Fabrication of large‐sized silica monolith exceeding 1000 mL with high structural homogeneity

Reproducible fabrication of the hierarchically porous monolithic silica in a large volume exceeding 1000 mL has been established. By the hydrothermal enlargement of the fully accessible small pores to exceed 50 nm in diameter, the capillary force emerged on solvent evaporation was dramatically reduced, which allowed the preparation of crack‐free monoliths with evaporative solvent removal under an ambient pressure. The local temperature inhomogeneity within a reaction vessel in a large volume was precisely controlled to cancel the heat evolved by the hydrolysis reaction of tetramethoxysilane and that consumed to melt ice cubes dispersed in the solution, resulting in large monolithic silica pieces with improved structural homogeneity. Homogeneity of the pore structure was confirmed, both on macro‐ and mesoscales, using SEM, mercury intrusion, and nitrogen adsorption/desorption measurements. Furthermore, the deviations in chromatographic performance were examined by evaluating multiple smaller monolithic columns prepared from the monolithic silica pieces cut from different parts of a large monolith. All the daughter columns thus prepared exhibited comparable performances to each other to prove the overall homogeneity of the mother monolith. Preliminary results on high‐speed separation of peptides and proteins by the octadecylsilylated silica monolith of the above production have also been demonstrated.     

药物利多卡因分子印迹聚合物的制备及识别特性

利多卡因与甲基丙烯酸为功能单体分别在低温(0～4℃)紫外光照、加热条件下制备利多卡因分子印迹聚合物,实验结果通过Scatchard方程分析可知,低温紫外光照下制备的利多卡因MIP对利多卡因具有良好的选择性,并可进一步应用于临床利多卡因药物的分离富集和检测.     

Y2O2S:Sm3+发光材料在不同激发波长的浓度特征

研究了在不同激发波长下三价钐离子掺杂硫氧化钇的发光强度对浓度的依赖关系。研究发现磷光体的发光强度不仅跟激活离子的浓度有关,而且跟激发时所采用的不同激发波长有关。磷光体发光强度与激活剂掺杂量的变化曲线表明,在不同激发路径下磷光体具有不同的发光性质。采用Sm^3 离子直接跃迁的413nm对样品进行激发时,发生猝灭的浓度低至约0．2mol％;当采用263nm高能紫外线激发时,浓度猝灭发生在较高浓度处(～2mol％),后者是前者的10倍。对Sm^3 离子发射强度与浓度关系曲线进行了拟合计算,结果表明Sm^3 在Y2O2S中浓度猝灭的原因主要是相邻中心的偶极-四极相互作用引起的交叉弛豫。     

ZnO纳米线场效应管的制备及I-V特性研究

采用静电探针和原子力探针技术,将化学气相沉积工艺制备的,长度为30-200μm,直径80-750 nm的单根半导体ZnO纳米线搭接在Au,Zn,Al不同功函的金属隔离沟道两端,构建出了最基本的ZnO纳米线绝缘栅场效应管.研究了沟道类型、纳米线直径、退火温度和外加栅压对ZnO纳米线场效应管I-V特性的影响.利用半导体与金属材料的肖特基接触、欧姆接触的产生机理及电子输运理论,对结果进行了分析和讨论.     

H2-broadening,shifting and mixing coefficients of the doublets in the ν2 and ν4 bands of PH3 at room temperature

The broadening, shifting and mixing coefficients of the doublet spectral lines in the ν₂ and ν₄ bands of PH₃ perturbed by H₂ have been determined at room temperature. Indeed, the collisional spectroscopic parameters: intensities, line widths, line shifts and line mixing parameters, are all grouped together in the collisional relaxation matrix. To analyse the collisional process and physical effects on spectra of phosphine (PH₃), we have used the measurements carried out using a tunable diode-laser spectrometer in the ν₂ and ν₄ bands of PH₃ perturbed by hydrogen (H₂) at room temperature. The recorded spectra are fitted by the Voigt profile and the speed-dependent uncorrelated hard collision model of Rautian and Sobelman. These profiles are developed in the studies of isolated lines and are modified to account for the line mixing effects in the overlapping lines. The line widths, line shifts and line mixing parameters are given for six A₁ and A₂ doublet lines with quantum numbers K = 3n,?(n = 1,?2, …) and overlapped by collisional broadening at pressures of less than 50 mbar.     

