IRIS-ICP光谱仪点火故障分析

从ICP光谱仪点火系统的组成部分、工作原理、参数分析入手,分析不能正常点火故障及排除方法.     

映谱仪常见故障的维修方法

映谱仪在使用一段时间后，往往会出现光路成像不清，机械可调部分失灵等故障，文中主要介绍了这些故障的排除方法。     

自旋极化电子碰撞谱仪的研制进展

与电子自旋相关的效应在散射过程中起着十分重要的作用,但却常常被较强的库仑相互作用所淹没,使得以自然电子为探针的散射实验很难对其进行直接观测.以极化电子作为探针,研制极化电子碰撞谱仪,将为开展自旋相关效应的实验研究奠定基础.本文简述了极化电子与原子分子碰撞研究的意义,并介绍了清华大学物理系极化物理实验室自行开发的GaAs极化电子源及基于该极化电子源的碰撞谱仪的研制情况.     

高能量分辨率的平面晶体位置灵敏谱仪

平面晶体波长色散位置灵敏谱仪是一新型高能量分辨率的X射线分析装置,可用于高能量分辨的元素分析、化学态及原子物理等研究中.这里简要介绍所研制的位置灵敏谱仪装置及其性能,以及位置灵敏谱仪与其核心部件──位置灵敏正比计数器的基本原理.所研制位置灵敏谱仪对55Fe,Ti和Si所达到的能量分辨率(FWHM)分别为25eV,15eV及7eV.因此,它将可以用作高分辨的元素分析.     

一种新型非肽类血管紧张素Ⅱ受体拮抗剂Candesartan Cilexetil的1H和13C NMR归属

利用超导核磁共振波谱仪，测定了Candesartan Cilexetil的¹H、¹H-¹H COSY、DEPT、HMQC、HMBC等谱，对该化合物的所有化学位移数据进行了归属.     

一种测量次级中子能谱的新方法

采用双飞行时间法创建了一台非常规快中子飞行时间谱仪,排除了用D(d,n)3He中子源测量8-13MeV能区次级中子双微分截面时源中破裂中子群对次级中子能谱测量的干扰.结合常规快中子飞行时间谱仪的测量,实现了用D(d,n)3He中子源开展8-13MeV中子能区次级中子双微分截面的测量.     

NMR波谱仪控制台系统的软件测试

作为保证软件质量的重要手段,软件测试多年来一直受到关注. 本文阐述了核磁共振（NMR）波谱仪研制中的软件测试方法,从软件测试的概念出发,结合波谱仪控制台系统的软件结构和核磁共振实验本身的特性,介绍了整个测试过程,分析了测试难点及其解决方法,并详细说明了软件测试的实现过程以及在提高波谱仪可靠性和稳定性上所起的积极作用.      

基于FPGA小型化谱仪控制台的设计

针对核磁共振波谱仪中控制台的功能需求,考虑到仪器小型化的趋势,提出了基于FPGA和ARM的小型化控制台设计方案. 该方案具有体积小、处理速度快、控制精准、开发周期短和成本低等特点. 该文着重介绍了FPGA在系统中的功能实现,包括命令字接收、参数配置、脉冲发射和数据采样模块. ARM嵌入式模块实现控制台与上位机的以太网通信,以及和FPGA的高速并行总线通信,使控制台内部运行不受网络状况的干扰. 最后针对该设计方案提出几点改进建议.     

追忆吴钦义先生

<正>吴钦义先生是我国磁共振波谱学的先驱者,尤其在磁共振谱仪的研制领域,是举国熟知的开拓者.我认识吴钦义先生是在1960年冬,当时我在中国科学院大连化学物理研究所工作.所领导指派我带领一个由四人组成的小组,去中国科学院长春应用化学研究所学习电子顺磁共振(包括谱仪和谱学).当时长春应用化学研究所正在"研制"(确切地说是"仿制")从苏联进口的ЭПР-2型顺磁共振谱仪.该项     

圆柱面和圆锥面弯晶谱仪的理论计算及设计

用光线追迹的方法对圆柱面和圆锥面弯晶谱仪进行了理论计算,得到了谱仪的空间与色散坐标、线色散率、角色散率、光谱分辨力、空间和光谱放大率以及谱仪亮度等参数的解析计算公式,并对两类谱仪进行了具体的参数设计及性能比较.结果表明,圆锥面弯晶谱仪比同类型的传统圆柱面弯晶谱仪有着更为良好的聚焦性能,能够进一步改善谱仪的光子收集效率、谱仪亮度以及空间分辨力.这项工作为谱仪研制提供了理论基础和设计依据.     

