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中文
Table of Content
24 February 1990, Volume 11 Issue 2
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Articles
Synthesis and Crystal Structure of Diaquo Bis(1, 10-phenanthroline-N-monoxide)copper ( Ⅱ )nitrate
Wang Xin, Gan Xinmin, Tan Minyu, Yuan Jingli, Wang Guilan, Yuan Wanzhong
1990, 11(2): 111-114.
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In the present work, we describe the synthesis and crystal structure of the title compound. The complex crystallizes in the monoclinic space group C2/c with Z=4. Lattice parameters are: a= 15. 724 (2) Å, b=8. 995(2)Å, c=18. 432(3)Å ,β= 112. 06(2)°. The structure was solved by the direct method and Fourier techniques and refined by full-matrix least-squares to R= 0. 077 for 2352 reflections. The Cu
2+
ion is six-coordinate, being bonded to two oxygen atoms, two nitrogen atoms belong to two ligands and two oxygen atoms belong to two water molecules; The coordinated configuration of Cu
2+
ion is a slightly distorted octahedron. The nitrate groups are not coordinated to Cu
2+
ion.
Syntheses and Properties of Adducts Between Heteropoly Tungstic and Molybdic Acids and Their Salts with Dimethyl Sulfoxide
Gu Yidong, Ding Jianping
1990, 11(2): 115-120.
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Nine dimethyl sulfoxide (DMSO) adducts of heteropoly tungstic and molybdic acids and their salts were synthesized in mixed solvent of acetonitrile and water. Their properties were characterized by IR, Raman, UV-Vis,
1
Hand
13
C NMRspectra, TG-DTAthermal analysis, and X-ray diffraction analysis. The results show that the coordinating atom of DMSOis the oxygen atom of S = Obond . In the adducts, the a-Keggin structure of heteropoly anions keeps well. The organic lig-ands do not coordinate directly with heteropoly anions, but with protons in heteropoly acids by hydrogen-bond, forming oxonium ions, or with metal cations in heteropoly acid salts by coordination bond, forming complex ions. The adducts lost their organic ligands in a few steps in the range of 100-450 ℃, and the a-Keggin structure of heteropoly anions decomposes as temperature is higher than 500 ℃-The crystallographic data of CaPW-DMSOand (Bu
3
NH)
3
PW-DMSOsingle crystals were also determined.
Syntheses and Structure of Substituted Derivatives of Fe
3
(CO)
9
(μ
3
-S)
2
with P(YR)
3
(Y=O, S)
Wang Guoqiang, Hu Xiang, Liu Shutang, Liu Qiwang
1990, 11(2): 121-126.
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The reactions of Fe
3
(CO)
9
(μ
3
-S)
2
with P(YR)
3
(Y=O, S) at mild conditions were investigated. Eight mono- and di-substituted new compounds were synthesized; IX-XVI: Fe
3
(CO)
8
[P(OR)
3
] (μ
3
-S)
2
(R=iso-C
3
H
7
, sec-C
4
H
9
, iso-C
4
H
9
, n-C
6
H
13
, cyclo-C
6
H
11
), Fe
3
(CO)
8
[P(S-nC
3
H
7
),](μ
3
-S)
2
, Fe
3
(CO)
7
[P(O-secC
4
H
9
)
3
]2(μ
3
-S)
2
and Fe
3
(CO)
8
[P(S-nC
3
H
7
)
3
]2(μ
3
-S)
2
. Also , eight novel compounds with new structure were synthesized: Ⅰ -Ⅷ: Fe
3
(CO)
8
[P(OR)
3
(μ
3
-S) (R = n-C
3
H
7
, iso-C
3
H
7
, n-C
4
H
9
, sec-C
4
H
9
, iso-C
4
H
9
,n-C
5
H
11
, n-C
6
H
13
, cyclo-C
6
H
11
). The features of this series clusters are dissociated with a μ
3
-Sand a terminal COchanged to a μ
2
-COduring the reaction. The Corresponding Fe
3
framework changes from opened-triangle to closed-trangle. Ⅰ -ⅩⅥ have been charac-terzed by IR,
1
H NMRand some by mass spectroscopy. The molecular structure of Fe
3
(CO)
8
[P(O-cyclo-C
6
Hn)
3
]
2
(μ
3
-S) has been determined by single crystal X-ray diffractomer.
