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中文
Table of Content
24 January 1990, Volume 11 Issue 1
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Articles
The Syntheses and Characterization of Ruthenium Carbonyl Chlorodimethylsilyl Derivatives
Hu Xiang
1990, 11(1): 1-6.
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The cholrodimethylsilyl ligand containing derⅣatⅣes of metal carbonyl is believed to be very sensitⅣe in air . The author reports here that the reaction of SiMe
2
ClHand Ru
3
(CO)
12
gⅣes cis-Ru(CO)
4
(SiMe
2
Cl)
2
( Ⅰ )and [Ru(CO)
4
(SiMe
2
Cl)]
2
( Ⅱ ). The SiMe
2
Cl ligand in ( Ⅰ ) and ( Ⅱ ) shows the large irons-effect and thus syntheses of a number of derⅣatⅣes of the types mer-M(CO)
3
(PR
3
)(SiMe
2
Cl)
2
(X) (Ⅲ) (M=Ru, Os,PR
3
= PPh
3
,ETPB), trans-Ru(CO)
4
(SiMe
2
Cl)(X) (Ⅳ) (X=Br, I), [Ru(CO)
3
(SiMe
2
Cl)(X)]
2
(V), and Ru
2
(CO)
5
(SiMenCl
3-n
)(X)
3
(Ⅵ)(n = 1,2; X =C1, Br, I ) are reported. The relationship between geometries and the IRvco band numder are described. Ⅰ -Ⅵ have been characterized by IR,
1
H NMRand mass spectrometries. The IR
v
co
band in some of the SiMe
2
Cl contaning metal carbonyls have been found to be splitted. This may be re-sponsed to the conformational isomeerism of the SiMe
2
Cl group.
Study on Gadolinium Nicotinate Coordination Compound with 1, 10-Phenanthroline
Zhang Zhongsheng, Wu Jigui, Deng Ruwen
1990, 11(1): 7-9.
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In this work, gadolinium nicotinate coordination compound with 1, 10-phenanthroline was synthesized and characterized as Gd(Phen)
2
L
3
·3H
2
O(where HL = nicotinic acid, Phen = 1,10-phenanthroline) by chemical analysis, IRspectrum, thermal analysis, crystal structure analysis. The crystal is triclinic with coordination number eight. The parameters of unit cell are a= 9. 031Å , 6= 12. 857Å, c=17. 747Å.a=84. 923°, β=80. 564°, γ=84. 706°. The bccteriostatic tests show that Gd(Phen)
2
L
3
· 3H
2
Ohas a stronger bacteriostasis than Phen and GdL
3
· 2H
2
O, especially to Candida albicans, hay bacillus and Pseudomonas aeruginosa.
Synthesis and Magnetism of Novel Copper (Ⅱ)-Manganese (Ⅱ) and Copper (Ⅱ)-Cobalt (Ⅱ) Complexes Containing Phenoxy-Bridge
Liao Daizheng, Zhao Qianhua, Zhang Zhixong.Wang Genglin
1990, 11(1): 10-14.
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New binuclear complexes, [Cu(samen)Mn(NO
2
-
Phen)
2
] (1), [Cu(sampn)Mn(NO
2
-
Phen)
2
] (2) and [Cu(samen)Co(terp)] (3) were synthesized,where samen
4-
, sampn
4-
, NO
2
-
Phen and terp denote N, N'-ethylenedisalicylamidate anion, N,N'-1,2-propanedissalicylamidate anion, 5-nitro-l,10-phenanthroline and terpyridyl respectively. The complexes were characterized with variable temperature magnetic susceptibility. The exchange integral, J ,was found to be -63 cm
-1
(1), - 65 cm
-1
(2) and -7. 68 cm
-1
(3), indicating that antiferromagnetic spin exchange interaction operates among the metal ions.
Application of Double-Probe Transducer and Differential Cell to Photoacoustic Detection of Liquid
Zuo Boli, Deng Yanzhuo, Zeng Yun'e
1990, 11(1): 15-17.
