Search NASA⌕ Search

SEARCH · Search NASA

Results for “nmr probes”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Pyridine-d 5 as a 2 H NMR probe for investigation of macrostructure and pore shapes in a layered Sn(iv) phosphonate–phosphate material

Isotropic and anisotropic motions and molecular states of pyridine-d 5 , adsorbed on the surface within the pores of a layered Sn(IV) phosphonate–phosphate material (1) have been characterized thermodynamically and kinetically by solid-state NMR. The data obtained provide formulation of macrostructure and shapes of pores in 1.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1986

Development of LC-13C NMR

This study involves the development of C-13 nuclear resonance as an on-line detector for liquid chromatography (LC-C-13 NMR) for the chemical characterization of aviation fuels. The initial focus of this study was the development of a high sensitivity flow C-13 NMR probe. Since C-13 NMR sensitivity is of paramount concern, considerable effort during the first year was directed at new NMR probe designs. In particular, various toroid coil designs were examined. In addition, corresponding shim coils for correcting the main magnetic field (B sub 0) homogeneity were examined. Based on these initial probe design studies, an LC-C-13 NMR probe was built and flow C-13 NMR data was obtained for a limited number of samples.

Dorn, H. C.↗
DOE OSTI2020

Probing the Electronic Structure of a Thorium Nitride Complex by Solid-State 15N NMR Spectroscopy

The solid-state 15N NMR powder spectra of the thorium nitride complex, [K(18-crown-6)(THF)2][(R2N)3Th(m-15N)(Th(NR2)3] ([K][1-15N], R = SiMe3), and the thorium amide complex, [Th(NR2)3(15NH2)] (2-15N) were recorded. The spectrum for [K][1-15N] represents the first reported solid-state 15N NMR data for an actinide nitride complex. The experimentally measured tensor spans are 847 ppm for [K][1-15N] and 237 ppm for 2-15N. Both shielding tensors exhibit a near-zero asymmetry parameter, which for [K][1-15N] is consistent with a local rotational symmetry of its 15N-labelled nitride ligand. For 2-15N, the lack of asymmetry can be rationalized by a quasi-free Th-NH2 bond rotation in the solid-state. DFT calculations overestimate the tensor span somewhat for [K][1-15N], but provide isotropic shifts in good agreement with both the solid-state and solution values for both complexes. Natural localized molecular orbital (NLMO) analyses of the nuclear shielding reveal that the larger tensor span in [K][1-15N] vs. 2-15N is primarily a consequence of more pronounced covalency of the N-Th bonds, and large spin-orbit coupling due to significant Th 5f orbital contribution to those bonds, impacting the principal components of the shielding tensor perpendicular to the Th-N-Th axis. Overall, our analysis confirms the involvement of the 5f orbitals in Th-N multiple bonds, and further demonstrates the value of solid-state NMR spectroscopy for interrogating actinide-ligand bonding.

actinides, covalent bonding, Nuclear Magnetic Reso↗
DOE OSTI2022

Magnetic Field Analysis for Fermilab Muon $g-2$

The Muon g-2 experiment E989 at Fermilab measures the anomalous magnetic moment of the muon $a_\mu$ with improved precision compared to the Brookhaven (E821) experiments. The Brookhaven results are in tension with the Standard Model by more than $3\sigma$. The determination of $a_\mu$ requires the measurement of both the muon anomaly frequency, $\omega_a$, and the magnetic field, $\mathbf{B}$, that confines muons in a storage ring. The field is monitored by a set of coordinated nuclear magnetic resonance (NMR) measurements. NMR probes at fixed locations above and below the storage region constantly monitor the field. An in-vacuum trolley equipped with 17 NMR probes maps the muon storage region, and a special water-based NMR probe provides the calibration for the trolley probes. This presentation focuses on the determination of the time-dependent field maps from combining the fixed probe measurements and the trolley maps. The field maps are combined with the muon distribution to derive the average field observed by the muons during the measurement. These proceedings will cover the analysis from the first data run.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

High-temperature NMR MAS probe with optimized temperature gradient across sample rotor

A rotor housing assembly for NMR spectroscopy. An elongate rotor has a distal drive end, a proximal end and an internal sample space positioned along its length between the drive and proximal ends. The rotor is driveable about a rotation axis by a drive gas flow. A rotor housing has an interior space in which the rotor is at least partially received. At least one first heated gas flow inlet is positioned opposite the internal sample space, through which a first heated gas flow is controllably flowable into the interior space to heat it and the rotor. At least a pair of spaced apart second heated gas flow outlets are axially spaced from the first heated gas flow inlet to controllably convey a second heated gas flow to heat distal and proximal areas of the sample space to minimize a temperature gradient extending axially within the sample space.