黄酮甙类化合物中的酰基取代及其取代位置的确定

研究了黄酮甙类化合物的酰基取代现象，借助２ Ｄ ＮＭＲ技术，举例研究了一黄酮醇三乙酰基三糖甙的结构，着重研究糖上酰基的取代位置，并归纳总结了黄酮甙类化合物中各种常见的酰基的＾１３ ＣＮＭＲ谱及其取代所产生的位移现象。     

NMR Spin Trapping: Insight into the Hidden Life of Free Radical Adducts

In our original work (V. Khramtsov, L.J. Berliner and T.L. Clanton, Magn. Reson. Med. 42:228??34, 1999), a ³¹P nuclear magnetic resonance spin trapping (ST NMR) approach aimed to overcome comparatively short lifetimes of the paramagnetic adducts by detecting stable diamagnetic adducts of the degradation of phosphorous-containing nitrone was proposed. High stability of the NMR adducts of the nitrone spin traps with C-centered radicals and the ability to track their origin from paramagnetic adducts make ST NMR a valuable tool for the studies of these radicals in chemical and biological systems. Complementary ST NMR and electron paramagnetic resonance studies of the nitrone adducts derived from the addition of O- and S-centered radicals and nucleophiles revealed new insights into the pathways of the paramagnetic and diamagnetic adduct formation and degradation. In particular, use of ST NMR allowed for observation of reversible nucleophilic addition to the nitrones. On one hand, nucleophilic addition may result in a possible spin trapping artifact via the Forrester–Hepburn mechanism; whereas, on the other hand, the reverse reaction provides the key step in the “recycling??mechanism that is important for the antioxidant actions of the nitrones.     

饱和恢复法人体核磁共振自旋-晶格弛豫时间成象方法

当前,在医学核磁共振成象领域内,临床上广泛采用的是近似的自旋密度象、T1-和T2-加权密度象。但是,由于人体的正常组织和肿瘤之间的密度差别不大,从质子密度象很难区分人体的正常组织与肿瘤,而肿瘤与人体正常组织之间的在弛豫时间T1、T2的数值上差别较大。另外,自七十年代以来,大量关于离体(in vitro)核磁共振弛豫时间测量的文献表明,肿瘤的核磁共振弛豫时间T1,T2值具有明显的规律性,从而利用核磁共振弛豫时间成象的方法,及人体正常组织、良性及恶性肿瘤的活体(in vivo)T1,T2数值的测量,将有助于实现肿瘤识别的定量方法。     

Water dynamics in ionic magnetic colloids studied by H nuclear magnetic resonance

In a previous nuclear magnetic resonance (NMR) study we observed that the NMR spectra of water in both surfacted and ionic ferrofluids are asymmetric and several orders of magnitude wider than the one of pure water. It has been proposed that this effect is produced by extremely strong magnetic field gradients in the intergrain volume and/or by surface interactions between the carrier liquid molecules and the grains surface. In the case of aqueous ionic ferrofluids the latter possibility should be interpreted as electric interactions between water (polar) molecules and the charges in the grain surface.

In this work we study a series of ionic and surfacted ferrofluids prepared at different magnetic grain concentrations and sizes, and with different surface charge densities. Our experiments clearly show that the sign and the density of the electric charge on the magnetic grains have no influence on NMR spectra. On the other hand, spectral widths increase with the magnetic grain concentration.     

