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中文
Table of Content
24 December 1985, Volume 6 Issue 12
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Articles
Study of the Accelerate Effect on the Transfer of UO
2
3+
in the Ion Exchanger Exerted by Cationic Ion and Carboxylic Acid by Elution Method
Jia Dongfang, Qiu Ling, Wen Zhixing, Qiu Yaowei
1985, 6(12): 1045-1050.
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The problem to accelerate the transfer of UO
2
2+
in cationic exchange resin with macro-pore was studied by analysing the elution chromatography.The accelerate, effect exerted by eight sorts of cationic ions: Ca
2+
, Mg
2+
,Mn
2+
,Co
2+
,Zn
2+
, Sc
3+
, Y
3+
and La
3+
and hydroxycarboxylic acid, dibasiccarboxylic acid and amino-aeid.was Studied and compared.It can be drawn that the parameter, τ, of material trasfer of UO
2
2+
decreases with the increase of the radius of the cationic ions existed in the exchange resin.Sc
3+
is an exception which is explanative.The apparent accelerate effect exerted by the dibasiccarboxylic acid was discovered and is ascribed to the formation of a neutral complex compound.
Study on the Complex Property of Benzo-15-Crown-5
Jin Xianglin, Tang Youqi, Wu Yangjie, An Haoyun, Hu Hongwen
1985, 6(12): 1051-1055.
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The single crystal of complex Na (benzo-l5-crown-5)-C
6
H
2
N
5
O
7
(C
6
H
5
N
3
O
7
=Picric acid) was obtained from the acetone-ethanol solvent.The crystal belongs to monoclinic space group C
2h
5
-P2
1
/n.The crystallography parameters arc:a=11.134 (3)Å,b=13.541(3)Å,c=14.927(4)Å, β=93.41 (2)°, V=2246.4Å
3
, Z=4.The crystal structure was solved by direct methed.The result shows that the electronic density on the aromatic ether oxygen atoms conjugated with the benzen ring can be transfered through the benzen ring.
Determination of Dissociation Constants of Chondroitin Salfate A and Stability Constants of Its Coordination Compounds
Tai Zihou, Wu Tiejun, Yuan Yusun
1985, 6(12): 1056-1058.
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We have measured a series of pH-Vtitration curves and have calculated dissociation constants of chondroitin sulfate Aand stability constants of seven metal ions by least squares approach and Bjerrum method.
Investigations on Oscillopolarographic Titrations(XXV)——Nitritometric Oscillopolarographic Titrations
Xu Weijian, Gao Hong
1985, 6(12): 1059-1062.
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This paper reports the titrations of Sn (Ⅱ), H
2
NSO
3
H, (N
3
H
4
)
3
-H
2
SO
4
, KMnO
4
, Ce(SO
4
)
2
, and semicarbazide, aminoguanidine, diphcnylaminc, resorci-nol, L-cysteine, dimcdonc, sulfanilamine, sulfadiazinc, sulfamcthoxazolc, dapsonc, sodium p-aminosalicylatc, mcloclopramide and procainc with standard nitrite solulion.These methods are rapid and accurate.
Discussion on the Chromatographic Behaviour of Carbonated Resins
Yun Xiqin, Zhang Zunxun, Kou Dengmin, Li Yanhong
1985, 6(12): 1063-1069.
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The heat of adsorption was derived from the temperature dependence of retention time for eluted peaks on a series of carbonated (pyrolyzed) resins.In view of chromatographic kinetics and thermodynamics the separative power, selectivity of the carbonaceous adsorbents and the factors influencing column efficiency are discussed theoretically.It is found that the diffusion effect controlled by inner structure of the adsorbent particle is the basic reason affecting separation and column efficiency.The conditions under which useful adsorbent could be made are revealed.
Determination of Trace Palladium by Anodic Stripping Catalytic Voltammetry
Xu Hongding, Guo Yinglan, Liu Zaixin
1985, 6(12): 1070-1074.
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Anew method for determination of trace palladium by anodic stripping-catalytic voltammetry has been established.The Pd(Ⅱ) was deposited with Hg (Ⅱ) on aglassy carbon electrode in NaCl-HCl-HgCl
2
base-solution at -0.80Vfor several minutes.After the depositing, the glassy-carbon electrode was removed itno another cell containing a catalytic system, HClO
4
-HCl-SnCl
2
.Astrippihg-catalytic peak of Pd at 0.40V(vs.Ag/AgCl) appeared when the potential was scanned forward positive.The height of the peak was linearly increased with the concentration of Pd(Ⅱ) over the range of 3 × 10
-10
- 1×10
-7
M.The detection limit was 1.2× 10
-10
M.The relative standard derivations were less than ± 7.5%.
