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中文
Table of Content
24 May 1992, Volume 13 Issue 5
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Articles
The Design for a Novel Topological Structure of Sieve CJU-18 with Super-Large 18 Membered Ring Open Pores
XU Yu-hua, ZHANG Li-ping, XU Ru-ren
1992, 13(5): 561-563.
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A novel topological framework structure of the molecular sieve named CJU-18 is obtained theoretically, which has 18 membered ring open pores.The structure is formed by the assemblage of the second building units: cancrinite cage, according to the hexagonal space groups P
6
3
/mmc.It has not only the 18-ring pore channel system which parallels to the c-axis as in VPI-5, but also 10-ring pore channel system along both a and b-axis.The results obtained from calculating the bond distances and angles between the atoms show that the structure may probably exist.By using the POWD-MODELING program and the X-ray powder diffraction pattern the topological structure is described.
The Synthesis and Structure Study of a New-kind of Carbonyl Cluster with Seven-Nuclear Co Atoms
ZHANG Wen-tao, LI Bing-xin, ZHANG Shu-yan, XU Xiu-ting, PIAO Gui-jin
1992, 13(5): 564-566.
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The product of reaction of C
2
H
5
SPCl
2
with Co
2
(CO)
8
was separated through column chromatography and the first band, which is deep brown in colour, was attributed to a loose a-tomic cluster of Co
7
(μ
7
-S)(μ
4
-PSC
2
H
5
)(μ-SC
2
H
5
)
2
(μ-CO)
2
(CO)
12
with a combination of an octahedral skeleton Co
4
PS and a tetrahedral skeleton Co
3
S by means of IR,
1
H NMR, elemental analysis and XRD.
Relationship Between Luminescent Properties and Structures of Li
2
O-CaO-Gd
2
O
3
-SiO
2
:Eu,Bi System
TIAN Yi-guang, WANG Chuan-sheng, LI Bin
1992, 13(5): 567-570.
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The variations of phase components depending on the concentrations of Gd
2
O
3
in the system of Li
2
O-CaO-Gd
2
O
3
-SiO
2
:Eu,Bi were studied by powder X-ray diffraction.It was investigated that the structures and species of silicates affect the luminescent properties of Eu(Ⅱ) ion and Bi(Ⅲ) ion.If Gd concentration is small, the product is β-Ca
2
SiO
4
.The phases Ca
2
Cd
8
(SiO
4
)
6
O
2
and LiCd
9
(SiO
4
)
6
O
2
appear and their contents increase with Gd
2
/O
3
being 0.25 when the ratio Gd
2
O
3
/SiO
2
is more than 2.5 wt% .The luminescence intensity of Eu
3+
ion in the sample is five times that of Eu
3+
ion in the sample with Gd
2
O
3
/SiO
2
being 0.2.The structures of the two phases containing Gd favor both red emission of Eu
3+
ion and energy transfer from sensitizer to activator.The solid solution formed by the two compounds is a better host material than single LiCd
9
(SiO
4
)
6
O
2
phase.
Studies of Ultrastable Faujasites Enriched in Silicon--Preparation, Characterization, Stability, Hydroxyl Acidity andcatalytic Activity
WANG Qiu-ying, SHENG Fen-ling, Jian Pan-ming, ZHU Chao, XU Yan-he, YAN Zi-feng, CHE Biao
1992, 13(5): 571-575.
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Faujasiste zeolites(FSY) with different Si/Al ratios(4.2~7.1) are prepared by secondary synthesis with (NH
4
)
2
SiF
6
.The corresponding US-SYC 4.2~7.1) samples are also prepared by the stabilization treatment of FSY samples at 500℃ hydrothermal condition.The XRD, DTA and IR studies show that the thermal stability and framework stability and acid strength of US-SYsamples are higher than that of FSYsamples.The catlalytic activity of USSY samples for the cumene cracking, toluene disproportionation and dealkylation actirity are superior to that of FSY samples.
Synthesis of Polynuclear Fc-M-Fc Complexes Containing N and S Atoms and Quenching the Luminescence of Ru(bpy)
3
2+
DUAN Chun-ying, XIA Xu-bing, ZHU Long-gen, YOU Jing-jing, CAO Hong
1992, 13(5): 576-579.
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Polynuclear complexes containing Nand Satoms [M(Fc-C(CH
3
)= NN=CSSR)
2
,R=—CH
3
, —CH
2
C
6
H
5
, M=Co
2+
, Ni
2+
, Cu
2+
, Zn
2+
, Cd
2+
] were synthesized.It was found that the coordination compounds could quench
*
Ru(bpy)
3
2+
with high efficiency.The Stern-Volmer plot is linear and yields the bi-molecular quenching rate constants for these compounds.The quenching luminescence of the
*
Ru(bpy)
3
2+
proceeded through the electron transfer mechanism.
