Signal enhancement for the sensitivity-limited solid state NMR experiments using a continuous, non-uniform acquisition scheme

We describe a sampling scheme for the two-dimensional (2D) solid state NMR experiments, which can be readily applied to the sensitivity-limited samples. The sampling scheme utilizes continuous, non-uniform sampling profile for the indirect dimension, i.e. the acquisition number decreases as a function of the evolution time (t1) in the indirect dimension. For a beta amyloid (Aβ) fibril sample, we observed overall 40-50% signal enhancement by measuring the cross peak volume, while the cross peak linewidths remained comparable to the linewidths obtained by regular sampling and processing strategies. Both the linear and Gaussian decay functions for the acquisition numbers result in similar percentage of increment in signal. In addition, we demonstrated that this sampling approach can be applied with different dipolar recoupling approaches such as radiofrequency assisted diffusion (RAD) and finite-pulse radio-frequency-driven recoupling (fpRFDR). This sampling scheme is especially suitable for the sensitivity-limited samples which require long signal averaging for each t1 point, for instance the biological membrane proteins where only a small fraction of the sample is isotopically labeled.     

Signal enhancement in laser spectroscopy of metastable states

A two laser excitation scheme has been applied to Ca atoms in an atomic beam. It permits to transfer narrow Doppler-free signals from a weak transition into a strong resonance line. This leads to a large increase of the signal-to-noise ratio and is of relevance for the application of the Ca intercombination transition as a possible new standard in the optical range.     

Signal enhancement in solid-state NMR of quadrupolar nuclei

Recent progress in the development and application of signal enhancement methods for NMR of quadrupolar nuclei in solids is presented. First, various pulse schemes for manipulating the populations of the satellite transitions in order to increase the signal of the central transition (CT) in stationary and rotating solids are evaluated (e.g., double-frequency sweeps, hyperbolic secant pulses). Second, the utility of the quadrupolar Carr–Purcell–Meiboom–Gill (QCPMG) and WURST-QCPMG pulse sequences for the rapid and efficient acquisition of particularly broad CT powder patterns is discussed. Third, less frequently used experiments involving polarization transfer from abundant nuclear spins (cross-polarization) or from unpaired electrons (dynamic nuclear polarization) are assessed in the context of recent examples. Advantages and disadvantages of particular enhancement schemes are highlighted and an outlook on possible future directions for the signal enhancement of quadrupolar nuclei in solids is offered.     

Sensitivity enhancement in multiple-quantum NMR experiments with CPMG detection

We present a modified multiple-quantum (MQ) experiment, which implements the Carr-Purcell-Meiboom-Gill (CPMG) detection scheme in the static MQ NMR experiment proposed by W. S. Warren et al. (1980, J. Chem. Phys.73, 2084-2099) and exploited further by O. N. Antzutkin and R. Tycko (1999, J. Chem. Phys.110, 2749-2752). It is demonstrated that a significant enhancement in the sensitivity can be achieved by acquiring echo trains in the MQ experiments for static powder samples. The modified scheme employing the CPMG detection was superior to the original MQ experiment, in particular for the carbonyl carbon with a very large chemical shift anisotropy.     

Signal enhancement and background cancellation in collinear two-dimensional spectroscopies

We present a polarization method that significantly improves the signal-to-noise ratio in two-dimensional (2D) spectra collected in a "pump-probe" phase-matching geometry by improving the signal strength and eliminating unwanted background signals. This beam geometry is particularly useful when collecting 2D spectra using a pulse shaper.     

Signal enhancement in a r.f. SQUID using stochastic resonance

Summary We describe an experiment on a simple superconducting loop with a Josephson junction subject to a time-sinusoidal magnetic flux embedded in a noise background. The response is shown to display thestochastic-resonance effect, wherein the output signal-to-noise-ratio passes through a maximum at a critical value of the noise strength. Escape times probability density functions are also obtained experimentally Paper presented at the International Workshop ?Fluctuations in Physics and Biology: Stochastic Resonance, Signal Processing and Related Phenomana?, Elba, 5–10 June 1994.     

High-resolution NMR spectra in inhomogeneous fields utilizing the CRAZED sequence without coherence selection gradients

Coherence selection gradients have been considered as indispensable for high-resolution NMR spectroscopy in inhomogeneous fields utilizing the CRAZED-type sequences. However, our experimental results demonstrate that these gradients can be omitted if an appropriate phase cycling is applied. The measured linewidth of reconstructing 1D high-resolution spectral peaks does not depend on the dipolar correlation distance determined by the coherence selection gradients, but is only affected by diffusion and T(2) relaxation. This finding suggests the need to reconsider the mechanism for the iMQC-based high-resolution spectroscopy.     

