仲氢诱导极化增强的核磁共振实验条件优化

仲氢诱导极化(Parahydrogen Induced Polarization, PHIP)技术能够极大地增强核磁共振信号,在化学、生物、医学等多方面具有广阔的应用前景．但在实际应用中,通过PHIP技术获得的核磁共振(NMR)信号增强倍数往往受到实际反应条件的影响．该文中以己炔的加氢反应为例,考察了氢气通入方式、反应温度和反应压强对PHIP实验中核磁共振信号增强倍数的影响．     

利用高温超导直流量子干涉器件进行10$lt;sup$gt;-6$lt;/sup$gt; T量级磁场下核磁共振的研究

研究了水样品在10^-6 T量级磁场下的核磁共振谱.核磁共振信号由一个工作在液氮温度的高温超导直流量子干涉仪记录,测量在一个简易磁屏蔽室中进行.在7—70 μT的磁场范围内都观察到了15 ml水样品的核磁共振信号.相应的^1H的核磁共振频率为300—3000 Hz.在实验中获取的单次测量信噪比约为4,通过对信号的100次平均,信噪比可达到约40.进一步讨论了剩余磁场、预极化时间和采样时间对结果的影响.最后用数字滤波之后平均的方法初步得到了时域的自由感应衰减信号. 关键词： 超导量子干涉仪 核磁共振     

核磁共振实验中调制磁场的作用

介绍了一种用示波器观察核磁共振的实验装置 ,并着重分析了利用调制磁场捕捉核磁共振信号的原理、方法。     

利用高温超导直流量子干涉器件进行10-6 T量级磁场下核磁共振的研究

研究了水样品在10-6 T量级磁场下的核磁共振谱.核磁共振信号由一个工作在液氮温度的高温超导直流量子干涉仪记录,测量在一个简易磁屏蔽室中进行.在7-70 μT的磁场范围内都观察到了15 ml水样品的核磁共振信号.相应的1 H的核磁共振频率为300-3000 Hz.在实验中获取的单次测量信噪比约为4,通过对信号的100次平均,信噪比可达到约40.进一步讨论了剩余磁场、预极化时间和采样时间对结果的影响.最后用数字滤波之后平均的方法初步得到了时域的自由感应衰减信号.     

阿达玛变换在核磁共振成象中的应用

阿达玛变换应用到核磁共振成象技术中,能提高成象技术的灵敏度。本文阐述了阿达玛变换在线扫描核磁共振成象中应用原理,推出了合成的激发信号相位与阿达玛编码关系。得到频率合成的激发信号相位表,据该表合成的激发信号产生多个自旋回波,能使核磁共振成象技术速度快、灵敏度高。文中还对该方法作了深入的讨论。     

DPSD在低场核磁共振回波信号检测中的应用

核磁共振回波信号幅度微弱,容易受到来自电子器件和外部环境噪声的干扰,要求回波检测方法既能实时采集回波数据,又能较好的抑制噪声. 对比分析不同微弱信号检测方法的优缺点,归纳出DPSD(Digital Phase-Sensitivity Detection)方法在回波检测应用中的优越性. 通过仿真计算, 提出适用于回波信号检测的最佳滤波器窗函数. 在自制的核磁共振仪器上进行实验,结果表明,DPSD方法在满足回波信号实时测量的同时,有效压制了噪声,能准确的提取出低场核磁共振回波信号的幅度和相位信息.     

基于小波滤波的低场NMR纤维上油率检测新方法

针对目前低场核磁共振纤维上油率检测存在的问题,提出了一种基于小波变换的纤维上油率检测新方法. 首先,用低场核磁共振采集标准纤维自由感应衰减信号进行线性拟合得到定标曲线;然后,用测试纤维采集多组叠加次数不同的核磁共振信号,并分别进行小波软阈值滤波;最后,将滤波后的多组结果代入定标曲线计算纤维的上油率. 检测结果和实际应用表明小波软阈值滤波可有效去除纤维FID信号中的噪声并大幅缩短检测时间. 此方法可为低场核磁共振纤维上油率快速、准确检测奠定基础.     

