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Table of Content
24 August 2001, Volume 17 Issue 3
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Articles
Synthesis and Structure of an Interlock Network Frame of Cobalt(Ⅱ) Coordination Polymer {[Co(azpy)
2
(NCS)
2
]·1/4EtOH·1/2H
2
O}
n
(azpy = 4,4' -Azobispyridine)
LI Bao-long, XU Yan, LIU Yong-jiang, XU Zheng
2001, 17(3): 237-242.
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A compound {[Co(azpy)
2
(NCS)
2
]·1/4EtOH·1/2H
2
O}
n
(1), where azpy=4,4'- azo-bispyridine, was synthesized and characterized by means of IR, TGA-DTA, magnetic susceptibility and X-ray single crystal diffraction.It consists of two independent sets of fully interlocked two-dimensional networks with the dihedral angle 61.7°, organized in parallel stacks of the sheets which are made of edge-shared [Co(Ⅱ)]
4
squares separated by 0.906 2 nm, and defined size rhombic channels.The thermal gravimetric analysis indicates that the framework is stable up to 198 C.The variable-temperature magnetic susceptibility measurements indicated that there is a weak antiferromagnetic interaction between the cobalt(Ⅱ) ions in the complex (1).
Studies on the Interaction of Cobalt Mixed-Ligand Coordination Compound Containing Tetrapyrido [3,2-a: 2′ 3′-c: 3″ 2″ h: 2′″, 3′″-j] phenazine with DNA
SONG Yu-fei, YANG Pin
2001, 17(3): 243-248.
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A new monometallic complex [Co(phen)
2
tpphz]
3+
(where tpphz is tetrapyrido [3,2-a: 2′,3′-c: 3″,2″-h: 2′″,3′″-j] phenazine) was synthesized by the reaction of 5,6-diamino-1,10-phenanthroline with [Co(phen)
2
(phendione)]
3+
.It was characterized by elemental analysis, molar conductivity, IR,
1
H NMR, ultraviolet and fluorescence spectroscopy.The interaction of the complex with DNA was also investigated.The complex shows the absorption hypochromicity, fluorescence enhancement, the specific viscosity increased when bound to calf thymus DNA.The cyclic voltammetry (CV) measurement showed a change in peak current with the addition of DNA.All the results provide the support for the intercalative binding mode of the mononuclear complex.
Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H
3
NC
2
H
4
NH
2
]VOPO
4
ZHANG Dong, SHI Zhan, FENG Shou-hua
2001, 17(3): 249-252.
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An inorganic-organic hybrid compound, [H
3
NC
2
H
4
NH
2
]VOPO
4
was synthesized by meansof the hydrothermal method.It was crystallized in a monoclinic system, a space group P2
1
/c,with the crystal cell parameters: a=0.922 85(11) nm, b=0.729 94(9) nm, c=0.984 95(11)nm, β=101.280(3)°, V=0.650 67(13) nm
3
, M
r
=223.02 g/mol, D
c
=2.277 g/cm
3
, Z=4,R= 0.031 5, ωR= 0.086 5, GOF = 1.085.The VO
5
N octahedra chains are corner-linked byPO
4
tetrahedra; the VO
5
N octahedra are all trans-linked with V-O bonds being alternately short and long.The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO
4
from a neighboring sheet.The elementary analysis, infrared spectrum characters and thermal stability were also given.
Flow Injection Determination of Oxalate Based on Its Catalytic Effect on the Oxidation of p-Chloride Aniline by Dichromate
LI Li-jun, WEI Hong-guang, ZHANG Ying
2001, 17(3): 253-258.
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In a sulfuric acid medium, oxalate exhibits a strong catalytic effect on the oxidation of p-chloride aniline (ClBN) by dichromate, and the red oxidation product of ClBN has a maximum absorbancy at 520 nm.Based on this founding, a new FI method for determining oxalate was developed.A calibration curve of oxalate in the range of 0.40-17.0 tg/mL was obtained.The detection limit was 0.10 μg/mL.Sampling rate was 103-samples/h.The possible interference by the co-existing substances or ions was examined.This new method was applied to the determination of micro amounts of oxalate in real samples with satisfactory results.
A Convenient Synthesis of Chrysin and Tectochrysin
ZHU Jin-tao, CHEN Ying-qi, DAI Li-yan, SUN Li-wen, YAO San-jing
2001, 17(3): 259-263.
