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中文
Table of Content
24 January 1989, Volume 10 Issue 1
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Articles
Studies on Coordination Compounds with Picolinaldehyde N-Oxide Derivatives as Ligands (Ⅰ)--syntheses and Crystal Structures of Cupric Complexes with Bis-Schiff Bases from Picolinaldehyde N-Oxide and Diamines
Zang Yan, Lu Qin, Yin Zhanfeng, Zeng Cheng, Dai Anbang, Zhou Zhongyuan
1989, 10(1): 1-5.
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Cupric complexes of bis-Schiff bases prepared by condensation of pico-linaldehyde N-Oxide(pio) with ethylene diamine(en) and trimethylene diamine(tn), [Cu(Pioen)H
2
O](ClO
4
)
2
and CCu(Piotn) (H
2
O)
2
](ClO
4
)
2
, were synthesised and their crystal structures were determined. The main crystallographic data are as follows. CCu(Pioen)H
2
CO(ClO
4
)
2
, ortborhombic system, space group P2
1
2
1
2
1
, a=7.9534(19)Å, b=9.6768(48)Å, c=26.1037(189)Å, Z=4 , R=0. 0771; CCu(Piotn) (H
2
O)
2
](ClO
4
)
2
, ortborhombic system, space group P
nam
,a=7.1360 (24)Å, 6=13.7887(42)Å.c=22.2556(81)Å,Z=4, R=0.0491. The intensity data were collected on R3m/Efour-circle diffractometer with Mo
K
a radiation. The structures were solved by Patterson method and refined by full matrix least-square method.
Studies on the Complexes of Sn (Ⅳ), Pd (Ⅱ) and Au (Ⅲ) with Di(2-Ethylhexyl) Sulfoxide
Wang Hanzhang, Liu Guoxing, Zhu Qinhua, Lu Zhonge
1989, 10(1): 6-10.
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The complexes of tin (Ⅳ), palladium (Ⅱ) and gold(Ⅲ) with di(2-ethylhexyl) sulfoxide (DEHSO) were synthesized in hydrocholoric acid medium. The compositions and the structures of Sn (DEHSO)
2
Cl
4
, (PdCl
2
DEHSO)
2
,H
3
O(DEHSO)
3
AuCl
4
are inferred by elemental analysis, molar conductance, IR and UV spectra.
Synergistic Extraction of Lanthanum with 1,9-Bis (1' -Phenyl-3' -Methyl-5' -Oxopyrazol-4' -yl) -1,9-Nonanedione and1,10-Phenanthroline or 2,2'-Bipyridyl
Lin Zhongping, Liu Songyu, Zhang Tianfa
1989, 10(1): 11-16.
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1, 9-bis( 1'-phenyl-3'-methyr-5'-oxopyrazol-4'-y1)-1, 9-nonanedione (H
2
A) was one of a series of bis acyl pyrazolone chelate extractants synthesized recently. In this paper, single and synergistic extraction by H
2
A and 1,10-phenanthroline or 2,2'-bipyridyl(simplified as B) for lanthanum from aqueous nitric acid or nitric acid and sodium acetate buffer have been investigated, respectively. By using slope analysis method the formulas of the extracted complexes have shown to be LaA· HA·B and the extraction equlibrium constants have been calculated. The values of the equlibrium constants (1gβ
281
) of LaA·HA·Bshow large synergistic effect. The solid extracted complexes were isolated from the solution. The compounds were studied by elemental analysis,TG-DTA, UV, IR,
1
HNMR and the solubility in chloroform was determined.
Studies on Complexes of Schiff Bases Containing Sulfur(Ⅶ) --Gomplexes'of Cobalt with o-Chlorobenzaldehyde and Benzal Acetone Schiff Bases
Yu Baoyuan, Sun Yifang, Fu Benqiu, Dai Huan
1989, 10(1): 17-20.
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The complexes of cobalt with Schiff bases derived from S-benzyldithio-carbazate have been prepared and characterized by elemental analysis, molar conductances, magnetic susceptibility, IRand UV-visible spectrosmetry.Based on these chemical properties examined, we can suggest that o-chloroben-zaldehyde Schiff base (HL
1
) forms a diamagnetic complex [Co(L
1
)
3
] having octahedral structure. Benzal acetone Schiff base (HL
2
) forms the dinuclear cobalt (Ⅱ) complexes [CCo
2
(HL
2
)
2
(L
2
)
2
X
2
] (where X=Ac
-
or Cl
-
) in which the two cobalt atoms are respectively bridged by two Ac
-
or Cl
-
. These complexes have subnormal magnetic moments, it clearly shows that there is a antiferromagnetic exchange interaction in it. Ligand HL
1
and [Co(L
1
)
3
] has also been screened for bactericidal activity.