Studies on the Macrocyclic Complexes of Transition Metal (Ⅳ)——The Synthesis and Properties of Schiff Base Type Macrocyclic Ligand Tetrafuran [26]-N
4
O
4
and Its Transition Metal Complexes
ZHANG Bao-long, JI Zhen-ping, XIAO Wen-jin, WU Cheng-tai, LIANG Ying-qiu
1992, 13(5): 580-582.
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A newly synthesized Schiff base type of macrocyclic ligand and its transition metal [Co(Ⅱ),Cu(Ⅱ),Zn(Ⅱ),Cd(Ⅱ)] complexes were investigated by elemental analysis, molar conductance, IR, MS,
1
H NMRetc.The results indicate that the planar configuration of free ligand changes with the formation of the complexes.
A Sensor for Guanine Using Brain Tissue of Rat
DENG Jia-qi, KONG Ji-lie, HE Hong
1992, 13(5): 583-585.
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An electrode for the determination of guanine was prepared, which employed brain tissue of rat as the biocatalyst and an ammonia gas sensing electrode as the base electrone.Its response characteristics, buffer conditions and strategies of immobilization were studied.The slope of guanine response curve E-lg[Guanine] is 46.5 mV/decade, linear range is 2.0×10
-5
~6.3×10
-4
mol/L, lifetime is over 28 days.
Investigation on Microelectrodes (Ⅹ)——The Steady-State Differential Voltammetry on Microdisc Electrode
JU Huang-xian, CHEN Hong-yuan, GAO Hong(H. Kao)
1992, 13(5): 586-589.
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The steady-state diffusion current equations of single-sweep, the first differential, the second differential and the third differential voltammetry on microdisc electrode were studied.These currents are directly proportional to r, C, D.The single-sweep limit current is independent of the sweep rate (v), and the first, second and third differential peak current are proportional to v, v
2
, v
3
, respectively.These results are verified experimental with carbon fiber microdisc electrode.
Determination of Acetone by Sensitized Room Temperature Phosphorimetry in Solution
CHEN Zu-wu, XU Jin-gou
1992, 13(5): 590-592.
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A sensitized room temperature/phosphorimetric method by using biacetyl as an energy acceptor for the determination of acetone in solution was developed.Acetone was excited at 274 nm and the phosphorescence intensity emitted from biacetyl was measured at 515 nm.The factors affecting the stability of the sensitized phosphorescence at room temperature in solution were investigated and discussed.Asimple and effective unit which can be operated on the cell holder for the deoxygenation of the solution with N
2
gas was also designed.The calibration curve was linear over the concentration range of 2.0×10
-4
~1.5×10
-2
mol/L(r=0.999) and the limit of detection was 8.0×10
-5
mol/L.
Determination of Thiourea with Inhibition Action of Electrochemiluminescence
AN Jing-ru, LIN Jian-guo
1992, 13(5): 593-595.
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The electrochemiluminescence of thiourea was studied in medium of Na
2
CO
3
-NaHCO
3
-KCl-DHDHD(pH= 9.8) by a self-made apparatus.Thiourea exhibits an evident inhibition action for electrochemiluminescence of DHDHD.It can be used for the determination of microamounts of thiourea.Alinear relationship between the concentration and intensity of light emitted is obtained in the range of 0.005~5 ppm for thiourea.The relative standard deviation is 2%.The mechanism of the electrochemiluminescence of thiourea is also discussed.
The Study and Application of Eosiny NaClO-CTMAB-H
2
O
2
-Ti(Ⅳ) Chemiluminescence System
LIU Yu-ying, YU Zhen-an
1992, 13(5): 596-598.
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In this paper a new sensitive and selective analytical method for the determination of trace amounts of Ti(Ⅳ) is proposed on the basis of chemiluminescence of eosiny and CTMABas surface active agent.Flow-injection technique was used.The linear range of the working curves is 4~800 ng/mLand the detection limit is 2.1 ng/mL Ti(Ⅳ).The method was applied to the determination of Ti(Ⅳ) in water and aluminium alloy with satisfactory results.
Determination of Fe, Co and Ni in Their Chelates with IAP-4S by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography
LIN Chang-shan, ZHANG Xiao-song, LIU Xue-zhu, FENG Jian-zhang, TONG Shen-yang
1992, 13(5): 599-601.
