Journal of Magnetic Resonance Open最新文献

{"title":"13C-Formate as an indirect low-temperature 1H lineshape polarimeter","authors":"Stuart J. Elliott ,&nbsp;Quentin Stern,&nbsp;Sami Jannin","doi":"10.1016/j.jmro.2024.100162","DOIUrl":"10.1016/j.jmro.2024.100162","url":null,"abstract":"<div><div>¹H polarization quantification is important for dissolution-dynamic nuclear polarization (<em>d</em>DNP) but can be cumbersome due to the requirement of acquiring thermal equilibrium signals and measurements that are complicated by large background signals. ¹H nuclear magnetic resonance (NMR) spectra can also be deleteriously influenced by line distortions linked with radiation damping from ¹H DNP and cannot be used for accurate calculation of ¹H polarization. Determining ¹H polarization via immediate ¹³C lineshape analysis of a simple molecule removes such complications. We present ¹³C-sodium formate as a straightforward system for indirect ¹H polarimetry. The ¹³C NMR spectra acquired under <em>d</em>DNP conditions have distinct features that are readily reproduced with ¹³C lineshape simulations. ¹H polarizations built-up during ¹H DNP were indirectly inferred by fitting simulations to ¹³C lineshapes. We provide the <em>MATLAB</em> scripts used for ¹³C lineshape analysis in order that the method can be readily implemented in other laboratories.</div></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"21 ","pages":"Article 100162"},"PeriodicalIF":2.624,"publicationDate":"2024-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142427292","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Investigation of biomolecular dynamics by sensitivity-enhanced 1H–2H CPMAS NMR using matrix-free dynamic nuclear polarization","authors":"Thomas Biedenbänder ,&nbsp;Aryana Rodgers ,&nbsp;Mirjam Schröder ,&nbsp;Liliya Vugmeyster ,&nbsp;Björn Corzilius","doi":"10.1016/j.jmro.2024.100161","DOIUrl":"10.1016/j.jmro.2024.100161","url":null,"abstract":"<div><div>Molecular dynamics of functional groups contain valuable information about structural properties and functional activities in biomolecules. NMR spectroscopy is a sensitive tool for the investigation of molecular dynamics over a wide range of timescales and thus may deepen the understanding of the biomolecules of interest. Here, we present an approach to use DNP-enhanced ²H NMR to study dynamics of selectively deuterated methyl groups in insoluble proteins such as amyloid beta (Aβ) fibrils. We adopted and optimized the matrix-free DNP approach by varying the amount of added polarizing agent as well as the rehydration level of model proteins. We show that the DNP enhancement obtained in ¹H–²H cross-polarization (CP) MAS spectra may increase the sensitivity for selectively deuterated Aβ fibril samples by more than one order of magnitude, accelerating the collection of spin-lattice relaxation data in the DNP-accessible temperature range between 100 and 150 K by up to 400-fold. However, below the coalescence temperature, which describes the transition from the fast to the slow exchange regime, the experimentally obtained relaxation time constants suffer from a paramagnetic relaxation enhancement effect due to the presence of the polarizing agent. This seems to be a general effect for biomolecules as it is also confirmed for two other protein model systems. Our demonstration opens the possibility to extend the scope of ²H NMR for dynamics measurements to effective concentrations and/or temperatures below what is currently accessible; however, the observed interplay between paramagnetic relaxation and molecular dynamics also emphasizes the necessity for a better understanding of relaxation effects in DNP-enhanced NMR.