1—苯乙酰基—4—芳酰基氨基硫脲的合成及其在碱催化下的环化反应

1-酰基-4-芳基氨基硫脲类化合物在碱性条件下环化为具有广泛生物活性的3-取代基-4-芳基-1,2,4-三唑啉-5-硫酮的反应报道甚多,但1,4-位都含羰基的酰氨基硫脲在碱性条件下环化反应迄今报道较少。我们曾研究了1-[5-(α-萘)-2H-四唑-2-乙酰基]-4-芳酰基氨基硫脲和1-(α-萘乙酰基)-4-芳酰基氨基硫脲在碱催化下环化为3-取代基-4-芳酰基-1,2,4-三唑啉-5-硫酮的反应,它们在低浓度下均有一定的生物活性。本文研究了1-苯乙酰基-4-芳酰基氨基硫脲1_(a～m)在1mol/L K_2CO_3溶液催化下的环化反应,得到环化产物3-苄基-4-芳酰基-1,2,     

242-260nm波长区CS2分子的多光子解离电离

在242－260nm波氏范围通过CS2分子的共振增强多光子电离（REMPI）获得了母体离子CS和碎片离子的分质量激发谱．在λ＜246.4nm区间，CS激发谱上呈现出来源于CS2双光子电离的弥散谱带,碎片离子激发谱的归属强烈提示多光子过程中有中性基电子态的CS和S（经由CS2的光解离）产生：（1）CS 的谱带主要来源于中性CS碎片经由单光子跃迁产生的（1＋1）共振增强电离，（2）除了部分S 的谱峰来自CS 的光解外，多数S 的锐谱峰来自中性S原子经由3p3（2D0）4p，3p3（4S0）np（n＝6，7，8）←3p43pJ（J＝2，1,0）双光子跃迁产生的（2＋1）共振增强电离．     

High-performance liquid chromatographic determination of 18 alpha-glycyrrhetinic acid and 18 beta-glycyrrhetinic acid in rat plasma: application to pharmacokinetic study.

A high-performance liquid chromatographic method for the separation and determination of 18 alpha-glycyrrhetinic acid and 18 beta-glycyrrhetinic acid has been developed. Indomethacin was used as an internal standard. The drugs were separated on a reversed-phase column and detected by UV detection at a wavelength of 254 nm. Methanol-water-perchloric acid-ammonia (80:20:0.4:0.4, v/v) was used as the mobile phase at pH of 7.0-7.5. The detection limit of both compounds was 0.1 microgram/ml in rat plasma. The method was applied to pharmacokinetic studies of glycyrrhetinic acids in rats. The results suggest that the pharmacokinetics appeared to be non-linear in nature.     

CRYSTALLIZATION AND MELTING OF POLY（ETHYLENE OXIDE） CONFINED IN NANOSTRUCTURED PARTICLES WITH CROSS-LINKED SHELLS OF POLYBUTADIENE

Small fixed aggregates of a poly(ethylene oxide)-block-polybutadiene diblock copolymer(PEO-b-PB)in THFsolution were obtained by adding a selective solvent for PB blocks,followed by cross-linking the PB shells.Themorphologies of the nanostructured particles with a cross-linked shell were investigated by atomic force microscopy andtransmission electron microscopy.The average behaviors of the PEO crystallization and melting confined within thenanostructured particles were studied by using differential scanning calorimetry experiments.For the deeply cross-linkedsample(SCL-1),the crystallization of the PEO blocks was fully confined.The individual nanoparticles only crystallized atvery low crystallization temperatures(T_cs),wherein the homogenous primary nucleation determined the overallcrystallization rate.For the lightly cross-linked sample(SCL-2),the confinement effect was T_c dependent.At T_c(?)42℃,thecrystallization and melting behaviors of SCL-2 were similar to those of the pure PEO-b-PB diblock copolymer.At T_c>42℃,SCL-2 could form PEO lamellae thicker than those of the pure PEO-b-PB crystallized at the same T_c.     

Low-temperature electrothermal vaporization of thenoyltrifluoroacetone complex of Sc(III) and Y(III) for sample introduction in an inductively coupled plasma atomic emission spectrometry,and their determination in biological samples

A new method for inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of trace Sc and Y, based on gaseous compound introduction into the plasma as their thenoyltrifluoroacetone (TTA) complexes by electrothermal vaporization was developed. Using the reagent TTA as chemical modifier can not only enhance the analytical signals, but also reduce the vaporization temperature. At a temperature of 1,000 °C the trace Sc and Y can be vaporized completely into ICP. The factors affecting the formation of the chelate and its vaporization behavior, such as drying time, vaporization temperature/time, reaction medium and the amount of TTA, were investigated in detail. Under the optimized conditions (drying temperature/time 100 °C/10 s, vaporization temperature/time 1,000 °C/4 s), the limits of detection for Sc and Y were 19 pg and 34 pg (3), respectively, and the relative standard deviations for Sc and Y were 4.2% (c _Sc=0.2 g mL^–1; n=7) and 2.6% (c _Y=0.5 g mL^–1; n=7). The linear ranges of the calibration graphs cover three orders of magnitude. The method was applied to the analysis of the biological reference materials (GBW 07602, bush branches and leaves; GBW 07604, poplar leaves), and the results obtained were in good agreement with the certified values.     