多孔介质渗透率的NMR测定

介绍了利用NMR T₂ 弛豫数据求取岩心物性参数--渗透率的方法. 国外学者在分析了大量数据的基础上,建立了3种由T₂ 弛豫数据计算渗透率的模型,分别简称为SDR,Coates-cutoff和Coates-sbvi. 其中SDR模型不受束缚水计算方法的影响,但对岩心孔隙中流体的性质很灵敏,比较适合于水基泥浆地层. coates-cutoff和Coates-sbvi模型对束缚水的计算精度很敏感,可动和不可动流体孔隙体积的测定对渗透率的计算结果影响也很大. 此外,这三种模型对于低渗透率岩石的计算误差都较大. 通过对不同类型岩心的T₂ 弛豫特性和用常规方法测得的渗透率进行系统分析,在SDR模型的基础上所建立的渗透率测定方法（SDR-REV）有三个可调整参数,计算渗透率适用范围更大,计算的结果与常规实验值更接近. 把SDR-REV方法用于砂岩、砾岩、凝灰岩和火成岩四类岩心样品渗透率的测定,说明SDR-REV方法具有更普遍的适用性. 特别是对于中国普遍存在的低渗透岩心,测定结果更为准确.     

Wave properties of a methyl group under ambient conditions

Liquid-phase NMR studies on hindered rotation of methyl group in a 9-methyltriptycene derivative are reported where the standard, classical jump model of the methyl dynamics proves inadequate. On the other hand, accurate reproduction of the observed NMR line shape effects is afforded by the use of a recent quantum mechanical model in which the relevant methyl dynamics are described in terms of two quantum rate (coherence-damping) processes, characterized by two different rate constants. For ambient temperatures, such a direct evidence of the quantum nature of a rate process generally believed to be classical seems to have no precedence in the literature.     

不均匀不稳定磁场下高分辨液体核磁共振新技术的研究进展

高分辨核磁共振（Nuclear Magnetic Resonance,NMR）谱的获得通常需要高度稳定且均匀的强静磁场. 阻抗磁体或阻抗－超导混合磁体可获得比超导磁体高得多的磁场, 但它们的磁场的稳定性与均匀性比较差;另一方面, 在活体定域波谱研究中,样品内部组分的磁化率差异,运动或生理活动等作用将不可避免地导致磁场的不均匀不稳定,并且这些不稳定不均匀性无法通过锁场匀场等传统的方法消除. 基于分子间零量子相干的方法、空间编码单扫描快速方法、反卷积技术等日渐成为在不均匀不稳定磁场下获取高分辨率的NMR谱的研究热点.     

Magnetic field dependence of13C photo-CIDNP MAS NMR in plant photosystems I and II

Photochemically induced dynamic nuclear polarization is observed in the two photosynthetic reaction centers of plants, photosystem I (PSI) and photosystem II (PSII) by¹³C magic-angle spinning nuclear magnetic resonance (NMR) at three different magnetic fields 17.6, 9.4, and 4.7 T. There is a significant difference in field dependence detected in the light-induced signal pattern of the two photosystems. For PSII the optimal NMR enhancement factor of about 5000 is observed at 4.7 T. On the other hand, the maximal light-induced signals of PSI are observed at 9.4 T.     

Multiple Quantum NMR in One-Dimensional and Nano-Scale Systems: Theory and Computer Simulations

We investigate several exactly solvable models of multiple quantum (MQ) NMR dynamics. We study MQ NMR dynamics of one-dimensional systems (chains and rings) and nano-voids filled with spin-carrying atoms or molecules in a strong external magnetic field. Our focus is the problem of the profile of MQ NMR coherences (i.e., the dependence of the intensities of MQ NMR coherences on their orders). We find that integrable one-dimensional systems exhibit peculiar behavior that does not shed much light on a more generic situation. On the other hand, important lessons can be extracted from our solution for the nano-scale systems. We find that the profile of the intensities of the MQ NMR coherences is rather exponential than Gaussian as was proposed earlier. We also address the cluster growth in the course of the evolution of MQ NMR coherences.     

Simple device for dissolution and sample transfer for applications in spin-hyperpolarization

ABSTRACT

Rapid dissolution and transfer of samples are crucial steps in hyperpolarization methods such as dissolution dynamic nuclear polarization (dDNP) and quantum-rotor-induced polarization (QRIP). Here we introduce a simple and modular dissolution transfer device, and we demonstrate its application for QRIP. This device operates with low pressures and solvent volumes compared to state-of-the-art dDNP setups. On the other hand, transfer times are longer, although sufficient for ¹³C NMR spectroscopy. Our approach does not require an additional cryostat.