超声辅助乳化液液微萃取-气相色谱-质谱分析水中的人工合成麝香

将超声辅助乳化与液液微萃取技术结合,建立了水体中人工合成麝香的气相色谱-质谱分析方法.优化前处理条件,包括萃取剂、萃取剂体积、萃取时间、萃取温度及离子强度的选择.结果表明:在10 mL水样中,加入50 μL氯苯作为萃取剂,4 0 MHz超声10 min,混匀,以4000 r/min离心10 min,移取下层有机相进样分析,效果佳.样品的富集倍数可达200倍,8种人工合成麝香在0.005～0.4 μg/L范围内线性关系良好,相关系数均大于0.994;检出限为0.3～0.5 ng/L;水样中加标回收率为96.2％～102.9％;相对标准偏差为2.3％～4.1％.本方法灵敏、快速、准确,可满足环境水样中痕量人工合成麝香监测的质控要求.     

Unexpected ring contraction and oxidation rearrangement reactions of securinine

The bromination and oxidation of securinine were studied. An interesting and surprising rearrangement was observed during the reaction of securinine with tribromo-isocyanuric acid or 1,3-dibromo-5,5-dimethylhydantoin in methanol, yielding a stereoselective ring contraction norsecurinine derivative. Meanwhile two oxidation rearrangement products were also reported. Some preliminary discussions on the reactivity of securinine were conducted from these rearrangements; it is believed to be induced by alkaline nitrogen atom of the molecule.     

Molecular assembling using axial phenolate on an iron N-confused porphyrin complex

The reaction of sodium phenolate and Fe(HCTPPH)Br assembles a dimeric iron(III) complex with a channel-like solid state packing; the intramolecular iron-to-iron distance of 8.864 A is the longest among the available N-confused porphyrin dimeric complexes.     

固相反应法制备BaHfO3∶Ce纳米粒子及发光特性

通过固相反应法合成了BaHfO3:Ce纳米粒子.采用XRD、SEM等手段分析了粉体合成过程的物相变化及形貌特性:用荧光光度计分析了样品的激发和发射光谱.结果表明:混合粉体经1000℃煅烧2 h,合成出近似球形、分散性良好的BaHfO3:Ce纳米粒子.一次粒径约30 nm.掺杂少量Ce3+离子能引起基质BaHfO3的晶格畸变,并未改变立方晶系结构.BaHfO3:Ce样品的激发光谱由2个激发峰构成,峰值分别位于396和446nm处.396 nm波长激发的发射光谱主要由2个发光谱带组成,其峰值分别位于531和591 nm波长处,发光机制对应Ce3+的5d→2F5/2和5→2F7/2能级跃迁.用446 nm波长激发时,只有一个宽带发射峰,峰值位于593 nm处,而530 nm附近的峰已趋于平缓.当掺杂Ce3+u的物质的量分数为0.9%时,发射峰值达到最大;当Ce3+含量为1.1%时,导致发射峰值强度降低,这是由于Ce3+的浓度猝灭产生的.     

大蒜汁在油田腐蚀介质中的缓蚀作用

本文利用失重法研究了大蒜汁在“碳钢－盐酸”、“碳钢－油田注水”以及分别进行充CO2或H2S“碳钢－油田注水”体系中的缓蚀效果,通过扫描电镜形貌观察和电化学测试初步探讨了缓蚀作用机理。结果发现,大蒜汁在酸性溶液中具有良好的缓蚀效果,在80℃下的15%盐酸溶液中缓蚀效率最高可达95.4%,缓蚀率随着酸浓度的增加而逐渐降低。大蒜汁在三种油田注水中也有一定的缓蚀作用,缓蚀效率在42%到64%之间。采用大蒜缓蚀的金属表面覆盖有一层致密的薄膜,动电位极化测试显示为吸附成膜。     

海-气耦合动力系统的改进变分迭代解法

研究了一个描述厄尔尼诺和南方涛动振荡物理机理的海-气耦合动力系统.利用改进变分迭代方法 (MVIM)简捷地得到了该非线性模型近似解的展开式.通过与特殊情形下模型精确解的比较,说明获得的MVIM 近似解具有非常好的准确度.     

Photoluminescence study of Ce-doped silica films

Ce-doped silica films with different Ce concentrations were prepared by ion-beam sputtering and ion implantation. The films containing 1.2 at% Ce were annealed at temperatures from 500 °C to 1200 °C in air ambient, and were annealed in different ambient at 1100 °C. Ce-related photoluminescence was observed in films sensitive to the Ce concentrations, annealing temperatures and the annealing ambient. The peak intensity of the photoluminescence band is approximately linear with Ce concentrations. Also, the photoluminescence intensity is dependent on the annealing temperatures and reaches its highest value after annealing at 700 °C. In addition, the experimental results show that compared with the annealing in an air ambient, the photoluminescence intensity can be enhanced with nitrogen gas. There would be no obvious change for the photoluminescence position or shape.     

汽车贴膜透光率的测定和实用性分析

测量市面上的汽车贴膜对波长在200—1000nm范围的光线的透光率,根据贴膜商家提供的贴膜功能:隔紫外线、隔热和保护隐私,由所测数据和图表分析汽车贴膜的上述各项功能。     

Modified Approach for Calculating Four-Quark Condensates

By differentiating the dressed quark propagator with respect to a variable background field,the linear response of the dressed quark propagator in the presence of the background field can be obtained.From this general method,using the vector background field as an illustration,we extract a general formula for the four-quark condensate〈(0)|-q(0)γμq(0)-q(0)γμq(0)|0〉.This formula contains the corresponding fully dressed vector vertex. We use this formula to analyze the factorization problem of the four-quark condensate and show that in the bare vertex approximation factorization holds exactly.     

弱阳离子整体柱在线富集分析尿液中盐酸雷尼替丁

不锈钢柱管中自制弱阳离子交换整体柱作为固相萃取材料,对尿样中盐酸雷尼替丁进行富集分析。以2.5mmol/LK2HPO4缓冲液作为富集流动相,结合柱切换法实现在线富集药物的同时去除尿液中蛋白等内源性物质。色谱分离条件为:C18反相色谱柱,在流速为1.0mL/min,检测波长为320nm条件下,用CH3OH-2.5mmol/LK2HPO4(2:1,V/V)进行洗脱。实验结果表明,盐酸雷尼替丁在0.05～5.0mg/L浓度范围内线性关系良好(r=0.9994,n=7);绝对回收率在75.0%～85.0%之间;检出限为0.01mg/L;日内、日间精密度(RSD)均小于5.0%,能够满足分析测定要求。本方法避免了繁琐的样品预处理过程,且所制弱离子整体柱可多次重复使用,为生物样品中痕量药物检测提供了一种快速、经济和有效的新方法。