Simultaneous determination of oxygen, nitrogen and hydrogen in metals by pulse heating and time of flight mass spectrometric method

The inert gas fusion and infrared absorption and thermal conductivity methods are widely used for quantitative determination of oxygen(O), nitrogen(N) and hydrogen(H) in metals. However, O, N and H cannot be determined simultaneously with this method in most cases and the sensitivity cannot meet the requirement of some new metal materials. Furthermore, there is no equipment or method reported for determination of Argon(Ar) or Helium(He) in metals till now. In this paper, a new method for simultaneous quantitative determination of O, N, H and Ar(or He) in metals has been described in detail, which combined the pulse heating inert gas fusion with time of flight mass spectrometric detection. The whole analyzing process was introduced, including sample retreatment, inert gas fusion, mass spectral line selection, signal acquisition, data processing and calibration. The detection limit, lower quantitative limit and linear range of each element were determined. The accuracy and precision of the new method have also been verified by measurements of several kinds of samples. The results were consistent with that obtained by the traditional method. It has shown that the new method is more sensitive and efficient than the existing method.     

不同结构的氧化钛纳米金复合薄膜的光伏特性

具有表面等离子体共振效应的金属和氧化物复合纳米结构被应用在染料敏化太阳能电池（DSSC）中以提高电池的光电转换效率,金属纳米粒子和氧化物薄膜的复合结构对于等离子体共振器件在电池上的效果有巨大的影响. 我们研究了不同氧化钛薄膜和纳米金复合体系（纳米金分别修饰在氧化钛薄膜的表面和下表面）的光电转换效果,其中当纳米金修饰在氧化钛薄膜表面时薄膜的紫外可见吸收增加最大. 然而,经过染料敏化之后,该体系的光电转换效率比未修饰的薄膜有所降低,而纳米金修饰在氧化钛薄膜下表面时,光电转换效率比未修饰时提高了37%,同时入射单色光子-电子转化效率（IPCE）也有相应提高. 为了进一步研究纳米金在复合薄膜中的作用,我们引入了TiO₂-Au-TiO₂的三明治体系,该体系的光电转换效率比未修饰的参比氧化钛薄膜仍有所提高. 上述研究结果表明等离子体共振器件的结构设计对于染料敏化太阳能电池的改善具有重要意义. 同时,我们对于纳米金的等离子体共振效应做了离散偶极子近似（Dipole Discrete Approximation）模拟计算,其结果支持了实验数据. 该研究对于未来太阳能电池中表面等离子体共振器件的设计具有一定指导意义.     

2，6-二氨基-3，5-二硝基-1-氧吡嗪合成中的氧化方法改进

以磁性Fe3O4负载质子化过氧钨酸盐为催化剂,在不用三氟乙酸的情况下,以双氧水为氧化剂,将2,6-二甲氧基吡嗪、2,6-二氯吡嗪和2-氯-6-甲氧基吡嗪高效地氧化为其相应的氮氧化物2,6-二氨基-3,5-二硝基-1-氧吡嗪(LLM-105)。 典型条件为：底物10 mmol,CH3CN 30 mL,催化剂Fe3O4/CS/HWO 0.1 g(约0.1 mmol),60 ℃分5次逐滴加入30%双氧水5 mL。 反应混合物溶液经萃取和柱色谱法提纯,得产物,收率一般为60%~73%。 使用高斯03量化计算程序对氧化过程进行了理论计算,结果与实验数据相符。     

实验环Betatron振荡随机冷却的模拟

随机冷却是一种基于带宽反馈系统对束流振荡进行衰减的冷却方法,更适合冷却较大发射度和动量分散的次级粒子束,与电子冷却互补,可以得到更高品质的束流。兰州重离子研究装置(HIRFL) 目前处于冷却存储环的实验环随机冷却系统的设计和建造阶段。通过对横向Betatron 振荡的模拟,得到了提高系统带宽、增加探测器(Pick-up) 和冲击器(Kicker) 的个数、降低系统噪声温度等对缩短冷却时间和减小冷却平衡值的重要作用。同时,分析了较大的动量分散或较大的放大器增益对Betatron 振荡冷却过程产生的加热现象。Stochastic cooling, based on a feedback system, aims at damping the oscillation of particles. Stochastic cooling is more suitable to cool secondary beam with larger size and momentum spread, and it is therefore can be complemented with electron cooling, in order to obtain beam of higher quality. Stochastic cooling system is being designed and constructed on the experimental Cooling Storage Ring of HIRFL. By simulation of Betatron stochastic cooling, it is obtained that the importance for shortening the cooling time and reducing cooling equilibrium by improving bandwidth, increasing the numbers of pickup and kicker, and decreasing the system noises. Meanwhile, the heating during the cooling process caused by larger momentum spread or larger gain of amplifier is analyzed.     