铜(l)与N一亚水杨基苯丙氨酸席夫碱和二胺类混配配合物的合成与表征

合成了N一亚水杨基苯丙氨酸席夫碱(L)及其与Cu(,)和二胺(邻苯二胺,L,s2,2‘一联P比吮,Lzs1,10一邻非罗啦,L,和2,2'一联哇嘛,L,)的四种三元混配配合物,用元素分析、摩尔电导、红外和紫外光谱,差热和热重分析等方法对配合物的性质进行了表征     

酸性水稻土有效态砷与糙米砷含量相关性的研究

为了更好地探究酸性水稻土中有效态砷和糙米砷含量的相关性,采用土液比1:10、振荡时间240 min和振荡速度200 r·min-1为中间条件,比较4种浸提剂0.01 mol·L-1 CaCl2-DTPA,0.5 mol·L-1 NaHCO3,0.05 mol·L-1 NH4H2PO4和0.43 mol·L-1 HNO3提取酸性水稻土中有效砷的提取效果。结果表明,4种浸提剂提取的土壤有效态砷与其糙米砷含量之间均存在显著相关,0.43 mol·L-1 HNO3提取的土壤有效态砷与糙米砷含量的相关性最高为0.828,土壤有效态砷平均提取率最高为8.63。选择0.43 mol·L-1 HNO3为提取酸性水稻土有效态砷的最优浸提剂,进一步优化浸提剂的提取条件,确定土液比1:10、振荡时间120 min和振荡速度200 r·min-1为酸性水稻土有效态砷最佳提取条件,土壤有效态砷与糙米砷含量的相关性最高为0.831。0.43 mol·L-1 HNO3提取酸性水稻土中有效砷的方法操作简便、试剂用量少,提取的土壤有效砷和糙米砷的相关性好,确定为酸性水稻土有效态砷的提取方法,为科学评价酸性水稻土壤有效态砷与糙米砷的生物有效性以及酸性水稻土壤砷环境风险评价提供参考依据。     

可见光协同钴铈铁氧体高效活化过一硫酸盐降解噻虫胺

本实验采用溶胶-凝胶燃烧的方法,将Co掺入到CeFeO3（CFO）钙钛矿晶格中制备了具有晶格缺陷的CeFe0.8Co0.2O3（CFCO）纳米颗粒催化剂。通过扫描电镜（SEM）、透射电镜（TEM）、X射线衍射（XRD）、Ｘ射线光电子能谱（XPS）等表征技术对CFCO催化剂进行表征分析,结果表明在CFCO上形成了表面氧空位（VO）。同时,还研究了过硫酸氢钾（PMS）用量、不同pH值对CFCO降解噻虫胺（CTD）的影响。结果表明,在CFCO投加量为0.6 g?L-1,PMS用量为0.8 mmol?L-1,pH为7时,20 mg?L-1的噻虫胺在30分钟内完全降解。并且经过4次循环使用后,噻虫胺降解率仍能达到91.2%。CFCO对于PMS的高效活化能力,主要归功于晶格缺陷所产生的电位差促使自由电子顺着氧空位快速定向传导到PMS上。为了模拟在天然水体环境中CFCO光催化活化PMS去除CTD,进行阴离子和有机酸的对比实验,分析了不同环境因素对CFCO降解噻虫胺的影响;此外,本文通过自由基淬灭实验与电子自旋共振（ESR）检测确定了CFCO光催化活化PMS降解噻虫胺实验中起主要作用的活性物种为单线态氧（1O2）与羟基自由基（?OH）,并分析推测了自由基的产生机理。最后采用高效液相色谱-质谱联用仪（LC-MS）检测分析了CTD降解过程中可能产生的代谢产物,并基于代谢产物的产生顺序归纳出了三条可能的降解路径。     

圆形可倾瓦推力轴承入油边界条件的确定

采用有限元法对Reynolds方程、能量方程及弹性方程进行了联立求解,通过计算瓦边法向平均速度,较精确地确定了瓦的入油边界条件,从而更精确地计算出圆形瓦的压力分布及温度分布,通过轴承试验台试验发现,计算结果和实验结果较吻合。