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中文
Table of Content
24 January 1997, Volume 18 Issue 1
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Articles
Photoluminescence of Eu
2+
and Mn
2+
in Sr
3
MgSi
2
O
8
YAO Guang-Qing, ZHANG Liang, SU Mian-Zeng
1997, 18(1): 1-5.
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The fluorescence of Eu
2+
and Mn
2+
coactivated Sr
3
MgSi
2
O
8
was studied.The emission bands of Eu
2+
and Mn
2+
peaking at 460 nm and 690 nm are originated from 5d-4f transition of Eu
2+
and
4
T
1
, (
4
G)-
6
A
1g
(
6
S) transition of Mn
2+
respectively.The fluorescence of Mn
2+
, singly doped in Sr
3
MgSi
2
O
8
has not been observed.However, codoping with Eu
2+
makes photoluminescence of Mn
2+
apPear at 690 nm.This shows that the emission of Mn
2+
is sensitized by Eu
2+
, and then the fluorescence lifetime of Eu
2+
is affected by Mn
2+
.The ex-perimental results indicate that there exists an effective energy transfer from Eu
2+
to Mn
2+
in Sr
3
MgSi
2
O
8
host.This kind of energy transfer is due to the electric dipole-dipole interaction of the resonance transfer.
The Synthesis and Catalytic Performance of Pd Cluster Encaged in Y-type Zeolite
JI Tian-Hao, MENG Xian-Ping, WU Nian-Zu, LI Shi-Jie, LIU Ying-Jun
1997, 18(1): 6-10.
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The palladium cluster encaged in Y-type zeolite has been synthesized by the method of microwave radiation ion exchange-hydrogen reduction with [Pd (NH
3
)
4
](NO
3
)
2
.H
2
Oas precursor of ion exchange.The results of XRDand XPSshow that calcination tem-perature has an important influence on the Pd atoms encaging into zeolite NaYand the for-mation of Pd clusters.When the Pd content in zeolite Yis 6.13%, Pd can be also encaged in zeolite Yand form cluster under the condition of preparation at 240 Cof calcination temper-ature and 210 Cof reduction temperature.Using the sample of Pd content 0.410% obtained under the same conditions, the conversion on COcomplete oxidation is 100% at room tem-perature and at 2000 h
-1
(space velocity).Therefor, Pd cluster encaged Y-type zeolite is an excellent catalyst for complete oxidation of carbon monoxide.
Synthesis and Crystal Structure of Protonated Sodium Potassium Dimeric(citrato)dioxovanadium(V)
ZHOU Zhao-Hui, MIAO Jian-Ying, WAN Hui-Lin
1997, 18(1): 11-14.
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The titled complex NaK
3
[VO
2
(Hcit)]
2
.7H
2
O (H
4
cit=citric acid) has been pre-pared and characterized by X-ray diffraction.It crystallizes in monoclinic space group P2
1
/n with unit cell parameters:a = 1.1258(2) nm, b=1.5774(3) nm, c=1.6559(1) nm, β=98.568 (9)°and D
c
= 1.851 g.cm
-3
, Z=4.Each dimer contains a quasi-centrosymmetric planar four-member V
2
O
2
ring with two exocyclic citrate entities coordinated by the oxygen atoms of the hydroxy- and a-carboxylate ligand, while the other two β-carboxylate groups remain uncomplexed as its deprotonated and protonated citratovanadate(V).
Studies on the Crystallization Behavior of Zeolite Silicalite-1 in (TPA)
2
O-Na
2
O-SiO
2
-H
2
O System(Ⅰ)──Crystallization Kinetics
WU Ai-Mei, LONG Ying-Cai
1997, 18(1): 15-20.
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Zeolite silicalite
-1
was hydrothermally synthesized in (TPA)
2
O-Na
2
O-SiO
2
-H
2
Osystem.The silica sources used were fumed silica(Ⅰ), silica sol (Ⅱ) and waterglass(Ⅲ).There are different crystallization kinetic curves in the temperature range from 140℃ to 180 ℃ for different silica source systems with the same molar ratio of reactant.The activation energy for nucleation (E
n
) and for crystallization (E
c
), which are calculated from the induc-tion time and growing rate, are 46/76 kJ/mol in system (Ⅰ), 41/43 kJ/mol in system (Ⅱ),and 38/78 kJ/mol in system (Ⅲ), respectively.The crystal size obtained in each system de-pends on the difference between E
n
and E
c
The highest product crystallinity determined both by XRDand by adsorption of n-hexane was obtained in fumed silica system.The quality of the zeolite obtained can be improved by increasing the temperature of crystallization.