水系钠离子电池电极材料研究进展

随着太阳能、风能等可再生能源发电并网普及应用和智能电网建设,储能技术成为能源优化利用的核心技术之一。水系钠离子电池具有资源丰富、价格低廉等优势,作为未来电网储能的重要选择而成为近年来电化学储能技术前沿的研究热点。由于受到水的热力学电化学窗口限制及嵌钠反应的特殊性(例如溶液的pH值、氧的溶解等),以及容量、电化学电位、适应性及催化效应等,电极材料选择面临挑战,进而影响水系钠离子电池的应用。因此,电极材料成为水系钠离子电池的研究重点。本文简要概括了水系钠离子电池的特点,并对氧化物、聚阴离子化合物、普鲁士蓝类似物和有机物等电极材料体系的最新研究进展进行了总结,并概括了将来的发展方向,为推动水系钠离子电池的发展和能源优化研究奠定了基础。     

A New Insight into Toxicity of Colchicine Analogues by Molecular Docking Analysis Based on Intestinal Tight Junction Protein ZO-1

Colchicine (COL) is a well-known plant alkaloid long used for medical purposes due to the selective anti-inflammatory effect on acute gouty arthritis. It is also a kind of mitosis toxin with strong inhibitory effects of cell division and is therefore being applied to the treatment of various cancers. However, this product shows a variety of adverse effects that are significantly correlated with the dosage and have attracted much attention. For the first time, the present work obtained a new insight into the gastrointestinal toxicity of colchicine analogues by molecular docking analysis, which was based on the 3D structure of intestinal tight junction protein ZO-1 and the ligand library containing dozens of small-molecule compounds with the basic skeleton of COL and its metabolites. The binding energy and mode of protein–ligand interaction were investigated to better understand the structure–toxicity relationships of COL analogues and the mechanism of action as well. Cluster analysis clearly demonstrated the strong correlation between the binding energy and toxicity of ligand molecules. The interaction mode further revealed that the hydrogen bonding (via the C-7 amide or C-9 carbonyl group) and hydrophobic effect (at ring A or C) were both responsible for ZO-1-related gastrointestinal toxicity of COL analogues, while metabolic transformation via phase I and/or phase II reaction would significantly attenuate the gastrointestinal toxicity of colchicine, indicating an effective detoxication pathway through metabolism.     

高速相干光通信系统中的自适应步长恒模算法

对于高速光通信系统中的相干检测来说,盲均衡是一项常用的恢复传输符号的技术。目前应用最广泛的盲均衡算法是恒模算法,但是一方面它不能兼顾收敛速度和收敛精度,另一方面在偏分复用系统中很容易陷入奇异性。因此提出了一种改进型的恒模算法———自适应步长恒模算法,并在112Gb/s偏分复用16进制正交幅度调制系统中对提出的算法进行了测试。与传统的恒模算法相比,改进后的算法收敛速度仅为恒模算法的1/20;收敛稳定后误差函数的方差比恒模算法降低了0.7dB;对偏分复用系统中的奇异性有很好的抵抗能力;在不考虑奇异性问题时,光信噪比代价与恒模算法相比降低了1.5dB。     

有机溶剂中微量水的荷移光谱法测定

研究了氯冉酸与有机溶剂中水的反应，确定了反应条件，氯冉酸与水的络合物的最大吸收波长为530nm。在乙醇、甲醇，正丙醇，异丙醇、正丁醇，正庚醇，正己醇溶剂中，水的含量分别在0－5％（V／V）或0－8％（V／V）范围内呈线性关系，相关系数为0．998或0．999；该方法重现性好，灵敏度高，操作简单，用于测定乙醇中微量水的含量，与标准值相符；加入回收法测得甲醇中水的回收率分别为98％－103％，结果令人满意。     

催化裂化待生剂上有机吸附物种的鉴别分析

为了鉴别分析催化裂化待生剂上分子筛孔道内、外的有机吸附物种,提出了超声萃取提取待生剂上外表面的有机吸附物种方法,优化了萃取条件;对分子筛孔道内的有机吸附物种,采用HF处理待生剂,溶解催化剂分子筛骨架以释放孔内积炭,并用二氯甲烷作溶剂萃取.采用GC-MS 分离并鉴别分子筛孔道内、外的有机吸附物种,实验结果显示在催化剂外表面主要是二环和三环芳烃,而在分子筛孔道内解吸的则是从双环到七元环的多环芳烃.这些结果对研究催化裂化催化剂的性能和结炭的机理提供了重要信息.