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中文
Table of Content
24 January 1992, Volume 13 Issue 1
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Articles
Synthesis and
1
H NMR Study of Rare Earth Complexes with Acyclic Glycols of Different Terminal Groups
CAI Le-zhen, YAO Ke-min, LI Jia-ling, BAO Zheng-cao, SHEN Lian-fang, TIAN Qing-ping
1992, 13(1): 1-5.
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Seventeen new complexes of rare earth perchlorates with diethylene glycol dimethyl ether (EO
2
Me
2
) and diethylene glycol bis(o-methoxy phenyl) ether [EO
2
(MeOP)
2
] were synthesized and characterized by elemental analysis, molar conductivity, XRD, IR, thermal analysis and
1
H NMR.The compositions can be formulated as Ln
3
(ClO
4
)
9
·(EO
2
Me
2
)
5
·18H
2
O(Ln = La, Pr, Nd),Ln(ClO
4
)
3
.EO
2
Me
2
·8H
2
O (Ln=Sm-Er, Yb.Y) and Ln(ClO
4
)
3
EO
2
(MeOP)
2
·6H
2
O (Ln = La,Pr, Nd,Eu,Gd).Their properties, especially NMRand IRspectra, were investigated.The effect of terminal group of acyclic glycol on the compositions and properties of the complexes studied was discussed in detail.Some significant results were obtained.
Synthesis and Magnetic Exchange Interaction of Novel Binuclear Copper Complexes of Keto and Enol Forms
CHEN Jing-tang, LIAO Dai-zheng, ZHANG Ruo-hua, CHEN Hui, LIU Wei-xiang
1992, 13(1): 6-9.
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Novel binuclear copper complexes [Cu
2
(H
2
L)Cl]Cl
2
(keto form) and [Cu
2
(L)Cl]·H
2
O(enol form), where L = N,N'-diisonicotinoyl-2-hydroxy-4-methyl-isophthalaldehyde dihy-drazone, were prepared and characterized.The analytical data show that the copper(Ⅱ) coordinated by ligand is the keto form and enol form respectively, and the anliferromagnetic interaction of enol form(J=-461.8 cm
-1
) is larger than that of keto form (J =- 33.16 cm
-1
).
Synthesis, Characterization and Structure Determination of Di(α-Hydroxyisobutyrate) Diaquo Neotlymium Nitrate
XU Cheng, NI Zhao-ai
1992, 13(1): 10-13.
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The synthesis, the crystal structure of neodymium complex Nd (C
4
H
7
O
3
)
2
·NO
3
·2H
2
O are presented in this report.The crystal structure was determined by X-ray single crystal diffrarction techniques.The structure was solved by the Patterson method and Fourier techniques and refined by full-matrix least square to give a final R = 0.036 for 1358 reflections.The crystal belongs to monodinic system with space group C2/c.The unit cell parameters are: a = 0.8996(1) nm, b=0.8601 (1) nm, c=2.1111(3) nm, β=92.38(1)°, V=1.6320 nm
3
, Z = 4, D=1.83 g/cm
3
.It is confirmed that neodymium is bonded with eight oxygen atoms.The nitrate group in the complex is not coordinated to neodymium, it bad two positions in the crystal.Each two neodymium atoms are connected with two bridging carboxyl group to form a chain polymeric molecule.
Studies on the Rare Earth Coordination Compounds (Ⅸ) ——Preparation and Characterization of Complexes of Rare Earths with BPMPPD
XING Ya-cheng, LI Xiao-jing, YAN Lan, YANG Ru-dong
1992, 13(1): 14-17.
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The present paper covers fifteen new solid complexes of rare earth synthsized by the reaction of rare earth nitrates and (NH
4
)
2
Ce(SO
4
)
3
with BPMPPD in the aqueous solution of ethanol.The compounds with a general formula: RE
2
(BPMPPD)
3
·nH
2
O(Re= La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Y.n = 3-7) ,Ce(BPMPPD)
2
·6H
2
O and (Y-Eu)
2
·(BPMPPD)
3
·8H
2
O(Y:95%; Eu: 5%), were obtained and characterized by elemental analysts, chemical analysis, IR, DTA-TG,
1
H NMRand fluorescence.