扫场对核磁共振测量的影响

在连续波核磁共振实验中，通常采用低频扫场产生重复再现的共振吸收信号。当处于磁场中的射频线圈引线回路等效面积不为零时，简谐扫场必然引起该闭合回路的磁通量变化，由此而产生同频简谐感生电动势并与核磁共振信号叠加共同构成振荡器输出信号。由于扫场上升和下降过程的感生电动势方向相反，从而扫场前半周和后半周所对应的共振吸收测量信号存在差异。实验结果表明：扫场强度及方向对核磁共振测量影响来源于实验测量技术缺陷，而非核磁共振的物理本质。     

利用核磁共振测量乙醇汽油溶液浓度

利用核磁共振成像分析仪测量了不同汽油体积含量的乙醇汽油溶液的核磁共振信号,分析了横向弛豫时间、信号强度与汽油浓度的关系.结果表明乙醇汽油溶液中汽油的体积含量与信号强度呈线性关系,因此利用低磁场核磁共振可以测量乙醇汽油浓度.     

样品弛豫时间对核磁共振信号的影响研究

研究了不同浓度CuSiO4水溶液样品的核磁共振信号的特点,讨论了在特定的磁场扫场周期下,样品横向弛豫时间对共振信号的影响.发现当样品的横向弛豫时间远远大于扫场周期时,微观磁矩的退相是造成核磁共振信号衰减的主要因素,此时在共振点前后都会形成周期性的振荡信号.     

Impurity proton NMR signals from common "proton-free" laboratory materials

For the study of small samples (tens of microns cubed) by NMR, impurities from the environment and construction materials (Teflon, Kel-F, glass NMR tubes, etc.) can dominate the signal, in particular for proton NMR. Using pulsed NMR with a resolution of several microseconds, we have studied a number of common construction materials considered to be proton-free and find considerable proton impurity. We present results in terms of impurity proton spins per milligram and discuss procedures to minimize the effects of impurity signal.     

利用相位步进脉冲消除探头13C NMR背景信号

由静态探头线圈外有机材料产生的¹³C NMR背景信号强度大，化学位移范围广（δ_C 20~250），此背景信号在交叉极化实验中还可被增强，并随着样品信号的累积而累积，严重影响谱图分析.将相位步进脉冲引入交叉极化实验（称为PIPCP）中可以有效去除经交叉极化增强的¹³C NMR背景信号，但样品信号不受影响.这是由于经过相位步进脉冲后，线圈外相位严重畸变，而且线圈外锁定场强度急剧降低，来自探头材料的¹³C NMR背景信号无法有效地进行交叉极化.而对于被测样品甘氨酸来说，由于I核和S核之间强烈的偶极耦合作用，所加相位步进脉冲对锁定场强度的影响只有1.4%.     

Nuclear-magnetic-resonance evidence for charge inhomogeneity in stripe ordered La(1.8-x)Eu0.2Sr(x)CuO4

We report 17O nuclear-magnetic-resonance (NMR) results in the stripe ordered La(1.8-x)Eu0.2Sr(x)CuO4 system. Below a temperature T(q) approximately 80 K, the local electric field gradient and the absolute intensity of the NMR signal of the planar O site exhibit a dramatic decrease. We interpret these results as microscopic evidence for a spatially inhomogeneous charge distribution, where the NMR signal from O sites in the domain walls of the spin density modulation are wiped out due to large hyperfine fields, and the remaining signal arises from the intervening Mott insulating regions.     

Direct nuclear resonance detection of second-order weak quadrupole effects

This direct method of detecting anisotropic effects of the second and higher orders in NMR systems with weak nuclear quadrupole interaction with a high signal/noise ratio, characteristic of standard NMR sweep spectroscopy, is based on orientationally modulated NMR (OM NMR). Expressions are derived to describe the observed OM NMR absorption signals and the factors determining the signal shape are analyzed. The main theoretical results are supported by experiment. Attention is drawn to the possible use of the effects under consideration for NMR analyses of crystals.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 9, pp. 110–115, September, 1991.     

The application of steady-state free precession in rapid 2DFT NMR imaging: FAST and CE-FAST sequences

In the classic spectroscopic steady-state free precession (SSFP) experiment, a regular sequence of phase-coherent radio frequency pulses is applied with constant flip angle and a repetition time shorter than the NMR relaxation times of the sample. As the steady state is reached, an NMR signal appears between pulses that consists of two distinct components: a free induction signal following the RF pulses and decaying during the repetition interval and a spin-echo-like signal forming at its end prior to the subsequent RF pulse. Both signals may be exploited for NMR imaging if the gradient schemes fulfill the phase coherence requirements of SSFP. This article describes two Fourier acquired steady-state sequences dubbed FAST and CE-FAST, which may be used for the rapid acquisition of NMR images from the SSFP signals.     

