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中文
Table of Content
24 August 1988, Volume 9 Issue 8
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Articles
Studies on Biologically Active Coordiation Compounds of Metal Ions(Ⅶ)——Synthesize, Character, Antituberculin and Toxicity of Rare Earth Para-Amino-Salicylates
Chen Shuying, Zhang Xinhua, Wang Jingyu, Yu Cuangming, Jiang Yuan, Zhang Xunkai
1988, 9(8): 759-763.
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Fourteen new rare earth para-aminosalicylates were synthesized and characterized by elemenial analysis, IR, UV, Molar conductance, TG-DTA, and X-ray powder diffraction, Their chemical formulae were proved to be RE(PAS)
3
nH
2
Owhere REare earth elements except Sc, Pm, Gd, PAS. para-aminosalicylate, n=1~3. The infrared spectra showed that rare earth elements are chelated by carboxyl group and hydroxyl group. Antituberculin and toxicity research showed rare earth para-aminosalicylates are less toxicity and alittle more efficient than sodium para-aminosalicylate in the inhibition of tuberculin.
The Crystal Crowth and Their Properties of cMn(H
2
O)
4
(NCS)
2
](18C6) and cCo(H
2
O)
4
(NCS)
2
](18C6)
Du Gaoying, Zhang Wenxing, Fan Yuepeng
1988, 9(8): 764-768.
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The crystal growth of CMn(H
2
O)
4
(NCS)
2
](18C6) and [Co(H
2
O)
4
-(NCS)
2
](18C6) were separated by gel diffusion method and solvent evaporation method.The pink slice like crystal and rose red lump like crystal were obtaimed. The elememtal analyses of complex crystals was done.The properties of solubility, electroconductivity measurement, IR, DTA-TG-DTGanalyses. and MSwere respectively tested. All results above and their designation were confirmed by X-ray single crystal structure analysis.
Luminescence of Cerium(3+) Activated Rare Earth Silicophosphates
Huang Zhupo, Ma Guoling, Jing Xipimg
1988, 9(8): 769-773.
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Rare earth silicophosphates with a general formula RE
2
O
3
·0.10SiO
2
·0.95P
2
O
5
were synthesized and developed as good host materials. This paper reports a systematic investigation on the luminescence properties of Ce
3+
-activated silicophosphates of lanthanum and gadolinium. Samples of definite composition and single phase were prepared by solid state reactions. Their crystal stuctures were determined by high resolution X-ray diffractometer D/maxra (4okV, 150mA) to be monodinic and isostructural with GdPO
4
(ASTM 26-660) (Fig. 2). The latice parameters were calculated(Table 1).The emission, excitation and diffuse reflectance spectra of these two phosphors are determined(Fig. 4, Fig.5).The temperature effect from 77 to 423Kon the luminescence of these phosphors has been studied. These appears the thermal shifts of sublevels of
2
F
7/2
of Ce
3+
(Fig,6, Fig.7)From the concentration dependence of Ce
3+
emission Igx-lgI/x a conclusion may be drown, that the concentration quenching of Ce
3+
in the LSPand GSPcomes from the dipole-dipole interaction(Fig.10, Fig.11).
Studies on the Highly Sensitive Colour Reaction of Tellurium(Ⅳ)-Potassium Iodide-Rhodamine B- Polyvinyl Alcohol System
Liu Shaopu, Liu Zhongfang
1988, 9(8): 774-779.
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On the basis of [TeI
8
]
4-
anion reacting with Rhodamine Bin the presence of polyvinyl alcohol to form ion-association complex, a highly sensitive spectroph otometric method was developed for determination of tellurium. The optimum medium of the colour reacion is a 0.64~1.28mol/Lphosphoric acid .solution. The complex has the composition [RhB]4[TeI8] established by the equilibrium shift and Job's method of continuous variations. The reation has a very high sensetivity, its molar absorptivity is 1.65×10
6
L·mol
-1
. cm
-1
at 600nm. The selectivity of this method is fairly good and can be applied for the spectrophotometric determination of trace amounts of tellurium in steel, sulfur and some other samples.
