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中文
Table of Content
24 August 1985, Volume 6 Issue 8
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Preface
Study on Boron Compounds (ⅩⅣ)——Synthesis and Properties of Boron-Containing Bis(π-Arene) Iron (Ⅱ) Compounds
Zhang Lun, Fang Xinqin, Zhang Guomin
1985, 6(8): 663-668.
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Thirteen bis(π-arene) iron (Ⅱ) compounds of [Ar
2
Fe]B
12
H
12
and [Ar
2
Fe] (PF
6
)
2
were synthesized, and these compounds have all been identified by elemental analysis and IRspectra, and some of them by MSand
1
H NMR.The thermal behavior of these compounds has been investigated by DTA-TGmethod and IRspectroscopy, and their thermal stability is described.
Complexes of Grown Ether with the Rare Earth Nitrates (Ⅶ)——Studies on Solubilities of the Ternary System Pr(NO
3
)
3
·4H
2
O-18C6-CH
5
COCH
3
at 18℃
Jiang Haiying, He Mingan, Li Chenlin, Ren Dehou, Ren Bo, Wan Youjia
1985, 6(8): 669-673.
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The solubilities of the Pr(NO
3
)
3
·4H
2
O-18C6-CH
3
COCH
3
ternary system at 18℃ have been determined by the scmimicro method. The results indicate that there is only one complex Pr(NO
3
)
3
·18C6·4H
2
Oformed,The different methods have been used to examine the behavior of water in the titled complex. The results indicate the posibility to obtaine a complex species Pr(NO
3
)
3
·18C6·2H
2
O, but our attempts met with the defeat.The stable species of the complex is Pr(NO
3
)
3
·18C6The thermal decomposition products and mechanism of this complex have been studied too.
Studies on White Powdery Tungstic Acid (Ⅴ)——Direct Preparation of 12-Tungstophosphoric Acid from White Powdery Tungstic Acid and Its Purification through n-Butyl Ether Extraction
Gu Yidong, Cui MeiFang
1985, 6(8): 674-676.
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The white powdery tungstic acid prepared according to previous reports
[1,2]
reacts directly with phosphoric acid solution to form a solution of 12-tungstophos-phoric acid with some other polytungstates.For purification, the solution was extracted with n-butyl ether under suitable addition of hydrochloric acid, so as to produce an oily layer which is not miscible with water and excessive n-butyl ether. The n-butyl ether layer was then stripped with water to obtain pure aqueous solution of 12-tungstophosphoric acid. On evaporation by heating, 12-tungstophosphoric acid gradually separated out as pure crystals.
Development of Double-Barrelled Calcium Ion-Selective Microelectrode
Zhuang Yunlong, Zhou Jianping, Qi Deyao
1985, 6(8): 677-680.
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Anew PVCmatrix membrane double-barrelled calcium ion-selective microelec-trodc based on liquid ion exchanger has been designed and constructed. The tip diameter of about 2.5μm as well as lower selectivity coefficients for K
+
, Na
+
and Mg
2+
are adequate for intracellular measurements of Ca
2+
activities.The inner wall of the selective channel was made by hydrophobic treatment with alcohols. By means of this microelectrode some physiological phenomena related to Ca
2+
activities have been studied, and Ca
2+
concentrations in clinical microsamples have also been determined.
Determination of Trace Organic Chlorine Compounds in Biological Samples by Acid Digestion-Open Tubular Glass Capillary Column GC
Wang Fendi, Cai Qingzhou, Zhang Guanshi, Wang Deling, Zhang Yihua, Jin Qinhan(Q. Jin)
1985, 6(8): 681-685.
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Anovel procedure using Na
2
SO
4
homogenization,HAc-HClO
4
digestion followed by concentrated sulfuric acid and florisil column cleaning for pretreatment of biological samples in determination of trace organic chlorine compouds was developed. In combination with an open tubular glass capillary column gas chromatography it can be used to determine various organic chlorine compounds in biological samples rapidly, sensitively and accurately with detection limits in the range of sub-ppt to ppb and recoveries over 80%.
