湿法消解-原子荧光法测定全血中硒

以全血样品为原料,探讨湿法消解-原子荧光法测定全血中的硒含量。血样经硝酸-高氯酸消解后,用硼氢化钠将硒还原成硒化氢,由氩气载入原子化器,产生的原子荧光强度与试液中硒元素含量在一定范围内呈正比,外标法定量。以消解效率为指标,优化样品的消解条件,测定血中硒在0-10μg/L范围内线性情况良好,相关系数为0.9992,最低检出限为0.143μg/L,相对标准偏差为1.51%-1.58%,平均加标回收率为90.86%-104.62%。血中硒的原子荧光测定法灵敏度高,精密度和稳定性好,可应用于血中硒的生物监测。     

An AIE-Active probe for detection and bioimaging of pH values based on lactone hydrolysis reaction

Cellular pH homeostasis is essential for many physiological and pathological processes. pH monitoring is helpful for the diagnosis, treatment and prevention of disorders and diseases. Herein, we developed a ratiometric fluorescent pH probe (TCC) based on a coumarin derivative containing a highly active lactone ring. TCC exhibited a typical AIE effect and emitted blue fluorescence under weak acidic condition. When under weak basic condition, the active lactone moiety underwent a hydrolysis reaction to afford a water-soluble product, which gave red-shifted emission. The emission color change from blue through cyan and then to yellow within pH 6.5–9.0 which is approximate to the biological pH range. And the fluorescence color change along with pH value is reversible. Furthermore, TCC was successfully utilized in the detection of the intracellular pH change of live HeLa cells, which indicated that TCC had practical potential in biomedical research.

     

中空介孔SiO2纳米球的制备、改性及其对Al3+荧光识别研究

中空介孔SiO2由于中空多孔的结构而常用作功能材料的基底.将中空介孔SiO2进行官能团修饰,并应用为荧光传感材料是中空介孔SiO2一个重要的研究领域.本论文采用聚丙烯酸(PAA)为中空模板,聚醚F127为造孔剂,正硅酸乙酯(TEOS)为硅源,氨水为催化剂在乙醇体系中制备了中空介孔SiO2纳米球.系统研究了搅拌速度和聚醚F127引入量对中空介孔SiO2纳米球形貌及比表面积的影响.通过透射电镜、N2-等温吸附脱附曲线等表征说明该合成方法具有很好的普适性,通过调节F127的引入可以实现对比表面积的有效控制.通过氨基化、席夫碱反应进行荧光修饰,进一步研究表明荧光修饰后的中空介孔SiO2纳米球在水溶液中能够实现对Al3+的有效检测,检测限为1.19×10 -7M.     

烧结温度对Cao.9(NaCe)0.05Bi2Nb2O9无铅压电陶瓷性能的影响

采用传统固相反应法制备了Ca0.9(NaCe)0.05Bi2 Nb2 O9铋层状无铅压电陶瓷.采用XRD、SEM、EDS及相关电学性能测试系统表征了样品的晶体结构、断面形貌、元素组成以及介电、压电、铁电等性能,探究不同烧结温度对于陶瓷性能的影响.结果表明:当烧结温度为1150℃时,样品的晶体结构单一均匀,呈现片层状结构,致密性较好,压电常数高达17 pC/N,介电损耗仅为0.42;,居里温度为908℃,并且具有很好的温度稳定性,说明固相反应法制备的Ca0.9(NaCe)0.05Bi2Nb2O9压电陶瓷最佳烧结温度为1150℃.     

基于响应面法的直拉硅单晶生长工艺参数优化方法

在直拉法制备硅单晶的过程中,要得到优质的晶体必须建立合理的温度分布,而单晶炉内热场的分布与工艺参数的设定密切相关.其中以晶体转速、坩埚转速和拉速等三个工艺参数对热场分布的影响尤为显著.为了确定最佳热场分布下晶转、埚转及拉速的设定值,本文采用响应面算法通过方程拟合、回归分析等步骤求解这三个工艺参量与温度梯度之间的最佳函数模型,并在该模型下同时对这三个工艺参量进行优化分析,且通过仿真实验和拉晶实验表明该方法的有效性.     