Theoretical Equation of E~t Curve of A. C. Oscillopolarogram
Xu Weijian, Gao Hong(H. Kao)
1988, 9(8): 780-785.
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Theoretical equation of E~t curve of A.C. oscillopolarogram is deduced from the concept of electrochemical impedance. The equation obtained is : similar to Micka's equation but the mathematical treatment is much simple. Equation of pure charging current obtained from Micka's equation is incorrect.
The Enhanced Effect of Surfactant on the Ag
+
-H
2
QS-K
2
S
2
O
8
Fluorescence System and Its Analytical Application
Guo Yaxian, Yu Shirong, Wei Qingxun, Sun Shuju
1988, 9(8): 786-789.
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The fluorescence of the Ag
+
-H
2
QS-K
2
S
2
O
8
system was greatly enhanced by cinnamic acid in the solution of pH10. The excitation maximum occured at 325nm with fluorescence occurred at 420nm.The sensitivity of this reaction is eight-fold higher than that of the reaction in an acid medium(pH1.5~3.5) without the cinnamic acid and the detection limit was found to be 2.0 μg/L. The influece of foreign ions can be eliminatied by ion exchange separation by using a column of anion exchanger of EDTA type.
Oscillographic Titrations
Gao Hong(H. Kao)
1988, 9(8): 790-796.
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Oscillographic titrations are electctrometric titrations which use the sudden change of an oscillogram observed on a cathode-ray oscillograph connected directly to the electrodes of the titration cell to indicate the end-point of titrations. Oscillographic titrations are classified as oscillographic polarographic titrations and oscillographic potentiometric titrations. Papers published in this field in recent years are reviewed.
The Study of Low Energy Electron Impact Mass Spectia of 4-Chloro-4' -Substituted Benzyl Butyl Ketones and Substituent Effect
Lin Xiaoyuan, Li Quo, Tang Huitong
1988, 9(8): 797-801.
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The investigation of the pathway of EIfragmentation of 4-chloro-4'-substituted benzyl butyl ketones with nine different ring substituents was accomplished by means of Mass-Analyzed Ion Kinetic Energy Spectra (MIKES). The results showed that the pathway was predominantly composed of Mclafferty Rearrangement of molecular ions followed by α-dissociation. Under lower impact electron energy down to 20eV, the α-disspciation leaction of product ions of Mclafferty Rearrangement could satisfactorily correspond with Hammeit eqtation resulting in the regression linear epuation lgZ/Z
0
=-0.378σ
p
-0.008 with correlation coefficient 0.9949. The substituent effect of monofnolecular dissociation in mass spectrometry was obviously shown from present work.
Synthesis and Structures of Iron-Sulfur Cluster Complexes: (μ-RS)(μ-R′/CO)Fe
2
(CO)
6
and (μ-RS)(μ-R"CH=CR')Fe
2
(CO)
6
Song Licheng, Liu Jinting, Liu Ronggang, Wang Jitao
1988, 9(8): 802-807.
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Triiron dodecacarbonyl reacts with mercaptans (RSH, R=Et, Me
3
C, CH
2
CH=CH
2
) in the presence of stoichiometric amount of Et
3
Nin THF to give the reactive salt Et
3
NH
+
[(μ-RS)(μ-CO)Fe
2
(CO)
6
]
-
. Reaction of the latter with acid chlorides (PhCOCl, p-MeC
6
H
4
COCl, α-C
10
H
7
COCl,PhCH=CHCOCl, CH
2
=C(CH
3
)COCl) have been studied. The reactions with aromatic acid chlorides give the complexes of type A, whereas those with α,β-unsaturated acid chlorides (phCH=CHCOCl, CH
2
=C(CH
3
)COCl) give the complexes of type Bas well as the corresponding complexes of type A.
Simultaneous Measurement of Primary and Secondary Kinetic Deuterium Isotope Effects by Natural-Abundance
2
HNMR (Ⅱ)——Inter-and Intramolecular Competition Using External Reference
Zhang Benli, Li Guigen, Gao Zhenheng(Kao Chen-heng), Wu Jiazhen
1988, 9(8): 808-813.
