超声辅助酶法提取-原子荧光光谱法测定富硒黑木耳中硒形态

建立了富硒黑木耳中硒代胱氨酸、硒代半胱氨酸、亚硒酸、硒蛋氨酸、硒酸5种硒形态的液相色谱-原子荧光光谱分析方法。通过链酶蛋白酶E酶解,结合超声提取后,选取Hamilton PRP-X100离子交换色谱柱(250 mm×4.1 mm,10μm),40 mmol/L的磷酸氢二铵为流动相,在16 min内,5种硒形态完全达到基线分离。5种硒形态在线性范围内相关系数R为0.9990~0.9999;加标回收率为76.1%~108%;检出限分别为硒代胱氨酸0.35μg/L、甲基-硒代半胱氨酸0.46μg/L、亚硒酸0.26μg/L、硒代蛋氨酸0.64μg/L、硒酸3.06μg/L;方法应用于富硒黑木耳中硒形态的分析,精密度高、重现性好、方法稳定、准确可靠,是测定富硒黑木耳中硒形态含量的有效方法。     

Isothermal melt and cold crystallization kinetics of poly(aryl ether ketone ether ketone ketone)

The isothermal melt and cold crystallization kinetics of poly(aryl ether ketone ether ketone ketone) are investigated by differential scanning calorimetry over two temperature regions. The Avrami equation describes the primary stage of isothermal crystallization kinetics with the exponent n ≈ 2 for both melt and cold crystallization. With the Hoffman–Weeks method, the equilibrium melting point is estimated to be 406 °C. From the spherulitic growth equation proposed by Hoffman and Lauritzen, the nucleation parameter (K_g) of the isothermal melt and cold crystallization is estimated. In addition, the K_g value of the isothermal melt crystallization is compared to those of the other poly(aryl ether ketone)s. © 2000 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 38: 1992–1997, 2000     

Pure Graphene Oxide Vertical p–n Junction with Remarkable Rectification Effect

Graphene p-n junctions have important applications in the fields of optical interconnection and low–power integrated circuits. Most current research is based on the lateral p-n junction prepared by chemical doping and other methods. Here, we report a new type of pure graphene oxide (pGO) vertical p-n junctions which do not dope any other elements but only controls the oxygen content of GO. The I–V curve of the pGO vertical p–n junction demonstrates a remarkable rectification effect. In addition, the pGO vertical p–n junction shows stability of its rectification characteristic over long-term storage for six months when sealed and stored in a PE bag. Moreover, the pGO vertical p–n junctions have obvious photoelectric response and various rectification effects with different thicknesses and an oxygen content of GO, humidity, and temperature. Hall effect test results show that rGO is an n–type semiconductor; theoretical calculations and research show that GO is generally a p–type semiconductor with a bandgap, thereby forming a p–n junction. Our work provides a method for preparing undoped GO vertical p–n junctions with advantages such as simplicity, convenience, and large–scale industrial preparation. Our work demonstrates great potential for application in electronics and highly sensitive sensors.     

Photopolymerization of N-substituted phenyl maleimide initiated with N,N-dimethyl-4-toluidine

Several N-phenyl maleimides with different p-substituents have been synthesized from the maleic anhydride and relevant aromatic amine. In the presence of N,N-dimethyl-4-toluidine (DMT), the N-substituted phenyl maleimide (4-XPhMIs) could be polymerized under UV irradiation. It was observed that a new absorption appeared on the UV-Vis spectrum of the mixture solution of 4-XPhMI and DMT, which reveals the formation of charge-transfer complex in the ground state. It was found that the fluorescence of DMT was quenched by 4-XPhMI and the quenching constant of 4-XPhMI, obtained from the Stern–Volmer plot, increases with the electron-deficiency of ethylene double bond of 4-XPhMI. The dynamic quenching of the fluorescence of DMT by 4-XPhMI suggests the formation of exciplex in excited state between DMT and 4-XPhMI. The radicals formed in the systems have been detected by spin-trapping techniques and electron paramagnetic resonance (EPR) spectrometer. Based on all of these results, it has been proposed that the initiation process of the polymerization involves the formation of exciplex and the initial radicals were produced by proton-transfer in the exciplex from DMT to 4-XPhMI. © 1997 John Wiley & Sons, Inc.     

