Solid-state NMR pulse sequences often feature fewer pulses and delays than the more common solution NMR experiments. This ostensible simplicity, however, belies the care with which experimental parameters must be determined, as solid-state NMR can be much less forgiving of improper experimental set-up. This is especially true of "semi-solid" samples, such as the phospholipid vesicles used to study membrane-associated peptides and proteins, which feature prominently in misfolding diseases. Protocols for the preparation of multilamellar vesicles for solid-state NMR studies of Aβ peptides are described, together with procedures for optimization of critical experimental parameters, such as spectral widths, delay times, and field strengths for (31)P, (2)H, and (13)C NMR spectroscopy.
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http://dx.doi.org/10.1007/978-1-60327-223-0_11 | DOI Listing |
Sci Rep
January 2025
Nonprofitable Organization Touche NPO, Sapporo, 060-004, Japan.
In this study, we explore the structural intricacies of cellulose, a polymer composed of glucose monomers arranged in a linear chain, primarily investigated through solid-state NMR techniques. Specifically, we employ low-field proton nuclear magnetic resonance (H-NMR) to delve into the diverse hydrogen atom types within the cellulose molecule. The low-field H-NMR technique allows us to discern these hydrogen atoms based on their distinct chemical shifts, providing valuable insights into the various functional groups present in cellulose.
View Article and Find Full Text PDFPhys Chem Chem Phys
January 2025
Institute for Frontier Materials, Deakin University, Geelong, Victoria 3216, Australia.
In this work, we investigate the development of polymer electrolytes for sodium batteries based on sulfonamide functional polymer nanoparticles (NaNPs). The synthesis of the polymer NaNPs is carried out by emulsion copolymerization of methyl methacrylate and sodium sulfonamide methacrylate in the presence of a crosslinker, resulting in particle sizes of 50 nm, as shown by electron microscopy. Then, gel polymer electrolytes are prepared by mixing polymer NPs and different organic plasticizers including carbonates, glymes, sulfolanes and ionic liquids.
View Article and Find Full Text PDFJ Colloid Interface Sci
January 2025
School of Chemistry and Chemical Engineering, Zhejiang Sci-Tech University, 928 Second Street, Hangzhou 310018 China; Zhejiang Sci-Tech University Shengzhou Innovation Research Institute, Shengzhou 312400, China. Electronic address:
To boost supercapacitor (SC) energy density, we introduced redox-active molecules into an aqueous HSO electrolyte. Using retrosynthetic analysis, we identified aminoquinones, specifically triaminochlorobenzoquinone (TACBQ), as promising candidates. Characterization via elemental analysis, Fourier Transform Infrared Spectrometer (FT-IR), nuclear magnetic resonance (NMR), and X-ray photoelectron spectroscopy (XPS) confirmed structure of TACBQ.
View Article and Find Full Text PDFChem Asian J
January 2025
Qingdao University of Science and Technology, College of Polymer Science and Engineering, 53 ZHENGZHOU ROAD, 266000, Qingdao, CHINA.
Constructing highly conjugated three-dimensional covalent organic frameworks (3D COFs), particularly those with luminescent features, remains a significant challenge. In this work, we successfully synthesized a 3D COF, named 3D-Py-SP-COF, using a rigid and orthogonal spirobifluorene building block for the spatial 3D structure construction and planar pyrene as luminescent units. The incorporation of the pyrene and the unique rigid 3D network structure endow 3D-Py-SP-COF with fluorescent properties.
View Article and Find Full Text PDFJ Am Chem Soc
January 2025
Department of Biochemistry, University of Wisconsin-Madison, Madison, Wisconsin 53706, United States.
NMR spectroscopy presents boundless opportunities for understanding the structure, dynamics, and function for a broad range of scientific applications. Solid-state NMR (SSNMR), in particular, provides novel insights into biological and material systems that are not amenable to other approaches. However, a major bottleneck is the extent of user training and the difficulty of obtaining reproducible, high-quality experimental results, especially for the sophisticated multidimensional pulse sequences that are essential to provide site-resolved measurements in large biomolecules.
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