The Spectrophotometric Study on TAM with Fe(Ⅱ) and Its Application
Feng Jianzhang, Zhang Baoxin
1985, 6(8): 686-688.
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The properties of 2-(2'-thia2olylazo)-5-dimethyIamino phenol(TAM) and its complex formation reaction with iron were studied. Asimple, sensitive and selective spectrophotometric method for the determination of the micro amounts of iron has been developed. The method has been applied successfully to the determination of iron in the biological and environmental samples,and excellent results were obtained.
Direct Determination of Trace Amount of Iron in the Phosphate by the Polaried Zeeman A. A. S.
He Jinlan, Tang Yurong
1985, 6(8): 689-690.
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In this paper, the determination of the trace amount of iron in the phosphate by AASwith graphite furnace atomizer is discussed. It was found that the interference of PO
4
-3
and some metal for iron can be suppressed by the use of the higher charring temperature (1300℃) and Zeeman effect.After the sample is dissolved, it can be measured directly, without using any way of separation.
A Study on the Adsorption Voltammetry of Europium-Xylenol orange System
Wang Lizeng, Jin Wenrui, Chen Rongli, Feng Changdong
1985, 6(8): 691-692.
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Anew high-performance trace analytical procedure with the voltammctric determination of Eu is described. The voltammetric method simply consists in the application of differental pulse voltammetry after prior intefacial accumulation by an adsorption layer of the complex Eu(Ⅲ)-XOat HMDE. In aqueous media the determination limit is 5 × 10
-10
M Eu and the linear range is 5 × 10
-9
——1 × 10
-6
M.
Determination of Ternary Mixtures of Acids by Potentiometric Titration——Linear Plot Method
Ni Yongnian
1985, 6(8): 693-695.
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Linear plot method for determination of component equivalence volumes of ternary mixtures of acids is presented. Linear titration cqualions arc derived. The experiments are carried out by potentiometric titration technique and performed by stcpwisc additions of equal volumes of titrants. Several examples of determinationof mixtures of acids by using this method are given and the results are satisfactory.
A Spectrophotometric Study of Copper(Ⅰ)-5-(3,5-Dibromo-2-Pyridylazo)-2,4-Diaminotoluene-Anion Sulfactant System and Its Applications
Pan Zuting, Xie Nensyong, Xu Mianyi, Liu Guoyuan
1985, 6(8): 696-698.
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Asensitive, practical colour reaction of copper(Ⅰ)-5-(3,5-dibromo-2-pyridy-lazo)-2,4-diaminotolucne-sodium lauryl sulfatc sulfactanls has been investigated spe-ctrophotomctri cally. The complex of copper (Ⅰ) was formed at about pH3.0 The apparent molar absorptivity was 8.26×10
4
at 492 nm.
Studies on Organoactinide Compounds (Ⅲ)——The New Preparation of Biuranocenylene and Its VT
1
H NMR
Wang Hsukun, Streitwieser, A. Jr., Solar, J. P., Lyttle, M. H.
1985, 6(8): 699-702.
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Biuranocenylene was prepared from the corresponding tetraanion of 1,1'-dicyclooctatetraenyluranocene. The VT
1
H NMRof biuranocenylene showed the two uranoccne moieties were twisted to each other.
A Quantum Chemical Study of the C
6
H
6
-NO
2
+ System(Ⅲ)——The Analysis of Intermediates, Transition States and Reaction Path
Pan Yinming, Zhao Xuezhuang, Liu Jingjiang, Kao Chenheng
1985, 6(8): 703-708.
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In this paper, the configurations for the intermediates and transition slates of C
6
H
8
-NO
2+
system, obtained by the SCF-CNDO/2 method, have been analyzed. The reaction path for nitration of benzene can be appraised. Additionally, some experiment phenomena in connection with this reaction may be explained, too.
