Ultrasound-assisted dispersive liquid–liquid microextraction combined with high-performance liquid chromatography-fluorescence detection for sensitive determination of biogenic amines in rice wine samples

Ultrasound-assisted dispersive liquid–liquid microextraction coupled with high-performance liquid chromatography-fluorescence detection was used for the extraction and determination of three biogenic amines including octopamine, tyramine and phenethylamine in rice wine samples. Fluorescence probe 2,6-dimethyl-4-quinolinecarboxylic acid N-hydroxysuccinimide ester was applied for derivatization of biogenic amines. Acetonitrile and 1-octanol were used as disperser solvent and extraction solvent, respectively. Extraction conditions including the type of extraction solvent, the volume of extraction solvent, ultrasonication time and centrifuging time were optimized. After extraction and centrifuging, analyte was injected rapidly into high-performance liquid chromatography and then detected with fluorescence. The calibration graph of the proposed method was linear in the range of 5–500 μg mL⁻¹ (octopamine and tyramine) and 0.025–2.5 μg mL⁻¹ (phenethylamine). The relative standard deviations were 2.4–3.2% (n = 6) and the limits of detection were in the range of 0.02–5 ng mL⁻¹. The method was applied to analyze the rice wine samples and spiked recoveries in the range of 95.42–104.56% were obtained. The results showed that ultrasound-assisted dispersive liquid–liquid microextraction was a very simple, rapid, sensitive and efficient analytical method for the determination of trace amount of biogenic amines.     

The Berezin Transform and Radial Operators on the Bergman Space of the Unit Ball

In this paper, we investigate the connection between compactness of operators on the Bergman space and the boundary behaviour of the corresponding Berezin transform. We prove that for a class of operators that we call radial operators, an oscillation criterion and diagonal are sufficient conditions under which the compactness of an operator is equivalent to the vanishing of the Berezin transform on the unit sphere. We further study a special class of radial operators, i.e., Toeplitz operators with a radial L ¹(B _n ) symbol.     

介质阻挡放电中放电丝结构相变过程研究

在氩气和空气混合气体介质阻挡放电中,研究了放电丝结构随外加电压及气体压强的变化,并从二维体系相变的角度进行了分析.随着电压的增加,放电丝结构的演变过程为:稀疏的随机放电丝—稠密的随机放电丝—六边形结构—超六边形结构—混沌态,此过程相应于二维体系的气相—液相—简单晶体—超点阵晶体—液相的相变过程.实验还研究了相变过程中超六边形形成中晶格常数及相邻格点间距离的变化、超六边形结构中大点的形成过程以及超六边形结构的Penta-Hepta缺陷.     

Al2O3陶瓷衬底碳离子预注入对金刚石薄膜应力的影响研究

通过对Al2O3陶瓷衬底进行碳离子预注入，大大降低了Al2O3陶瓷衬底上金刚石薄膜的应力，且金刚石薄膜中的压应力随碳离子注入剂量的增加而线性下降.通过对Al2O3陶瓷衬底注入前后的对比分析表明，高能量的碳离子注入Al2O3陶瓷衬底以后，并没有产生过渡层性质的新相，而是大量累积在Al2O3晶格的间隙位，使Al2O3晶格发生畸变.而且，随着碳离子注入剂量的增加，Al2O3基体内晶格畸变加剧，注入层残余压应力也随之上升.当金刚石薄膜沉积以后，在降温的过程中衬底这部分残余应力得到释放，从而部分弛豫了金刚石薄膜中的 关键词： 金刚石薄膜 应力 离子注入 Al2O3陶瓷     

Realizing green phosphorescent light-emitting materials from rhenium(i) pyrazolato diimine complexes

Two neutral pyrazolato diimine rhenium(I) carbonyl complexes with formula [Re(CO)(3)(N-N)(btpz)] where N-N = 2,2'-bipyridine (1) and 1,10-phenanathroline (2), and btpz = 3,5-bis(trifluoromethyl) pyrazolate, were synthesized and characterized by elemental analysis, routine spectroscopic methods, and single-crystal X-ray diffraction study. Ground and excited state properties of these complexes were investigated by steady-state and time-resolved spectroscopies. Complexes 1 and 2 show photoluminescent emission in both solution and solid-state at room temperature, arising from metal to ligand charge-transfer (MLCT) transition with strong overlapping of intraligand pi --> pi transitions. The long-lived excited state lifetimes of complexes 1 and 2, which are on the order of microseconds, indicate the presence of phosphorescent emission. As these complexes hold the potential to serve as phosphors for organic light-emitting diodes (OLEDs), their electroluminescent performances were evaluated by employing them as dopants of various electron transport layer (ETL) or hole transport layer (HTL) hosts. For complex 1, a green electrophosphorescence emission centered at lambda(max) = 530 nm was observed at low turn-on voltage ( approximately 6 V) with luminous power efficiency of 0.72 lm/W, external quantum efficiency of 0.82%, and luminance of 2300 cd/m(2) at a current density of 100 mA/cm(2).     