</div></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"21 ","pages":"Article 100161"},"PeriodicalIF":2.624,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142320067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"DNP enhanced solid-state NMR – A powerful tool to address the surface functionalization of cellulose/paper derived materials","authors":"Mark V. Höfler ,&nbsp;Jonas Lins ,&nbsp;David Seelinger ,&nbsp;Lukas Pachernegg ,&nbsp;Timmy Schäfer ,&nbsp;Stefan Spirk ,&nbsp;Markus Biesalski ,&nbsp;Torsten Gutmann","doi":"10.1016/j.jmro.2024.100163","DOIUrl":"10.1016/j.jmro.2024.100163","url":null,"abstract":"<div><div>This concept summarizes recent advances in development and application of DNP enhanced multinuclear solid-state NMR to study the molecular structure and surface functionalization of cellulose and paper-based materials. Moreover, a novel application is presented where DNP enhanced ¹³C and ¹⁵N solid-state NMR is used to identify structure moieties formed by cross-linking of hydroxypropyl cellulose. Given these two aspects of this concept-type of article, we thus combine both, a review on recent findings already published and unpublished recent data that complement the existing knowledge in the field of characterization of functional lignocellulosic materials by DNP enhanced solid-state NMR.</div></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"21 ","pages":"Article 100163"},"PeriodicalIF":2.624,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142320068","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Dual hyperpolarized [1-13C]pyruvate and [13C]urea magnetic resonance imaging of prostate cancer","authors":"Ivan de Kouchkovsky ,&nbsp;Hao Nguyen ,&nbsp;Hsin-Yu Chen ,&nbsp;Xiaoxi Liu ,&nbsp;Hecong Qin ,&nbsp;Bradley A. Stohr ,&nbsp;Romelyn Delos Santos ,&nbsp;Michael A. Ohliger ,&nbsp;Zhen Jane Wang ,&nbsp;Robert A. Bok ,&nbsp;Jeremy W. Gordon ,&nbsp;Peder E.Z. Larson ,&nbsp;Mary Frost ,&nbsp;Kimberly Okamoto ,&nbsp;Daniel Gebrezgiabhier ,&nbsp;Matthew Cooperberg ,&nbsp;Daniel B. Vigneron ,&nbsp;John Kurhanewicz ,&nbsp;Rahul Aggarwal","doi":"10.1016/j.jmro.2024.100165","DOIUrl":"10.1016/j.jmro.2024.100165","url":null,"abstract":"&lt;div&gt;&lt;h3&gt;Background&lt;/h3&gt;&lt;p&gt;Although multiparametric (mp) &lt;sup&gt;1&lt;/sup&gt;H magnetic resonance imaging (MRI) is increasingly used to detect and localize prostate cancer (PC), its correlation with tumor grade is limited. Hyperpolarized (HP) carbon-13 (&lt;sup&gt;13&lt;/sup&gt;C) MR is an emerging imaging technique, which can be used to interrogate key biologic processes through in vivo detection of various HP probes. A distinct attribute of HP &lt;sup&gt;13&lt;/sup&gt;C MRI is the ability to detect multiple HP probes within a single acquisition. Here we report on the first simultaneous dual HP [1-&lt;sup&gt;13&lt;/sup&gt;C]pyruvate and [&lt;sup&gt;13&lt;/sup&gt;C]urea MRI with correlations to histopathologic findings in a patient with localized PC scheduled for radical prostatectomy.&lt;/p&gt;&lt;/div&gt;&lt;div&gt;&lt;h3&gt;Material and methods&lt;/h3&gt;&lt;p&gt;Paired HP &lt;sup&gt;13&lt;/sup&gt;C and standard mp &lt;sup&gt;1&lt;/sup&gt;H MRI were performed in a patient with biopsy-proven Gleason score 4 + 3 = 7 adenocarcinoma of the prostate scheduled for radical prostatectomy through a first-in-human pilot study of dual-agent HP MRI (NCT02526368). HP &lt;sup&gt;13&lt;/sup&gt;C MRI was performed using a clinical 3T scanner with &lt;sup&gt;13&lt;/sup&gt;C transmit-and-receive capabilities. Dynamic series of HP &lt;sup&gt;13&lt;/sup&gt;C pyruvate, lactate and urea imaging were acquired following intravenous (IV) injection of co-hyperpolarized [&lt;sup&gt;13&lt;/sup&gt;C]urea (25 mM) and [1–&lt;sup&gt;13&lt;/sup&gt;C]pyruvate (125 mM). The [1-&lt;sup&gt;13&lt;/sup&gt;C]pyruvate-to-[1-&lt;sup&gt;13&lt;/sup&gt;C]lactate conversion rate (k&lt;sub&gt;PL&lt;/sub&gt;) was calculated using an inputless two-site exchange model; AUC&lt;sub&gt;urea&lt;/sub&gt; was the [&lt;sup&gt;13&lt;/sup&gt;C]urea signal summed over time. Following radical prostatectomy, whole-mount prostate histopathological slides were prepared and reviewed by an experienced genitourinary pathologist.