Low-temperature electrothermal vaporization of thenoyltrifluoroacetone complex of Sc(III) and Y(III) for sample introduction in an inductively coupled plasma atomic emission spectrometry,and their determination in biological samples

A new method for inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of trace Sc and Y, based on gaseous compound introduction into the plasma as their thenoyltrifluoroacetone (TTA) complexes by electrothermal vaporization was developed. Using the reagent TTA as chemical modifier can not only enhance the analytical signals, but also reduce the vaporization temperature. At a temperature of 1,000 °C the trace Sc and Y can be vaporized completely into ICP. The factors affecting the formation of the chelate and its vaporization behavior, such as drying time, vaporization temperature/time, reaction medium and the amount of TTA, were investigated in detail. Under the optimized conditions (drying temperature/time 100 °C/10 s, vaporization temperature/time 1,000 °C/4 s), the limits of detection for Sc and Y were 19 pg and 34 pg (3), respectively, and the relative standard deviations for Sc and Y were 4.2% (c _Sc=0.2 g mL^–1; n=7) and 2.6% (c _Y=0.5 g mL^–1; n=7). The linear ranges of the calibration graphs cover three orders of magnitude. The method was applied to the analysis of the biological reference materials (GBW 07602, bush branches and leaves; GBW 07604, poplar leaves), and the results obtained were in good agreement with the certified values.     

Microfluidics: from dynamic lattices to periodic arrays of polymer disks

We used coupling of flow and geometric confinement to assemble emulsion droplets in two-dimensional gliding lattices with a high degree of order and symmetry. Highly monodisperse discoid droplets with circular shapes were generated in a microfluidic flow-focusing device. Originally, close-packed lattices formed from these circular discoid droplets. Progressive confinement led to the gradual deformation of the circular disks: first, they elongated in the direction parallel to the direction of flow and then transformed into hexagons. Assembly driven by the combination of flow and confinement also allowed for the formation of lattices from droplets with a bimodal size distribution. We used photopolymerization of the monomer droplets to trap the lattice structure in the solid state and produce highly periodic arrays of solid polymer disks.     

Sequential C–O decarboxylative vinylation/C–H arylation of cyclic oxalates via a nickel-catalyzed multicomponent radical cascade

A selective, sequential C–O decarboxylative vinylation/C–H arylation of cyclic alcohol derivatives enabled by visible-light photoredox/nickel dual catalysis is described. This protocol utilizes a multicomponent radical cascade process, i.e. decarboxylative vinylation/1,5-HAT/aryl cross-coupling, to achieve efficient, site-selective dual-functionalization of saturated cyclic hydrocarbons in one single operation. This synergistic protocol provides straightforward access to sp³-enriched scaffolds and an alternative retrosynthetic disconnection to diversely functionalized saturated ring systems from the simple starting materials.

A selective, sequential C–O decarboxylative vinylation/C–H arylation of cyclic alcohol derivatives enabled by visible-light photoredox/nickel dual catalysis has been described.     

Polymer microgels: reactors for semiconductor, metal, and magnetic nanoparticles

We report a strategy for the production of materials with structural hierarchy. The approach employs polymer microgels as templates for the synthesis of semiconductor, metal, or magnetic nanoparticles (NPs). We show that NPs with predetermined dimensions and size-dependent properties can be synthesized by using a very delicate balance between the reaction conditions, the composition and the structure of microgel templates, and the concentration of NPs in the microgel. Postheat treatment of microgels doped with semiconductor nanoparticles reduces NP polydispersity and allows control of their photoluminescence. Microgel templates are particularly beneficial in the synthesis of polymer microspheres heavily loaded with monodisperse superparamagnetic Fe(3)O(4) NPs. Hybrid submicrometer-size microgels have promising potential applications in photonics, catalysis, and separation technologies.     

Sulfonylation from sodium dithionite or thiourea dioxide

The cheap and easily available sodium dithionite and thiourea dioxide have been used as the source of sulfonyl group in the synthesis of sulfones and sulfonamides recently.Compared with other methods for the sulfonylation reactions,the strategies using sodium dithionite or thiourea dioxide provide an alternative and complementary route to diverse sulfonyl compounds.During the reaction process,sulfur dioxide anion radical is the key intermediate,which is usually generated from a single electron transfer under suitable conditions.The advantages using sodium dithionite or thiourea dioxide in the sulfonylation reactions include mild conditions and broad substrate scope with excellent functional group compatibility.Further applications by using sodium dithionite and thiourea dioxide in organic transformations will be anticipated.     