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The double-probe transducer and differential cell for photoacoustic detection of liquid were suggested. The overlapped PAsignals, obtained by using such transducer, significantly increase sensitivity or effectually eliminate PAbackground signal due to a solvent. Application of this method to detection of Co
2+
by nltroso-R-salt reagent at 532 nm was demontrated. The lowest determination concentration is 0. 3 ng/mL, correspounding to 4. 25×10
-5
in absorptivity.
Application of Wall-Jet Electrode in Anodic Stripping Voltammetry with Flow Injection Analysis
Gao Guoqiang, Qi Deyao
1990, 11(1): 18-21.
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Awall-jet electrode was used in anodic stripping voitammetry with flow injection analysis. The equation derived from conventional stripping voltammetry with steady state deposition current is not applicable to a nonsteady state deposition process as in the FIAsystem, Atheoretical equation for the stripping peak current under flow injection condition was proposed. The peak current is predicted to be proportional to the R
3/4
(Ris the radius of the working electrode). This relation was verified through experiment results. With this system the experiment results show that the relative standard deviation is 0. 94% for determining 5×10
-7
mol/L Cd( Ⅱ ).
Studies on the Syntheses and Optical Properties of 5,5'-Bis(p-Substituted Phenyl)-2,2'-Bioxazoles
Qin Yuanxi, Wang Mingzhen, Gao Zhenheng
1990, 11(1): 22-25.
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Eight of 5,5’-bis(p-substituted phenyl)-2,2’-bloxazoles were synthesized, among them, six are new compounds. The relationships between optical properties and structures of these compounds were discussed. Acomparison between the optical properties of these compounds and those of corresponding 5,5’-bis(p-substituted phenyl)-2,2’-bl-1,3,4-oxadiazoles was made.
Investigation on Oxidation-Reduction Reaction of Biomimetic Insecticide [(CH
3
)
2
NHCH(CH
2
S
2
O
3
,)
2
Na·H
2
O] with Bromine
Zhang Changgeng, Luo Hongwei, You Ying, Wang Xin, Li Haiquan
1990, 11(1): 26-30.
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Oxidation-reduction reaction of biomimetic insecticide (CH
3
)
2
NHCH(CH
2
S
2
O
3
)
2
Na .H
2
Owith bromine has been investigated by X-ray single crystal structure analysis ,mass spectrometry, gravimetric analysis and coulometric titration. Our research shows that the reaction is homogeneous, there is transfer of six electrons in the reaction.
Research on Substituted 2-(2’-Phenylpropenyl) Benzoxazoles
Pan Jiaxing, Wang Chaojie, Gao Zhenheng, Yao Xinkan, Wang Ruji
1990, 11(1): 31-35.
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Eleven substituted 2-(2’-phenylpropenyl)benzoxazoles and nine substituted 2-(2’-pnenyl-propenyl)-5-methylbenzoxazoles were synthesized by the modified Wittig reaction. All of them were identified by elemental analysis, IRand NMRspectrometry. The crystal and molecular structure of 2-(2’-bromophenyl-propenyl)benzoxazole were determined by X-ray diffraction method.
Investigation of Electrochemical Characteristics of a New (Tailed Iron(Ⅲ) Porphyrin(Ⅰ)—Solvent Effects of Tailed Iron ( Ⅲ ) Porphyrin
Cao Xizhang, Wang Qingmin, Zhang Shuguo
1990, 11(1): 36-40.
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The electrochemical behavior and solvent effects of a new biological model compound—tailed porphyrin iron ( Ⅲ ) complex, meso-mono(o-(4-diethyl amino) butyramidophenyl) triphenyl porphyrin iron( Ⅲ) (meso-MDBPTPPFe( Ⅲ )Cl) was investigated by cyclic voltammetry. The experimental results demonstrate that (1) the terminal base in meso-MDBPTPPFeCl plays a part of potential modulation, and thus stabilizes the oxidation state of iron( Ⅱ ). (2) The half wave potential of each electronic pair for meso-MDBPTPPFe( Ⅲ)Cl is different with different solvents. Furthermore, the half wave potential of Fe( Ⅲ)/Fe( Ⅱ ) is almost directly proportional to the donor number of solvents, while that of Fe( Ⅱ )/Fe( Ⅰ ) is almost inversely proportional to the donor number of solvents.
