Notes on Lepton Gyromagnetic Ratios
A compendium for outsiders.
72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
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Correction of Q Factor Effects for Simultaneous Collection of Elemental Analysis and Relaxation Times by Nuclear Magnetic Resonance
A new method for measurement of elemental analysis by nuclear magnetic resonance (NMR) of unknown samples is discussed in this report as a quick and robust means to measure elemental ratios without the use of internal or external calibration standards. The determination of elemental ratios was done by normalizing the signal intensities by the frequency dependent quality factor (Q) and the gyromagnetic ratios (γ) for each measured nucleus. The correction for the frequency dependence was found by characterizing the output signal of the probe as a function of the quality factor (Q) and the frequency, and the correction for γ was discussed in a previous study. A Carr–Purcell–Meiboom–Gill (CPMG) pulse sequence was used for evaluation of the relative signal intensities, which allows for derivation of elemental ratios, and was correspondingly used to simultaneously measure the T 2 * of samples for an added parameter for more accurate identification of unknown samples.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Multinuclear PFGSTE NMR description of 39 K, 23 Na, 7 Li, and 1 H specific activation energies governing diffusion in alkali nitrite solutions
While pulsed field gradient stimulated echo nuclear magnetic resonance (PFGSTE NMR) spectroscopy has found widespread use in the quantification of self-diffusivity for many NMR-active nuclei, extending this technique to uncommon nuclei with unfavorable NMR properties remains an active area of research. Potassium-39 ( 39 K) is an archetypical NMR nucleus exhibiting an unfavorable gyromagnetic ratio combined with a very low Larmor frequency. Despite these unfavorable properties, this work demonstrates that 39 K PFGSTE NMR experiments are possible in aqueous solutions of concentrated potassium nitrite. Further, analysis of the results indicates that 39 K NMR diffusometry is feasible when the nuclei exhibit spin–lattice and spin–spin relaxation coefficients on the order of 60–100 ms and 50–100 ms, respectively. The diffusivity of 39 K followed Arrhenius behavior, and comparative 23 Na, 7 Li, and 1 H PFGSTE NMR studies of equimolal sodium nitrite and lithium nitrite solutions led to correlations between the enthalpy of hydration with the activation energy governing self-diffusion of the cations and also of water. Realizing the feasibility of 39 K PFGSTE NMR spectroscopy has a widespread impact across energy sciences because potassium is a common alkali element in energy storage materials and other applications.
74 ATOMIC AND MOLECULAR PHYSICS↗
Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy
Dynamic nuclear polarization (DNP) and indirect detection are two commonly applied approaches for enhancing the sensitivity of solid-state NMR spectroscopy. However, their use in tandem has not yet been investigated. With the advent of low-temperature fast magic angle spinning (MAS) probes with 1.3-mm diameter rotors capable of MAS at 40 kHz it becomes feasible to combine these two techniques. In this study, we performed DNP-enhanced 2D indirectly detected heteronuclear correlation (idHETCOR) experiments on 13 C, 15 N, 113 Cd and 89 Y nuclei in functionalized mesoporous silica, CdS nanoparticles, and Y 2 O 3 nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP polarization transfer efficiencies and large proton linewidth, the sensitivity gains achieved by indirect detection alone were lower than in conventional (non-DNP) experiments. Nevertheless, despite the smaller sample volume the 2D idHETCOR experiments showed better absolute sensitivities than 2D HETCOR experiments for nuclei with the lowest gyromagnetic ratios. Finally, for 89 Y, 2D idHETCOR provided 8.2 times better sensitivity than the 1 D 89 Y-detected CP experiment performed with a 3.2-mm rotor.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
t 1 -noise elimination by continuous chemical shift anisotropy refocusing
We report that due to their high gyromagnetic ratio, there is considerable interest in measuring distances and correlations involving protons, but such measurements are compounded by the simultaneous recoupling of chemical shift anisotropy (CSA). This secondary recoupling adds additional modulations to the signal intensities that ultimately lead to t 1 -noise and signal decay. Recently, Venkatesh et al. demonstrated that the addition of CSA refocusing periods during 1 H-X dipolar recoupling led to sequences with far higher stability and performance. Herein, we describe a related effort and develop a symmetry-based recoupling sequence that continually refocuses the 1 H CSA. This sequence shows superior performance to the regular and t1-noise eliminated D-HMQC sequences in the case of spin-1/2 nuclei and comparable performance to the later for half-integer quadrupoles.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Determination of the mutual orientation between proton CSA tensors mediated through band-selective 1 H– 1 H recoupling under fast MAS
We report the mutual orientation of nuclear spin interaction tensors provides critical information on the conformation and arrangement of molecules in chemicals, materials, and biological systems at an atomic level. Proton is a ubiquitous and important element in a variety of substances, and its NMR is highly sensitive due to their virtually 100% natural abundance and large gyromagnetic ratio. Nevertheless, the measurement of mutual orientation between the 1 H CSA tensors has remained largely untouched in the past due to strong 1 H– 1 H homonuclear interactions in a dense network of protons. In this study, we have developed a proton-detected 3D 1 H CSA/ 1 H CSA/ 1 H CS correlation method that utilizes three techniques to manage homonuclear interactions, namely fast magic-angle spinning, windowless C-symmetry-based CSA recoupling (windowless-ROCSA), and a band-selective 1 H– 1 H polarization transfer. The asymmetric 1 H CSA/ 1 H CSA correlated powder patterns produced by the C-symmetry-based methods are highly sensitive to the sign and asymmetry parameter of the 1 H CSA, and the Euler angle β as compared to the symmetric pattern obtained by the existing γ-encoded R-symmetry-based CSA/CSA correlation methods and allows a larger spectral area for data fitting. These features are beneficial for determining the mutual orientation between the nuclear spin interaction tensors with improved accuracy.