The Mathematical Model for Simultaneous Determination of Rare Earth Mixture with Differential Kinetic Analysis by Means of Ligand-Exchange Reaction
Xu Liang, Gu Zhicheng
1990, 11(2): 127-130.
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In this paper, an imitation of the experimental data with a mathematical model for the reversible reaction has been proposed, which is corroborated by the ligand-exchange reacion between RE-ArⅢ (the coordination compound of rare earth and arsenazo Ⅲ) and CyDTA. By the method, the experimental curve is in good agreement with the theoretical, so the accuracy for the determination of rare earth mixture by differential kinetic analysis is improved.
Oscillopolarographic Titrations Using Higher Order Differentiation and Feeding Back Current
Yang Zhaollang, Gao Hong(H Kao)
1990, 11(2): 131-135.
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In some cases, feeding back a current proportional to dE/dt will make the incision on the higher order differentiation more sensitive. The end-point will be very sharp. Smaller | dC
d
/dE | and | d
2
C
d
/dE
2
| values at the incision potential make the incision sensitivity increase to a greater extent by feeding back a current. Using ion incisions on the higher order differentiations to indicate the end-point of titrations, Cd
2+
, Ni
2+
, Co
2+
, Pb
2+
and Zn
2+
can be directly titrated with EDTAor CyDTA, Ni in Al-Ni alloy can be accurately determined by addition of excess EDTAfollowed by back titrations of the excess amount with Zn
2+
.
Ion Chromatographic Analysis for Simultaneously Determining Trace Amounts of Hg, Cd, Zn Using Meso-Tetra(4-Sulfonatophenyl) Porphyrin as Post-Chromatographic Derivatization Agent
Yan Daren, Zhang Jingan, Georg Schwedt
1990, 11(2): 136-139.
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An ion chromatographic methodising porphyrin TPPS
4
as post-chromatographic derivatiza-tion agent has been developed for simultaneously determining trace amounts of Hg, Cd, Zn. The factors affecting the derivatization reaction rate were investigated. Adetection system consisting of TPPS
4
with PARas accelerating agent of derivatization in the buffer of Na
2
B
4
O
7
-NaOH(pH10.3-12) containing NaCl was proposed. Aseparation system with sillica gel chemically bonded cation exchanger as stationary phase and the tartaric acid-NaCl as mobile phase was selected for separation of these metal ions. The separation can be finished in 10 min and the elution order can be adjusted from Zn-Cd to Cd-Zn. This method was applied to the analysis of waste water, sillicate and the corn with satisfactory results.
Identification of Chemical Behaviour of Chromium in water by Flow Injection-Spectrophotometry
Wei Qingxun, Wang Shengtian, Wang Li'an
1990, 11(2): 140-143.
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Amethod of sequential determination of Cr ( Ⅵ) and T-Cr by FIA-SPin water was developed. The Cr( Ⅵ ) was directly measured with DPCby FIA-SPanalysis and the determination of T-Cr was carried out after the pre-oxidation of Cr( Ⅲ ) to Cr(Ⅵ) with PbO
2
column at 80℃ before sample injection.Using the method described in this paper Cr( Ⅵ) or T-Cr can be determined at the concentration rangeof 0.05 - 3.0 mg/L. The sampling rate is 120 and 200 h
-1
for T-Cr and Cr ( Ⅵ ) respectively.This method was applied to practical samples and the results obtained is satisfactory.
Determination for Traces of Osmium with Spectrophotometric Method in the System of DPCI-Os(Ⅳ)-OP-10
Li Lingying, Li Daorong, Zhang Shurong
1990, 11(2): 144-147.
