微量OVARC肽的1H NMR谱线归属

Serpin家族中的卵清蛋白,其反应中心肽段(OVARC,23肽)对应于卵清蛋白序列中343 位至366位残基. 建立在魔角旋转基础之上的Nano探头是一种全新的超微量探头. 本文运用魔角旋转微量检测新技术进行了有关2D NMR实验,完成了卵清蛋白反应中心肽段的¹H NMR 谱线归属.     

单晶化学位移张量测量的二维变角相关谱

描述了谱仪的同步控制装置.利用该装置,在MSL-400潜仪上实现了单晶化学位移张量的二维变角相关谱方法测量,获得了典型单晶的DGO (2NH₃⁺CH₂COO^-·2·COOH)的¹³C化学位移张量。     

HR/MAS高分辨魔角微量探头用于天然橡胶固体1H、13C NMR测试及其与液体BBO探头、固体CP/MAS探头测试的比较

采用BRUKER高分辨魔角微量探头（HR/MAS），液相宽带BBO探头和固体CP/MAS探头，对天然橡胶固体、乳液以及天然橡胶溶于氘代苯的溶液进行了¹H、¹³C 1D和2D NMR谱的测试和比较. 发现HR/MAS探头用于天然橡胶固体和乳液时可以得到高分辨的¹H、¹³C谱，克服了CP/MAS探头测试固体¹³C NMR谱或者是固体¹H NMR谱时，谱图存在S/N值可能较小、谱峰可能宽化的弱点.     

体内31P NMR表面线圈探头的研制

报道一种为进行活体小动物核磁共振实验而研制的体内³¹P NMK表面线圈探头.该探头工作频率为161.83MHz,无载Q值为300,可无损伤地研究生命体内各部位的性质.本文给出了用该探头所测得的小鼠体内肝脏、大腿肌肉、大脑以及大脑缺氧状态下³¹P NMR谱图实例.     

阿糖胞苷HepDirect前药MB07133的波谱特征与晶体结构

用¹H和¹³C NMR和多种2D NMR谱表征了阿糖胞苷的磷酸盐或磷酸酯肝靶向前体药物（HepDirect前药）-- MB07133的结构,对其NMR谱进行了归属;用X-射线单晶衍射测定了单晶的晶体结构．讨论了该化合物的波谱数据和晶体结构数据,验证了其结构的正确性并探讨了其化学结构对药物特性的影响．     

用于木材水分检测的单边核磁共振传感器设计

为了实现对木材水分的无损检测,设计了一种单边核磁共振（unilateral nuclear magnetic resonance,UMR）传感器,该传感器由单边磁体、抗涡流板、射频线圈、阻抗匹配和调谐电路构成．在距离传感器表面上方75 mm处的50 mm×50 mm的平面内,建立了71.1 mT（共振频率为3.027 MHz）的静态磁场．本文详细介绍了该传感器的设计思路和实现方法,并开展了初步的木材水分无损测量实验．对圆柱形树桩的径向水分分布进行了一维扫描测量,观察了水分由树皮向树芯逐步深入过程中横向弛豫时间（T₂）的变化规律,还使用UMR仪对木材干燥过程中水分的挥发进行了测量.实验结果表明,随着干燥的加剧,被测样品T₂谱的长T₂波峰明显左移、积分面积渐减,而且积分面积与木材样品含水率呈正比．本文为木材研究提供了一种便携的NMR测量设备设计方案,且可以实现野外活体树木的无损测量．     

以NMR手段为主进行结构分析一则

某固体化合物极易溶于水但未能制得其单晶.为测定其结构可充分发挥NMR的特长.利用NMR的多种技术,包括常规¹H谱、¹³C谱,一维、二维谱,确定脂肪链X-CH₂-CH₂-CH₂-Y与芳香基团Y的存在;利用¹³C-¹H长程耦合相关谱(用反相探头)可确定脂肪链与芳香基团间的联接关系,于是立即可确定该物的有机主体骨架应为X-CH₂-CH₂-CH₂-Y.从IR谱得知该物除存在C-N基团外,还存在-SO₃-基团等.从元素成分分析和M8谱,包括FAB-MS谱等分析结果,最终推断该固体化合物为丙磺酸吡啶内鎓盐,它的分子结构应为:      

通过高斯加权的1H CPMG弛豫曲线测定橡胶交联密度

CPMG（Carr-Purcell-Meiboom-Gill）回波法是测量橡胶交联密度[常用交联点之间的分子量（M_c）表示]的一种常用核磁共振（NMR）技术,但实验发现通过该技术获得的M_c对于CPMG序列中脉冲间隔时间具有较强的依赖性,导致交联密度NMR测量值与橡胶材料硬度的相关性低.为了克服这一缺点,本文对不同脉冲间隔时间下CPMG实验测得的质子横向驰豫曲线进行高斯加权.通过对高斯加权求和后的质子横向驰豫曲线进行处理分析,实现了对橡胶交联密度更加准确地测量,大幅提升了天然橡胶交联密度NMR测量值与材料硬度的相关性.本文方案测量能获得与¹H DQ NMR方法相当,或比之更佳的交联密度-硬度相关性.同时,本文方案比¹H DQ NMR方法更为高效,整体测量时间缩短为¹H DQ NMR实验时间的1/10.     