Studies on Nitroxides (Ⅺ)——One-Electron Transfer Reaction of Piperidine Nitroxides with Hydroxylamine
Liu Youcheng, Wu Shuping, Jiang Zhiqin, Zhang Maoxi
1985, 6(8): 709-713.
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The redox reactions of 4-substituted piperidinc nitroxidcs with hydroxylamine (NH
2
OH) in mcthanol over a wide range of pHvalues were investigated. It was found that the nitroxides were rapidly reduced to the corresponding hydroxylamine hydrochlorides in acidic medium, while hydroxylamine was oxidized to nitrous oxide. Futhcrmore, the reaction also took place slowly in alkaline media, but the piperidinc hydroxylamincs formed arc unstable under alkaline conditions and readily oxidized by oxygen in the air to regenerate the nitroxidc radicals. In order to examine this reaction, an alternative route to prepare the piperidine hydroxylamines was carried out via the reactions of the nitroxides with vitamin C.
Studies on Thermokinetics (Ⅱ)——Thermokinetic Method for the First Order Reactions
Deng Yu, Xu Yinghong
1985, 6(8): 714-718.
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On the theoretical basis of thermokinetics proposed in previous article, the fundamental equations of thermokinetic method for the first order reactions are derived in this paper.This method has been used to study the saponification of two esters in aqueous alcohol solvents. The rate constants of these reactions claculated with this method are in agreement with the values in literatures. And therefore, the theoretical basis of this method is believed to be correct.
The STO-xG Fixed Single ξ Basis Functions of Variable Expansion Length
Ning Shiguang, Xuan Zhongliang
1985, 6(8): 719-724.
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The STO-xGfixed single ξ basis functions of variable expansion length with the regression values of ζ or any values belong 10 the ζ interval of confidence level of 99.7% are presented. Comparison of the STO-xG (for example STO-6.3G) fixed single ζ mini, basis set with the appropriate STO-KG (for instance STO-4G)basis set in SCFcalculations illustrates that the former not only takes less CPUtime and provides better results, but also is practical and systematical. In addition, the results of this paper express that the proportion of kinds of basis functions of different angular momenta in the extented part of extented basis set should not overlooked, and the ζ interval of confidence level of 99.7% is valuable in considering the regions for optimizing ζ values.
Determination of the Graft Degree on the Surface of Silica GEL by XPS
Huang Huizhong, Guo Qinlin, Gui Linlin, Wang Qinwei, Duan Xiaoqing
1985, 6(8): 725-728.
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Attention is being increasingly paid to the new material prepared by bonding organic molecules to the surface of silica gel in the preparation of catalyst or packing material for liquid chromatographic column.There has not been a quantitative method for determining or characterizing the graft degree on the silica gel surface yet. This paper provides a new semi-quantitative method.
Fourier Transform Infrared Spectra of Dimethylformamide at Variable Temperatures
Wu Jinguang, Liang Xiangxing, Lin Yingzhang, Guo Hai, Xu Guangxian
1985, 6(8): 729-734.
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In the previous report we studied the FTIRspectra and normal coordinate analysis of dimethylformamide (DMF), an important solvent having many desirable properties. In order to understand the nature of interaction between DMFmolecules in the vapor, liquid and solution stales, we have taken the advantages of the high resolving power and sensitivity of FTIRand studied the spectra of liquid DMFin the temperature range between 20° to 120℃ at 5° intervals and the effect of concentration on the spectra of DMFin CCl
4
solution. It has been found that the liquid DMFexists in dimeric form through the formation of an unusual hydrogen bond between C-H…O, and in CCl
4
solution, equilibrium exists between the dimeric and monomeric forms of DMF, the position of equilibrium is dependent upon the concentration.
The Crystal and Molecular Structure of Neodymium Chloride Isopropyl Alcohol Complex
Jin Zbongsheng, Wang Shenglong, Wang Fusong, Shen Cheng, Yang Guangdi, Fan Yuguo
1985, 6(8): 735-737.
