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中文
Table of Content
24 June 1987, Volume 8 Issue 6
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Articles
A Study on the Ternary System La(ClO
4
)
3
-C
11
H
12
ON
2
(Antipyrine)-H
2
O at 0℃ and the Preparation and Characteristics of the Hexaantipyrine Complex of Lanthanum Perchlorate La(C
11
H
12
ON
2
)
6
(ClO
4
)
3
Tang Zongxun, Chen Yunsheng, Zou Youzhong
1987, 8(6): 481-484.
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The solubility of the ternary system La(ClO
4
)
3
-C
11
H
12
ON
2
(antipyrine)-H
2
O at 0 ℃ was studied. The hexaantipyrine complex of fhe lanthanum perch-lorate, La(C
11
H
12
ON
2
)
6
(C
1
O
4
)
3
, has been found in the system. The infrared spectrum, X-ray powder diffraction, solubility at 0 ℃ in water, melting point and density of the complex are recorded.
Synthesis of Hg(HPMBP),(PMBP)
2
and Zn(PMBP)(H
2
O)Cl Complexes and Their IR and
1
H NMR
An Xingmin, Jia Dianzheng, Li Yong
1987, 8(6): 485-488.
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The coordination compounds of 1-phenyl-3-methyl-4-benzoylpyrazolone-5 (HPMBP) with Hg(Ⅱ) and Zn(Ⅱ) have been synthesised. The structures and properties of the compounds formed have been characterized by elemental analysis, IR,
1
HNMR and Conductance measurements. The ligand used has been found to change from keto form to enolic form during the chelation reaction.The Hg(Ⅱ) is bohded by both the keto and enolic form producing a seldom 8-coordination compound.
Studies on the Mo[S
2
GN(G
2
H
5
)
2
]
4
[MoCl
5
] by the Infrared and Ultraviolet Absorption Spectra
Zhang Guangren, Qu Xiangbang, Huang Shipu, Tang Zhongkun, Huang Qijun, Sun Chunting
1987, 8(6): 489-491.
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The infrared and ultraviolet absorption spectra of tetrakis carbomoto moly-bdeunm (Ⅴ) hexachloromolybdate were determined, and the structural analysis was carried out by means of comparison.
The Single Crystal Growth of ZSM-39 in Gel of MA-SiO
3
-H
2
O System
Long Yingcai
1987, 8(6): 492-494.
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The single crystals of ZSM-39, being 150-200μm in size, were hydrother-mally grown in gel of MA(methylamine)-SiO
2
-H
2
O system at 200℃, The mole composition of the gel is:H
+
: MA:SiO
2
:H
3
O=(0-0.15):(0.5-4):1:(5-25). The single crystals obtained are uniform and perfect suitable for investigating the crystal structure.
Thermal Lens Spectrophotometry Based on Strong Pulsed Laser Excitation
Deng Yanzhuo, Cao Jianwen, Liu Cun, Chen Guanquan, Zeng Yun'e
1987, 8(6): 495-498.
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The thermal lens effects based on the strong pulsed laser excitation were observed by using the home-made experimental apparatus. In acetone-water mixture concentrations of CoCl
2
as low as 3×10
-7
M have been determined with present setup, which corresponds to an absorbance of 6×10
-6
. In thermal lens measurements the noise level due to shot-term instability of the He-Ne laser output amplitude can be reduced down by the use of differential amplification technique, thus the S/N ratio is improved appreciably.
Ion Exchange Behaviour of Uranyl in Solution of Acetate onto D-290 Macroporous Resin
Mao Xueqin, Tang Fulong
1987, 8(6): 499-501.
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The papar describes ion exchange behaviour of uranyl in solution of acetate on D-290 resin. The capacity, equilibrium constant and distribution coefficient of uranyl onto D-290 resin were studied by the batch method.In the case of EDTA used as masking agent, this method can be successfully applied to preconcentration by column method and the spectrophotometric determination of trace uranyl in waste water of uranite.
Oscillopolarographic Titrations Without Incisions
Xu Weijian, Zhang Shengyi, Gao Hong(H. Kao)
1987, 8(6): 502-504.
