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131.
132.
The dielectric constant ?' and loss tangent tan δ of chlorobenzene-cis-decalin mixtures have been measured in the temperature range 77 K to 330 K and frequency range 0.1 to 100 kHz. On cooling, ?' increases with decreasing temperature upto about 135 K, after which it drops rapidly with decreasing T followed by a slow decrease. This indicates that the liquid mixture goes to an amorphous phase which transforms to a glass phase of restricted dipole rotation below Tg; however, the peak in ?' is due to relaxation in the amorphous phase (α relaxation) and does not give an exact Tg. On heating, the behaviour of the cooling curve is retraced upto 160 K, after which ?' drops suddenly to a value lower than that at 77 K in the glass phase. This indicates the transition to a crystalline phase in which dipole rotational freedom is completely lost. The crystalline phase changes to a eutectic liquid phase of high ?' at a temperature (200 K) lower than the melting point of chlorobenzene and cis-decalin. Dielectric dispersion is observed only in the glass and amorphous phases. The dielectric relaxation time is independent of the concentration of chlorobenzene. 相似文献
133.
Prakash O Kaur H Batra H Rani N Singh SP Moriarty RM 《The Journal of organic chemistry》2001,66(6):2019-2023
The combination reagent (dichloroiodo)benzene and lead(II) thiocyanate in dichloromethane effects oxidation of various enol silyl ethers, ketene silyl acetals, and beta-dicarbonyl compounds, thereby providing an efficient and convenient method for alpha-thiocyanation of carbonyl and beta-dicarbonyl compounds. 相似文献
134.
Trimethylsilyldiethylamine Me3SiNEt2 and MoOCl4 (1:1) undergo a free radical redox reaction in CH2Cl2 or Et2O to form MoCl3O(HNEt2). Reduction occurs even in aprotic media like CCl4 and CS2 to give MoV complexes Mo2Cl6O2(N2Et4) and Mo2Cl6O2[(SCNEt2)2S2], respectively. A 2:1 reaction in nonionizing protic solvents undergoes redox cum cleavage to provide MoCl2O(NEt2) (HNEt2) but a reaction at reflux temperature in 1,2-dichloroethane leads to diethylammonium salt, [Et2NH2][MoCl4O(HNEt2)]. Higher molar reactions (3:1, 4:1) in CH2Cl2 or Et2O are associated with redox reaction as well as oxygen atom abstraction to form de-oxo MoIV complex MoCl3(NEt2)(HNEt2)2, whereas, a 3:1 reaction in CS2 forms Mo2Cl4O(S2CNEt2)4. Compounds have been characterized by elemental analyses, redox titration, magnetic moment, conductance, infrared, electronic absorption and 1H-NMR measurements. 相似文献
135.
Synthesis of cis-hydrindane analogues (2,3) of Cecropia juvenile hormone-I from common intermediate cis-hydrindane-2, 5-dione is presented. The analogues are only moderately active against Dysdercus cingulatus. 相似文献
136.
Shefali Pal Sailendra Nath Poddar Gurucharan Mukherjee 《Transition Metal Chemistry》1994,19(4):449-452
Summary Nickel(II) and palladium(II) complexes of the 1,3-di(o-aminophenylthio) propane (H2L1) and 1,2-di(o-aminophenylthio)xylene (H2L2) ligands have been prepared and characterized. The hydrobromide salt of H2L1 gave a 12 ligand-metal complex of PdII, whereas free H2L1 formed the usual 1:1 species. The reaction of Na2PdCl4 with H2L2 resulted in S,S-dealkylation of the ligand and formation of a mononuclear complex of the corresponding thiol, i.e. 2-aminobenzenethiol. NiCl2, NiBr2 and Ni(ClO4)2 did not react directly with H2L2. NiII is a fairly hard ion and therefore does not coordinate to the soft thioether moiety in H2L2 in the absence of soft anions which symbiotically motivate NiII to act as a soft acceptor. It thus does not react with H2L2 in the presence of hard ions such as Cl–, Br- and ClO
4
–
, but, the in situ reaction of the constituents produced the tetrahedral NiII complex, contrary to earlier reports of similar types of octahedral species. 相似文献
137.
R. P. Rastogi Kehar Singh Ram Shabd B. M. Upadhyay 《Journal of colloid and interface science》1981,80(2):402-411
Electrical properties of cholesterol interfaces have been investigated. For this purpose electroosmotic and hydrodynamic permeation of water, sodium chloride, barium chloride, aluminum chloride, and urea solutions across a cholesterol plug have been investigated. Dependence of electroosmotic permeability on concentration of electrolytes has also been studied. Electrophoretic mobility of cholesterol particles of known size distribution and dispersed in solutions of varying concentrations of electrolytes and urea has also been studied. The data have been used to estimate ζ potentials in order to have a plausible picture of the electrical double layer at the cholesterol/ solution interfaces. 相似文献
138.