The Phase Transition in Alumina Studied by Eu
3+
Ion Probe
LIU Bing, YANG Pin, HAN Gao-Yi
1997, 18(1): 21-23.
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Because of industrial interest, techniques to prepare a thermally stabilized active alumina have been developed.Ionic probe has been widely used in the studying of structure and function on biomacromolecules.In this paper, the phase transition in alumina at differ-ent sintering temperatures was first studied by Eu
3+
ion fluorescent probe.The XRD, FTIRand fluorescence spectra measurements show that γ-phase is dominated in alumina at below 1000℃; the mixed γ-and phases in the sample are produced at 1100 ℃;but α-phase in alumina is dominated at 1200 ℃.It is shown in FTIRspectra that the peak of Eu-Ostretching vibration increases dramatically at 1200 ℃ Meanwhile, fluorescence spectra in-dicate that the peak of 613 nm is weakned gradually whereas the peak of 617 nm is strength-ened in
5
D
0
-
7
F
2
supersensitive transition of Eu
3+
when the sintering temperature increases.However, the peak of
5
D
0
-
7
F
4
transition splits evidently at 1200 ℃ because of the decreasing of symmetry in Eu
3+
coordination site.
Analysis and Elimination of Trace Organic Compounds in Smoke from Burning Coal
WANG Xiu-Hong, XIAO Tian-Cun, YANG Bin, WANG Shu-Ren, OU Qing-Yu
1997, 18(1): 24-28.
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An analysis system of trace organic compounds in smoke from burning coal was established, which included concentration of organic compounds by adsorbent, super critical fluid extraction (SFE), and gas chromatography-mass spectroscopy for identification.The abilities of four kinds of adsorbents were compared.SFEis superior to solvent extraction in extracting organic compound in coal smoke, More than 130 compounds were detected, in-cluding alkane, alkene, aromatic hydrocarbon with low ring number, alcohol, aldehyde, ke-tone, acid, ester, phenol, polyring compounds and heterocyclic compounds.The possibility of elimination organic compounds by using catalyst of CuO-Mn/Al
2
O
3
was researched for the first time.It was shown that thls kind of catalyst can eliminate most of the organic contami-nats in smoke effectively and economically.
Charge Transport of Indigo-Carmine Doped Polypyrrole
YANG Chun-He, LI Yi-Jun, DONG Shao-Jun
1997, 18(1): 29-32.
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Charge transport in polypyrrole doped with indigo-carmine was investigated by the method of electrochemical alternating current impedance.By the nonllnear least square fitting, the equivalent circuit and parameter of each component are obtained.The apparent diffusion coefficients and heterogeneous electron transfer constants are given.It is found that, along with the increasing of film thickness, D
app
and k
o
increase also.
Studies on the Chemical Kinetics in Flow Injection Analysis System
LIU Zhen, ZOU Gong-Wei, ZHANG Yu-Kui
1997, 18(1): 33-36.
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Covection-diffusion model was used to study the chemical kinetics in flow injection analysis(FIA) system.Based on the expression of concentration distribution of physical dis-persion of sample without chemical reaction, the expressions of concentration distribution of product in single-line FlAsystem with first-order and second-order chemical reaction under certain conditions were derlved by mathmatical inductive method.The analytical solutions are very simple so that they can be applied to simulate the produced curves with computer easily.The experimental fact that double-humped peak occurred when sample volume is very large in second-order reaction system was interpreted by the results computer-simulated.In addition, other information concerning chemical kinetics was discussed.
Studies on Voltammetric Behaviour and Reaction Mechanism of Bleomycin
LI Qi-Long, TAN Xue-Cai, HU Jin-Bo
1997, 18(1): 37-41.
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In 0.05mol/L H
2
SO
4
solution, two reductive peaks P
1
and P
2
of bleomycin A5were obtained.The peak potentials E
p
1
, and E
p
2
are -0.83 Vand - 1.09 V(vs., Ag/AgCl),respectively.The voltammetrlc behaviour and reaction mechanism of bleomycin A
5
, have been studied by means of linear sweep and cyclic voltammetry, NPP, ACpolarography and UVspectrophotometry.The experiments have proved that P
1
is irreversible adsorption wave,which involves two electrons process for the reduction of 3, 4(N = C) group in pyrimidine cyclic of bleomycin A
5
.P
2
is also the irreversible adsorption wave, which involves further re-duction of pyrimidine cycle and catalyt1c hydrogen wave.
Studies on the RP-HPLC Retention Behavior Relationship Between the Structure of Hydroxy Compounds and Their Glucuronides
LUAN Lian-Jun, ZENG Su, LIU Zhi-Qiang, FU Xu-Chun
1997, 18(1): 42-45.
