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DOE OSTI2021

Efficiency analysis of helium-cooled MAS DNP: case studies of surface-modified nanoparticles and homogeneous small-molecule solutions

Despite the growing number of successful applications of dynamic nuclear polarization (DNP)-enhanced magic-angle spinning (MAS) NMR in structural biology and materials science, the nuclear polarizations achieved by current MAS DNP instrumentation are still considerably lower than the theoretical maximum. Here, the method could be significantly strengthened if experiments were performed at temperatures much lower than those currently widely used (~100 K). Recently, the prospects of helium (He)-cooled MAS DNP have been increased with the instrumental developments in MAS technology that uses cold helium gas for sample cooling. Despite the additional gains in sensitivity that have been observed with He-cooled MAS DNP, the performance of the technique has not been evaluated in the case of surfaces and interfaces that benefit the most from DNP. Herein, we studied the efficiency of DNP at temperatures between ~30 K and ~100 K for organically functionalized silica material and a homogeneous solution of small organic molecules at a magnetic field B 0 = 16.4 T. We recorded the changes in signal enhancement, paramagnet-induced quenching and depolarization effects, DNP build-up rate, and Boltzmann polarization. For these samples, the increases in MAS-induced depolarization and DNP build-up times at around 30 K were not as severe as anticipated. In the case of the surface species, we determined that MAS DNP at 30 K provided ~10 times higher sensitivity than MAS DNP at 90 K, which corresponds to the acceleration of experiments by multiplicative factors of up to 100.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

MAS: A versatile Landau-fluid eigenvalue code for plasma stability analysis in general geometry

We have developed a new global eigenvalue code, Multiscale Analysis for plasma Stabilities (MAS), for studying plasma problems with wave toroidal mode number (n) and frequency (ω) in a broad range of interest in general tokamak geometry, based on a five-field Landau-fluid description of thermal plasmas. Beyond keeping the necessary plasma fluid response, we further retain the important kinetic effects including diamagnetic drift, ion finite Larmor radius, finite parallel electric field (E||), ion and electron Landau resonances in a self-consistent and non-perturbative manner without sacrificing the attractive efficiency in computation. The physical capabilities of the code are evaluated and examined in the aspects of both theory and simulation. In theory, the comprehensive Landau-fluid model implemented in MAS can be reduced to the well-known ideal MHD model, electrostatic ion-fluid model, and drift-kinetic model in various limits, which clearly delineates the physics validity regime. In simulation, MAS has been well benchmarked with theory and other gyrokinetic and kinetic-MHD hybrid codes in a manner of adopting the unified physical and numerical framework, which covers the kinetic Alfv\'en wave (KAW), ion sound wave (ISW), low-n kink, high-n ion temperature gradient mode (ITG) and kinetic ballooning mode (KBM). Moreover, MAS is successfully applied to model the Alfv\'en eigenmode (AE) activities in DIII-D discharge #159243, which faithfully captures the frequency sweeping of reversed shear Alfv\'en eigenmode (RSAE), the tunneling damping of toroidal Alfv\'en eigenmode (TAE), as well as the polarization characteristics of kinetic beta-induced Alfv\'en eigenmode (KBAE) and beta-induced Alfv\'en-acoustic eigenmode (BAAE) being consistent with former gyrokinetic theory and simulation. With respect to the key progress contributed to the community, MAS has the advantage of combining rich physics ingredients, realistic global geometry and high computation efficiency together for plasma stability analysis in linear regime.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1993

Intercomparison of MAS, AVIRIS, and HIS data from FIRE cirrus 2

The NASA ER-2 flight on 5 Dec. 1991 is unique among the FIRE Cirrus 2 missions in that data were acquired simultaneously by the MODIS Airborne Simulator (MAS), the Airborne Visible/Infrared Imaging Spectrometer (AVIRIS), and the High Resolution Interferometer Sounder (HIS). These data represent a unique source of information about the spatial and spectral properties of cirrus clouds. The MAS is a new instrument which will aid in defining algorithms and building an understanding of the ability of the Moderate Resolution Imaging Spectroradiometer (MODIS) to remotely sense atmospheric conditions for assessing global change. In order to establish confidence in the absolute calibration accuracy of the MAS radiances, an inter-comparison of MAS radiances with AVIRIS and HIS has been undertaken.