&lt;/p&gt;&lt;/div&gt;&lt;div&gt;&lt;h3&gt;Results&lt;/h3&gt;&lt;p&gt;Following informed consent, the patient underwent paired mp &lt;sup&gt;1&lt;/sup&gt;H MRI and dual-agent HP MRI. mp &lt;sup&gt;1&lt;/sup&gt;H MRI revealed a 1.2 cm lesion in the left apical posterior zone. Dual-agent HP MRI identified a focus of increased [1-&lt;sup&gt;13&lt;/sup&gt;C]pyruvate-to-[1-&lt;sup&gt;13&lt;/sup&gt;C]lactate conversion rate (k&lt;sub&gt;PL&lt;/sub&gt;) extending from the left apical posterior peripheral zone to the right gland. A corresponding area of abnormal tissue perfusion (AUC&lt;sub&gt;urea&lt;/sub&gt;) was seen in the left gland. Metabolism-perfusion mismatch (with several foci of increased &lt;em&gt;k&lt;sub&gt;PL&lt;/sub&gt;&lt;/em&gt;/AUC&lt;sub&gt;urea&lt;/sub&gt;) was observed throughout the tumor. Tumor extension to the right midgland was confirmed at the time of radical prostatectomy and staining for lactate dehydrogenase-A was increased throughout the tumor relative to surrounding benign prostatic tissue.&lt;/p&gt;&lt;/div&gt;&lt;div&gt;&lt;h3&gt;Conclusion&lt;/h3&gt;&lt;p&gt;This first-in-human radiopathologic study demonstrates the feasibility of dual-agent HP MRI in PC patients. Simultaneous assessment of tumor metabolism and perfusion was able to detect occult disease as well as to show a significant mismatch between intra-tumoral metabolism and tissue perfusion in high-grade PC. ","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"21 ","pages":"Article 100165"},"PeriodicalIF":2.624,"publicationDate":"2024-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000207/pdfft?md5=7b66657cb74e70c1242c4491d6fa3a40&pid=1-s2.0-S2666441024000207-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142232386","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Discontinuous hyperpolarization schemes in liquid-state overhauser dynamic nuclear polarization experiments","authors":"Alex van der Ham","doi":"10.1016/j.jmro.2024.100160","DOIUrl":"10.1016/j.jmro.2024.100160","url":null,"abstract":"<div><p>Liquid-state Overhauser Dynamic Nuclear Polarization (ODNP) is an emerging technique, aimed at shortening NMR experiment times. It achieves this by increasing the otherwise poor nuclear polarization at room temperature, by polarization transfer from excited electron spins. The present work explores two ideas, aimed at achieving the optimal signal-to-noise per time unit for a given system, and quantitation of spectra showing a large disparity in ODNP enhancements at high magnetic fields (≥ 9.4 T). Both of these ideas are predicated on, perhaps counterintuitively, not allowing full dynamic nuclear polarization to build up, either by rapid rf pulsing, or gating of the microwave irradiation.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"21 ","pages":"Article 100160"},"PeriodicalIF":2.624,"publicationDate":"2024-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000153/pdfft?md5=1b851004339d56ccb0489d8db665fe26&pid=1-s2.0-S2666441024000153-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142167439","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Creating high, portable proton polarization with photo-excited triplet DNP","authors":"P. Hautle,&nbsp;W.Th. Wenckebach","doi":"10.1016/j.jmro.2024.100159","DOIUrl":"10.1016/j.jmro.2024.100159","url":null,"abstract":"<div><p>Dynamic nuclear polarization (DNP) is a powerful tool to polarize nuclear spins and enhance the intensity of their magnetic resonance signal. For DNP a sample is doped with an agent providing unpaired electron spins. Then the sample is cooled in a strong magnetic field to polarize these electron spins and a microwave field is applied to transfer this polarization to the nuclear spins. While DNP is very efficient, it has two inherent issues: the electron spins needed to polarize the nuclear spins are also the main source of polarization decay. Furthermore, polarizing the electron spins requires strong magnets and powerful cryogenics, that may obstruct further use of the polarized nuclear spins.</p><p>These issues can be addressed by using the electron spin of photo-excited triplet states for DNP. After DNP the light creating the electron spins can be shut off, thus eliminating the main source of decay of the nuclear polarization. Moreover, for some well-chosen molecules the photo-excitation process creates the triplet state in a highly polarized state, so magnets and cryogenics can be significantly simplified.