Studies on the Exchange and Catalytic Activity of Magnesium Aluminophosphate Molecular Sieve
Han Shuyun,Wu Zhiyun, Kan Qiubin, Zhou Caiju, Yang Jun
1990, 11(1): 41-45.
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By means of infrared spectra and temperature programmed desorption, the surface acidity of magnesium alumlnophosphate molecular sieve(MAPO-5) was studied. The ion-exchange isotherm was measured for Ni
2+
-MAPO-5 system at 94℃. Catalytic hydrogenation activity over MAPO-5 and Ni-MAPO-5 catalysts was examined using ethylene hydrogenation as a probe reaction. The results indicate that the turnover number is increased with the increasing of reduction temperature for Ni
2+
-MAPO-5 catalyasts. The highest activity can be obtained on the catalysts reduced at 3201℃. and their activities decrease when the temperature is further increased. It may be found that the turnover number of ethylene on Ni atoms has unchanged whether the amount of Ni on the catalysts varied or not, within its concentration range, 0.4~3.2% wt. MAPO-5 has no activity for ethylene hydrogenation. The catalytic cracking activity of a-hexadecane over the same catalysts was also tested. The experimental results showed that the activities of Ni
2+
-MAPO-5 and MAPO-5 catalysts much higher than those of AlPO
4
-5 perhaps is due to the high acidities of the two types of the catalysts(MAPO-5).
The Crystal Structure of [UO
2
(NO
3
)
2
(H
2
O)
2
]·(DB18C
6
)
2
Gan Xinmin, Tang Ning, Wang Xin, Zhu Ying, Tan Minyu
1990, 11(1): 46-48.
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The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction. The complex crystal belongs to a monoclinic, space group P2
1
/n with Z=2. Lattice parameters are: a=11.782(2)Å, b=8.584(2)Å, c=22. 631(2)Å,β=98.29(2)°, V= 2265.1 Å
3
. The structure was analyzed by Patterson and Fourier techniques and refined by full-matrix least-squares to R=0. 066 for 3024 reflections. The uranyl group is not located within the crown ether. Rather, the structure consists of neutral UO
2
(NO
3
)
2
(H
2
O)
2
units and separate crown ether molecules connected by hydrogen bonding through coordinate water molecules. The oxygen atoms of the linear uranyl group are coordinated only to uranium; the eight-coordination of uranium is completed by six equatorial oxygen donors, two from water and four from bidentate nitrate groups. Each uranium is coordinated in a slight distorted hexagonal bipyramid configuration.
Relativistic Pseudopotential Ab Initio Study of Boron Halides
Ma Zhongxin, Li Xiping, Dai Shushan
1990, 11(1): 49-53.
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The relativistic effective core potential ab initio was presented for boron halides BX
3
(X=F, Cl, Br, I). The optimized geometries were obtained, and it is found that the σ-bonding decreases and π-bonding increases by degrees from BF
3
to BI
3
. Using one-electron S-Ooperator method, the photo-electron spectra of BX
3
were reassigned.
Laser Raman Spectrometric Determination of the Monolayer Dispersion Capacities of MoO
3
on Supports
Zhao Biying, Xu Qiang, Xie Youchang, Yang Xianchun
1990, 11(1): 54-57.
