具有禁带展宽特性的一维光子晶体

提出了介质的光学厚度系数成圆形分布的一维光子晶体结构,与周期结构的光子晶体相比,该结构具有禁带展宽特性.同时讨论了起止膜层及膜层的光学厚度对该结构禁带特性的影响,优化出了在所选材料的介电常数所允许的频率范围内,具有完全禁带特征的光子晶体结构.     

超高效液相色谱法测定水产品中违禁兽药氯霉素、呋喃唑酮和甲硝唑残留

建立了超高效液相色谱(UPLC)同时测定水产品中氯霉素、呋喃唑酮和甲硝唑3种兽药的分析方法.样品采用乙酸乙酯提取,无水Na2SO4脱水,减压浓缩至干,用甲醇溶解,正己烷脱脂.采用ACQUITYTM UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以乙腈-0.004% H3PO4溶液为流动相梯度洗脱,结合波长变化程序,在7.0 min内可完成3种违禁兽药的多残留检测.在0.01～10 mg/L线性范围内,线性相关系数r为0.9997,检出限(LOD)为0.01 mg/L,最低定量限(LOQ)为1.0 μg/kg.空白样品中4个添加水平(1、2、5和10 μg/kg)下,3种违禁兽药的平均回收率为72.3%～119.6%;日内及日间相对标准偏差为2.2%～9.9%.     

新型1,3,4-噁二唑衍生物的合成与性质研究

研制高效载流子传输材料是提高有机电致发光器件性能的关键. 采用对酯对二酰氯(5)与含不同链长烷氧取代基的苯甲酰肼(2)缩合制备了一系列腰接羧基1,3,4-噁二唑衍生物, 即1,4-二[5-(4-烷氧基苯)-1,3,4-噁二唑基]-2,5-二羧基苯(7; 烷氧基＝OCnH2n＋1; n＝8, 12, 16), 并采用UV-vis吸收和荧光光谱对合成物进行了表征. 结果表明: 7的分子结构中羧基的横向引入, 对化合物的光物理性质和能带结构产生较大影响. 这些噁二唑化合物的LUMO及HOMO值分别介于－3.62与－3.58 eV之间及－6.94与－6.90 eV之间, 说明它们可能具有良好的电子传输性.     

超高效液相色谱-串联质谱法测定牛奶和奶粉中6种聚醚类抗生素残留量

建立了用于检测牛奶和奶粉中拉沙洛菌素、莫能菌素、尼日利亚菌素、盐霉素、甲基盐霉素和马杜霉素铵6种聚醚类抗生素残留量的超高效液相色谱-串联质谱分析方法.用乙腈提取样品中的聚醚类抗生素,提取液经HLB固相萃取柱净化,采用超高效液相色谱分离,以电喷雾离子源正离子多反应监测模式进行质谱分析.6种抗生素在0.5～100.0 μg/L范围内均呈线性,相关系数r>0.99.在空白样品中添加6种聚醚类抗生素的回收率均在74.0%～98.5%之间; 精密度(RSD)4.8%～17.2%.牛奶中6种聚醚类抗生素检出限均为0.2 μg/L;奶粉中6种聚醚类抗生素检出限均为1.6 μg/kg.     

Theoretical Study on the Structural and Electronic Properties of Thiocarbamide Hydrochloride

In the present paper, the electronic band structure, density of states （DOS）, and projected density of states （PDOS） analysis of thiocarbamide hydrochloride are reported. Calculations of the electronic properties have been carried out on the basis of fully self-consistent pseudopotential method using DFT. The results show that near the Fermi level, more prominent densities of states are seen between -8 eV and -6 eV in the valence band mainly due to the Cl-3p, N-2p and S-3p orbitals.     

Theoretical understanding on the v(1)-SO4(2-) band perturbed by the formation of magnesium sulfate ion pairs

The factors determining the spectroscopic characteristics of the v(1)-SO4(2-) band of the MgSO4 ion pairs are discussed via ab initio calculation, including coupling effect, hydrogen bonding effect, and direct contact effect of Mg2+ with SO4(2-). With the calculation of the heavy water hydrated contact ion pairs (CIP), the overlap between the librations of water and the v(1)-SO4(2-) band can be separated, and thus the coupling effect is abstracted, and this coupling effect leads to a blue shift for the v(1)-SO4(2-) band of 5.6 cm(-1) in the monodentate CIP and 3.6 cm(-1) in the bidentate CIP. The hydrogen bonding between each water molecule without relation to Mg2+ and the sulfate ion makes the v(1)-SO4(2-) band blue shift of 3.7 cm(-1). When the outer-sphere water around Mg2+ are hydrogen bonded between SO4(2-) and Mg2+, it will make the largest disturbance to the v(1)-SO4(2-) band. Moreover, the inner-sphere water can affect the v(1)-SO4(2-) band conjunct with the direct contact of Mg2+ with SO4(2-), showing a blue shift of 14.4 cm(-1) in the solvent-shared ion pair, 22.6 cm(-1) in the monodentate CIP, 4.3 cm(-1) in the bidentate CIP, and 21.4 cm(-1) in the tridentate CIP. At last, the Raman spectral evolution in the efflorescence production process is tried to be rationalized. The shoulder at 995 cm(-1) is attributed to the monodentate CIP with 2-3 outer-sphere water molecules, whereas the new peak at 1021 cm(-1) at high concentration is assigned to the formation of aqueous triple ion.     

