新型氮杂环卡宾催化剂的合成及其在烯烃的自由基氟烷基酰化反应中的应用研究

以环庚酮及环己（庚）胺为起始原料,经溴代、环化、脱硫等反应,以良好的收率合成了环烷基取代的新型噻唑骨架的氮杂环卡宾催化剂。结果表明,在该催化剂催化下成功地实现了烯烃的自由基氟烷基酰化反应,以中等的收率完成了三种类型的γ-氟烷基取代酮的高效合成。所得化合物通过¹H NMR, ¹³C NMR, ¹⁹F NMR和HR-MS（ESI-TOF）进行表征。     

Quick stabilization of capillary for rapid determination of potassium ions in the blood of epilepsy patients by capillary electrophoresis without sample pretreatment

Mutations in the potassium channel genes may be linked to the development of epilepsy and affect the blood potassium levels. Therefore, accurate determination of potassium in the blood will be critical to diagnose the cause of epilepsy. CE is a competent technique for the fast detection of multiple ions, but complicated matrices of a blood sample may cause significant variation of migration times and the peak shape. In this work, a procedure for rapid stabilization of the capillary inner surface through preflushing of a blood sample was employed. The process takes only 40 min for a capillary and then it can be used for more than 2 weeks. No pretreatment of the blood sample or other surface modification of the capillary is needed for the analysis. The RSDs of the migration time and peak area were reduced to 1.5 and 5.1% from 12.6 and 14.5%, respectively. The proposed method has been successfully applied to the determination of the potassium contents in the blood sample of patients with epilepsy at different stages. The recoveries of potassium ions in these blood samples are in a range from 86.5 to 104.5%.     

连续相位板远场焦斑能量集中度实验研究

在惯性约束聚变（ICF）研究过程中,焦面上聚焦光斑形态要求极为苛刻。基于离线测试平台,从实验上研究了各种应用误差对连续相位板（CPP）远场焦斑能量集中度的影响。得出光束旋转误差、口径误差、平移误差和倾斜误差在可控范围内CPP远场焦斑能量集中度均高于95%,其波动范围小于0.5%,CPP的容忍度较强。而实验畸变波前属于空间频率小于0.02 mm-1的低频波前,严重影响了CPP的整形能力,波前畸变是影响能量集中度高于90%的主要因素。     

大口径连续相位板远场光强的离线测试实验

为了准确测试和评价大口径连续相位板（CPP）元件的远场光强性能,根据激光装置需求建立了351 nm波长下大口径CPP远场光强离线测试系统,开展了330 mm330 mm口径CPP元件测试实验,并与标量衍射计算结果进行对比,分析了系统的测试重复性和测试精度。实测系统远场弥散斑大小为2.9倍衍射极限,可测试最大口径为圆形f600 mm和方形430 mm430 mm。测试系统在焦点2 mm范围内的能量集中度测试重复性优于0.2 %。计算和实验焦斑形貌及分布吻合,实测能量集中度比计算结果小0.85%、焦斑半径大13 m左右,差异由实测系统的时间匀滑作用引起,可通过缩短曝光时间和减小系统像差等措施进一步提高测试精度。     

梯恩梯(TNT)爆轰初期形成富碳团簇分子及类石墨结构的分子动力学模拟

富碳炸药在爆轰过程中可产生团簇分子,而现有的实验手段不能直接观测团簇分子的形成过程.本文采用ReaxFF/lg力场对梯恩梯（TNT）在不同温度下的热分解过程进行了模拟.研究发现：团簇分子在反应初始阶段形成缓慢,大约一次增加一个TNT相对分子质量.随着反应进行,团簇分子迅速增大,最大团簇分子相对分子质量可达8000~10000,约占体系质量的18%.分析团簇分子的结构发现,团簇分子中一部分苯环被破坏,形成五元环和夹杂N、O原子的六元环,在3500 K条件下还形成了更为复杂的七元环等结构.通过体积膨胀和直接降温的方法,研究了团簇分子的稳定性：体积膨胀使得团簇分子迅速分解;而直接降温,团簇分子又聚合成更大的团簇.分析类石墨结构的产生过程,发现先膨胀然后降温是必不可少的步骤.比较团簇分子和TNT分子中各原子质量所占比,团簇分子中C原子质量比始终在增加.     

