聚2,6-二氨基-4,5,6,7-四氢苯并噻唑修饰玻碳电极伏安法测定多巴胺和尿酸

将经过抛光、清洗的GCE置于1mmol·L-1 2,6-二氨基-4,5,6,7-四氢苯并噻唑(DATHBT)溶液中,用循环伏安法以0.05V·s-1扫描速率在-0.6~2.0V电位范围内循环扫描15圈,制得PDATHBT薄膜修饰的玻碳电极(PDATHBT/GCE)。试验表明:该修饰电极对多巴胺(DA)和尿酸(UA)的电极反应具有催化作用,而且使原来在裸GCE上产生的DA和UA重叠的氧化峰分开成为两个独立的灵敏氧化峰,其氧化峰电流与DA和UA的浓度分别在0.1~100μmol·L-1和2~1 000μmol·L-1之间呈线性关系,两者的检出限(3S/N)依次为0.05,0.2μmol·L-1。加标回收率在97.0%~100%之间(DA)和96.5%~110%之间(UA),测定值的相对标准偏差(n=6)均小于3.5%。     

1,3-二吡啶基苯和4,4′-二羧基二苯砜构筑的钴(Ⅱ)配合物合成、结构和性质(英文)

以两种V型的配体4,4′-二吡啶基苯(1,3-dpb)和4,4′-二羧基二苯砜(H2sdb),和钴(Ⅱ)通过溶剂热反应合成了1个配位聚合物{[Co(dpb)(sdb)(H2O)2]·2H2O·DMF}n(1)。对其进行了红外、热重、粉晶衍射、单晶衍射等表征,配合物属于三斜晶系,空间群P1。其中Co(Ⅱ)的2个顶点被水分子占据,相邻的钴(Ⅱ)离子连接着1,3-二吡啶基苯和4,4′-二羧基二苯砜形成一维的双绳链,相邻的链之间通过羧基-配位水和配位水-配位水间的氢键相互连接形成二维的层状结构,层状结构之间通过砜基-配位水间的氢键又相互连接形成三维结构。此外,还研究了配合物的固体紫外-可见光谱。     

液相色谱法测定中药材中的富马酸单甲酯与富马酸二甲酯

建立了同时测定中药材中富马酸单甲酯(MMF)和富马酸二甲酯(DMF)的高效液相色谱方法。样品经乙酸乙酯提取、氨基复合石墨碳固相萃取柱净化后,C18柱分离,二极管阵列检测器检测。在0.025~5.0μg/mL浓度范围内,色谱峰面积与分析物浓度呈良好线性关系,MMF和DMF的检出限(S/N=3)分别为0.015、0.020 mg/kg,定量下限(S/N=10)分别为0.05、0.06 mg/kg。当加标浓度水平为0.1、0.2、0.5mg/kg时,MMF和DMF的回收率为78.9%~97.3%,相对标准偏差(RSD,n=6)为1.7%~6.0%。方法灵敏、可靠,能够满足中药材中MMF和DMF残留检测的要求。     

利用REDUCE语言识别结构系统的支承刚度

本文提出一种识别结构系统支承刚度的新方法，该方法以传递矩阵法为基础，利用ＲＥＤＵＣＥ计算机代数语言推导以刚度参数为未知数的非线性方程组，进而解此方程组识别结构系统的支承刚度。模态试验及计算实例验证了该方法的有效性和正确性。     

掺入Mg2+对CsNiCl3晶体的基态能级、零场分裂参量及Jahn-Teller效应的影响

应用不可约张量理论构造了三角对称晶场中3d²/3d^８态离子的45阶可完全对角化的微扰哈密顿矩阵，在考虑了以前工作中被忽略的自旋-自旋耦合作用的基础上计算了CsNiCl₃晶体和CsNiCl₃:Mg²⁺晶体的基态能级、晶体结构、零场分裂参量和Jahn-Teller效应，研究了掺入Mg²⁺对CsNiCl₃晶体的光谱、零场分裂参量及Jahn-Teller效应的影响和自旋单重态对基态能级的贡献，发现掺杂使得晶体结构产生畸变，从而改变晶体光谱的精细结构和零场分裂参量，不改变Jahn-Teller效应的分裂规律但改变分裂的大小. 关键词： 基态能级 掺杂 零场分裂 自旋-自旋耦合     