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Anovel method for simultaneous measurement of primary and secondary kinetic deuterium isotope effects (KDIEs') by natural-abundance
2
H NMRusing external reference was established. The method takes into account both inter- and intramolecular competitions.
Activity Coefficients of Aromatic-Aromatic Derivative Systems by Gas-Liquid Chromatography
Zheng Guokang, Zhu Yan, Zhou Xiaoxian, Chen Wufeng
1988, 9(8): 814-818.
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The thermostat of the gas chromatograph is a well stirred liquid bath, in which the column temperature is to be kept within±0.01℃.The infinite dilution activity coefficients of C
6
~C
8
aromatics, namely, benzene,toluene,ethylbenzene,p-xylene,m-xylene and o-xylene in aromatic derivative, dibenzyl, diphenylmethane, diphenylacetylene, 4-benzylbiphenyl, benzophenone, dibenzylether, diphenylamine, N, N-diphenylformamide and diphenylsulphoxide, all of them contained two or three aromatic rings have been measured.
Synthesis and Crystal Structure of HMTTeF·I
2
and Its Solid State Properties
Li Zhushi, Jin Zhongsheng, Hu Ninghai, Liu Yongsheng
1988, 9(8): 819-822.
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The crystal of the salt HMTTeF·I
2
was obtained by electrolysis in the diphase mixture solution. It crystallizes in the monodinic space group P2
1
/n, with Z = 4. Lattice parameters are: a=10.942(2), 6=14.294(2), c= 11.415(2)Å, β= 104.32(1)°. Ionization takes place on a pair of lone electrons of tellurium atom. The electrical conductivity (powder/pellet) at room temperature is 4.1×10
-5
Scm
-1
. In this paper the relationship between the structure and the properties of HMTTeF.I
2
was discussed.
Chemistry of Ion Exchange and Adsorption of Gold(Ⅱ)——Adsorption Equilibrium and Breackthrough Process of AuCI
4
-
on the Macroporous Crosslinked Polyacrylate Resin MET-802
Chen Jingren, Qiu Ling, Chang Zheng, Lin Xue, He Binglin
1988, 9(8): 823-828.
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The adsorption equilibrium and breackthrough process of AuCl
4
-
in the medium of hydrochloric acid on MET-802 (corresponding to Amberlite XAD-7) has been studied.In the range of 0.25mol/L~1.00mol/L HCl the selectivity coefficients of AuCl
4
-
to Cl
-
have been calculated from the experimental values. It has been confirmed that transfer of AuCl
4
-
in the breackthrough process is main-controlled by the film diffusion process.The thickness of film δ= 5.8×10
-2
(v)
-0.65
, which is independent of both the concentration of AuCl
4
-
and the size of the resin. HETPis followed by Snyder equations h= 1.8 ×10
2
(v)
0.35
.
The Effect of Ring Formation on the Sol-Gel Distribution (Ⅰ)——A
a
-B
b
Type Polycondensation
Zhang Wanjin, Tang Xinyi
1988, 9(8): 829-833.
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By the use of probability method, the sol-gel distribution equations including intramolecular reaction of sol are deduced. The theoretical and experimental values are coincident.
Application of Surface Photovoltage Technique in Catalysis Studies on Rare Earth Heteropoly Acids
Wu Zhiyun, Wang Dejun, Zhao Zhongqing
1988, 9(8): 834-835.
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We set up a photovoltage spectrometer suitable for studing catalysts and carried out an investigation of a series of bis- (silico-11-tungstic) -rare earth heter-opoly acids called for RE (SiW)
2
. Aset of typical SPV spectra of RE(SiW
2
) are given. The threshold wavelength (TW) producing surface photovoltage varies with the displacement of REelement, and is a vaiuable information for studing catalyst.
Calculation of Vibration-Rotational Energy Levels for Polyatomic Molecules by Ladder Operator Method
Tian Anmin, Liu Ruifeng, Zhou Xuefeng, Sun Zemin, Yan Guosen
1988, 9(8): 836-837.
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One program has been developed for the variational calculation of vib-rationrotational energy levels of non-linear polyatomic molecules. The elements of the secular equation are computated by Huber's Ladder operator method. With this program the vibration-rotational spectra of Ozone and Formaldehyde have been calculated. Good agreement between the theoretical and exerimental results is obtained.