</p><p>The present article presents the state of the art of producing a high proton polarization – up to 0.80 – with a long lifetime – typically 50 h at liquid nitrogen temperature and in a field of 0.75 T – using the photo-excited triplet state of pentacene in a naphthalene host. It describes sample preparation, experimental equipment and procedures required to obtain this result, as well the theoretical background required to maximize the polarization transfer from the triplet spins to the proton spins and to optimize the photo-excitation process. It finishes with methods for long-distance transport and final application of polarized samples.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"20 ","pages":"Article 100159"},"PeriodicalIF":2.624,"publicationDate":"2024-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000141/pdfft?md5=002d182c52f0ebba51698515177991e9&pid=1-s2.0-S2666441024000141-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142041289","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Understanding magnetic fields, for NMR/MRI","authors":"Mark S. Conradi","doi":"10.1016/j.jmro.2024.100158","DOIUrl":"10.1016/j.jmro.2024.100158","url":null,"abstract":"<div><p>The basic physics of magnetic fields is presented for a target audience of NMR workers. This group often does not have formal training in electromagnetism, but could benefit from an understanding of a <em>selected subset</em> of topics. The focus here is on a relatively non-mathematical view, intended to deliver an intuitive understanding of the topic. The covered topics start with the fields arising from simple idealized currents, including long straight wires, short flat coils, infinite current sheets, long solenoids, and magnetic dipole moments. The generation of field gradients and shim fields is discussed. All of these can be unified by considering the divergence and curl of the magnetic field. Magnetic materials are treated, both linear magnetizable materials (including the sample itself) and permanently magnetized materials; the approaches of equivalent currents and Ampere's theorem for magnetic circuits are presented.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"20 ","pages":"Article 100158"},"PeriodicalIF":2.624,"publicationDate":"2024-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S266644102400013X/pdfft?md5=5ee9eaa54dcb6dba86c4de3a544c31db&pid=1-s2.0-S266644102400013X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141945612","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Fast quantitative MRI: Spiral Acquisition Matching-Based Algorithm (SAMBA) for Robust T1 and T2 Mapping","authors":"Mireia Perera-Gonzalez ,&nbsp;Christina J. MacAskill ,&nbsp;Heather A. Clark ,&nbsp;Chris A. Flask","doi":"10.1016/j.jmro.2024.100157","DOIUrl":"10.1016/j.jmro.2024.100157","url":null,"abstract":"<div><p>Conventional diagnostic images from Magnetic Resonance Imaging (MRI) are typically qualitative and require subjective interpretation. Alternatively, quantitative MRI (qMRI) methods have become more prevalent in recent years with multiple clinical and preclinical imaging applications. Quantitative MRI studies on preclinical MRI scanners are being used to objectively assess tissues and pathologies in animal models and to evaluate new molecular MRI contrast agents. Low-field preclinical MRI scanners (<span><math><mo>≤</mo></math></span>3.0T) are particularly important in terms of evaluating these new MRI contrast agents at human MRI field strengths. Unfortunately, these low-field preclinical qMRI methods are challenged by long acquisition times, intrinsically low MRI signal levels, and susceptibility to motion artifacts. In this study, we present a new rapid qMRI method for a preclinical 3.0T MRI scanner that combines a Spiral Acquisition with a Matching-Based Algorithm (SAMBA) to rapidly and quantitatively evaluate MRI contrast agents. In this initial development, we compared SAMBA with gold-standard Spin Echo MRI methods using Least Squares Fitting (SELSF) in vitro phantoms and demonstrated shorter scan times without compromising measurement accuracy or repeatability. These initial results will pave the way for future in vivo qMRI studies using state-of-the-art chemical probes.