多检测GPC/SEC技术在高分子表征中的应用Ⅳ.氘化高分子的溶液性质

采用体积排斥色谱法／ 示差折光指数／ 直角激光光散射／ 示差粘度三检测联用技术表征了氘化聚苯乙烯、聚苯乙烯和氘化聚苯乙烯－ 聚异戊二烯。结果表明,在θ条件下,虽然氘化聚苯乙烯的化学依赖性常数υＴ,ＤＰＳ比聚苯乙烯的化学依赖性常数υＴ,ＰＳ大,但２５ ℃时在四氢呋喃中,氘化聚苯乙烯的分子尺寸仍小于聚苯乙烯的分子尺寸。由于嵌段共聚物的淋洗体积随组成变化,所以用传统的ＳＥＣ／ＲＩ得不到准确的分子量。经比较膜渗透、小角激光光散射和基质辅助激光脱吸与离子化时间飞行质谱等的实验结果,证明体积排斥色谱法／ 示差折光指数／ 直角激光光散射／ 示差粘度三检测技术能准确地得到氘化二嵌段共聚物的分子量以及其它重要信息。     

Oxidative transformation of azides to aryl nitriles using DIB/TBHP: scope and mechanistic insights

Bis(tert-butylperoxy)iodobenzene, generated in situ by the reaction between diacetoxyl iodobenzene (DIB) and tert-butyl hydroperoxide (TBHP), was used in the oxidative transformation of primary azides to nitriles, and secondary azides to ketones.     

Total synthesis of (±)-antofine

An efficient preparation of (±)-antofine is described. The main steps involved in this synthesis are the Horner–Wadsworth–Emmons reaction, the intramolecular Schmidt reaction of an azido aldehyde, and the one-pot deprotection of the N-formyl group, followed by Pictet–Spengler cyclization. The asymmetric hydrogenation of the trisubstituted α,β-unsaturated ester is also explored, however only moderate enantio-control (55% ee) is obtained. Finally, (±)-antofine is prepared in six steps from the phenanthryl aldehyde 5 with an overall yield of 35%.     

Polydopamine-Assisted Rapid One-Step Immobilization of L-Arginine in Capillary as Immobilized Chiral Ligands for Enantioseparation of Dansyl Amino Acids by Chiral Ligand Exchange Capillary Electrochromatography

Herein, a novel L-arginine (L-Arg)-modified polydopamine (PDA)-coated capillary (PDA/L-Arg@capillary) was firstly fabricated via the basic amino-acid-induced PDA co-deposition strategy and employed to constitute a new chiral ligand exchange capillary electrochromatography (CLE-CEC) method for the high-performance enantioseparation of D,L-amino acids (D,L-AAs) with L-Arg as the immobilized chiral ligand coordinating with the central metal ion Zn(II) as running buffer. Assisted by hydrothermal treatment, the robust immobilization of L-Arg on the capillary inner wall could be facilely achieved within 1 h, prominently improving the synthesis efficiency and simplifying the preparation procedure. The successful preparation of PDA/L-Arg coatings in the capillary was systematically characterized and confirmed using several methods. In comparison with bare and PDA-functionalized capillaries, the enantioseparation capability of the presented CLE-CEC system was significantly enhanced. Eight D,L-AAs were completely separated and three pairs were partially separated under the optimal conditions. The prepared PDA/L-Arg@capillary showed good repeatability and stability. The potential mechanism of the greatly enhanced enantioseparation performance obtained by PDA/L-Arg@capillary was also explored. Moreover, the proposed method was further utilized for studying the enzyme kinetics of L-glutamic dehydrogenase, exhibiting its promising prospects in enzyme assays and other related applications.     

Copper‐Catalyzed Aerobic Oxidative Reaction of Sulfonyl Hydrazides with Alcohols: An Easy Access to Sulfinates

A Cu‐catalyzed aerobic oxidative reaction between sulfonyl hydrazides and alcohols has been developed. In this reaction, sulfonyl hydrazides act as the sulfinic acid precursors to react with alcohols, resulting in sulfinic esters with up to 72 % yield. This catalytic system tolerates a wide range of sulfonyl hydrazide substrates, and represents a new strategy for the transformation of readily available sulfonyl hydrazides.     

“强光一号”加速器Z箍缩丝阵负载的零维模拟

作为丝阵Z箍缩实验的基础,丝阵负载的设计具有重要意义。主要介绍了Z箍缩丝阵负载设计的slug模型, 首先对该模型的原理进行了分析,然后对该模型进行编程,并利用美国Saturn加速器上的丝阵负载实验结果进行验证,计算结果表明了程序的可靠性。最后应用该模型及所编写程序对“强光一号”加速器上丝阵负载的Z箍缩实验进行了模拟,获得了偏差小于5%的模拟结果。     

双脉冲电子束源实验研究

利用现有2MeV直线感应注入器,通过改造,将其次级功率源和8个感应腔分成2组,使之交替工作,建立了一台双脉冲电子束源。二极管电压脉冲幅度达到1MeV,电子束脉冲持续时间为120ns,脉冲间隔可以根据需要在100~500ns间进行调节。实验结果表明：该双脉冲电子束源可以产生双脉冲电子束,其电压幅度差值小于2%,束流可达3kA,并且工作稳定,利用该装置可以进行多脉冲二极管物理和天鹅绒多脉冲发射特性实验研究。     

用自积分式罗氏线圈测量纳秒级高压脉冲电流

介绍了测量纳秒级高压脉冲大电流信号用的自积分式罗氏线圈的优点、用途、基本原理及设计。利用传输理论分析了它的信号响应及干扰。对研制出的罗氏线圈进行了标定。设计的线圈的灵敏度在1.4mV/A,可以采用的上升时间小于2ns,脉宽小于200ns,电流信号10A～40kA。自积分式罗氏线圈广泛用于脉冲功率技术中的快过程大电流测量。     

同轴虚阴极振荡器实验研究

介绍了中国工程物理研究院应用电子学研究所关于同轴虚阴极振荡器实验的最新进展。实验结果表明,带阳极反射板结构的同轴虚阴极振荡器比不带阳极反射板结构的同轴虚阴极振荡器输出微波功率更高,频谱更纯。在二极管电压350 kV,电流23 kA条件下,输出微波峰值功率500 MW,能量转换效率约6.2%,工作频率为3.3 GHz。对实验结果进行了理论分析。