Studies on the Synthesis and Properties of Silicoalumihophosphate-17 Molecular Sieve
Han Shuyun, Zhang Wuyang, Lu Dexin, Zhou Caiju
1988, 9(8): 838-840.
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Silicoaluminophosphate-17(SAPO-17) Molecular Sieve was synthesized by hydrothermal method. The X-Ray diffraction parameteres of the unite cell and chemical composition of SAPO-17 have been determined. The properties of SAPO-17 such as crystal morphology, thermal stability, adsorption capacity and catalytic activity have been studied.
The Preparation and Properties of Na
3.3
Zr
1.65-x
·Ti
x
Si
1.9
P
1.1
O
11.5
System
Wang Wenji, Zhang Zhibin, Zhao Jingzong
1988, 9(8): 841-843.
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Sodium fast ion conductors Na
3.3
Zr
1.65-x
·Ti
x
Si
1.9
P
1.1
O
11.5
were prepared from mixtures of Na
3
PO
4
,ZrP
2
O
7
-ZrO
2
-TiO
2
-SiO
2
in platinum vessel at temperatures of 1173.2~1473.2Kfor several hours to 20 hand 40 h. Most of reactions were carried out at the temperature range 1373.2-1423.2 K. The phases, of NASICONplus ZrO
2
were found, in the composition range x = 0~0.4. Apure NASlCONphase was found with x = 0.5~0.9. Agalss state appeared in x>0.9. Theoretical densities were evaluated according to the cell parameters determined. Electrical conductivities were measured from room temperature to 673.2K. In the same phase range, the conductivity always decreases with increasing x. The best conductor is Na
3.3
Zr
1.05
Ti
0.6
Si
1.9
P
1.1
O
11.5
with conductivity . 47.2(S·m
-1
) ,at 673.2 K. The activation energy data show that most compositions of Na
3.3
Zr
1.65-x
·Ti
x
Si
1.9
P
1.1
O
11.5
system are good conductors.
Studies on the Rare Earth Coordination Compounds (Ⅲ)——Preparation and Characterization of Ternary Complexes of Rare Earths with HPMBP and 1-Nitroso-2-Naphthol
Qi Yulan, Peng Gaocong, Li Xiaojing, Wu Yuansheng, Yang Rudong
1988, 9(8): 844-846.
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This paper reports the preparation and properties of the complexes of rare earths with 1-phenyl- 3-metlfyl-4-benz6yl-pyrazolone-5 (HPMBP) and 1-nitroso-2-naphthol (NN).Compounds of general formulas RE(PMBP)
3
(NN) (whereRE=La, Pr,Nd,Sm,Lu and Y)were obtained and characterized by elemental ana-lysis,IRspectra and
1
H NMR.All fourteen-complexes obtained are gray-violet crystal. They are soluble in ethanol, acetone and benzene, but insoluble in water. In atmosphere, these complexes are stable at room temperture.
Studies on PVC Lithium Ion-Selective Electrodes Based on Tetraphenylborates
Zhuang Yunlong, Qi Deyao
1988, 9(8): 847-849.
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This paper describes the selectivities of a PVCmembrane based on tetra-phenylborate (NaTPBor KTPB) containing dioctyl phenylphosphonate (DOPP) or tributylphosphate (TBP) as mediator solvent for metal ions. The results obtained showed that a lithium ion-selective electrode based on KTPBwith DOPPas. mediator solvent is better, giving linear response in the activity range of 5×10
-5
-10
-1
mol/LLi
+
and detection limit of 6.5×10
-6
mol/LLi
+
. Selectivity coefficients are as follows: The performances of the electrode were compared with those of typical lithium selective electrodes reported recently. This electrode is an useful sensor for lithium.
Quick Determination of Neodymium in Mixtures of Rare Earths by Derivative Spectrophotometric Method
Zhou Shifu, Li Zhong
1988, 9(8): 850-852.