Polarographic Adsorptive Wave of Copper-
meso
-Tetra(4- trimethylammoniumphenyl) Porphyrin Complex
Wang Changfa, Zhao Zaofan
1989, 10(1): 21-25.
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The sensitive adsorptive complex wave of copper-meso-tetra(4-trime-thylammoniumphenyl)porphyrin(T(4-TMAP)P) complex was studied in detial. The. peak potential of the wave is about-1.24V(vs.SCE) in 1mol/L KOH solution. The detection limit is 2×10
-8
mol/L. The peak height is linearly proportional to . the copper concentration over the range of 2×10
-8
mol/L to 9×10
-6
mol/L. In' the presence of 5 × 10
-3
mol/L EDTA and 5×10
-2
mol/Ltartrate, at least 100. times that of common cations and anions, except more than 10times that of Pd
2+
. and SeO
3
2-
, do not interfere the determination of copper. The method was success-fully applied to the determination of trace amounts of copper in hair, waste water, liver and aluminium alloy samples.The mechanism of the polarographic wave was studied by several electrochemical methods. The composition and conditional stablity constant of Cu(Ⅱ)-T(4-TMAP)P complex were determined by "Polarographically continuous variation method". The results show that the ratio of Cu:T(4-TMAP)P in the complex is 1:1; the conditional stablity constant of complex β' is 7.5 ×10
7
.
Determination of Tellurium with Atomic Absorption Spectro- metry by Using Hydride Generation Under Subatmos- pheric Pressure and Vacuum Flameless Atomizer
Zhang Baogui, Tao Keyi, Feng Jianxing
1989, 10(1): 26-29.
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A new method for the determination of tellurium at sub-microgram levels by vacuum flameless atomic absorption spectrometry is described. Tellurium hydride is generated and collected under subatmospheric pressure. The hydride is then put into a vacuum quartz tube with a vacuum pump. It was found that the sensitivity of determining tellurium was increased by adding a small amount of oxygen or air to the hydride generator after the formation of the hydride. The detection limit (based on three times the standard deviation of twenty blank measurements) was 0.026ng. Ten replicate determinations of 2.0 ng Te gave a relative standard deviation of 3.9%.
Study on Anodic Stripping Voltammetry of Trace Lead at Oxalic Acid Modified Electrode
Fang Yuzhi, Bai Zhuping, Jin Litong
1989, 10(1): 30-34.
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In this paper, the preparation of oxalic acid modified electrode, reaction mechanism and electrochemical characteristics of trace lead on the electrode arereported. The Si(CH
2
)
3
NHCCOH group was covalently bonded to glass carbonelectrode surface through chemical reaction. The group could form stable complex with lead in solution and increase the deposition amount of lead on the electrode surface with electrochemical reaction. The behavior of the lead at electrode was investigated by anodic stripping voltammetry in following conditions: 15ng/mL of lead in HAc-NaAc system was preconcentrated at a controlled potential of -0.90 V(vs,SCE) for 2 min, then followed by scanning till -0.10 V(vs, SCE). The anodic stripping voltammograms showed an increase of current at about -0.54V (vs,SCE). Its sensitivity was 7.5 times highter than that of normal glass carbon electrode. The peak height is linearly related to the concentration of lead in the range of 1.0-15.0ng/mL. The relative standard deviation for twelve parallel determinations is 3%. The lead in urine was determined by oxalic acid modified electrode with satisfactory results.
Syntheses of Some Endo-o-Substituted-o-methyl Bicyclo[2,2,1]heptane-2-methanols and Relations Between Their Structures and Odors
Wang Xiaolan, Tang Shixiong, You Sbaocbun, Wang Cbangfeng, Cao Yurong
1989, 10(1): 35-39.
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Eighteen title compounds were synthesized. The refractive indices (or melting points), retention times in GLC, Rf in TLC, MS, IR and
1
HNMR spectra of these compounds were obtained. Their olfactory characteristics were evaluated and compared with endo-a-substituted-a-methylbicyclo[2, 2, 1]hept-5-ene-2-methanols. The relations between structures and odors were discussed.
Synthesis and Structure-Activity Relationship of (Z), (E)-α-Chlorocinnamamides
Wang Shuyu, Wang Yingfen, Liu Weiqin, Hu Gaoyun, Shi Simin, Zong Jingmin, Tao Cheng
1989, 10(1): 40-44.
