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中文
Table of Content
23 October 1985, Volume 6 Issue 10
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Articles
The Mechanism of Formation and Crystal Growth of Molecular Sieve Zeolite (ⅩⅢ)——The Crystallization Kinetic Model for a Spontaneous Nucleation System of the M-Si-ZSM-5-type Zeolites
Feng Shouhua, Li Shougui, Xu Ruren, Fei Pusheng
1985, 6(10): 855-860.
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Acrystallization kinetic model for a spontaneous nucleation system of the M-Si- ZSM-5-type zeolites (M = B,Al,Ga,Ti, V,Cr or Fe) has been suggested on the basis of the investigation of the hydrothermal synthesis for this type of zeolites in tic. system of Na
2
O-HMDA-M
2
O
3
-SiO
2
-H
2
Oat 150℃. The crystallization kinetic curves for the various M-Si-ZSM-5-type zeolites, obtained by calculation of the model, agree well with the experimental values.
Studies on Synthesis, Structure and Properties of the Cluster Complex [(C
4
H
9
)
4
N]
2
[Mo
2
S
6
O
2
]
Zhang Zhigui, Li Shuqin, Zhang Zeying, Shao Meicheng
1985, 6(10): 861-865.
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The crystal of the cluster complex, [(C
4
H
9
)
4
N]
2
[Mo
2
S
6
O
2
] was obtained by the reaction of (NH
4
)
2
MoS
4
, FeCl
5
and (C
4
H
9
)NBr in CH
3
OH-CH
5
ONa. The crystal structure of the cluster complex was measured by X-ray. The crystal belongs to D
2h
15
-P
cah
space group. The crystal cell parameter are a=15.876(3)Å,b=17.786(6)Å,c=31.90(1)Å,V=9008.7Å
3
. The structure was refired by leastsquares. The value of Rwas 0.0659. The properties of IR, Raman, UV-Visible spectra and electrochemistry of the cluster complex have been investigated.
Coordination of Scandium with Oxalate Ions in Aqueous Medium
Xu Shaoquan
1985, 6(10): 866-868.
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The solubilities of scandium-oxalate in solutions of various concentration of ammonium oxalate and ammonium perchlorate (the latter is to maintain a constant ionic strength of 2) were measured at 25℃. The existence of complexes ions [ScC
2
O
4
]
+
[Sc(C
2
O
4
)
2
]
-
and [Sc(C
2
O
4
)
2
]
3-
have been revealed from the treatment of experimented data by useing of qraphic extrapolation. The solubility product of scandium oxalate was also calculated to be 1.22×10
-22
(μ = 2, pH=1). The succesive stability constants of the complexes formed were calculated by two ways: relaxation method and a least-squares technique on a computer. The results are as follows: β
1
= 1.94 × 10
8
; β
2
= 5.5 × 10
15
; β
5
= 2.0 × 10
16
.
Study on the Characters of HZSM-5 Molecular Sieve Interacting with Various Liquids from Heats of Immersion
Li Yuguang, Zhong Qiumei, Zeng Zhaohuai
1985, 6(10): 869-871.
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Heat of immersion of zeolite HZSM-5 outgassed at high temperatures and in vacuum have been determined in various organic liquids. The value in terms of kilojoules per avogadro No. of unit cells, Quc, is quite different in each liquid being studied. The order of Quc was found to be n-hexane>n-heptane>n-decane> n-dodecane; benzene < toluene <p-xylene;p-xylene>xylene>xylcnc; methanol< cthanol; and the smallest in cyclohexanc.
Studies on Boron Compounds (ⅩⅥ)——The Syntheses of π-Cyclopentadinyl-Bis(Triphenylphosphine)- Nickel(Ⅱ) Hydroborates
Zhang Lun, Huang Yuyuan, Chen Xinlan, He Jianshe
1985, 6(10): 872-874.