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"20 ","pages":"Article 100157"},"PeriodicalIF":2.624,"publicationDate":"2024-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000128/pdfft?md5=6a04edfdeeca12220ce76d49dd902c23&pid=1-s2.0-S2666441024000128-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141963223","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Automated hyperpolarized 129Xe gas generator for nuclear magnetic resonance spectroscopy and imaging applications","authors":"Mineyuki Hattori ,&nbsp;Takashi Hiraga ,&nbsp;Kazuhiro Homma ,&nbsp;Norio Ohtake","doi":"10.1016/j.jmro.2024.100154","DOIUrl":"https://doi.org/10.1016/j.jmro.2024.100154","url":null,"abstract":"<div><p>We describe a method and an apparatus for producing hyperpolarized (HP) Xe gas of high concentration without Xe condensation. The HP Xe generator works under atmospheric pressure and employs a quasi-continuous method to provide a continuous supply of HP Xe gas by adopting technologies for supplying a highly pure gas, a gas control system and precise pressure control. The apparatus has a glass cell containing solid Rb metal and solid Xe in vacuum at a low temperature and is heated so that the Xe becomes a gas and Rb exists in a gas-liquid mixture. Then a magnetic field is applied with laser beam irradiation to produce polarized Xe gas of high concentration. The device was evaluated using a 2T magnetic resonance imaging (MRI) scanner. Long-term experimental operation demonstrated the continuous collection of 30 ml syringes of HP Xe gas with a sufficient polarization rate for fast one scan acquisition. A practical device for the automated manufacture of HP ¹²⁹Xe gas was thus successfully developed.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"20 ","pages":"Article 100154"},"PeriodicalIF":2.624,"publicationDate":"2024-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000098/pdfft?md5=b9d93058d60dbb47913e59da366288d6&pid=1-s2.0-S2666441024000098-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141583180","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A comprehensive solid-state NMR and theoretical modeling study to reveal the structural evolution of layered yttrium hydroxide upon calcination","authors":"Yanxin Liu ,&nbsp;Xinyue Sheng ,&nbsp;Hui Ding,&nbsp;Jun Xu","doi":"10.1016/j.jmro.2024.100155","DOIUrl":"https://doi.org/10.1016/j.jmro.2024.100155","url":null,"abstract":"<div><p>Layered rare earth hydroxides (LREHs) are a new family of ion-exchangeable layered metal hydroxides, which have extensive applications in various fields due to the unique properties of rare earth cations in the layered structure and the anion exchange capacity. The transformation of layered metal hydroxides to new layered phases that can be restored through the memory effect is critical for their chemistry and applications. However, the structure details of these new phases such as the coordination environments of rare earth cations/counterions and their evolution as a function of calcination temperature remain unclear to date. Herein, a comprehensive ⁸⁹Y/³⁵Cl solid-state NMR (ssNMR) and theoretical modeling approach was used to reveal the structural evolution of a representative LREH, namely LYH-Cl, upon calcination. We first identified partial decomposition products of Y₃O(OH)₅Cl₂ and Y(OH)₃ during the dehydration stage, then uncovered the preferential removal of hydroxide ions on yttrium sites coordinated with chlorine during the dehydroxylation stage, and finally determined the preferential removal of chlorine exposed to the surface of layers during the dechlorination stage. The coordination environments of Y³⁺ and Cl⁻ undergo significant changes upon calcination, revealed by ssNMR experiments. These findings thus help us to overcome the obstacles impeding the rational design and synthesis of LREH-based functional materials via memory effect, underscoring the vast potential of ssNMR in deepening the understanding of layered metal hydroxides and related materials.</p></div>","PeriodicalId":365,"journal":{"name":"Journal of Magnetic Resonance Open","volume":"20 ","pages":"Article 100155"},"PeriodicalIF":2.624,"publicationDate":"2024-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666441024000104/pdfft?md5=287c5bd3157fdc6d9649443e59ae270a&pid=1-s2.0-S2666441024000104-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141303279","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}