Gumley, Liam E.↗

NASA NTRS2000

BOREAS Level-1B MAS Imagery At-sensor Radiance, Relative X and Y Coordinates

For BOReal Ecosystem-Atmosphere Study (BOREAS), the MODIS Airborne Simulator (MAS) images, along with the other remotely sensed data, were collected to provide spatially extensive information over the primary study areas. This information includes detailed land cover and biophysical parameter maps such as fraction of Photosynthetically Active Radiation (fPAR) and Leaf Area Index (LAI). Collection of the MAS images occurred over the study areas during the 1994 field campaigns. The level-1b MAS data cover the dates of 21-Jul-1994, 24-Jul-1994, 04-Aug-1994, and 08-Aug-1994. The data are not geographically/geometrically corrected; however, files of relative X and Y coordinates for each image pixel were derived by using the C-130 INS data in a MAS scan model. The data are provided in binary image format files.

Strub, Richard↗

NASA NTRS2000

BOREAS Level-2 MAS Surface Reflectance and Temperature Images in BSQ Format

The BOReal Ecosystem-Atmosphere Study (BOREAS) Staff Science Aircraft Data Acquisition Program focused on providing the research teams with the remotely sensed aircraft data products they needed to compare and spatially extend point results. The MODIS Airborne Simulator (MAS) images, along with other remotely sensed data, were collected to provide spatially extensive information over the primary study areas. This information includes biophysical parameter maps such as surface reflectance and temperature. Collection of the MAS images occurred over the study areas during the 1994 field campaigns. The level-2 MAS data cover the dates of 21-Jul-1994, 24-Jul-1994, 04-Aug-1994, and 08-Aug-1994. The data are not geographically/geometrically corrected; however, files of relative X and Y coordinates for each image pixel were derived by using the C130 navigation data in a MAS scan model. The data are provided in binary image format files.

Hall, Forrest G.↗

NASA NTRS2008

Cassini's Maneuver Automation Software (MAS) Process: How to Successfully Command 200 Navigation Maneuvers

To keep Cassini on its complex trajectory, more than 200 orbit trim maneuvers (OTMs) have been planned from July 2004 to July 2010. With only a few days between many of these OTMs, the operations process of planning and executing the necessary commands had to be automated. The resulting Maneuver Automation Software (MAS) process minimizes the workforce required for, and maximizes the efficiency of, the maneuver design and uplink activities. The MAS process is a well-organized and logically constructed interface between Cassini's Navigation (NAV), Spacecraft Operations (SCO), and Ground Software teams. Upon delivery of an orbit determination (OD) from NAV, the MAS process can generate a maneuver design and all related uplink and verification products within 30 minutes. To date, all 112 OTMs executed by the Cassini spacecraft have been successful. MAS was even used to successfully design and execute a maneuver while the spacecraft was in safe mode.

Yang, Genevie Velarde↗

NASA NTRS1988

Millimeter-Wave Atmospheric Sounder (MAS)

MAS is a remote sensing instrument for passive sounding (limb sounding) of the earth's atmosphere from the Space Shuttle. The main objective of the MAS is to study the composition and dynamic structure of the stratosphere, mesosphere, and lower thermosphere in the height range 20 to 100 km, the region known as the middle atmosphere. The MAS will be flown on the Atmospheric Laboratory for Applications and Science (ATLAS 1) NASA mission scheduled for late 1990. The Millimeter-Wave Atmospheric Sounder will provide, for the first time, information obtained simultaneously on the temperature and on ozone concentrations in the 20 to 90 km altitude region. The information will cover a large area of the globe, will have high accuracy and high vertical resolution, and will cover both day and night times. Additionally, data on the two important molecules, H2O and ClO, will also be provided.