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The study of spectrophotometric determination of traces of osmium with 1,5-diphenylcar-bazide in the presence of non-ionic surfactant OP-10 at pH3.5 HAc-NaAc buffer solution is given in this paper. The effects of other noble metals and base metals were investigated. The non-ionic sufac-tant OP-10 phlys an important role in increasing sensitivity and stability. The molar ratio of osmium to the reagent is 1 : 1. The calibration graph for measurement at 570 nm is linear in the range of 0.1 -5.0 mg of osmium per 10 mL, with a molar absorptivity of 3. 50×10
5
L · mol
-1
· cm
-1
. The relative standard deviation is smaller than 4.0%.
Studies on Acylthiosemicarbazides and Related Heterocyclic Derivatives (XII)—Synthetic and Spectroscopic Studies on l-Nicotinyl-4-Aryl Thiosemicarbazides and Substituted 1,2,4-Triazoles
Zhang Lixue, Zhang Ziyi, Zeng Fuli
1990, 11(2): 148-153.
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Aseries of 1-nicotinyl-4-arylthiosemicarbazides and 3-(3-pyridyl-4-aryl-1,2,4-triazoIine-5-thiones were synthesized and their IR,1H NMRand MSspectra have been studied. All the new compounds were screened for biological activity. Most of them were found to possess significant promoting plant growth activity at a low concentration.
Synthesis and Characterization of Butterfly-shaped Fe
2
SP Clusters(μ-Ar
2
P)(μ-RS)Fe
2
(CO)
6
and (μ-p-CH
3
C
6
H
4
PCl)(μ-RS)Fe
2
(CO)
6
Song Licheng, Li Yu, Hu Qingmei, Wang Jitao, Zhao Weijun, Fang Yanquan, Zhang Shuji, Lu Xiuqing, Li Guowei
1990, 11(2): 154-158.
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Seven butterfly-shaped Fe,SPcluster complexes: (μ-Ph
2
P)(μ-RS)Fe
2
(CO)
6
(R = Pr
m
, Pr
i
, Bu
l
), [μ-(p-CH
2
C
6
H
4
)
2
P](μ-Pr
i
S)Fe
2
(CO)
6
, and (μ-p-CH
2
C
6
H
4
PCl) (μ-RS)Fe
2
(CO)
6
(R = Et, Pr
i
, Bu
l
) have been synthesized by the reaction of an intermediate [(μ-CO) (μ-RS)Fe
2
(CO)
6
]Et
3
NH (formed from Fe
2
(CO)
12
, RSHand Et
3
N) with Ph
2
PCl, (p-CH
3
C
6
H
4
)
2
,PCl or p-CH
2
C
6
H
4
PCl
2
. For these new complexes the relationship between the
1
H NMR,
31
P NMRspectroscopic features and the possible conformers has been discussed. In addition, a kind of catalytic reactivity for the complex of (μ-Ph
2
P)(μ-Bu
l
S)Fe
2
(CO)
6
has been investigated preliminarily.
Study on the Synthesis and Spectral Properties of Some E-1 ,2-bis(1',3'-benzoxazolyl-2')ethene and Its Derivatives
Zhou Yimin, Xia Xiaoping, Gao Chenheng
1990, 11(2): 159-163.
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Fourteen of E-1,2-bis(1',3'-benzoxazolyl-2')ethene and its derivatives are synthesized in this report, in which twelve are new compounds. The IR, UVabsorption spectra, fluorescence emission spectra, fluorescence quantum efficiencies and laser conversion efficiencies of the compounds are recorded. The photo-dimerization of XIVon direct irrediation with 400 watt high-pressure mecury arc lamp is observed.
The Study of Weak Metal-Metal Bond in Mo
4
(μ
3
-O)
2
O
4
·Cl
2
(O
2
CC
6
H
5
)
6
and Mo
4
(μ
3
-O)
2
O
4
Cl
2
(O
2
CC
6
H
4
CH
3
)
6
·2C
6
H
5
ClClusters
Jiang Yueshun, Chai Xjangdong, Zhang Hengbin, Shun Chun ting, Li Tiejin, Jiang Yian
1990, 11(2): 164-167.
