超声辅助浊点萃取-原子荧光光谱法测定水中痕量汞

为了适应水中痕量汞的分析要求,降低汞的检出限,建立了一种超声辅助浊点萃取预富集联合原子荧光光谱法测定水样中痕量汞的方法。该方法采用硫代米氏酮为络合剂,以非离子型表面活性剂Triton X-114为萃取剂,将水样中的痕量汞富集于表面活性剂相。在原子荧光光谱分析前,加入磷酸三丁酯作为消泡剂,用5%盐酸溶液定容,富集倍数可以达到10倍。优化萃取体系pH、络合剂用量、萃取剂用量、超声平衡条件等浊点萃取的条件,在最优条件下,该方法检出限为0.003 μg/L,相对标准偏差为4.2%~8.6%,加标回收率为85%~106%。结果表明,超声辅助浊点萃取-原子荧光法能够适用于对地表水、自来水等清洁水样中痕量汞的分析,且具有更低的检出限,良好的准确度和精密度,能够适应于更高的样品分析要求。     

Acyl-lithiation of olefins: formation of cyclopentenones from 1-lithio-butadienes and CO

[reaction: see text] Intramolecular acyl-lithiation of C=C double bonds proceeds following carbonylation of 1-lithio-1,3-dienes with CO to afford 2- or 3-cyclopentenone derivatives in good to excellent yields after hydrolysis. Addition of electrophiles to the carbonylation reaction mixtures affords various multiply substituted cyclopentenones.     

序约束下多元正态均值的检验问题

设有k组均值有简单半序约束,协方差阵未知的p维正态分布．Sasabuchi等在2003年研究了均值是否相等的检验问题．考虑到似然比检验统计量的临界点难以获得,以致于它不容易实施,Sasabuchi提出了一个检验方法．称为Sasabuchi检验．Sasabuchi检验的一个不足之处在于,它并不优于经典的MANOVA检验．作者提出了一个新的检验方法,它比Sasabuchi检验有一致优的势,而且形式更为简单．通过模拟发现这个检验方法还优势于MANOVA．最后导出了这个检验统计量的渐近零分布．     

Intrinsically stable phase-modulated polarization encoding system for quantum key distribution

We demonstrate experimentally an intrinsically stable polarization coding and decoding system composed of optical-fiber Sagnac interferometers with integrated phase modulators for quantum key distribution. An interference visibility of 98.35% can be kept longtime during the experiment without any efforts of active compensation for coding all four desired polarization states.     

Novel cycloaddition of nitriles with monolithio- and dilithiobutadienes

Two novel and synthetically useful reaction patterns of organolithium compounds with nitriles are reported to afford pyridine derivatives as the final products. Both 1-lithio-1,3-dienes and 1,4-dilithio-1,3-dienes, which can be easily generated in situ by lithiation of their corresponding iodo compounds, react with nitriles in the presence of HMPA to form substituted pyridines including 2,2'-bipyridines and tetrahydroisoquinolines in high yields.     

Electrochemical in-vivo sensors using nanomaterials made from carbon species,noble metals,or semiconductors

Electrochemical analytical methods have the advantages of simplicity, direct measurements, and ease of miniaturization which pave the way for real time detection and sensing. However, the complexity of living systems usually requires electrochemical sensors to display high selectivity, sensitivity, accuracy, biocompatibility and stability over time. Nanomaterials possess attractive properties in terms of surface modification, catalysis, and functionality. These open new avenues with respect to electrochemical enzymatic determination of neurochemicals such as dopamine, serotonin and ascorbate, biological small molecules such as H₂O₂ and metal ions such as copper(II) in-vivo. Three properties of nanomaterials make their use particularly attractive, namely the larger surface-to-volume ratio area, their unique surface, and the ease of electron transfer between enzymes and electrodes. These properties make them more sensitive, selective and stable. The article is subdivided into sections that cover applications of the following materials: carbonaceous materials (mainly carbon nanotube), noble metal particles (mainly gold and platinum particles), and semiconductor (mainly metal oxide) nanomaterials. A conclusion and outlook section addresses current chances and limitations. The review contains 99 references. Figure

Three attractive properties of nanomaterials: the larger surface-to-volume ratio area, unique surface, and facilitating the electron transfer between enzyme and electrode, can improve the analytical performance of electrode, fulfilling the requirements in sensitivity, selectivity and stability for in vivo electrochemistry.     

纳米级SnO2或Yb2O3对熔融石英陶瓷析晶性能的影响

通过XRD分析和热膨胀率实验,从析晶角度探讨了添加纳米级SnO2或Yb2 O3对熔融石英陶瓷析晶性能的影响.结果表明:熔融石英陶瓷高温析晶的主要晶化产物为方石英,方石英析出量随烧结温度的提高而逐渐增多;纳米级SnO2或Yb2 O3的引入可通过抑制熔融石英中方石英的析出,有效地降低熔融石英材料在升温过程中的热膨胀率,并且...     

位置参数变点的非参数检验及其渐近性质

本文基于Ｕ－统计量,对于位置参数模型,讨论了位置参数变点的检验问题,给出了检验统计量并研究它的分市的极限性质,证明了检验统计量的极限分布是ｓｕｐ|Ｂ(ｔ)|,其中{Ｂ(ｔ),０＜ｔ＜１}是一个Ｂｒｏｗｎ桥．将此结果应用到了双参数指数分布和Ｗｅｉｂｕｌｌ分布尺度参数变点的检验问题中．