Hartmann, G. K.↗

NASA NTRS2003

Remote Sensing of Liquid Water and Ice Cloud Optical Thickness and Effective Radius in the Arctic: Application of Airborne Multispectral MAS Data

A multispectral scanning spectrometer was used to obtain measurements of the reflection function and brightness temperature of clouds, sea ice, snow, and tundra surfaces at 50 discrete wavelengths between 0.47 and 14.0 microns. These observations were obtained from the NASA ER-2 aircraft as part of the FIRE Arctic Clouds Experiment, conducted over a 1600 x 500 km region of the north slope of Alaska and surrounding Beaufort and Chukchi Seas between 18 May and 6 June 1998. Multispectral images of the reflection function and brightness temperature in 11 distinct bands of the MODIS Airborne Simulator (MAS) were used to derive a confidence in clear sky (or alternatively the probability of cloud), shadow, and heavy aerosol over five different ecosystems. Based on the results of individual tests run as part of the cloud mask, an algorithm was developed to estimate the phase of the clouds (water, ice, or undetermined phase). Finally, the cloud optical thickness and effective radius were derived for both water and ice clouds that were detected during one flight line on 4 June. This analysis shows that the cloud mask developed for operational use on MODIS, and tested using MAS data in Alaska, is quite capable of distinguishing clouds from bright sea ice surfaces during daytime conditions in the high Arctic. Results of individual tests, however, make it difficult to distinguish ice clouds over snow and sea ice surfaces, so additional tests were added to enhance the confidence in the thermodynamic phase of clouds over the Beaufort Sea. The cloud optical thickness and effective radius retrievals used 3 distinct bands of the MAS, with the newly developed 1.62 and 2.13 micron bands being used quite successfully over snow and sea ice surfaces. These results are contrasted with a MODIS-based algorithm that relies on spectral reflectance at 0.87 and 2.13 micron.

King, Michael D.↗

NASA NTRS2007

Remote Sensing of the Radiative and Microphysical Properties of Clouds during TC4: Results from MAS, MASTER, MODIS, and MISR

The MODIS Airborne Simulator (MAS) and MODIS/ASTER Airborne Simulator (MASTER) were used to obtain measurements of the bidirectional reflectance and brightness temperature of clouds at 50 discrete wavelengths between 0.47 and 14.3 (12.9 m for MASTER). These observations were obtained from the NASA ER-2 aircraft as part of the Tropical Composition, Clouds and Climate Coupling Experiment (TC4) conducted over Central America and surrounding Pacific and Atlantic Oceans between July 17 and August 8, 2007. Multispectral images in eight distinct bands were used to derive a confidence in clear sky (or alternatively the probability of cloud) over land and ocean ecosystems. Based on the results of individual tests run as part of this cloud mask, an algorithm was developed to estimate the phase of the clouds (liquid water, ice, or undetermined phase). Finally, the cloud optical thickness and effective radius were derived for both liquid water and ice clouds that were detected during each flight, using a nearly identical algorithm as that implemented operationally to process MODIS cloud data from the Aqua and Terra satellites (Collection 5). This analysis shows that the cloud mask developed for operational use on MODIS, and tested using MAS and MASTER date in TC4, is quite capable of distinguishing both liquid water and ice clouds during daytime conditions over both land and ocean. The cloud optical thickness and effective radius retrievals used three distinct bands of the MAS (or MASTER), and these results were compared with nearly simultaneous retrievals of MODIS on the Terra spacecraft. Finally, this MODIS-based algorithm was adapted to MISR data to infer the cloud optical thickness of liquid water clouds from MISR. Results of this analysis will be presented and discussed.

