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Table of Content
24 June 1985, Volume 1 Issue 1
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Articles
Studies on Rare Earth Metal-Hydroboron Componuds(Ⅰ) Syntheses and Properties of Benzoylhydrazine Chelates of Rare Earth Metal (Ⅲ) Dodecahydrododecaborates
Zhang Lun, Hu Peizhi, Qian Chunhua, Zhang Guomin
1985, 1(1): 1-6.
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In this paper,the bcnzoylhydrazine chelates of rare earth metal (Ⅱ) dodecahydro-dodccaboratcs have been synthesized and eaxmined by elemental analysis,IRspectra and clectroconductar.ee measurements.They have the following formulae [Ln(BH)
4
]
2
(B
12
H
12
)
3
(Ln=La,Pr,Nd,Sm,Eu,Gd,Tb,Ho,Er,Tm,Yb;BH=Benzoylhy-drazint).DTAresults point out that these chelalrs are thermally stable.
On Studies of Crystal Structure and Electron Paramagnetic Resonance of(η
5
-C
5
H
5
)
2
Nb[CH
2
S(CH
3
)
3
]
2
Liu Juzheng, Pelersen J. L.
1985, 1(1): 7-14.
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(η
5
-C
6
H
5
)
2
Nb[CH
2
Si(CH
3
)
3
]
2
has been prepared and characterized by X-ray diffraction method and solution and frozen-glass EPR.The compound crystallizes in a monoclinic space group P2
1
/Owith lattice parameters a=13.291(Å),b=12.406(Å),σ=13.901Å,β=115.40,V=2070Å
5
and Z=4 Full-matrix least-squares refinement of the diffractometry data led to final discrepancy indices of K(F
0
)=0.043,R(F
0
2
)=0.057,R
w
(F
0
2
)=0.071.From computer simulation of the frozen-glass spec trum of the compound,the principal components of the g and Ttensors are g
x
=1.9840.g
y
=2.0075,g
z
=2.0020,T
x
=-89.2G,T
y
=-136.9G,T
z
=-50.0G.The observed anisotropy for the hyperfine interaction arises from the admixture of 4d
z
2
and 4d
x
2
-y
2
character in the HOMO.The ratio of mixing coefficients a
2
/b
2
=10.3.
Synergic Extraction of Uranium Thiocyanate by the Ternary System of ABC Species Composed of PMBP-TBP-(C
6
H
5
)
4
AsCI
Yi Min, Chen Dingfong, Mou Xiru, Wang Wenqing
1985, 1(1): 15-20.
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The synergic extraction of uranyl thiocyanate with binary system of 1-phenyl-3-methy1-4-benzoylpyrazolone-5(PMBP)and tributyl phosphate(TBP)or tetraphenylarsonium chloride [(C
6
H
5
)
4
AsCl] and ternary system of PMBP-TBP-(C
6
H
5
)
4
AsCl was studied.There was an obvious synergic effect of uranium (VI)from thiocyanate medium in binary and ternary systems.The formation of a ternary extracted complex,(C
6
H
5
)
4
AsUO
2
(NCS)A
2
TBP,was confirmed by the slope method.Amethod was first proposed for the calculation of the equilibrium constant of ternary synergic reaction.
On the Phase Diagram of LiF-KCI-KBr and KF-NaCI-NaBr Systems
Yan Licheng, Zhu Yingying, Chen Nianyi
1985, 1(1): 21-24.
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The phase diagrams of LiF-KCl-KBr and KF-NaCl-NaBr systems have been de'er-mined by visual polythermal method with the X-ray diffraction analysis of solid phases.The thermodynamical behaviour of the molten salt solutions of these systems are estimated on the basis of the data of phase diagrams.The thermodynamical behaviour of these recipioral-salt-pair containing systems is explained by the results of the computerized simulation using Monte Carlo method.
Calorimetric Study on LaNi
4
M(M=Ni,Cu,Fe)-H Systems
Shen Panwen, Wang Genshi, Song Deying, Lu Shuqin
1985, 1(1): 25-31.
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The relative partial molar enthalpies and the partial molar free energiesof hydrogen dissolved in LaNi
5
,LaNi
4
Cu,and LaNi
4
Fe were measured respectively by acalorimetric system at 298.3K,and the partial molar entropies were also calculated By X-ray diffraction analysis the unit cell volumes Vwere calculated.It was found that both and vary with Vaccording to the following linear relations
The Speciatipn of Mercury in Soil and Sediment
Zhang Hanqi, Li Wanchu, Wu Baohua, Wang Fengchi, Jin Qinhan(Q. Jin)
1985, 1(1): 32-38.