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The quantitative relationship between the structure of solutes and their chro-matographic retention behavior has been studied for many years.This paper discussed main-ly the retention behavior of hydroxy compound glucuronides.The samples were incubated in vitro.In conclusion, the retention behavior of glucuronides can be predicted by two ways:(1) prediction of capacity factor (k') for hydroxy compounds and their glucuroIlides is based on chemi-physical constantsi (2) prediction of glucuronides capacity factor is based on the capacity factor of parent compound.The paper solved a knotty problem, the lack of glu-curonide reference by using biological synthesis method.It is very useful for the study on drug phase Ⅱ metabolism.Predicting retention behavior of metabolites based on the parent compounds is also a new idea for studying QSRRfor drug metabolites.
Studies on the Spectral Line Profiles in Zeeman Effect Atomic Absorption Spectroscopy (Ⅳ)-Te214.3 nm and Te225.9 nm Lines
CHEN Jiang-Han, HE Zhi-Rong, GONG Hui-Ling, SHU Yong-Hong, HE Hua-Kun
1997, 18(1): 46-48.
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The effect of different modulated modes on the analytical performances of Te 214.3nm and 225.9 nm in Zeeman AAShas been studied and discussed theoretically and ex-perimentally in this paper, based on the overlapping relationship of AE, AAand ZAAcalcu-lated theoretically and plotted line profiles for Te 214.3 nm and 225.9 nm.The experimental results are consistent with those in theory.
Methods of Handling Discrete Data for Deconvolution Voltammetry (Ⅰ)──-Wavelet Transform Smoothing
LU Xiao-Quan, Mo Jin-Yuan
1997, 18(1): 49-51.
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Anew method which is caIled orthogonal wavelet transform was introduced into deconvolution voltammetry to deal with discrete data containing strong random noise.From simulated data and experimental data, the processed results show that wavelet trans form would be the best method in processing complex discrete signal containing high white noise,and was compared with Fourier least square method.Wavelet transform has many merits than Fourier method.
Non-enzymatic System for Catalytic Fluorometric Determination of Glucose Oxidase
LI Qing-Ge, XU Jin-Gou, HUANG Xian-Zhi, CHEN Guo-Zhen
1997, 18(1): 52-54.
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Anovel non-enzymatic method for the determination of oxidases and their sub-strates was proposed.The principle was examined by fluorometric determination of glucose oxidase(GOD).Using EGTA (NH
4
)
2
Fe (SO
4
), as modified Fenton reagent, H
2
O
2
, the prod-uct of GODcatalytic reaction was converted into hydroxyl radical, the later oxidized tereph-thalic acid, which was chosen from four fluorogenic indicator of hydroxyl radical, into fluo-rescent product GODwas thus measured according to the reaction rates.The rnethod is sim-ple, stable, cheap and at least as sensitive as its counterpart enzymatic method-
Studies on Synthesis and Fungicidal Activity of S-Alkyl-O-(2, 6-dichloro-4-substituted phenyl)Thiophosphates (-phosphonates)
TANGChu-Chi, WANG You-Ming, LANG Hui-Fang, HE Zheng-Jie
1997, 18(1): 55-59.
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S-Alkyl thiophosphoro (-phosphono-)chloridates 4 were prepared by the isomer-ization/chlorination reaction of O,O-dialkyl thiophosphates(-phosphonates)3 with phospho-rus oxychloride- The isomerization/chlorination of 3 containing bulkier Rand R
1
groups re-quire higher reaction temperatures and Ionger reaction time.4 reacted with 2, 6-dichloro-4-substituted phenols to give 26 new target compounds 6, which were tested in vitro against many fungi such as P.Zeae, P.Piricola, R.Solani, A- Solani and D.Arachidicala, etc.The bioassay results show they have some fungicidal activity.
Using Molecular Graphics, Molecular Mechanics, Quantum Chemistry and Electrostatic Potential Methods to Study Structure-Property Relationship on Pesticides(Ⅸ)─Effect of Selecting Structural Parameters and Calculating Methods on Improving the Acc
WANG Xia, YUAN Man-Xue, LAI Cheng-Ming, LIU Jie, LI Zheng-Ming
1997, 18(1): 60-63.
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In this paper, we discussed mainly two sldes of factors-structural parameters and calculating methods, which improved the accuracy of forecasting activities on sulfony-lure a molecules.When selecting the structural parameters, we considered not only the radi-cal effect of molecules, but also their characteristics as a whole-the values of conforma-tion difference between the most active molecule and other molecules were computed, and at the same time, we applied the optimum calculating method - Artificial Neural Networks (ANN).Then we calculated the PI
50
values of 35 newly synthesized sulfonylurea molecules,which were almost in agreement with experimental data(mse=0.073) and superior to those of multiregression analysis (mse=0.82).