Studies on the Solid State Reactions of Coordination Compounds (ⅩⅩⅩⅩⅣ) ——Solid State Synthesis and Crystal Structure of [C
5
H
5
N(C
16
H
33
)]
4
[Cu
4
Br
8
]
LANG Jian-ping, ZHU Hui-zhen, XIN Xin-quan, CHEN Min-qin
1992, 13(1): 18-21.
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A dark solid was obtained by the solid state reaction of (NH
4
)
2
MoS
4
, CuBr and [C
16
H
33
)C
5
H
5
NBr·H
2
O.The solid was treated with CH
2
Cl
2
and then diffused with CH
3
OH to produce the yellow single crystal [C
5
H
5
N(C
16
H
33
)]
4
[Cu
4
Br
8
].The crystal is triclinic with a = 0.9762(2) nm, b=3.1948(4) nm, c=0.9143(2) nm;a= 94.71 (1)°,β= 116.48(2)°, γ = 92.54(1)°,space group P1, Z= 1.The title compound is a chain-like one of four copper atoms bridged by Br atoms.The average Cu-Br distances of the four-coordinated coppers and the three-coordinated coppers are 0.2664(2) nm and 0.2517(2) nm, respectively.The distance between copper atoms in[Cu
4
Br
8
]
2-
ranges from 0.2956(3) to 0.3202(3) nm.
Synthesis and Characterization of 2,7,12,17-Tetra(methylthio)-3,8, 13,18-Tetra(benzoyIthio)tetraazaporphyrin and Its Coordination Compounds with Mg(Ⅱ), Cu(Ⅱ) and Ni(Ⅱ)
TANG Yue-qun, PENG Zheng-he, QIN Zi-bin
1992, 13(1): 22-23.
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The title compounds, 2, 7,12,17-Tetra(methylthio)-3,8,13,18-tetra(benzoylthio) tetraazaporphyrin [H
2
T(mbm)TAP] and its metal complexes[MT(mbm)TAP, M = Mg(Ⅱ), Cu (Ⅱ), Ni (Ⅱ)], were synthesized from l-methylthio-2-benzoylthiomaleonitrile.The new compounds were characterized by elemental analysis, IR, UV-Vis spectra and DTA.
Studies on TTHA A. C. Oscillopolarographic Titration
WANG Xiu-ling, YU Lan-ping, WANG Ya-fan, YIN Shu-hua
1992, 13(1): 24-26.
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The present paper covers the analytical method for determination of some metal ions by triethyltetraaminehexaacetic acid(TTHA) oscillopolarographic titration.The method is rapid and accurate, and the end point is sharp.
A New Nickel Ion Selective Electrode with Hexadecyl Iso-nicotinate as a Neutral Carrier
YUAN Ruo, WU Hai-long, YU Ru-qin, ZHANG Yong-hua, WU Jin-Ian
1992, 13(1): 27-30.
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The present paper describes a new nickel ion selective electrode with a neutral carrier, hexadecyl iso-nicotinate synthesized in our laboratory.The electrode shows a linear response to Ni
2+
ions in the range of 10
-1
~ 8×10
-5
mol/Lwith a slope -25.5 ± 0.4 mV/pC(20±1℃).The potentiometric selectivity coefficients for nickel ions with respect to Na
+
, K
+
, Li
+
, Ca
2+
, Sn
2+
, Fe
2+
, Co
2+
and Cu
2+
are 8.1×10
-5
, 8.6×10
-5
, 8.2×10
-5
, 4.1×10
-3
, 7.5×10
-4
, 3.2 × 10
-2
, 8.0 × 10
-2
and 4.4 × 10
-1
, respectively.The electrode has a fair reproducibility and quick potential response.The conductivity mechanism of the membrane was studied with A.C.impedance method.The experimental results show that the transfer process of Ni
2+
ions across the solvent polymeric membrane is controlled by the diffusion process.
