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Table of Content
24 August 1997, Volume 13 Issue 3
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Review
Effects of Y (Ⅲ) Ions on the Fluorescence Properties of Ce(Ⅲ) Ion and the Organic Ligands in the Complex
LI Wen-lian, Takayuku Mishima, Gin-Ya Adachi, Jiro Shiokawa
1997, 13(3): 189-194.
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The enhancement effects of Y ( Ⅲ) ions on the fluorescence of Ce ( Ⅲ) in Ce ( Ⅲ)-Y ( Ⅲ)-PMMA (polymethylmethacrylate ) or Ce ( Ⅲ)-Y ( Ⅲ)-PVC (polyvinyl chloride ) complex systems were observed. The influence of Y ( Ⅲ) ions on the emission spectra of PMMA ligands in PMMA-Y ( Ⅲ) and the fluorescent enhance- ment of Y( Ⅲ) on Ce( Ⅲ) emission in PMMA-Ce-Y by Y( Ⅲ) ion were studied. It was also of interest to note that when Y ( Ⅲ) ions were added into PMMA and into bpy(bipyridine ), respectively, the emission spectrum of PMMA ligands was split into fine structure bands by Y ( Ⅲ), and the fluorescence intensities of bpy ligands in bpy-Y ( Ⅲ) complexes were considerably increased.
Articles
Synthesis, Structure and Properties of Inverse-Keggin Potassium Tetraniobooctatungstosilicate
YUE Bin, TANG Li-hao, RUI Cheng-guo, LIU Hui-zhang, JIN Song-lin, ZHU Si-san, LIU Jie, CHEN Min-yin
1997, 13(3): 195-200.
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Potassium tetraniobooccatungotosilicate, K
8
[SiNb
4
W
8
O
40
]·12H
2
O was pre-pared by the reaction of white powdery tungstic acid, potassium niobate and potas -sium silicate in aqueous solution with pH value adjusted by potassium carbonate。The heteropolyniobotungstate crystallized in cubic space group P
m3m
with unit cellparameters ;: a = 1.0640(1)nm,Z=1,V=1 .2045(5)nm
3
,R=0.055,R
w
=0.062。The anion has inverse,Keggin structure,in which the central SiO
4
tetrahedron isdistributed statistically in two orientations。The twelve outer metal positions arerandomly occupied by four niobium and eight tungsten atoms. Moreover, infraredspectrat electronic :spectra and thermogram were measured。
Studies on the Binding of Tris(1,10-phenanthroline)Nickel(Ⅱ) to Calf Thymus DNA
JIN Lan, YANG Pin, LI Qing-shan, YANG Bin-sheng
1997, 13(3): 201-206.
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Absorbance and fluorescence methods were used to study the interaction of - and A-tris (phenanthroline) nickel ( Ⅱ) complex with calf thymus DNA. It was con- cluded that Δ-Ni(phen)
3
2+
preferentially bound to DNA. Especially the fluorescence Scatchard plots were discussed for the binding of EthBr to calf thymus DNA in the presence of varying concentrations of the metal complex. Theses studies indicated that both the isomers bound to DNA by two acting types, namely, intercalative and electrostatic bound modes.
Voltammmetric Determination of Uric Acid in the Presence of Ascorbates Using OveroxidizedPolypyrrole Film Coated Glassy Carbon Electrodes
KANG Tian-fang, SHEN Guo-li, YU Ru-qin
1997, 13(3): 207-214.
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The voltammetric behaviour of uric acid at overoxidized polypyrrole (OPPY ) film-coated glassy carbon (GC ) electrodes was investigaied. The chemically modi- fied electrodes exhilbited an excellent permselectivity for uric acid of undissociated form in an acidic medium. The current response sensitivity of uric acid at the modi- fied electrodes was markedly increased by properly anodizing activation of underly- ing electrodes and overoxidizing treatment of polypyrrole film. The voltammetric response of uric acid at the chemically modified electrode was linearly related to itinvestigatedtion in the range of 4. 0 ×10
-7
—8. 0 ×10
-5
mol/L in pH 5 buffer solu- tions. Ascorbic acid in less than 150-fold excess did not interfere with the voltam- metric determination of uric acid. The proposed procedure was utilized to determine uric acicl in human urine and serum samples without any pretreatment.
Separation and Determination of Basesby Capillary Zone Electrophoresis
ZHAO Tao, LIU Qi-ping, CHENG Jie-ke
1997, 13(3): 215-220.
