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中文
Table of Content
24 April 1987, Volume 8 Issue 4
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Articles
Studies on the Kinetics of Solvent Extraction Process
Gai Huifa, Gao Zili, Sun Sixiu, Zheng Liliang, Shen Jinglan
1987, 8(4): 291-296.
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The extraction kinetics and mechanism of palladium (Ⅱ) from chloride medium with trioctylamine (TOA) were studied by means of PVC-membrane Pd(Ⅱ) ion selective electrode and stationary interface stirring cell. The experimental results showed that the extraction process is controlled by the following reactions,(这里有图片198704-296-1.gif)where (i) and (o) represent the interface and the organic phase, respectively. The values of k
1
, k
-2
and k
2
/k
-1
were calculated by computer. The influences of the temperature, acidity and added substance (n-octoh) in the organic phase on extraction rate are also discussed.
The Molecular and Crystalline Structure of Barium 18-Crown-6 with Cobalt(Ⅱ) Thiocyanates
Fan Yuepeng, Zhang Wenxing, Wang Xiuwen
1987, 8(4): 297-300.
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This Paper reports on the coordination compound grown in a gel reaction of 18-crown-6 with cobalt(Ⅱ) chloride and barium thiocyanates. The crystal contains water molecules with the chemical formula of [Ba(C
12
H
24
O
6
)(H
2
O)
2
]·[Co(NCS)
4
]. Its composition was determined by elemental analysis and X-ray spectrum. Adark blue crystal of dimensions 0.2-0.7 mm was selected.The intensity data were collected on a Enraf-Noius CAD-4 four-circle diff-ractometer by using MoK
α
radialion(=0.71069A). There were 5553 independent reflections and 4254 visible intensity data were obtained. The structure was solved by Patterson method and Fourier method and refined by block-least square method,R= 0.029, R
w
= 0.031. The crystal belongs to the rhomb system and the space group is D
2h
16
-P
nma
with crystal parameters α=12.136(3)Å, b=14.586 (3)Å, c=16.475(4)Å, α= β=γ= 90, V= 2916.19Å
3
and Z=4. The calculated density of the crystal is D
c
= 1.619g/cm
3
and the linear absorption coefficient is = 22.2cm
-1
(MoK
α
).
Studies on the Solubility and the Isothermal Evaporation Process in the Quinary System Li, Na, K, Mg/Cl-H
2
O at 25℃
Zhang Fengxing, Guo Zhizhen, Chen Peiheng, Ma Jinhua, Chen Yunsheng
1987, 8(4): 301-305.
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The phase diagram of the title quinary system at 25℃ has been constructed for the first time. There are five crystallization surfaces corresponding to the eutectic solutions saturated with NaCl and KCl, LiCl·H
2
O, MgCl
2
·6H
2
O, Li-Carnallite and K-Carnallite respectively;the monovariant lines. P
3
T
1
(corresponding to NaCl+ KCl+ K-Carnallite), E
5
T
1
(NaCl+ KCl+LiCl·H
2
O ), E
4
P(NaCl+K-Carnallite+MgCl
2
·6H
2
O), PT
2
( NaCl+K-Carnallite+ Li-Carnallite), T
1
T
2
( NaCl+K-Carnallite+LiCl·H
2
O), P
2
P( NaCl+MgCl
2
·6H
2
O+Li-Carna-llite), E
3
T
2
(NaCl+Li-Carnallitc+LiCl·H
2
O), E
1
T
1
( KCl+LiCl·H
2
O+K-Car-nallitc), E
2
T
2
(LiCl·H
2
O+Li-Carnallite+ K-Carnallite), P
1
P( MgCl
2
·6H
2
O+ Li-Carnallite+K-Carnallite), respcctivoly; and three quinary invariant points: T
1
, T
2
, Pcorresponding to the solutions saturated with LiCl·H
2
O+NaCl+KCl+ K-Carnallitc, LiCl·H
2
O+NaCl+Li-Carnallite+ K-Carnallite and Nacl+ MgCl
2
·6H
2
O+Li-Carnallite+ K-Carnallite.The results of studying the isothermal evaporation of mixtures showed that there was not any metastable solid phase occurring in the system and the supersaturation phenomena were unconsidcred.
