scholarly journals Relaxation-induced dipolar exchange with recoupling (RIDER) distortions in CODEX experiments

2020 ◽  
Vol 1 (2) ◽  
pp. 247-259
Author(s):  
Alexey Krushelnitsky ◽  
Kay Saalwächter
Keyword(s):  
Time Dependence ◽  
Mixing Time ◽  
Chemical Shift Anisotropy ◽  
Dipolar Interaction ◽  
Quantitative Information ◽  
Back Exchange ◽  
Rocking Motion ◽  
Rigid Model ◽  
Model Substances ◽  
Spin Flips

Abstract. Chemical shift anisotropy (CSA) and dipolar CODEX (Cenralband Only Detection of EXchange) experiments enable abundant quantitative information on the reorientation of the CSA and dipolar tensors to be obtained on millisecond–second timescales. At the same time, proper performance of the experiments and data analysis can often be a challenge since CODEX is prone to some interfering effects that may lead to incorrect interpretation of the experimental results. One of the most important such effects is RIDER (relaxation-induced dipolar exchange with recoupling). It appears due to the dipolar interaction of the observed X nuclei with some other nuclei, which causes an apparent decay in the mixing time dependence of the signal intensity reflecting not molecular motion, but spin flips of the adjacent nuclei. This may hamper obtaining correct values of the parameters of molecular mobility. In this contribution we consider in detail the reasons why the RIDER distortions remain even under decoupling conditions and propose measures to eliminate them. That is, we suggest (1) using an additional Z filter between the cross-polarization (CP) section and the CODEX recoupling blocks that suppresses the interfering anti-phase coherence responsible for the X-H RIDER and (2) recording only the cosine component of the CODEX signal since it is less prone to the RIDER distortions in comparison to the sine component. The experiments were conducted on rigid model substances as well as microcrystalline 2H ∕ 15N-enriched proteins (GB1 and SH3) with a partial back-exchange of labile protons. Standard CSA and dipolar CODEX experiments reveal a fast-decaying component in the mixing time dependence of 15N nuclei in proteins, which can be misinterpreted as a slow overall protein rocking motion. However, the RIDER-free experimental setup provides flat mixing time dependences, meaning that the studied proteins do not undergo global motions on the millisecond timescale.

scholarly journals RIDER distortions in the CODEX experiments

2020 ◽  
Author(s):  
Alexey Krushelnitsky ◽  
Kay Saalwächter
Keyword(s):  
Time Dependence ◽  
Mixing Time ◽  
Dipolar Interaction ◽  
Quantitative Information ◽  
Back Exchange ◽  
Rocking Motion ◽  
Time Dependencies ◽  
Millisecond Time Scale ◽  
Rigid Model ◽  
Spin Flips

Abstract. CSA and dipolar CODEX experiments enable obtaining abundant quantitative information on the reorientation of the CSA and dipolar tensors on the millisecond-second time scales. At the same time, proper performance of the experiments and data analysis can often be a challenge since CODEX is prone to some interfering effects that may lead to incorrect interpretation of the experimental results. One of the most important such effects is RIDER (Relaxation Induced Dipolar Exchange with Recoupling). It appears due to the dipolar interaction of the observed X-nuclei with some other nuclei, which causes an apparent decay in the mixing time dependence of the signal intensity reflecting not molecular motion but spin-flips of the adjacent nuclei. This may hamper obtaining correct values of the parameters of molecular mobility. In this contribution we consider in detail the reasons, why the RIDER distortions remain even under decoupling conditions and propose measures to eliminate them. Namely, we suggest the additional Z-filter between the cross-polarization section and the CODEX recoupling blocks, which suppresses the interfering anti-phase coherence responsible for the X-H RIDER. The experiments were conducted on rigid model substances as well as microcrystalline 2H/15N-enriched proteins (GB1 and SH3) with a partial back-exchange of labile protons. Standard CSA and dipolar CODEX experiments reveal a fast decaying component in the mixing time dependence of 15N nuclei in proteins, which can be interpreted as a slow overall protein rocking motion. However, the RIDER-free experimental setup provides flat mixing time dependencies meaning that the studied proteins do not undergo global motions on the millisecond time scale.

Some Results of the Spectroscopic Study of Four Close Binary Systems of Early Spectral Types

1965 ◽  
Vol 5 ◽  
pp. 120-130
Author(s):  
T. S. Galkina
Keyword(s):  
Spectroscopic Study ◽  
Spectral Type ◽  
Spectroscopic Investigation ◽  
Binary Systems ◽  
Quantitative Information ◽  
Close Binary ◽  
Physical Parameters ◽  
Absorption And Emission ◽  
Close Binary Systems ◽  
Quantitative Estimates

It is necessary to have quantitative estimates of the intensity of lines (both absorption and emission) to obtain the physical parameters of the atmosphere of components.Some years ago at the Crimean observatory we began the spectroscopic investigation of close binary systems of the early spectral type with components WR, Of, O, B to try and obtain more quantitative information from the study of the spectra of the components.

