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Investigation of 15N-SABRE hyperpolarization at high pressures and in supercritical fluids 高压和超临界流体中的 15N-SABRE 超极化研究
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-04-26 DOI: 10.1016/j.jmr.2025.107876
Xiaoqing Li , Jacob R. Lindale , Loren L. Smith , Warren S. Warren
{"title":"Investigation of 15N-SABRE hyperpolarization at high pressures and in supercritical fluids","authors":"Xiaoqing Li ,&nbsp;Jacob R. Lindale ,&nbsp;Loren L. Smith ,&nbsp;Warren S. Warren","doi":"10.1016/j.jmr.2025.107876","DOIUrl":"10.1016/j.jmr.2025.107876","url":null,"abstract":"<div><div>Signal Amplification By Reversible Exchange (SABRE) is a parahydrogen-based hyperpolarization technique that can generate orders-of-magnitude larger signals than thermal spin polarization within a minute. However, this method is limited by the availability of parahydrogen to the solution. Previous work demonstrated SABRE-derived <sup>1</sup>H hyperpolarization at pressures up to 200 bar and using liquid carbon dioxide as a solvent. Here, we extend this work to demonstrate heteronuclear (<sup>15</sup>N) SABRE hyperpolarization using conventional solvents with hydrogen pressures up to 400 bar as well as the possibility of using supercritical CO<sub>2</sub> as the solvent. We demonstrate that in both modes, <sup>15</sup>N hyperpolarization comparable to SABRE-SHEATH may be achieved, providing a route for future optimization efforts as well as scale-up. We also present first steps towards exploring SABRE hyperpolarization of <sup>129</sup>Xe.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"375 ","pages":"Article 107876"},"PeriodicalIF":2.0,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143877082","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Single and double-selective split-inversion pulse and recovery (SIP-R) sequences for targeted T1 relaxation measurements
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-04-17 DOI: 10.1016/j.jmr.2025.107884
Zachary G. Mayes, Yugandhara A.M. Eriyagama, Lingyu Chi, Thomas P. Schuman, Klaus Woelk
{"title":"Single and double-selective split-inversion pulse and recovery (SIP-R) sequences for targeted T1 relaxation measurements","authors":"Zachary G. Mayes,&nbsp;Yugandhara A.M. Eriyagama,&nbsp;Lingyu Chi,&nbsp;Thomas P. Schuman,&nbsp;Klaus Woelk","doi":"10.1016/j.jmr.2025.107884","DOIUrl":"10.1016/j.jmr.2025.107884","url":null,"abstract":"<div><div>Split-Inversion-Pulse and Recovery (SIP-R) is a recently introduced NMR methodology for acquiring spin-lattice relaxation data with a robust decay-to-zero intensity profile as a function of recovery time. This decay-to-zero behavior is particularly advantageous for extracting multiple relaxation times and coefficients using inverse Laplace transformation (ILT) algorithms. In this study, two frequency-selective adaptations of SIP-R are introduced, incorporating either one or two frequency-selective pulses in the SIP-R dual-scan experiment to excite only specific spectral regions. In a test using a non-viscous, small-molecule solution of ethanol in D₂O, both single- and double-selective SIP-R sequences reproduced reasonably well the relaxation times obtained with the non-selective SIP-R method. However, the double-selective SIP-R experiment introduced additional, shorter relaxation times, which were interpreted as artifacts due to the extended duration of the second frequency-selective pulse. Applying the non-selective SIP-R method to a polymer hydrogel enabled the quantitative differentiation of freely moving water molecules (95 %) and water tightly bound to the polymer chains (5 %). The frequency-selective SIP-R variants revealed strong NOE effects between water and polymeric amide resonances, similar to previous findings that suggest strong interactions between water molecules and amine groups in a different type of polymer hydrogel.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"375 ","pages":"Article 107884"},"PeriodicalIF":2.0,"publicationDate":"2025-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143847904","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Exact solution of the parameter identification inverse problem for the Bloch–McConnell equations. Longitudinal magnetization
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-30 DOI: 10.1016/j.jmr.2025.107873
Ivan Argatov, Vitaly Kocherbitov