Synthesis and characterization of ABA-type block copolymer of poly(trimethylene carbonate) with poly(ethylene glycol): Bioerodible copolymer

ABA-type block copolymers of poly(trimethylene carbonate) with poly(ethylene glycol) (M_n 6820), PTMC-b-PEG-b-PTMC, were synthesized by the ring-opening polymerization of 1,3-dioxan-2-one (trimethylene carbonate) in the presence of poly-(ethylene glycol) with stannous octoate catalyst, and the copolymers with various compositions were obtained. The PTMC-b-PEG-b-PTMC copolymers were characterized with Fourier transform infrared and nuclear magnetic resonance spectroscopies. The intrinsic viscosities of resulting copolymers increased with the increase of 1,3-dioxan-2-one content in feed while the molar ratio of monomer over catalyst kept constant. It has been observed that the glass transition temperature (T_g) of the PTMC segments in copolymers, recorded from differential scanning calorimetry, was dependent on the composition of copolymers. The melting temperature (T_m) of PEG blocks in copolymer was lower than that of PEG polymer, and then disappeared as the length of PTMC blocks increased. The results of dynamic contact angle measurement clearly revealed that the hydrophilicity of resulting copolymers increased greatly with the increase of PEG content in copolymers. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 695–702, 1998     

BeF2分子基态势能函数研究

利用密度泛函理论（DFT）B3LYP/aug-cc-PVTZ方法对BeF和BeF2分子进行计算, BeF分子的基态电子态为X2Σ+,平衡核间距Re=0.1367 nm,BeF2分子最稳定构型为D∞h构型,基态电子态为X1Σg+,离解能De=13.4 eV。利用最小二乘法拟合了BeF分子基态的Murrell-Sorbie势能函数,并得到其光谱数据与力常数。结合全局多体项展式方法,导出了基态BeF2分子基态势能函数的解析表达式,该函数准确反映了BeF2分子的结构以及静态反应特征,这些结果为进一步探索BeF2的微观分子反应动力学提供了基础。     

Synthesis of arylsulfonyl-substituted indolo[2,1-a]isoquinolin-6(5H)-one derivatives via a TBAI-catalyzed radical cascade cyclization

We have developed a metal-free radical cascade reaction of N-substituted 2-aryl indoles with readily available sulfonyl hydrazides for the rapid construction of arylsulfonyl-substituted indolo[2,1-a]isoquinolin-6(5H)-one derivatives. With the TBAI–TBHP catalytic system, a broad series of structurally diverse indolo[2,1-a]isoquinolin-6(5H)-one derivatives were obtained in moderate to excellent yields. The reaction features mild reaction conditions, operationally easiness, scaled-up feasibility, and high functional-group-tolerance.     

超宽禁带半导体 β-Ga2O3单晶生长突破2英寸

<正>氧化镓(β-Ga_2O_3)单晶是一种第四代超宽禁带氧化物半导体,其禁带宽度为4.8~4.9eV,具有独特的紫外透过特性(吸收截止边~260nm);击穿电场强度高达8MV/cm,是Si的近27倍、SiC及GaN的2倍以上,巴利加优值分别是SiC、GaN的10倍、4倍以上,并且可以采用熔体法生长大尺寸体单晶,因此β-Ga_2O_3已成为超高压功率器件和深紫外光电子器件的优选材料之一。由于其在军事、能源、医疗、环境等领域的重要应用价值,近年来,氧化镓材料及器件的研究与应用成为当前美国、日本、德国等国家的研究热点和竞争重     

2D/3D ZnIn2S4/TiO2复合物的原位构筑及其提高的光催化性能

通过高温煅烧和油浴的方法构筑二维/三维(2D/3D) ZnIn₂S₄/TiO₂异质结, 应用于光催化降解罗丹明B (RhB)和四环素(TC), 来研究异质结的构筑对TiO₂可见光响应范围和光生载流子对分离效率的影响. 结果表明, TiO₂维持了MOFs的形貌, 显示窄的可见光响应范围和高的光生电荷复合率, 与ZnIn₂S₄纳米片复合后, TiO₂的比表面积增大, 光催化活性位点增多. 带隙宽度也由TiO₂的3.23 eV减小到ZnIn₂S₄/TiO₂-II的2.52 eV, 从而获得了更宽的可见光响应范围. 能带结构表明ZnIn₂S₄/TiO₂是type II型异质结, 提高了光生载流子对的分离与转移效率. 在可见光照射下, ZnIn₂S₄/TiO₂-II显示了最高的RhB光催化降解效率(93%), 分别是TiO₂和ZnIn₂S₄的18和2倍. 同时, ZnIn₂S₄/TiO₂-II也显示出比TiO₂和ZnIn₂S₄更高的TC降解效率(90%). 循环实验表明ZnIn₂S₄/TiO₂-II能保持良好的稳定性, 经5次循环实验后仍能降解83%的RhB. 研究表明基于MOFs衍生的TiO₂构筑2D/3D ZnIn₂S₄/TiO₂异质结是提高TiO₂光催化性能的一条有效途径.