Low-density extraction solvent-based solvent terminated dispersive liquid–liquid microextraction combined with gas chromatography-tandem mass spectrometry for the determination of carbamate pesticides in water samples

A simple and fast method of low-density extraction solvent-based solvent terminated dispersive liquid–liquid microextraction (ST-DLLME) was developed for the highly sensitive determination of carbamate pesticides in the water samples by gas chromatography-tandem mass spectrometry (GC-MSMS). After dispersing, the obtained emulsion cleared into two phases quickly when an aliquot of acetonitrile was introduced as a chemical demulsifier into the aqueous bulk. Therefore, the developed procedure does not need centrifugation to achieve phase separation. It was convenient for the usage of low-density extraction solvents in DLLME. Under the optimized conditions, the limits of detection for all target carbamate pesticides were in range of 0.001–0.50 ng mL⁻¹ and the precisions were in the range of 2.3–6.8% (RSDs, 2 ng mL⁻¹, n = 5). The proposed method has been successfully applied to the analysis of real water samples and good spiked recoveries over the range of 94.5–104% were obtained.     

谈物理教学中培养学生画图处理问题的习惯

1图形在物理学习中的重要性 心理学研究表明,人的大脑对通过不同渠道对知识的吸收比例是大不相同的:视觉83%、听觉11%、嗅觉3.5%、味觉1%、触觉1.5%.因而可以说,大脑中储存的知识,极大多数是通过视觉和听觉获得的,与视觉有关的"图形信息"占绝对高的比例,物理知识更是如此.     

纳米钯膜电极的制备、结构表征和特殊反应性能

用循环伏安方法制备纳米钯膜电极,运用扫描隧道显微镜和原位红外光谱等方法研究其结构和反应性能.STM图像表明,制备的纳米钯膜具有特殊的层状结构,纳米级厚度的层状晶体由直径6nm左右的Pd微晶聚集而成.发现当钯膜厚度为几个纳米时,CO的吸附表现出异常红外效应,即红外谱峰反向和红外吸收显著增强(增强因子可达42.6).纳米钯膜电极对氢的反应也具有特殊的性能,与氢向钯晶格扩散吸收过程相比较,氢吸脱附的表面过程成为主要反应.研究结果还指出,纳米钯膜电极的异常红外效应和对氢反应的特殊性能与钯膜厚度密切关联,并可归结为钯膜材料的纳米尺度效应.     

基于聚类NASVD的CE2-GRS月表放射性元素Th计数率分布

月表Th 元素分布特征对于分析月表岩石成因及化学特征等提供了重要依据。为了减小嫦娥二号伽玛谱(CE2-GRS) 噪声对获取Th 元素分布特征的影响,提出了一种基于噪声调整的奇异值分解(NASVD) 去噪算法。通过伽玛谱预处理、去噪、本底扣除及净峰面积求解等步骤,获得月表放射性元素Th计数率全月分布图。通过与国内外其他方法所获得的Th 元素计数率分布图对比有较高的一致性。与传统伽玛谱去噪算法比较,聚类NASVD算法能有效地去除统计涨落噪声影响,提取出嫦娥二号伽玛谱中的特征峰信息。The distribution of thorium on the lunar surface provides the important evidence for lunar evolution history. It is difficult to obtain the distribution of thorium on the lunar surface from CE2-GRS because of noise in the spectrum. The method for smoothing the spectrum is proposed which is based on cluster NASVD. The counting rate map of thorium on the lunar surface is achieved from CE2-GRS. Counting rate map of thorium gamma-rays shows a surface thorium distribution that is in general agreement with other measurement from LP-GRS and SLENE GRS which have better accuracy. It is more effectively to reduce the noise and get the weak information of characteristic peak used the method of cluster NASVD than other traditional methods for smoothing gamma-ray spectrum.     

原位微区X射线荧光分析在矿物学研究中的应用

从新疆采集了13件岩矿石样品,用于研究蚀变过程中矿物的元素含量变化特征。成都理工大学研制的IED-6000型原位微区X射线荧光分析仪被应用于获得蚀变过程中矿物的化学和物理数据。这种无损的微区X射线荧光分析仪主要是以低功耗X光管和电致冷Si-PIN半导体探测器为基础,采用毛细管X射线透镜实现微区测量的功能,并且能够集成到任何显微镜上进行测量,焦斑长轴直径约110 μm。通过微区X射线荧光测量,将黝铜矿更正为黄铁矿,提高了矿物鉴定的效率及准确性;在蚀变剖面研究中,矿化岩石样品的长石颗粒都富含Cu和Zn元素,可以作为找矿直接指示元素。Cr,Mn和Co等元素含量与矿化程度呈负相关。