HLB柱净化-高效液相色谱法分析水产品中甲基睾酮残留物

建立了水产品中甲基睾酮的高效液相色谱检测方法。样品用乙酸乙酯提取,平行蒸发仪浓缩,甲醇溶液溶解残留物,HLB柱固相萃取净化,高效液相色谱-紫外检测法分析,外标法定量。甲基睾酮质量浓度在0.02~2.0μg/mL范围内线性关系良好,R2>0.9999。添加水平在10.0,20.0,50.0μg/kg时加标平均回收率在72.8%~93.2%,RSD≤8.5%。方法适用于水产冻品中甲基睾酮残留物的测定。     

BiOI/Bi_2WO_6对甲基橙和苯酚的光催化降解及光催化机理(英文)

采用简单的沉积方法制备了不同碘化氧铋含量的BiOI/Bi2WO6光催化剂,通过X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HR-TEM)、紫外-可见漫反射光谱(UV-Vis DRS)和BET比表面积测量对其进行了表征。在紫外和可见光的照射下,使用甲基橙和苯酚的光催化降解评价了BiOI/Bi2WO6催化剂的光催化性能。结果表明:与商业P25和纯Bi2WO6相比,13.2%BiOI/Bi2WO6光催化剂具有更高的紫外和可见光催化性能。这明显增加的光催化活性主要归功于光生电子和空穴在Bi2WO6和BiOI界面上的有效转移,降低了电子-空穴对的复合。基于BiOI和Bi2WO6的能带结构,提出了光生载流子的一种转移过程。自由基清除剂的实验表明,·OH,h+,·O2-和H2O2,特别是h+,共同支配了甲基橙和苯酚的光催化降解过程。     

助剂Fe对Ir/SiO2催化剂的巴豆醛选择性加氢性能的影响

以SiO2为载体采用分步浸渍法制备了Fe/Ir/SiO2催化剂,考察了助剂Fe对Ir/SiO2催化剂气相巴豆醛选择性加氢性能的影响.采用X射线粉末衍射(XRD)、CO化学吸附、H2-程序升温还原(H2-TPR)和拉曼光谱(Raman)等技术对催化剂进行了表征.结果表明,助剂Fe能有效提高Ir/SiO2催化剂的巴豆醛转化率和巴豆醇选择性.Fe含量为0.087%的0.087Fe/Ir/SiO2催化剂的反应性能最佳,反应进行9 h的巴豆醛转化率36.9%,巴豆醇选择性83%.随着催化剂CO吸附量的下降(Fe覆盖的增加),催化剂的转换频率(turn over frequency,TOF)明显增加,这表明Fe促进Ir/SiO2催化剂表面活性位的加氢活性.然而,Fe的掺杂使得Ir/SiO2催化剂存在明显的活性下降现象,归因于Fe导致Ir/SiO2催化剂表面积炭和CO中毒.     

改性活性炭对土壤镉的吸附性影响

目的研究3种改性活性炭对菜地、河流底泥、荷花底泥镉吸附性的影响。方法对活性炭进行酸改性、碱改性和氧化改性,采用双硫腙分光光度法测定镉含量。结果对实验土样,最佳活性炭添加量为0.025 g/g。随着初始镉含量的升高,土壤对镉的吸附量不断增大。结论 3种改性活性炭相比普通活性炭对湿地土壤的镉吸附量均有不同程度的提升,荷花底泥中,酸性、氧化改性活性炭相比普通活性炭,吸附效果提高7.7%,8.3%,吸附效果提升显著。     

基于石墨烯和金纳米笼修饰的无标记型微囊藻毒素免疫传感器的研制

利用石墨烯及中空结构的金纳米笼构建了无标记型电化学免疫传感器,并用于微囊藻毒素的检测。利用多元醇还原法合成制备了导电性好、催化性强、生物相容性好的金纳米笼;再利用高分散的石墨烯将其固定于玻碳电极表面,进一步吸附固定微囊藻毒素抗体。在无微囊藻毒素存在时,电化学探针[Fe(CN)6]3!/4!在传感器界面上能获得较高的电流响应信号。当培育了微囊藻毒素后,抗体与微囊藻毒素形成免疫结合物,增加了电极表面的电荷密度和传质阻力,阻碍[Fe(CN)6]3!/4!扩散到电极表面,导致[Fe(CN)6]3!/4!的电流响应信号明显降低,电流减小的程度间接地与微囊藻毒素的浓度成比例,可实现对微囊藻毒素的检测。实验考察了抗原培育时间,抗体浓度等条件对该传感器响应性能的影响。结果表明,此传感器对微囊藻毒素的线性响应范围为0.05~1000μg/L,检出限为0.017μg/L,优于文献报道。此传感器操作简单,并且具有良好的稳定性,将其用于实际水样中微囊藻毒素的检测,平均加标回收率为94.1%。     