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The relationship between aggregative MoO
3
and total MoO
3
loading in MoO
3
/γ-Al
2
O
3
, MoO
3
/TiO
2
and MoO
3
/SiO
2
was determined by LRS. KNO
3
was used as the internal standard for the measurement of intensities. The obtained monolayer dispersion capacities by extrapolation correspond to those obtained by XPS, XRDand surface acidity measurement.Raman spectrometry can be used to indentify all molybdenum oxide species, for example the aggregative MoO
3
fine particles, Al
2
(MoO
4
)
3
and two dimensional Mo interaction species (monolayer dispersed MoO
3
). So this result is a direct and convincible evidence for the view of monolayer dispersion. Some informations about the structure of catalysts supporting MoO
3
have been obtained by LRS, which was not obtained by XPS, XRD. The trouble in the quantitative LRSdetermination for catalysts, its cause and the method to overcome it are also discussed.
Crystal Structure of 2,2'-Tetramethylene-Dioxodi(8-N- Salicylideneimino-naphthalene) Copper Complex
Liu Zuocai, Shao Meicheng, Tang Youqi
1990, 11(1): 58-61.
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The crystal structure of the title complex was determined by X-ray diffraction. It belongs to the monoclinic system, space group is P2
1
/a with cell dimensions a =9. 824(3)Å , b=35. 530(9)ÅA. c=17.552(6)Å,β=98. 97(2)°, V=6053(4)Å
3
and Z=8. The structure was analyzed by Patterson and Fourier technique and refined by block-matrix least squares to final residual factor of R = 0. 064. The complex is a trans-planar "capped" structure, with average bond length Cu-O 1.870Å ,Cu-N 2.007Å. There are two crystallographically independent molecules.
The Trace of the Curing Process of Alkyd Resin with FTIR
Hu Yuxin, Mao Kunyuan, Sun Yunxiu, Wu Tonghao, Yang Hongmao, Zhang Huixiang, Tang Xinyi
1990, 11(1): 62-65.
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The curing process of alkyd resin is investigated with FT-IRin this paper. The vibration of unsaturated carbon-hydrogen bonds was chosen as the characteristic change at 3007 cm
-1
and the stretching vibration of phenyl group at 1600 cm
-1
was chosen as the internal standard sign in the curing process of alkyd resin. The results show that the number of unsaturated bonds gradually reduces and the number of the functional groups containing oxygen, such as hydroxyl groups and carboxyl groups, gradually increases along with the curing process which indicates that some oxygen has been absorbed into the film. The curing speed of alkyd resin is related to the thickness of alkyd resin film. The curing speed of alkyd resin is controlled by the diffusion process of oxygen.
An ESR Study on Irradiation Crosslinked Poly (Methyr Vinyl Siloxane)
Lu Junhuai, Wu Ke, Ma Jitao, Yao Kangde
1990, 11(1): 66-70.
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The ESRspectra of all samples prepared in the previous paper are obtained at room and low temperature (liquid nitrogen 77K). The quartet with a hyperfine splitting of 23 gauss is due to radicals of type · CH
3
;the triplet with a hyperfine splitting of 22 gauss,due to · CH-Si≡ and the singlet due to ·Si≡ or · O-Si . The spectrum differs with the change in the silica filler content.The radicals produced in the irradiated PMVSare stable and decay slowly on keeping the samples at 77Kor room temperature, while warming the samples from 77K to room temperature, the radical .signal becomes weaken. Furthermore,the radicals in all samples almost disappear over 100℃ for 2h or more. These samples have a stable gel content at room temperature. In this way, the radicals in radiation crosslinked PMVScan be cleared up.The radiation behavior of PMVSand the influence of silica filler on the crosslinking are also studied in present work. The radicals in silica filler are observed. These radicals may couple with the main chain scission radicals resulted from mechanical processing to form crosslinks. The coupling of radicals has more chances in radiation crosslinking process, and PMVSwith filler does crosslink easier than PMVSwithout filler. So the enhancement of silica filler to radiation crosslinking of PMVSis mainly chemical mechanism.
Study of Immobilized Laccase and Its Properties
Zhan Dongfeng, Du Yumin, Qian Baogong
1990, 11(1): 71-74.
