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中文
Table of Content
24 December 1989, Volume 10 Issue 12
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Articles
Studies on Synthesis, Properties and Thermal Analysis of Complexes of Rare Earth Isothiocyanates with Dimethyl Sulfoxide
Sun Tongshan, Zhang Jianhua, Jiang Bengao, Yin Jingzhi
1989, 10(12): 1167-1172.
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Fifteen new solid complexes of rare earth isothiocyanates with dimethyl sulfoxide (DMSO) were synthesized and characterized by chemical analysis, IR and X-ray diffraction.Compositions of the complexes conform to the formula RE(NCS)
3
·mDMSO(RE=La, Ce, Pr, Nd, Sm, Eu, Gd, m=5, RE=Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, m=4).Thermal decompositions of the complexes were studied by TG-DTA-DTG.The values of activation energy and reaction order for the first steps of decomposition of the complexes were determined from TGcurves, using the Coats-Redfern method.The results show that the activation energy depends on the atomic number of lanthanoids, and "double peak phenomenon" is observed.
An Investigation on the Phase Diagram of Ternary System PrCl
3
-SrCl
2
-NaCl
Zheng Chaogui, Wang Xiaolin, Chai Liang, Qiao Zhiyu, Ye Yupu
1989, 10(12): 1173-1176.
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The phase diagram of ternary systerm PrCl
3
-SrCl
2
-NaCl has been investigated by means of DTAand X-ray diffraction analysis.It was found that there are 4 fields corresponding to the primary crystallization of PrCl
3
, SrCl
2
, NaCl and Sr
3
PrCl
9
respectively and 5 univarant lines related to the secondary crystallization in this system.The two reactions occured in this system are:(这里有图片19891202-1173-1.gif)Acompound, formed in the solid state,was found, and it decomposes at 440℃.
The Templating Effect During the Formation of ZSM-5 Type Molecular Sieve(Ⅱ)——The Study of the Templating Effect of Alcohol by High-Resolution Solid-State
23
Na-MAS-NMR Technique
Song Tianyou, Xu Ruren, Li Liyun, Ye Zhaohui
1989, 10(12): 1177-1179.
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On the basis of synthesizing ZSM-5 type zeolite with alcohol,the high-resolution solid-state
23
Na-MAS-NMRtechnique was used to investigate ZSM-5 type zeolite precursor,zeolite baked for 2 h at 600℃,and zeolite after baking and adsorbing water saturately.Analysing the chemical shift and the half-height width, the chemical enviroments of Na+ in the ZSM- 5 type zeolites prepared in alcohol and with direct method and the templating effect of alcohol during the formation of ZSM-5 type zeolite were discussed.
Studies on Voltammetric Adsorptive Wave of Gallium-Salicyl Fluorone Complex
Chen Rongli, Zhang Xiaoli, Wang Lizeng, Wang Shuren
1989, 10(12): 1180-1184.
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In a supporting solution containing 5.0× 10
6
mol/Lsalicyl fluorone, 0.2 mol/Lpotassium hydrogen phthalate- HCl, at pH=3.0, a sensitive adsorptive wave of gallium- salicyl fluorone complex was obtained by using linear scanning voltammetry.The peak potential is - 0.93 V(vs, SCE).The change of peak height with the concentration of gallium is linear in the range of 7.5× 10
-9
～3.8× 10
-7
mol/L.The electrode processes of the adsorptive wave of the complex may be presented as follows: 1.Complexing reaction in the bulk solution is Ga(Ⅲ)+H
4
L=GaH
3
L
2+
+H
+
2.GaH
3
L
2+
diffuses to the electrode surface and is adsorbed on it GaH
3
L
2+
=GaH
3
L
nds
2+
3.When Ep
(2)
=-0.93 V, the ligand and the center ion of the complex are simultaneously reduced GaH
3
L
2+
=GaH
3
L
nds
2+
+5e+3H
+
→Ga(Hg)+H
4
L
ads
Elimination of Interferences in ICP-AES by Flow Injection Gradient Technique-Generalized Standard Addition Method
Luo Jianbo, Zhang Zhanxia, Qian Haowen, Cai Mingxiang
1989, 10(12): 1185-1188.
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Amethod based on a flow injection gradient technique (FIGT) and generalized standard addition method GSAMis developed for the elimination of matrix and/or spectra interferences.Only one standard for an analyte is used to obtain the signals required for the evaluation in the GSAM.Operating parameters, including the carrier flow rates and residence times, are discussed in detail.To assess the proposed method, two synthetic samples, tow types of Cu alloys and steel were analysed for Zn, Mn and As respectively.The Relative Standard Deviations are in the range of 0.5～1.9%.
