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Table of Content
24 April 1988, Volume 4 Issue 2
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Articles
Synthesis and Crystal Structure of GaPO
4
-C
4
: Ga
3
P
3
O
12
·H
2
O·H
2
NCH
2
CH
2
NH
2
Feng Shouhua, Xu Ruren, Yang Guangdi, Sun Honglin
1988, 4(2): 1-7.
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A gallophosphate, Ga
3
P
3
O
12
·H
2
O·H
2
NCH
2
CH
2
NH
2
, named GaPO
4
-C
4
was hydrothermally synthesized from EDA(ethylenediamine)-Ga
2
O
3
-P
2
O
5
-H
2
O systems. The crystal structure of GaPO
4
-C
4
was determined by single crystal X-ray diffraction. The compound crystallizes in monoclinic system with space group P2
1/n
, a=8.688(4)Å, b = 17.952(6)Å, c=9.104(3)Å, β=108.27(3), V=1348.3Å
3
. The framework of GaPO
4
-C
4
contains three types of P atoms and three types of Ga atoms. Of the three types of gallium atoms, two types are located in distorted trigonal bipyramids and the third type lies at tetrahedral centre. The three-dimensional framework is built of two-dimensional nets which consist of irregular 3-, 4-, 5- and 8-rings and contains 8-ring channels running along [101], in which ethylenediamine templates are located.
A Study on Thermal Decomposition of K
3
[Fe(CN)
6
] and KFe[Fe(CN)
6
] in Helium
Chen Hanwen, Xin Xinquan, Niu Junning, Dai Anbang(A. P. Tai), Wang Xin, Zhang Yuchang
1988, 4(2): 8-11.
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K
3
[Fe(CN)
6
] and KFe[Fe(CN)
6
] are classical coordination compounds. However, the mechanism of decomposition reactions has not been well expounded. The gas products of thermal decomposition were examined by gas chroma tography (GC), and the structure of the solid products by Mossbauer spectroscopy(MS) and X-ray diffraction(XRD). The findings are explained in terms of the theory of coordination chemistry and a decomposition mechanism is proposed in this study. On the basis of various experimental results, the first stage of the decomposition of K
3
[Fe(CN)
6
] in He was found to be the evolution of(CN)
2
resulting in the reduction of Fe(Ⅲ):12K
3
[Fe(CN)
6
]→9K
4
[Fe(CN)
6
] + Fe
2
[Fe(CN)
6
] + 6 ( CN)
2
For KFe [Fe(CN)
6
], the first stage of decomposition man be represented as 6KFe[Fe(CN)
6
]→3K
2
Fe[Fe(CN)
6
] + 2Fe
2
[Fe(CN)
6
+ 3(CN)
2
At higher temperatures, the decomposition of both K
3
[Fe(CN)
6
) and KFe[Fe(CN)
6
] to form KCN and Fe
2
C was accomplished by the release of(CN)
2
and N
2
.
Spectrophotometric Study of Reaction Between Platinum and α,β,γ,δ-Tetra-(2-Chlorophenyl) Porphyrin
Li Youfen, Xiao Hong
1988, 4(2): 12-16.
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The present paper describes the complex reaction of α, β,γ, δ-tetra-(2-chlorophenyl} porphyrin with platinum in the presence of the mixture surfactant, sodium dodecylbenzene sulfonate and OP, and a new highly sensitive method for spectrophotometric determination of micro amounts of platinum. Beer's Law was obeyed when the concentration of platinum was in the range of 0-1.2μg/25ml. The molar absorptivity was found to be 3.1×10
6
L mol
-1
cm
-1
at 417nm.
Studies on the Solution Equilibrium of 7-(2-Pyridylazo)-8-Hydroxyq uinoline
Tong Shenyang, Zeng Wei
1988, 4(2): 17-24.
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The dissociation constant of PAOx was determined spectro-photometrically in the presence or absence of surfactants. The state of PAOx in aqueous solutions was studied by using spectro-photometric and quantum chemical methods. The tautometric equilibrium is shifted to the quinone-hydrazone form in the presence of CTMAB.
Photoacoustic Spectrometry Investigation and Determination of Rare Earth Ions Ho
3+
and Nd
3+
in a Solution
Yan Hongtao, Deng Yanzhuo, Zeng Yun'e
1988, 4(2): 25-30.
