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Table of Content
24 June 2004, Volume 20 Issue 3
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Articles
Surface-treatment of Alkaline Earth Sulfides Based Phosphor
GUO Chong-feng, CHU Ben-li, XU Jian, SU Qiang
2004, 20(3): 253-257.
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A series of alkaline earth sulfides based phosphors Ca
0.8
Sr
0.2
S∶Eu
2+
, Tm
3+
were covered with a layer of protective coating with alkaline earth fluorides by heating the mixture of phosphor and NH
4
HF
2
at elevated temperatures. The coatings were characterized by means of XRD and SEM. The optical properties of the coated phosphors and the influences of the coating on their properties have been discussed extensively. The stabilities of the coated and uncoated phosphors have been compared.
Synthesis, Structure Characterization and Biological Activity of Adenine Salt of 12-Phosphotungstic Acid
LI Juan, QI Yan-fei, HAN Zheng-bo, WANG En-bo, LI Jing, WU Xin-yu, WANG Hong-fang
2004, 20(3): 258-261.
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A novel adenine(Ade) salt of 12-phosphotungstic acid was synthesized and characterized by elemental analyses, IR,
1
H NMR, CV and single crystal X-ray diffraction. The compound crystallized in a triclinic system with a space group P1 and a=1.3108(3) nm, b=1.3515(3) nm, c=1.3870(3) nm, V=2.0217(7) nm
3
, Z=1, R
1
=0.0391, wR
2
=0.0959. The structure unit of the complex was constructed from [HPW
12
·O
40
]
-
, (C
5
H
6
N
5
)
+
and C
3
H
7
NO, which further extends to form a novel three-dimensional host-guest network via hydrogen-bonding interactions. The anti-tumor activity of the compound was examined in two human tumor cell lines in vitro.
Investigation of Light-harvest Material: Synthesis and Characterization of Nanometer Porphyrin Trimer
SHI Ying-yan, WANG Xing-qiao, LI Xiang-qing, ZHENG Wen-qi, DING Hong, ZHU Guang-shan, LIU Guo-fa
2004, 20(3): 262-265.
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ω-Bromopropylporphyrin ether synthesized from the raction of 1,3-dibromopropane as the bridge-linked reagent and 5-(4-hydroxyphenyl)-10,15,20-triphenylporphyrin (H
2
MHTPP) as the matrix reacts with 5, 15-di(4- hydroxyphenyl)-10, 20-diphenyl porphyrin(trans-H
2
DHDPP) to give the title nanometer porphyrin trimer. The characterization was carried out by means of elemental analyses, UV-Vis, IR,
1
H NMR and XRD.
Hydrothermal Synthesis and Characterization of [V
16
O
38
(Cl)][Cu(enMe)
2
]
3.5
·2H
2
O Containing {V
16
O
38
} Cluster
CUI Xiao-bing, ZHENG Shou-tian, SUN Yan-qiong, YANG Guo-yu
2004, 20(3): 266-269.
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Compound [V
16
O
38
(Cl)][Cu(enMe)
2
]
3.5
·2H
2
O(1) has been hydrothermally synthesized and characterized by means of single-crystal X-ray diffraction, elemental analysis, IR, EPR and TGA analysis. The X-ray crystallography shows that compound 1 contains a new {V
16
O
38
} cluster shell, which is connected by [Cu(enMe)
2
]
2+
coordination fragments into a 3-D framework. The compound crystallized in a monoclinic system with space group P2(1)/n, M=2235.82, a=1.26076(3) nm, b=2.55802(6) nm, c=2.14742(4) nm, β=90.7380(10)°, V=6.9250(3) nm
3
, Z=4, F(000)=4418, D
c
=2.145 g·cm
-3
, μ=3.227 mm
-1
,(Δ/σ)=0.000, S=1.066.
Synthesis and Characterization of 2-Decyl-DTPA and Its Gd(Ⅲ) Chelate
FENG Zhi-ming, LI Feng, CHEN Rong, ZHU Xiao-juan, LI Xiao-ru
2004, 20(3): 270-273.