二维相关分析中参考谱的选择对分离重叠峰的影响

二维相关光谱是一项将光谱强度看作两个独立的光谱变量的函数的技术, 它是由动态光谱经过数学转化后得到的. 在扰动过程中, 动态光谱等于实际测得的光谱减去参考谱, 参考谱的选择是任意的, 甚至可以为0, 但是在实际应用时, 人们逐渐发现参考谱的选择会对二维相关光谱产生一定的影响. 本篇文章采用模拟的方法, 建立光谱模型, 光谱强度按e指数形式单调变化, 比较以平均谱为参考谱和不设参考谱得到的二维相关光谱图, 分析它们的区别, 在不同参考谱条件下, 利用二维相关光谱分离重叠峰, 得到的结果也不相同, 将两种条件综合利用可以得到更多更正确的信息.     

Solid-state natural abundance 25Mg NMR studies of Na2MgEDTA x 4 H2O--a possible new reference compound for 25Mg NMR spectroscopy

Natural abundance solid-state (25)Mg NMR measurements were made of the disodium salt of magnesium ethylenediaminetetraacetate tetrahydrate (Na(2)MgEDTA x 4 H(2)O). Both magic angle spinning (MAS) and static experiments were employed to determine the quadrupole coupling constant (C(q)) and the asymmetry parameter (eta(q)) of the electric field gradient (EFG) tensor associated with (25)Mg in this compound, giving the values C(q) = 1.675(5) MHz and eta(q) = 0.15(1). The isotropic chemical shift was determined to be delta(iso) = 0.25(10) ppm (relative to 11 M MgCl(2) aqueous solution) and a small chemical shift anisotropy (CSA) contribution (approximately -13 ppm) was detected, one of the first CSA reports in (25)Mg NMR. This compound exhibited remarkably good (25)Mg NMR sensitivity, due to its fast spin-lattice relaxation and modest quadrupole coupling, which allowed its use as a secondary shift reference and as a test sample for the implementation and optimisation of signal-enhancement methods in (25)Mg NMR spectroscopy, such as double frequency sweeps (DFS) and the use of adiabatic hyperbolic secant (HS) and WURST pulses.     

酸性络蓝K双波长信号系数光度法测定钙镁

基于在氢氧化钠溶液中,钙、镁均与酸性络蓝K(ACBK)形成暗红色配合物,提出了测定钙和镁的双波长信号系数光度法.该法不仅消除了钙、镁之间的吸收干扰,且消除了一定量的共存离子的干扰.利用褪色法与生色法的吸光度之和作为信号吸光度,使方法的灵敏度大为提高.测定钙、镁总量时,分别用钙、镁吸收曲线正峰与负峰上的等吸收波长470.5 nm(λPa)及559.5 nm(λNa)处测定吸光度APa和ANa,求得总量的信号系数fs为2.439.于λPa470.5 nm处测得任一浓度钙、镁试液的吸光度APa′,其信号吸光度As=fsAλPa′.测定镁时,以试剂ACBK褪色对钙配合物生色的完全相消干扰的波长539 nm(Pa)作为测定波长,负峰波长583 nm为Na.按相同方法测得镁的信号系数fs为4.148.     

球磨法制备异质结型光催化剂ZnO/Bi_4Ti_3O_(12)及催化性能

本文用水作为分散介质,掺杂一定量的ZnO于Bi_4Ti_3O_(12)中,采用高能球磨法制备了异质结型光催化剂ZnO/Bi_4Ti_3O_(12).利用UV-Vis、XRD、SEM和PL等仪器对样品进行了分析与表征.以375 W中压汞灯为光源,通过对亚甲基蓝的氧化来研究其光催化活性.结果表明,对于光氧化亚甲基蓝(MB),异质结型光催化剂ZnO/Bi_4Ti_3O_(12)光催化活性高于钛酸铋的光催化活性.当ZnO的掺杂量分别是0.0和0.5wt.%,异质结型光催化剂ZnO/Bi_4Ti_3O_(12)对亚甲基蓝光氧化率分别达到50.2和80.3 %.