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Oscillopolarographic titrations are usually carried out on Hg or Pt electrode using the appearance or disappearance of the incisions to indicate the end point of titration. This requires the reagent to give oscillopolarogram with sensitire incision. This paper reports that oscillopolarographic titrations can be carried out on Pt electrodes using the sudden change of the whole oscillogram (increase or decrease in size, shift in position) to indicate the end point. This is very common in redox titrations. The titrations of Cu
2+
with EDTA, Cl
-
with AgNO
3
and many neutralization titrations as well as redox titrations can be carried out in this way.
Hydrodynamic Voltammetry at Tubular Electrode
Wan Zhen, Chen Qiang
1987, 8(6): 505-507.
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A theory of catalytic currents at a tubular electrode has been developed. The theory was applied to the catalytic currents observed in the reduction of ferric ions at the tubular gold electrode in the presence of hydrogen peroxide. The results showed that the diffusion coefficient and rate constant of the chemical reaction are 4.6×10
-6
cm
2
/sec and 105.8lit/mol·sec, respectively, in our experiments. Experimental data are in good agreement with the theory.
Spectrophotometric Determinating of Ferric-Thiocyanate Complexes in Microemulsion Medium
Guo Rong, Zhu Xiashi
1987, 8(6): 508-510.
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The effect of anion microemulsion SDS/n-C
4
H
9
OH/n-C
7
H
16
H
2
O as a medium on Ferric-Thiocyanate complexes is studied at 20℃. The results show that the maximum absorption wave λ
max
balhochromic shift and the sensitivity is raised in comparison with water as a medium when the three kinds of microemulsions are used as the medium respectively such as O/W, W/O and transitional structure between them, hut the W/O microemulsion is the best medium. And the λ
max
ba-thochromic shift 20nm and the sensitivity is enhanced about one time when the W/O microemulsion containing 20% water is used.
Studies on C-Glycosides(Ⅰ)--The Reaction Between Substituted Phenylmagnesium Bromides and α-D-Tetraacetyl-Glucopyranosyl Halide
Cai Mengshen, Yeu Baozhen, Wang Shaonong, Mao Ali, Qiu Dongxu
1987, 8(6): 511-516.
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The reactions between substituted phenylmagnesium bromides and α-D-tetra-acetyl-glucopyranosyl halides were studied. 4-methoxy phenylmagnesium bromides gave mainly β-C-glucoside.In the case of 2-methoxy-phenylmagnesium bromide,four products were obtained. They were l-α-(2-methoxy phenyl)-2,3,4,6-D-tetraace-tyl glucopyranoside, 1-β-(2-methoxy phenyl)-D-triacetyl-glucopyranoside, D-tetra-acetylglucopyranose,and l-deoxy-2-(2-methoxy phenyl)-2,3,4,6-D-tetraacetylglu-copyranoside. 2, 4-dimethoxyphenylmagncsium bromide, both α-and β-C-glucosides were separated. In the cases of 2-benzyloxy and 2,6-dibenzyloxy phenylmagne-sium bromides, the steric effect of the bulky substituents at ortho position prevented normol coupling reaction.
The Synthesis of Some Pyrethroids with Trichloromethyl Group in Alcohol Moiety
Hu Bingfang, Fang Yuan
1987, 8(6): 517-522.
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Sixteen new pyrethroids with the following general formula were synthesised,Y =3,4-dichloro,4-methoxy,4-methoxymethyl,3-phenoxy or 3,4-methylenedioxy. Only the compounds with Y=3-phenoxy or 3,4-methylenedioxy were found effective against armyworm with moderate activity.
Chemistry of 1,2,4-Triazines(Ⅸ)--Synthesis of Chemical Properties of 3-Oxo-2,3-Dihydro-6-Methylthio-Pyrazolo(3,4-e)-1,2,4-Triazine
Cai Mengshen, Chen Wenzheng, Cheng Tiemin
1987, 8(6): 523-527.
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3-Oxo-2,3-dihydro-6-methylthio-pyrazolo(3,4-e)-l,2,4-triazine was prepared. Its stability to diluted acid and base and substitution reaction, with amines were studied. The activity of nucleophillic substitution reaction of the key intermediate ethyl 3,5-dimethylthio-1,2,4-triazine-6-carboxylate was investigated.