A Study on the Process of Bronze Corrosion by the Methods of IR-Reflection and IR-Photoacoustics Spectra
FAN Chong-zheng, HU Ke-liang, WANG Chang-sui, WANG Sheng-jun, WU You-shi
1992, 13(1): 31-34.
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The surface of self-made Cu-Sn-Pb alloy was corroded by HCl, and the process of corrosion was detected by the methods of IR-reflection and IR-photoacoustic spectra in situ.It was found that the powder rust-eaten product (Cu
2
(OH)
3
Cl) develops fast; the bronze corrosion forms via the intermediate CuCl; the powder state corrosion (PSC) was infectious; and that the particle of PSCscattered light seriously.The results above is discussed and the mechanism of PSC-formation is searched with the thermodynamical calculations.
Studies on the Electrocatalysis of Polynaphthytamine CME(Ⅰ)
HUANG Sha-sheng, YU Yao-qiang, LIN Hui-gai, YU Ru-qin
1992, 13(1): 35-36.
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The electrocatalysis characteristic of Ni-PNAchemically modified electrode was studied.Asimplex method was used for the experimental design.The cyclic voltammetry studies on PNAand Ni-PNAfilm were carried out.It was observed that the Ni-PNAfilm showed electrocatalysis for the oxidation of amino-acid and ascorbic acid in a basic medium.The CMEcan be used for determination of ascorbic acid.
Time Resolved——Window Technique and Its Application
LI Jian-jun, ZENG Yun-e, CHEN Guan-quan
1992, 13(1): 37-39.
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A new time resolved fluorescence spectra technique——window technique is theoretically studied.The technique gives a new way to reduce the interference from the signal with a long lifetime to the determination of fluorescence signal with a short lifetime.The method was applied to the simultaneous determination of europium and samarium, and satisfactory results were gained.
Separation and Determination of Ln
3+
-5-Br-PADAP Complexes by HPLC
GAO Jin-zhang, WANG ji-min, HOU Jing-gou, XIN Wen-ii, BAI Guang-bi, KANG Jing-wan
1992, 13(1): 40-41.
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In this paper, a reversed-phase HPLCis employed to the separation and determination of complexes of Ln
3+
-5-Br-PADAPon a C
18
(5 μm, 150 × 6.0 mm i.d.) column.The pre-column derivatization method was used.We studied the effects of the composition of mobile phase, the amount of buffer in the mobile phase, foreign ions, the column temperature and the flow rate on the separation and determination of Ln
3+
-5-Br-PADAPand determined the rare earth element in mineral.
Studies on Polarographic Adsorption Wave of Mn(Ⅱ)-PAR Complex and Its Analytical Application
CAI Qian-tao, SHI Wen-zhao, LI Ao, LUO Xiao-Ian, WU Ming-jian
1992, 13(1): 42-44.
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In Na
2
B4O
7
(0.08 mol/L)-NaOHmedium at pH12.5, the complex compound of Mn (Ⅱ)-4-(2-pyridyazo)-resorcinol (PAR) gives a sensitive polarographic adsorption wave with relation to the concentration of Mn(Ⅱ) at -0.94 V(vs.SCE) in single-sweep oscillopolarograph, on the basis of which a new sensitive method for the determination of manganese by this polarographic adsorptive wave is established.There is a good linear relationship between the peak height of this wave and the concentration of Mn(Ⅱ) in the range of 4.0×10
-8
~ 5.2×10
-6
mol/Land the detection limit is 1.0×10
-8
mol Mn(Ⅱ)/L.
The Application of Micellar Electrokinetic Capillary Chromatography to Analysis in the Synthesis of Mandelic Acid
FU Xiao-yun, LU Jian-de, LU Yi-jing, XU Hui-feng
1992, 13(1): 45-47.