Mehta, Hardeep S.↗
DOE OSTI2022

1 H chemical shift anisotropy: a high sensitivity solid-state NMR dynamics probe for surface studies?

We report dynamics play significant roles in chemistry and biochemistry-molecular motions impact both large- and small-scale chemical reactions in addition to biochemical processes. In many systems, including heterogeneous catalysts, the characterization of dynamics remains a challenge. The most common approaches involve the solid-state NMR measurement of anisotropic interactions, in particular 2 H quadrupolar coupling and 1 H–X dipolar coupling, which generally require isotope enrichment. Due to the high sensitivity of 1 H NMR, 1 H chemical shift anisotropy (CSA) is a particularly enticing, and underexplored, dynamics probe. We carried out 1 H CSA and 1 H– 13 C dipolar coupling measurements in a series of model supported complexes to understand how 1 H CSA can be leveraged to gain dynamic information for heterogeneous catalysts. Mathematical descriptions are given for the dynamic averaging of the CSA tensor, and its dependence on orientation and asymmetry. The variability of the orientation of the tensor in the molecular frame, in addition to its magnitude and asymmetry, negatively impacts attempts to extract quantitative dynamic information. Nevertheless, 1 H CSA measurements can reveal useful qualitative insights into the motions of a particularly dilute site, such as from a surface species.

1H chemical shift anisotropy↗
DOE OSTI2020

Design and performance of an in-vacuum, magnetic field mapping system for the Muon g-2 experiment

The Muon g - 2 experiment at Fermilab (E989) aims to measure the anomalous magnetic moment, a μ , of the muon with a precision of 140 parts-per-billion. This requires a precise measurement of both the anomalous spin precession frequency, ω α , of muons stored in a magnetic field of 1.45 T, and a precise measurement of that magnetic field in terms of the shielded proton Larmor frequency, ω' ρ . The measurement of ω' ρ with a total systematic uncertainty of 70 parts-perbillion involves a combination of various nuclear magnetic resonance (NMR) probes. There are 378 probes mounted in fixed locations that constantly monitor field drifts. A water-based, cylindrical calibration probe provides the calibration in terms of the shielded proton Larmor frequency. A crucial element for the multi-step measurement of ω' ρ is the regular mapping of the magnetic field over the muon storage region. The former experiment at Brookhaven National Laboratory (BNL) employed an in-vacuum field mapping system equipped with 17 NMR probes, which was developed by the University of Heidelberg. We have refurbished and upgraded this system with new probes and electronics. The upgrades include the addition of 16-bit, 1 MSPS digitization of the NMR signals, which replaced the hardware-implemented zero-crossing counting of the system at Brookhaven. The digitized signals offer new capabilities in the NMR frequency analysis and its related systematic uncertainties. To sustain the higher data rates, a new communication scheme with time-division multiplexing was implemented to separate the important NMR reference clock from the data communication in order to reach the specifications for the accuracy and stability of the reference clock. A new barcode reader provides more precise azimuthal position determination during the measurement and calibration. While the mechanical systems that move the field mapper inside the storage ring have been mostly refurbished from BNL, the motion control system was completely replaced with a custom-built electronics centered around a commercial Galil motion controller. Both the field mapping NMR system and its motion control were successfully commissioned at Fermilab and have been in reliable operation during the first three data taking periods of the experiment at Fermilab. Finally, this article will provide the details of the upgrades of the field mapper and its performance.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Design and performance of an in-vacuum, magnetic field mapping system for the Muon g-2 experiment