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)
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A systematic procedure for speciation of mercury in soil and sediment was established Experimental conditions were optimized,and interference between different species was studied.The procedure was applied to practical samples and the results obtained were satisfactory.
Study on the Texture of Zinc Electrodeposits by X-ray Diffraction
Xu Shukai, Huang Taishan, Zhou Shaomin
1985, 1(1): 39-46.
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)
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The texture of zinc electrodeposits obtained under potentiostatic and galvanostatic conditions was studied by X-ray diffraction.It is found that the crystal orientation of zinc electrodeposits depends strongly upon the potentials and duration of deposition,the results are discussed in terms of the geometric selection theory and the "outward" growth mode,crystallographic and electrochemical factors are considered together.
Spectrophotometric-Complexometric Titrations(Ⅲ)--The Titration of Micro-quantities of Titanium (Using Benzilic Acid as Masking Agent)
Chen Yongzhao(Chen Yungchao), Qin Ruolan, Chen Huanguang, Qin Ruolan
1985, 1(1): 47-52.
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)
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When DCTA is used as the titrant,benzilic acid is a specific masking agent for Ti (IV).Using the DCTA-benzilic acid masicing method and spectrophotometric end point,90 ppb of Ti can be [selectively titrated.Micro-quantities of Ti in quartz samples can be accurately titrated without prior seperation.We have found that malonic acid is a specific masking agent for Al.When it is used simultaneously with benzilic acid,Ti and Al or Ti,Al and Fe (II) can be titrated stepwise.
Studies on the Chemical Structure of llexolide A
Zeng Longmei, Su Jingyu, Zhang Shude
1985, 1(1): 53-58.
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A new tritcrpene glycoside,ilexolidc-A(Ⅰ),exhibiting cardiac activity,has been isolated from the root of ilex publcscens HorJk et Am.(Ⅰ) has been determined as a β-xyloside of iicxolic acid(Ⅱ),(Ⅱ) is also a new triterpenic acid,and its structure has been assigned as 18-dehydro-20-epi-ursolic acid by chemical reactions and physical methods.The stcreochcnrstry of iicxolic acid was mainly confirmed by X-ray single crystal diffraction method.
Analysis of Chemical Incredients of Angelica Sinnesis--Analysis of Non-Volatile Constituents of Roots
Chen Yaozu, Zhang Huidi
1985, 1(1): 59-67.
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)
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In the present investigation,the non-volatile constituents of Danguei (Tang-Kuei) roots of Gansu origin [Angelica sinensis (Oliv.) Diels] were analyzed and thirty seven organic constituin s were also identified,fifteen of which have not been recorded in literature before,including a new optically active compound named as Angelicide and an antibiotie,Brereldin A.By plasma emission spectrometry,thirteen minor elements were also detecled
Synthesis of lsochroman-4-one and Its Derivatives (Ⅰ)
Tan Zhiming, Yin Bingzhu, Jiang Guiji, Li Hesong
1985, 1(1): 68-76.
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)
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The medium was modified in the synthesis of the isochroman-4-one.Twenty-one of isochroman-4-one derivatives were synthesized.Among those there were five o-acyl oximes,six mannich bases,four 3-methylene substituted compounds and six pyrimidino and pyrazolo derivatives of isochroman-4-one.Part of the Mannich bases of isochromanone in animal indication was tested
Synthesis of a New Type of Nitrogen Crown Ether Compounds
Wu Chenglai, He Yongbing
1985, 1(1): 77-81.
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)
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A large number of various nitrogen-containing macrocyclic poiyether compounds has been synthesized in recent years.Their structure,synthetic methods and applications have been discussed in detail.
Research on 2,5-Disubstituted Oxadiazoles
Pan Jiaxing, Liu Yadong, Gao Zhenheng
1985, 1(1): 82-88.
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)
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2-Phenyl-5-(4'-biphenylyl)-oxadiazole-1,3,4 and twenty five of its 2-substituled phenyl derivatives were synthesized,Their m.p.,λ
max
of UV absorption spectra and fluorescence emission spectra,fluorescence quantum yield as well as laser properties arc given in tables It is found that seventeen of them give higher conversion efficiency than PPO in near UVreion.