Studies on the Mechanism of the Polarographic Catalytic Wave of Chromium(Ⅵ) in the Buffer System of (o-Phen)-NaNO
2
-
NH
3
-NH
4
Cl
Han Jilin, Chen Hongyuan, Gao Hong
1989, 10(12): 1189-1193.
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Anew viewpoint elucidating the mechanism of a highly sensitive polarographic catalytic wave of Cr(Ⅵ) in the medium of 1,10-phenanthroline-nitrite-NH
3
-NH
4
Cl (pH 9.4) is presented.This wave is not a catalytic hydrogen wave, but a catalytic (EC-EC') reaction in which Cr(Ⅵ) is firstly reduced to Cr(Ⅲ), then it forms a multi-coordination compound A (as electroactive species) in the following chemical reaction.In the second step of the electrode reaction, the ligand NO
2
-
in the compound Ais reduced, then the product of Ais oxidized by NO
2
-
in solution to regenerate the starting material Aagain.The composition of the multi-coordination compound and the conditional formation constant for various ligands are determined.
Study on Selective Flow Injection Analysis of Palladium
Cai Yaqi, He Xingcun, Gong Haiping, Hu Zhide
1989, 10(12): 1194-1196.
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Anew flow injection analysis method was developed for the spectrophotometric determination of palladium.The system involved the measurement of the absorbances of palladium——(DBC-Chlorophosphonazo) complex at 620nm.The limit of detection for palladium is 0.10μg/mL.Sample solution could be analysed at rates of 62 h
-1
.The method was applied to determine palladium in anode mud and chloride residue with satisfactory results.
Addition Reaction of l,3,2-Benzodiazaphosphorin-4(1H)-one 2 Oxides with Alkene
Chen Ruyu, Bao Rong
1989, 10(12): 1197-1201.
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The addition reaction of 1, 3,2-benzodiazaphosphorin-4(1H)-one 2 oxides with(这里有图片19891208-1197-1.gif) has been studied.The structures of the eighteen new compounds synthesized have been confirmed by elemental analysis, IR,
1
H NMRand MS.The condition of the reaction and conformation of P-Cof products were discussed.It was found that when the mol ratio of sodium ethoide/ I was 1: 1, the ring of compound Iwould open and when the mol ratio was 1:5, the addition reaction with would take place.But, if sodium hydride of equal mol ratio to Iwas used as the catalyst, the addition reaction of compound I with(这里有图片19891208-1197-1.gif) would take place exclusively.
Studies on the Synthesis and Anticancer Activity of N-Carbamoyl-N'-(1-Oxyl-2,2,5,5-Tetramethyl-Pyrrolin-3-yl)Urea Compounds
Zhang Ziyi, Wei Lulin, Liu Lisheng, Zheng Rongliang
1989, 10(12): 1202-1207.
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By the addition of l-oxyl-2, 2, 5, 5-tetramethyl-pyrroline-3-isocyanate (I), synthesized by seven steps,to substituted hydrazides with biological activity, nineteen N-carbamoyl-N'-(1-oxyl-2,2,5,5-tetramethyl-pyrrolin-3-yl) urea compounds were synthesized, The characteristics of electron spin resonance spectra, infrared spectra and mass spectra of some typical compounds of (Ⅲ) were discussed.The preliminary experiment showed that compounds (Ⅲ) possess a inhibiting activity on L7712-leukemia cell and ascitic hepatoma.Especially, the activity of (Ⅲ)
e
, as well as of (Ⅲ)
g
are more striking.
Organic Reactions in Chiral Micelles (V)——Asymmetric Epoxidation of Chalkoncs in Chiral Micelles System
Zhang Yongmin, Fu Chunling, Lu Ping, Fan Weiqiang
1989, 10(12): 1208-1210.
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Chalkones were asymmetrically epoxidized by H
2
O
2
to their corresponding chiral α,β-epoxy ketones in aqueous chiral micelles formed from the chiral surfactants, N-dodecyl-N, N-dimethyl ephedrine bromides (1a) and N-hexadecyl-N,N-dimethyl ephedrine bromide (1b).The enantiomer excesses ranged from 5% to 8%.
The Construction and Calibration of a Precision Solution Calorimeter
Zou Lizhuang, Zhang Zhonghai, Xu Guiduan, Qu Songsheng
1989, 10(12): 1211-1214.