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Seven π-cycllpentadinyl-bis (triphenylphosphine)- nickel( Ⅱ) hydroborates were synthesised by the reaction between hydroborate ions (B
12
H
12
2-
,B
10
H
10
2-
,B
11
H
14
-
, B
3
N
8
-
, B
10
Cl
10
2-
, B
10
H
2
Br
8
2-
, B
10
H
4
I
6
2-
) and π-C
5
H
5
NiPPh
3
Cl in the presence of PPh
3
. These compounds were characterized by elemental analysis, IR, and molecular conductivity.The thermal stability of these complexes was examined by DTAmethod.
Studies on the Dissociation of Ghlorophosphonazo-mA [2-(4-Ghloro-2-Phosphonobenzenenazo)-7-(3- Acetylbenzenenazo)-1,8-Dihydroxynaphthalene-3,6- Disulfonic Acid
Zhao Hoag, Zhu Chuanzheng, Zhou Weiliang, Pan Jiaomai
1985, 6(10): 875-880.
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The purification of chlorophosphonazo-mAwas reported. The dissociation of chlorophosphonazo-mAin aqueous solution was studied by spectrophtometric and potentiometric titration methods. The values of dissociation constants, pK
1
=0.38, pK
2
=1.12, pK
3
= 2.74, pK
4
= 6.79, pK
5
= 9.73, pK
6
= 11.46, were determined by spectrophotomeric method at identical temperature and ionic strength (20℃, μ = 0.4). Under identical conditions the results, pK
3
= 3.11, pK
4
= 6.83, pK
5
= 9.75, pK
6
= 11.52, obtained by using the potentio metric tritration method agreed well with those obtained by the spectrophoto metric method.The dissociation constants were measured by the potentio metric titration method at various temperatures. The thermodynamic parameters, ΔG°,ΔH° and ΔS°, for the dissociation process were calculated.The difference between the dissociation constants of chlorophosphonazo-mAand chlorophosphonazo-pNwas satisfactorily interpreted by the difference in the values of net atomic charge density distribution obtained with quantum chemistry calculations.
Spectrophotometric Study of Heteronuclear Complex of Lanthanum and Copper with Alizarine Fluorine Blue
He Xiwen, Li Hong, Shi Huiming
1985, 6(10): 881-886.
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Astudy on the interaction of Lanthanum and Copper with Alizarine Fluorine Blue has been made. It has been found that La and Cu react with the reagent in a molar ratio of 1:3:3. This ratio was obtained by the improved slope ratio method and modified limited logarithm method. The Forming mechanism of the heteronuclear complex was preseantd.At pH4.0 a red-violet form with maximum absorption at 550 nm is prevalent conditions for the formation of the colour complex were considered. The heteronuclear complex seems to be a more sensitive and accurate system for the determination of copper than the single and isopolynuclear ones.
The Application of Ghromous Solution to Chemical Analysis——The Monitoring of Mercury in Environmental Waters with Continous Liquid Flow Analysis System
Tian Liqing, Masashi Goto, Daido Ishii
1985, 6(10): 887-890.
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The successful application of chromous solution in chemical analysis is still limited. Here we studied how to use it as a reducing agent for reducing mercury with continous liquid flow analysis system and without the disadvantage of forming metastannic precipitation. Hence it can be used for determining and continous monitoring of mercury in environmental waters. The linear relationship between the absorbance and the concentration of total mercury is covered 0.5-6.0 ppb.The detection limit is about 0.1 ppb. The amounts of reagents required and the waste solution expelled each day are small.
The Analytical Application of Water Insoluble Porphine (Ⅱ)——Spectrophotometric Study of the Reaction between Cadmium and α,β,γ,δ-Tetra-(4-Chlorophenyl) porphine
He Shuqiong, Huang Zexing, Chen Ming, He Yuhang
1985, 6(10): 891-893.
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In this paper, the complex formation reaction of α,β,γ,δ-tetra-(4-chlor-ophenyl) porphine CT(4-Cl)PPDwith Cadmium in the presence of mixture surfactant, sodium dodecyl benzene sulfonate and tritonX-100 was studied, and a new highly sensitive method for spectrophotometric determination of micro amounts of cadmium has been developed, utilizing the soret band of the cadmium-T( 4-Cl)PPcomplex. Apparent molar absorption coefficient is 4.1 × 10
5
.