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The present paper covers the separation and determination of cytosine, 9-N-di- hydroxypropyltheophylline, theobromine, adenine, guanine, uracil, theophylline, 1-hydroxyethyl-5-fluorouracil, xanthine, uric acid, 6-mercaptopurine, 5-fluo- rouracil and 1 -propionyloxyuracil by capillary zone electrophoresis. In an uncoated silica capillary(70 cm ×75 μm i. d. effective length 63 cm), thirteen bases could be separated within 11 min under the optimum conditions : 0.01 mol/L(pH 10.0) bo-rate buffer, 40℃, 15 kV, 260 nm and 2 s load. Efficiencies up to 3.1 ×10
5
theoreti-cal plates (4.9 ×10
5
plates/m) were achieved.
Detection of Catecholic Compounds withField-ampilfied CZE-Amperometry
HU Shen, PANG Dai-wen, HU Yong-gang, CHENG Jie-ke
1997, 13(3): 221-228.
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On-column sample stacking technique has been used extensively in capillary zone electrophoresis (CZE) to enhance the sensitivity of the measurements with UV-Vis detection. However, the detection limits for CZE-separation are still limit- ed due to the poor sensitivity of a UV-Vis detector. We incorporated field-amplified sample stacking technique into CZE with amperometric detection. Compared with the conventional electromigration injection, a negative peak of water was observed and a great enhancement of signals was obtained. The results in phosphate buffer with sodium dodecyl sulfate (SDS ) and 2-N-(morpholino) ethane sulphonic acid ( MES ) buffer were compared. Subnanomolar concentration limits for cate- cholamine neurotransmitters (dopamine, norepinephrine, epinephriine) and isopro- terenol were achieved in the 25 um capillary with two or three orders of magnitude lower than those with amperometric detection reported previously.
A New Method for Brucine AnalysisBased on Its ChemiluminescenceReaction with Potassium Permanganate
YANG Min-li, FENG Man-Iang, LU Jiu-ru
1997, 13(3): 229-234.
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The chemiluminescence reaction between potassium permanganate and brucine was thoroughly investigated, and a new method for brucine determination based on the chemiluminescence reaction was established. The method possesses the poten- tial advantages of simplicity on instrument, high sensitivity and precision, commer-ically available reagents to be used, and is suitable for on-line analysis. The linear range and detection limit of this method are from 4 ×10
-9
to 8×10
-5
g·mL
-1
and 1. 5 ×10
-9
g·mL
-1
, respectively. The standard deviation in the whole linear range is less than 2.0%. This method has been used to determine the brucine in nux vom- ica with a recovery ratio of 97% to 108%.
New Application of bond Function Basis Sets──ab initio Calculations of Nonlinear OpticalProperties of CH
4-n
F
n
(n=1,2,3)
Li-Zhi-ru, TAO Fu-ming, PAN Yuh-kang, FENG Ji-kang, WU Di, HUANG Xu-ri, SUN Ghia-Chung
1997, 13(3): 235-239.
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On the basis of adding the bond functions (3s 3p 2d) to the basis sets 6-311G ( 2d 2p ) for increasing the efficiency of the basis sets, we have carried out the MP2 calculations of nonlinear optical properties includintg dipole moment uo,polarizibili- ty μ
o
and hyperpolarizability β
o
for CH
4-n
F
n
(n = 1, 2, 3). The results are in good a- greement with those of experimentsl The roles of the bond functions in the calcula- tions are shown (μ
o
, α
o
, β
o
) the improved values of the properties are about 2%-7% at the SCF level and about 6%-30% at the correlated level (MP2). It is shown that the more important role of the bond functions in calculating is the im- provement of the effects of the corrections of electronic correlations and the increase of the effects is in the order of μ
o
<α
o
<β
o
In addition, it is also shown that the cal-, culated value of a property does not change with the bond-function location in our calculations except for the regions close to the nuclei in a molecule.
On the of Bond Function in NonlinearOoptical Property Calculations forHF, HCI, LiH,H
2
O and NH
3
Zhi-ru, TAO Fu-ming, PAN Yuh-Kang, FENG Ji-Kang, SUN Chia-Chung
1997, 13(3): 240-243.
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Dond function basis sets have been used to calculate the molecular nonlinear optical properties which include hyperpolarizability β
o
, polarizability a
o
, and dipole moment μ
o
for six molecules. The calculations at the fourth-order Moller-Plesset approximation (MP4) have recovered more than 90% of the experimental values β
o
, comparecl to that as low as 75% by the other authors. The calculated values of α
o
and μ
o
are also in good agreement with those of experiments and superior to that from other work. It is shown that the bond functions improve the calculated results at SCF level and especially at the level of the correction of electronic correlation (MP2 and MP4).