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Chrysin(1) and tectochrysin(2) were respectively synthesized in four steps from 1,3,5-tri-bromobenzene in an overall yield of 46.8% and that of 37.0% with the key step being theBu4NBr catalyzed hydrolysis of 1-phenyl-3- (2', 4',6'-trimethoxyphenyl)-1,3-propanedione (11) under different conditions.
Cobalt Determination by Means of Flow Injection On-line Sorbent Preconcentration-Flame Atomic Absorption Spectrometry with 1-Nitroso-2-naphthol as a Complexing Reagent
YIN Xue-feng, ALI Akbar, XU Guang-ming, LING Yun-yang, GAO Jian, YE Mei-ying
2001, 17(3): 264-270.
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The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcen tration of cobalt eluted on the C
18
microcolumn by means of the FI-FAAS system was tested.Various parameters affecting the complex formation and its elution were optimized.A 2.3 × 10
-3
mol/L reagent solution and the aqueous sample solution acidified with 0.1 % (volume fraction) nitric acid were on-line mixed (6.4 mL/ min) on a reaction coil set at (65 ±1) ℃ and flowed through the microcolumn for 30 s.The pH of the mixed solution was adjusted to 3-4 with HNO
3
(1 mol/L) or NaOH(1 mol/L).The adsorbed complexes in the microcolumn were eluted into the nebulizer of FAAS in 10 s with ethanol acidified with 1 % HNO
3
(3.0 mL/min).A good precision(1.6 % for 100 μg/L Co(Ⅱ), n=10), a high enrichment factor 17.2, with detection limit (3σ) 3.2 μg/L, and sample throughput (90 h
-1
) were obtained.The method was applied to the certified reference materials(CRMs), NBS-362 and NBS-364, for the determination of cobalt and the results were in good agreement with the certified values.
Syntheses and Configuration Inversion of Substituted Oxazolines
YANG Shao-rong, HU Quan-yuan, LIU Jun, YANG Hui, HU Xian-ming
2001, 17(3): 271-275.
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The present paper covers the simply and highly stereoselective syntheses of (α-S, 4S)-2-dichloromethyl- 4, 5-dihydro-α- (4-nitrophenyl)- 4-oxazolemethanol (4a), (α-S,4S)-2-methyl-4,5-dihydro-α- (4-nitrophenyl)-4-oxazolemethanol (4b), and (α-R, 4R)-2-dichloromethyl-4,5-di-hydro-α- [ (4-methylsulfonyl) phenyl] - 4 -oxazolemethanol (4c) with good yields (80 % - 900%).A configuration inversion product, (1R, 2S)-2-dichloroacetamido-1-(4-nitrophenyl)-1, 3-propane-diol (8), was obtained during our attempting to convert compound 4a into (4S, 5R)-2-(dichloromethyl)-4,5-dihydro-5- (4-nitrophenyl)-4-oxazolemethanol(7).
Langmuir-Blodgett Films from Schiff Base Aluminium (Ⅲ) Complex
LIAN Wei, CAO Wei, WANG Gang, WEI Li, HONG Xia, SHEN Dong-fang, LIU Chun-yan, SHAO Hui-bo, BAI Yu-bai
2001, 17(3): 276-280.
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The characteristics of the LB films of Schiff base aluminium(Ⅲ), tris(2-hydroxy-5-nitro N-dodecyl-benzylideneaminato) aluminium (Ⅲ) [Al (TA 12)
3
], were studied.The surface pres sure-area(r-A) isotherm of Al(TA12)
3
in the pure water subphase was investigated.The molec ular area, 0.48 nm
2
, is one-third of the expected value that indicates the formation of an aggre gate.The Langmuir-Blodgett (LB) films of Al(TA12)
3
were transferred and characterized.The UV-Vis spectra and the AFM image both confirmed that the J-aggregates formed.The polarized UV-Vis spectra indicated that the complex plane had to be oriented with an angle of about 30° to the substrate surface.The IR spectra suggested that the complexation took place between aluminium ions and the oxygen atoms of the ligand rather than the nitrogen atom.
Iron-Doped Titania Nanoparticles for the Photocatalytic Oxidative Degradation of Nitrite
XU An-wu, ZHU Jing-yan, GAO Yuan, LIU Han-qin
2001, 17(3): 281-286.