Isolation and Identification of the Chemical Constituents of Chinese Medicinal Herb Rodgersia Aesculiflia Batal
Shen Xuwei, Zheng Shangzhen, Fu Zhengsheng, Chen Hao
1987, 8(6): 528-532.
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Rodgersia aesculi folia batal is an effective antibacterial and antiviral Chinese medicinal herbal for the treatment of asthma bronchial and inflammation. From the roots of rodgersia aesculifolia batal, ten constituents were isolated and identified, among which nine compounds were found in this Chinese medicinal herd for first time. Compound Ⅱ and compound Ⅳ were two new compounds. Their structures were elucidated by means of spectral as well as chemical methods as 7-methoxybergenin and methyl-2,6-dihydroxyphcnyl acetate respectively.
Reaction and Synthesis of 8-Carboxyethyl ⊿
9
Hexahydrocoumarin
Huang Huamin, Li Yezhi, Wang Zhongren
1987, 8(6): 533-537.
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2,6-Di(β-cyanoethyl) cyclohexanone 1 was prepared by treating cyclohexa-none with acrylonitrile in the presence of KOH/ethyleneglycol, then 1 was converted to 2,6-di(carboxyelhyl) cyclohexanone 2 by refluxing with dil HCl. When 2 was heated in xylene with ferric sulfate 8-carboxyethyl ⊿
9
hexahydrocoumarin 3 was formed. 2 reacted with alcohols (ethanol, propanol, butanol, pentanol) by the action of hydrated ferric sulfate as catalyst, the esters 4,5,6 and 7 were obtained, respectively. 3 could easily be hydrolyzed, alcoholyzed and ammonolyzed to give 2,6,7 and 8. 3 reacted with bromine and then heated, hydrobromied was quickly liberated from the addition product thus 9 was formed. When a xylene solution of 9 and maleic anhydride was refluxed for 11h the adduct 10 was obtained.
Analysis of Volatile Constituents of Hedysarum Polybotrys Hand, by Capillary Gas C hromatography-Mass Spectrometry
Chen Yaozu, Wang Rui, Xue Dongyuan, Li Zhaolin, Han Hui
1987, 8(6): 538-541.
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The volatile constituents of the roots of Hedysarum Polybotrys Hand, collected from Cansu Province, have been analysed by capillary column GG/MS. Thirty compounds were preliminarily identified. They hare not been found in this species previously.
Study of the Relationship Between Acidity of SO
4
2-
/ZrO
2
Solid Superacid and Its Catalytic Activity in Olefin Alkylation
Cui Shengfan, Wang Jiang, Zhang Songsheng, Wen Lingsheng, Sun Zhongqi, Qian Zaihu
1987, 8(6): 542-546.
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This paper reports the relationship between the acidity of SO
4
2-
/ZrO
2
type solid superacid and its catalytic activity in olefin alkylation, and the correlation of the acidity, activity and selectivity of the superacid as a catalyst with the ratio of the quantity of Bronsted acid site to that of Lewis acid site (B/L) on it is observed. As the value of B/L approaches to 2, it shows the highest acid strength and the optimum catalytic activity and selectivity.
Effects of the Additive DB on the Electronucleation of Zinc
Wu Huihuang, Xu Shukai, Zhou Shaomin
1987, 8(6): 547-550.
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Using an electrochemical setup controlled by a microcomputer, the influence of DB, an additive for forming Zn deposits with low brittleness, on the electronu-cleation of zinc was investigated. The results showed that the nucleation follows the progressive mechanism. The relation of the nucleation rate constants Ato the electrode potentials Eprovided the evidence of the validity of the classical nucle-ation-rate law, and the emprical equation N
s
=N
∞
{1-exp[-b(E-E
cr
)]}was obtained after fitting the saturated nuclear number densities N
s
with E. At a constant potential, however, both N
s
and Adecreased with increasing DBconcentrations. The effects of the additive and ovcrpotential were discussed in terms of heterogeneous nucleation theory.