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The fast and simultaneous analysis of benzyl alcohol, benzaldehyde, benzoic acid and mandelic acid was studied by Micellar Electrokinetic Capillary Chromatography (MECC).The raw material, semifinished products and purified products in the synthesis of mandelic acid were analyzed.The samples synthesized under different conditions were analyzed by using internal standard method.The resutls were used to optimize the synthesis of mandelic acid.
Studies on the Reaction of 2-Acetyl-5-Methyl-1,2,3-Diazaphosphole with Propynol
HE Lan-ling, LIN Chui, LAI Cheng-ming, CAI Bao-zhong, XU Jin-min, WANG Yong-tai
1992, 13(1): 48-51.
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The kinetics of the reaction of 2-acetyl-5-methyl-1,2, 3-diazaphosphole was investigated with FTIRand
31
P NMR.The mechanism of this reaction was suggested, which was verified in comparison with the reaction between 2-acetyl-3-chloro-5-methyl-1,2,3-diazaphospholene and propynol in the presence of triethylamine.
Studies on the Synthesis and Biological Activity of 1-Alkyl(or Aryl)- 5-Substituted Amino-4-(N-Alkyl carbamoyl)pyrazole
CHEN Ru-yu, WANG Jian-wu
1992, 13(1): 52-55.
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In order to look for biologically active heterocyclic compounds, pyrazolo[3,4-d]-1 ,3-oxazin-6-ones(Ⅱ) were reacted with primary amines, l-alkyl(or aryl)-5-benzoylamino-4-(N-alkyl carbamoyDpyrazole (Ⅱ) were obtained.By the reduction of Ⅱ, it was found for the first time that only one of the two amide groups in compound Ⅱ was reduced selectively to give 1-alkyl (or aryl)-5-substituted amino-4-(N-alkyl carbamoyl) pyrazole (Ⅲ).Twenty three new compounds were prepared and identified by
1
H NMR,
13
C NMI,IRand MS.The preliminary biological activities of the products indicate that some of them possess antitumor and pesticidal activities.
Preparation of α-Oxo Ketene Cyclic Dithioacetals
LIU Qun, ZHANG Shu-jia, ZHANG Jing-ping
1992, 13(1): 56-59.
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Three compounds of a-oxo ketene dithioacetals were prepared by Dieter's method.When 1,2- and 1,3-diiodoalkane in the form of diluted solution were added into the reaction system, four analogues of a-oxo ketene cyclic dithioacetals were obtained in high yields by starting from appropriate a-methylene ketones.
A Study on Mass Spectra of Organophosphorous Compounds (Ⅵ) ——The EIMS and CIMS of Derivatives of Phosphorodiamidoates
JIA Wei-ping, LIU Shu-ying, CAO Jie, LAI Peng-xiang, CHEN Ru-yu
1992, 13(1): 60-64.
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The electron impact mass spectra (EIMS) and chemical ionization mass spectra (CIMS) of seven new N-alkyl-N'-ethoxycarbonylmethyl-N'-arylsulfonyl-O-ethyl phosphorodia-midoates are reported.The results show the EIMSand CIMSof this type compound all have many ion peaks produced through skeleton rearrangements.The difference of substituents has an effect on the mass spectra.P-Nbond cleavage is important mass spectra behaviour in EIMS.MH
+
ions have higher relative intensity in CIMS case.There are many products from ion-molecular reaction.
New Ester-Containing Porous Polymeric Beads as Gas Chromatographic Stationary Phase
ZUO Yu-min, LIU Shu-yuan, LI Li-geng, WANG Yong-hui
1992, 13(1): 65-67.
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A series of porous copolymers from diallyl m-phthalate, divinylbenzene and acryloni-trile were prepared by suspension polymerization in the presence of a mixture of toluene and C
9
～G
13
alcohols as a diluent, using azo-bis-isobutyronitrile as an initiator.By changing the molar fractions of the monomers, the GCcolumn packing materials of different polarities have been obtained.The porous structure of the polymeric beads is mainly dependent on the amount and constituents of the diluent.The physicochemical and gas chromatographic properties of these new ester-containing polymeric beads were determined and the polarities were evaluated by means of modified McReynolds polarity scale.The excellent selectivity of these GCstationary phases is well documented through several examples.