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It is known that the Neodymium Tiron complex has a characteristic abso-rption (578nm) which can be used to determine Nd. If derivative spectrum is used to replace common spectrophotometry, interferences of Ce and Pr can be avoided. The authors have found the other two strong absorption peaks (255nm> 310nm) possessed by rare earths in ultraviolet region. The peak (255nm) has no selectivity but lies at the same wavelength and the molar absorbance coefficient e is a very near thing on all rare earth elements. Thus this peak can be used to determine the total amount of rareearth. Based on this, we measured it at two wavelengths (578nm and 255nm). As a result, a non-weighing derivative spectrophotometric methodfor quick determination of Nd, in mixtures of Rare Earths is established by us.This method has been used in three synthesizing samples and a real sample. Theresults obtained are qutie satisfactory.
Studies on Flavonoids(Ⅷ)——Synthesis of 7-Substituted Flavones and 2',4-Dihydroxy-3-methoxy-4'-Substituted Chalcones
Sun Jinqin, Liu Luwei, Tian Xiujie, Cai Mengshen
1988, 9(8): 853-855.
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The new 7-substituted flavones and four new 2', 4-dihydroxy-3-metho-xy-4'-substituted chalcones were synthesized. The structures of these products were, proved by
1
H NMR, high resolution MSand elemental analysis.
Synthesis of Binuclear Cobalt Clusters(C
6
H
8
C
2
R)Co
2
(CO)
6
Meng Qingjin, Sun Shouheng, Bu Xiuren, You Xiaozeng
1988, 9(8): 856-858.
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Several new acetylene derivatives of Co
2
(CO)
8
have been synthesized by the reaction of acetylenes with Co
2
(CO)
8
. The products have been identified by m.p., element analysis, IR, UVand
1
H NMR. Aliner Hammett relationship is found between λ
max
and σ
p
.
Synthesis of Aminophenylporphyrin Compounds
Xie Hong, Han Shilian, Cui Kairong, Liu Yanqin, zhang Changjiu
1988, 9(8): 859-860.
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This paper reports the synthesis of 5 new aminophenylpoprphyrin compounds. These porphyrin derivatives were separated by method of cutting chromat-ographic column. All these compounds were identified by MS, NMR, IRand UV.
Studies on the Electrocatalytic Reduction of Carbon Dioxide (Ⅲ)——The Electrocatalytic Activities of Metalloporphyrin of TPP, TMAP, TMAPT Series
Cao Xizhang, Zheng Guodong, Teng Yongfu
1988, 9(8): 861-863.
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The Catalytic actions of five water-nonsoluble coordination compounds of metal-tetraphenylporphyrin MTPP(M = Mn,Fe,Co, Ni) and cobalt tetra (dime-thylaniline) porphyrin CoTMAP and four water-soluble coordination compounds of tetrakis (4-trimethylaniline) porphyrin iodide MTMAPI(M = Mn, Fe, Pd and Rh) for the electroreduction of CO
2
has been studied. The result is as follows: at 1.4Vmaximum current efficiencies were obtained for CoTPP CoTMAP and FeTMAPI. Their values(%) are 64 for CoTPP. 76 CoTMAP and 98 FeTMAPI
On the Explanation of the Shift of Raman Frequency of Oxyanions in Molten Salts
Shao Jun, Ma Jianpeng, Yan Licheng, Chen Nianyi
1988, 9(8): 864-865.
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Aquantum chemical interpretation of the shifts of v
1
peaks of Ramanspectra of the oxyanions in molten salt systems has been proposed, based on thecalculation by EHMO method. It can be seen that the cations of alkaline metalswith higher Z/r values make the electron overlap population of X—O bondincreased, and give rise to the Raman spectra with higher v
1
frequency.
The Monte Carlo Simulation of Iodide-Catalyzed H
2
O
2
-BAT Reaction
Wang Kemin, Yu Ruqin
1988, 9(8): 866-869.
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Monte Carlo method was used for computer simulation of the possible reaction route of the iodide-catalyzed H
2
O
2
-BATreaction. For the simulation of the effective collision between the reactant and catalyst particles, some additional hypotheses were proposed and a new Monte Carlo simulation algorithm was worked out. The algorithm can provide useful information for probing the schemes of this type of reaction.
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