混合物理化学气相沉积法制备MgB$lt;sub$gt;2$lt;/sub$gt;单晶纳米晶片的研究

利用混合物理化学气相沉积法在石墨衬底上制备出了晶形为六角结构、厚度不同、径向尺寸不一的MgB₂单晶纳米晶片. 利用纳米定向转移技术将此晶片转移到了碳支持膜铜网上, 以便对其精细结构等物性进行表征. 电输运测量和磁性测量结果都表明晶片具有超导电性: T_conset=38 K, T_c(0)=33 K. 扫描电子显微镜图像表明, 晶片表面平整、厚度分布在几个纳米到200 nm之间, 宽度从几微米到上百微米; 高分辨透射电镜图像显示出晶片具有周期性晶格条纹. 选区电子衍射数据与MgB₂已有的单晶衍射数据相符. 这些测量结果证实了其确为高质量单晶MgB₂超导纳米晶片. 本文不仅提出了一种全新的制备单晶MgB₂的方法, 也观察到了纳米尺度MgB₂单晶的零电阻现象, 为后续的磁通钉扎、纳米力学性能等领域的深入研究提供了合适的素材. 关键词： 2')" href="#">单晶MgB₂ 超导纳米晶片 零电阻 混合物理化学气相沉积法     

高分辨魔角旋转核磁共振技术（HR/MAS）在固相合成中的应用

使用微量探头分析了不同树脂、溶剂、温度对¹H NMR线宽的影响，并运用高分辨魔角旋转核磁共振技术跟踪固相载体上羟基氨基酸的糖基化反应. 该研究表明使用高分辨魔角旋转核磁共振探头可以快速、直接鉴定树脂上的产物，是固相合成中重要的分析工具.     

High-pressure,high-resolution NMR probe working at 400 MHZ

Abstract

A probe for obtaining high-resolution multinuclear NMR spectra at elevated pressures with a Bruker AM-400 spectrometer is described. The probe is designed for pressures up to 200 MPa and has been used between -40 to 150°C. We obtain routinely a resolution of about 1 Hz for proton (400 MHz) spectra using deuterium as an internal field lock. This probe is easily interchangeable with a commercial probe. We also describe a simple sample tube made of a 5 mm commercial NMR tube and a machinable glass cap with a total volume of about 1 cm³.     

Signal-to-noise ratio improvements in in vivo high resolution micro-volume selected spectroscopy

A system capable of in vivo volume selected 1H NMR spectroscopy of voxels as small as 0.2 cm3 is described. Signal-to-noise ratio improvements with probe design and a novel signal steering device are detailed. A high-resolution, image-directed proton spectrum from 0.2 cm3 of a rat's brain at 200 MHz obtained using the SUBMERGE/SPACE pulse sequence is presented. Single-scan voxel shimming was implemented to improve spectral resolution.     

HL-2A等离子体边缘的快速单探针测量

介绍了对HL-2A装置中平面边缘等离子体的单探针测量。单探针是安装在可径向移动、并可绕轴旋 转360o的传动杆上的。在1MHz的快速采样频率下,测量了主等离子体边缘的温度、密度、悬浮电位、空间电位、极 向等离子体流速的径向分布。测量的结果表明,利用单探针测量的主等离子体边缘参数与朗缪尔四探针测量结果 基本一致。     

高能质子单粒子翻转效应的模拟计算

在分析质子与硅反应的基础上,提出质子单粒子翻转截面理论计算模型,建立了模拟计算方法.计算得到了不同能量的高能质子在存储单元的灵敏区内沉积的能量.指出高能质子主要通过与硅反应产生的重离子在存储单元灵敏区内沉积能量,产生电荷,导致单粒子效应,得到了单粒子翻转截面与质子能量以及随临界电荷变化的关系.并将计算得到的单粒子翻转截面与实验数据进行了比较.     

ENDOR evidence for the quantum exchange of the methylene protons

ENDOR spectroscopy was used for studying methylene proton couplings in the 6-yl (or H-addition) radical in a single crystal of 1-methyluracil at 4.2K. The two methylene protons were magnetically equivalent in all crystal (radical) orientations in the magnetic field, indicating proton quantum exchange. The two protons compose magnetically single entity with spin I=1. The observed small ENDOR line splittings of about 0.60MHz agree well with the theoretical expectations for such a system.     