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The crystal structure of [NdCl
5
·(CH
5
CHOHCH
3
)]
2
has been determined by X-ray diffraction method. It is triclinic and the space group is P1, with dimensions: a= 11.184(2)Å, b= 13.462(3)Å,c = 5.9794(9)Å, α = 101.37(2) °β = 93.6l(2)°,γ= 69.46(2)°. The structure was solved by patterson method. The final residual factor is R= 0.038. The feature of the crystal structure is that every two Nd ions are linked in pairs through a chlorine bridge o?two chlorine ions to form a complex molecule and every Nd ion is seven-coordinate.
Correlation Between the Coke Formation and Structural Hydroxyl in NaHY Zeolite
Li Rongsheng, Zhang Wuyang, Liu Jun, Zhao Zhiming
1985, 6(8): 738-740.
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In this article the correlation between the coke formation and structural hydroxyls in NaHYzeolite was investigated by using ESRtechnique in cumcne cracking, and the following were observed.1.With the pretrcatmcnt temperature of zeolite increasing the cumcne cracking activity decreased and the coke formation declined.2.Also with the calcination time being prolonged the cumcne cracking activity decreased and the coke formation declined.3.The higher the exchange degree of zeolite, the higher the cracking activity of zeolite and the more the coke formation.The tendency of changes of both the cracking activity and the coke formation was in accordance with that of changes of the amount of the structural hydroxyls in NaHYzeolite as function of the prctrcatment temperature, time and the exchange degree of zeolite. On those results above it was concluded that the coke formation was a secondary reaction for the cracking of cumene,that is, not only the structural hydroxyls in NaHYwere active sites for the cracking, but also for the coke formation.
Studies on Methyl Methacrylate Polymerization Initiated with Piperidine Derivatives and Organic Peroxide Systems
Zhang Jingyi, Qiu Kunyuan, Feng Xinde
1985, 6(8): 741-746.
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The polymerization of methyl methacrylate initiated with piperidine derivatives (piperidine, 2,-2, 6, 6-tetramethyl-4-hydroxyl piperidinc, N-cthyl piperidine, 1,2, 2, 6, 6-pentamethyl-4-hydroxyl piperidine) and organic peroxides (benzoyl peroxide, lauroyl peroxide, t-butyl hydroperoxidc, t-butyl peroxybcnzoatc) systems was studi-ed in this paper. The polymerization rate cquation and the activation energy of polymerization were determined respectively.
Synthesis of Macrocyclic Poly(α-Methylstyrene) and Characterization of Some Properties of the Solution
He Binglin, Huang Jiaxian, Pu Minli, Zhou Changxing
1985, 6(8): 747-752.
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The article describes the synthesis of macrocyclic poly(α-methylstyrene) by the reaction of living bifunctional poly(α-methylstyrene) with the p-bis(chloromethyl)-benzene at very low concentration. The samples thus obtained are fractionated and the fractions are characterized by the methods of light scattering, osmotic pressure and viscosity.The ratios ([η]
exp
)/[η]
linear
) of the intrinsic viscosities in toluene of the two fractions of the lowest molecular weight of cyclic products to that of the linear polymer with the same molecular weight are found to be 0.684 and 0.707 respectively.
Concentration Effect on GPC Retention Volume
Zhang Hongan, Teng Fachun, Ge Weidong, Zhang Min-shu
1985, 6(8): 753-757.
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Concentration effect in the high performance GFChas been investigated. The study of the contraction of hydromechanical volume has been made htough determination of the varying values of the being clution volume with the change of concentrations.On the case of higher molecular weights and higher concentration, the curve of V
c
-Cin good solvent crosses with the V
c
-Ccurve in bad loivend for the samples with the same molecular weight. The point of intersection of the curves shifts to the direction of the lower concentration as the molecular weight increases.
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