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The present paper covers the synthesis and the characterization of ligand 2-decyl-3, 6, 9-tris(carboxymethyl)-3,6,9-triazaundecan-1,11-dioic acid, H5L, and its Gd(Ⅲ) chelate. The protonation constants for H
5
L(lgK
i
H
=10.90, 8.50, 4.55, 2.92, 2.20) and the stability constant for GdL
2-
(lgK
GdL
2-
=22.80) were determined by means of potentiometric titration. They are similar to the corresponding values of DTPA and Gd-DTPA, respectively. The results obtained show that the basicity of the ligand and the stability constant of its Gd(Ⅲ) chelate are not obviously altered after the introduction of a linear chain decyl group into the terminal acetic acid residue of DTPA. The Gd(Ⅲ) chelate may be a potential contrast agent with liver-specificity for magnetic resonance imaging(MRI).
Synthesis of Five-coordinated Anionic Tin(Ⅳ) Complexes and Crystal Structure of [(I-Pr)
2
NH
2
][PhSn(μ
2
-SCH
2
COO)
2
]
ZHONG Gui-yun, SONG Hai-bin, XIE Qing-lan, SUN Li-juan
2004, 20(3): 274-276.
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Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R
n
NH
4-n
][PhSn(μ
2
-SCH
2
COO)
2
] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR,
1
H NMR and MS spectroscopies. The crystal structure of [(i-Pr)
2
NH
2
][PhSn(μ
2
-SCH
2
COO)
2
] was determined by X-ray diffraction. In the crystal structure, the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a=1.1766(11) nm, b=1.3144(14) nm, c=1.3336(15) nm, β=90° and Z=4.
A Novel Layered Complex with Rhomboidal Channels: Hydrothermal Synthesis, Crystal Structure, and Properties of Cu(4,4′-bipy)
2
(H
2
PO
4
)
2
(H
2
O)
2
(bipy=bipyridine)
MAO Hong-yan, LIU Hong-lei, ZHANG Hong-yun, XU Chen, WANG En-bo, HAN Hua-yun, WU Qing-an, ZHU Yu
2004, 20(3): 277-280.
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The combination of both 4,4′-bipyridine(4,4′-bipy) and dihydrogen phosphate anion ligands with copper(Ⅱ) results in the formation of a novel layered compound Cu(4,4′-bipy)
2
(H
2
PO
4
)
2
(H
2
O)
2
. The crystal structure comprises discrete neutral Cu(4,4′-bipy)
2
(H
2
PO
4
)
2
(H
2
O)
2
units. The copper atom, located on the crystallographic twofold axis, is coordinated with two nitrogen atoms of terminal 4,4′-bipy ligands and two water molecules at the equatorial positions, and two dihydrogen phosphate oxygen atoms at the axial positions, forming an elongated octahedron. The complex is a two-dimensional distorted rhomboidal network possessing two kinds of rhomboids with dimensions of ca. 1.6792 nm×0.3203 nm and 1.2778 nm×0.3198 nm, respectively. The two-dimensional networks are stacked parallelly on each other along c-axis to give an extended three-dimensional channel network with an interlayer distance of ca. 0.5030 nm. Crystal data: triclinic, space group P1, a=1.0253(2) nm, b=1.4501(3) nm, c=0.79715(16) nm, α=97.91(3)°, β=90.99(3)°, γ=85.54(3)°, V=1.1703(4) nm
3
, Z=2, R=0.0892, wR=0.2451.
A New Equation for Solute Retention in Liquid Chromatography
BIAN Liu-jiao, YANG Xiao-yan
2004, 20(3): 281-284.