King, Michael D.↗

NASA NTRS2010

Remote Sensing of Radiative and Microphysical Properties of Clouds During TC (sup 4): Results from MAS, MASTER, MODIS, and MISR

The Moderate Resolution Imaging Spectroradiometer (MODIS) Airborne Simulator (MAS) and MODIS/Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) Airborne Simulator (MASTER) were used to obtain measurements of the bidirectional reflectance and brightness temperature of clouds at 50 discrete wavelengths between 0.47 and 14.2 microns (12.9 microns for MASTER). These observations were obtained from the NASA ER-2 aircraft as part of the Tropical Composition, Cloud and Climate Coupling (TC4) experiment conducted over Central America and surrounding Pacific and Atlantic Oceans between 17 July and 8 August 2007. Multispectral images in eleven distinct bands were used to derive a confidence in clear sky (or alternatively the probability Of cloud) over land and ocean ecosystems. Based on the results of individual tests run as part of the cloud mask, an algorithm was developed to estimate the phase of the clouds (liquid water, ice, or undetermined phase). The cloud optical thickness and effective radius were derived for both liquid water and ice clouds that were detected during each flight, using a nearly identical algorithm to that implemented operationally to process MODIS Cloud data from the Aqua and Terra satellites (Collection 5). This analysis shows that the cloud mask developed for operational use on MODIS, and tested using MAS and MASTER data in TC(sup 4), is quite capable of distinguishing both liquid water and ice clouds during daytime conditions over both land and ocean. The cloud optical thickness and effective radius retrievals use five distinct bands of the MAS (or MASTER), and these results were compared with nearly simultaneous retrievals of marine liquid water clouds from MODIS on the Terra spacecraft. Finally, this MODIS-based algorithm was adapted to Multiangle Imaging SpectroRadiometer (MISR) data to infer the cloud optical thickness Of liquid water clouds from MISR. Results of this analysis are compared and contrasted.

King, Michael D.↗

DOE OSTI2020

29 Si solid state MAS NMR study on leaching behaviors and chemical stability of different Mg-silicate structures for CO 2 sequestration

Silicon is one of the most earth abundant elements, and thus, the fate and reactivity of silicate materials are often important for various energy and environmental technologies including carbon sequestration, where CO 2 is captured and stored as a thermodynamically stable solid carbonate phase. Thus, understanding the structures and chemistries of different silicate phases has become an important research aim. Here in this study, the changes in the silicate structures (Q 0 –Q 4 ) of heat-treated Mg-bearing mineral (serpentine) exposed to a CO 2 -water system (carbonic acid) was investigated using 29 Si MAS NMR, XRPD and ICP-OES and the identified structures were employed to explain complex leaching behaviors of silicate materials. The 29 Si MAS NMR and XRPD analysis indicated that the heat-treated serpentine is a mixture of amorphous (Q 1 : dehydroxylate I, Q 2 : enstatite, Q 4 : silica) and crystalline (Q 0 : forsterite, Q 3 : dehydroxylate II and serpentine) phase, while natural serpentine mineral has single crystalline Q 3 silicate structure. The leaching experiments showed that both Mg and Si in the amorphous silicate structures (Q 1 : dehydroxylate I, Q 2 : enstatite) are more soluble than those in crystalline phase (Q 0 : forsterite, Q 3 : dehydroxylate II and serpentine). Therefore, tuning the silicate structure towards Q 1 and Q 2 would significantly improve carbon sequestration potential of silicate minerals, whereas silicate materials with Q 3 structure would provide great chemical stabilities in acidic conditions. The solubilities of silicate structures were in the order of Q 1 (dehydroxylate I) > Q2 (enstatite) >> Q0 (forsterite) > Q3 (dehydroxylate II) > Q 3 (serpentine) and this finding can be used to better design a wide range of energy and environmental materials and reaction systems.

