硼离子对铕掺杂SiO2干凝胶发光性能的影响

采用溶胶-凝胶法制备了Al单掺和B，Al共掺的Eu掺杂SiO2干凝胶。利用荧光光谱、IR，XRD，DSC，TG／DTG等技术研究了硼离子、退火温度对样品发光性质的影响。经500℃以上退火处理用248nm激发的样品，产生Eu^3＋离子^5D0→^7FJ的特征发射，^5D0→^7F1的跃迁分裂为两个峰。比较615nm处的发光强度，掺硼酸样品的发光强度是不加硼酸发光强度的3．3倍。这是因为B离子的加入，在材料中形成了Si—O—B键，破坏了网络的对称性，加强了Eu^3＋的红光发射。当退火温度上升到850℃用350nm激发时，样品有很强的Eu^2＋蓝光发射。Al单掺的发射中心在437nm处，发射半峰宽约为70nm，而B，Al共掺样品的发光中心蓝移到425nm处，单掺样品的蓝光强度几乎是共掺样品强度的2倍。这是由于硼酸的加入改变了基质的网络结构，从而导致单掺和共掺样品发射峰位和强度的改变。     

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.     

高效液相色谱法检测保健食品中大豆异黄酮含量

建立了保健食品中大豆异黄酮的高效液相色谱检测方法 ,通过正交试验法得出保健食品中大豆异黄酮的最佳水解条件为 :盐酸浓度2.0mol/L,酸体积40mL ,水解温度80℃ ,水解时间3h;采用HypersilODS2C18 色谱柱 (250mm×4.6mmID ,5μm) ,流动相为甲醇 -水(体积比47∶53) ,流速1.0mL/min ,检测波长260nm ,柱温40℃ ,线性范围在0.5～96mg/L ,相关系数r为0.999 ,相对标准偏差 (RSD)2.09% ,回收率在98.5 %～100.5 %。     

镨、钕、钇、甘氨酸三元配合物的晶体结构

在水溶液中培养了镨、钕、钇与甘氨酸形成的三元配合物。元素分析和热分析表明，该配合物可用Ｐｒ_ｘＮｄ_ｙＹ_ｚ（Ｇｌｙ）_６（Ｈ_２Ｏ）_４（ＣｌＯ_４）_６·５Ｈ_２Ｏ（Ｘ＋ｙ＋ｚ＝２）表示其分子式。Ｘ射线衍射方法测定了其单晶结构，结果表明，该晶体属三斜晶系，空间群Ｐ１，化学式Ｐｒ_（０．７７５）Ｎｄ_（０．７００）Ｙ_（０．５２５）Ｃｌ_６Ｏ_（４５）Ｎ_６Ｃ_（１２）Ｈ_（４８），Ｍ_ｒ＝１４６６．０９，晶胞参数如下：ａ＝１１．５６４（１），ｂ＝１４．１１８（３），ｃ＝１５．６６８（２）Ａ，α＝９６．９９（１），β＝１０２．７２（１），γ＝１０５．３３（１）°，晶胞体积Ｖ＝２３６２（１）Ａ~３，Ｚ＝２，Ｄ_ｃ＝２．０６０ｇ／ｃｍ~３，结构偏离因子Ｒ＝０．０３２，Ｒ_ｗ＝０．０４８。晶胞中存在两个络合单元，每个单元可用Ｍ_１Ｍ２（Ｇｌｙ）_６（ＣｌＯ_４）_６（Ｈ_２Ｏ）_４．５Ｈ_２Ｏ表示，Ｍ_１＝０．４Ｐｒ＋０．３７５Ｎｄ＋０．２２５Ｙ，Ｍ２＝０．３７５Ｐｒ＋０．３２５Ｎｄ＋０．３０Ｙ。三种稀土元素按一定比例统计性地占有两个格位。羧基以桥式联结金属离子，形成一维链式聚合物结构。在络合单元中，一个稀土离子是９配位，其配位多面体为畸变?     

电极材料对NPB/Alq3有机电致发光器件性能的影响

采用不同材料作为有机电致发光器件(OELDs)的电极, 制备了基本结构为[阳极/NPB(40 nm)]/Alq3(50 nm)/阴极]的异质结双层器件, 并通过改变OELDs器件的阴极或阳极来研究电极材料对器件光电性能的影响. 研究结果表明, 各器件电流-电压(I-V)关系的基本特征与陷阱电荷限制电流(TCLC)机制的拟合情况相符. 由于有机材料本身能级的无序性以及载流子迁移率对温度和电场的依赖性, 不同电极的载流子注入能力与其功函数并无直接关系. 双层器件中由于空穴传输层的引入, 使得载流子复合区域位于有机层异质结界面处, 降低了金属阴极对激子的猝灭作用, 从而大大提高了器件性能. 此外, 金属电极OLEDs器件结构具有的微腔效应会导致发射光谱的位移和谱峰宽度变窄, 这表明通过对金属电极的表面改性和优化可使器件性能超过常规结构的器件.     