Studies on Stabilities of Some Lead(Ⅱ) Mixed Ligand Complexes Containing Oxygen and Nitrogen as the Coordination Atom(Ⅱ)
Zhang Feng, Liu Qitao
1987, 8(4): 306-308.
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The stability constants of 1:1:1 mixed ligang complexes of Pb(Ⅱ) with 2,2' -dipyridyl(dipy) or 1,10-phcnanthrolinc(phcn) as the first ligand,and malo-natc (mal) as the second ligand were determined at 25±0.1℃ with ionic strength 0.10 (maintained by KNO
2
) by using potcntiometric method. The △logK and logX of these mixed ligand complexes and their statistical expected values were calculated. The results showed that the above mixed ligand complexes have an enhanced stability.The reasons that lead to this results are discussed.
Investigation on the Optimization of Gradient Loaded Column to Analytic Time in Gas Chromatography
Yun Xiqin, Kou Dengmin, Long Yicheng, Men Yi, Yu Zhongjian
1987, 8(4): 309-313.
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Equations were derived and the optimum programs for gradient loaded column were presented. Theoretical and practical problems concerned with the optimization of gradient loaded column are discussed so as to demonstrate the effects of optimum programming on retention time and column efficiency.
Application of Arc Sampling Combined with Inductively Coupled Plasma Atomic Emission Spectrometry to the Determination of Trace Elements in Alloy Steels
Jiang Zucheng, Fassel V. A.
1987, 8(4): 314-318.
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A sensitive method for the determination of trace elements in alloy steels by using arc sampling combined with ICP-AES has been developed. The d.c. arc discharge as a vaporization device is used to produce metal vapour from sample surface, and then the vapour is introduced to ICP by carrier gas Ar. The behaviour of sample vaporization, the effect of discharge gas and matrix, and TCPexcitation parameters were investigated. The detection limits are in the range of 0.x to x μg/g. The method has been applied to the analysis of some low-alloy and high-alloy steels, and the results obtained are in good agreement with the values of NBS.
The Computer Analysis of the Linear and Non-Linear Gas Packed-Column Chromatography
Lin Bingchang, Wang Jida, Lin Bingcheng
1987, 8(4): 319-321.
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The well-posed problem of the gas packed-column chromatography, and the relation between the form of the elution curve and partition coefficients in different feed time is discussed. The results are in agreement with the perturbation analysis.
The Determination of Chromium(Ⅵ) in the High Acidic Medium by Mono- and Dual- Wavelength Spectrophotometry
Wang Zhenqing, Xu Guanghui, Shen Hanxi
1987, 8(4): 322-324.
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A simple and rapid spectrophotometric method for the determination of chromium (Ⅵ) with 9-orthochloropheny1-2,3,7-trihydroxyfluorone (o-Cl-pF) has been investigated. This method is based on the formation of a complex in the hydrochloric and phosphoric acid medium (0.4N HCl+3N H
3
PO
4
).The complex has an absorption maximum at 497nm. The value of molar absorption cofficient is 2.33×10
4
at λ
515nm
. Beer' s law is obeyed over the range 0-30μg/25ml of Cr.The two wavelengths for the determination of 0-10μg/25ml of Cr by using dual-wavelength method are 462 and 497nm. By using the proposed method, the Cr contents in alloy and metallic materials were determined with satisfactory results.
The Studies of 1,4-Bis(2-Phenyl-1,3,4-Oxadiazol-5-yl) Benzene and Its Derivatives (Ⅰ)
Chen Jingshan, Pan Jiaxing, Gao Zhenheng
1987, 8(4): 325-330.
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1,4-Bis(2-Phenyl-1,3,4-Oxadiazol-5-yl ) benzene and nineteen of its derivatives are prepared. The relationships between the constitution of these compounds and their UV, FLas well as IRspectra are discussed respectively. The laser conversion efficiency are taken.
Studies on Flavonoids (Ⅱ)--Synthesis of 2,8-Substituted-Aryl-Benzo-(1,2-b:5,4-b' )Dipyran-4,6-Dione
Lu Yixian, Mao Shuren, Li Gengxin, Cai Mengshen
1987, 8(4): 331-335.
