NMR Dataset from "NMR relaxometry probes solvent-polarity-dependent molecular interactions in stimuli-responsive lyogels" DOI of this dataset: 10.15480/882.15898 README file creation date: 16 September 2025 1. General information: * Measurement of lyogel with varying solvent polarity and crosslinker concentration employing MR techniques * Investigation of how solvent polarity and crosslinking degree influence lyogel swelling and the resulting changes in molecular structure * A combination of standard gel characterization techniques with NMR relaxometry and diffusometry to elucidate solvent-polymer interactions at equilibrium * Data was collected on the dates indicated by the folder naming * Data was collected at Hamburg University of Technology * Muhammad Adrian (muhammad.adrian@tuhh.de, ORCID 0009-0008-3634-9518, Affiliation: a) Institute of Process Imaging, Hamburg University of Technology, Hamburg, Germany, *Corresponding author), Kathrin Marina Eckert, (kathrin.eckert@tuhh.de ORCID 0000-0002-8454-4886, Affiliation: b) Institute of Thermal Separation Processes, Hamburg University of Technology, Hamburg, Germany, g)United Nations University Hub on Engineering to Face Climate Change at the Hamburg University of Technology, United Nations University Institute of Water, Environment and Health, Hamburg, Germany,), M. Raquel Serial, (m.r.serial@tudelft.nl, ORCID 0000-0003-3052-4916, Affiliation: a) Institute of Process Imaging, Hamburg University of Technology, Hamburg, Germany, c) Department of Process and Energy, Delft University of Technology, Delft, The Netherlands), Artyom Tsanda, (artyom.tsanda@tuhh.de, ORCID 0009-0009-7765-4604, Affiliation: d) Institute for Biomedical Imaging, Hamburg University of Technology, Hamburg, Germany, e) Section for Biomedical Imaging, University Medical Center Hamburg-Eppendorf, Hamburg, Germany,), Lukas Rennpferdt, (lukas.rennpferdt@tuhh.de, ORCID 0000-0003-2938-694X, Affiliation: f) Institute of Microsystems Technology , Hamburg University of Technology, Hamburg, Germany,), Stefan Benders (stefan.benders@tuhh.de, ORCID 0000-0002-9823-1928, Affiliation: a) Institute of Process Imaging, Hamburg University of Technology, Hamburg, Germany,g)United Nations University Hub on Engineering to Face Climate Change at the Hamburg University of Technology, United Nations University Institute of Water, Environment and Health, Hamburg, Germany,), Hoc Khiem Trieu, (trieu@tuhh.de, ORCID 0000-0002-6102-4132, Affiliation: f) Institute of Microsystems Technology , Hamburg University of Technology, Hamburg, Germany,), Tobias Knopp, (tobias.knopp@tuhh.de, ORCID 0000-0002-1589-8517, Affiliation: d) Institute for Biomedical Imaging, Hamburg University of Technology, Hamburg, Germany, e) Section for Biomedical Imaging, University Medical Center Hamburg-Eppendorf, Hamburg, Germany,), Irina Smirnova,(irina.smirnova@tuhh.de, ORCID 0000-0003-4503-4039, Affiliation: b) Institute of Thermal Separation Processes, Hamburg University of Technology, Hamburg, Germany, g)United Nations University Hub on Engineering to Face Climate Change at the Hamburg University of Technology, United Nations University Institute of Water, Environment and Health, Hamburg, Germany,), Alexander Penn (alexander.penn@tuhh.de, ORCID 0000-0001-5596-6310, a) Institute of Process Imaging, Hamburg University of Technology, Hamburg, Germany, g)United Nations University Hub on Engineering to Face Climate Change at the Hamburg University of Technology, United Nations University Institute of Water, Environment and Health, Hamburg, Germany,) 2. Data overview: * The dataset includes the raw data of the Spinsolve measurements, available in .csv, .1d and .2d files, also including the parameters in .par, sorted in folders * These data can be processed with the script provided in https://collaborating.tuhh.de/v-10/public/manuscripts/lyogel-relaxometry * Processed data can be retrieved by executing the scripts * Folder structure: The dataset is organized into folders named lyogel_EtOH and lyogel_BuAc, corresponding to lyogel dispersed in EtOH and BuAc. Within each replicate folder, measurement files are arranged chronologically by date and time. Each file is labeled with the measurement type (Proton, T2Bulk, T1IRT2 or PGSTE) and the solvent (EtOH/BuAc), the measurement batch (batch number .1, or .2 or .3), the corresponding crosslinker concentration (1.) with: 1. correspond to 0.007 g/g crosslinker concentration 2. correspond to 0.014 g/g crosslinker concentration 3. correspond to 0.020 g/g crosslinker concentration 4. correspond to 0.035 g/g crosslinker concentration 5. correspond to 0.050 g/g crosslinker concentration Further details on list of chemical used and additional raw data mass are available in Supplementary Information. 3. Variable definitions: n/a 4. Data Collection Methods: The data was generated by measuring with a Spinsolve 60 at the IPI at Hamburg University of Technology. * Lyogel synthesis: Lyogels were synthesized by dissolving 2.175 g of NIPAM with N,N′-methylenebisacrylamide (MBA) in 23 g of deionized water, followed by nitrogen degassing for 30 min. The initiators, sodium metabisulfite (SMBS, 2.5 mg) and ammonium persulfate (APS, 2.5 mg), were each dissolved in 1 mL of deionized water and subsequently added to the mixture. Lyogels with varying crosslinker concentrations (0.007– 0.050 g crosslinker per g monomer) were prepared using MBA as the crosslinker. The resulting lyogel monoliths were cast in 10 mL syringes sealed with parafilm. After polymerization, the gels were cut into 1.5 cm cylinders and thoroughly washed with deionized water for three days. Lyogel synthesis was performed via a two-step solvent exchange protocol designed to probe the influence of solvent polarity. Ethanol (EtOH) was selected as a representative high-polarity solvent, while butyl acetate (BuAc) represented a low-polarity solvent. For EtOH-based lyogels, samples underwent three successive solvent exchanges followed by equilibration for 48 h at 25◦C. In the case of BuAc-based lyogels, an additional solvent exchange step was introduced to transition from EtOH to BuAc. 5. File formats used: * Files are located in experiment folders, named after year-month-day-samplename. * Files have .csv, .1d .2d (binary) and .par endings * Pulse sequences are embedded in the folders by ppcode 6. Dependencies and Tools: Dependencies are given in the Gitlab repository, where python libraries including versions are declared. 7. Limitations and known issues * Acquisition & Control: scripts depend on Spinsolve software running with Expert modules. * Format Issues: might be encountered and folders/naming vary between versions. * Processing Differences: smoothing-Python results will differ unless replicated. 8. Usage Rights and Citation: The data is published under CC BY-NC-ND 4.0 license. The dataset can be cited by the DOI provided by TORE. By using the data in your work, you agree to cite the original work.