Studies on the Mannich-type Reaction of p-Toluenesulfonylurea
DAI Qing, CHEN Ru-Yu
1997, 18(1): 64-67.
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The Mannich-type reaction invoIving p-toluenesulfonylurea with aromatic aldehy-des and dialkyl phosphite was studied and the reactivities of various kinds of amides were compared by a competing reaction.Anew type of a-amino phosphonic acid derivatives were synthesized and the structures of the products were confirmed by
1
HNMRand elemental analyses.The bioassay shows that some of them possess good anti-TMV(Tobacco Mosaic Virus) activity.
The Chemistry of α-Oxo Ketene Cyclic Dithioacetal(XXXVI)──Studies on Silica G Catalyzed Decomposition or Adducts of β, β-1, 3-Propylenedithio-α,β-unsaturated Arylketones with Grignard Reagents
DONG De-Wen, XIE Zhen-Li, LIU Qun, YANG Zhi-Yun, LIU Jing-Fu
1997, 18(1): 68-72.
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β, β-1, 3-Propylenedithio-α, β-unsaturated arylketones 2 via chemoselective 1, 2-addition with allyl or benzyl Grignard reagents afforded the corresponding carbinols 3 and 4.Catalyzed by silica gel, the carbinols 3 and 4 were converted to the β, γ-unsaturated arylke-tones 5, 6.The mechanism and reaction condition were discussed.
Application of Phenyl(phenylethynyl)iodonium Tosylate──Synthesis of Isopropylidene-5-alkyl-5-phenyle Malonates
ZHAO Jing-Guo, CHEN Zhen-Chu
1997, 18(1): 73-75.
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Ageneral method for the synthesis of isopropylidene-5-alkyl-5-phenylemalonates via the reaction of phenyl (phenylethynyl)iodonium tosylate with isopropylidene 5-alkyl malonates in the presence of NaH/THF(or t-BuONa/t-BuOH, K
2
CO
3
/TEBA/CHCl
3
,K
2
CO
3
/18-Crown-6/THF) is reported in this paper.
Synthesis and Bioactivity of 1-(Substituted silylmethylthio)methyl-2, 8, 9-trioxa-5-aza-1-silabicyclo[3.3.3]undecanes
HE Zheng-Jie, LI Zheng-Ming, YANG Zhi-Qiang
1997, 18(1): 76-78.
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By the reactlon of (substituted silyl)methanethiols with 1-chloromethyl-2, 8, 9-tri-oxa- 5-aza-1-silabicyclo [3.3, 3] undecane, eleven novel organosilicon compounds were syn-thesized.Their structures were confirmed by
1
HNMR, MSand elementary analysis.Arare rearrangement breakdown pattern was found ln their mass spectra.Preliminary bioassay re-sults showed these compounds have some antitumor activity.
Studies on Synthesis and Properties of Amidate Crown Ether Liquid Crystals
JIANG Qing, XIE Ming-Gui, RUAN Ji-Wu, PENG Ming-Sheng, FANG Cheng, LI Long-Zhang
1997, 18(1): 79-81.
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Five novel amldate crown ethers were deslgned and synthesized.The structures of all the compounds synthesized are characterized by elementary analysis, IR, MSand
1
HNMR spectroscopy.The liquld crystal properties of three compounds 4-6 have been characterized by DSC.
Studies on Carbohydrates (XVI)──Synthetic Study on the Precursor of Macrocyclic Compound Clemochinenoside-A
MAO Jian-Min, CHEN Hong-Ming, CAI Meng-Shen
1997, 18(1): 82-84.
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Herein we wlsh to report the synthetic study on the precursor (10) of clemochi-nenoside-A(1), a new kind of macrocyclic glycoside, which was found in the roots of Clem-atics chinesis Osbeck (wei ling xian) that was used as Chinese herbal medicine for treatment of anthritis, arthralgia, headache and inflarnmation.The key steps were stereoselective gly-cosidation of 6 and selective mesylation of 9.Further studies are still going on,
Studies on 2, 5-Diaryloxadiazoles (Ⅲ)—The Synthesis, Spectra and optical Properties of trans-2-{4-[2-(4-R-phenyl) ethenyl]phenyl}-5-(4-biphenyl)oxadiazole
ZHANG Wen-Qin, YANG Mei, SUN Yan, ZHOU Yi-Min
1997, 18(1): 85-87.
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Eight of trans-2-{4-[2-(4-R-Phenyl) ethenyl] phenyl} -5- (4-biphenyl) oxadiazoles (R=H, i-Pr, t-Bu, Ph, OMe, F, Cl, Br) were synthesized.Their UV, MS, FLspectra,fluorescence quantum yields and laser conversion efficiencies as well as fluorescence lifetime,laser turning range are given and discussed.