Signal enhancement in 5QMAS spectra of spin-5/2 quadrupolar nuclei

5QMAS experiments on spin-5/2 systems display a low sensitivity compared with their 3QMAS counterparts. Nevertheless, the superior resolution of 5QMAS over 3QMAS makes these experiments a favorable choice for many materials. We report an enhancement scheme for the 5QMAS experiment, using an improved five-quantum excitation pulse scheme combined with a FAM-II conversion pulse. The results are verified experimentally on a polycrystalline sample of gamma-(27)Al(2)O(3), showing an enhancement factor of 2.4 over the simple two-pulse (CW) 5QMAS scheme. Numerical computations of the efficiency parameter epsilon support these results.     

Signal enhancement in Rayleigh wave interactions using a laser-ultrasound/EMAT imaging system

Enhancement of signal amplitudes from Rayleigh wave interaction at solid surface features has been investigated when signals were detected by an in-plane electromagnetic acoustic transducer (EMAT). A laser-ultrasound system was used to inspect surface-breaking slots, serving as artificial defects. Nd:YAG laser pulses were delivered onto a metal surface via an optical fiber and focused to a line source by a cylindrical lens. An in-plane EMAT receiver detected transient surface acoustic waves. A-scan signals and B-scan images from surface defects revealed increased signal amplitude up to 2.8+/-0.3 depending on the distance of the transducer from a slot. An explanation is based on the interaction of the EMAT sensor with the Rayleigh wave. A supporting computer model was derived to show that experimental signal enhancements were consistent with numerical predictions.     

Resolution enhancement in 13C and 15N magic-angle turning experiments with TPPM decoupling

Many solid-state spectra have been shown to have problems related to the poor proton decoupling of carbon nuclei in methylene groups under conditions of slow magic-angle turning. Two-pulse phase-modulation (TPPM) decoupling during the 2D PHORMAT chemical shift separation experiment is shown to be more effective in comparison to that obtainable at much higher spin rates using conventional CW decoupling. TPPM decoupling can also alleviate similar inadequacies when observing the 15N nucleus, particularly with NH2 groups. This is demonstrated in the 15N resonances of fully labeled l-arginine hydrochloride, where a line narrowing of about a factor of two was observed at moderate rotation rates. This significant advantage was also obtained at turning frequencies as low as 500 Hz.     

Sensitivity to local dipole fields in the CRAZED experiment: an approach to bright spot MRI

Local dipole fields such as those created by small iron-oxide particles are used to produce regions of low intensity (dark contrast) in many molecular magnetic resonance imaging applications. We have investigated, with computer simulations and experiments at 17.6 T, how the COSY revamped with asymmetric z-gradient echo detection (CRAZED) experiment that selects intermolecular double-quantum coherences can also be used to visualize such local dipole fields. Application of the coherence-selection gradient pulses parallel to the main magnetic field produced similar, dark contrast as conventional gradient echo imaging. Application of the gradient along the magic angle leads to total loss of signal intensity in homogeneous samples. In the presence of local dipole fields, the contrast was inverted and bright signals from the dipoles were observed over a very low background. Both simulations and experiments showed that the signal strongly decreased when a phase-cycle suppressing single-quantum coherences was employed. Therefore, we conclude that most of the signal comes from directly refocused magnetization or intermolecular single-quantum coherences. Finally, we demonstrate that bright contrast from local dipole fields can also be obtained, when the pair of coherence-selection gradient pulses is deliberately mismatched. Both methods allowed visualization of local dipole fields in phantoms in experimental times of about 3 min.     

Signal enhancement by diffusion: experimental observation of the "DESIRE" effect

Inadequate signal-to-noise ratio is a major factor limiting applications of magnetic resonance microscopy. The "Diffusion Enhancement of Signal and Resolution" (DESIRE) scheme promises potential sensitivity enhancements of between one and three orders of magnitude, but images using this mechanism have not been shown to date. Here, we report the first images obtained using the DESIRE method, and obtain excellent agreement between numerical simulations and experimental data with signal-to-noise enhancements of close to one order of magnitude.     