Investigation of mononuclear,dinuclear, and trinuclear transition metal (II) complexes derived from an asymmetric Salamo‐based ligand possessing three different coordination modes

A new asymmetric Salamo‐based ligand H₂L was synthesized using 3‐tert‐butyl‐salicylaldehyde and 6‐methoxy‐2‐[O‐(1‐ethyloxyamide)]‐oxime‐1‐phenol. By adjusting the ratio of the ligand H₂L and Cu (II), Co (II), and Ni (II) ions, mononuclear, dinuclear, and trinuclear transition metal (II) complexes, [Cu(L)], [{Co(L)}₂], and [{Ni(L)(CH₃COO)(CH₃CH₂OH)}₂Ni] with the ligand H₂L possessing completely different coordination modes were obtained, respectively. The optical spectra of ligand H₂L and its Cu (II), Co (II) and Ni (II) complexes were investigated. The Cu (II) complex is a mononuclear structure, and the Cu (II) atom is tetracoordinated to form a planar quadrilateral structure. The Co (II) complex is dinuclear, and the two Co (II) atoms are pentacoordinated and have coordination geometries of distorted triangular bipyramid. The Ni (II) complex is a trinuclear structure, and the terminal and central Ni (II) atoms are all hexacoordinated, forming distorted octahedral geometries. Furthermore, optical properties including UV–Vis, IR, and fluorescence of the Cu (II), Co (II), and Ni (II) complexes were investigated. Finally, the antibacterial activities of the Cu (II), Co (II), and Ni (II) complexes were explored. According to the experimental results, the inhibitory effect was found to be enhanced with increasing concentrations of the Cu (II), Co (II), and Ni (II) complexes.     

细胞松弛素B阻断微核法鉴定男性个体辐射敏感性的方法初探

初步研究了男性个体辐射敏感性的鉴定方法及标准。采集50名男性志愿者的外周血，分别给予不同剂量X射线照射，采用细胞松弛素B阻断双核法测定微核率(MNF)，通过二阶多项拟合法，绘制微核剂量效应选项中心标准曲线，将个人微核剂量效应曲线与标准曲线比对后判断个体辐射敏感性。 $0.0\sim2.5 $ Gy剂量范围内，剂量效应二阶多项拟合的中心方程为(MNF=0.014 7+0.036 2D+0.023 1D 2， r=0.726)。50名志愿者中，辐射敏感的有13人，辐射抗性的有14人，基本符合正态分布。Spearman秩和相关分析结果显示，MNF在各个辐射剂量点与辐射敏感性均存在正相关,与辐射抗性呈负相关,MNF随剂量增加而增加。本研究初步建立了“以线代点”男性个体辐射敏感性鉴定方法,并发现男性外周血淋巴细胞的本底微核率与个体辐射敏感性呈正相关。     

磁场下有原子自旋轨道耦合的各向异性量子点的精确解析传播子

量子力学中很少有系统能够精确地计算传播子, 特别是在考虑了自旋轨道耦合效应的情况下. 利用相空间的群论方法, 首先导出了有原子自旋轨道耦合的各向异性量子点传播子的精确解析表达式. 随后利用传播子来计算自旋高斯波包的演化与相应的概率密度, 并研究了原子自旋轨道耦合效应和磁场强度对距离期望值的影响.     

自由基浓度测定方法的再验证及其在煤化学中应用

对前人建立的标准曲线法测煤中自由基浓度进行优化,以DPPH标准样品和基准样品的二次积分面积比值为新参数,结果显示新参数标准曲线法的实测值与理论值相对误差都在5%以内;重复性、复现性实验的相对标准偏差都小于3%。将新参数标准曲线法用于分析不同煤化程度煤和新疆黑山煤(HS)沥青质的自由基浓度,发现随着煤化程度增加,其煤中自由基浓度逐渐增大,从低阶褐煤的8.531×10~(17)/g上升到高阶无烟煤3.37899×10~(19)/g;而在HS煤液化过程中,随着加氢液化温度的升高,其沥青质自由基浓度逐渐下降,从290℃的1.5793×10~(18)/g降到450℃的7.410×10~(17)/g,沥青质自由基浓度变化趋势与其产率变化趋势相一致。