Abstract
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A home-made high sensitive photoacoustic transducer was used to determine the photoacoustic signal in a solution. The photoacoustic spectra of Ho
3+
in different solvents were measured and comparedwith its absorption spectrum. The affection factors of photoacousticsensitivity are discussed. The trivalent rare earth ions Ho
3+
and Nd
3+
in an aqueous acetonitrile solution were determined. The detection limit is 5×10
-8
mol/L for Ho
3+
and 1.0 ×10
-7
mol/L for Nd
3+
, and corresponds to the absorbance of 1.5×10
-7
and 6.3×10
-7
,respectively.
Studies on the Automated Determination of Total Rare Earths in Al-Re Alloys by Automated Flow Injection Device with DBC-CPA Reagent
Chen Danhua, Cai Ruxiu, Zeng Yun'e
1988, 4(2): 31-38.
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)
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The automatic determination of the total rare earths in the aluminium-rare earth alloys was studied by using our recently designed automated flow injection device and the high sensitive and selective rare earth reagent-DBC-CPA (2 -(2-phosphono-4-chlorophen-ylazo)-7-(2,,6-dibromo-4-chlorophenylazo)-1,8-dihydroxy-3, 6 - dis-ulfonaphthalene). The automated flow injection device consists of an Apple Ⅱ microcomputer, two peristaltic pumps and a spectrophoto-meter. It has good automatic degree and high producibility, the sampling volume and rotation velocity of the pumps can be changed continuously and automatically. The total rare earths in aluminium-rare earth alloys were automatically determined at 645nm wavelength in the medium of 1.Omol/L HC1 and 1% H
2
C
2
O
4
. Fe Cu, Al, Mg, Ni, Zn and Cr don't interfere with the determination and temperature has no effect on the sensitivity in the range of 10～49℃ above zero. The calibration curves for cerium group and yttrium group rare earths are close to each other. The relative standard deviation of repetitive detection of 7 times for various types of aluminium-rare earth alloys is in 1% or so with a sampling frequency of 200 samples per hour. The results correspond to that of the manual spectrophotometric method well. This simple, rapid and exact method is best suited to the analysis in batches of the total rare earths in all aluminium-rare earth alloys.
Theory of Triangular-wave Oscillovoltametry -Single Electrode Reaction
Qi Hong, Ma Xinsheng, Gao Hong(H. Kao)
1988, 4(2): 39-44.
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The theory of single electrode reaction in triangular-wave a.c. oscillovoltametry is presented. Theoretical equation for E-t curve is derived, and transition time, incision potential and incision height are described quantitatively.some important results are expresed below:(这里有图片19880207-39-1.GIF)
Syntheses and Structures of Rare Earth Nitrate Complexes with 2.6-Diacetylpyridinebis(Semicarbazone)
Pan Xiangyang, Yan Shiping, Wang Genglin, Wang Honggen, Wang Ruji, Yao Xinkan
1988, 4(2): 45-53.
Abstract
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)
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Six rare earth nitrate complexes of 2, 6-diacetylpyridinebis (semicarbazone) (DAPSC) were synthesized and characterized by elemental analysis, IR spectra and electrical conductance. Molecular and crystal structures of complex [Sm(DAPSC)(NO
3
)
2
(EtOH)]NO
3
were determined by X-ray diffraction method. C
13
H
21
N
10
O
12
Sm crystallized in the monoclinic apace group C
2/c
with the following unit-cell constants, a=16.674(2)Å, b = 10. 715(2)Å, c = 25.242(4)Å . β = 100.077(11)°; z=8, the final R factor is 0.025. The coordination number of Sm
3+
is ten.
Studies on Chemical Ingredients of Fruit of Alpinia Galanga, (L.) Swarts(Ⅱ) -Four Esters and Their Hydrolysis
Xue Dunyuan, Sheng Fenling, Song Maosen, Chen Ning, Li Zhaolin, Chen Yaozu(Y. Z. Chen)
1988, 4(2): 54-60.