Novel CaCO3/g-C3N4 composites with enhanced charge separation and photocatalytic activity

A novel CaCO₃/graphitic carbon nitride (g-C₃N₄) photocatalyst was synthesized for the first time via a facile calcination method using CaCO₃ and melamine as precursors. The as-prepared samples were characterized using various techniques, such as scanning and transmission electron microscopy, X-ray diffraction, Brunauer-Emmett-Teller analysis, as well as Fourier-transform infrared, X-ray photoelectron, photoluminescence, and UV–vis diffuse reflectance spectroscopy. The results of the experiments confirm the successful coupling of CaCO₃ to g-C₃N₄. The photocatalytic activity of the synthesized CaCO₃/g-C₃N₄ composites was evaluated by assessing their performance in the photocatalytic degradation of crystal violet (CV) in water under visible light irradiation. The analysis shows that CaCO₃/g-C₃N₄ exhibits higher photocatalytic activity towards CV degradation (76.0%) than pristine g-C₃N₄ (21.6%) and CaCO₃ (23.2%). Radical trapping and electron spin resonance experiments show that hydroxyl radicals (OH) and holes (h⁺) are the key reactive species in the photocatalytic process. The enhanced photocatalytic activity of the composite is mainly attributed to the efficient separation rate of electron-hole pairs achieved through the incorporation of CaCO₃.     

四(三苯基氧膦)高氯酸钕合乙醇配合物的合成及结构测定

合成了Nd(ClO_4)_3·4phP=O·C_2H_5OH配合物,用四园衍射仪测定了它的分子及晶体结构,此晶体属三斜晶系P1空间群,晶胞参数为:a=13.475(61)A;b=15.003(15)A;c=18.697(15)A;α=85.44(7);β=78.49(24)°;γ=83.13(26)°;V=3671.2A,分子由99个非氢原子组成,实际上分子可分为三个部分即:配阳离子[Nd(ClO_4)_2·4phPO]~+;阴离子ClO_4和溶剂合分子C_2H_5OH配阳离子的钕与八个氧配位,四个氧来自双齿配位的ClO_4,四个氧来自四个ph_3PO,八个配位氧组成三角十二面体。 中性膦(磷)类化合物包括(RO)_3P=O和R_3P=O是一类重要的萃取剂。工业上已应用的TBP和TOPO都属于这一类。为了研究这类萃取剂在不同底液中萃取行为之所以不同的内在因素,我们制备了不同希土盐类与三苯基氧膦的配合物,并对它们进行了结构测定。已知的中性氧膦希土配合物中进行过结构测定的有Ce(NO)·2phP=O、Nd(NO)_2·2php=O·C_2HOH、La(NO_3)_3·3php=O·C_2H_5OH·CHCl_3和Nd(NCS)·4php=O。这些配合物晶体及分子结构各异,这表明了三苯基氧膦在形成配合物时的复杂性。本文报导的Nd(ClO_4)·4phP=O·C_2H_5OH实际上是由三部分组成;即[Nd(ClO_4)_2·4phP=O]~+外界的ClO_4和溶剂合分子。这在中性配体与高氯酸希土形成的配合物中时有发现。已知结构的     

2020 Roadmap on two-dimensional nanomaterials for environmental catalysis

This roadmap demonstrates a series of two-dimensional nanomaterials, such as graphene, black phosphorus, oxides, layered double hydroxides, chalcogenides, bismuth-based layered compounds, MXenes, metal organic frameworks, covalent organic frameworks, and others, for environmental catalysis.     

An unmediated hydrogen peroxide biosensor based on hemoglobin incorporated in a montmorillonite membrane

Hemoglobin was incorporated in a montmorillonite membrane. Electrochemical and spectroscopic studies revealed that the electron transfer reactivity and peroxidase activity of the protein were both enhanced. Nevertheless, its structure was still maintained native-like in the membrane. An unmediated hydrogen peroxide biosensor was accordingly prepared. The calibration plot of this H202 sensor was linear in the range of 1.0 x 10(-6)-6.0 x 10(-4) mol L(-1). The relative standard deviation was 3.1% for six successive determinations at a concentration of 1.0 x 10(-4) mol L(-1). The detection limit was 6.0 x 10(-7) mol L(-1). Possible interferences in real sample analyses are discussed.     

Titanium(IV) isopropoxide mediated solution phase reductive amination on an automated platform: application in the generation of urea and amide libraries

Amine libraries and their derivatives are important targets for high throughput synthesis because of their versatility as medicinal agents and agrochemicals. As a part of our efforts towards automated chemical library synthesis, a titanium(IV) isopropoxide mediated solution phase reductive amination protocol was successfully translated to automation on the Trident(TM) library synthesizer of Argonaut Technologies. An array of 24 secondary amines was prepared in high yield and purity from 4 primary amines and 6 carbonyl compounds. These secondary amines were further utilized in a split synthesis to generate libraries of ureas, amides and sulfonamides in solution phase on the Trident(TM). The automated runs included 192 reactions to synthesize 96 ureas in duplicate and 96 reactions to synthesize 48 amides and 48 sulfonamides. A number of polymer-assisted solution phase protocols were employed for parallel work-up and purification of the products in each step.