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In consideration of the adsorption of solvent, diluent and solute molecules on the surface of a stationary phase, a new equation for solute retention in liquid chromatography is presented. This equation includes three parameters: the displacement equilibrium constant(K
sd
) between the solvent and diluent molecules on the surface of the stationary phase, the total number(N) of the solvent and diluent molecules released from the stationary phase after one solute molecule being adsorbed, and the parameter(I) related to the thermodynamic equilibrium constant for the solute adsorption on the stationary phase. Over the whole concentration range of the solvent in the mobile phase, the experimental retention data can be well described by this equation, parameters K
sd
, N and I can be obtained by the regression analysis of the experimental retention data, and consequently the number of the solvent and the diluent molecules displaced by one solute molecule from the stationary phase can also be derived at different solvent concentrations in the mobile phase.
Researches on Formation of Haloacetic Acids in Chlorination of Drinking Water by a Novel Technique
LI Xin, REN Yue-ming, QIANG Liang-sheng, ZHAO Hong-bin
2004, 20(3): 285-288.
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Haloacetic acids(HAAs) are formed during the chlorination of drinking water, which are harmful to people′s health due to their carcinogenic and mutagenic effects. In the present study, a detection method combining methyl tert-butyl ether(MtBE) extraction with acid catalysis and gas chromatography coupled with an electron capture detector(GC/ECD) was developed for determining HAAs. The detection limit of this method(MDL) and relative standard deviation(RSD) were below 0.37 μg/L and 6.2%, respectively. The laboratory chlorination experiments were conducted with the purpose of investigating the influences of reaction time, temperature, UV
254
, bromide and ammonia-nitrogen on the formation of HAAs. The results show that the formation amount of HAAs increases with increasing reaction time and temperature, respectively; and there exists a linear relationship between the formation of HAAs and UV
254
. The formation amount of HAAs decreases first and then increases as the bromide ion concentration increases, and adding NH
4
+
is a possible way to control the formation of HAAs.
Determination of Reactive Intermediates During Anodic Oxygen-transfer Reactions at Lead Dioxide
AI Shi-yun, ZHANG Wen, GAO Meng-nan, GU Fen-lin, WANG Qing-jiang, JIN Li-tong
2004, 20(3): 289-293.
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The anodic discharge of water to produce adsorbed hydroxyl free radicals(·OH) is considered to be a prerequisite to anodic O-transfer reactions at a PbO
2
electrode. In this work, a method was studied by means of high-performance liquid chromatography(HPLC) combined with electrochemical detection(ED) so as to investigate the production of hydroxyl free radicals(·OH) in the process of the anodic discharge of H
2
O at a PbO
2
electrode. The voltammetric data obtained at the PbO
2
electrode for the oxidation of salicylic acid to salicylate hydroxylation products(DHBAs) and the detection of DHBAs by means of HPLC-ED confirm the proposed mechanism.
Three-Dimension Mathematical Model of Total Phosphor in the Reservoir and Application
NIE Jing, YANG Tian-xing, LIU Xiao-duan
2004, 20(3): 294-298.
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Taking the transport of total phosphor pollutants in the Beijing Miyun reservoir for example, we have obtained three dimensional distributing regularity of total phosphor pollutants by the calculation of the linear interpolation value of each point between horizontal layers. The credibility analysis in allusion to this method was carried out and the programming scheme for realizing this method was set forth.
Syntheses of 2- or 6-Substituted Chromones and Chromone Ring-opening Reaction in Polyphosphoric Acid
HE Xun-gui, YOU Qi-dong, LI Zhi-yu
2004, 20(3): 299-304.
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In an attempt to find new antitumor agents, a novel class of chromone compounds with a benzimidazole or a benzoxazole ring in positions 2 or 6 were synthesized via condensation in polyphosphoric acid(PPA) by using chromone acids as the starting materials. During the preparation process, it was found that PPA could cleave the chromone ring to produce a ring-opening compound(6). The molar ratio of the chromone compound(5) to the ring-opening compound(6) varied with the change of reaction temperature and time. Based on MTT protocol, the antitumor activity of each of the compounds obtained was evaluated against three human cancer cell lines: KB(oral epidermal), A2780(ovary) and Bel7402(liver). The IC50 varied from 54.7 μmol/L to more than 180 μmol/L.