Organic peroxide production in the Cl2-ethane-air photoreaction system

HPLC along with FT-IR technique was used to study the formation of organic peroxides in the Cl₂-ethane-air photoreaction system. Ethyl hydroperoxide (CH₃CH₂₁OOH, EHP) and peroxyacetic acid ( CH₃C(O)OOH, PAA) were conformed to be the peroxide product in the reaction system. In addition, methyl hydroperoxide (CH₃OOH, hydroxymethyl hydroperoxide (HOCH₂OOH, HMHP) and two unidentified organic peroxides were detected for the first time. EHP and were the dominant peroxide products. The identification of HMHP showed that Criegee biradical CH₂OO may be formed as an intermediate in the oxidation of ethane. Simulation results showed that photooxidation of ethane may make substantial contribution to source of organic peroxides in the atmosphere.     

Synthesis of Cs2.5H0.5PW12O40/TiO2 Nanocomposites with Dominant TiO2 {001} Facets and Related Photocatalytic Properties

TiO₂ nanosheets with dominant {001} facets, coupled with Cs_2.5H_0.5PW₁₂O₄₀, were successfully synthesized by a one‐step hydrothermal reaction. The photocatalytic activity of nanocatalysts was evaluated by the degradation of Rhodamine B under UV light irradiation. The results showed that both the addition of Cs_2.5H_0.5PW₁₂O₄₀ and the exposed {001} facets of TiO₂ have a positive effect on the photocatalytic activity. The improved photoactivity of nanocomposites in comparison with that of TiO₂ nanosheets could be attributed to the synergistic effect between Cs_2.5H_0.5PW₁₂O₄₀ and TiO₂ which facilitates the separation of photo‐induced hole‐electron pairs.     

激光诱导等离子体光谱元素成像技术研究进展及其在核材料检测领域的应用

激光诱导等离子体光谱元素成像技术以其具备测量不受辐射本底影响,测量速度快,样品制备相对简单,可远程分析放射性样品等优势在核材料检测领域展现出巨大的潜力。本文将激光诱导等离子体光谱元素成像技术分为成像系统和数据处理两个方面进行介绍,并对其研究进展和在核材料检测领域的应用进行综合分析,最后总结了LIPS元素成像技术的优势与面临的挑战,对LIPS元素成像技术在核材料检测领域的发展趋势进行展望。     

Organic-inorganic hybrids assembled by bis(undecatungstophosphate) lanthanates and dinuclear copper(II)-oxalate complexes

A series of organic-inorganic hybrid compounds, K2H7[{Ln(PW11O39)2}{Cu2(bpy)2(mu-ox)}].xH2O (Ln = La, x approximately = 18 (1); Ln = Pr, x approximately = 18(2); Ln = Eu, x approximately = 16(3); Ln = Gd, x approximately 22(4); Ln = Yb, x approximately = 19 (5); bpy = 2,2'-bipyridine and ox = oxalate), have been isolated by the conventional solution method. Single-crystal X-ray diffraction studies reveal that compounds 1-5 are isomorphic and consist of one-dimensional chains, which are constructed by alternating bis(undecatungstophosphate) lanthanates [Ln(PW11O39)2](11-) and dinuclear copper(II)-oxalate complexes [Cu2(bpy)2(mu-ox)]2+.pi-pi interactions of the bpy ligands from adjacent chains lead to their three-dimensional structures. An analogue of potassium K2H9[{K(PW11O39)2}{Cu2(bpy)2(mu-ox)}1].approximately 20.5H2O(6) has also been obtained. The syntheses and structures of these compounds are reported here. Magnetic properties of 1, 2 and 3 are discussed as well. Attempts to crystallize similar compounds containing Co(II) and Ni(II) were unsuccessful.     

Large-area perovskite films for PV applications: A perspective from nucleation and crystallization

Perovskite solar cells (PSCs) have attracted significant research interest due to the rapid rise in efficiency.However,a large efficiency gap still exists betwe...