Journal of Magnetic Resonance

Nuclear spin hyperpolarization techniques, such as dynamic nuclear polarization (DNP) and parahydrogen-induced polarization (PHIP), have revolutionized nuclear magnetic resonance and magnetic resonance imaging. In these methods, a readily available source of high spin order, either electron spins in DNP or singlet states in hydrogen for PHIP, is brought into close proximity with nuclear spin targets, enabling efficient transfer of spin order under external quantum control. Despite vast disparities in energy scales and interaction mechanisms between electron spins in DNP and nuclear singlet states in PHIP, a pseudo-spin formalism allows us to establish an intriguing equivalence...

We reveal an interplay between temperature and radical concentration necessary to establish thermal mixing (TM) as an efficient dynamic nuclear polarization (DNP) mechanism. We conducted DNP experiments by hyperpolarizing widely used DNP samples, i.e., sodium pyruvate-1-13 C in water/glycerol mixtures at varying nitroxide radical (TEMPOL) concentrations and microwave irradiation frequencies, measuring proton and carbon-13 spin temperatures. Using a cryogen consumption-free prototype-DNP apparatus, we could probe cryogenic temperatures between 1...

MRI systems have a thin conducting layer placed between the gradient and RF coils, this acts as a shield at the RF-frequency, minimizing noise coupled into the experiment, and decreasing the coupling between the RF and gradient coils. Ideally, this layer should be transparent to the gradient fields to reduce eddy currents. In this work the design of such a shield, specifically for low-field point-of-care Halbach based MRI devices, is discussed. A segmented double layer shield is designed and constructed based on eddy current simulations...

The rapid advancement of parahydrogen-induced hyperpolarization (PHIP) and its diverse array of applications highlights the critical need for enhanced signals in both 1 H NMR and heteronuclear NMR spectroscopy. Simultaneously, there is an increasing interest in utilizing benchtop NMR analysis across various laboratory settings. However, due to their lower magnetic fields, benchtop NMR spectrometers inherently produce weaker signal intensities. Here, PHIP is a well-established solution to this challenge. Consequently, we are expanding our cost-effective PHIP setup from a high-field NMR spectrometer (11...

Proton-detected INADEQUATE NMR experiments are widely used for structure elucidation of small molecules, in particular the implementations that display 13 C single-quantum rather than double-quantum frequencies in the indirect dimension of 2D spectra. But unfortunately, such spectra in addition to the desired 1 H-13 C two-bond correlations also contain HSQC artifacts of comparable magnitude. The redesigned versatile experiment presented in this paper requires no compromise based on different 13 C multiplicities and suppresses the HSQC artifacts that are a source of possible spectral misinterpretation...

The measurement of translational diffusion coefficients by NMR generally makes use basically of two magnetic field gradient pulses separated by a so-called diffusion interval. The magnetic field gradient arises either from the static magnetic field (denoted by B0 used for polarizing the nuclear spins) or from the radio-frequency field (denoted by B1 used for inducing NMR transitions). The B0 method may be hampered by short effective transverse relaxation times (T2 ∗ ), by important gradient rise and fall times or by eddy currents...

Solution NMR spectroscopy has tremendous potential for providing atomic resolution insights into the interactions between proteins and nucleic acids partitioned into condensed phases of phase-separated systems. However, the highly viscous nature of the condensed phase challenges applications, and in particular, the extraction of quantitative, site-specific information. Here, we present a delayed decoupling-based HMQC pulse sequence for methyl-TROSY studies of 'client' proteins and nucleic acids partitioned into 'scaffold' proteinaceous phase-separated solvents...

Identification of reservoir rock types is necessary for the exploration and recovery of oil and gas. It involves determining the petrophysical properties of rocks such as porosity and permeability which play a significant role in developing reservoir models, estimating the volumes of oil and gas reserves, and planning production methods. Nuclear magnetic resonance (NMR) technology is a fast and accurate tool for petrophysical rock characterization. The distributions of relaxation times (T2 distributions) offer valuable insights into the distribution of pore sizes in rocks, and these distributions are closely linked to important petrophysical parameters like porosity, permeability, and bound fluid volume (BFV)...

The open-source console MaRCoS, which stands for "Magnetic Resonance Control System", combines hardware, firmware and software elements for integral control of Magnetic Resonance Imaging (MRI) scanners. Previous developments have focused on making the system robust and reliable, rather than on users, who have been somewhat overlooked. This work describes a Graphical User Interface (GUI) designed for intuitive control of MaRCoS, as well as compatibility with clinical environments. The GUI is based on an arrangement of tabs and a renewed Application Program Interface (API)...

The NMRduino is a compact, cost-effective, sub-MHz NMR spectrometer that utilizes readily available open-source hardware and software components. One of its aims is to simplify the processes of instrument setup and data acquisition control to make experimental NMR spectroscopy accessible to a broader audience. In this introductory paper, the key features and potential applications of NMRduino are described to highlight its versatility both for research and education.