S. D. Dogmane R. K. Singh D. D. Bajpai J. N. Mathur 《Journal of Radioanalytical and Nuclear Chemistry》2002,253(3):477-482
Extraction of U(VI) from HNO3, HCl and HClO4 media using cyanex-272 (bis[2,4,4 trimethyl pentyl] phosphinic acid)/n-dodecane has been carried out. In the case of HNO3 and HClO4 media, the distribution ratio (D) value first decreases and then increases, whereas from HCl medium it first decreases and then remains constant with increase in H+ ion concentration. At lower acidities, U(VI) was extracted as UO2(HA2)2 by an ion exchange mechanism, whereas at higher acidities as UO2(NO3)2
.2(H2A2) following a solvation mechanism. The D for U(VI) by cyanex-272, PC-88A and DEHPA at low acidities follows the order cyanex-272 > PC-88A > DEHPA. Also, cyanex-272 was found to extract U(VI) more efficiently than TBP at 2M HNO3. The effect of diluents on the extraction of U(VI) by cyanex-272 followed the order cyclohexane > n-dodecane > CCl4 > benzene. The loading of U(VI) into cyanex-272/n-dodecane from 2M HNO3 has shown that at saturation point, cyanex-272 was 78% loaded. No third phase was observed at the saturation level. The stripping of U(VI) from the loaded organic phase was not possible with water, it was poor with acetic acid and sodium acetate but quantitative with oxalic acid, ammonium carbonate and sodium carbonate. 相似文献
139.
P. B. Ruikar M. S. Nagar M. S. Subramanian K. K. Gupta N. Varadarajan R. K. Singh 《Journal of Radioanalytical and Nuclear Chemistry》1995,201(2):125-134
The extraction of plutonium(IV), uranium(VI), zirconium(IV), europium(III) and ruthenium(III) with -pre-irradiated n-dodecane solutions of methylbutyl substituted hexanamide (MBHA), octanamide (MBOA) and decanamide (MBDA) from 3.5M HNO3 has been studied as a function of absorbed dose up to 184×104 Gray. The distribution ratios (Kd) of uranium(VI) decreased gradually up to a dose of 50×104 Gray and became almost constant thereafter, while ruthenium(III) and europium(III) were not extracted in the entire dose range studied. The Kd values of Pu(IV) decreased gradually up to 10×104 Gray, for MBOA, and 30×104 Gray for MBHA and MBDA and then increased up to a dose of 72×104 Gray, indicating the synergistic effect of radiolytic products at higher doses. The extraction of zirconium(IV) was found to increase gradually up to 72×104 Gray. However, the steep fall in Kd values of plutonium(IV), zirconium(IV) beyond a dose of 72×104 Gray was atrributed to third phase formation. The radiolytic degradation of amides was monitored by quantitative IR spectroscopy and was found to follow the order MBOA>MBDA>MBHA at 184×104 Gray having the amines and carboxylic acids as the main radiolytic products. 相似文献
140.
Yu K Singh S Patrito N Chu V 《Langmuir : the ACS journal of surfaces and colloids》2004,20(25):11161-11168
Using cadium oxide (CdO) as the Cd precursor and tri-n-octylphosphine selenide (TOPSe) as the Se source, TOP-capped and TOP/tri-n-octylphosphine oxide (TOPO)-capped CdSe nanocrystals were synthesized without the use of an acid. The synthetic approach involved the addition of a TOPSe/TOP solution into a CdO/TOP solution with or without TOPO at one temperature and subsequent growth at a lower temperature. The temporal evolution of the optical properties, namely, absorption and luminescence, of the growing nanocrystals was monitored in detail. A comprehensive examination on the control of the photoluminescence (PL) properties was performed by systematically varying the TOP/TOPO weight ratio of the reaction media. Surprisingly, a rational choice of 100% TOP or 80% TOP was found to produce "quality" nanocrystals when monitored under the present experimental conditions and growth-time scale. The term "quality" is mainly based on the sharp features and rich substructure exhibited in the absorption spectra of the growing nanocrystals, as well as the sharp features in the emission spectra with narrow full width at half-maximum (fwhm). There are two distinguishable stages of growth: an early stage (<5 min) and a later stage. TOP plays a major role in the control of a slow growth rate in the early stage, while TOPO controls slow growth in the later stage. The optical sensitivity of the growing nanocrystals when dispersed in nonpolar or polar solvents was studied, including two size-dependent parameters, namely, the solvent sensitivity (PL intensity) and nonresonant Stokes shift (NRSS). The insights gained from the present study enable a synthetic approach in which high-quality CdSe nanocrystals are achieved with high synthetic reproducibility. 相似文献