Analysis Of Volatile Constituents Of Chinese Medicinal Herbs by Flash Distillation-Capillary Gas Chromatography-Mass Spectrometry
Chen Yaozu, Li Zhaolin, Xue Dunyuan, Han Hui, Yang Yuchcng
1985, 6(12): 1075-1079.
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In present paper, the principal volatilc constituents of Chinese medicinal herbs, Curcuma longa L., A.lancea(Thunb.)DC.,Foeniculum vulgare Mill.And cinna-momun cassia presl have been analyzed by means of flash distillation/capillary gas chromatography/mass spectrometry.The results obtained were similar to that of conventional steam distillation-extration method.But this new technique possesses such advantages: rapidity, simple manipulation, micro quantity of plant sample used and the exclusion of interference from impurities in the extrating solvents.It proves to be a promising tool for analysis of volatile constituents of natural products.The optimum condition of flash distillation has also been studied.
Spectrophotometric Determination of Trace Amounts of Iron with meso-Tetrakis-(4-Trimethylammoniumphenyl)-porphine under the Existence of BeryllonⅡ
Zhang Chuanyou, Yao Xingdong, Cheng Jieke
1985, 6(12): 1080-1082.
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The complexing reaction of Fe(Ⅱ)with meso-tetrakis(4-trimethylammoniumphe-nyl) porphine [T(4-TAP)P] has been studied.It was found that the reaction can be accelarated by some reagents, such as beryllon Ⅱ etc,and completed in 10-15min at 100℃ and pH4.5 The complex has an absorption peak at 395nm with a molar absorptivity of 1.3×10
5
.Beer's law is obeyed for Fed) in the range of 0-4.5μg/25ml.The interference ions can be separated by extracting Fe(Ⅲ) with MIBK.The high sensitive method has been applied to the determination of trace amounts of iron in some samples.
Stereoselective Synthesis of Trisubstituted Alkenes via Titanocycles
Liu Yiyin, Chen Meiwen, Li Yan, Wang Jitao
1985, 6(12): 1083-1088.
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By previously reported modified Masai-Rausch method for synthesizing titano-Cycles, followed by add hydrolysis, trisubstituted alkenes were synthesized, yields obtained were higher than that reported in literature.Starting from unsymmetrical alkyne substrates, twelve different types of substituted alkenes were synthesized, among which only two were found of single component, others were of isomer mixtures.Besides conventional analytical methods, NMRspectral analysis of titanocycle intermedlates and the products was used to identify the isomeric structures as well as their relative contents.
Determination of the Percentage of Guanine Plus Cytosine in Deoxyribonucleic Acid by Ion Pair Reversed Phase High Performance Liquid Chromatography
Du Henghua, Zhang Jianrong
1985, 6(12): 1089-1093.
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The percentage of guanine (G) plus cylosinc (C) in DNApreparations after acid hydrolysis in 88% formic acid is determined by ion pair reversed phase high performance liquid chromatography.By stepwisc gradient technique, uracil, cytosine, thymine, guanine, and adeninc are separated on a column of YWG -CH(C
18
) with 2.5mM KH
2
PO
4
buffer solution (pH=5.5) containing 5mMheptane sulfonate as the eluent(1), then with 2.5mM KH
2
PO
4
buffer solution (pH=5.5) containing 18% methanol as the eluent(2).The results for the percentage determination of (G+C) are in close agreement with thermal melting point and buoyant density values determined for the DNAof calf thymus and sperm.
The Synthesis and Spectral Characteristic of Pentamethylcyclopentadiene
Jin Changchun, Liu Juzheng
1985, 6(12): 1094-1096.
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In the paper we describe a modification of Bercaw's method to prepare pentamethycyclopentadiene, which was characterized by Chromatography-mass Spectrometry, Chromatography-infrared Spectrometry, Raman, UV, and
1
H,
13
C NMR Spectrometry.
A Study on the Behaviour and Mechanism of Extracting Au (Ⅲ) with PTSO
Li Lingying, Sun Yuanmiag, Ren Hongji, Di Ping
1985, 6(12): 1097-1101.
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PTSOis abbreviated from di-p-tolyl sulphoxide having a >S=Ogroup and is a neutral extractant.We have studied the separation behaviour of Au (Ⅲ) with other elements on a column packed with silica gel loaded with PTSOsince 1981 and have proved that PTSOis a new specific stationary phase for saparation and concentration of gold.The behaviour and mechanism using PTSOto extract gold were studied first in this paper by atomic-absorption spectrophotometry, ultraviolet spectrophotometry and infra-red spectrophotometry.The mechanism has been further improved by the electroconductivity method.The distribution ratios increase with increased HCl concentrations and the salt strength in aqueous phase but decrease with increasing temperatures.The constituent of the extracted complex is established as Au:H:Cl:PTSO=1:l:4:3 and its possible structure form is suggested.