25 ENERGY STORAGE↗

DOE OSTI2021

Proton-detected 15 N- 1 H dipolar coupling/ 1 H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR

Measurement of distances from dipolar couplings is essential for structural characterization, refinement and validation using the solid-state nuclear magnetic resonance (ssNMR) spectroscopy. Particularly, knowledge about NH dipolar interactions in biological solids is important for understanding the hydrogen (H)-bonding interactions, molecular geometry and spin dynamics. In this regard, we have proposed a proton-detected two-dimensional (2D) 15 N- 1 H dipolar coupling/ 1 H chemical shift correlation experiment using the C-symmetry based windowless recoupling of chemical shift anisotropy (ROCSA) in combination with the DIPSHIFT pulse-based method for the measurement of short NH distances in the isotopically labeled and naturally abundant biological solids at fast magic angle spinning (MAS) rates (40–70 kHz). Our proposed method results in undistorted recoupled 15 N- 1 H dipolar coupling powder lineshapes that are free from the recoupled 1 H CSA contributions under the 15 N evolution, a feature that is essential for the measurement of NH distances with improved accuracy (± 500 Hz in terms of the NH dipolar couplings). The pulse sequence developed in the present study is also insensitive to the 1H–1H homonuclear dipolar interactions, relaxation effects owing to its constant-time implementation, and t1-noise from the fluctuations in the MAS.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2021

Unexpected structural/motional mode of water intercalated into an α-crystalline zirconium phosphate deduced by 31 P and 2 H solid-state MAS NMR spectra

Here, in developing the approach to understanding dynamics of intercalates in layered materials, crystalline-layered zirconium phosphate Zr (HPO 4 ) 2 ·0.35D2O has been prepared and characterized by the 1 H, 31 P, and 2 H solid-state MAS NMR spectra, including 31 P and 2 H T 1 measurements. At temperatures >253 K, the intercalated water shows two spectrally-distinguished deuterons unprecedentedly with different DQCC's and 2 H T 1 times, one of which is hydrogen bonded. The collected data allowed to identify an unexpected bonding/dynamic mode of water molecules, which experience fast rotation around the hydrogen bond, formed with a zirconium-coordinated oxygen. The low-temperature 2 H MAS NMR experiments have demonstrated the presence of additional hydrogen bond P—(H)O˙˙˙ DO, population of which grows on cooling to 195 K corresponding to the doubly hydrogen-bonded immobile water molecule.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Elucidating structure and dynamics of crystalline α-zirconium phosphates intercalated with water and methanol by multinuclear solid-state MAS NMR: A comprehensive NMR approach

Solid-state NMR experiments on 2 H, 31 P, 13 C, and 1 H nuclei, including 31 P T 1 , 1 H T 1 , and 1 H T 1ρ measurements, as well as on the kinetics of proton-phosphorus cross-polarization have been performed to characterize the crystalline and amorphous α-zirconium phosphates, which were intercalated with D 2 O and/or CD 3 OD. The 13 C{ 1 H} CP MAS NMR experiment performed for compound 1-CD 3 OD (Zr (HPO 4 ) 2 .0.2CD 3 OD) with carbon cross-polarization via protons of phosphate groups has provided a prove that the methanol was intercalated into the interlayer spaces of this compound. The variable-temperature 2 H solid-echo MAS NMR spectra of intercalated compounds demonstrated that the methanol molecules, in contrast to the mobile water, were immobile, keeping, however, free CD 3 rotations around the C 3 -axis. It has been demonstrated that the intercalated species, D 2 O and CD 3 OD, do not affect the high-frequency motions of the phosphate groups. By utilizing local structural models that satisfy the constraints of the experimental data, it has been suggested that the immobile methanol molecules are located in the cavity between two neighboring layers of the zirconium phosphates. Here, the present work illustrates the reliable criteria in a comprehensive NMR approach to structural and dynamic studies of such systems.