Dual-wavelength Spectrophotometric Determination of a Microamount of Silver with 1,10-Phenantholine and Phloxine B
Zhang Youxian, He Runxi, Hu Yongling
1985, 6(10): 894-896.
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In the solution of Na
2
HPO
4
-NaH
2
PO
4
at pH 5.7 and the presence of gelatin a soluble red-violet ternary complex of silver with 1,10-phenanthroliee and phlox ine Bcan be formed. On the basis of this fact we directly determined silver in aqueous solution with dual-wavelength at λ
R
542nm and λ
s
571nm. Beer's law is obeyed in the range of 0-42.7μg/25ml and Ae is 5.76×10
4
. After separation with ion exchange this method was applied to determine a microamount of silver in anode mud and etc.
Studies on the Ortho Effects in Quantitative Structure Herbicidal Activity Relationship of O-Ethyl O-Aryl N-Isopropylphosphoramidothioates
Chen Ruyu, Yang Huazheng, Xing Xiaodong, Zhang Zhenpu, Wang Lingxiu, Cheng Muru, Li Fuxin, Wang Huilin, Cao Ruzhen
1985, 6(10): 897-902.
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Using π,Σσ F, Verloop's STERIMOLparameters and an indicator variable for hydrogen-bonding possibility by ortho-substituents, the quantitative correlation of structure-herbicidal activity of 39 O-ethyl O-aryl N-iso-propylphosphoramidothioates was studied and the contributions of the herbicidal activities by ortho-substituentswere discussed.
The Syntheses of Derivatives of Nucleoside 3',5' -Cyclic Phosphate
Zhang Lihe, Ma Lintai, Xu Chen, Dong Lingjiao, Wang Qi, Wang Xu
1985, 6(10): 903-909.
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By using tosyl chloride or triphenyl phosphine/carbon tetrachloride as condensing reagents, 2'-tosyl c-AMPreacted with ROHor RNH
2
to give nucleoside 3',5'-cyclic phosphotri-esters and phosphoramidates in 30-60% yield. Detosylation was carried out by using sodium naphthaline at -60℃+ in DMEin 70-90% yield. The stereoisomers of these compounds have been separated and the structures have been identified by
1
H NMR,
13
C NMR,
31
P NMRand FDMS.
Study on Transition-Metal Organic Compounds Containing Perhaloaryl Ligands(Ⅶ)——Synthesis and Reactions of Pentabromophenylnickel Complexes with Diphenylalkylphosphine
Zhang Zhengzhi, Wang Hsukun
1985, 6(10): 910-912.
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The complexes of general formula (ph
2
PR)
2
Ni(C
6
Br
5
)Br(R=CH
3
,C
2
H
5
, n-C
3
H
7
,ph) were synthesized. Their chemical reactions with inorganic halides and pseudohalides were investigated and compared With corresponding C
6
Cl
5
containing complexes.
A Convenient Synthesis of Phenyl Ethers Using Supported Reagents
Wang Jinxian, Han Jinding
1985, 6(10): 913-916.
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This study relates to the preparation of phenyl ethers by the reaction of phenols with organic halidcs using a supported reagents as the condensing agent. We have found that sodium hydroxide on alumina when used in the condensation reaction gives significantly higher yields of phenyl ethers than the ordinary reagents used.
Synthesis and Properties of 1-Aryl-3-Benzoyl-2,5- Diphenyl Pyrrole
Li Bao, Zhang Zhenli
1985, 6(10): 917-918.
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Dibenzoylmcthanc was treated with ω-bromoacetophenone to give 1,4-diphenyl -2-benzoyl-1,4-butandionc(1). Eight new 1-aryl-2,5-diphenyl-3-benzoyl pyrroles (2)-(9) were obtained by reactions of (1) with various primary aromatic amines. Semicarbazoncs (10)-(17) were prepared form (2)-(9). Compounds from (1)-(17) were reported for the first time.
The Calculation of Liquid Activity Coefficient and Vapor Liquid Equilibrium Data from Excess Volume Data
Zhang Bingjian, Han Shijun
1985, 6(10): 919-924.