A Study on Photoelectrochenlical Solar Cell of Polycrystalline Thin-Film CdTe Electrodeposited
Shen Yuenian, Huang Wende, Yuan Tao, Wu Yijun
1985, 6(12): 1102-1106.
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Thin films of polycrystal CdTe were deposited on brass foil substrates by catho-dic electrodeposition.Photoelectrochemical solar cells were made of photoelectrode CdTe, counter electrode Cu
2
Sand electrolyte polysulfide redox system (S + Na
2
S + NaOH).Solar conversion efficiencies up to 3.6% for photoelectrochemical cell with small area were obtained.The effects of thin film uniformity, temperature and selective etch treatments on J
sc
,V
oc
,F
F
and efficiency η were presented, some coments or explanations were suggested also.
The TPD Study of H
2
from the Cu/ZnO/Al
2
O
3
Catalyst of the Low Temperature Shift Reaction
Duan Xue, Gao Zhengzhong, Wang Qi
1985, 6(12): 1107-1111.
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The desorption kinetics of H
2
from the Cu/ZnO/Al
2
O
3
catalyst of the low temperature shift reaction has been studied by TPD.It is represented that, for H
2
, Cu/ZnO/Al
2
O
3
has two active sites (Ⅰ) and (Ⅱ) which have distinct characteristics of energy as the temperature <350℃.The detailed analysis for (Ⅰ) and (Ⅱ) with the desorption rate isotherms method gave the desortion kinetic parameters and determined the desorption rate equations.It was discovered that the effective surface of Cu/ZnO/Al
2
O
3
catalyst is not an ideal surface and the contribution for effective surface area is 27.6% for (Ⅰ) and 72.4% for (Ⅱ).
Construction of a Vaporization Calorimeter and Determination of Latent Heats of Vaporization
Li Xiangsheng, Yen Wen-hsing
1985, 6(12): 1112-1116.
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By modifying Mathews' apparatus, an isolhermal-adiabatic vaporization calorimeter was constructed.Latent heats of vaporization of pure methanol, ethanol, benzene, toluene and water were determined with an accuracy of 0.1-0.2%, agreeing with literature in less than 0.3%.Binary systems of water-ethanol and benzene-methanol and domestic crude cuts were also studied.
Calculation of Molecular Dipole Moments by Vector Sum of Bond Dipole Moments
Li Hongtu, Wang Ningdong, Dong Chunfeng
1985, 6(12): 1117-1119.
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According to the principle of vector sum of bond dipole moments a VSBDprogram has been carried out.More than one hundred dipole moment of organic molecules are calculated.The results of calculation are in agreement with experimental data.Hence this program can be used for approximate calculation of dipole moment of bigger molecules.
The Study of Promoter Distribution on the Surface of Catalytic Support in the Oxidation of o-Xylene by Method of Molecular Probe
Tang Xinshuo, Shu Geping, Hu Xicheng, Lu Guojian, Wang Li, Ye Xiaomci
1985, 6(12): 1120-1122.
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The method of Melecular Probe to determine the surface structure of three supporters was described.The influence of adsorption center groups of supporters on the distribution of catalytic promoter and the result of significant difference in catalyst characteristics were discussed.
Study on the Copolymerization of Citraconic Anhydride and β-Chloroethyl Vinyl Ether
Wu Gongsheng, G. B. Butler
1985, 6(12): 1123-1126.
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Copolymerization of citraconic anhydride and β-chloroethyl vinyl ether in benzene or toluene using AIBNas initiator was investigated.The effect of reaction conditions on comonomer conversion and molecular weight and- molecular distribution of copolymer was reported in this paper.
Linear Oligomerization of Propylene with Chelated Nickel Complex Catalyst
Gao Zhanxian, Liu Zhiguang, Wang Hong, Zhou Kcyan
1985, 6(12): 1127-1133.
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Propylenc was oligomerized by the complex catalyst prepared in situ from the nickel salt of 1, 1, 1,5,5,5-hexafluoropentane-2,4-dione and diisobutyl aluminum hydride.The linearity of the propylene dimers is in the range of 75-80%.It was observed that the Al/Ni (Molar ratio) value and the reaction temperature exerted evident influence on the activity of the catalyst and the linearity of propylene dimers.The reaction mechanism of the catalyst system has been discussed preliminarily.
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