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The(Z), (E)-or-chlorocinnamic acid with different substituents on the aromatic ring could be obtained by the alkaline elimination of α,β-dichlorophen-ylpropionic acids. The position of the substituents on the benzene ring showed important influence on the ratio of the (Z) and (E) isomers.The substituted (Z), (E)-α-chlorocinnamic acids were converted into corresponding (Z), (E)-α-chlorocinnamamides by means of acid chlorides and amin-olysis. After chromatography, we isolated ten pairs of geometric isomers including (z) and (E)-m-chloro-α-chloro-N-sec-butyl-cinnamamides.The configurations of α-chlorocinnamamides were assigned based on UV λ
max
, ε
max
and chemical shifts of amide and olefinic protons. The values of UV λ
max
, ε
max
and of chemical shifts (ppm) were greater for (Z) form and less for (E) form. The configurations were also confirmed by X-ray diffraction.Among ten pairs of isomers, (Z)-p-bromo-α-chlorocinnamoyl sec-butyl-amine was found to be more potent in anticonvulsive activity than others. The pharmacological evaluation showed that the configuration and the substituents at amide group displayed important effect on the biological activity.
Studies on Nitroxides(XXI)--Contact Charge Transfer Complexes of Piperidine Nitroxides with Halomethanes and Their Photo induced Reaction
Jiang Zhiqin, Wu Shuping, Zhang Maoxi, Liu Youcheng
1989, 10(1): 45-50.
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The contact Charge transfer (CCT) complexes formed from piperidine nitroxides and halomethanes and their photo-induced electron transfer reactions were studied by UVabsorption spectrometry. It was found that the π-π
*
transition of the nitroxides in halomethahes showed red shift, and the values of the determined complex stability constants between nitroxides and halomethanes were very low. This was consistent with the formation of their characteristic CCT complexes. The radical 2 as an electron donor underwent a rapid photo-induced redox reaction in carbon tetrachloride leading to the formation of the corresponding piperidine hydroxylamine hydrochloride. Oxygen showed a little influence upon the reaction. The reaction mechanism caused by CCT was briefly described.
The Synthesis and Properties of α,ω-Dihydrocarbyl Substituted Permethylpolysilanes
Guo Yuping, Xu Shansheng, Zbou Xiuzhong
1989, 10(1): 51-55.
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Eighteen sym- and unsym-a,w-dihydrocarbyl substituted permethylpoly-silane were synthesized by means of the reaction of a, w-dichloropermethylpolysi-lane and the corresponding Grignard reagents. The IRspectral data showed that the C=CH
2
out-of-plane bending bands of vinyl substituted compounds are ～13cm
-1
larger than that of the corresponding allylic compounds, it may be interpreted by the d
si
-π effect. The UVspectral bathochromic shift of vinyl substituted permeth-ylpolysilane is greater than that of the corresponding allylic compounds,it is due to the σ
si-si
-π
*
conjugative effect. The rearranged fragments of ArRMeSi
++
. appeared in the MSspectra of some of these compounds.The peaks of ArRMe
2
Si
++
. are the base peaks.It showed that the stability of Ar-Si bonds has been enhanced by the d
is
-π effect.
Studies on Electronie Structures of Cluster Compounds [Fe
4
S
4
Cl
4-n
(S
2
CNEt
2
)
n
)
2-
(n=0, 1, 2, 4)
Guo Chunxiao, Xu Jiqing, Wei Quan
1989, 10(1): 56-61.
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The electronic structures of cubane-like series Fe-Scluster compounds [Fe
4
S
4
Cl
4-n
(S
2
CNEt
2
)
n
]
2-
(n=0,1,2,4) have been studied by using CNDO/2 method. The bonding between Fe atoms, the effect of chelating ligands (S
2
CNEt
2
)
-
on the electronic structures, and the oxidizing-reducing properties of these cluster compounds have been discussed.The following results have been obtained: There are two types of Fe atoms of different valence states in the cluster compounds with (S
2
CNEt
2
)
-
ligands, and the electrons of μ
3
-S, are delocalized in [Fe
4
S
4
]
2+
frameworks. These results are in agreement with that of Mossbauer spectra exactly.
A Theoretical Study of Localized Orbital of the Molecules Containing C, H, O and N Atoms and Double Bonds
Ding Yu, Yu Hengtai, Yang Zhongzhi
1989, 10(1): 62-67.