Studies on the Intercalation of n-Alkylamine and n-Amino-alcohol in Layered Zirconium Phosphate
XU Jin-Suo, TANG Yi, ZHANG Hua, GAO Zi
1997, 18(1): 88-92.
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For the purpose of preparing pillared phosphates, the intercalation of n-alky-lamine and n-amino-alcohol in layered α-Zr(HPO
4
)
2
·H
2
O(α-ZrP) and its effect on the struc-ture and properties of the layered phosphate have been investigated in detail. It was found that the delamination degree is related with the nature and the amount of amine added, and the extent of HPO
4
2-
hydrolysis is dependent both on the basicity of the amine and the delam-ination degree.The delaminated sheets are metastable, and they may recover their ordered arrangement and experience phase transformations in air.The XRDresults and the approxi-mate calculation of the model structures of the intercalates show that a bilayer orientation of the n-alkylamine and n-amino-alcohol molecules is formed when the intercalates are saturat-ed- After long time exposure in air, the intercalates of methylamine and ethylamlne will lose about 50% of the amine and transfer to a monolayer orientation, but the intercalates of n-propylamine, n-butylamine and n-animo-alcohol still keep a bilayer orientation.
Studies on Colloidization and Stability of Layered Phosphates in Amine Hydrous Solution
XU Jin-Suo, TANG Yi, ZHANG Hua, GAO Zi
1997, 18(1): 93-98.
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The colloidization (exfoliation) and hydrolysis of layered zirconium phosphate (α-ZrP-R), tin phosphate (α-SnP-R) and titanium phosphate (α-Tip-R) were investigated systematically.When the phosphate sheets exfoliate, HPO
4
2-
and M
4+
(M=Zr, Sn, Ti)leave the sheet surface and enter tl1e solution through hydrolysis.The hydrolysis of HPO
4
2-
takes place before the loss of M
4+
, and as the hydrolysis extent of HPO
4
2-
exceeds 40%, the layered structure of the phosphates will be destroyed.The colloidization and hydrolysls de-gree of the three phosphates in the same amine solutlon differ from each other.The sheets of α-TiP-Rhydrolyze readily and exfoliate wlth difficulty.In most cases the ex foliation of α-TiP-Roccurs only around the boundary of its sheets, and the complete exfoliation is hardly observed.The sheets of α-SnP-Rare more stable than those of α-TiP-R.They hydrolyze less readily and exfoliate more easily.The sheets of α-ZrP-Rare most stable toward hydrolysis and exfoliate easily in amine solution.For each kind of layered phosphates the adoption of an appropriate amine and suitable experirnental conditions are necessary to control the hydroly-sis and exfoliation of the phosphate sheets during preparation of various types of pillared phosphates or multifunctional films.
Microwave Effects on Oxidative Coupling of Methane over Solid Oxygen Ion Conductors
CHEN Chang-Lin, HONG Pin-Jie, DAI Shu-Shan, ZHANG Cheng-Cong, YANG Xiao-Yun
1997, 18(1): 99-102.
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The oxidative coupling of methane over 6-Bi
2
O
3
phase solid oxygen ion conductors irradiated by microwave has been studied.Compared with the conventional heating mode, the use of microwave irradiation appears to have some beneficial effects: (1) at the same methane conversion level, the temperature of catalyst bed is much lower with the microwave irradiation than with the conventional heating mode, this is due to "microwave hot spot"effect; (2) the C
2
selectivity obtained with microwave irradiation is much higher than with conventional heating especially in the lower temperature range.This difference might arise from the reduction of oxidation products (ethane, ethylene) in the gas phase under mi-crowave irradiation.
Spectroscopic Characterization of the Active Site of NC208 Modified Copper-based Catalyst for Methanol Synthesis
YANG Yi-Quan, LIN Zhong-Yu, CHE Chang-Zhen, YUANG You-Zhu, LIN Ren-Cun, DONG Yuan-Qun
1997, 18(1): 103-104.
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Spectroscopic characterization of the active base of an industrial catalysts and NC208 modlfied copper-based catalysts for methanol synthesis has been carried out by means of XRDand FTIRrnethods.The experimental results showed that active site on functioning copper-based catalysts for methanol synthesis is probably Cu
2
0
-Cu
+
-O-Zn
2+
/Al
2
O
3
-MO
x
and that the surface concentration of Cu
+
-site on functioning NC208, prepared by adding small amount of the metal oxide MO
x
.to industrial catalyst C207, was higher than that of C207 catalyst, and that the surface of functioning NC208 catalyst had higher Cu
+
/Cu
0
ratio and valence stability than that of C207 These pecullarities have close a relation with more persistent activity and higher thermal stability than modified NC208 catalyst.