Modulation effects in non-drilling NMR in the Earth’s field

The paper describes the variant of nuclear magnetic resonance (NMR) in the Earth’s field using no prepolarization. This method can be employed to record the NMR signal of underground proton-containing liquids, such as water, located at the depth of more than 100 m without drilling. The non-drilling NMR in the Earth’s field is recorded by locating on the surface the circular wire with a diameter of about 100 m. This wire serves as an antenna for the exciting field source and the NMR signal receiver. The radiofrequency pulse with the carrier frequency equal to that of proton resonance in the Earth’s field is passed through the wire. When the exciting pulse is switched off, the induction e.m.f. signal caused by the free Larmor nuclear precession in the geomagnetic fields is observed. An important case when in the non-drilling NMR in the Earth’s field the signal is excited and observed at different frequencies is studied both from theoretical and practical viewpoints. The resulting modulation effects are considered. Such situations arise e.g. either in magnetic rocks or upon magnetic storms.     

Three-dimensional correlated accordion NMR spectroscopy of proteins

A major step toward the protein structure determination by nuclear magnetic resonance (NMR) spectroscopy is the assignment of multidimensional NMR signals that provide through-bond and through-space inter-atomic correlations. Ambiguities often occur during the assignment process due to resonance degeneracy, which challenges high resolution and larger size protein structure determination. Here, we present a method that will significantly improve the efficiency and accuracy of the NMR signal assignment. The method is based on a correlated accordion principle that, when incorporated into conventional three-dimensional (3D) heteronuclear NMR experiments, allows the retrieval of additional frequency correlation information at high resolution. We show that 3D spectra derived from this method are as effective as the impractical high resolution four-dimensional (4D) spectra with substantially reduced signal ambiguity as compared to their conventional counterparts. The approach promises increased accuracy and size of protein structures determined by NMR.     

Measurement of magnetic field intensity by means of NMR. I. Accuracy of measurement

The influence of various parameters (e.g. polarization and intensity of high frequency field, NMR relaxation times, signal to noise ratio of the measuring apparatus) on the determination of NMR resonance point of a nuclear system with exactly known value of gyromagnetic factor is discussed. Special attention is given to the case of real field, which is not stable in time. It is shown that the transverse NMR relaxation time of the nuclei in the sample has to be selected in correlation with the properties of the field (e.g. time instability, spatial inhomogeneity) and of the measuring equipment (e.g. signal to noise ratio), if the lowest obtainable uncertainty of field intensity NMR measurement is to be achieved.     

Solvent-localized NMR spectroscopy using the distant dipolar field: a method for NMR separations with a single gradient

Solvent-localized NMR (SOLO) is a new method which allows the separation of NMR spectra of substances dissolved in different solvents. It uses the selective HOMOGENIZED pulse sequence to produce a two-dimensional NMR spectrum resulting from intermolecular zero-quantum coherences in one distinct solvent. The detected signal is locally refocused by the action of the distant dipolar field, which is created by a frequency selective pulse only in regions containing the selected solvent. The prerequisites are that the different solvents have sufficiently different chemical shifts to be excited separately and that compartments with different solvents are spatially separated by more than the typical diffusion distance. Here, the method is demonstrated for the solvents water and DMSO on a length scale of 0.5 mm. Because signal in the spectra is refocused locally, SOLO is insensitive to variations in the magnetic field which may result from inhomogeneities or structures in the sample. This makes applications in strongly structured samples possible. SOLO is the first method that achieves localization of NMR signal with a single gradient pulse. Therefore, it can be used in conventional NMR spectrometers with one-axis gradient systems and lends itself to a wide range of applications including in vivo NMR.     

MEASUREMENTS OF 129Xe NUCLEAR MAGNETIC RESONANCE IN GASEOUS,LIQUID AND SOLID XENON

Natural xenon, contained in a ceil at a pressure of 6.5 atm, is frozen from 303 to 137 K on an WP-80SY NMR spectrometer. NMR signals of ¹²⁹Xe atoms in gaseous, liquid and solid phases are measured at various temperatures, We found that the chemical shift of NMR signal of liquid ¹²⁹Xe (expressed as ΔH) is directly proportional to the density of the sample with a coefficient of (4.73±0.05)×10^-7; and the chemical shift of NMR signal of solid ¹²⁹Xe (expressed as ΔH) is nearly proportional to the density of the sample with a coefficient of (5.00±0.08)×10^-7.