The radio-frequency design of an iris-type coupler for the CPHS radio-frequency quadrupole

The Compact Pulsed Hadron Source (CPHS) project is a university-based proton accelerator platform (13 MeV, 16 kW, 50 mA peak current, 0.5 ms pulse width at 50 Hz) for multi-disciplinary neutron and proton applications. The CPHS linac consists of a 3 MeV radio-frequency quadrupole (RFQ) linac and a 13 MeV drift tube linac (DTL). Both the RFQ and DTL share a 325 MHz, 2.1 MW klystron source. A single iris-type radio-frequency (RF) coupler is used to feed 537 kW of RF power to the RFQ cavity. Three-dimensional electromagnetic models of the ridge-loaded tapered waveguide (RLWG) and the coupler-cavity system are presented, and the design process and results of the RLWG and iris plate are described in detail.     

The effect of dexamethasone on tissue water distribution and proton relaxation in Panc02 tumors

The present experiments were conducted to determine the effects of dexamethasone mediated changes in tumor water distribution on proton relaxation times (T1, T2) in a murine pancreatic adenocarcinoma (Panc02). Spin lattice (T1) and spin-spin (T2) relaxation times were determined by ex vivo methods (10MHz) and by in vivo imaging techniques (6.25 MHz) at various intervals after single or multiple dexamethasone treatments. In complementary studies, dexamethasone mediated changes in tumor capillary permeability, tumor water distribution, relative tumor blood flow and tumor cell proliferation were also determined.

Proton spin lattice (T1) and spin-spin (T2 relaxation times for Panc02 tumors shortened within two hours of a single dexamethasone treatment. The time course and magnitude of this response was dexamethasone dose dependent. The time dependent changes in T1 and T2 after dexamethasone were similar at 10 MHz (ex vivo) and 6.25 MHz (in vivo imaging). Although dexamethasone produced little or no change in total tumor water content and tumor cell proliferation, transient changes in the physiologic distribution of tumor water were clearly demonstrated.

The data supports the idea that dexamethasone induced changes in the distribution of tumor water were mediated by changes in capillary permeability and tumor blood flow. These physiologic responses produced serial changes in tumor extracellular extravascular water content that were consistent with the observed changes in tumor T1 and T2. The results from these experiments might imply that therapy associated changes in tumor proton relaxation times may not only reflect changes in tissue water content, but may also reflect physiologic responses which alter the distribution of tissue water and solute.     

A multi‐MHz single‐shot data acquisition scheme with high dynamic range: pump–probe X‐ray experiments at synchrotrons

The technical implementation of a multi‐MHz data acquisition scheme for laser–X‐ray pump–probe experiments with pulse limited temporal resolution (100 ps) is presented. Such techniques are very attractive to benefit from the high‐repetition rates of X‐ray pulses delivered from advanced synchrotron radiation sources. Exploiting a synchronized 3.9 MHz laser excitation source, experiments in 60‐bunch mode (7.8 MHz) at beamline P01 of the PETRA III storage ring are performed. Hereby molecular systems in liquid solutions are excited by the pulsed laser source and the total X‐ray fluorescence yield (TFY) from the sample is recorded using silicon avalanche photodiode detectors (APDs). The subsequent digitizer card samples the APD signal traces in 0.5 ns steps with 12‐bit resolution. These traces are then processed to deliver an integrated value for each recorded single X‐ray pulse intensity and sorted into bins according to whether the laser excited the sample or not. For each subgroup the recorded single‐shot values are averaged over ～10⁷ pulses to deliver a mean TFY value with its standard error for each data point, e.g. at a given X‐ray probe energy. The sensitivity reaches down to the shot‐noise limit, and signal‐to‐noise ratios approaching 1000 are achievable in only a few seconds collection time per data point. The dynamic range covers 100 photons pulse^?1 and is only technically limited by the utilized APD.     

Achievement of a 920-MHz high resolution NMR

We have developed a 920-MHz NMR system and performed the proton NMR measurement of H(2)O and ethylbenzene using the superconducting magnet operating at 21.6 T (920 MHz for proton), which is the highest field produced by a superconducting NMR magnet in the persistent mode. From the NMR measurements, it is verified that both homogeneity and stability of the magnet have a specification sufficient for a high resolution NMR.     

The ultrasonic probe for the investigating of internal object structure by ultrasound transmission tomography

The main component of every device used for investigating internal object structure by Ultrasound Transmission Tomography (UTT) is a special ultrasonic probe. This paper presents the structure of model multielement ring probe for examining objects using this method in divergent ray projection geometry. The probe is made up of 1024 rectangular separate piezoelectric transducers working at frequency f=1.7 MHz, placed inside a ring with diameter D=30 cm and height h=9 cm. Each element of the probe is equipped with a quarter-wave matching layer. All the transducers function as transmitters and receivers, and can be joined in groups both during transmitting and during receiving. Some examples of admittance characteristics of a single piezoelectric transducer and examples of shapes of pulses generated and received by particular transducers were presented. Important factors affecting the measurement resolution are the sizes of the active surface of the transducers.