The E989 Muon g-2 experiment at Fermilab aims to measure the anomalous magnetic moment, a$_\mu$, of the muon with a precision of 140 parts-per-billion. This requires a precise measurement of both the anomalous spin precession frequency, $\omega_a$, and the average magnetic field in terms of the equivalent, free proton Larmor frequency, $\omega_p$. The measurement of $\omega_p$ with a total systematic uncertainty of 70 parts-per-billion involves a combination of various NMR probes. There are 378 probes in fixed locations constantly monitoring field drifts. A water-based probe provides the calibration in terms of $\omega_p$. A crucial element for the multi-step measurement of $\omega_p$ is the regular mapping of the magnetic field over the muon storage region. The former E821 experiment at Brookhaven employed an in-vacuum field mapping system equipped with 17 NMR probes, which was developed by the University of Heidelberg. We have refurbished and upgraded this system with new probes and electronics. The upgrades include a new communication scheme incorporating time-division multiplexing to separate the important NMR reference clock from the data communication. The addition digitization of the NMR signals replaced the hardware-implemented zero-crossing counting of the E821 system. The digitized signals offer new capabilities in the NMR frequency analysis and its related systematic uncertainties. While the mechanical systems that move the field mapper around the ring have been mostly refurbished, the motion control system was completely replaced with a custom-built electronics centered around a commercial Galil motion controller. Both the field mapping NMR system and its motion control were successfully commissioned at Fermilab and have been in reliable operation during the first data taking periods. This article provides details of the upgrades of the field mapper and its performance.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

The fixed probe storage ring magnetometer for the Muon g-2 experiment at Fermi National Accelerator Laboratory

The goal of the FNAL E989 experiment is to measure the muon magnetic anomaly to unprecedented accuracy and precision at the Fermi National Accelerator Laboratory. To meet this goal, the time and space averaged magnetic environment in the muon storage volume must be known to better than 70 ppb. A new pulsed proton nuclear magnetic resonance (NMR) magnetometer was designed and built at the University of Washington, Seattle to track the temporal stability of the 1.45 T magnetic field in the muon storage ring at this precision. It consists of an array of 378 petroleum jelly based NMR probes that are embedded in the walls of muon storage ring vacuum chambers and custom electronics built with readily available modular radio frequency (RF) components. We give NMR probe construction details and describe the functions of the custom electronic subsystems. The excellent performance metrics of the magnetometer are discussed, where after 8 years of operation the median single shot resolution of the array of probes remains at 650 ppb.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Local order, disorder, and everything in between: using 91 Zr solid-state NMR spectroscopy to probe zirconium-based metal–organic frameworks

Characterization of metal centers in metal–organic frameworks (MOFs) is critical for rational design and further understanding of structure–property relationships. The short-range structure about Zr atoms is challenging to properly elucidate in many Zr MOFs, particularly when local disorder is present. Static 91 Zr solid-state NMR spectra of the seven zirconium MOFs UiO-66, UiO-66-NH 2 , UiO-67, MOF-801, MOF-808, DUT-68 and DUT-69 have been acquired at high magnetic fields of 35.2 T and 19.6 T, yielding valuable information on the local structure, site symmetry and order about Zr. 91 Zr NMR is very sensitive to differences in MOF short-range structure caused by guest molecules, linker substitution and post-synthetic treatment. Complementary density functional theory (DFT) calculations assist in the interpretation and assignment of 91 Zr solid-state NMR spectra, lend insight into structural origins of 91 Zr NMR parameters and enable determination of local Zr coordination environments. This approach can be extended to many other materials containing zirconium.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Software Architecture and Hardware Organization in Mu2e Solenoid Field Mapping System

Herein, the Mu2e field mapping system is designed to produce high accuracy field maps of the detector solenoid used in the experiment. The data acquisition system is mobile and uses a self-propelled mapper with rotating arms equipped with 3D Hall probes. The measurements require not only accurate magnetic field readouts, but also accurate locations of all Hall probes while measuring data. The latter is accomplished by using the laser tracker to measure positions of several retroreflectors on the field mapper during data acquisition. The measurement process requires scanning the whole space inside the large solenoid and takes many hours to complete, which necessitates its full automation. The automation software includes control of the mapper, readout of Hall and NMR probes and control of a laser tracker, including prediction of retroreflector positions and execution of quality control checks. The software architecture and data acquisition hardware of the field mapping system are described, with special attention given to control of the laser tracker and its integration with the rest of the system.