Structure and Biological Activities of 3-Phenyl-2-[1-benzoyl-1-(1,2,4-triazol-1-yl)] Methenyl Thiazolidine
XU Liang-zhong, JIAN Fang-fang, QIN Yong-qi, YU Guan-ping, JIAO Kui
2004, 20(3): 305-307.
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The title compound 3-phenyl-2-[1-benzoyl-1-(1,2,4-triazol-1-yl)]methenyl thiazolidine was synthesized from acetophenone, triazole, phenylthioisocyanate and 1,2-dibromo-ethane by several step reactions. Its structure was identified by means of
1
H NMR, MS and IR spectrometries. The single crystal structure of 3-phenyl-2-[1-benzoyl-1-(1,2,4-triazol-1-yl)]methenyl thiazolidine was determined by X-ray diffraction. The preliminary bioassays have shown that the title compound exhibits the weak activities of fungicide and plant growth regulator.
Selectivity of Organosamarium(Ⅲ) Hydride in Reducing Unsaturated Carbonyl Compounds
YUE Zheng-yu, GAO Ting, XIE Xiao-min, SUN Hong-yan, GAO Jin-sheng, YAN Peng-fei
2004, 20(3): 308-310.
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The selectivity of organosamarium(Ⅲ) hydride in reducing unsaturated carbonyl compounds has been studied. Dimeric organosamarium hydride[(C
9
H
7
)
2
SmH]
2
·4THF·NaCl prepared by the reaction of (C
9
H
7
)
2
SmCl·2THF with NaH in THF reacts with unsaturated carbonyl compounds to give the corresponding reduction products with a high selectivity. The carbonyl groups have been reduced while the carbon-carbon double bonds are not affected.
Analysis of Essential Oil from Stems of
Schisandra Chinensis(Turc z.) Baill
LI Hong-jun, MENG Xiang-ying, WU Yin, BAO Yong-li, LI Yu-xin
2004, 20(3): 311-313.
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The essential oil of
Schisandra Chinensis(Turc z.) Baill
was extracted and analyzed. The essential oil was obtained in a 1.8%(mL/100 g material) yield. Forty eight compounds were isolated and characterized from the oil. The results show that the content(20.42%) of β-pinene of naturally essential oil is the highest among the components of the oil, which has laid a foundation for the futher development and application of the stems of
Schisandra Chinensis(Turc z.) Baill
.
Analysis of Significance of Unite Examination of AFP and DNA Polymorphism of P3 Promoter of IGF-ⅡGene
LUO Su, ZHANG Feng-chun, SUN Chang-jiang, LIU Cheng-bai, ZHUANG Jiang-xing, ZHANG Jin
2004, 20(3): 314-316.
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The DNA of P3 promoter region of IGF-Ⅱ gene was obtained by means of PCR technique. The examination of DNA polymorphism by restriction endonuclease BstE Ⅱ and the examination of AFP by bioluminescence immunoassay technique were carried out. The results have a significant difference(P<0.005). But the positive rate of AFP is higher than that of DNA polymorphism. The experimental result shows that the change of the DNA polymorphism of IGF-Ⅱis not the only carcinogenic factor. The suggested unite examination is the best method for the diagnosis of the primary hepatocellular carcinoma.
Soluble Expression, Purification and Characterization of Single-chain Fv Catalytic Antibody(sFv-2F3)
SUN Ye, LI Wei-jia, MA Ji-sheng, MU Ying, DU Xiu-bo, YAN Gang-lin, LUO Gui-min
2004, 20(3): 317-322.