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Iron-doped titania nanoparticles exhibit a higher photocatalytic activity than pure TiO
2
for the degradation of nitrite.The optimum Fe-doped content in terms of activity is approximately 0.5 %.The increase in photoactivity is probably due to the higher adsorption and the inhibition of electron-hole recombination.The photocatalytic oxidation reaction of nitrite over the Fe-doped TiO
2
catalyst follows zero-order kinetics, which is different from that over pure TiO
2
.The reaction rate decreases linearly with the increase of the pH of the solution.
Electrocatalysis of Oxygen Evolution Reaction on Ti/SnO
2
+ RuO
2
+ MnO
2
/MnO
2
Electrode in Sulfuric Acid Solution
LIANG Zhen-hai, FAN Cai-mei, SUN Yan-ping
2001, 17(3): 287-292.
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The Ti-Supported MnO
2
electrode was modified by introducing SnO
2
+RuO
2
+MnO
2
as an intermediate layer into the Ti/MnO
2
interface.The anodic polarization curves were measured at various temperatures ranging from 30 to 80 ℃ and the activation energy for the oxygen evolution reaction was evaluated.The experimental activation energy increased linearly with increasing the overpotential.The activation energy at the equilibrium potential was linearly correlated with the difference between the crystal field stabilization energies of Mn
4+
at initial state and Mn
4+
at transition state.The electrocatalysis characteristics of the anode were discussed by means of themechanism of the substitution reaction of the ligand(S
N
1 and S
N
2) and molecular orbital theory.The results show that the anode has better electrocatalystic characteristics.
Catalytic Oxidation of Hexanol to Hexanal with H
2
O
2
Over P-W Heteropoly Compounds
ZHOU Guang-dong, GUO Xiao-hong, LIU Yan, BI Ying-li, ZHEN Kai-ji
2001, 17(3): 293-298.
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The syntheses of Keggin and Dawson-structural phospho-tungsto heteropoly compounds and their Peroxo-derivatives(PCWP), and the catalytic performance over this series of catalysts for the selective oxidation of hexanol to hexylaldehyde are reported.By means of IR, NMR and UV-DRS techniques the catalysts were characterized and a comparison of the structural properties of these catalysts before and after the reaction was made.The correlation between the catalytic performance and the structure of this series of catalysts was discussed as well.
Bioscillation and Birhythmicity in the H
2
O
2
-KSCN-CuSO
4
-NaOH System
GAO Qing-yu, SUN Kang, MENG Fan-yong, CAI Zun-sheng, ZHAO Xue-zhuang
2001, 17(3): 299-304.
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Two kinds of different mechanistic oscillations can be displayed in the H
2
O
2
-KSCN-CuSO
4
NaOH system.One discovered by this study is the pH oscillation in a continuous flow stirred tank reactor(CSTR) resulting from the oxidation of KSCN.The other is the oscillation of H
2
O
2
experimental conditions, the system exhibits a birhythmicity in a CSTR.Two different pH oscillations are reported here.The pH oscillations which accompany the decomposition of H
2
O
2
exist in the batch reactor and the CSTR at a high flowrate, but the pH oscillations in a CSTR at a low flowrate originates from proton positive and negative feedback in the oxidation of KSCN.The os-cillation of non-catalyzed oxidation of KSCN by hydrogen peroxide in a CSTR can be found.Also we have observed whether Cu
2+
exists or not in the batch system, the pH increases to near neutral ultimately after pH drops twice.
A Quantum Chemistry Study of Inhibition Properties of Imidazole and Its Derivatives on Iron Surface Corrosion
YAN Xiao-ci, XIA Wen-bing, LIU Jie, OU YANG-li, LUO Ming-dao, YANG Feng, MIN Xin-min
2001, 17(3): 305-310.
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The geometries of imidazole and its derivatives were respectively optimized by using ab initio method, and the molecular orbital energy levels and the charge densities were obtained for their optimum geometries.The frontier orbital energy levels, and the net charges of N (1) atom and the imidazole ring of those molecules were obtained with ab initio and SCC-DV-Xα methods.It was found that the inhibition properties of those compounds change with the highest occupied molecular orbital energy levels, and the net charges of N(1) atom.We took four iron atoms on the crystal plane (100) of α-iron as the surface which was used to study the adsorption towards the inhibitors.The adsorption models of the inhibitor to be adsorbed on the Fe-cluster surface were optimized with SCC-DV-Xα method.It turns out that the most favorable model is that the inhibitor molecule is adsorbed on the Fe-cluster surface in an inclined state.The calculation shows that the stabilization energies of the systems are well correlated with the inhibition efficien cies.