Determination of gamma-globulin at nanogram levels by its enhancement effect on the resonance light scattering of functionalized HgS nanoparticles

A novel assay of γ-globulin (γ-IgG) with a sensitivity at the nanogram level is proposed based on the measurement of enhanced resonance light-scattering (RLS) signals resulting from the interaction of functionalized nano-HgS with γ-globulin. At pH 5.03, the RLS signals of functionalized nano-HgS were greatly enhanced by γ-globulin in the region of 200-700 nm characterized by the peak around 362 nm. Linear relationship can be established between the enhanced RLS intensity and γ-globulin concentration in the range of 10-140 ng ml⁻¹. The limit of detection is 2.71 ng ml⁻¹. Based on this, a new direct quantitative determination method for γ-globulin in blood serum samples without separation of human serum albumin (HSA) is established. The contents of γ-IgG in blood serum samples were determined with recovery of 95.7-102.5% and R.S.D. of 1.6-2.4%. This method is proved to be very sensitive, rapid, simple and tolerance of most interfering substances.     

Ionic limiting molar conductivity calculation of Li-ion battery electrolyte based on mode coupling theory

A method is proposed based on mode coupling theory in which the ion transference number is introduced into the theory. The ionic limiting molar conductivities of LiPF6, LiClO4, LiBF4, LiCF3SO3, Li(CF3SO3)2N, LiC4F9SO3, and LiAsF6 in PC(propylene carbonate), GBL(gamma-butyrolactone), PC(propylene carbonate)/EMC(ethylmethyl carbonate), and PC(propylene carbonate)/DME(dimethoxyethane) are calculated based on this method, which does not involve any adjustable parameter. The results fit well to the literature data which are calculated by an empirically adjusted formula. This presents a potential way to calculate the conductivities of Li-ion battery electrolytes.     

Stimulated emissions in aligned CdS nanowires at room temperature

Aligned CdS nanowires (NWs) were obtained through a simple thermal evaporation process with highly active CdS nanoparticles as the evaporation source. These NWs show prominent optical waveguides behavior under a continuous-wave (CW) laser excitation. Excitation intensity-dependent photoluminescence (PL) measurements show that these NWs exhibited both broad and supernarrow stimulated emission (lasing) under intense pulse optical excitation at room temperature. Raman scattering and time-resolved PL measurements were used to investigate the optical properties. The results indicated that the stimulated emission in these NWs involves the electron-hole plasma (EHP) and Farby-Perot (F-P) optical resonant processes at room temperature.     

Surface-enhanced Raman scattering of pyridine using different metals: differences and explanation based on the selective formation of alpha-pyridyl on metal surfaces

A simple method has been developed to produce SERS-active metal surfaces. Six metal surfaces (cadmium, nickel, gold, iron, copper, and silver) have been prepared on an aluminum foil underlayment by chemical reduction and strong surface-enhanced Raman signals have been observed for pyridine species on these surfaces. This permits the direct comparison of pyridine spectra on different metal surfaces prepared by the same chemically clean method. The differences among the SER spectra of the aqueous pyridine species using different metals generally follow the trend of silver, cadmium, nickel, iron, gold, and copper, which can be explained by the selective formation of alpha-pyridyl species and the equilibria between end-on adsorbed pyridines and edge-on adsorbed alpha-pyridyl species on the different metal surfaces.     

Aminonaphthalic anhydrides as red-emitting materials: electroluminescence, crystal structure, and photophysical properties

The red and orange emitters (ANA-1-3) consisting of a 4-amino-1,8-naphthalic anhydride group were synthesized. The lowest absorption band of these ANA molecules centered at approximately 450 nm is assigned to be a charge-transfer transition with emission at 514-536 nm in nonpolar solvents such as n-hexane and at approximately 590-640 nm in polar solvents such as THF and CH(2)Cl(2) and in the solid states. Emission lifetimes are measured with time-correlated single photon counting. Shorter lifetimes are observed for the ANA molecules when dissolved in polar solvents compared with those in nonpolar solvents. Strong dipole-dipole interaction of ANA molecules with solvents is indicated. At high concentrations the measured emission lifetimes, generally shortened from self-quenching, are found to remain about the same order of magnitude in ANAs. This implies that the exciton states of aggregates are formed and they exhibit a relatively long lifetime. Crystallographic data of 4-(phenyl antracen-9-yl) (ANA-2) and 4-(phenyl-2-naphthyl) amino-1,8-naphthalic anhydrides (ANA-3) show that the molecules exist as dimeric structures with antiparallel head-to-tail stacking of naphthalic anhydride planes in addition to other pi-pi stacking. The strong dipole-dipole interactions and the pi-pi stacking account for the observed red-shifted emissions of ANAs in the powders. For films prepared from vacuum sublimation, a structure similar to that in the crystal but with less crystalline order is expected based on the emission wavelength. Several electroluminescent devices based on these ANAs are reported here; they emit orange-red light at 602-628 nm with high brightness and steady external quantum efficiency.