药用中间体苯丙酮含量的气相色谱/质谱分析

苯丙酮是合成利胆药苯丙醇的重要中间体。本文建立了用气相色谱 /质谱法 (GC/MS)测定苯丙酮含量的方法。组分的定性依靠GC/MS联用技术和NIST谱库标准质谱图对照分析。以苯乙酮为内标 ,苯丙酮含量在 1.0× 10 -5～ 2 .0× 10 -4g/mL范围内呈线性 ,线性相关系数r =0 .994 9,苯丙酮最低检测浓度为 1.0× 10 -8g/mL。该法操作简便、快速 ,结果准确可靠 ,且具有很好的实用价值     

Sol–Gel Processing and Microwave Characteristics of Ba(Mg⅓Ta⅔)O3 Dielectrics

The sol–gel method has been developed for the preparation of pure Ba(Mg_1/3Ta_2/3)O₃ ceramics. This involves the reaction of the heterometallic alkoxide Ta₂Mg(OEt)₁₂ with hydrated barium hydroxide Ba(OH)₂·8H₂O. Complete crystallization of the sol–gel-derived powder is achieved at 600°C, leading to a cubic perovskite type phase. After sintering at 1400°C (2–5 h), a trigonal cell arises from Mg–Ta ordering (the degree of order is greater than 0.9), and about 98.5% of the theoretical density is obtained. Preliminary microwave dielectric measurements show that the dielectric constant and the unloaded Q _u of the ceramics are 24.2 and 6750, respectively, at 7.7 GHz.     

一种基于条带划分的低延迟帧内编码方法

现有编解码系统所产生的固有延迟比较大,例如对于标清视频,系统延迟要大于260ms,因此难以用于对延迟有严格要求的系统中。为此,研究了一种新的低延迟帧内编解码结构,在该结构中,将输入的视频划分成若干个条带,在采集端以条带为单位进行采集,以有效降低采集延迟;同时,给出了以条带为基本单位的I帧编码方法,对每一编码条带下采样,将其分成4个子图,以子图为单位进行预测,以提高预测的精度,进而降低编码延时。实验表明,新的编码结构在采集和编码过程中能有效降低帧内编码延迟,在保证恢复图像质量的同时,可以将延迟降低到150ms。     

基于Lucene和LSA的法律咨询系统

本文设计的法律咨询系统,结合法律行业的现状,以中文问答系统为原型,结合了开源数据检索项目Lucene.net,扩展了数据的存储类型. 本文借助中科院研发的中文分词系统,集成到Lucene.Net平台上,弥补了其分词不足. 并使用互信息技术,使同义的法律相关词语优先进行检索. 在中文问答系统的答案提取时,经常出现答案的“漏取”和“错取”的情况,本文提出了一种基于潜在语义分析（LSA）的问题和答案句子相似度计算方法,利用空间向量模型作为表示方法,借助潜在语义分析理论,通过奇异值分解的降维方法构建了一个低维的语义空间,并在语义空间上实现了问题与答案句子相似度计算. 经试验证明,本系统具有较精准的查询正确率以及较少的运行计算时间.     

由3-吲哚乙酰胺制备色胺

色胺(Tryptamine)，化学名为3-(2-氨乙基)吲哚，是合成具有治疗脑动脉硬化作用的长春胺和脱水长春胺乙酯等生物碱的中间体。文献报道的合成方法较多，如以γ-氯丁醛和苯肼缩合法、3-氯丙基丙二酸乙酯和氯化重氮苯偶合法、乙酰吲哚满基酮为原料的Wittuig反应法、以丙烯腈和丙二酸乙酯为原料的6步法等，这些方法或总收率低、或中间体制备困难、或反应条件苛刻、     

Blends,hydrogen bonds,and orientation: Understanding the role of interactions

A review of past and present studies on orientation, rheology, and FTIR investigations on a hydrogen bond–forming polymer, poly(vinyl phenol) (PVPh), and its blends with polyethylene oxide (PEO), poly(methyl methacrylate) (PMMA), and poly(vinyl methyl ether) (PVME) is presented. Orientation is analyzed on the basis of deformation‐induced orientation and relaxation. For deformation, it is proposed from recent molecular modeling studies that orientation is similar for flexible backbone polymers of the types studied. To investigate relaxation, dynamical rheology analysis was performed previously on PVPh/PEO blends and global molecular weight between entanglement, M_e, and chain friction ζ were estimated. M_e remained close to that of the polymer forming the dominant network, a discontinuity being observed near 50 mole percent. Friction coefficient exhibited a maximum near that of the orientation function of this system. Near‐infrared measurements also showed a maximum in the number of interchain hydrogen bonds at this concentration, although broader than that of orientation or of the friction coefficient. For strongly interacting blends, it is proposed that a break in orientation behavior would be associated with the dominant network present, and therefore to M_e, whereas ζ will dictate whether orientation decreases or increases in a given network domain.     

Influence of the preparation conditions on the properties of gold catalysts for the oxidation of glucose

In this work, two deposition–precipitation methods for the preparation of gold catalysts for glucose oxidation were investigated. Thus far, gold colloids immobilized on carbon have been used for catalytic glucose oxidation, but the long-term stability of these systems was not sufficient. To improve the long-term stability we used the deposition–precipitation methods using NaOH (DP NaOH) or urea (DP urea) as precipitation agents as they were described by Haruta and Dekkers, respectively, using alumina as a support material. With these methods, it was possible to prepare highly active and selective catalysts which showed an excellent long-term stability. DP urea was found to be the preferred method, because in contrast to DP NaOH, no losses of gold occurred during the preparation, and it was possible to adjust various gold contents up to 10 wt% Au.     

GaN基LED与Si键合技术的研究

采用金属键合技术结合激光剥离技术将GaN基LED从蓝宝石衬底成功转移到Si衬底上。利用X射线光电子谱(XPS)研究不同阻挡层对Au向GaN扩散所起的阻挡作用,确定键合所需的金属过渡层。利用多层金属过渡层,在真空、温度400℃和加压300 N下实现GaN基LED和Si的键合,通过激光剥离技术将蓝宝石衬底从键合结构上剥离下来,形成GaN基LED/金属层/Si结构。用金相显微镜及原子力显微镜(AFM)观察结构的表面形貌,测得表面粗糙度(RMS)为12.1 nm。X射线衍射(XRD)和Raman测试结果表明,衬底转移后,GaN基LED的结构及其晶体质量没有发生明显变化,而且GaN与蓝宝石衬底间的压应力得到了释放,使得Si衬底上GaN基LED的电致发光(EL)波长发生红移现象。