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The chelates of iron, cobalt and nickel with 2-(2-imidazolylazo)-phenol-4-sulphonic acid IAP-4Swere separated on a column (250×4 mm) of Nucleosil C
18
(5μm) with a mobile phase (0.7 mL/min) of methanol-water (30:70, V/V) containing 0.01 mol/L KH
2
PO
4
-Na
2
HPO
4
buffer (pH 7.5) and 2×10
-3
mol/Ltetrabutyl ammonium bromide, and were detected at 550 nm.The calibration graphs are rectilinear from 0.1~5 ppm for iron, 0.05~5 ppm for both cobalt and nickel.The detection limits are 0.25 ng for iron, 0.16 ng for both cobalt and nickel.The method was applied to the analysis of real samples.
Synthesis and Analytical Application of the Salicylidene-8-Aminoquinoline(Ⅰ)——Fluorimetric Determination of Trace Amounts of Gallium
KANG Xin-huang, YANG ZHi-bin
1992, 13(5): 602-604.
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A new Schiff base, salicylidene-8-aminoquinoline(SAAQ), was prepared and characterized by elementary analysis, IRand UV.The optimal conditions for the fluorescent complex formation of SAAQ with gallium (Ⅱ) are established in this paper.The excitation and emission wave lengths are 418 nm and 513 nm respectively, the molar ratio of Ga( Ⅱ) to SAAQ was determined to be 1:2.The quantum yield is 0.69 at pH 3.20~4.50.The proposed method was used for the determination of gallium in alloy samples in the range of 2~280 ppb.
The Principle of Oscillopolarographic Neutralization Indicators (Ⅰ)——Aniline and Fluorescein Sodium
CHEN Yang, WENG Yun-rong, GAO Hong(H. Kao)
1992, 13(5): 605-607.
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The present paper covers the mechanism of incision formation in oscillopolarograms about aniline and fluorescein sodium as oscillopolarographic neutralization indicators.The incision change of fluorescein sodium is due to oxido-reduction and that of aniline due to absorption of the indicators at the polarized electrode.
Determination of Morphine in Urine of Drug Addicts by Gas Chromatography-Mass Spectrometry
XU You-xuan, ZHU Shao-tang, ZHANG Chang-jiu, WU Yun, ZHANG You-jie
1992, 13(5): 608-610.
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A rapid sensitive method has been developed for the determination of the concentration of morphine in drug addicts'urine by using GC/MScombined with Selected Ion Monitoring (SIM) technique.The peak area ratio of morphine to dihydrocodeine(internal standard) is proportional to the concentration of morphine from 10 ng/mLto 1000 ng/mL.The recovery and detection limit are 96.6±1.8(n=4) and 0.5 ng.The method has been used to determine the concentration of drug addicts who were being treated in a hospital.
Studies on the Synthesis of Phosphonodipeptides and Their Herbicidal Activity (Ⅱ)
CHEN Ru-yu, ZHANG Yue-hua, CHENG Mu-ru
1992, 13(5): 611-616.
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It was reported in literature that phosphonodipeptides had significant biological activities.In order to look for new herbicides, a series of novel phosphonodipeptides have been prepared by the reaction of (PhO)
2
P(O)CH
2
NH
2
or (EtO)
2
P(O)CH
2
NH
2
with ClCH
2
CONHCHR COOR'and ClCH
2
CONHCHRP(O)(OPh)
2
separately in the presence of triethylamine in benzene.The structures of all the compounds prepared were proved by
1
H NMR, IR and MS.Their spectroscopic spectra and biological activities were discussed.It was found that some of them showed good herbicidal activity.
Studies on the Synthesis of C-Nucleosides--Synthesis of 3-β-D-XyIopyranosyl-1,2,4-Oxadiazoles
DONG Ling-jiao, LI Li, MA Ling-tai, ZHANG Li-he
1992, 13(5): 617-622.
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Fourteen new derivatives of 3-β-D-xylopyranosyl 1,2,4-oxadiazole were synthesized via condensating protected β-D-xylopyranosyl amidoxime with anhydrides or various substituted benzoyl chlorides in good yields.The 1,2,4-oxadiazole ring was formed directly by condensation of xylopyranosyl amidoxime and various anhydrides, but if the condensation occured by using substituted benzoyl chloride instead of anhydride, the cyclization was completed by two steps.The mechanism was discussed, 3-β-.D-xylopyranosyl-1,2,4-oxadiazole is stable under the condition of 1 mol/L HCl, 1 mol/L NaOH or at high temperature.