Analytic Solution of the Three-Variable Dynamical Equations of Oscillation Phenomena in B-Z Reaction
LU Ling
2001, 17(3): 311-314.
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The dynamical behaviour of the inorganic bromate oscillator catalyzed by manganese ions in the B-Z reaction is discussed, a three-variable nonlinear dynamical equations of the oscillation phenomena have been obtained, and an analytic solution and numerical results of the equations are given.
Conformation of 1,2-Dimethoxyethane in Water
LIU Yue, YANG Xiao-zhen, DAI Bai-qing, SU Zhong-min, WANG Qi
2001, 17(3): 315-317.
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To understand the conformation of 1,2-dimethoxyethane (DME) in water, a system of two kinds of molecules, DME and H
2
O, was focused.The interaction of various conformers of DME with water was studied by means of ab initio molecular orbital calculation with 6-31G(d)basis set.It is shown that there are two forms of interactions between the two molecules in the sys tem, the close touched (H
2
O attaches to the two oxygen atoms of DME) and the open touched (H
2
O attaches to one oxygen atom of DME) structures.The conformation of DME is remark ably influenced by the interactions.Instead the ttt conformer is preferred in the gas state, with a close touched H
2
O the tgt conformer becomes the most stable one.The obtained hydration ener gies show that the stabilized order of DME conformers by water is tgt＞tgg'＞ttt.
Studies on the Coordination Polymer of Copper Electropolyurushiol
TANG Jie-yuan, ZHANG Wen-gong, SHEN Guo-cai, GAO Feng
2001, 17(3): 318-324.
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The coordination polymer of copper electropolyurushiol(EPU-Cu
2+
) was obtained by the reaction of copper chloride with electropolyurushiol (EPU) in an isopropyl alcohol solution.The properties of EPU-Cu
2+
were studied by means of ESR, FTIR, XPS, DMTA and TG-DTA.The results of AES show that the content of Cu
2+
was 8.63%.The electric resistances of EPUCu
2+
and EPU were determined to be 9.37×10
10
Ω and 7.90×10
10
Ω respectively.It was also ascertained that in EPU-Cu
2+
each Cu
2+
is coordinated with two units hydroxyl in EPU, making the EPU-Cu
2+
cross-link further.As a result, the title polymer exhibits an insolubility in most of organic solutions, a higher glass transition temperature and thermal resistance.
Microemulsion Polymerization of Methyl Methacrylat
DAN Yi, YANG Yun-hua, CHEN San-yu
2001, 17(3): 325-330.
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The microemulsion polymerization of methyl methacrylate was studied.The effects of feeding modes on the structure and the properties of the obtained polymer microlatex were investigated by measuring the conversion, the transmittance and the refractive index of the latex, and by measuring the particle size, the molecular weight and the glass transition temperature (Tg) of the polymers.The results show that compared to the batch feeding mode, the semi-continuous feeding mode is more favorable to form a PMMA microlatex with a higher transmittance, a smaller particle size, a higher molecular weight and a higher T
g
.And the obtained PMMA microlatex has a 30 %-40 % (mass fraction) polymer content, a 0.03 emulsifier/water weight ratio, a 0.05emulsifier/monomer weight ratio and a 17 nm average particle diameter, which is very important for the industrialization of the microemulsion polymerization technique.
Letters
Hyperbranched Polyurethane Acrylate Applied to UV Curable Flame Retardant Coatings
ZHU Sheng-Wu, SHI Wen-Fang
2001, 17(3): 331-333.
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)
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Graft Polymerization of Acryloyloxystarch with Poly(D,L-lactide) Macromonomer--A Potential Drug Delivery Carrier for Oral Administration
WANG Li-qun, TU Ke-hua, WANG Yan-bing, LI Xiang-rong
2001, 17(3): 334-337.
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Research Notes
Some Rare Earth Metallic Organohydrides with Biindenyl as the Ligand
GE Yue, YUE Zheng-yu, GAO Jin-sheng, YAN Peng-fei
2001, 17(3): 338-340.
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)
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Studies on the PEO-PPO-PEO Block Copolymer Release from Alginate Hydrogel
SU Yan-lei, GUO Chen, LIU Hui-zhou
2001, 17(3): 341-346.
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)
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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