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Aprecision solution calorimeter was constructed in the laboratory.Athermsistor thermometer was used for temperature measurement.The calorimeter was calibrated with calorimetric standardreference materials——spectroscopically pure potassium chloride and tris (hydroxymethyl)aminomethane from N.B.S.-724 a in USA.The results obtained at 25℃ was found to be 17518± 15 J.mol
-1
for the enthalpy of solution of potassium chloride in water and -29729 ±31 J.mol
-1
for the enthalpy of reaction of TRISin 0.1008 mol/L HCl.The values are well in agreement with the published results.The reliability of this apparatus was confirmed
Studies on Electronic Structures of Vanadium Carbonyls V(CO)
n
Guo Chunxiao, Chen Maiming, Wang Jingli, Chen Erting
1989, 10(12): 1215-1220.
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The relationship between electronic structures of V(CO)
n
(n=1～6) with open shell system and it' s corresponding configurations were studied by restricted open shell CNDO/2 method.The diagram of orbital energy level correlation was given, which can well explain the correlation and stability of a variety of carbonyl configurations.Such a diagram of energy level correlation may not be obtained by.UHFself-consistent field method.Meanwhile the possible configurations of COstretching vi-brational frequencies obtained in infrared spectra have also been assigned.
In Situ FTIR Spectroscopic Study of β-Ni(OH)
2
Electrode
Jiang Zhiyu, Yan Manming, Wang Jie
1989, 10(12): 1221-1224.
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The electrochemical behavior of β-Ni(OH)
2
electrode in 3mol/L NaOHwas investigated by using in situ subtractsvely normalized interfacial FTIRspectrometry(SNIFTIRS).It was found from in situ SNIFTIRSspectra, that the surface of β-Ni(OH)
2
layer is changed to β-NiOOHobviously when the potential is higher than 0.5 V.The anodic oxidation of β-Ni(OH)
2
layer is started from β-Ni((OH)
2
/solution interface.But the cathodic reduction of β-NiOOHlayer is possibly started from Ni/β-NiOOHinterface.The influence of solvent on SNIFTIRSspectra of β-Ni(OH)
2
can be reduced by using NaODheavy water solution instead of NaOHsolution.
Determination of Equilibrium Constants for the Adductive Reaction of Bis-(O,O'-Dicyclohexyl-Dithiophosphato) Nickel(Ⅱ) with Pyridine and the Crystal Structure of Ni[(C
6
H
11
O)
2
PS
2
]
2
·2Py
Liu Shixiong, Lin Xichang, Xu Zheng, Lin Jianhua, Yu Yunpeng, You Xiaozeng
1989, 10(12): 1225-1228.
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Reaction of Ni[(C
6
H
11
O)
2
PS
2
]
2
with pyridine was studied spectrophotometrically and the equilibrium constants was found to be k=15.4±1.40(mol/L)-1 and β
2
=(1.43±0.41)× 10
3
(mol/L)
-2
.The crystal structure of Ni[(C
6
H
11
O)
2
PS
2
]
2
.2Py was measured by X-ray diffraction method.The crystal belongs to a monoclinic system with the parameters of unit cell a=8.938(3)Å，b=19.885(6)Å, c=6.366(3)Å,a=99.25(4)°,β=93.96(4)°, γ=92.01(3)°,V=787Å
3
, D
c
= 1.70 g·cm
-3
, Z= 1, F(000)=426e.Space group is P
1
R=0.085.
Unitary Group Calculus and Programing for Strong Ligand Field
Dou Yusheng, Wen Zhenyi, Liu Zhaomeng, Wang Yubin, Zhang Di
1989, 10(12): 1229-1234.
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Aunitary group treatment for the strong-field model is discussed in this paper.All the formulas necessary for calculation of an octahedral symmetry field are geven and programed in IBM PC/ XT.The program has low storage requirement and reasonable speed.Energy parameters and eigen-functions obtained by fitting spectroscopy experiments are satisfactory, which will be used to calculate magnetic and other properties of complex compounds.
Theory of the Analytical Method Based on Electrodeposition and Frequency Shift Measurement and its Verification
Nie Lihua, Tan Shenglian, Yao Shouzhuo
1989, 10(12): 1235-1237.
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The principle of the analytical method based on electrodeposition and frequency shift measurement by means of a piezoelectric quartz crystal is discussed theoretically and verified experimentally.Equations are derived to relate the frequency shift and the parameters concerned for the controlled-potential electro-deposition and the constant-current electrodeposition.
IRC Approach to Dehydrogenation and Isomerization of N
2
H
2
Li Xuekui, Sun Chiachung
1989, 10(12): 1238-1241.
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Dehydrogenation and isomerization of N
2
H
2
were studied by means of intrinsic reaction coordinate (IRC) method.Rearrangement and dissociation processes on H
2
H
2
potential energy surface are presented.Equilibrium and transition state geometries have been located by using ab initio SCFwith split-valence 4-31Gbasis set.
A Study on Synthesis and Properties of Block Polyurea with Different Hard Segment Content
Chen Zhusheng
1989, 10(12): 1242-1245.