Structure Determination of
Nephalsterol
A and B with 19-hydroxy Group from Soft Corals
Nephthea
WANG Guiyang-sheng, LI Feng-ying, ZENG Long-mei, MA Li-bin, TU Guang-zhong
1992, 13(5): 623-627.
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Two 19-hydroxylated sterols, name ne phalsterd-A (1) and B (2) were isolated from the soft corals, Nephthea albida and Nephthea tiexieral verseveldt collected off Xisha and Nansha Islands respectively.On the basis of one and two dimensional NMR and other spectroscopy methods, the structures of 1 and 2 were characterized as 24-methylene-cholestan-3β,5α,6β,19-tetrol and 24-methylene-cholestan-5-ene-3β, 7β, 19-triol respectively.1 is an unknown compound.The structure of 2 is identical with the sterols which was isolated from the soft coral Litophyton viridis by M.Bortolotto.The
1
H and
13
C NMR data of 1 and 2 were first assigned from the
1
H-
1
H and
13
C-1H COSY and COLOC spectra in this paper.
Acetoxy Phyllofolactone A——a Novel Bishomoscalarane Sesterterpene form the South China Sea Sponge
Phyllospongia Foliascens
FU Xiong, ZENG Long-mei, SU Jing-yu
1992, 13(5): 628-629.
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A novel bishomoscalarane sesterterpene (1) has been isolated form the South China Sea sponge Phyllospongia foliascens.Its structure was determined as acetoxy phyllofolactone Aon the basis of spectral data and by comparison of its spectral data with those of phyllofolactone A.
Synthesis of 5-(2'-Carboxyethyl)-6-Alkyl-3,4-Dihydropyrone
HUANG Hua-min, LI Ye-zhi, REN Zhong-jao, XU Ya-qin
1992, 13(5): 630-632.
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5-(2'-Carboxyethyl)-6-methyl-3,4-dihydropyrone(2
a
) and 5-(2'-carboxyethyl)-6-isobutyl-3,4-dihydropyrone (2
c
) were prepared from 4-acetyl heptanedioic acid (1
a
) and 4-iso-valeryl hyptanedioic acid (1
c
) in the presence of acetic anhydride with yields of 63%, 68% respectively.When 1
c
was refluxed with ferric sulfate hydrate as the catalyst product 2
c
also formed in 63% yield.2
a,c
or 5-(2'-carboxyethyl)-6-isopropyl-3, 4-dihydropyrone (2
b
) reacted with ethyl alcohol to afford 4-acylheptanedioic acid diethyl ester (3
a-c
) in the presence of hydrochlo-ride.Treatment of 2
a-c
with ammonia water gave 5-(2'-carboxyethyl)-6-alkyl-3, 4-dihydro pyridone (4
a-c
) in 55%~72% yields.
Studies on Synthesis and Reaction of N-Ferrocenylamic Acid
MA Huai-rang, CHEN Zhi-bing, YANG Bing-qin, LI Jin-song
1992, 13(5): 633-635.
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Seven N-ferrocenylamic acids have been synthesized and characterized by elemental analysis, IR and
1
H NMR.The investigation on the chelation of acid Awith Cu
2+
and Zn
2+
ions demonstrates the coordination of the oxygen atom on the amide group to the metallic ion.
XPS Analysis of Cabane-like Fe
4
S
4
Clusters
WEI Quan, XU Ji-qing, NAN Yu-ming, QIAN Ji-song, CAI Hui, YAN Ying-zhuo
1992, 13(5): 636-638.
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The XPSof cabane-like Fe
4
S
4
clusters were studied.The valence of Fe was examined, the 2p binding energy of the framework Sin Fe
4
S
4
is first reported.The proportion of all sorts of Sand Nby peak synthesis is in agreement with the values obtained from the calculation on the basis of structure formulas.
Studies on Ion Exchange and Adsorption of Au(Ⅰ), Ag(Ⅰ) and Other Metal Cyanide Anions by BPR Resin (Ⅱ) ——Determination of Intraparticle Diffusion Coefficient and Study on the Mass Transfer Process
GAN Wei-tang, LIU Yan-ming, ZHANG Yu-fan
1992, 13(5): 639-642.
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The intraparticle diffusion coefficient and activation energy of Au (Ⅰ), Ag (Ⅰ), Ni (Ⅰ), Fe(Ⅱ) cyanide anions were determined in Cl, NO
3
, OH-type BPRresin at different temperatures.It is found from the experimental results that the mechanism for extracting Au (Ⅰ), Ag(Ⅰ) and other metal cyanide anions by BPRresin belongs to ion exchange process.The difference of activation entropy of some metal cyanide anions (△S-△S) was evaluated.