Dielectric Analysis for the Model of Dilute Cell Suspension
ZHAO Kong-Shuang
1997, 18(1): 107-111.
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Amethod of numerical analysis is proposed based on a dielectric model of dilute cell suspension to calculate the phase parameters from the dielectric parameters observed.The reason of the dielectric relaxations is represented through phenomenologically in view-point of interfacial polarization.Furthermore, the procedure of calculation upon the theoreti-cal formulation is applied to the data observed for the system composed of a single microcap-sule and distilled water, the results show that the phase parameters obtained are reliable and the model proposed is reasonable.
Influences of Electrode Surface Structure and Organic Additives on the Electroreduction of Fullerene
YANG Yong, JIANG Yi-Song, LIN Zu-Geng
1997, 18(1): 112-115.
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The influences of electrode surface structure and organic additives such as aniline and o-aminophenol on the electroreduction of fullerene are investigated in this paper.It is found that the activity of electroreduction of fullerene and fulleride anions ls dependent on the electrode surface structure.The reduction current of fullerene at polycrystal electrode is higher than those at Pt (111) and Pt (110).Some negative shifts of reduction potential of C
60
-
and C
60
2-
at Pt (111) and Pt (110) are observed.In addition, the effects of some organic additives, such as aniline and o-aminophenol on the reduction of fullerene are also investigat-ed.Different reduction mechanisms are proposed for these two systems, i.e.one is due to the formation of C
60
-
aniline complex, the other is due to chemical reaction between C
60
with o-aminophenol in the reduction process.
A Harmonic Potential Energy Function Constructed from New Hession Matrix and Its Application
LI Shen-Min, WAMG Ming-Liang, YANG Zhong-Zhi
1997, 18(1): 116-119.
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By using Hession matrix obtained from ab initio calculations, a new Hession ma-trix was formed through simply matrix transformation.With the new Hession matrix, a har-monic potential energy function of polyatomic molecules was constructed, which could accu-rately fit the experiment vibrational frequency.On this basis, with the QCTmethod, the dy-namic process of intermolecular energy transfer for H
2
O, SiH
4
was simulated. The results were in accordance with expriments and theoretical calculations.
On Order Parameters and Activity Coefficients of Mixed Model Membranes
HUANG Qiang, CHEN Geng-Hua, HAN Shi-Jun
1997, 18(1): 120-123.
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In this paper, a theoretical analysis on the relation between order parameters and activity coefficients of mixed model membranes is presented to overcome its empiricism in the previous studies- On the basis of statistical mechanics of order parameter, our discussion employs the mean-field approximation and leads, by means of classic thermodynamics, to a theoretical expression which demonstrates the concerned relation.Then a primary test that calculates the activity coefficients of POPCof system cholesterol/POPC (1-palmitoyl-2-oleoyl-sn-glycero-phosphatidylch by the proposed expression is carried out- Calculated values of activity coefficients for two concentrations at five temperatures are obtained.Com-pared to the.literature method, this work can better represent the behavior that activity coef-ficient changes with respect to temperature.In addition, the result shows that activity coeffi-cients are not sensitive to temperature within the given range of temperature.This indicates that the effect of temperature upon molecular interaction in the lipid bilayer of cholesterol/POPCis not s'ignificant.
Production of Diamond Nanospherulite at Carbon-Water Interface by Laser Ablation and Its Characterization by TEM
WANG Yu-Huang, YU Rong-Qing, LIU Zhao-Yang, HUANG Rong-Bin, ZHENG Lan-Sun, ZHANG Xiao-Feng, HU Gang, ZHANG Ze
1997, 18(1): 124-126.
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Carbon nanoparticle appearing in perfect spherical shape, with sizes varying from tens nanometers to several micrometers, can be produced by pulsed-laser ablating different elementary carbon samples immersed in water.Avariety of samples including HOPG,graphite, arcdischarging deposite, glassy-carbon and imitation-diamond have been tried.The yield of the diamand nanospherulite is found to depend on the structure of the sample.The SAEDpattern of the carbon-sphere produced from arc-discharging deposite can be at-tributed to the hexagonal structure of diamond, and its HREMimage exihibits 0.38nm×0.31 nm lattice, which is just three times of the distances for (110) (d=0.126 nm) and (004) (d=0.1030nm) crystal layers of hexagonal diamond, respectively.While the SAEDpattern from glassy-carbon sample displays a cubic-diamond structure.Furthermore, Raman spectra and
13
C NMRindicate tetrahedral network of the spheres.