NMR Study on the Hydration of Ions in Microemulsion--Bis-2-Ethylhexyl Phosphoric Acid-Alcohol-Kerosine-Water System
Wu Jinguang, Gao Hongchen, Chen Dian, Jin Tianzhu, Xu Guangxian(K. H. Hsu), Sun Xianyu, Zhang Shuizhen, Wu Huaju, Wang Changjin
1985, 1(1): 89-92.
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In the present investigation we have observed the proton shift of water of hydration of metal ions in a microemulsion formed by adding water gradually front 0.05% to 20% to a moisture-free bis-2-ethflhexyl phosphoric acid-alcohol-kerosine sistem saponified by metallic sodium,so that the mole ratio of concentration (M
+
)/V(H
2
O) can be varied from 100:1 to 1:100.Under such conditions,we have obtained the lirni's of SMEfor various cations as follows 6.78PPm(NH
4+
),6.80(Li
+
).5.96(Na
+
).6.40(K
+
),in comparison with the proton shift of liquid water,δ
258
H
2
O=4.80PPm.
Study on Lithium Isotope Enrichment by Band Displacement Process
Ling Daren, Zheng Zuying, Yue Tingsheng, Xu Huiqun, Yang Kunshan, wang Yani, Lu Xianyao
1985, 1(1): 93-100.
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Based on the equilibrium plate model of the distillation type,a set of theoretical equations has been deduced for the isotope's stationary band,and a new method of calculating the height equivalent to a theoretical plate (HETP) used for isotope enrichment was suggested.Moreover,the quantitative relations between the total enrichment and the experimental parameters (concentration of eluant,flow rate,length of band and displaced distance) were established.The expression of enrichment variation,while approaching the stationary state,was corrected and demonstrated experimentally.By the use of that expression,the semicontinuous isotope enrichment process was successfully estimated.
Electrophoretic Study of Surfactant Adsorption
Ma Chiming, Di Jifang
1985, 1(1): 101-108.
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)
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The efforts of adsorption of alkyltrimethyl ammonium bromides on the electrophoretic mobility of a monodisperse polystyrene latex were examined experimentally.The adsorption isotherms were obtained from the electrophoretic data in terms of Stern electrical double layer model.An improved method was proposed for evaluating the number of adsorption sites and adsorption free energy,and the possible mechanism of adsorption was discussed.
The Synthesis, Crystal and Molecular Structure of Tetrakis Dithiocarbamato Molybdenum(Ⅴ)Hexacloromolybdate
Shen Cheng, Sun Chunting
1985, 1(1): 109-113.
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)
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The title compound {Mo[S
2
CN( C
2
H
5
)
2
]
4
}
+1
MoCl
6
}
-1
was synthesized,and its crystal structure was determined by X-ray diffraction.It is nionoclinic,space group P2
1
/a with a=14.761(6)Å b=16.012(6)Å,c=17.108(9)Å,β=102.63(4) and Z=4.The coordinates of a molybdenum atom were deduced from the Patterson function,and parameters of other atoms were found from successive Fourier syntheses.The block-diagonal least-siuares refinement for all alons gave final residual factors R=0.0908,R
w
=0.0761.
Hetero-Atom Zeolite (Ⅱ)--Studies on the Crystal Structures of B-Si Pentasil zeolite Molecular Sieves
Pang Wenqin, Li Guowen, Li Wangrong, Zhang Wanjing, Lin Bingxiong
1985, 1(1): 114-120.
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)
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The crystal structure of B-Si pentasil zeolite molecular sieve was determined by means of the x-ray diffraction for polycrystalline samples and refined by Rietveld method.The parameters of the unit cell are a=19.983(1)Å;b=19.773(1)Å;c=13.303(1)Å.Its space group is D
2h
16
-P
nma
The framework topology found agrees with reported Si-Al ZSM-5zeolite molecular sieves.It is concluded from the structural determination that Bis introduced into the framework of this sample.
Solubility of Electrolyte in Mixed Solvent-Salt-DMSO or DMF-Inert Solvent System
Yang Jiazhun, Liu Ruilin, Yang Jiazhun
1985, 1(1): 121-128.
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This paper reports the solubilities of salts in mixed solvents of DMSO or DMF with 1 enzene,toluene and p-Xylene or rarlon teirachloride.The result Is in accord with the empiricalformula Apreliminary discussion on was given.Based on the nrod-ifled Porn equation,the transrer Gihis free energy formula has been got,and the app oach of Kis given asThe meanns of the aho e formula,calculaed value and condition of ionic solvation veed seussed.
Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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