1H CSA↗
Coherent Erbium Spin Defects in Colloidal Nanocrystal Hosts
We demonstrate nearly a microsecond of spin coherence in Er 3+ ions doped in cerium dioxide nanocrystal hosts, despite a large gyromagnetic ratio and nanometric proximity of the spin defect to the nanocrystal surface. The long spin coherence is enabled by reducing the dopant density below the instantaneous diffusion limit in a nuclear spin-free host material, reaching the limit of a single erbium spin defect per nanocrystal. We observe a large Orbach energy in a highly symmetric cubic site, further protecting the coherence in a qubit that would otherwise rapidly decohere. Spatially correlated electron spectroscopy measurements reveal the presence of Ce 3+ at the nanocrystal surface, which likely acts as extraneous paramagnetic spin noise. Even with these factors, defect-embedded nanocrystal hosts show tremendous promise for quantum sensing and quantum communication applications, with multiple avenues, including core-shell fabrication, redox tuning of oxygen vacancies, and organic surfactant modification, available to further enhance their spin coherence and functionality in the future.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Optically Enhanced Solid-State 1 H NMR Spectroscopy
Low sensitivity is the primary limitation to extending nuclear magnetic resonance (NMR) techniques to more advanced chemical and structural studies. Photochemically induced dynamic nuclear polarization (photo-CIDNP) is an NMR hyperpolarization technique where light is used to excite a suitable donor–acceptor system, creating a spin-correlated radical pair whose evolution drives nuclear hyperpolarization. Systems that exhibit photo-CIDNP in solids are not common, and this effect has, up to now, only been observed for 13 C and 15 N nuclei. However, the low gyromagnetic ratio and natural abundance of these nuclei trap the local hyperpolarization in the vicinity of the chromophore and limit the utility for bulk hyperpolarization. Here, we report the first example of optically enhanced solid-state 1 H NMR spectroscopy in the high-field regime. This is achieved via photo-CIDNP of a donor–chromophore–acceptor molecule in a frozen solution at 0.3 T and 85 K, where spontaneous spin diffusion among the abundant strongly coupled 1 H nuclei relays polarization through the whole sample, yielding a 16-fold bulk 1 H signal enhancement under continuous laser irradiation at 450 nm. These findings enable a new strategy for hyperpolarized NMR beyond the current limits of conventional microwave-driven DNP.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Changes of Magnetism in a Magnetic Insulator due to Proximity to a Topological Insulator
We report here the modification of magnetism in a magnetic insulator Y 3 Fe 5 O 12 thin film by topological surface states (TSS) in an adjacent topological insulator Bi 2 Se 3 thin film. Ferromagnetic resonance measurements show that the TSS in Bi2Se3 produces a perpendicular magnetic anisotropy, results in a decrease in the gyromagnetic ratio, and enhances the damping in Y 3 Fe 5 O 12 . Such TSS-induced changes become more pronounced as the temperature decreases from 300 to 50 K. These results suggest a completely new approach for control of magnetism in magnetic thin films.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Fundamental 235 Uranium Nuclear Resonance Spectroscopy (End of Year Report)
Uranium-235 is ubiquitous in the nuclear industry however, detailed characterization by magnetic resonance spectroscopy has remained largely elusive to-date. Conventional nuclear magnetic resonance techniques are ill-suited for characterizing 235 U due to the small gyromagnetic ratio and extremely large quadrupole moment of this spin$^{7}$ /2 isotope. Thus, we have designed and built a high-frequency nuclear quadrupole resonance spectrometer for measuring the quadrupole resonance of this important isotope. A successful nuclear quadrupole resonance measurement of 235 U would be a significant accomplishment and could yield valuable physical parameters such as chemical shifts, local electric field gradients, and through-bond and through-space internuclear couplings, all of which are directly related to local structure. These terms can be used to understand structural details of poorly characterized uranium materials and can improve computational models of uranium for which accurate reference data is lacking
07 ISOTOPE AND RADIATION SOURCES↗