Studies on the Mechanism of the Direct Synthesisof Styrene form Benzene and Ethylene
ZHANG Qiang, JIN Ri-guang, YANG Jun
1997, 13(3): 244-248.
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The adsorption behavior and description behavior of benzene, ethylene and ethylbenzene over HZSM-5 and Co/HZSM-5 catalysts were studied by means of TPSR (Temperature programmed surface reaction) technique. TPSR results of ben- zene and ethylene co-adsorption show that the maian products are styrene, ethylben- zene, toluene, propane, and butane. In a separate experiment of ethylbenzene ad- sorption, styrene . toluene and benzene are formed due to cracking and dehydro- genation. The mechanism of styrene formation was proposed, i. e., the reaction was carried out via. the dehydrogenation of mediate species ethylbenzene according to the results of TPSR-MS, activity testing and thermodynamic analysis.
IN SITU Confocal Microprobe Raman SpectroscopicStudies on Defective La-based Complex Oxides
CHEN Du-hui, CAI Jun-xiu, LIAO Yuan-yian, WAN Hui-lin
1997, 13(3): 249-255.
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The adsorption of O
2
over defective La
2
O
3
-based OCM catalysts with anionic vacancies, and the reaction of surface oxygen species with CH
4
were studied by means of in situ confocal microprobe Raman spectra. The partially reduced oxygen species O
2
-
, O
2
2-
, O
2
δ-
(O<δ<1 ) and even the lattice oxygen ion O
2-
can be detected on the surface of O
2-
pretreated La
2
O
3
-based catalysts. At lower temperatures (< 573 K) it is peroxide species O
2
2-
or O
-
that is more essential for the coupling of methane,while at higher temperature. the superoxide O
2
-
and lattice oxygen species O
2-
are rather important. It is easier for fluoride-containing La
2
O
3
-based catalysts to induce the oxygen species with fewer negative charges and the basicity of the cat- alyst surface is weakened, so that the C
2
selectivity for OCM reaction is improved.
Theoretical Studies on the Structures and Reactions of Halocarbenoids(Ⅰ)Structures and Stability of Chlorocarbenoid CHCl
2
Li-LI Ji-hai, FENG Sheng-yu,Liu-Wei
1997, 13(3): 256-261.
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The chlorocarbenoid, CHCl
2
Li, was studied by means of ab initio molecular orbital theory. Three equilibrium structures and two isomerization transition states were located. The calculations showed that the three-membered ring structure is the most stable. The "classical tetrahedral" structure is not the local minimum on the potential energy surface.
Quantum Chemistry Studies on the Heteropoly Bluesof Molybdosilic Series with α-Keggin Structure
FU Qiang, YANG Ming, CHEN Bin, WANC En-Bo, XIE De-Min, JIANG Zhong-Ming,PENG Jun
1997, 13(3): 262-267.
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SCC-DV-X method was used for the theoretical calculation of heteropoly an- ion, [SiMo
12
v1
O40]
4-
,
and heteropoly blue anions,[SiMo2
v
Mo10
v1
O40]
6-
and [SiMo4
v
Mo8
v1
OO40]
8-
. The frontier molecular orbitals, orbital energies, Fermi 1evels, the occupied numbers of basis functions, free valences, Mulliken populations and the figure of the total density of states have been obtained. The theoretical analysis indicates that all the atoms in the anions participate in chemical reactions, but Oc and Od have higher chemical activities than other atonts, which is supported by the ex- perimental results. The heteropoly hue anions with the α-Keggin structure distort a little and the levels of valence orbitals demonstrate that [SiMo4
v
Mo8
v1
OO40]
8-
can form a six-electron heteropoly blue anoint by accepting two electrons.
Preparation of YSZ Microporous Membranes on Porous a-Alumina with Metal Chlorides as Precursor
PENG Ding-kun, LIU Tao, YANG Ping-hua, XIA Chang-rong, MENG Guang-yao
1997, 13(3): 268-275.
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A sol-gel process for YSZ membrane prepared with less expensive chemicals, ZrOCI
2
·8H
2
0 and YC1
3
, has been developed. The sol viscosity as a function of concentration, acidity and temperature was brane formation processes were also studied. investigated. And gelation and Based on an optimized procedure memhole and crack-free YSZ membranes with the pore size less than 100 nm have obtained on coarse porous a-alumina.
The Electrochemical Polymerizationof Brilliant Cresyl Blue and ItsElectrocatalytic Oxidatiomn for NADH
WANG Yun, ZHOU Dong-mei,CHEN Hong-yuan
1997, 13(3): 276-282.
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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