3d hall probes↗
DOE OSTI2024

Repulsive Tomonaga-Luttinger liquid in the quasi-one-dimensional alternating spin-$\frac{1}{2}$ antiferromagnet NaVOPO 4

Here, we probe the magnetic field-induced Tomonaga-Luttinger liquid (TLL) state in the bond-alternating spin1/2 antiferromagnetic (AFM) chain compound NaVOPO 4 using thermodynamic as well as local μSR and 31 P NMR probes down to mK temperatures in magnetic fields up to 14 T. The μSR and NMR relaxation rates in the gapless TLL regime decay slowly following characteristic power-law behavior, enabling us to directly determine the interaction parameter K as a function of the magnetic field. These estimates are crosschecked using magnetization and specific heat data. The field-dependent K lies in the range of 0.4 < K < 1 and indicates the repulsive nature of interactions between the spinless fermions, in line with the theoretical predictions. This renders NaVOPO 4 the first experimental realization of TLL with repulsive fermionic interactions in hitherto studied S = 1/2 bond-alternating AFM-AFM chain compounds.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

High precision magnetic field measurement and mapping of the LEReC 180 degree bending magnet using very low field NMR with hall combined probe (140 - 350 gauss)

The Relativistic Heavy Ion Collider (RHIC) at BNL are using the Low Energy RHIC Electron Cooling (LEReC) to conduct experiments that search for the quantum chromodynamic (QCD) critical point. The first ever electron cooling based on the RF acceleration of electron beams was experimentally demonstrated on April 5, 2019 at LEReC at BNL. The first critical step in obtaining successful 3D non-magnetized cooling of the Au ion bunches in the RHIC cooling section was matching the electron beam energy with a relative error less than 5*10 -4 to the ion beam energy. Part of the LEReC beamline is a dipole magnet that bends the electron beam 180 degree. One of the most outstanding measurement challenges is that the dipole field is so low (≈200 G). Most of the existing NMR probes can only measure fields >400 G. Lower signal-to-noise ratio at low fields is requires the use of larger sample volumes. Working with CAYLAR, a NMR probe has been redesigned and optimized for these low field measurements with high resolution. We report the methods, challenges, and results for extensive magnetic field mappings of the 180 dipole magnet. A combination of NMR and Hall sensors has been successfully implemented to measure uniform field regimes inside the magnet center area and non-uniform field regimes at the magnet ends. Detailed measurement and mapping have been performed at five radii and five heights along the beam trajectory. Meanwhile a finite element magnetic modeling simulation of the magnet using Opera software has been performed. The calculated and measured data are compared, and the calculated data is good reference for measured data over long length mapping from magnet edge to center. The measured magnetic measurement data is directly useful for beam instrumentation, diagnostics and operation.

Magnetic Field Measurement↗
DOE OSTI2021

On the Use of Aqueous Metal-Aqua p K a Values as a Descriptor of Lewis Acidity

The behavior of Lewis acidic metal ions in multimetallic systems has become a subject of intense interest in recent years. Parametrizing the behavior of these ions in non-aqueous conditions, commonly used in the field, is challenging due to the lack of direct measures of the Lewis acidity of metal ions in polar organic solvents. Here, we report the use of triphenylphosphine oxide (TPPO) as a 31 P nuclear magnetic resonance (NMR) probe to quantify the Lewis acidity of a library of metal triflate salts using the Gutmann-Beckett method. Plots of the pK a values of the corresponding metal-aqua species, [M(H 2 O) m ] n+ , measured in H 2 O vs. the 31 P NMR shifts of TPPO in the presence of these metals in deuterated acetonitrile (d3-MeCN) and deuterated dichloromethane (CD 2 Cl 2 ) display tightly co-linear relationships, suggesting similar behavior for these ions in water, d 3 -MeCN, and CD 2 Cl 2 . This collinearity reinforces the utility of the common approach of using the aqueous pK a values as a descriptor of Lewis acidity, regardless of the solvent used in the immediate experiments, and provides an insight into the usefulness of this descriptor in wide-ranging applications. Titration studies in d 3 -MeCN suggest 1:1 binding of TPPO with monovalent ions, greater than 1:1 binding with divalent ions, and formation of multiple species with the highly Lewis acidic trivalent ions. Altogether, these data suggest that both aqueous pK a values and other single-measurement descriptors, while useful, provide only a snapshot of the influence of Lewis acidity on multimetallic chemical systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Universal fluctuating regime in triangular chromate antiferromagnets