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High molecular weight linear polyureas with different hard-segment contents were obtained by using a two-step solution polymerization.Elimination of water, careful choice of solvent, reactant concentration, and good control of reaction temperature are essential to obtain satisfactory results.DMSand DSCwere used to elucidate properties of these polyureas.The polyureas were transformed from a soft elastomer to a high modulus plastic with the increase of segment content.
Synthesis of Narrow Distribution Polystyrene in RLi-Ligand Complex Systems
Cao Junkui, Yoshio Okamoto, Shiro Honda, Koichi Hatada
1989, 10(12): 1246-1250.
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The synthesis of narrow distribution polystyrene by anionic polymerization in RLi-ligand complex system was investigated.It is found that RLi-(-)-sparteine and RLi-N,N,N',N'-tetram-ethylethylenediamine as the ligand complex systems are effective for preparation of narrow distribution of polystyrene with molecular weight in the range of 10
2
～10
5
through using hexane, heptane and toluene as solvents respectively.By adding THFto the above systems we also obtained the narrow distribution polystyrene with molecular weight in the range of 10
4
～10
5
.
Synthesis and Structures of PPh
3
-or AsPh
3
-Substituted Derivatives of Complexes (μ-RS)(μ-R'S)Fe
2
(CO)
6
Song Licheng, Hu Qingmei, Wang Jingduan
1989, 10(12): 1251-1253.
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Through the reaction of (μ-RS)(μ-R'S)Fe
2
(CO)
6
Awith PPh
3
in boiling benzene or toluene for several hours, four mono PPh
3
-substituted complexes (μ-RS)(μ-R'S)Fe
2
(CO)
5
PPh
3
Band three bis-PPh
3
-substituted complexes (μ-RS)(μ-R'S)(Fe
2
(CO)
4
(PPh
3
)
2
Cwere synthesized, respectively; similarly, the reaction of Awith AsPh
3
in boiling toluene afforded two bis-AsPh
3
-substi-tuted derivatives (μ-RS)(μ-R'S)Fe
2
(CO)
4
(AsPh
3
)
2
D.The relative reactivity of PPh
3
and AsPh
3
towards C≡Osubstitution and some influences of the two ligands on IRand
1
H NMRspectra of the complexes were pointed out, as well as the structural characterization of these new complexes were determined by elemental analysis, IRand
1
H NMR.
Studies on the Synthesis and Antitumor Activity of 3-(Arylmethyleneamino)propylsilatrane-Metal Complexes
Ding Qizhu, Luo Xuangan, Zhuo Renxi
1989, 10(12): 1254-1256.
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Ten 3-(arylmethyleneamino)propylsilatrane-metal complexes were synthesized by the reaction of metal salt with 3- (2-hydroxybenzylideneamino) propylsilatrane or 3-(2, 4-dihydroxyben-zylideneamino)propylsilatrane in methanol.The structure of these new complexes were identified by
1
H NMR, IRand elemental analysis.Animal screening data show that the inhibition ratio of bis-[N-(3-silatranylpropyl)-2-hydroxybenzylideneaminato] copper(Ⅱ) against Erlich ascites cancer in mice is 42.7%.
Synthesis of Optically Active Titatranes
Liu Hanxing, Yin Chenglie
1989, 10(12): 1257-1259.
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Six pairs of new optically active titatranes (Ⅱ) were synthesized by cyclization of acy-loxytriisopropyl titanate with (+) or (-)N,N-dihydroxyethyl-2-aminobutan
-1
-ol.Some of their physico-chemical constants, such as IR,
1
H NMRand specific rotation were determined.
Studies on the Electrochemical Epoxidation of Cyclohexene
Zhang Wenzhi, Wu Xizun
1989, 10(12): 1260-1262.
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The electrochemical epoxidation of cyclohexene on smooth platinum was investigated by means of convolution potential sweep voltammetry and potential step in H
2
O-NaBr-MeCN-(这里有图片19891223-1260-1.gif) system.It is further proved that the electrochemical oxidation of Br
-
is irreversible in the system, and the electrochemical epoxidation of cyclohexene shows a characteristic of ECcatatytic mechanism.Based on the analysis of data, some kinetic parameters were determined.
Study on the Coordination of Uranium (VI) with Gallic Acid and Its Analogues by Spectrophotometry
Wang Yingwei, Zeng Weihong
1989, 10(12): 1263-1265.
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The coordination of uranyl ion with gallic acid, pyrogallol, propyl gallate and 3,4,5-trimethoxybenzoic acid was studied by spectrophotometric method.The compositions and the structural formulae of the complexes formed are presented.Their stability constants are also calculated.
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