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To find optimal conditions for expressing the soluble form of sFv-2F3 and to study the purification and property of its derivative Se-sFv-2F3, the preferred expression conditions were investigated by means of orthogonal design. These culture conditions included incubation temperature, inducer concentration, induction time and cell concentration. The evaluation of expression was accomplished by the analysis of whole cell lysates and the yield of soluble sFv-2F3 was calculated according to the analysis of Profinder(FTI-500,Pharmacia). The purification procedure was carried out via a two-step purification procedure consisting of ion-exchange chromatography, followed by immobilized metal affinity chromatography(IMAC). The antioxidant efficacy of Se-sFv-2F3 was demonstrated by the determination of the content of the main product of lipid peroxidation, MDA, the viability of cells and the activity of LDH. We obtained the preferred culture conditions to grow the engineered bacteria and the procedure for preparing soluble sFv-2F3 and confirmed the antioxidant efficacy of Se-sFv-2F3.
Effect of Excipients on Stability and Structure of rhCuZn-SOD Encapsulated in PLGA Microspheres
LIU Ling, GE Yu, YUAN Qin-sheng
2004, 20(3): 323-327.
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When a protein is encapsulated into poly(DL-lactide-co-glycolide)(PLGA) microspheres by means of the double-emulsion method, the harsh microspheres formation process including ultrasonification, exposure to an organic solvent and a polymer may cause the denaturation of the protein. In this study, we investigated the enzymatic activity change and the effect of the excipients on the stability of recombinant human Cu,Zn-superoxide dismutase(rhCu, Zn-SOD) during the emulsification. The specific activity recovery was found to be concentration dependent and the excipients involved such as PEG 600 and Tween 20, and trehalose were shown to increase the stability of rhCu, Zn-SOD. The protein structural integrity within the microspheres was analyzed by FTIR. The structure of rhCu, Zn-SOD within PLGA microspheres containing trehalose was found to be similar to that of the native solid state, whereas the protein encapsulated during the preparation in the absence of any excipient changed due to the possible hydrophobic interaction with the polymer. The results suggest that a rational stability strategy for protein to be encapsulated into microspheres should aim at different processes.
Effect of 2-Selenium Bridged β-Cyclodextrin, Glutathione Peroxidase Mimic on Stroke of Stroke-prone Spontaneously Hypertensive Rats
JIA Zhi-dan, SUN Ye, MU Ying, MA Ji-sheng, YAN Gang-lin, LUO Gui-min
2004, 20(3): 328-333.
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To investigate the treatment effect of 2-selenium bridged β-cyclodextrin(2-SeCD), a GPX mimic, on the stroke of stroke-prone spontaneously hypertensive rats(SHRSP), fifty-two SHRSP of 8-week old were randomly divided into four groups A, B, C and control group D. The rats of groups A, B, C and D were given 1.0%-1.5% NaCl mass fraction as drinking fluid. After onset of stroke, groups A, B and C were given orally 16.05, 160.5 and 1605 mg·kg
-1
·day
-1
of 2-SeCD, respectively, and group D was given water for 2 weeks. The clinical score of stroke, systolic blood pressure(SBP), survival time of rats were recorded and the histopathologic examinations of their brain and carotid artery were made after decapitation. The clinical scores of stroke after treatment with 160.5 mg·kg
-1
·day
-1
(Group B) and 1605 mg·kg
-1
·day
-1
(Group C) of 2-SeCD are 2.55±0.98 and 1.98±0.79, respectively, those are obviously lower than that of group D(3.41±0.83, p<0.01). The survival days in group B(10.0±8.6) and group C(14.4±7.9) are longer than that for group D(4.7±2.9, p<0.01). The electron microscope study showed that the endothelium of carotid artery was near to normal in group B and group C, while it was seriously injured in control group D and mildly injured in group A. 2-SeCD may effectively be used to treat the stroke for SHRSP.
Synthesis and Characterization of A Small Molecule CFTR Chloride Channel Inhibitor
HE Cheng-yan, ZHANG Heng-jun, SU Zhong-min, ZHOU Jin-song, YANG Hong, MA Tong-hui
2004, 20(3): 334-337.