结晶碳酸钕的水热合成、外观形貌及其组成

Crystalline neodymium carbonates were prepared by treating the amorphous precipitate formed from the reaction between neodymium chloride and ammonium bicarbonate under hydrothermal condition. Their composition, morphology and crystal phase were identified by means of elemental analysis, SEM and XRD. It was found that Nd₂(CO₃)₃·2.5H₂O with tengerite-type structure and sheet morphology was obtained when the feed molar ratio(FMR=n_(NH4)2CO2/n_NdCl3)was 2 or 1.8 and hydrothermally treated at 150 ℃ for 12h. However, orthogonal NdOHCO₃ particles agglomerated with long rod crystals were formed when lowering FMR to 1.5 under the same hydrothermal condition. Phase transformation from tengerite-type Nd₂(CO₃)₃·2.5H₂O to orthogonal NdOHCO₃ was occurred when increasing hydrothermal temperature or prolonging hydrothermal time, which is beneficial to the preparation of neodymium hydroxyl-carbonate with neodymium oxide content higher than 70%.     

Pt-WO3/C电极表面活化对乙二醇和CO氧化的作用

用丙酮和四氢呋喃混合溶液对Pt—WO3/C电极进行表面活化处理后，乙二醇在Pt—WO3/C电极上的电催化氧化活性大幅度提高．发现无论在中性溶液中还是在酸性溶液中，表面活化处理后的Pt—WO3/C电极，乙二醇的起始氧化电位负移，氧化峰电流在酸性介质中增加到表面活化处理前的3．2倍：中性介质中增加到表面处理前的4．7倍，其主要原因是表面活化处理后，一方面增加了催化剂Pt的活性表面，另一方面也促进了电极表面吸附的CO的电氧化，减少了CO对电极表面的毒化作用．     

纳米TiO2表面接枝聚苯乙烯及其抗紫外老化研究

利用偶联剂γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)对纳米TiO₂进行表面预处理, 在此基础上通过分散聚合工艺制备聚苯乙烯(PSt)接枝包覆纳米TiO₂. 运用红外光谱、热重分析及透射电镜对处理前后纳米TiO₂进行了表征, 并通过紫外人工加速老化试验比较了表面处理前后纳米TiO₂对聚丙烯/聚苯乙烯(PP/PSt)体系的抗紫外老化性能. 结果显示: KH570与纳米TiO₂表面羟基进行了缩合, PSt在粒子表面实现了接枝聚合, 接枝率约为60% (w); PSt接枝包覆纳米TiO₂呈均匀的微球形, 纳米TiO₂被包覆于微球内部; PSt接枝包覆后纳米TiO₂在PP/PSt中的分散效果较改性前有显著的改进, 其抗紫外老化性能明显优于改性前体系.     

Enantioseparation of Tropic Acid and Its Esters by CEKC Using Sulfated β-Cyclodextrin as a Chiral Selector

Capillary electrokinetic chromatography was successfully applied to the enantioseparation of tropic acid and its four alkyl esters (methyl, ethyl, propyl and butyl), with the same chiral center, Separation was with sulfated β-cyclodextrin (4%, m/v) containing 20 mM phosphate buffer at pH 3.0 as background electrolyte at 20 °C. The results showed that, besides hydrogen-bonding interactions between these compounds with sulfated β-CD, for tropic acid and its methyl ester the steric hindrance effect was also an important factor. However, for the other esters (ethyl, propyl and butyl), the hydrophobicity effect was higher.

     

Characterization of InN epilayers grown on Si(1 1 1) substrates at various temperatures by MBE

InN films have been grown by plasma-assisted molecular beam epitaxy (PAMBE) and characterized by various technologies. It was found that the structural, optical and electrical properties can be drastically improved by raising growth temperature from 440 to 525 °C. Grainy morphology was found in the grain size was found in atomic force microscope images. The large grain size was about 360 nm for a film grown at 525 °C. These films exhibited Wurtzite structure with a c/a ratio ranging from 1.59 to 1.609. The dislocation densities estimated by X-ray diffraction techniques closely agreed with those analyzed by plan-view transmission electron microscopy. Photoluminescence (PL) studies confirmed near band-to-band transitions and the narrowest low-temperature PL peak width was found to be 24 meV at 0.666 eV. Carrier concentrations decreased from 1.44×10¹⁹ to 1.66×10¹⁸ cm⁻³ and Hall mobility increased from 226 to 946 cm² V⁻¹ s⁻¹ as the growth temperature is progressively increased from 440 to 525 °C. Raman spectra also indicated improved crystal quality as the growth temperature was raised.