{"title":"Exact solution of the parameter identification inverse problem for the Bloch–McConnell equations. Longitudinal magnetization","authors":"Ivan Argatov,&nbsp;Vitaly Kocherbitov","doi":"10.1016/j.jmr.2025.107873","DOIUrl":"10.1016/j.jmr.2025.107873","url":null,"abstract":"<div><div>A two-site magnetic exchange model comprising a set of two linear first-order differential Bloch–McConnell equations is considered. The relaxation and exchange behavior is described using a symmetrical form of the general solution derived in the case of longitudinal magnetization for the zero initial conditions. The inverse problem with limited magnetization information has been solved exactly in an analytical explicit form under mild <em>a priori</em> knowledge about the exchange and relaxation parameters.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"375 ","pages":"Article 107873"},"PeriodicalIF":2.0,"publicationDate":"2025-03-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143760667","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Chemical exchange in unstable emulsions
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-28 DOI: 10.1016/j.jmr.2025.107875
Ke Xu, Jörn Schmedt auf der Günne
{"title":"Chemical exchange in unstable emulsions","authors":"Ke Xu,&nbsp;Jörn Schmedt auf der Günne","doi":"10.1016/j.jmr.2025.107875","DOIUrl":"10.1016/j.jmr.2025.107875","url":null,"abstract":"<div><div>Nuclear magnetic resonance (NMR) is a routine method to study chemical exchange in reactions and molecular rearrangements in solution. However, when it comes to exchange of molecular species in liquid-liquid, two phase systems like in phase-transfer catalysis, the rate becomes a function of the surface area between two phases, which means that only persistent emulsions could be studied with standard equipment. Unstable emulsions, which rapidly demix, require a continuous application of shear forces by stirring. Here, a setup is described with which unstable emulsions can be produced and studied in-situ by solution NMR spectroscopy. The setup provides sufficient torque and spinning frequency for generating an unstable two-phase water/oil mixture by rapid stirring. The pneumatically driven stirrer in the probe head was designed using ideas borrowed from magic angle sample spinning and a prototype was produced by 3D printing. As proof of concept, the dynamics in an aniline water emulsion over the phase boundary are studied by regular exchange spectroscopy NMR experiments.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"375 ","pages":"Article 107875"},"PeriodicalIF":2.0,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143746888","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Cryogenic field-cycling instrument for optical NMR hyperpolarization studies
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-28 DOI: 10.1016/j.jmr.2025.107874
Noella D'Souza , Kieren A. Harkins , Cooper Selco , Ushoshi Basumallick , Samantha Breuer , Zhuorui Zhang , Paul Reshetikhin , Marcus Ho , Aniruddha Nayak , Maxwell McAllister , Emanuel Druga , David Marchiori , Ashok Ajoy
{"title":"Cryogenic field-cycling instrument for optical NMR hyperpolarization studies","authors":"Noella D'Souza ,&nbsp;Kieren A. Harkins ,&nbsp;Cooper Selco ,&nbsp;Ushoshi Basumallick ,&nbsp;Samantha Breuer ,&nbsp;Zhuorui Zhang ,&nbsp;Paul Reshetikhin ,&nbsp;Marcus Ho ,&nbsp;Aniruddha Nayak ,&nbsp;Maxwell McAllister ,&nbsp;Emanuel Druga ,&nbsp;David Marchiori ,&nbsp;Ashok Ajoy","doi":"10.1016/j.jmr.2025.107874","DOIUrl":"10.1016/j.jmr.2025.107874","url":null,"abstract":"<div><div>Optical dynamic nuclear polarization (DNP) offers an attractive approach to enhancing the sensitivity of nuclear magnetic resonance (NMR) spectroscopy. Efficient, optically-generated electron polarization can be leveraged to operate across a broad range of temperatures and magnetic fields, making it particularly appealing for applications requiring high DNP efficiency or spatial resolution. While a large class of systems hold promise for optical DNP, many candidates display both variable electron polarizability and electron and nuclear <em>T</em><sub>1</sub> relaxation times as functions of magnetic field and temperature. This necessitates tools capable of studying DNP under diverse experimental conditions. To address this, we introduce a cryogenic field cycling instrument that facilitates optical DNP studies across a wide range of magnetic fields (10 mT–9.4 T) and temperatures (∼10 K–300 K) for wide-bore magnets. Continuous cryogen replenishment enables sustained, long-term operation. Additionally, the system supports the ability to manipulate and probe rapidly hyperpolarized (∼60 s) nuclear spins via pulse sequences involving millions of RF pulses. We describe innovations in the device design and demonstrate its operation on a model system of <sup>13</sup>C nuclear spins in diamond polarized through optically pumped nitrogen vacancy (NV) centers. We anticipate the use of the instrument for a broad range of optical DNP systems and studies.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"375 ","pages":"Article 107874"},"PeriodicalIF":2.0,"publicationDate":"2025-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143814904","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A concept of volume wireless receive-only coil for 1.5T MRI