The Bond Properties of Ce(C
8
H
8
)
2
and Ce(C
8
H
8
)
2
-
WANG Yi
1992, 13(5): 643-644.
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By assigning the bonding forms of dicyclooctatetraenyl cerium as: (1)ion aggregation state Ce
4+
(C
8
H
8
)
2
-
;(2) s and p orbitals of cerium are used to form the covalent bond of cerium and the ligand;(3) d orbital of cerium is used to form the covalent bond of cerium and the ligand;(4) f orbital of cerium is used to form the covalent bond of cerium and the ligand;(5) s, p, d and / orbitals of cerium are used to form the covalent bond of cerium and the ligand.The bond properties of Ce(C
8
H
8
)
2
and Ce(C
8
H
8
)
2
-
are analysed in energy with the improved Xa-SWmethod and Ziegler's transition state method.
Studies on Emission Spectra of the Catalysts of Alkali Alkaline-Earth Rare-Earth Metal Oxides
YANG Xiang-guang, BI Ying-li, ZHEN Kai-ji, Li Sen-zi, WANG Ji-xiang, WU Yue
1992, 13(5): 645-647.
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The formation of O
-
species in oxide catalysts was investigated by characterization of emission spectra of Eu
3+
ion.The experimental results show that in M/MgO and M/CaO sys-tems(M=Li
+
, Na
+
and K
+
) Li
+
and Na
+
can enter into the lattice of MgO, and Li
+
, Na
+
and K
+
ions can enter into the lattice of CaO.These conclusions are in good agreement with what was found by Lunsford in his ESR studies.Based on the results of emission spectra investigation > an evidence that Li
+
ion can not enter into the lattice of La
2
O
3
in Li/La
2
O
3
mixed oxide and, as a result, no O
-
species can be formed was gained.The obtained experimental data also provided some useful information about the coordination conditions for simultaneous entrance of both mono- and tri-valence ions into the lattice of alkaline-earth metal oxides.
Studies on HPA Catalysis for the Reaction of Toluene Sulfonation to 4,4'-Dimethyl diphenylsulfone
WU Tong-hao, LI Yong-guo, YANG Hong-mao, WANG Guo-jia, HUA Shi-ying, JIANG Yu-zi, YU Jian-feng
1992, 13(5): 648-650.
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It is proved by the experiment that HPAis a good catalyst for the reaction of toluene sulfonation to 4,4'-dimethyldiphenyl sulfone.The effect of HPAon p-methyl sulfonic acid has been studied by means of UVand variable-temperature
1
H NMR.The preliminary catalytic mechnism is also proposed.
Determination of the Acidity of H(Mg)AlPO
4
-5 and H(Co)AlPO
4
-5 Molecular Sieves
XIAO Feng-shou, XU Ru-ren, XIN Qin
1992, 13(5): 651-653.
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The acidic sites of aluminophosphate molecular sieves, AlPO
4
-5, containing various heteroatoms such as Mg
2+
and Co
2+
were investigated by using IRspectroscopy of adsorbed pyridine and temperature-programmed desorption(TPD) of NH
3.
The band at 3680 cm
-1
is assigned to P—OH, and the band at 3820 cm
-1
can be attributed to the terminal Al—OH.The bands appearing in the region from 3660 to 3568 cm
-1
is possibly assigned to the bridging hy-droxyl groups M (OH) P (M=Mg,Co).The decreasing acidity sequence of acidic sites is: Co(OH)P>Mg(OH)P>P(OH)>Al(OH).The IRspectra of pyridine adsorbing these samples reveal that there are strong Band Lacidic sites in H(Mg)AlPO
4
-5 and H(Co)AlPO
4
-5, in contrast to AlPO
4
-5.Additionally, the TPD-NH
3
experiments show the order of the acidic strength of these samples: H(Co)AlPO
4
-5>H(Mg)AlPO
4
-5>>AlPO
4
-5.
Studies on the Surface OH Groups and Acidic Properties of LaDAIY
FU Jun, BAO Shu-lin, Xu Qin-hua
1992, 13(5): 654-657.