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The localized molecular orbitals(LMO) of selected 22 organic small molecules containing C, H, O and Natoms and double bonds are studied by use of ab initio STO-3Gand Foster-Boys localized program. The energies of the LMO's are obtained and the interactions between corresponding LMO's are examined. The photoelectronic spectra of the molecules of ehtylene series are analyzed by using LMO model and the results are consistent with experiments.
Studies on Clonidine Hydrochloride Selective Coated Wire Electrode with Bilayer Polymeric Films
Hu Xiaoya, Leng Zongzhou
1989, 10(1): 68-71.
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A new type of coated wire electrode (CWE) with bilayer .polymeric films is reported. Platinum wire is modified by conductive polyaniline and then with a film of PVC (containing electroactive species). This kind of electrode not only has merits of CWE, but also has fine stability and repro-ducibility. With successive determination of 8 hours, the potential drifts are about 0.8mV. The Nernstian linear range of electrode shows 1 × 10
-1
～8×10
-6
mol/L with an average slope of 56.7mV/decade. The direct potentiometry for samples shows 100.9% of average recovery and 1.3% of standard deviation.
Theoretical Study of UV Spectra for Nitrophenylpolysilanes
Li Zhiru, Wu Yanhuo, Sun Jiazhong
1989, 10(1): 72-76.
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The UV spectra of p-NO
2
-m-(SiMe
m-3
)
n
(SiMe
3
)
n
and m-NO
2
-ph (SiMe
m-3
) (SiMe
3
)
m
systems (m= 1, n=0,1,2; m=2n= 1) are analyzed by means of the EHMO-CI-SPIN-FREE method with four orbital model. The first, second and third absorpt on bands arise in essence from π→π
*
transitions. Furthermore, the d atomic orbital of silicon chain may play an important role in the red shift of first absorption bands of p-NO
2
-ph(SiMe
3-m
)
n
, (SiMe
3
)
m
system. This can be considered due to two effects. One of them is the conjugation of d orbital (π
d
(Si)) with π
*
(ph) in LUMO. The other is the changing of electronic repulsion by changing d orbital and NO
2
group components in LUMO.
Synthesis and Structure of {(NH
4
)(18-Crown-6)][Bi(NCS)Cl
3
)]}
n
Fan Yuepeng, Xu Hongwei, Zhang Wenxing
1989, 10(1): 77-82.
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This paper reports on the synthesis of the title compound by means of using gel method. The compound was characterized by elemental analysis, IR, MS and differential thermal-thermal gravimetric analysis. Using a four cycle diffractometer determined the crystal structure.The crystal belongs to the triclinic system and the space group is P1with cell parameters, α=9. 097(2)Å, b=15.754(3)Å, c= 16.556(2)Å, α=88.08 (1)°, β=81.29(1)°, γ=86.62(2)°, Z=2. The result of crystal structure analysis shows that the 18-crown-6 coordinates with ammonium to form cation and the Bi(Ⅲ) is coordinated by thiocynates and chloride ions to form a polymeric negative ion chain.
A Study on Living Radical Polymerization by Using BDC as Photoiniferter
Li Zengji, Shen Jiacong, Dong Fengxia, Zheng Yingguang
1989, 10(1): 83-86.
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The polymerization of St by using BDG as photoiniferter was studied. In the photopolymerization, both the yields and average-molecular weights of polymers were found to increase with the reaction time. The polymers with functional end groups were obtained. In the 'polymerization process, the stable small radical which was produced by photolysis of BDCor functional end groups and the propagating radical of St were determined by ESR. This living radical photopolymerization mechanism was explained.
Synthesis of Two Component Interpenetrating Polymer Network
Geng Kuishi, Su Yanxi, Cai Dongrui, Yu Xuehai, Chen Qiugmin
1989, 10(1): 87-91.
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Interpenetrating polymer network materials based on castor oil urethane acrylate (network Ⅰ) and a castor oil-polypropyleneoxide tolylene diisocyanate urethane system (network Ⅱ) were synthesized by using thermo- and photo-polymerization alternately.The dynamic mechanical and stress strain properties of IPNsamples with different weight ratio of network Ⅰ and network Ⅱ and varying molar ratio components in network Ⅱ were also investigated.The dynamic mechanical spectra shows that all the samples exhibit two TAN maxima which indicate a two phase morphology.The stress at break was found to increase with increasing the network Ⅰ and the different molar ratios in network Ⅱ and possess a considerable effect on the tensile properties.
Characterization of Acrylic Elastomer
Zhang Banghua, Chen Junjie, Song Moudao, Zheng Junwen, He Binglin
1989, 10(1): 92-96.