Synthesis and Crystal Structure of a New Pr(Ⅲ)–K(Ⅰ) Heterometallic Oxalate Coordination Polymer

A new 3D heterometallic coordination polymer, namely [K2Pr2(C2O4)4·H2O]n(1), has been successfully synthesized under hydrothermal conditions. X-ray single-crystal diffraction determination reveals that 1 crystallizes in monoclinic system, space group P21/n with a = 12.060(4), b = 8.493(3), c = 15.776(5)(A), β = 93.235(3)°, V = 1613.4(9) 3, Z = 4, Mr = 730.12, Dc = 3.006 Mg/m3, μ = 6.581 mm-1, F(000) = 1368, the final R = 0.0283 and w R = 0.0866 for 2939 observed reflections with I 2σ(I). Complex 1 features an unusual 3D heterometallic coordination framework, in which oxalates exhibit three different coordination behaviours. Moreover, powder X-ray diffraction and thermal properties for 1 have also been investigated.     

介孔SBA-15棒负载的Pd3Cl催化剂催化Sonogashira偶联反应（英文）

通过静电吸引策略将具有高度分散性的原子精确纳米团簇[Pd3Cl(PPh2)2(PPh3)3]+(Pd3Cl)负载在介孔SBA-15棒上。结构明确的Pd3Cl/SBA-15催化剂在以水作为溶剂以及温和的反应条件下对催化Sonogashira碳-碳偶联反应展现了较好的催化性能以及循环性。在此基础上,我们研究了Pd3Cl团簇结构与性能之间的关系,并证实内核的Pdδ+(0<δ<2)与配体之间的协同效应是催化反应的关键。     

Effects of mechanical loadings on the performance of a piezoelectric hetero-junction

A fully-coupled model for a piezoelectric hetero-junction subjected to a pair of stresses is proposed by discarding the depletion layer approximation. The effect of mechanical loadings on PN junction performance is discussed in detail. Numerical examples are carried out for a p-Si/ZnO-n hetero-junction under a pair of stresses acting on the ntype ZnO portion near the PN interface, where ZnO has the piezoelectric property while Si is not. It is found that the bottom of conduction band is lowered/raised near the two loading points due to the decrease/increase in the electron potential energy there induced by a tensile-stress mode via sucking in majority-carriers from two outside regions, which implies appearance of a potential barrier and a potential well near two loading points. Furthermore, the barrier height and well depth gradually become large with increasing tensile stress such that more and more electrons/holes are inhaled in loading region from the n-/p-zone, respectively. Conversely, rising/dropping of conduction band bottom is brought out near the two loading points by a compressive-stress mode due to the increase/decrease in the potential energy of electrons by pumping out the majority-carriers from the loading region to the two outside regions. Therefore, a potential well and a potential barrier are induced near the two loading points, such that more and more electrons/holes are driven away from the loading region to the n-zone/p-zone, respectively, with the increasing compressive stress. These effects are important to tune the carrier recombination rate near the PN interface. Thus, the present study possesses great referential significance to piezotronic devices.     

Snap-through path in a bistable dielectric elastomer actuator

The dielectric elastomer (DE) has attracted significant attention due to its desired features, including large deformation, fast response, and high energy density. However, for a DE actuator (DEA) utilizing a snap-through deformation mode, most existing theoretical models fail to predict its deformation path. This paper develops a new finite element method (FEM) based on the three-parameter Gent-Gent model suitable for capturing strain-stiffening behaviors. The simulation results are verified by experiments, indicating that the FEM can accurately characterize the snap-through path of a DE. The method proposed in this paper provides theoretical guidance and inspiration for designing and applying DEs and bistable electroactive actuators.     

Synthesis and Complexation Properties of Novel Chiral Calix[4]-1,3-aza-crown and Calix[4]arene Hydrazone Derivative

<正>Refluxing calix[4]-1,3-substituted benzaldehyde derivative(4) with glycine hydrazide derivative,we obtained a novel calix[4]arene hydrazone derivative(5) via"1+2"condensation in a yield of 78%.In the reaction of compound 4 with L-leucine hydrazide derivative at room temperature,lariat calix[4]-1,3-aza-crown(6) with chiral amino acid group as branched chain was synthesized via"1+1"addition in a yield of 70%.The preliminary extraction experiments suggested that hosting compounds 5 and 6 possessed good complexation abilities forα-amino acids.