Steroidal Saponins from
Smilax Lebrunii
JIA Zhong-jian, JU Yong
1992, 13(1): 68-69.
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Two new steroidal saponins were isolated from 70% EtOHextract of the rhizomes of Smilax lebrunii Levl.On the basis of spectral and chemical methods, their structures were established as: 25-R-spirostan-3β-of-6-one-3-O-[a-L-arabinopyranosyl (1-6)]-β-D-glucopyra-noside(1) and 25-S-spirostan-5-en-3β, 27-diol-3-O-[a-L-arabinopyranosyl(1-6)]-β-D-glucopy-ranoside (2).
Synthesis of 5-Alkyl-2,3-Dimethylpyrazine-mono-N-Oxides
CAI Song-chuan, ZHAO Tao-nan, SUN De-hua, ZHANG Dao-xin, BAO Yan-chu
1992, 13(1): 70-72.
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N-oxidation of 5-alkyl-2, 3-dimethylpyrazines with 30% H
2
O
2
-AcOHusually gives 1-N-oxides, 4-N-oxides and 1,4-N-dioxides.When the molar ratio of pyrazines/H
2
O
2
/AcOHis 1 : 1.2 : 15 at 70℃, the reaction is gives mono-N-oxides with best yields.N-oxidation of ten 5-alkyl-2,3-dimethylpyrazines were carried out under the above conditions, giving thirteen new compounds 5-alkyl-2,3-dimethylpyrazine-mono-N--oxid.es with satisfactory yields (50%～70%).Their structures were confirmed by elemental analysis, IR,
1
H NMRand MSspectrometry.The structures of 1-N-oxides and 4-N-oxides were determined on the basis of
1
H NMRspectral data, since the N-oxide group in substituted pyrazine mono-N-oxides gives the anisotropic effect.Additionally, the structures of eight new 1,4-N-dioxides obtained were confirmed by elemental analysis, IRand
1
H NMRspectrometry.
Studies on the Electronic Structures of Sandwich Clusters (Mo
3
S
4
)
2
M
8+
(Mo, Sn, Cu
2
)
LI Jun-qian, WANG Zhe-min, HUANG Jin-ling, CHENG Wen-dan
1992, 13(1): 73-77.
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By analyzing the MOand electronic structure for a series of sandwich cluster compounds (H
2
O)
9
Mo
3
S
4
MS
4
Mo
3
(H
2
O)
9
8+
(M = Mo, Sn, Cu
2
) we found that it is with the multiple center d-p π orbitals that "ligand" Mo
3
S
4
4+
bonds to the center atom Mto form this class clusters.The mechanism is similar to that of the formation of the classic sandwich complexes in which the ligands are conjugate organic ring.Additionally, the configurtion, the electronic spectrum and the magnetism of these sandwich clusters were accounted for on the MO's origin, and the linkage between the change in multiple center d-pπ bond and the properties of these clusters was given.
Ab initio Studies on the Molecular Complexes Between CO
2
and HCN, NH
3
or H
2
O
XU Sen, FANG De-cai, FU Xiao-yuan
1992, 13(1): 78-80.
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All of the geometries of the title complexes are optimized by the energy gradient technique based on ab initio SCF MOby using 3-21Gbasis.The results show that the molecular complexes CO
2
-HCN, CO
2
-NH
3
, CO
2
-H
2
O all have T-shaped equilibrium structures.The van der Waals'bond lengths of the three complexes are 0.2865, 0.2775 and 0.2543 nm, respectively.The binding energies are 14.8, 27.0 and 31.2 kJ/mol, respectively.The results of energy decomposition show that the interaction energy INTis mainly contributed by the electrostatic interaction ESand is slightly by the charge transfer energy CT.
Multinuclear NMR Study of Aqueous Lanthanide-TTHA Complexes
HUA Shi-ying, SONG Rui-fang, HUANG Gui-qing
1992, 13(1): 81-84.
