysilatranes was studied, one of them had good curative effects on Ehrlich cancer.
The Study of Synergism of Acid and Base Centers in Catalytic Dehydration for Propanol-[2]
Qian Zaihu, Tang Qun, Chui Shengfan, Wen Lingsheng
1988, 9(5): 470-474.
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Based on the experimental results of IRdetection of the absorbed species and effect of acid-base strength on the catalytic properties,it is shown that the activity and selectivity for catalytic dehydration of propanol-[2] are high at an appropriate acid, and basic strength and a H
0,max
value. The existance of an adsorbed species (-CH
2
) on catalyst surface verified by IRmeasurement, means that the reaction takes place by interactions between OHgroups of propanol-[2] and acid centers of the given catalyst surface and between Hgroups ofβ-Cin the reactant and base centers of catalyst.It is possible that the acid-base center synergism enables the given reaction to taske place.
Surface Acidic and Catalytic Properties of H(M=Al, Ga, Fe)ZSM-5 Zeolite
Jiang Dazhen, Xiao Fengshou, Liu Ziyang, Xu Ruren
1988, 9(5): 475-478.
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The surface acidities and catalytic activities of some trivalent heteroatom-containing H(M)ZSM-5 (M=A1, Ga, Fe) zeolite have been studied by means of TPD, IRand cracking of n-pentadecane.The results indicate that Bronsted and Lewis acidic sites are present in these zeolites but the C
L
/C
B
on the surfaces of H(Ga)ZSM-5 and H(Fe)ZSM-5 are more higher than that on the surface of H(Aj)ZSM-5. Besides, there exist in the order of the acidic strength H(Al)ZSM-5>H(Ga)ZSM-5>H(Fe)ZSM-5. Cracking activities have been found to be dependent on the heteroatom in the framework of the zeolite. The normalized activity and the selectivity of gas-oil increase in the order as H(Ga)ZSM-5>H(Al)ZSM-5>H(Fe)ZSM-5. These results suggest that the Lewis acidic site play an important part in the cracking of n-pentadecane.
Energy Level Structure of KTbP
4
O
12
and Ligand Field Theoretical Calculation
Kan Qiubin, Bai Yubai, Zhao Yongnian, Li Tiejin, Hou Weixing
1988, 9(5): 479-483.
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In the present work, the fluorescence spectra of single crystal of KTbP
4
O
12
have been measured at 77K. Most of the observed transitions were identified and the energy level structure of the
7
F multiplet was also defined. The coordination of Tb
3+
ion by oxygen atoms is eight-fold with the geometry of a slightly distorted square antiprism. In other words, the local symmetry of Tb
3+
ion in KTbP
4
O
12
belongs to C
4v
. There is the same symmetry of Tb
3+
ion in TbP
5
O
14
. So the symbols of Stark energy levels are of the same as in TbP
5
O
14
. The ligand field calculation was performed for such symmetry and gave a respectab-le to fit the observed Stark splitting of
7
F
J
(J = 0~6) multiplet.The comparison between the experimental and the calculated energy level shows that the RMSdeviation and the maximum deviation are 10cm
-1
and 24cm
-1
, respectively.
Crystal and Molecular Structure of Dibenzoyl-Bis-(Thiosemicarbazone) Copper(Ⅱ)
Yao Xinkan, Wang Honggen. Wang Ruji, Huang Ling, Wang Genglin
1988, 9(5): 484-487.
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The complexes of some transition metals coordinated with Nand Satoms of Schiff bases have been show to be effective as anticancers. Of all them, the kind of bis- (thiosemicarbazone) copper ( Ⅱ) is the best one. The crystal and molecular structure of dibenzoyl-bis- (thiosemicarbazone) copper (Ⅱ) (CuL) has been determined. Its crystal data are triclinic, space group P1 a = 8.9491(7), b = 9.595(1), c= 10.882(1)Å; α = 99.42(1)°, β = 106.19(1)°, γ=92.43(1)°; Z=2, D= 1.582 g/cm
3
; R=0.025.Cu (Ⅱ) is coordinated by N
11
, N
21
, S
1
, S
2
atoms of the ligand, giving rise to a distorted planar square coordination. It can be found from the bond angle data that there is some tension here. Probably the LFSEof Cu (Ⅱ) (d
9
) can make compensation for it. Two benzene rings are nearly normal to this planar section. The structure of Cu-KTShas been discribed as containing chains of coppeffr(Ⅱ) with axial Cu-Sbonding tendency, but there are no chains in the structure of CuLowing to the existence of benzene rings.Then, it would be helpful to the understanding of the biological function of these compounds for us whe ther CuLhas the anticancer activity like Cu-KTS.