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The surface hydroxyl groups and acidic properties of LaDAlY were examined by means of IR spectroscopy with pyridine adsorption and NH
3
-TPD method.From the variations of hydroxyl groups, it is shown that La
3+
ions are located at different positions in NH
4
Y and DA1Y.The experiments further indicate that the number of both Bronsted and Lewis acid sites on DA1Y and NH
4
Y was decreased after La
3+
ions-exchanged.The NH
3
-TPD results show that the strength of weak acid sites of DA1Y was increased, while the strength of strong acid sites was almost not changed after La
3+
ions-exchanged, and the number of acid intes was decreased generally.The results are consistent with these obtained by infrared studies.
Studies on Chemical Constituents of Fritillaria in Hubei(Ⅻ)--X-Ray Determination of Stereo-Structure of
Ebeiensine
WU Ji-zhou, SHENG Liao-rong, LUO Bao-sheng
1992, 13(5): 658-661.
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The ebeiensine was isolated from the bulb of Fritillaria ebeiensis G.D.Yu et G.Q.Ji and Fritillaria ,ebeiensis var.purpurea G. D. Yu et P. Li.The result of the complete X-ray structural analysis shows that ebeiensine with the molecular formula C
27
H
41
NO
3
·H
2
O, belongs to the rhombic system with space group P2
1
2
1
2
1
, and the lattice parameters are as follows- a=0.6952(2) nm, b=1.5150(2) nm, c=2.5359(7) nm, 7=2.53260×10
-27
m
3
, Z=4, R=0.055.Ebeiensine has an 11-deoxo-5,6-dihydrojervanine heterocyclic skeleton and a stereochem-ical structure of 5a, 14α,20β-jervanine-3β-hydroxy-6-one.At the same time, C
17
—O—C
23
was confirmed as β-configuration.
Studies on Electrochemical Behaviour of Pt Electrode in KCl Solution by
In situ
STM and EMUV-VRS
LUO Jin, LIN Zhong-hua, TIAN Zhao-wu
1992, 13(5): 662-665.
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The electrochemical behaviour of Pt polycrystalline electrode in 0.1 mol/L KCl solution was investigated by using in situ scanning tunneling microscopy (STM) and elect rochemically modulated UV-Vis reflection spectroscopy (EMUV-VRS).The results of STM and electrore-flectance effect show that the anodic dissolution/cathodic deposition is a dominant oxidation-reduction process of Pt electrode in the potential regions between 0.0 and 1.0 Vvs.SCE, and that the anodic process involves the formation of surface complex consisting of platinum ions and Cl
-
ions, and the heterogeneous dissolution of Pt electrode surface.It is also shown that STM can give much better spatial resolution than EMUV-VRS.
CO
2
Photoelectrochemical Reduction at Copper Anode Oxide Film
LUO Jin, LIN Zhong-hua, TIAN Zhao-wu
1992, 13(5): 666-669.
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The photoelectrochemical reduction of CO
2
was studied at copper anode oxide film.The anodic oxide film on copper electrode consists of Cu
2
O and CuO, which are p-type semiconductors.In the case of lower electric quantity (Q<0.10 C) for reduction, the higher Faradaic efficiencies for CH
4
were achieved on the film, and in the case of higher electric quantity for reduction, however, CH
3
OH was the main product.The Faradaic efficiency for CH
4
as a function of the applied potential, the electric quantity for reduction and the condition of forming the anodic oxide film were determined.The preliminary mechanism of CO
2
photoelectrochemical reduction is presented.
Cluster Growth Under the Field of Homogeneous Probability-Density
WANG Ze-xin, ZHANG Ji-shu, ZHAO Chang-gui, XU Zheng-ling, CHEN Zong-qi
1992, 13(5): 670-674.
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The model on self-adjusted growth of clusters was analysed and the morphologic characteristics of the cluster growth was obtained under the field of homogeneous probability-density with respect to diffusion of particles.The physical meanings of fractal dimensions characterizing the morphologic structure of clusters were revealed, which indicated the extent of the clusters self-adjusting and the interaction between the particles.Furthermore, the effects of the lattice models on the forms of the cluster growth and dynamic properties of the growth model were also investigated.
Studies on Dynamic Surface Tension of the Aqueous Surfactant Solutions
ZHANG Lan-hui, ZHAO Guo-xi
1992, 13(5): 675-678.
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The dynamic surface tensions of the aqueous solutions of per-fluorooctanoic acid, sodium dodecylsulfate and diethylene glycol mono-w-octyl ether were measured at different temperatures by the oscillating jet method, respectively.The results show that the surface adsorption of all these systems is diffusion-controlled.
Electrical Conductivity and Chemical Bonding Property of HMTTeF-TCNQF
4
Compound
LI Zhu-shi
1992, 13(5): 679-681.