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In this paper, synthesis of the diflavones(Ⅲ
a-e
) from dichalcones(Ⅱ
a-e
) in one step using I
2
-DMSO-H
2
SO
4
system was reported. The dichalcones were first heated at 100℃ for about 10 min. With DMSO and a small amount of H
2
SO
4
, then a catalytic amount of iodine was added and the reaction mixture was further heated to give 72-100% yields of diflavones.The reaction intermediates Ⅳ
a
, and Ⅳ
b
were isolated by column chromato-graphy and reaction mechanism was discussed.
Asymmetric Induction Under Two-Phase Conditions (Ⅰ)--Asymmetric Induction in the Gabriel Reaction by Means of Two-Phase System-Synthesis of Optically Active Amino Acids
Vu Lingchong, Wang Fei
1987, 8(4): 336-340.
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Reaction of potassium phthalimide and ethyl α-bromocarboxylates under solid-liquid phase-transfer conditions, using chiral ammonium quaternary salts as phase transfer catalyst, affords twelve optically active 2-phthalimido-esters. The N-substituted phthalimide by hydrazinolysis, the resulting esters of amino acids can readily be hydrolyzed to the corresponding optically active amino acids with optical yield 3.6-17.8%.
A New Method for the Synthesis of β-Lactam Compounds from β-Amino Acids
Huang Huamin, Wu Shengli
1987, 8(4): 341-343.
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Various β-lactams arc prepared in good yields under mild reaction conditions from the corresponding β-amino acids by the use of cyanuric chloride and dimethylformamidc as a condensing reagent.
Study on Synthesis of 3-Methoxymethylenetetrahydrothiophene and Its Reactivity
Li Yuchang, Rewicki, D.
1987, 8(4): 344-346.
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A new compound 3-methoxymethylenetetrahydrothiophene (Ⅰ) has been prepared and the reactivity of the α-H of (Ⅰ) was studied. Anew possibility is given for the synthesis of aromatic substance "Kahweo-furan"(Ⅱ).
Study of the Esterification Reaction of Acetic Acid by Alcohol on HZSM-5 Zeolite
Zhang Huaibin, Gao Feng, Zhong Pucha, Li Hexuan
1987, 8(4): 347-350.
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It is reported the esterification reaction of acetic acid with alcohol on HZSM -5 zeolite. With a series of HNaZSM-5 zeolite catalysts, the effect of the degree of cation exchange on the activities and the selectivities of the catalysts were discussed. The effect of calcination temperature of HZSM-5 zeolite on the activity and the selectivity was investigated. The surface acidity of HZSM-5 zeolite was determined by JR-spectroscopic method. It Was found that the esterification reaction can take place both at the Bronsted acid sites and the Lewis acid sites, while ether was produced mainly at strong Bronsted acid sites. Since the activity of the catalyst was not reduced remarkably by 4-mcthylquinoline, the esterification must mainly occured on the internal surface of zeolite.
Electrochemical Studies on Europium Nitrate Complexes with Cryptands
Liu Shichang, Zhu Tianpei
1987, 8(4): 351-354.
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Electrochemical reduction of europium cryptatcs Eu(NO
3
)
3
(2,2) and Eu2(NO
3
)
6
(2,2,2) were investigated by means of cyclic voltametry in dichloro-methane, dichloroethane, acetonitrile, acetone, benzonitrile, pyridine, dimcthyl-formamidc and dimethyl sulioxide, The halfwave potentials of redox reaction and electron-transfer rate constants were determined, and the effects of solvent and supporting electrolyte on E
1/2
and k
s
were discussed.
The Strong Field Scheme of Point Group C
2h
for System d
5
and the Absorption Spectrum of MnCl
2
·H
2
O
Zhao Shangbo, Wang Huisu
1987, 8(4): 355-358.
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A simple and convenient strong field scheme for treating the absorption spectra of the complex ions with lower symmetry groups is suggested. The complete energy matrices of terms corresponding to the irreducible representations of C
2h
point group for d
5
system are derived.The complicated electronic absorption spectrum of Mn
2+
in MnCl
2
·2H
2
O is analyzed and explained by means of these matrices and by considering the vibronic coupling and double electron excitation.
BF
3
-H
3
PO
4
/ZrO
2
Catalyst for Isobutane-Butene Alkylation
Wen Lingsheng, Li Yi, Peng Yin, Cui Shengfan, Sun Zhongqi, Zhou Lehui, Qian Zaihu
1987, 8(4): 359-360.