Formation and Special Solubility of Endohedral Thulium Metallofullerenes
SUN Da-Yong, LIU Zi-Yang, GUO Xing-Hua, XU Wen-Guo, HAO Chun-Yan, LIU Shu-Ying
1997, 18(1): 127-129.
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Endohedral metallofullerenes Tm@C
2n
were synthesized with the carbon-arc dis-charge method of activating the Tm
2
O
3
-containing graphite anode in situ and back-burning technique.ToIuene soxhlet extraction, toluene and pyridine high-temperature and high-pres-sure extraction technique were employed for the effective extraction of Tm@C
2n
.The forma-tion of Tm@C
2n
was confirmed by LD-TOFand DEIMScharacterization.The mass spectro-metric results indicate that Tm@C
2n
.have a better solubility in toluene and worse solubility in pyridine than other metallofullerenes.
Synergic Effect on the Hydrogenation of Aromatic Nitrocompounds Catalyzed by Water Soluble Bimetallic Catalysts
JIANG Heng, XU Yun, LIAO Shi-Jian, YU Dao-Rong, CHEN Hua, LI Xian-Jun
1997, 18(1): 130-131.
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For the hydrogenatlon of aromatic nitrocompounds, PdCl
2
(TPPTS)
2
-H
2
PtCl
6
ex-hibited much higher catalytic activity than that of PdCl
2
(TPPTS)
2
or H
2
PtCl
6
.The synergic effect can also be observed even if the composition of Pt was 2% (molar ratio).Ahigh selec-tivity for the chloroaniline was obtained in the hydrogenation of nitrochlorobenzene catalyzed by PdCl
2
(TPPTS)
2
and bimetallic catalyst PdCl
2
(TPPTS)
2
-H
2
PtCl
6
.
Studies on the Utility of Chiral Reagent TMPEA for Measuring of Enantiomeric Purity of Chiral Ketones
Y0U Tian-Pa, HU Xiao-Ming, ZHANG Da-Yong
1997, 18(1): 132-133.
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Chiral amine TMPEAwas found to be useful in measuring of enantiomeric purityof chiraIketones.Four pairs of diastereomeric ketimines were prepared from R-(-)-TM-PEAand dl-TMPEAwith vari0us chiral ketones, the chemical shift differences between di-astereotopic protons (OCH
3
) were 0' 085-0.115, while fluorines (CF
3
) were 0' 17-0.45.
The Structure Analysis and Characterization of N-100 by NMR
LUO Shan-Guo, TAN Hui-Min, ZHANG Jian-Guo, WU Yi-Jie, DING Feng-Ying, XIAO Yan-Wen, PEI Feng-Kui
1997, 18(1): 134-139.
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To improve the mechanics properties of polyurethane materials at a high or low temperature, a hydroxy compound N-100 of HDIwas synthesized.The structure analysis and characterization were made by NMR (
1
H,
13
C,
1
H-
1
H COSY,
13
C-
1
H COSY).In addi-tion, quantitative description of the network was made on the basis of some ideal assump-tions.1Dand 2D NMRcan differentiate four sorts of carbonyl groups and establish the con-nections of all carbon and hydrogen atoms of mixed structures that originated from five dif-ferent substitutions.Besides, the alkene and isocyanate, urea, biuret and trimerized isocya-nuric groups were also detected.Therefore, the structure of N-100 was suggested be a poly-isocyanate with complicated network which contained nitrogen atom as cross-linkage, iso-cyanate and alkene as end groups.The consistence of calculated values with tested values of isocyanate content, mean function degree and mean molecular weight demonstrated the cor-rect of structure characterization and the validity of network description.
A Study on Impact Properties of γ-Ray Irradiated LLDPE Filled with Alumina Trihydrate
XU Wen, XIAO Wang-Dong, XU Xi
1997, 18(1): 140-144.
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Alumina trihydrate(ATH) can be used as a fire retardant of polyethylene which is incompatible with ATH.Functional groups(mainly carbonyl and hydroxyl groups) are intro-duced to LLDPEmolecular chains by γ-rays in air so as to improve the affinity between LLDPEand ATH.The effect of dose rate on oxidation and degradation of LLDPEexposed to γ-rays in air under the same integrated dose, and the impact properties of LLDPE/γ-LLDPE/ATHblend were studied in this paper.The experimental results show that the lower dose rate favors oxidation and degradation of LLDPE.γ-LLDPEcan distinctly increase the impact strength of LLDPE/ATHblend, and improve the dispersion of ATHin LLDPEmatrix.By adding 10% γ-LLDPE (0.1 kGy/h, 50 kGy) of the matrix to ATH (50% by weight) fi1led LLDPE, the impact strength of blend can increase from 65 J/m to 260 J/m.