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The UVspectra and cyclic voltammetry property of the two clusters, Mo
4
(μs-O)
2
O
4
Cl2(O
2
CC
6
H
5
)
6
and Mo
4
(μ3-O)
2
O
4
Cl2(O
2
CC
6
H
4
CH
3
)
6
· 2C
6
H
5
Cl, desolved in N, N-dimetylformamide and the SPY (Surface Photovoltage) spectra, Photoacoustic spectra of this two solid state samples are measured. We discuss the properties of the weak metal-metal bond of the Mo2(V) structure unit and assign symmetry properties of Mo-Mo frontier orbits.
Application of XPS to investigating Mo-Bi-Ce/SiO
2
Catalyst
Guo Qingling, Gui Linlin, Yu Qiquan, Jin Yun
1990, 11(2): 168-171.
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Mo-Bi-Ce/SiO
2
has been investigated by XPStechnique before and after reduction with mathanol. The result shows that the catalyst consists of Bi1
2
(MoO
4
)
3
and CeO
2
before reduction, and after reduction with mathanol Ce
4+
reduces to Ce
0
with a small amount of Ce
2
O
3
and Bi, Mo reduces to lower valence state. The sequence of reduction is Ce, Bi, Mo. Before reduction Bi resides at the external layer in the catalyst and then diffuses into internal layer during reduction. The reduced catalyst re-oxidized with oxygen in pulse experiment shows that all of active components are reoxidized and the sequence of oxidation is Mo, Bi, Ce. Bi migrates back to surface during reoxidation.
A Study on the Synthesis and Performance of a New Type of Bifunctional O
2
Electrode Material—Pb-Sb-Ru Pyrochlore Oxides
Yang Yifu, Zhou Yuenhong, Cha Chuanxin
1990, 11(2): 172-175.
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Anew method of coprecipitation in aqueous solution for synthesizing pyrochlore oxides with the formula Pb
2
[Ru
2-s-y
Sb
x
Pb
y
]-O
7-s
was established. These oxides rich in Pb have a relatively high surface area and a very good electrical conductivity. The good conductivity comes from the changeability of valence of Pb and Ru, and the co-existance of more than one valent states for an element. The polarization curves and life tests for O
2
reduction and evolution on the porous electrode made from such materials were measured. The results show that these materials have high electrocatalytical activities and stabilities for both O
2
reduction and evolution in a alkaline solution and at room temperature.
On the Oscillating Behaviors of Piezoelectric Quartz Crystal in Aqueous Electrolyte Solutions—Frequency and Frequency Shift
Zhou Tiean, Zhang Wenjlu, Nie Lihua, Yao Shouzhou
1990, 11(2): 176-179.
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Based on the equivalent circuit model of a piezoelectric crystal with both sides of electrodes immersed in liquid and the solution of the oscillating equation of Pierce oscillator, the relationship formula between the crystal oscillation frequency in electrolyte solution (F
1
) and the specific conductance of the solution (K) is derived as follows, F
l
=(1/2π)(1/C
1
+1/C
2
)(1/X
e
)[θ
2
(R
e
2
+X
e
2
)K
2
+2θR
e
x+1]. The validity of the F
l
-x relationship is demonstrated in KCl and Na
2
SO
4
aqueous solutions.
Studies on Thermodynamics of the Dissociation of Amino Acid in Mixed Solvents ( Ⅰ ) —Glycine
-1
,2-Propanediol-Water System at
278.15
-318. 15 K
Yang Jiazhen, Zhang Litian, Men Dianyuan, Liang Chunyu, He Limin, Sun Ailian
1990, 11(2): 180-183.