Measurements of pressure induced self-broadening and frequency shift coefficients of methane R9 manifold of 2v_3 band

An external-cavity diode laser (ECDL) has been used to investigate pressure-induced self-broadening as well as frequency shift of 2v3 band R9 manifold of methane. A phase sensitivity detection technology has been employed to determine the pressure induced frequency shift coefficient, however, which is obtained by line shape analyses of the recorded absorption spectrum. F1 and F2 unresolved double lines near 6105.626 cm-1 were measured as an object because they are often used to the high sensitivity detection of trace methane. The results show that the self-broadening and pressure induced frequency shift coefficients are 0.0232±0.003 and 0.0055±　0.0007 MHz/Pa, respectively.     

高功率二极管泵浦腔内倍频激光器

 成功研制了一台高功率二极管泵浦声光Q开关腔内倍频Nd:YAG激光器。当泵浦功率约为350W时，采用透过率为30%的输出耦合镜，调Q激光输出功率32.5W，脉宽约200ns，重复频率7kHz；采用Ⅱ类匹配KTP晶体腔内倍频，获得了32.5W的绿光输出，脉宽约120ns。输出光束平滑，远场为类高斯分布，测得的光束质量因子为3.6。     

一种便携集成式伴随保障系统

为解决弱测试性武器装备的外场级快速保障问题,提出并研发了一种便携集成式伴随保障系统,该系统由平板电脑、数据采集机箱、信号调理单元以及测试电缆组成,兼备IETM、远程数据终端、测试维修设备等多种功能。硬件部分的平板电脑具有IETM的完整功能,可与装备通信系统实现无缝链接;数据采集机箱与信号调理单元之间采用卡具连接,便于功能拓展,与平板电脑无线连接后,应用诊断软件能够实现典型装备的系统级故障诊断。软件部分基于Lab windows、Visio VBA和Access数据库联合开发,重点解决了基于顶层故障现象智能推理、故障树自动生成、判断节点自动检测等功能。该系统经过试验验证,能够准确调用软件各功能模块,能够完成装备系统级故障诊断以及与指控通信系统之间的数据传输。     

Review of methodological and experimental LIBS techniques for coal analysis and their application in power plants in China

Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical spectroscopy technique. This review presents the main recent developments in China regarding the implementation of LIBS for coal analysis. The paper mainly focuses on the progress of the past few years in the fundamentals, data pretreatment, calibration model, and experimental issues of LIBS and its application to coal analysis. Many important domestic studies focusing on coal quality analysis have been conducted. For example, a proposed novel hybrid quantification model can provide more reproducible quantitative analytical results; the model obtained the average absolute errors (AREs) of 0.42%, 0.05%, 0.07%, and 0.17% for carbon, hydrogen, volatiles, and ash, respectively, and a heat value of 0.07 MJ/kg. Atomic/ionic emission lines and molecular bands, such as CN and C₂, have been employed to generate more accurate analysis results, achieving an ARE of 0.26% and a 0.16% limit of detection (LOD) for the prediction of unburned carbon in fly ashes. Both laboratory and on-line LIBS apparatuses have been developed for field application in coal-fired power plants. We consider that both the accuracy and the repeatability of the elemental and proximate analysis of coal have increased significantly and further efforts will be devoted to realizing large-scale commercialization of coal quality analyzer in China.     

强酸性阳离子交换树脂负载金属离子改性催化合成乙酸丁酯

用两种强酸性阳离子交换树脂进行金属离子负载改性制备酯化催化剂,考察了金属盐种类,盐浓度,沉浸时间,沉浸温度等因素对催化剂性能的影响.用在优化条件下制备的催化剂催化乙酸和正丁醇酯化反应体系,反应1h乙酸的转化率达到69%.