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Four esters have been isolated from a Chinese medicinal herb, fruit of Alpinia galanga(L.) Swarts, and identified as 1'-acetoxychavicol acetate(1), trans-p-acetoxycinnamyl acetate(2), 1'-acetoxyeugenol acetate(3), and trans-3'-acetoxytsoeugenol acetate(4). Among them compound 2 has not been reported in literature and compound 4 has nor been found in natural product before. Compound 1 and 3 were hydrclysed rapidly in boiling wacerinto 1'-hydroxychavicol acetate(5), tians-p-acetoxycinudmic alcnhol (6), 1'-hydroxyeugenol acetate (7) and trans-3' - hydroxyisoeueugenol acetate(8) respectively. The mechanism of these hydrolyses is discussed. The mass spectrometric fragmentations of these compounds are proposed.
Studies on the Hydrosilation of Aromatic Aldehydes
Geng Bolin, Xu Shansheng, Huang Changhua, Zhou Xiuzhong, Wang yongtai, Lin Chui
1988, 4(2): 61-66.
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The dependence of reactivity on molecular structure in hydro-silation of aromatic aldehydes catalyzed by (PPh
3
)
3
RhCl was studied by "IN SITU" FT-IR technique and a plausible mechanism was proposed.The results show that: (1) Model reaction Ⅰ, Ⅱ and Ⅲ are all characterized by an induction period; (2) The reaction constant of model reaction Ⅰ is +1.57, so the rare of reaction Ⅰ is increased by the electron-withdrawing groups; (3) The rate of model reaction Ⅲ decreases when the size of R
1
becomes larger; (4) The reaction constant of model reaction Ⅲ is -0. 50, so the rate of it is increased by electron-donating groups.
Mannich Reaction with Arylamine as Amino Component(Ⅶ)
Zhao Dong, Xu Xiujuan, Liu Yao, Chen Guangxu(K. H. Chen)
1988, 4(2): 67-71.
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2-Arylaminomethyl-1-tetralone and 2-arylaminomethyl-6 (or 7)-methyl (or me thoxy) -1 - tetralone were synthesized by the Mannich reaction which was carried out directly on the condensation product of arylamine with formaldehyde or arylamine-HC1 and 1-tetralone derivatives in ethanol-HCl solution. Twenty-five compounds were obtained in high yields.
Acidity of (CH
3
)
3
SiCl-Modified ZSM-5 Zeolite and Its Catalysis in Toluene Disproportionation Reaction
Li Jieming, Jiang Dazhen, Fan Shuguang, Sun Zhongqi
1988, 4(2): 72-80.
Abstract
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HZSM-5 zeolites modified by Si(CH
3
)
3
Cl were studied by TPD, IK and
27
Al NMR to characterize their surface properties and bycatalytic reaction of toluene disproportionation.It was found that the concentration of the stronger Bronsted acid sites were decreased and the stronger Lewis acid sites were increased after modifieation with Si(CH
3
)
3
Cl. The TPD peaks of NH
3
, presumally attributed to stronger acid sites (peak Ⅱ ) were decreased by the deposition of Si(CH
3
)
3
Cl on the surface of the zeolites.The selectivity to the para xylene can be attained not only by controlling the pore opening and channels of the zeolite, hut also by changing the concentration of the stronger acid sites and the acidic type on the surface of the zeolite.
Calculation of the Multicenter Integrals for the Two-Electron Operators
Xu Zonqrong, Wu Yuying
1988, 4(2): 81-84.
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)
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The Study of Oxygen Transfer Kinetics for MoO
2
(S
2
CENt
2
)
2
in Various Solvents
Yang Huixing, Chen Yu, He Hong
1988, 4(2): 85-90.
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)
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The reaction kinetics between MoO
2
(S
2
CNEt
2
)
2
and triphenylphos-phine (PPh
3
) were studied in various organic solvents with the aid of the stopped-flow technique. The linear correlations were found for rate constants or activation energy versus the function of refractive index (n
2
- 1)/(2n
2
+ 1). It was also found that pre-factor increases with the descent of ( n
2
- l)/(2n
2
- 1) slightly.One step mechanism which supposes the lone pair of electrons on P atom of triphenylphosphine enters directly into the Ⅱ
*
antibonding orbital, which makes the Mo= O bond broken, is suggested.
Studies on the Light Scattering Substance in Gastric Juice from the Patients
Wang Jindui, Tian Ke, Dai Jin, Ma Rongjiu, Zhang Lifang, Chen Xiaoguang, Li Tiejin, Cheng Yuhua, Liu Zhiguang, Zheng Fumin
1988, 4(2): 91-94.
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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