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-21 DOI: 10.1016/j.jmr.2025.107841
Aleksandr Fedotov , Pavel Tikhonov , Viktor Puchnin , Ekaterina Brui , Anatoliy Levchuk , Ayshat Karaeva , Alena Shchelokova , Georgiy Solomakha , Anna Hurshkainen
{"title":"A concept of volume wireless receive-only coil for 1.5T MRI","authors":"Aleksandr Fedotov ,&nbsp;Pavel Tikhonov ,&nbsp;Viktor Puchnin ,&nbsp;Ekaterina Brui ,&nbsp;Anatoliy Levchuk ,&nbsp;Ayshat Karaeva ,&nbsp;Alena Shchelokova ,&nbsp;Georgiy Solomakha ,&nbsp;Anna Hurshkainen","doi":"10.1016/j.jmr.2025.107841","DOIUrl":"10.1016/j.jmr.2025.107841","url":null,"abstract":"<div><div>Wireless radio frequency coils offer an alternative to conventional cable-connected coils due to their compatibility with multiple vendor MRI systems and reduced electromagnetic interaction with the environment of the MRI scanner. However, wireless coils being inductively coupled with a transceiver body coil require manual input power calibration due to the significant increase of a body coil transmit efficiency locally in the region of interest and disturbance of <span><math><msubsup><mrow><mi>B</mi></mrow><mrow><mn>1</mn></mrow><mrow><mo>+</mo></mrow></msubsup></math></span> homogeneity complicating routine scanning procedures. This study aims to implement the concept of a wireless receive-only coil for female breast MRI at 1.5T. The approach combines the advantages of wireless coils to increase signal to noise ratio of transceiver body coil in the target region of interest and the ability to perform the automatic reference voltage calibration.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"374 ","pages":"Article 107841"},"PeriodicalIF":2.0,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143716197","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Design of planar transmission line microwave probes for broadband EPR spectroscopy
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-18 DOI: 10.1016/j.jmr.2025.107866
Selina Eckel , Julian Nagel , Mazin Jouda , Jan Gerrit Korvink , Ahmet Çağrı Ulusoy
{"title":"Design of planar transmission line microwave probes for broadband EPR spectroscopy","authors":"Selina Eckel ,&nbsp;Julian Nagel ,&nbsp;Mazin Jouda ,&nbsp;Jan Gerrit Korvink ,&nbsp;Ahmet Çağrı Ulusoy","doi":"10.1016/j.jmr.2025.107866","DOIUrl":"10.1016/j.jmr.2025.107866","url":null,"abstract":"<div><div>In broadband transmission-based electron paramagnetic resonance (EPR) spectrometers, non-resonant planar microwave probes play a key role, but very few systematic explorations of their design space exist. We develop design guidelines for two common types of transmission lines, microstrip and coplanar waveguide, to achieve a high effective microwave magnetic field strength, which ultimately leads to a more sensitive EPR measurement set-up. We compare the optimized transmission line structures and show that the coplanar waveguide achieves a higher simulated effective magnetic field strength. The simulation results are confirmed by EPR measurements up to a microwave frequency of 45<!--> <!-->GHz.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"374 ","pages":"Article 107866"},"PeriodicalIF":2.0,"publicationDate":"2025-03-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143684075","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
NMR of a single nuclear spin detected by a scanning tunnelling microscope 用扫描隧道显微镜探测单个核自旋的核磁共振成像
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-11 DOI: 10.1016/j.jmr.2025.107863
Yishay Manassen , Michael Averbukh , Zion Hazan , Yahel Tzuriel , Pino Boscolo , Alexander Shnirman , Baruch Horovitz