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The shift reagent properties of eleven Ln(TTHA)
3-
complexes were studied on the basis of measuring the chemical shifts of
23
Na,
2
H,
17
O,
35
Cl induced by these complexes.The results indicate that the axially symmetric Ln(TTHA)
3-
complexes are better aqueous shift reagents, especially the shifts of
23
Na are consistent with theoretical dipolar shifts, indicating that the Ln(TTHA)
3-
complexes are the best one for positively charged substrates.
The Basic Vectors of
d
n
Ion in Pentagonal Field and Related Matrix Elements
SHA Kun-yuan
1992, 13(1): 85-88.
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It is proved that by employing the ten spin-d-orbitals matched for group chain (SO
3
⊃D
n
⊃C
n
) ×SU(2), the Slater functions of the direct product for the single electron can be used as the basic vectors of the irreducible representations of
d
n
ion or the direct summation representations of two one-dimensional representation.The related matrix element expressions and the calculation of EPRparameters are systematically derived to realize computation on a mini-computer for all dNion in pentagonal field.
The Electrochemical Behavior of Benzyl Viologen Bication on Glassy Carbon Electrode
DAI Hong-ping, WU Hui-huang, ZHOU Shao-min
1992, 13(1): 89-92.
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The electrochemical behavior of benzyl viologen bication (BV
2+
) on glassy carbn (GC) electrode in phosphate buffer (pH=6.8) was studied by cyclic voltammetry.The redox process of BV
2+
on unactivated GCelectrodes depends strongly on the concentration of BV
2+
, potential range and scan rates.BV
2+
ions are reduced in two steps, the neutral viologen deposited on the electrode.On electrochemically activated GCelectrode the adsorption of BV
2+
is greatlyenhanced, and only adsorbed BV
2+
shows its redox process in the dilute BV
2+
solution, however, the adsorbed BV
2+
and BV
2+
in the solution take part in the electrode process in the concentrated solution.The possible effect of electrochemical activation of GCelectrode was discussed.
Photosensitive Characteristic of FET Devices Modified by CuTsPc Supermolecular Films
JIANG Lei, ZHU Ming, LIU Wang, TIAN Ke, BAI Yu-bai, LI Tie-Jin
1992, 13(1): 93-96.
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In this paper, a new type of photosensitive.device is reported, it was made by modifying
8
layers of copper tetrasulfonatophalocyaine(CuTsPc) supermolecular films onto FETdevice.The measuring results of characteristic device show that the device has a stable threshold voltage (V
T
), better output characteristic and a spectral response which is in agreement with that of the absorption spectra.Finally, the mechanism of the device was studied by using surface photovolt-age spectrascopy.
The Effect of Magnetic Field on ξ Potential of Ferric Hydroxide Colloid
SHEN He-bai, ZHU Chuan-zheng, TIAN Su-lian, HUANG Zi-qiang
1992, 13(1): 97-99.
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In this paper, the effect of magnetic field on ζ potential of ferric hydroxide colloid is studied.The experiment result shows that there is a pronounced change in ζ potential, electric conductivity and coagulation value of the colloid when it is magnetized.The magnitude of this effect is found to be connected with the intensity of magnetic field, the time for the colloid to be magnetized and the concentration of the colloid.In the meantime, we have observed the difference before and-after the magnetization of the colloid under an electron microscope.The results of our experiment are also discussed.
Determination of Crystallinity of Synthetic Molecular Sieve by μ Value Method of X-ray Diffraction
CHU Gang, ZHANG Jing, WANG Yi
1992, 13(1): 100-102.
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The μ value method of the quantitative phase analysis by X-ray diffraction is presented.The method is used to determine the samples when no standard or reference samples can be found.In this method, the crystallinity determined is only related to the diffraction intensity of the samples and the mass absorption coefficients of the phases.The least square regressive analysis is also adopted to decrease the test deviation.