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The two thermodynamic dissociation constants of glycine at 5 different temperatures from 278.15 to 318.15 Kin 0.05 mole fraction 1,2-propanediol-water mixed solvent were determined from precise EMFmeasurements hydrogen-silver chloride electrondes in cells without liguid junction by using the polynomial approach proposed in this paper on the basis of Pitzer's electrolytic solution theory. As compared with traditional extrapolation on the basis of extended Debye-Huckel equation, the results obtained from both methods are in agreement with each other. The change of the first or second dissociation constants is given as a function of the thermodynamic temperature Tby empirical pK = A
1
/(T+A
2
+A
3
T). The thermodynamic quantities of dissociation in the mixed solvent are calculated and the results are discussed.
The Syntheses and Properties of Molybdovanadophosphoric Acid and Its Salts with Lanthanum
Wu Tonghao, Leng Yuchun, Yang Hongmao, Wang Guojia, Hua Shiying, Zhang Hengbin, Jiang Yuzi, Zhen Kaiji
1990, 11(2): 184-187.
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It is very important to synthesize and characterize molybdovanadophosphoric acid and its salts correctly for the fundamental investigation of these kinds of the catalysts. In this report, it is suggested that
51
V NMR, CV, IR, XRD, DTGand element analysis are used as the effective methods for checking the purity and characterizing the catalysts.
Studies on the Synthesis and Properties of Stannum Aluminophosphate Molecular Sieve
Han Shuyun, Zhou Shihong, Kan Qiubin, Wu Zhiyun, Wei Quan
1990, 11(2): 188-192.
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The pure Stannum Aluminophosphate molecular sieve was synthesized by means of hy-drothermal method. The structure of stannum aluminophosphate molecular sieve (SnAPO-5) was studied by X-ray diffraction analysis, XPS, infrared spectroscopy, electron probe, Mossbauer spec-troscopy. The lattice parameters and chemical composition of SnAPO-5 were determined. Some physicochemical properties and catalytic activity of SnAPO-5 molecular sieve were investigated. These results shows that the structure of SnAPO-5 is AlPO
4
-5 type and Sn
4+
does situate in the framework of the SnAPO-5 molecular sieve.
Kinetics of Ethylene Polymerization and Regulation of Molecular Weight with ZnCl
2
Zhao Zhenhe, Zhou Xinhua, Lu Zejian, Lu Yun, Lin Shangan
1990, 11(2): 193-196.
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The kinetics of the polymerization of ethylene has been studied at normal pressure with the highly active catalyst system TiCl
4
,NdCl
3
/MgCl
2
/Al(C
2
H
5
)
3
. The rate of polymerization V
P
,the specific number of active centers [C
*
] , the propagation rate constant k
P
,the activation energy ΔE and the lifetime of growing chain Lwere obtained by a kinetics method for the polymerization of ethylene. The influence of ZnCl
2
on the polymerization of ethylene has been investigated. It has been found that ZnCl
2
is a considerably effective transfer agent. Not only it decreases the molecular weight of polyethylene, but raises the catalytic efficiency notably as well. However, at a higher ZnCl
2
concentration, the rate of polymerization was decreased.
Analysis and Application of Pynamic Mechanical Temperature Spectra
Zang Kun
1990, 11(2): 197-201.
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In this paper, the relaxation time spectra are derived from the dynamic mechanical temperature spectra and the influences of the thermal treatment conditions on the fine structure of the samples are analyzed from the changes of the relaxation time spectra. Furthermore, the relationship between the ratio C
1
/C
2
of the parameters in the WLFequation and the super-molecular structure of the samples is discussed.
Studies on the Chemical Constituents of Saussurea Medusa Maxim (Ⅱ)
Jia Zhongjian, Gong Nichun, Du Mei
1990, 11(2): 202-204.