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Amethod of Rhus vernicifera laccase immobilized by using hydrous transition metal oxides is introduced and a possiblle model of hydroxyl groups of polysaccharide, which is a part of the enzyme, complexed with transition metal ions is given. The optimal condition of immobilization of laccase by chelating .method is investigated. The properties ef the free laccase and the immobilized laccase are compared and the possible reasons for the differences of them are discussed.
Studies on the Synergistic Extraction of Gold( Ⅲ) with N
1923
and Ph
3
PO
Jiang Dehua, Wang Boyong, Shen Jinglan
1990, 11(1): 75-77.
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The synergistic effect of the extraction of Au( Ⅲ) from HCl medium with N
1923
(primary amine)-Ph
3
POin CHC1
3
was investigated. The effects of the concentration of AuCl
4
-
Cl
-
and H
+
ions in aqueous phase and that of Ph
3
POand N
1923
in the organic phase on the synergistic extraction of Au( Ⅲ ) with N
1923
-Ph
3
PO-CHCl
3
were studied respectively by the slope method.
Studies on Boron Compounds (ⅩⅩⅢ)—Reaction of Potassium Tetrahydroborate with Ferrocenylmethyl Trihydrocarbyl Ammonium Chlorides
Zhang Guomin, Jiang Fengchao, Zhang Lun
1990, 11(1): 78-80.
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In this work , the reactioin of KBH
4
with C
5
H
5
FeC
5
H
4
CH
2
NMe
2
(R)Xin aqueous solution is investigated. It is found that when Ris an electron-drawing group, the product is a quaternary ammonium salt of BH
4
-
when Ris an electron-donating group or H , the product is a complex of BH
3
. The compositions of the products were identified by elemental analyses and IRspectrometry. The reaction provides a simple , high-yield synthetic procedure for quaternary ammonium salts of BH
4
-
and complexes of borane.
Peroxidase Catalytic Fluorescence Reaction with Tyrosine as Substrate
Ci Yunxiang, Chen Lie, Wei Shan
1990, 11(1): 81-83.
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Fluorescence behaviours of L-Tyr-H
2
O
2
-HRPsystem were investigated. The results indicate that tyrosine is not equal to homovanillic acid for the structure of the substrate, but tyrosine and ho-movanillic acid have the same linear ranges and sensitivities in the enzymatic analysis, and tyrosine can replace homovanillic acid. Therefore, it is possible to make good use of that reaction. The method has been used to determine glucose and tyrosine in human sera and the results are obtained satisfactory.
Study on petermination of Tellurium by MIPAES
Yu Shirong, Zhang Hanqi, Jin Qinhan(Q. Jin)
1990, 11(1): 84-86.
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In this paper, the determination of tellurium by ETV-MIPwith a new micro sample introduction system was studied. It was shown that the addition of SnCl
2
AEScan increase the emission signal of Te at 214.3 nm. The detection limit is shown to be 5.0 ng/mL. The influence of alkali halide in the aqueous solutions with SnCl2 and without SnCl2 on the emission signal of Te 214.3 nm line was studied in some detail.
Studies on Luminol-KIO
4
-Triton X-100-Ru(Ⅳ) Chemiluminescence System and Microdetermination of Ru in Au-Os-Ru Mixture
Xu Xiaowen, Li Ungying, Hu Chengwen, Wang Rong
1990, 11(1): 87-89.
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The sensitization effect of Triton X-100 for the chemiluminescence system of Luminol -KIO
4
-Ru(Ⅳ) has been first reported. The detection limit of Ru( Ⅳ) has come down to 3.9×10
-4
μg/ mL. After Au-Os-Ru mixture is separated by reversed phase paper chromatography with di-p-methyl phenyl sulfoxide as the stationary phase,this method can be used in the microdetermination of rutheni-um(Ⅳ). The results of recovery with 95%-106% are satisfactory.