Studies on Molecular Motion of Star-shaped Polystyrenes in Solution by Carbon-13 NMR(Ⅱ)
Wang Jian, Hua Shiying, Qiu Zuwen, Shen Jiacong
1988, 9(5): 488-492.
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The carbon-13 relaxation parameters were measured for star-shaped polystyrenes with different branch degree and different molecular weight of parent chain in a 20% (W/V) solution. The backbone segmental motion is interpreted in terms of the lg-X
2
, Cole-Cole and a conformational jump model. The internal rotation motion of aromatic ring is analysed and the activation energies and jump rates are obtained. The results show that light chemical crosslinks has, to some extent, an influence on the distribution of correlation time, but no distinct effect on the potential for segmental motion. The dependence of carbon-13 relaxation on the molecular weight is similar to that of linear polymers.
Studies on the Retention Mechanism for Ester-Containing Porous Polymer Beads as Stationary Phase
Zuo Yumin, Xie Mengxia, Yang Zhiqiang, Qi Mei, Yang Xuejin
1988, 9(5): 493-498.
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The dependence of the logarithms of the specific retention volumes for C
5
—C
8
alkanes and McReynolds standard compounds on the reciprocal temperature was investigated for two types of ester-containing polymer beads as stationary phase. Within the temperature ranges investigated the dependence is linear. Hence it could be assumed that the retention mechanism would not be with abrupt change.The calibration curves for water and methanol are linear, but the extrapolation to zero point yields a positive intercept which is attributed to the adsorption on the stationary phase.The hydrogen exchange between methanol -D
4
and D
2
O on polymer beads was found by GC.Based on the relationship between the specific retention volume and specific surface area shown below V
g
= K
i
σ+ K
1
where K
i
and K
1
represent the adsorption coefficient and partition coefficient, respectively, it was shown that adsorption on the surface of beads is the decisive factor determining the retention value, at least for our polymers.
Syntheses and Properties of Triblock Copolymers with Poly-α-methylstyrene as Hard Blocks
Li Youxin, Jiang Shuojian, Feng Xinde
1988, 9(5): 499-503.
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Triblock copolymers with polya-methylstyrene as hard blocks and with poly-butadiene and hydrogenated polybutadiene as soft blocks were synthesized,and their polymerization processes, structures and properties were studied. Although these two kinds of triblock copolymers exhibited the similar T
gs
(both about-25℃) of their soft blocks, the tensile strength and elongation of break, resilience and T
g
of the hard blocks of PaMS-HPBD-PaMSall are lower evidently than those of PaMS-PBD-PaMS. The reason is that the solubility parameter of HPBDis higher than that of PBD,so the solubility of HPBDin PaMSis higher than that of PBD. The dynamical properties" of PaMS-PBD-PaMSare better than those of ABCtriblock copolymer of PaMS-PBD-PPVL, because it is incompatible between crystalline PPVL and radom PaMS blocks.
A Study of Syntheses and Properties of Ethylxanthate and Pyridine Base Complexes of Nickel and Zinc
Zhang Wenzhao, Dai Huan, Yu Baoyuan, Zhang Lingsen
1988, 9(5): 504-507.
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The mixed complexes of three nickel and two zinc xanthates with pyridine bases were synthesized and characterized by infrared spectra,thermogravimetric(TG), bifferential thermal analyses (DTA), electronic spectra and magnetic susceptibilities. The relationship between their structures and properties are also studied. The thermal stabilities of nickel (or zinc) complexes are in the order. Ni(Exan)
2
·2γ-pic>Ni(Exan)
2
·2Py>Ni(Exan)
2
·2P3a
Infrared Studies of the Frameworks on ZSM-5 and ZSM-11 Zeolites with Different Ratios of Si/Al
Xu Qinhua, Yu Qiuming
1988, 9(5): 508-509.
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The frameworks on ZSM-5 and ZSM-11 zeolites with different ratios of Si/Al were studied by means of IRmethod. The internal tetrahedral asymmetrical stretch vibration frequencies of ZSM-5 and ZSM-ll increased linearly with the increasing of SiO
2
/Al
2
O
3
ratios. SiO
2
/Al
2
O
3
ratios obtained by IRmethod rather agreed with those obtained by chemical analytic method.
The Preparation and Its Analytical Performance of the CPA-Ⅲ Chelate-forming Resin
Zhang Kai, Yang Yu, Wang Duoxi
1988, 9(5): 510-512.
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This paper reports the preparation of the CPA-Ⅲ Chelate-forming resin, its analytical performance towards rare-earth elements, such as the effect of pHon the adsorption of CPA-Ⅲ onto D
290
resin, the exchange capacity of D
290
resin, the adsorption capacity of CPA-Ⅲ chelate-forming resin for Ce, the stability of CPA-Ⅲ resin in different mediums etc, and the law of synthesizing well-behaved chelateforming resin.