The Synthesis of Zirconium Bis(Monooctyl Phosphate) and Indexing on its Polycrystalline X-ray Diffraction Pattern
WANG Bo, CHEN Yun-qing, WANG Zhen-jun
1992, 13(1): 103-106.
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A new Componnd of Zirconium bis(monooctyl phosphate) was prepared.The powder .crystals with higher crystallinity degree were obtained by HFacid recrystalization.The study of elemental analysis and IR, TGA, DTAshows that the molecular formula of zirconium bis (monooctyl phosphate) can be expressed as Zr(G
8
H
17
OPO
3
)
2
. The X-ray powder diffraction pattern of Zirconium bis(monooctyl phosphate) was determined and all X-ray diffraction lines were indexed.The indexing results show the crystal belongs to monoclinic system with simple mon-oclinic lattice.The cell parameters of the crystal here are a=1.699 nm, b=1.537 nm, c=2.454 nm, β=123.56°.Based on this each cell has 8 "molecules".
Synthesis and Characterization of Catalytic Property of Rare Earth Complex Oxides Dy
0.5
Sr
1.5
MO
4
(M = Mn, Fe, Co, Ni) with K
2
NiF
4
Type Structure
CAO Lai-zhang, MA Fu-tai, LÜ Guang-lie
1992, 13(1): 107-110.
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The rare earth complex oxides Dy
0.5
Sr
1.5
MO
4
(M = Mn, Fe, Co, Ni) were prepared.Their crystal structures have been studied by means of X-ray diffraction technique.The complex oxides with K
2
NiF
4
tetragonal type structure have been obtained.The catalytic property has been characterized with micro-reactor and temperature programed desorption (TPD) technique.Besides, the availability of tolerance factor(t) has been discussed.
A Study of Structure of Perovskite Oxide LnAlO
3
and Their Catalytic Properties for Methane Coupling
WANG Jiang, ZHEN Kai-ji, BI Ying-li
1992, 13(1): 111-114.
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The bulk Structure and deformation of the perovskite oxides——LnAlO
3
were characterized by using XRDand the behavior of oxygen adsorption on these catalysts was investigated by using TPD.The corelation between the crystalline structure and the catalytic properties indicates that a high degree deformation of structure and a large amount of surface defect may cause a strong ability of oxygen adsorption, as a result, leading to a nice catalytic activation.An as-sumeption was made that the adsorbed oxygen atom is the species for the activation of methane.
The Effects of Substituents at Phenyl Ring of Tetraphenylporphyrins on Intramolecular Energy Transfer of Zinc-metal-free Porphyrin Dimers
HUANG Jin-wang, TAN Qiao, QIN Xia, JI Liang-nian
1992, 13(1): 115-116.
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Two new zinc-metal-free bis-porphyrin dimers linked by a flexible alkoxy chain were synthesized.Their absorption spectra and steady-state fluorescence spectra show the existence of intramolecular energy transfer processes in these porphyrin dimers and the efficiency of the intramolecular energy transfer of the porphyrin dinner with electron-donating substituents at .meso-po-sition of phenyl of metal-free porphyrin is greater than that of the dimer with electron-withdrawing substituentes.It seems that the porphyrin dimer with a -OCH
3
group at weso-position of phenyl of porphyrin is a better model of biological photosynthetic reaction.
Character of Gelatin Membrane for Separation of Ethanol/Water Mixture
DING Ma-tai, XIA Hai-ping, DING Jun-qi, HE Xu-min
1992, 13(1): 117-118.
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After cross-linked by using Cr
2
(SO
4
)
3
, gelatin membrane was used successfully for separation of ethanol/water mixture by pervaporation.And the effects of time, downstream pressure, temparature, and feed concentration on flux and separation coefficient were studied.
Catalytic Behaviour of Cross-linked Saponite in Dehydration- Amination of Methanol with Ammonia
SUN Xiu-li, REN Bei-yuan, JIANG Da-zhen
1992, 13(1): 119-121.