Orientation Effect and Charge Distribution in Monosubstituted Benzenes
Yuan Hanjie
1987, 8(6): 551-555.
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A simple and new method for calculating charge distributions at ortho-, meta-and para-positions,δQ
o
, δQ
m
and δQ
p
, in monosubstituted benzene molecules is presented. Several empirical rules to judge orientation effect in aromatic electrophilic substitution reactions are found. These are:1.when δQ
p
/δQ
m
>1 but △δQ<0, groups of this kind are ortho-and para-position directing with activation; 2. when δQ
p
/δQ
m
>l but △δQ>0, groups of this kind are ortho- and para-position directing with deactivation; 3. when δQ
p
,/δQ
m
<1 but △δQ>0, groups of this kind arc meta-position directing with deactivation.
Crystal and Molecular Structure of 2,2'-Binaphthyl
Chen Minqin, Wu Gnang, Zhuang Shanming, Huang Zuen, Qiu Wenjie, Wu Wenling
1987, 8(6): 556-558.
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2,2'-binaphthyl C
30
H
14
, crystallized in the space group P2
1
/c with α=13.517(2), b=5.991(1), c=8.148(3)Å, β=85. 69(2)°, V=657.9Å
3
, d
c
=1.294g·cm
-3
, Z =2,,μ(MoK
α
)=0.679cm
-1
, F(000)=268. The structure was solved by Direct method and refined by full matrix least squares technique with a final R =0.034 for 821 unique observed reflections (I≥3σ)
Crystal and Molecular Structure of Ce(NO
3
)
3
·18-Crown-6 Complex
Yao lingwen, Luo Baosheng, Wang Jingqiu, Zhang Shaohui
1987, 8(6): 559-561.
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Complex Ce(NO
3
)
3
·18-crown-6 crystallizes in space group Pbca with α-12.223(2),b=15.617(3),c=21.806(4)Å, Z=8. 3419 independent reflexions were collected on Enraf-Nonius CAD4 diffractometer,of which 2972 with I>3σ
1
. The structure was solved by Patterson method and subsequent Fourier syntheses. Block-matrix least-squares refinement with parameters for all atoms led to R =0.025 and R
w
=0.032. The Ce
3+
ion has a distorted twelve-coordination, six coordinate Oxygens are from the crown ring.
Comparison of Different Methods of Immobilized Glucose Oxidase
Li Lixia, Lu Ge, Chen Changzhi, Yu Yaoting
1987, 8(6): 562-567.
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In this study, the bcsi condition of immobilized glucose oxidase using different supports and different methods was studied, and compared. An improved method of glucose oxidase immobilization method using glutaric dialdehyde was studied.One end of the glutaric dialdehyde molecule was first protected by diethanol-amine and the other end was linked to the carrier. Then the protected end was hydrolysed and glucose oxidase was linked to it. Clucose oxidase prepared according to the above method had the highest activity. The enzyme activity was 10% more than the didzo-reaction method and twice nigher than the polyacrylamide entrapment method.
Study of Pourous Polystyrene Gel--The Relationship Between Phase Separation Conditions and Pore Structrue
Bian Fenglan, Zhang Hongan, Shen Jiacong
1987, 8(6): 568-571.
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The present paper describes the investigation of polystyrene gel. The conversion and the distribution curve of gel and sol were measured, during the pore-forming process. It was found that earlier phase separation leads to a decrease in pore volume and strength of the resin. On the basis of this point, we proposed that the nonsolvent was added to adjust the pore volume and pore diameter when the resin became plastic and viscous, and designed a series of experiments.
Synthesis of High Molecular Weight Epoxy Resin Improved by Bisphenol-S
Gao Jungang, Wang Fengli, Shi Linqi, liu Weihong, Liu Cangjun
1987, 8(6): 572-574.
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The high molecular weight epoxy resin has been synthesised under phase transfer catalysis. The method involves the reaction of bisphenol-Aand bisphe-nol-Swith epichlohydrin in aqueous alkali-dioxane system, at reflux temperature, using polyoxyethene as a phase transfer catalyst. The reactivity ratio of monomers and some reaction conditions were investigated in this paper.
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