In situ NMR is a valuable tool for studying electrochemical devices, including redox flow batteries and electrocatalytic reactors, capable of detecting reaction intermediates, metastable states, time evolution of processes or monitoring stability as a function of electrochemical conditions. Here we report a parallel line detector for spatially selective in situ electrochemical NMR spectroscopy. The detector consists of 17 copper wires and is doubly tuned to 1 H/19 F and X nuclei ranging from 63 Cu (106...

Accurate signal assignments can be challenging for congested solid-state NMR (ssNMR) spectra. We describe an automatic sequential assignment program (ASAP) to partially overcome this challenge. ASAP takes three input files: the residue type assignments (RTAs) determined from the better-resolved NCACX spectrum, the full peak list of the NCOCX spectrum, and the protein sequence. It integrates our auto-residue type assignment strategy (ARTIST) with the Monte Carlo simulated annealing (MCSA) algorithm to overcome the hurdle for accurate signal assignments caused by incomplete side-chain resonances and spectral congestion...

Intrinsically disordered proteins (IDPs) defy the conventional structure-function paradigm by lacking a well-defined tertiary structure and exhibiting inherent flexibility. This flexibility leads to distinctive spin relaxation modes, reflecting isolated and specific motions within individual peptide planes. In this work, we propose a new pulse sequence to measure the longitudinal 13 C' CSA-13 C' -13 Cα DD CCR rate [Formula: see text] and present a novel 3D version of the transverse [Formula: see text] CCR rate, adopting the symmetrical reconversion approach...

In continuous-wave electron paramagnetic resonance imaging (CW EPRI), data are collected generally at densely sampled views sufficient for achieving accurate reconstruction of a four dimensional spectral-spatial (4DSS) image by use of the conventional filtered-backprojection (FBP) algorithm. It is desirable to minimize the scan time by collection of data only at sparsely sampled views, referred to as sparse-view data. Interest thus remains in investigation of algorithms for accurate reconstruction of 4DSS images from sparse-view data collected for potentially enabling fast data acquisition in CW EPRI...

Precise radiation guided by oxygen images has demonstrated superiority over the traditional radiation methods. Electron paramagnetic resonance (EPR) imaging has proven to be the most advanced oxygen imaging modality. However, the main drawback of EPR imaging is the long scan time. For each projection, we usually need to collect the projection many times and then average them to achieve high signal-to-noise ratio (SNR). One approach to fast scan is to reduce the repeating time for each projection. While the projections would be noisy and thus the traditional commonly-use filtered backprojection (FBP) algorithm would not be capable of accurately reconstructing images...

Nuclear magnetic resonance (NMR) based 13 C tracing has broad applications across medical and environmental research. As many biological and environmental samples are heterogeneous, they experience considerable spectral overlap and relatively low signal. Here a 1D 1 H-12 C/13 C is introduced that uses "in-phase/opposite-phase" encoding to simultaneously detect and discriminate both protons attached to 12 C and 13 C at full 1 H sensitivity in every scan. Unlike traditional approaches that focus on the 12 C/13 C satellite ratios in a 1 H spectrum, this approach creates separate sub-spectra for the 12 C and 13 C bound protons...

Spectral diffusion of electron spin polarization plays a key part in dynamic nuclear polarization (DNP). It determines the distribution of polarization across the electron spin resonance (ESR) line and consequently the polarization that is available for transfer to the nuclear spins. Various authors have studied it experimentally by means of electron-electron double resonance (ELDOR) and proposed and used macroscopic models to interpret these experiments. However, microscopic models predicting the rate of spectral diffusion are scarce...

Biomolecular solid-state magic angle spinning (MAS) NMR spectroscopy frequently relies on selective 13 C-15 N magnetization transfers, for various kinds of correlation experiments. Introduced in 1998, spectrally induced filtering in combination with cross polarization (SPECIFIC-CP) is a selective heteronuclear magnetization transfer experiment widely used for biological applications. At MAS frequencies below 20 kHz, commonly used for 13 C-detected MAS NMR experiments, SPECIFIC-CP transfer between amide 15 N and 13 Cα atoms (NCA) is typically performed with radiofrequency (rf) fields set higher than the MAS frequency for both 13 C and 15 N channels, and high-power 1 H decoupling rf field is simultaneously applied...

MRI is essential for evaluating and diagnosing various conditions affecting the temporomandibular joint (TMJ) and surrounding structures, as it provides highly detailed images that enable healthcare professionals to assess the joints and surroundings in great detail. While commercial MRI scanners typically come equipped with basic receive coils, such as the head receive array, RF coils tailored for specialized applications like TMJ MRI must be obtained separately. Consequently, TMJ MRI scans are often conducted using the head receive array, yet this configuration proves suboptimal due to the lack of specialized coils...

In this work we achieve a significant overpopulation (PLLS ≈1%) of the long-lived spin state (LLS) of methylene protons in 2-bromoethan(2 H)ol (BrEtOD) obtained in a reaction between ethylene with non-equilibrium nuclear spin order and bromine water. Given all protons in ethylene are magnetically equivalent, its nuclear states are classified into nuclear spin isomers (NSIM) with total spin I = 2,1,0. Addition of parahydrogen to acetylene produces ethylene with a population of only those NSIMs with I = 1,0...