Chemical Constituents of the Essential Oil of Hyssopus Cuspidatus Boriss
Xue Dunyuan, Chen Ning, Pan Xinfu, Liu Yongmin
1990, 11(1): 90-92.
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Hyssopus cuspidatus Bariss was found to contain d-pinocarvone (44.3%) as main component in essential oil by means of preparative chromatography and IR,
1
H NMRand MSspectrometry. However it was reported in literature that .this species contains Z-pinocamphone as main component. Three other high-content components, l-pinocamphone, β-pinene and 1,8-cineole also were isolated and identified. All the 32 components were identified and estimated from the essential iol both by capillary gas chromatography /mass spectrometry and by the.Kovats Index of the components.
The Synthesis of the Analogues of 9-β-D-Xylofuranosyl-Adenine
Dong Lingjiao, Shi Yunchuo, Ma Lingtai, Zhang Lihe
1990, 11(1): 93-95.
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8-Substituted amino derivatives of 9-β-D-xylofuranosyl-adenine were prepared. The structures of these compounds were identified by UV, 1H NMRand mass spectra. All these compounds are of β-configuration. The yields ranged from 79% to 32%. The procedure of key intermediate was improved to give a yield increased to 21%.
Catalytic Asymmetric Darzens Condensation in the Presence of β-Cyclodextrin
Huang Naiju, Huang Yongming, Meng Weidong, Zhang Daodao
1990, 11(1): 96-98.
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Darzens condensation of aromatic aldehydes with phenacyl halides in the presence of B-cy-clodextrin afforded the corresponding epoxykedones with enantiomeric excess up to 9%.
Studies on Flavonoids(XIV)— Debromination Reaction in the Synthesis of Bromoisoflavones
Yue Baozhen, Zhou Zewei, Cai Mengsben
1990, 11(1): 99-101.
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6- Bromoisoflavone was prepared from 4- bromoresorcinol. Debromination reaction was found in the acylation of the starting material by using BF
3
as catalyst, and a by-product, 4,6-dibro-moresorcinol, was also isolated. The reaction mechanism probably involves a bromonium ion.
The Crystal Structure of JR-( -)-Chloromethyl-4-Ethylsilatrane
Yang Yunyun, Yin Chenglie, Chen Guangxu, He Cunheng
1990, 11(1): 102-104.
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The title compounds crystallized in orthorhombic system with space group P2
1
2
1
2
1
and cell dimensions a = 7. 964 (2)Å , b = 9.047(4)Å, c= 16. 864(8)Å , V=1215.0Å
3
, Z=4, D
e
= 1. 375 g ·cm
-1
, λ=1. 5418 A, μ=13.067 cm
-1
. The structure was solved by direct method and refined by block-matrix least-squares. The final discrepancy factors are R=0. 034 and R
w
=0.040 for 959 reflections with I>2. 5<r(I). The Si←Nbond length is 2.102(3)Å.
Kinetics and Mechanism of Oxygen Atom Transfer Reactions to M
3
(CO)
11
L(M=Fe, Ru, Os)
Shen Jiankun, Gao Yici, Shi Qizhen
1990, 11(1): 105-107.
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Detailed kinetic data are reported for substitution reactions of M
3
(CO)
11
L(M=Fe, Ru, Os) in CHCl3 in the presence of Me
3
NO. Amechanism is proposed, and the effects of substituted ligands are discussed.
Study on Permeability of PU-PDMS Semi-IPN
Xiao Hong, Ping Zhenghua, Xie Jingwei, Yu Tongyin
1990, 11(1): 108-110.
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In this paper, the permeability of Polyurethane-Polydimethylsiloxane (PU-PDMS) semi-IPNwas studied. It is found that the gas permeability coefficient Pand the selective separation factors ao
2
/N
2
are determined by the composition of the semi-IPNand the crosslinking density of PDMScomponent. In the midrange composition, Pis equal to 2. 26 × 10
-12
(cm
3
·cm/cm
2
·s·Pa) and ao
2
/N
2
is 3.05.
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