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A thiazolidinone CFTR inhibitor(CFTR
inh-172
) was synthesized by a three-step procedure with trifluromethylaniline as the starting material. The synthesized CFTR inhibitor was characterized structurally by means of
1
H NMR and functionally in a CFTR-expressing cell line FRT/hCFTR/EYFP-H148Q by both fluorescent and electrophysiological methods. A large amount(100 g) of high-quality small molecule thiazolidinone CFTR chloride channel inhibitor, CFTR
inh-172
, can be produced with this simple three-step synthetic procedure. The structure of the final product 2-thioxo-3-(3-trifluromethylphenyl)-5-[4-carboxyphenyl-methylene]-4-thiazolidinone was confirmed by
1
H NMR. The overall yield was 58% with a purity over 99% as analyzed by HPLC. The synthesized CFTR
inh-172
specifically inhibited CFTR chloride channel function in a cell-based fluorescence assay(K
d
≈1.5 μmol/L) and in a Ussing chamber-based short-circuit current assay(K
d
≈0.2 μmol/L), indicating better quality than that of the commercial combinatorial compound. The synthesized inhibitor is nontoxic to cultured cells at a high concentration and to mouse at a high dose. The synthetic procedure developed here can be used to produce a large amount of the high-quality CFTR
inh-172
suitable for antidiarrheal studies and for creation of cystic fibrosis models in large animals. The procedure can be used to synthesize radiolabled CFTR
inh-172
for
in vivo
pharmacokinetics studies.
Synthesis and Structure of Manganese Coordinated Polymer with Regular X-shaped Cavity
MA Dong-sheng, Gao Shan, HUO Li-hua, GAO Jing-sheng, SUN Zhi-zhong
2004, 20(3): 338-340.
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A coordination polymer [Mn(IDA)
2
(H
2
O)
4
]
n
(H
2
IDA=N-iminodiacetic acid) was synthesized and characterized by single crystal X-ray diffraction. The crystal belongs to the tetragonal system, the space group is P-42
1
C with the crystal cell parameters a=0.81120(8) nm, b=0.81120(8) nm, c=0.96196(4) nm, V=0.6330(1) nm
3
, M
r
=355.17, R=0.0224, wR=0.061. The four carboxylic oxygen atoms of the different N-iminodiacetic acid ligands and two water molecules coordinate to the manganese atom. The manganese atom is in an approximates octahedral coordination sphere. Each carboxylic acid ligand bridges two manganese atoms, forming two zig-zag supramolecular chains. The twisted chains construct a two-dimension layer structure with regularly arranged X-shaped window cavity. The three-dimension supramolecular network is formed by coordination bonds and hydrogen bonds.
Synthesis, Crystal Structure and Properties of Complex VO(C
12
H
12
N
2
O
2
)(C
13
H
10
NO
2
)
MA Dong-sheng, Gao Shan, HUO Li-hua, GAO Jing-sheng
2004, 20(3): 341-344.
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)
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Complex VO(C
12
H
12
N2O
2
)(C
13
H
10
NO
2
)(C
12
H
12
N
2
O
2
2-
=acetylacetone benzoylhydrozanate, C
13
H
10
NO
2
-
=N-phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis, IR and UV spectroscopies, cyclic voltammetry and single crystal X-ray diffraction. The complex crystallized in the monoclinic system with space group P2
1
/n and the crystal cell parameters a=1.3003(1) nm, b=0.88836(6) nm, c=2.0196(2) nm, β=95.065(8)°, V=2.3238(3) nm
3
, M
r
=495.40 and Z=4. The two oxygen and one nitrogen atoms of the tridentate hydrazone ligand coordinate to the vanadium atom, forming an equatorial plane. And the coordinated vanadium atom exhibits a distorted octahedral geometry. The atom in the transposition to the oxo O atom is the carbonyl oxygen atom of the hydroxamate ligand in the complex. The half-wave redox potential of the title complex in the three different solvents positively shifts in the order of CH
2
Cl
2
<CH
3
CN<DMF.