Studies on Ti-Mg Supported Catalysts for the Gas-Phase Polymerization of Ethylene-The Influence of Properties and Morphology of Particle of Catalyst on the Gas-Phase Polymerization of Ethylene and the Morphology of the Product
ZHANG Qi-Xing, WANG Hai-Hua, WU Qing, OU YANG-Wei, LU Ze-Jian
1997, 18(1): 145-148.
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Two kinds of Ti-Mg supperted catalysts for gas-phase polymerization of ethylene were studied.The Ti
3+
content in the milling-made catalyst (CMtype) containing titanium 3-4%-4.0% by mass is 15%-25% of the total titanium.The surface area of the catalyst and catalytic activity for the polymerization are 130m
2
/g and 9.20 kg PE/(gTi.h).The polymerization showed quickly decaying kinetics.The Ti
3+
content in the reacting-made cat-alyst(MG-2 type) containing titanium 7.0%-8.0% by mass is 55 %-69% of the total tita-nium.The surface area of the catalyst and catalytic activity are 78 m
2
/g and 4.45 kgPE/(gTi.h).The polymerization was relative steady.The average value of diameter (D
av
) and D
avmax
/D
avmin
of the CMand MG-2 catalyst particles are 6.8 pm, 33 pm and 9.2, 7.0, respec-tively, and corresponding values of polymerization product PEparticles are 155μm, 263μm,and 10.8, 9.0, respectively.The results indicated that the morphology of the polymerization product reproduced that of the catalyst particle.
Studies on the Tyrosine-Based Polyphosphate Antitumor Drugs
FAN Chang-Lie, HU Bin, ZHUO Ren-Xi, DU Yang
1997, 18(1): 149-153.
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New polyphosphate antitumor durgs containing 5-Fu or MTXwere synthesized by macromolecular reaction of polyphosphates with the corresponding drug molecules.All these polyphosphates obtained are amphiphilic, some of them have micelle-forming properties.The hydrolysis and in vitro drug release properties of these polyphosphates were studied.The in vitro antitumor activity data showed that some of these polyphosphates exhibit good antitumor activity.
Hofmann Degradation of Macroporous Polyacrylamide Resin(Ⅱ)
YUAN Zhi, SHEN Li-Hua, YANG De-Fu, HE Bing-Lin
1997, 18(1): 154-157.
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Macroporous polyvinylamine resin was prepared by Hofmann degradation of poly-acrylamide.The factors influence the reaction were discussed.The results show that the degradation reaction of macroporous polyacrylamide resin at 0℃ as well as at -10℃ can happen.As the increase of Rfrom 13 to 20, the conversion increased.When r was 1.2 and Rwas 19, the best conversion was obtained.
Studies on Carbosilane Liquid Crystalline Dendrimer
ZHANG Qi-Zhen, SUN Ji-Run, CUI Li, PAN Jing-Xi
1997, 18(1): 158-159.
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Aliquid crystalline carbosilane dendrimer has been synthesized in successive steps, resulting in the formation of defined, unimolecular compound.12 AZO-meso-units were attached on its periphery and it has a three dimentional, tree-like, starburst structure.Its phase behavior was K64 S
x
115 S
A
123N138I.Compared with its AZO-meso-unit, 4-nitro-4'- (llydroxyhexyl)-azobenzene, whose phase behavior was K122N132I, its phase range was enlarged about 64 ℃ and two more liquid crystalline phases S
A
·S
x
were found.
A New Electric Insulating Film ──Poly(ethylene terephthalate p-Oxybenzoate)
TIAN Zheng-Hua, DENG Yuan, ZHU Bao-Xiang
1997, 18(1): 160-162.
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Aseries of copolyesters poly(ethylene terephthalate p-oxybenzoate) (PETO) de-rived from terephthalic acid, ethylene glycol and 4, 4' -oxybis (benzoic acid) were easily pre-pared by using DMT method and thermally investigated.Introduction of 4, 4' -oxydipheny-lene group into the main chain resulted in a lowering of T
m
.a decrease of crystallization rate and an increase of thermal-oxidative stability of the copolyesters.By static elongation of PETO, transparent films with qualified electrical properties and mechanical properties were easily obtained with film forming rate 100%.In comparison with poly (ethylene terephthalate) (PET) film, PETOfilm had obviously low T
m
.and low crystallization temper-ature.Due to the presence of stable aromatic ether structure, decrease in T
m
.could not lead to any reduction in thermal-oxidative stability, on the contrary, slight increase was ob-served.PETOfilm could be used in making heat resistant thick film for channel insulators of electric motor.
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