Signal enhancement in the triple-quantum magic-angle spinning NMR of spins-3/2 in solids: the FAM-RIACT-FAM sequence

We achieve a significant signal enhancement for the triple-quantum magic-angle spinning NMR of a spin-3/2 system, by using an amplitude-modulated radiofrequency field, followed by a selective 90 degrees pulse and a phase-shifted strong rf field, for the triple-quantum excitation, and an amplitude-modulated radiofrequency field for the conversion of triple-quantum coherence to observable single-quantum coherence. The experiment is demonstrated on the (87)Rb NMR of polycrystalline rubidium nitrate.     

The effect of experimental parameters on the signal decay in double-PGSE experiments: negative diffractions and enhancement of structural information

Double pulsed gradient spin echo (d-PGSE) experiment has been recently suggested for detecting microscopic anisotropy in macroscopically isotropic samples. This sequence is complex and has many variables, including, intra alia, combinations of directions and amplitudes of the pulsed gradients, diffusion times in each of the encoding periods and the mixing time period. The effect of these experimental parameters of the d-PGSE sequence was studied in an array of water filled microcapillaries of micron diameters. We found that negative diffractions occur, as indeed predicted by recently published simulations. We also found differential effects of prolongation of the mixing time between collinear and orthogonal d-PGSE experiments. The d-PGSE experiment in the collinear direction perpendicular to the long axis of the cylinder exhibited a marked dependence on the mixing time, while the orthogonal d-PGSE experiment exhibited no such dependence at all. Interestingly, one of the most important predictions by the simulations was that the d-PGSE sequence could potentially discriminate between compartments of different sizes better than the single PGSE (s-PGSE) and it seems that our experimental results indeed corroborate these predictions.     

Signal enhancement of a novel multi-address coding lidar backscatters based on a combined technique of demodulation and wavelet de-noising

Multi-address coding (MAC) lidar is a novel lidar system recently developed by our laboratory. By applying a new combined technique of multi-address encoding, multiplexing and decoding, range resolution is effectively improved. In data processing, a signal enhancement method involving laser signal demodulation and wavelet de-noising in the downlink is proposed to improve the signal to noise ratio (SNR) of raw signal and the capability of remote application. In this paper, the working mechanism of MAC lidar is introduced and the implementation of encoding and decoding is also illustrated. We focus on the signal enhancement method and provide the mathematical model and analysis of an algorithm on the basis of the combined method of demodulation and wavelet de-noising. The experimental results and analysis demonstrate that the signal enhancement approach improves the SNR of raw data. Overall, compared with conventional lidar system, MAC lidar achieves a higher resolution and better de-noising performance in long-range detection.     

Signal enhancement using 45 degrees water flipback for 3D 15N-edited ROESY and NOESY HMQC and HSQC.

A novel implementation of the water flipback technique employing a 45 degrees flip-angle water-selective pulse is presented. The use of this water flipback technique is shown to significantly enhance signal in 3D 15N-edited ROESY in a 20 kDa complex of the vnd/NK-2 homeodomain bound to DNA. The enhancement is seen relative to the same experiment using weak water presaturation during the recovery delay. This enhancement is observed for the signals from both labile and nonlabile protons. ROESY and NOESY pulse sequences with 45 degrees water flipback are presented using both HMQC and HSQC for the 15N dimension. The 45 degrees flipback pulse is followed by a gradient, a water selective 180 degrees pulse, and another gradient to remove quadrature images and crosspeak phase distortion near the water frequency. Radiation damping of the water magnetization during the t1 and t2 evolution periods is suppressed using gradients. Water resonance planes from NOESY-HMQC and NOESY-HSQC spectra show that the HMQC version of the pulse sequences can provide stronger signal for very fast exchanging protons. The HSQC versions of the ROESY and NOESY pulse sequences are designed for the quantitative determination of protein-water crossrelaxation rates, with no water-selective pulses during the mixing time and with phase cycling and other measures for reducing axial artifacts in the water signal.     

Scaling in semi-inclusive experiments

In bubble chamber experiments (in contrast to counter experiments) the semi-inclusive experiment a+b→c+(n−1) charged + anything neutral is more natural than the corresponding inclusive experiment a+b→c+anything. We argue that the cross sections for semi-inclusive experiments have very neat scaling properties.     

物理学中的示零实验

示零实验采用完全补偿法 ,在物理实验中具有独特的作用 .本文介绍了示零实验在提高测量精度、修正系统误差和为理论提供依据方面的特殊功能