Ultraviolet-visible and Surface-enhanced Raman Scattering Spectroscopy Studies on Ruthenium Phthalocyanine Monolayer Films Formed on Terephthalonitrile-modified Silver Substrates
LI Xiao-ling, XU Wei-qing, JIA Hui-ying, WANG Xu, ZHAO Bing, LI Bo-fu, OZAKI Yukihiro
2004, 20(3): 345-349.
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A self-assembled monolayer film(SAM) of ruthenium phthalocyanine(RuPc) fabricated on a silver substrate premodified with an SAM of terephthalonitrile(TPN) was studied by means of surface-enhanced Raman scattering(SERS) and ultraviolet-visible(UV-Vis) spectroscopies. TPN was used as a ligand to link RuPc since it can not only modify the silver substrate but also deliver the nitrile groups protruding from the silver surface. Therefore, we can explore the relationship between the structure and the orientation of RuPc and the TPN-modified substrate. The UV-Vis spectra indicate a strong interaction between RuPc and TPN in the composite film. The result is further confirmed by the SERS spectra of RuPc-TPN SAM, in which the vibrational bands arising from both the RuPc and TPN moieties appear clearly, indicating that the RuPc is successfully assembled on the TPN film.
Performances of Aluminum-cobalt Co-substituted α-Ni(OH)
2
Electrodes
ZHANG Heng-bin, LIU Han-san, CAO Xue-jing, SUN Chia-chung
2004, 20(3): 350-353.
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Aluminum-cobalt co-substituted α-Ni(OH)
2
was prepared by means of the titration method in a buffer solution, the structure was characterized by XRD analysis. With above mentioned α-Ni(OH)
2
as the positive electrode of a nickel-metal hydride cell, the discharge performances were examined by constant-current charge-discharge experiments. In comparison with the electrodes made of aluminum substituted or cobalt substituted Ni(OH)
2
materials, the aluminum-cobalt co-substituted composite electrodes possess an excellent electrochemical performance and are of practical significance.
Ab initio
Studies on Intermolecular Interaction of Formamide and Hydroxyacetonitrile Dimers
JU Xue-hai, XIE Lun-jia, XIA Qi-ying, XIAO He-ming
2004, 20(3): 354-357.
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The structures, the binding energies and the thermodynamic properties of formamide and hydroxyacetonitrile(HAN) dimers have been studied by means of the self-consistent ab initio Hartree-Fock and the second-order Mφller-Plesset correlation energy correction methods. The counterpoise procedure was used to check the basis set superposition error(BSSE) of the binding energies. There exist cyclic structures in a formamide dimer(Ⅰ), a HAN dimer(Ⅱ) and their heterodimer(Ⅲ). The corrected binding energies for dimers Ⅰ, Ⅱ and Ⅲ are respectively -45.53, -45.83 and -43.89 kJ/mol at the MP2/aug-cc-p VDZ//HF/aug-cc-p VDZ level. The change of the Gibbs free energies(ΔG) in the process of Ⅰ+Ⅱ
→
2Ⅲ was predicted to be -2.74 kJ/mol at 298.15 K. Dimer Ⅲ can be spontaneously produced in the mixture of formamide and HAN, which is in agreement with the experimental fact that most cyanohydrins are capable of interacting with dipeptide cyclo-His-Phe(CHP).
Role of Bismuth Oxide in Bi-Mco
2
O
4
(M=Co,Ni,Cu,Zn) Catalysts for Wet Air Oxidation of Acetic Acid
JIANG Peng-bo, CHENG Tie-xin, ZHUANG Hong, CUI Xiang-hao, BI Ying-li, ZHEN Kai-ji
2004, 20(3): 358-361.