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The title compound, Hexamethylenetetratellurafulvalene (HMTTeF) and tetrafluo-rotetracyano-p-quinodimethane(TCNQF
4
) with component ratio between the electron donor and acceptor being 1.07:1, was prepared by the chemical method.The degree of charge transfer of HMTTeF-TCNQF
4
, determined by X-ray photoelectron spectroscopy of 1s electrons of nitrogen and Raman spectroscopy are:ρ
xps
=0.74 and ρ
RS
=0.75, respectively.The ionization of the conjugate ρ-electron in the compound was found.The form of valence in the compound is: ([HMTTEF]
+
0.79
+[HMTTeF]
0
0.28
·([TCNQF
4
]
-
0.79
+[TCNQF
4
]
0
0.21
).This is consistent with the result of higher electrical conductivity measured.
Studies on Monodispersed Colloid(Ⅳ)——Preparation of Monodispersed Particles of Strontium Titanate
WANG Guang-xin, HOU Yao-yong, CHEN Zhong-qi
1992, 13(5): 682-683.
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A convenient and quick method for preparation of SrTiO(C
2
O
4
)
2
monodispersed sol is developed in this paper.After the particles isolated from this sol were calcined, the monodispersed spherical particles of SrTiO
3
formed.It will be possible to produce the monodispersed particles in an industrial scale by using this method.
Studies on Nitrogen Fixation in Air for Preparing Nitric Acid at Low Temperature and Low Pressure
YU Zhong-pu, LU Jian-xin, WU Tong-hao, YU Jian-feng
1992, 13(5): 684-685.
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This paper introduces a new kind of method of nitrogen fixation in air for preparing HNO
3
under the gentle conditions.Air and water were used as raw materials, NO
x
and steam of HNO
3
were used as active reaction medium.The reaction temperature and pressure are 160~360℃, 0.02~0.4 MPa, respectively.The concentration of the new product NO
x
can reach 4~6 wt%.
Infrared and Raman Spectra of [Pd
2
Cl
2
(PPh
3
)
4
]·B
12
H
12
HE Ji-ping, SUN Li, CHEN Xin-lan, ZHANG Lun
1992, 13(5): 686-687.
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The IRand Raman spectra of PdCl
2
(PPh
3
)
2
and [Pd
2
Cl
2
(PPh
3
)
4
]·B
12
H
12
were determined.Based on the observed Raman frequencies, the Pd—Cl stretching vibration can be assigned at 311-312 cm
-1
(one band) for [Pd
2
Cl
2
(PPh
3
)
4
]·Bi
2
H
12
. Similarly, the Pd-Pstretching bands are assigned at 153~156 cm
-1
and at 147 cm
-1
for [Pd
2
Cl
2
(PPh
3
)
4
] ·B
12
H
12
.
Ionic Polarization and CASP Scale of Thermal Stability Law of Perchlorates
DAI Zhang-wen, DAI Xiao-hong
1992, 13(5): 688-690.
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In this paper, a quantitative relationship between the ionic polarization and the thermal stability of perchlorates is investigated by means of the bond parameter function CASPscale.An optimized semiempirical and linear equation for estimating the thermal decomposition temperature of the perchlorates is established, and the T
d
values of some perchlorates are calculated.The results, except those for AgClO
4
, are in good agreement with the values from the literatures.
Studies on MOSE Curved Surface and Geometric Configuration of
d
9
Coordination Compound
JIAO Qing-zhu, YUE Yun-feng, HAN Cheng-li
1992, 13(5): 691-692.
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The molecular orbital stabilization energy resulting from the coordination of ligands was calculated for the
d
9
coordination compounds, in which the ligands are coordinated from different space directions into the centre ion with different distributions of electrons.The molecular orbital stabilization energy curved surface has been drawn.Consequently, the geometric configuration of
d
9
coordination compound has been satisfactorily accounted for.
Thermal and Mechanical Behavior of High Density Polyethylene/ Isotactic Polypropylene Ultradrawn Fibers
MA Rong-tang, WANG Ping-yue, Greco R., Martuscelli E.
1992, 13(5): 693-696.
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Ultradrawn fibers of high density polyethylene (HDPE)/isotactic polypropylene (iPP) blends have been prepared by hot-drawing and the influences of draw ratio and component ratio on the thermal and mechanical behavior of the ultradrawn fibers were investigated by thermal analyses and tensile tests respectively.The DSC result shows that with increasing the draw ratio, the crystallinities of HDPEand iPP, as well as their blends, and the melting temperatures are increased, whereas the melting range is reduced.The crystallinities of both HDPE and iPPare reduced in blends and the melting temperature and melting range of the two components are not affected by the component ratio.The result of tensile tests shows that the tensile modulus of ultradrawn fibers is increased with the increase of draw ratio and the tensile strength of HDPE rich-in fibers is increased with increasing the draw ratio, whereas the tensile strength of iPPrich-in fibers is decreased when the draw ratio is increased to a certain value.