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Six compounds were isolated from Saussurea Medusa Maxim and identified by means of MS, 1H NMR,
13
C NMR, UV, IRand chemical methods. They are: Ⅰ , Luteolin-7-O-a-L-rhamnopyra-nosyl-(1→2)-BBB-D-glucopyranoside; Ⅱ , Apigenin-7-O-a-L-rhamnopyranosyl-(1→2)-BBB-D-glucopy-ranoside; Ⅲ, Quercetin-3-O-BBB-D-glucopyranoside; Ⅳ, Apigenin; V, Luteolin; , Ⅵ Arctiin, respectively.The presence of compounds Ⅰ,Ⅱ,Ⅲ and Ⅳ in this genus are reported for the first time and are significant to chemical taxonomy.
Synthesis of l-(2-Benzothiazolyl)-3-Phenyl Pyrazoline and Its Derivatives
Li Dongfeng, Jiang Guiji, Li Jingshu
1990, 11(2): 205-207.
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Twenty four 1-(2-benzothiazolyl)-3-phenyl pyrazoline derivatives have been synthesized. Their fluorescence properties and application possibilities are discussed.
Study on Chemical Constituents of Volatile Oils of Three Species of Rabdosias from Tibet
Li Zhaolin, Wang Mingkui, Chen Ning, Li Yuanzhong, Chen Yaozu
1990, 11(2): 208-211.
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In this paper, the chemical constituents of the volatile iols of three species of Rabdosias from tibet: Ⅰ. Rabdosia Parrifolia (Boital) Haara: Ⅱ . Rabdosia pseudo-irrorata C. y. Wu. ; Ⅲ. Rabdosia rugosa (Wall. )hara have been alalyzed by GC/MS. From Ⅰ , 84 peaks were separated, of which 27 major components were identified, constituting 60% of the total peak area. From Ⅱ , 72 peaks were separated, of which 39 major components were identified, consituting 82.5% of the total peak area. From Ⅱ , 90 peaks were separated, of which 39 major components were identified, constituting 62.1 % of the total peak area. The constituents and ralative quantity of the three oils were compared.
Influences of Iron and Cerium on Photoreduction Separation of Europium
Li Ruixiang, Yang Rudong
1990, 11(2): 212-214.
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In this paper, the influences of iron and cerium on the yield and induction time of photore-duction of europium are investigated with a low pressure mercury lamp(20 W) as the light source, the mixture of formic acid and sodium formate as the scavenger for OHradical and sodium sulfate as the precipitating agent for europium ( Ⅱ). The results show that the iron (Ⅱ) and cerium ( Ⅲ ) can be oxidized to iron (Ⅲ ) and cerium (Ⅳ ) in the photochemical process, and the europium ( Ⅱ ) is oxidized by iron ( Ⅲ ) and cerium (Ⅳ ) formed in this system, so that the yield of photoreduction of europium is decreased and the induction time of photochemical process is increased respectively with increasing of concentrations of iron and cerium in the solution to be photolyzed.
Graft Copolymerization of Starch-acrylamide Initiated by Manganic Pyrophosphate Complex
Feng Zhenguo
1990, 11(2): 215-217.
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Aseries of starch-polyacrylamide graft copolymers (ST-g-PAM) were prepared by Mn
3+
-initiated graft copolymerizations of acrylamide (AM) onto starch (ST) dissolved in water at 30℃. The effects of solution acidity and concentrations of monomer, starch and initiator on graft copolymer-ization were investigated.The copolymerization was much more susceptible to pHvalue of the reaction solution.Reaction mechanisms responsible for the initiation of graft copolymerization and homopolymeriza-tion of AMare proposed and discussed.
Polymerization of Pentacosa-8,10-diynoic acid LB Film
He Pingsheng, Han Qingping, Qin Zhihai, Wang Yongzhong, Chen Xin
1990, 11(2): 218-220.
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Pentacosa-8,10-diynoic acid has been synthesized and its LBfilm has been deposited. The polymerization of LBfilm of pentacosa-8,10-diynoic acid under UV-radiation was monitored by UV-visible,IRspectroscopies and X-ray diffraction. From this point, the possible arrangement of penta-cosa-8,10-diynoic acid molecules in LBfilm before and after polymerization was estimated.
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