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Two series of cobalt(Ⅲ)-containing spinel catalysts were prepared by the decomposition of the corresponding nitrates. The catalysts doped with bismuth oxide exhibit a higher activity in the wet air oxidation of acetic acid than those without dopant bismuth oxide. The catalysts were investigated by XRD, TEM, ESR, UV-DRS and XPS, and the interaction between Co and Bi was studied as well. It has been found that nano-sized bismuth oxide is paved on the surface of cobalt spinel crystal and the structures of cobalt(Ⅲ)-containing spinel are still maintained. The shift of the binding energy of Bi
4f
7/2
is related to the catalytic activity of these catalysts doped with bismuth oxide.
Synthesis of Acrylic Acid/Kaoline Powder Superabsorbent Composite by Inverse-suspending Polymerization
ZHONG Jin-feng, XUE Yi-ming, WU Ji-huai, LIN Jian-ming, WEI Yue-lin
2004, 20(3): 362-365.
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An acrylic acid/kaoline powder superabsorbent composite with a water absorbency of the superabsorbent composite about 1/800 was synthesized by inverse-suspending polymerization reaction between acrylic acid monomer and kaoline ultrafine powder. The influence of the dispersant agent on the configuration of the products in the inverse suspension polymerization is investigated. The influences of the kaoline powder, cross-linker, initiator, neutralization degree and the volume ratio of oil to water phase on the water absorbency of the superabsorbent composites are discussed in the paper.
Structure Characterization and Thermal Properties of PMMA/Montmorillonite Nanocomposites
via
Emulsion Polymerization
QU Xiong-wei, GUAN Tong-hua, LIU Guo-dong, WANG Mei-ying, ZHANG Liu-cheng
2004, 20(3): 366-372.
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Montmorillonite(MMT) modified with sodium silicate can change the arrangement of its layers from edge-face and edge-edge to face-face. With the fine dispersion of the modified MMT in water, the cation-exchange reaction was carried out with cetyltrimethyl ammonium bromide(CTAB) to obtain organo-montmorillonite(OMMT). As OMMT was uniformly dispersed in methyl methacrylate(MMA) monomer, PMMA/OMMT nanocomposites were formed via a common emulsion polymerization. The products were extracted with hot acetone and characterized by FTIR, molecular weight, X-ray diffraction(XRD), transmission electron microscopy(TEM), DSC and TGA. These results show that most of the OMMT layers have been exfoliated, while the thermal stability is increased obviously. By means of FTIR spectral analysis, the ratios of the macromolecular radicals′ termination of disproportionation patterns to combination are increased with the addition of OMMT. This result further confirms the increase of the thermal degradation temperatures and glass transition temperatures of the PMMA/OMMT nanocomposites.
Studies on Thermodynamic Properties of Adsorption of Theophylline by Phenolic Resin Adsorbents
WANG Zhong, SHI Zuo-qing, SHI Rong-fu, FAN Yun-ge, YAN Yi-Zhong
2004, 20(3): 373-376.
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In the present work, the equilibrium adsorption of theophylline was studied by phenolic resin adsorbents: JDW-2(made by ourselves) and Duolite S-761 within a temperature range of 303-323 K. The experimental results show that the Freundlich adsorption law is applicable to the adsorption of theophylline on the two adsorbents, the exponents n＞1 indicate that they are favorable to the adsorptions; the negative values of all the isosteric adsorption enthalpies for the theophylline indicate the exothermic process of the adsorption, while the range(10-40 kJ/mol) of their magnitudes manifests the physisorption process; other thermodynamic properties, the free energy changes and the entropy change associated with adsorption have been calculated from the Gibbs adsorption equation and the Gibbs-Helmholtz equation.
Hydrothermal Synthesis and Crystal Structure of Zinc(Ⅱ) Dinicotinate Complex [Zn(nic)
2
(H
2
O)
4
](nic=nicotinic acid):A Three-dimensional Hydrogen-bond Network
MAO Hong-yan, ZHANG Zong-pei, ZHANG Hong-yun, XU Chen, WANG En-bo, WU Qing-an, ZHU Yu
2004, 20(3): 377-379.
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