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In this paper, isobutane-butene alkylation has been studied by using BF
3
-H
3
PO
4
/ZrO
2
as a catalyst. It was found that the catalyst 404 showed high activity, selectivity and stability at 100℃, 1 atm. and with an isoparaffin to olefin ratio of 6.5:1.
A Study of Intelligent Evaluation for Dissociation Constants of Unknown Polybasic Acid
Xu Xiaoma, You Daheng
1987, 8(4): 361-365.
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A new mathematical model is described for deforming dissociation constants of unknown polybasic acids. The polybasic acids are titrated by caustic alkali potentiomctrically. The calculation is carried out by employing Gordon' s mathematical model and simplex optimization method, with a new computer programme "GORDANACID".
The Pattern Calculating Method for Mixed Acids (Poly Acids) Analysis
Cai Huamin, Yu Daheng
1987, 8(4): 366-368.
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The pattern calculating method for mixed acids (poly acids) is presented. It is to use a patlcrn for finding out dissociation constant pk
A
i
and the number of acids in one sample. This method is more reliable and simple, by which a set of artificial mixed acids was determined.
Studies on Bismuth (Ⅲ) Halogeno-Complex Ion-Selective Electrodes
Qi Hongtao, Kuang Shumin
1987, 8(4): 369-371.
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Three new PVC matrix membrane bismuth (Ⅲ) ion-selective electrodes based on triheptyldodecyl-ammonium and iodo-complex, bromo-complex, chloro-complex of bismuth (Ⅲ) ion pair were described. The electrodes show Nernstian ranges from 10
-2
Mto 3×10
-6
M Bi
3+
(in 0.15 M KIsolution), from 5×10
-3
M to 4×10
-6
M Bi
3+
(in 0.40 M KBr solution), and from 10
-2
Mto 4×10
-5
M Bi
2+
(in 1.5 M NaCl solution) with the slopes of 60, 40, 38 mV/pBi, respectively. The potential selectivity coefficients and other characteristics of the electrodes were reported. The selective conditions of the ligand of complex anion and the law of interference of foreign cations were discussed.
New Synthesis of Fluorinated Organosilicon Compounds
Du Zuodong, Chen Jianhua, Zhang Chengzhi
1987, 8(4): 372-376.
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CuCl/HOC
2
H
4
NH
2
catalystic system is used for catalysis of the addition of 1, 2-dibromotetrafluoroethane to organosilicon compounds containing vinyl group. Aseries of unreported organosilicon compounds containing fluorine have been synthesized. The structures of the compounds synthesized have been determinated by elemental analysis and spectroscopic methods (
1
HNMR and IR). Factors of affection on the reaction are investigated.
Photocrosslinking Reaction of 3,4-Polyisoprene in the Presence of Sensitizers
Huang Junlian, Yu Tongyin
1987, 8(4): 377-382.
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This paper studied the benzophenone-sensitized photocrosslinking reaction of 3,4-polyisoprene. It was found that when benzophenone-sensitized 3,4-polyisoprene was irradiated by 80 Whigh pressure mercury lamp, the photocrosslinking reaction could take place. The gel fraction and crosslinking density were dependent on the irradiation time, the amount of benzophenone used and molecular weight of 3,4-polyisoprene.By means of FTIR and C
13
NMR, it was confirmed that in the presence of benzophenone the photocrosslinking reaction of 3,4-polyisoprene is essentially 2+2 addition.
Interaction Between Polyacrylamide and Sodium Dodecyl Sulfate--The Effect in Solubilizing to Dimethylaminoazobenzene
Zeng Lirong, Zhang Yujun, Wang Guoting
1987, 8(4): 383-385.
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The interaction between polyacrylamide (PAM) and sodium dodecyl sulfate (SDS) has been studied in terms of the solubilization of dimethylaminoazobenzene (DMAB). The solubilizing power of SDS becomes greater with the addition of PAM, the extent depending on the molecular weight. The amount of solubilized DMAB increases with the raising temperture. On adding NaCl in SDS solution, the solubilization ability increases, but in SDS-PAM solution, decreases. Thus it is deduced that DMAB taking neutral form solubilizes in the core of micelle in SDS solution and taking acidic form solubilizes on the palisade of micelle in SDS-PAM solution.
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