The Superoxide Dismutase Activity of Binuclear Model Compounds Containing Copper (Ⅱ), Iron(Ⅲ) and Manganese (Ⅱ)
LIAO Zhan-ru, HUANG Yan, SHI Ju-en, LU Chang-lin
1992, 13(5): 697-700.
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We synthesized and characterized a ligand, N,N,N',N'-tetrakis (2'-benzimidazolyl methyl)-1,4-diethylene amino glycol ether (EGTB) and its binuclear complexes containing cop-per(Ⅱ), iron(Ⅲ) and manganese(Ⅱ).An assay of superoxide dismutase (SOD) activity was performed by means of pyrogallol autoxidation.It was found that all model compounds possess excellent SODactivity and they show more than 50% inhibition ratio in the concentration range of 10
-6
~10
-7
mol/L of the complexes.
The Weight Average Molecular Weight of Nonlinear Polycondensates
ZHAO Dong-hui, JIANG Zhen-hua, TANG Xin-yi
1992, 13(5): 701-704.
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In this paper, the method of mathematical expectation is used to study the weight average molecular weight of A
a
-B
b
(B
*
)
b
C
c
, D
d
type of nonlinear polycondensates and its expression of weight average molecular weight is obtained.The results show that the experimental values are basically coincident with theoretical ones.
Investigation on the Adsorption Properties of Thirty-five Polar Polymeric Adsorbents for Baicalin and Baicalein
MA Jian-biao, WANG Li-min, LI Jian-min, ZHAO Cun-xiang, SHI Zuo-qing, HE Bing-lin
1992, 13(5): 705-708.
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In search of a polymeric adsorbent suitable for the separation or purification of flavones and other phenolic natural products, the adsorption capacities of thirty-five polar polymeric adsorbents for baicalin and baicalein were measured respectively.The results show that some basic adsorbents possess larger capacities.The adsorption kinetics of aminomethylated cross-linked polystyrene was then determined.Its adsorption for baicalein would reach to an equilibrium in about five hours.
Studies on Acrylamide-Dicyanodiamide Macromer and Its Copolymer with Styrene (Ⅰ) ——The Synthesis and Characterization of Macromer and Its Copolymer
ZANG Qing-da, LI Zhuo-mei
1992, 13(5): 709-713.
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Acrylamide-dicyanodiamide macromer (M) is a condensation polymer of acrylamide, formaldehyde and dicyanodiamide with C=C as one of the end groups.The process of condensation was monitored by high-pressure liquid chromatography and C=C double bond was identified by
1
H NMR.Molecular wight M
w
of macromer was determined by SALLS method.Copolymer of the macromer with styrene P-M-St was prepared with AIBN as the initiator and DMSO as the solvent.The copolymer consists of hydrophobic groups along the main chain and the hydrophilic groups along the graft side chain.The graft copolymer was identified by GPC, IRspectrum and solubility-test.P-M-St with low content of styrene is water-soluble.Its charge density and degree of branching were determined by conductometric titration and its molecular weight M
w
by using SALLS method.The viscosity behavior of P-M-St in MeOH/H
2
O shows that the copolymer is a polyelectrolyte containing hydrophobic groups.
Crystal Structure of N
2
-(
p
-Toluenesulfonyl)-
L
-Giutamine
LIU Zhi-lan, ZHUO Ren-xi, ZHANG Yan-ming, ZHANG Shao-hui
1992, 13(5): 714-716.
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The title compound, an analogue of hydrolysate of antineoplaston A
10
(3-phenylacety-lamino-2,6-piperidinedione) was prepared by the condensation of L-glutamine and p-toluenesul-fonic chloride.Its crystal structure was studied by X-ray diffraction analysis.Molecular formula C
12
H
16
N
2
O
5
S, M
r
=300.31.Space group P2
1
, α=1.2784(4) nm, 6=0.5240(1) nm, c=2.1356(4) nm; α=89.96(2)°, β=93.28(2)°,γ=90.02(2)°; V= 1.4264 nm
3
, Z=4, D
c
=1.398 g/cm
3
, R=0.042.In the crystal, two molecules form a dimer with two hydrogen bonds.
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