A Theoretical Study of Optimum Ligand Concentration Ratio in a Mixed Ligand Complex
Gao Zhisheng
1988, 9(5): 513-515.
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In a solution of a ternary mixed ligand complex, the distribution of metal complex species is greatly dependent on theconcentrations of two kinds of ligands. When the ligands are in excess, the optimum ligand concentration ratio for the formation of ternary complex MA
a
B
b
is given by,[A]
n
/[B]
m
=a β
MB
m
/(n-a)β
MA
n
.
Determination of Trace Copper in Natural Water by Fluororoetry
Zhang Luduan, Liu lianqing, Zhang Zhujun
1988, 9(5): 516-518.
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A new method based on fluorescence quenching for determination of trace copper is reported,8-anilino-1-naphthalenesulfoic acid(ANS) is an important fluorescence probe. It can combine with polyethyleneimine- and makes an increase of quantum efficiency of fluorescence. Copper combines with polyethyleneimine to form strong complex. ANScan be bound to cationic copper-polyethyleneimine polymer as an ion pair. On the polymer the paramagnetic copper ion causes fluorescence to be quenched. These reactions can be applied to determining the trace copper in natural water after separation and preconcentration by sulfhydryl cotton fiber. The detection limit is 4.7 ppb. The relative standard error is not higher than 2.0% for determination of copper in range of 5 to 100ppb.
Chemiluminescence Determination of Trace Molybdenum(Ⅵ) by H
2
O
2
-I
-
-Luminol System
Zhang Zhujun, Lu Jiuru, Zhang Xinrong, Liang Yarning
1988, 9(5): 519-521.
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A inderect chemiluminescence method for determination of trace Mo(Ⅵ) has been presented in this paper. The principle of the method is that the reaction of I
-
with H
2
O
2
is accelereted by Mo(Ⅵ) to produce I
2
, and I
2
oxidize luminol to produce chemiluminescence. The detection limit is 6×10
-10
g/cm
3
Mo. The linear arnge of the calibration cuvers is 1 × 10
-9
~1×10
-7
g/cm
3
Mo. The relative standard deviation is less than 6%. This method has been used for the .determination of trace Mo in the grains.
Studies on the Insect Sex Pheromones(Ⅴ)——The Synthesis of the Housefly Sex Attractant Z-9-Tricosene
Liu Tianlin, Li Zhengming, Wang Likun, Liang Ge
1988, 9(5): 522-524.
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Oleyl alcohol was used as a starting material and converted into oleyl tosylate with tosyl chloride and pyridine. By reduction of this tosylate with lithium aluminium hydride and then ozonization, the intermidiate 1-nonanal was obtained. (Z)-9-tricosene was (Z)-stereoselectively prepared by Wittig reaction of 1-nonanal with lithium salt-free phosphorus ylide generated from the reaction of n-tetradecyltriphenylphosphonium bromide and sodium bis(trimethylsilyl)amide.
The Synthesis of Bis(O,O-Diarylthiophosphoryl) Polysulfides
Chen Wanyi, Tian Mengchao
1988, 9(5): 525-528.
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In order to get new fungicidal compounds, seventeen bis(O,O-diarylthiophos-phoryl) polysulfides (Ⅰ) were synthesized.
The Calculation of the Interaction Between Insulin Molecules
Shao Jun, Wen Yuankai, Li Zhenmin
1988, 9(5): 529-530.
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On the basis of zero differential overlap and the monopole model, the interaction energies between two insulin molecules have been calculated when they get close each other. It is shown that the energy of the whole system decrease continually as two molecules approach at a definite direction. The energy decreases until the stable position is arrived, namely θ= 0°, d= -0.5Å. The calculated data are very similar to the position the crystal structure data present. If they are forced to close each other, the energy, especially the repulsive force will increase rapidly. The total interaction energy and its constitutes at different distance and orientation are analysed.
Theory of Gas-Phase Acidity (Ⅱ)——the Effect of the Strength of the Bond Linking the Hydrogen
Chen Zhixing
1988, 9(5): 531-533.
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CNDO/2 study of neutral and cationic HH, CH, NH, FH, SiH, PH, SH, and CIHacids shows that acidity relates to the strength of the bontl linking the acidic hydrogen as well as the charge of the hydrogen. Using diatomic contribution to energy as a measure of bond strength, we performed linearly regressions of depr'otonation energy with respect to hydrogen charge and the diatomic contribution to energy. The correlation is good in the case of cationic acids and worse in the, case of neutral acids.
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