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Anew model (EVLACmodel) which can directly predict liquid activity coefficient from excess volume data are established by means of statistical thermodynamics. Anew partition function equation is developed and then V
E
-x equation and γ-x equation can be derived mainly from the concepts of two liquid cell and local compositions. If V
E
-x data at only one temperature are available, the isothermal γ-x data and VLE. data at different temperatures and the isobaric VLE. data at different pressures can be calculated. This method can be extended to multi-component systems without increasing any multi-component parameters.About eighty sets isothermal activity coefficients of twenty five binary systems and fifteen sets isobaric activity coefficients and VLE. data are predicted by means of this new method. Good agreements between experimental data and predicted values are obtained.
Research on the Molecular Orbital Graph Contraction Theorem
He Wenchen
1985, 6(10): 925-929.
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This paper is aimed to make the contraction theorem, which was developed by Tang Auchin, more generalized and to widen its applicable range.
The Map Analysis of Bonding orbital Wave Function of Fe-Mo-S Cluster the Analogue of the Nitrogenase Fe-Mo-Cofactor
Guo Chunxiao, Shen Erzhong
1985, 6(10): 930-934.
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In this paper, using the program JDPLOTfor drawing wave function, which is made by ourself,we have drawn the isovalue maps and electronic density contour maps of bonding orbital wave function of four element ring FeS
2
,Mo of Fe-Mo-Scluster (the analogue of the nitrogenase) and analyzed the property of the bonding orbitals between Fe and Mo atoms. The existence of comparatively strong metal-metal bond between Fe and Mo atoms was further verified.
Kinetics of Oxidative Dehydrogenation of Butene-1 to Butadiene over Fe-Zn-Mg Catalyst
Jin Yun, Yu Qiquan, Xu Xiaoqin
1985, 6(10): 935-940.
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The kinetics of oxidative clehydrogenation of butene-1 to butadiene over Fe4.9 Zn
0.9
Mg
0.9
(atomic ratio) catalyst has been investigated in a flow-reeirculation glass reactor. The Kinetics of oxidative dehydrogcnation of butene-1 to butadiene and deep oxidation of butene-1 and butadiene to CO
2
is described by the equations of Longmuir Hinshelwood mechanism of strong adsorption of bimolecular reaction. The kinetic parameters of rate equations were estimated by non-linear least square.The rate equation for formation of butadiene is
A Study on Pyridoxinc-Selective Electrode
Shen Guoli, Han Mei, Liu Hong, Yu Ruqin
1985, 6(10): 941-944.
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Using pyridoxine-tetraphenylboratc or pyridoxine-dipicrylamine ion-pair cpmplexes as active materials, PVCmembrane pyridoxine ion selective electrodes were prepared. The effects of various factors on the performances of electrodes were studied and the optimum condition of membrane preparation was found. The use of p-yridoine-dipicrylamine as active material and dibutylphthalate as solvent medium gives best electrode characteristics. This electrode shows Nernstian range from 1.0×10
-1
Mto 1.0×10
-5
M, with a slope of 61 mV/decade. The stability and reprdducibility ofthe electrode were tested and the pyridoxine samplcs were analyzed by diractpotcntiometry and potentiometric titration procedures. The pKvalue of pyridoxinewas determined potentio-metrically by using the proposed pyridoxine electrode.
Kinetics of Butadiene Polymerization with Molybdenum (IV) Catalyst System
Xia Shaowu, Wang Changmin, Xu Ling, Tang Xueming
1985, 6(10): 945-949.
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Kinetics on the polymerization of butadiene with MoCl
2
(n-C
8
H
17
O)
2
- (i-Bu)
2
AlOph as catalyst has been studied. The result shows that the polymerization is a first order reaction for both Mo(Ⅳ) catalyst arid monomer. The apparent activation energy for the polymerization is 18.5 Kcal mol
-1
and the preexponential factor 1.6 × 10
10
min
-1
. Some of the kinetic parameters, such as the efficiency of catalyst (α), the concentration of active center (P), and the meen lifetime of living polymer chain (τ) in different temperatures have been determined. This has proved that the time of equal rate polymerization (τ
0
) is approximately equal to the lifetime of living polymer chain (τ).
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