{"title":"NMR of a single nuclear spin detected by a scanning tunnelling microscope","authors":"Yishay Manassen ,&nbsp;Michael Averbukh ,&nbsp;Zion Hazan ,&nbsp;Yahel Tzuriel ,&nbsp;Pino Boscolo ,&nbsp;Alexander Shnirman ,&nbsp;Baruch Horovitz","doi":"10.1016/j.jmr.2025.107863","DOIUrl":"10.1016/j.jmr.2025.107863","url":null,"abstract":"<div><div>We detect a single spin nuclear magnetic resonance (NMR) by monitoring the intensity modulations of a selected hyperfine line in the electron spin resonance (ESR) spectrum. We analyse the power spectrum of the corresponding hyperfine intensity and obtain the nuclear magnetic resonance (NMR) spectrum. Our process also demonstrates ionization of a molecule with the bias voltage of a Scanning Tunnelling Microscope (STM), allowing detection of NMR even in molecules that are non-radical in their neutral state. We have observed this phenomenon in four types of molecules: toluene, triphenylphosphine, TEMPO and adenosine triphosphate (ATP) showing NMR of <span><math><msup><mrow></mrow><mrow><mn>1</mn></mrow></msup></math></span>H, <sup>13</sup>C, <sup>31</sup>P and <sup>14</sup>N nuclei. The spectra are detailed and show signatures of the chemical environment, i.e. chemical shifts. A theoretical model to account for these data is outlined.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"374 ","pages":"Article 107863"},"PeriodicalIF":2.0,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143628443","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Construction and testing of a high-homogeneity 55 T pulsed magnet for high-field nuclear magnetic resonance measurements
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-08 DOI: 10.1016/j.jmr.2025.107862
Wenqi Wei, Luchen Wei, Shunkun Ouyang, Kangjian Luo, Zhuo Wang, Shiyu Liu, Yongkang Luo, Xiaotao Han
{"title":"Construction and testing of a high-homogeneity 55 T pulsed magnet for high-field nuclear magnetic resonance measurements","authors":"Wenqi Wei,&nbsp;Luchen Wei,&nbsp;Shunkun Ouyang,&nbsp;Kangjian Luo,&nbsp;Zhuo Wang,&nbsp;Shiyu Liu,&nbsp;Yongkang Luo,&nbsp;Xiaotao Han","doi":"10.1016/j.jmr.2025.107862","DOIUrl":"10.1016/j.jmr.2025.107862","url":null,"abstract":"<div><div>High-field nuclear magnetic resonance (NMR) experiments call for the further development of pulsed magnets with a more practical winding structure and higher magnetic field homogeneity. This study presents the construction method and test results of a high-homogeneity pulsed magnet based on an optimized localized split structure. A winding craft using gap spacers was developed for the precise winding of split-gap transition wires. Magnetic field mapping was achieved in a steady-state low field of 32 mT using a Hall probe, with a measured magnetic field inhomogeneity of 198 ± 19 ppm over 1 cm diameter of spherical volume (DSV). The full-width at half-maximum (FWHM) of NMR spectra was adopted as a means of evaluating the magnetic field homogeneity in the pulsed field. In the optimal position, the measured FWHM is 42.2 ± 2.5 ppm at the low field of 7.7 T over a sample volume of 12.6 mm<sup>3</sup>. At the high field of 50 T, the FWHM decreases to 16.2 ± 0.8 ppm, which is a superior value achieved in similar reported pulsed magnets.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"374 ","pages":"Article 107862"},"PeriodicalIF":2.0,"publicationDate":"2025-03-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143593396","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Relativistic effects on the magnetic shielding in solids: First-principles computation in a plane wave code
IF 2 3区 化学
Journal of magnetic resonance Pub Date : 2025-03-07 DOI: 10.1016/j.jmr.2025.107861
J.W. Zwanziger, A.R. Farrant, U. Werner-Zwanziger
{"title":"Relativistic effects on the magnetic shielding in solids: First-principles computation in a plane wave code","authors":"J.W. Zwanziger,&nbsp;A.R. Farrant,&nbsp;U. Werner-Zwanziger","doi":"10.1016/j.jmr.2025.107861","DOIUrl":"10.1016/j.jmr.2025.107861","url":null,"abstract":"<div><div>For computing the magnetic shielding in solids, density functional theory as implemented in a plane wave basis has proven to be a reasonably accurate and efficient framework, at least for lighter atoms through the third row of the periodic table. In materials with heavier atoms, terms not usually included in the electronic Hamiltonian can become significant, limiting accuracy. Here we derive and implement the zeroth-order regular approximation (ZORA) relativistic terms in the presence of both external magnetic fields and internal nuclear magnetic dipoles, to derive the ZORA-corrected magnetic shielding in the context of periodic boundary conditions and a plane wave basis. We describe our implementation in an open source code, <span>Abinit</span>, and show how it correctly predicts magnetic shieldings in various scenarios, for example the heavy atom next to light atom cases of the III–V semiconductors such as AlSb.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"374 ","pages":"Article 107861"},"PeriodicalIF":2.0,"publicationDate":"2025-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143578012","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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