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Acrylic impact modifiers(ACR) for poly (vinyl chloride) (PVC) were prepared by free-radical-initiated polymerization. ACRelastomers prepared from various components of butyl acrylate (BA), methyl methacrylate (MMA) and crosslinker, have been studied by dynamic mechanical viscoelastometer and infrared spectroscopy. It is shown that there are two glass transition temperature for each ACRelastomer. The experimental result of PVC/ACR blends shows that ACR-Ⅰ-3 and ACR- Ⅱ-3 are excellent impact modifiers for PVC.
Surface Structure and Properties of Mica Treated with Plasma
Xu Xi, Gong Xiaoyi, Liu Xueshu
1989, 10(1): 97-100.
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The chemical structure of mica surface treated with ethylene plasma of radio frequency and plasma polymerization reaction of ethylene in the presence of mica were studied by means of elemental analysis, GC-MS, PGC and ESR. It shows that the mica particle is wrapped by a dozens-of-angstroms-thick film, the chemical structure of which is the same as that polymerized in the absence of mica. Using SEM, we found for the first time the star fish-like morphology of plasma polymerized film. The "star fish" expands with the plasma treating time while its shape remains unchanged. The contact angle of water on mica surface treated by different methods at various conditions was measured. The results indicate that hydrophobicity of mica surface resulting from ethylene plasma treatment is greater than that both from Ar Plasma treatment and from silicane or titanate coupling agents.
Investigation of Adsorptivt-Complex Waves of Nickel and Cobalt with Zincon --Consecutive Determination of Trace Nickel and Cobalt in Copper Ore Concentrate
Lin Yilan, Cai Sula, He Keren
1989, 10(1): 101-103.
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In the solution of 4 × 10
-5
mol/L Zincon-o.4mol/LNH
4
Cl-0.6% Na
2
SO
3
two sensitive adsorptive-complex waves of Ni-Zincon and Co-Zincon were observed by single-sweep polarography. The peak potentials of the waves are -0.84V and -0.96V (vs. SCE), respectively. Various conditions of adsorptive-complex waves of Ni and Co in this system were studied; and the properties of these waves were investigated. The compositions of the complex of Ni and Co with Zincon also were determined to be 1:1.
Study on Charge Transfer of Ethyl Violet-Perchlorate Ion Pair System Across the Interface of Water/1,2-Dichloroethane
Shao Yuanhua, Yuan Haibe, Li Peibiao, Zhao Zaofan
1989, 10(1): 104-105.
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The electroactive system of ethyl violet-perchlorate for perchlorate electrode was studied by Current scan polarography and chronopotentiometry. The results showed that the transfer process of perchlorate ion across the interface of W/DCE is reversible. The response mechanism of perchlorate electrode was verified as a Nernstian response. The standard potential and standard transfer free energy of perchlorate ion are Δ
O
W
Φ
0
=-0.12V and ΔG
tr
0W-O
=-11.58kJ·mol.
Simultaneous Determination of Niobium and Tantalum with Dual-Wavelength Spectrophotometry
Ni Yongnian, Huang Guoping
1989, 10(1): 106-108.
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Adual wavelength spectrophotometric method for the simultaneous determination of niobium and tantalum is presented. This method is based on measuring the absorbance of colored products of niobium and tantalum with 2-(5-bromo-2-pyridylazo) -5-(djethylamino)phenol at two wavelengths. The reference wavelength is at the absorbance peak of the reagent.This method can be used to calibrate the deviations of absorbance from the Beer's law and is probably better than the traditional dual-wavelength spectrophotometries. Several synthetic samples were determined and the results are satisfactory by comparison with the standard addition values.
Study on Chemical Ingredients of Poiygonum Aubertii (L. Henry) from Tibetan Medicinal Herbs
Cuen Yaozu, Zhang Huidi, Zhang Shuoming
1989, 10(1): 109-111.
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The chemical ingredients of a tibetan medicinal herb, collected from South Gansu Tibetan Autonomous Region in August 1986 and identified as polygo-num aubertii (L.Henry) , have boon studied. From the aerol part of this herb, seven crystalline compounds have been isolated by extraction, liquid chro-matography and fractional recrystallization. Based on the chemical and spectral (UV, IR,
1
HNMR,
13
CNMR and MS) evidences, they were identified as α-L-butyl sorbopyranoside, 2,4-diphenylpyrrole, stagmast-4-en-3-one, stagmast-5-en-3-01-7-one, syringic acid, β-sitosterol, and tetracosanoic acid. These compounds have not been found in this herb previously.
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