1H↗

DOE OSTI2022

Utilization of 29Si MAS-NMR to Understand Solid State Diffusion in Energy Storage Materials

The properties of many solid-state materials arise from critical interfaces tied to the structure, morphology, and composition of the materials under study. For many materials, identifying components that may be invisible to diffraction techniques or other bulk sensitive techniques (i.e. inductively coupled plasma (ICP)), may cause important information to be overlooked. These can include grain boundary phases, nanoscale coatings, amorphous layers, or second phases that influence the materials environment. In this short review, the use of 29 Si MAS NMR as a local probe to detect silicon-containing phases in complex energy storage systems is explored with a focus is on silicon-containing materials and silicon electrodes. Examples highlighting the utility of 29 Si MAS NMR include 1) examining copper diffusion into silicon as a method to create 3 dimensional electrodes, 2) using Mg(II) electrolyte additives to create in-situ nanoscale silicide coatings to inhibit low voltage parasitic side reactions and extend calendar life, and 3) studying the lithiation reactions of passivated silicon on different time scales.

Dogan, Fulya↗

NASA NTRS1996

A Comparison of Ozone Measurements Made by the ATMOS, MAS, and SSBUV Instruments During ATLAS 1,2, and 3

Ozone profile measurements were made by three instruments, ATMOS, MAS, and SSBUV, using distinctly different observing techniques, as part of the ATLAS Space Shuttle missions in March 1992, April 1993, and November 1994. ATMOS makes solar-occultation observations of infrared spectra using a Fourier transform interferometer. MAS uses a limb-scanning antenna to measure emission spectra at millimeter wavelengths. SSBUV is a nadir-viewing instrument measuring the transmission of scattered solar ultraviolet radiation modified by ozone absorption. A sample of zonal-mean mixing ratio profiles indicates that these three ATLAS instruments generally agree to within 10%, although a few potential biases have been noted. There are significant differences in the character of the agreement between ATLAS 1 and ATLAS 2 which will require further study.

Kriebel, D. L.↗

DOE OSTI2026

MAS-CCD: New technique for measuring low-level charge content based on the multiple amplifier architecture

Low-noise detectors are a key technology for the next generation of astronomical instruments aimed at spectroscopy of faint objects and the search for exoplanets. In this context, the multiple-amplifier sensing charge-coupled device (MAS-CCD) emerges as a promising technology for future scientific instruments. A critical parameter affecting the performance of these devices is spurious charge, produced by the clocking of the gates. Its measurement is typically challenging with existing methods. In practice, the optimization of this parameter often relies on empirical procedures that require significant time and careful consideration of the trade-off with full-well capacity. In this work, we present a new technique to estimate spurious charge based on covariance analysis of the output amplifiers of the MAS-CCD, which measures the same charge packet in different amplifiers at different times. The method enables fast and precise measurements of spurious charge under operating conditions where conventional approaches are difficult to apply. We develop the theoretical framework of the method and validate the model through simulations. The results demonstrate the feasibility of this approach and suggest that it could serve as a basis for reliable large-scale characterization of sensor performance.

Gamero, Miqueas E. [Buenos Aires, CONICET; Fermila↗

DOE OSTI2023

Determination of the relative orientation between 15 N- 1 H dipolar coupling and 1 H chemical shift anisotropy tensors under fast MAS solid-state NMR

Here, in this work, we have proposed a proton-detected three-dimensional (3D) 15 N- 1 H dipolar coupling (DIP)/ 1 H chemical shift anisotropy (CSA)/ 1 H chemical shift (CS) correlation experiment to measure the relative orientation between the 15 N- 1 H dipolar coupling and the 1 H CSA tensors under fast magic angle spinning (MAS) solid-state NMR. In the 3D correlation experiment, the 15 N- 1 H dipolar coupling and 1 H CSA tensors are recoupled using our recently developed windowless C-symmetry-based $C3^{1}_{3}$-ROCSA (recoupling of chemical shift anisotropy) DIPSHIFT and $C3^{1}_{3}$-ROCSA pulse-based methods, respectively. The 2D 15 N- 1 H DIP/ 1 H CSA powder lineshapes extracted using the proposed 3D correlation method are shown to be sensitive to the sign and asymmetry of the 1 H CSA tensor, a feature that allows the determination of the relative orientation between the two correlating tensors with improved accuracy. The experimental method developed in this study is demonstrated on a powdered U- 15 N L-Histidine.HCl·H 2 O sample.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