The O–C diagrams of minor planets − a new approach to modelling the rotation

1999 ◽  
Vol 173 ◽  
pp. 185-188
Author(s):  
Gy. Szabó ◽  
K. Sárneczky ◽  
L.L. Kiss
Keyword(s):  
Error Analysis ◽  
Time Dependence ◽  
Theoretical Work ◽  
Minor Planet ◽  
Minor Planets ◽  
New Approach ◽  
Preliminary Results ◽  
Ccd Observations

AbstractA widely used tool in studying quasi-monoperiodic processes is the O–C diagram. This paper deals with the application of this diagram in minor planet studies. The main difference between our approach and the classical O–C diagram is that we transform the epoch (=time) dependence into the geocentric longitude domain. We outline a rotation modelling using this modified O–C and illustrate the abilities with detailed error analysis. The primary assumption, that the monotonity and the shape of this diagram is (almost) independent of the geometry of the asteroids is discussed and tested. The monotonity enables an unambiguous distinction between the prograde and retrograde rotation, thus the four-fold (or in some cases the two-fold) ambiguities can be avoided. This turned out to be the main advantage of the O–C examination. As an extension to the theoretical work, we present some preliminary results on 1727 Mette based on new CCD observations.

The direct determination of magnetic domain wall profiles using a split detector STEM

1978 ◽  
Vol 36 (1) ◽  
pp. 466-467
Author(s):  
J.N. Chapman ◽  
P.E. Batson ◽  
E.M. Waddell ◽  
R.P. Ferrier
Keyword(s):  
Electron Microscope ◽  
Domain Wall ◽  
Transmission Electron Microscope ◽  
Domain Walls ◽  
Photographic Plate ◽  
Magnetic Domain ◽  
Direct Determination ◽  
Quantitative Information ◽  
Scanning Transmission Electron Microscope ◽  
Transmission Electron

By far the most commonly used mode of Lorentz microscopy in the examination of ferromagnetic thin films is the Fresnel or defocus mode. Use of this mode in the conventional transmission electron microscope (CTEM) is straightforward and immediately reveals the existence of all domain walls present. However, if such quantitative information as the domain wall profile is required, the technique suffers from several disadvantages. These include the inability to directly observe fine image detail on the viewing screen because of the stringent illumination coherence requirements, the difficulty of accurately translating part of a photographic plate into quantitative electron intensity data, and, perhaps most severe, the difficulty of interpreting this data. One solution to the first-named problem is to use a CTEM equipped with a field emission gun (FEG) (Inoue, Harada and Yamamoto 1977) whilst a second is to use the equivalent mode of image formation in a scanning transmission electron microscope (STEM) (Chapman, Batson, Waddell, Ferrier and Craven 1977), a technique which largely overcomes the second-named problem as well.

In situ microprobe quantitation of inorganic particle burden in paraffin sections of lung tissue

1988 ◽  
Vol 46 ◽  
pp. 990-991
Author(s):  
Jerrold L. Abraham
Keyword(s):  
Lung Tissue ◽  
Quantitative Information ◽  
Particulate Material ◽  
Paraffin Sections ◽  
Tissue Samples ◽  
Qualitative And Quantitative ◽  
The Past ◽  
Quantitative Analyses ◽  
Data Result

Inorganic particulate material of diverse types is present in the ambient and occupational environment, and exposure to such materials is a well recognized cause of some lung disease. To investigate the interaction of inhaled inorganic particulates with the lung it is necessary to obtain quantitative information on the particulate burden of lung tissue in a wide variety of situations. The vast majority of diagnostic and experimental tissue samples (biopsies and autopsies) are fixed with formaldehyde solutions, dehydrated with organic solvents and embedded in paraffin wax. Over the past 16 years, I have attempted to obtain maximal analytical use of such tissue with minimal preparative steps. Unique diagnostic and research data result from both qualitative and quantitative analyses of sections. Most of the data has been related to inhaled inorganic particulates in lungs, but the basic methods are applicable to any tissues. The preparations are primarily designed for SEM use, but they are stable for storage and transport to other laboratories and several other instruments (e.g., for SIMS techniques).