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The pillared saponites were prepared by replacing the interlayer cation in the saponites synthesized by using hydrothermal method with [Al
13
O
4
(OH)
24
(H
2
O)
12
]
7+
.The linkage mode of pillar with layer may be Al-O-Al
p
obtained by means of hydroxyl group condensition acom-panying the breaking of Si-Obond in the tetrahedral sheet according to the results of MAS NMR, XRDand chemical analysis.The dehydration-amination of methanol with ammonia was studied over the pillared saponites at 375 - 450℃ under ambient pressure.It is found that the methanol conversion and amine selectivity incresase with the acid amount on the surface of pillared saponite which is correlative with pillar density.The trimethylamine was suppressed with the increase of pillar density which is.correlative with the size and shape of pore structure.It means that the pillared saponite possesses the function of shape selectivity.
Temperature Dependence of the Pattern of Hydrogen Bonding in o-ethoxybenzoic Acid
WANG Yan, SUN Zi-ming, DAI Xiao-chang
1992, 13(1): 122-124.
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The temperature-dependent IR spectra of o-ethoxy benzole acid reveal that the inter-molecular structure patterns in the liquid state are basically the same as those in the solid state close to its melting point, which exist in the form of intramolecular H-bonding.But at - 150℃ the characteristic carboxyl dimer absorptions were observed, whose intensities increase with the fall of temperature.Their OHvibrations were proved by the spectra of C
2
H
5
OC
6
H
5
COOD and C
2
H
5
OC
6
H
5
COCl.
Studies on Poly(2,6-Ethylene Naphthalene Dicarboxylate) Electrets
ZHOU Yi-qin, XU Hai-yan, ZHANG Ji-xiang
1992, 13(1): 125-128.
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The detrapping currents from poly(2,6-ethylene naphthalene dicarboxylate) (PEN) films r-irradiated at doses ranged over 5× 10
4
Gy were determined by means of Thermally Stimulated Current (TSC) technique, and the various electrode materials were used.The sign transition of main species of charge carriers in biaxial stretched PENfilm was observed.It is explained that this transition results from shifting of sub-Fermi levels of electrons and holes since the r-irra-diation causes decreasing of mean trap levels.The de-electreting phenomena of both amorphous and biaxial stretched PENelectrets have been investigated.The mechanism of moving of charge carriers during de-electreting process is discussed.
Calculation of the Distribution Function of the Radius of Gyration for Random Walk Chains
WU Shao-zeng, ZHANG Cheng-xiang
1992, 13(1): 129-132.
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General expressions of the moments of the distribution function of the radius of gyration for linear chains were obtained by using the random walk model.It was proved that for the long chains, the asymptotic result is the same as that of Gaussian chains.An approximation method for calculating the moments of distribution function is given and explicit expressions for the first three moments are obtained.
A Study of the Applicability of GPC Universal Calibration to a Long Branched Chain of Poly vinyl chloride
CHENG Shu-yao
1992, 13(1): 133-136.
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The applicability of universal calibration to a long branched chain of polyvinylchloride is researched immediately by the apparatus of GPCcombined with a continuous viscometer and a low angle laser light scattering photometer.Results show that universal calibrations are all applicable to fractions of all branched polyvinylchloride whose branched parameter g'(= [η]
b
/[η]
l
) is more than 0.4 and the fractions of linear polyvinylchloride.
Plurality of Active Centers on Heterogeneous Ziegler-Natta Catalysts (Ⅱ)——Kinetic Parameters of Four Kinds of Active Centers
FAN Zhi-qiang, FENG Lin-xian, YANG Shi-lin
1992, 13(1): 137-140.
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The molecular-weight distribution (MWD) of polyoctene-1 synthesized by Complex- II TiCl
3
-AlEt
3
catalyst was determined, and the MWD curves were precisely fitted by four Schulz-Flory "most probable" distributions with different parameters, indicating the pres-ence of four kinds of active center in the studied system.By using of the results of MWDanalysis and polymerization kinetics measurements, R
p
, [C
*
], k
p
, k
tr
and other parameters of the four kinds of active center were determined.The structures of the active centers and the polymerization mechanism are discussed.
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