In this work, we report x-ray diffraction, magnetic susceptibility, heat capacity, 1 H nuclear magnetic resonance (NMR), and muon spin relaxation (μSR) measurements, as well as density-functional band-structure calculations for the frustrated S=3/2 triangular lattice Heisenberg antiferromagnet (TLHAF) α-HCrO 2 (trigonal, space group: $R\bar{3}m$). This compound undergoes a clear magnetic transition at T N ≃22.5 K, as seen from the drop in the muon paramagnetic fraction and concurrent anomalies in the magnetic susceptibility and specific heat capacity. Local probes (NMR and μSR) reveal a broad regime with slow fluctuations down to 0.7T N , this temperature corresponding to the maximum in the μSR relaxation rate and in the NMR wipe-out. From the comparison with NaCrO 2 and α-KCrO 2 , the fluctuating regime and slow dynamics below T N appear to be hallmarks of the TLHAF with ABC stacking. We discuss the role of interlayer frustration, which may have impacted recent spin-liquid candidates with triangular geometry.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Measurement of the anomalous precession frequency in the Muon $g-2$ experiment at Fermilab

The muon anomalous magnetic moment, $a_\mu=\frac{g-2}{2}$, is a low energy observable that can be both measured and computed with high precision, therefore it can provide an important test of the Standard Model and it is a sensitive probe for new physics. In particular, any discrepancy between the experimental value and the theoretical prediction can be due to Beyond Standard Model physics contribution. The E989 Muon $g-2$ Experiment at Fermilab aims to measure $a_\mu$ with a precision of 140 parts per billion, four time more precisely than the previous experiment at Brookhaven National Laboratory (BNL). E989 seeks to either resolve or confirm the observed discrepancy of $3.7\sigma$ between the Standard Model value and the experimental one. The $a_\mu$ measurement requires a precise determination of both the muon spin anomalous precession frequency and the average magnetic field seen by the muons as they circulate in a storage ring. The anomalous precession frequency measurement is b ased on the time distribution of high-energy decay positrons observed by 24 electromagnetic calorimeters placed around the inner circumference of the ring, while the magnetic field is constantly monitored by NMR probes. Last spring, E989 has published a new measurement of $a_\mu$ from the 2018 data-taking campaign, confirming the previous BNL value with comparable precision, bringing the discrepancy with the theoretical value to $4.2\sigma$. The candidate worked on the measurement of the anomalous precession frequency and on the estimate of the related systematic uncertainties of the 2018 data, giving an important contribution to the data analysis. The result presented in chapters 4 and 5 of this dissertation was included, among three other analyses, to determine the estimate of the anomalous magnetic moment by the Muon g-2 experiment. This work will present the anomalous precession frequency analysis technique and its result, the related systematics and finally the latest $a_\mu$ result.

Sorbara, Matteo↗
DOE OSTI2025

Quantifying the Lewis Acidity of Mono-, Di-, and Trivalent Cations in Anhydrous Bis(trifluoromethylsulfonyl)imide Salts

While the bis(trifluoromethylsulfonyl)imide anion (TFSI – ; formula [N(SO 2 CF 3 ) 2 ] – ) has been noted for its practical utility, the use of TFSI – salts as sources of Lewis acidic metal cations for studies of cation-driven tuning effects has not been reported. Here, the effective Lewis acidity of mono-, di-, and trivalent cations (namely, K + , Na + , Li + , Ba 2+ , Ca 2+ , Mg 2+ , Zn 2+ , La 3+ , Y 3+ , Lu 3+ , and Sc 3+ ) in the form of their TFSI – salts is described, along with quantitative comparisons to salts of several other weakly coordinating anions (namely, SO 3 CF 3 – , PF 6 – , and BArF 24 – ). Triphenylphosphine oxide (TPPO) was used as a 31 P NMR probe in titration experiments for quantification of key parameters describing the effective Lewis acidity of the salts in acetonitrile (CH 3 CN) solutions. Notably, the TFSI – salts of di- and trivalent cations were found to display strong binding to TPPO with significant speciation and were found to be quite hygroscopic. Taken together, the measurements demonstrate that TFSI – salts are systematically better/stronger effective Lewis acids than their triflate analogues. And, considering the excellent solubility of TFSI – salts, these materials appear attractive for further use and development in Lewis-acidity-dependent applications, including catalysis and tuning of multimetallic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