Comparison of Techniques for EELS Mapping in Biology

1996 ◽  
Vol 54 ◽  
pp. 300-301
Author(s):  
R.D. Leapman ◽  
S.B. Andrews
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Image Data ◽  
Beam Current ◽  
Quantitative Information ◽  
Acquisition Time ◽  
Uniform Thickness ◽  
Electron Dose ◽  
Array Detectors ◽  
Transmission Electron

Elemental mapping of biological specimens by electron energy loss spectroscopy (EELS) can be carried out both in the scanning transmission electron microscope (STEM), and in the energy-filtering transmission electron microscope (EFTEM). Choosing between these two approaches is complicated by the variety of specimens that are encountered (e.g., cells or macromolecules; cryosections, plastic sections or thin films) and by the range of elemental concentrations that occur (from a few percent down to a few parts per million). Our aim here is to consider the strengths of each technique for determining elemental distributions in these different types of specimen.On one hand, it is desirable to collect a parallel EELS spectrum at each point in the specimen using the ‘spectrum-imaging’ technique in the STEM. This minimizes the electron dose and retains as much quantitative information as possible about the inelastic scattering processes in the specimen. On the other hand, collection times in the STEM are often limited by the detector read-out and by available probe current. For example, a 256 x 256 pixel image in the STEM takes at least 30 minutes to acquire with read-out time of 25 ms. The EFTEM is able to collect parallel image data using slow-scan CCD array detectors from as many as 1024 x 1024 pixels with integration times of a few seconds. Furthermore, the EFTEM has an available beam current in the µA range compared with just a few nA in the STEM. Indeed, for some applications this can result in a factor of ~100 shorter acquisition time for the EFTEM relative to the STEM. However, the EFTEM provides much less spectral information, so that the technique of choice ultimately depends on requirements for processing the spectrum at each pixel (viz., isolated edges vs. overlapping edges, uniform thickness vs. non-uniform thickness, molar vs. millimolar concentrations).

The use of high-resolution FESEM to study solid-state phase transformations and reactions

1994 ◽  
Vol 52 ◽  
pp. 1028-1029
Author(s):  
P. G. Kotula ◽  
D. D. Erickson ◽  
C. B. Carter
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Phase Transformations ◽  
High Efficiency ◽  
Sol Gel ◽  
Quantitative Information ◽  
Solid State Reactions ◽  
Critical Dimensions ◽  
Backscattered Electrons ◽  
Backscattered Electron

High-resolution field-emission-gun scanning electron microscopy (FESEM) has recently emerged as an extremely powerful method for characterizing the micro- or nanostructure of materials. The development of high efficiency backscattered-electron detectors has increased the resolution attainable with backscattered-electrons to almost that attainable with secondary-electrons. This increased resolution allows backscattered-electron imaging to be utilized to study materials once possible only by TEM. In addition to providing quantitative information, such as critical dimensions, SEM is more statistically representative. That is, the amount of material that can be sampled with SEM for a given measurement is many orders of magnitude greater than that with TEM.In the present work, a Hitachi S-900 FESEM (operating at 5kV) equipped with a high-resolution backscattered electron detector, has been used to study the α-Fe2O3 enhanced or seeded solid-state phase transformations of sol-gel alumina and solid-state reactions in the NiO/α-Al2O3 system. In both cases, a thin-film cross-section approach has been developed to facilitate the investigation. Specifically, the FESEM allows transformed- or reaction-layer thicknesses along interfaces that are millimeters in length to be measured with a resolution of better than 10nm.

Practical applications of scanning tunneling microscopy

1989 ◽  
Vol 47 ◽  
pp. 18-19
Author(s):  
D. R. Denley
Keyword(s):  
High Resolution ◽  
Scanning Tunneling Microscopy ◽  
Quantitative Information ◽  
Digital Data ◽  
Scanning Tunneling ◽  
Ambient Atmosphere ◽  
Tunneling Microscopy ◽  
Clear Trend ◽  
Practical Applications ◽  
Promising Tool

Scanning tunneling microscopy (STM) has recently been introduced as a promising tool for analyzing surface atomic structure. We have used STM for its extremely high resolution (especially the direction normal to surfaces) and its ability for imaging in ambient atmosphere. We have examined surfaces of metals, semiconductors, and molecules deposited on these materials to achieve atomic resolution in favorable cases.When the high resolution capability is coupled with digital data acquisition, it is simple to get quantitative information on surface texture. This is illustrated for the measurement of surface roughness of evaporated gold films as a function of deposition temperature and annealing time in Figure 1. These results show a clear trend for which the roughness, as well as the experimental deviance of the roughness is found to be minimal for evaporation at 300°C. It is also possible to contrast different measures of roughness.

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