This readme.txt file was generated on 20220602 by Lucy Liberman ------------------- GENERAL INFORMATION ------------------- Recommended citation for the data: Liberman, Lucy; Schmidt, Peter W; Coughlin, McKenzie L; Matatyaho Ya'akobi, Asia; Davidovich, Irina; Edmund, Jerrick; Ertem, Sedef P; Morozova, Svetlana; Talmon, Yeshayahu; Bates, Frank S; Lodge, Timothy P. (2022). Supporting Data for Salt-Dependent Structure in Methylcellulose Fibrillar Gels. Retrieved from the Data Repository for the University of Minnesota, https://doi.org/10.13020/dc5t-te76. 1. Title of Dataset: Supporting Data for “Salt-Dependent Structure in Methylcellulose Fibrillar Gels” 2. Author Information Group Author: Material Research Science and Engineering Center (MRESC) Principal Investigator Contact Information Name: Timothy P. Lodge Institution: Department of Chemistry and Chemical Engineering & Materials Science, University of Minnesota Address: 235 Smith Hall, 207 Pleasant Street SE, Minneapolis, MN 55455 Email: lodge@umn.edu ORCID: http://orcid.org/0000-0001-5916-8834 Associate or Co-investigator Contact Information Name: Frank S. Bates Institution: Department of Chemical Engineering and Materials Science, University of Minnesota Address: 358 Amundson Hall, 421 Washington Ave SE, Minneapolis, MN 55455 Email: bates001@umn.edu ORCID: http://orcid.org/0000-0003-3977-1278 3. Date of data collection: 20180910-20200829 4. Geographic locations of data collection: The X-ray scattering experiments and data collection were performed at DuPont-Northwestern-Dow Collaborative Access Team (DND-CAT) 5-ID at the Advanced Photon Source, Argonne National Laboratory in Lemont, IL, USA. The phase plate cryogenic transmission electron microscopy experiments and data collection were performed at the Technion-Israel Institute of Technology in Haifa, Israel. All other experiments and data collection were conducted at the University of Minnesota, Minneapolis, MN, USA. 5. Information about funding sources that supported the collection of the data: The collection of this data was supported primarily by the National Science Foundation through University of Minnesota MRSEC under award number DMR-1420013. -------------------------- SHARING/ACCESS INFORMATION -------------------------- 1. Licenses/restrictions placed on the data: CC0 1.0 Universal 2. Links to publications that cite or use the data: "Salt-Dependent Structure in Methylcellulose Fibrillar Gels”, L. Liberman P. W. Schmidt, M. L. Coughlin, A. Mayatyaho Ya’akobi, I. Davidovich, J. Edmund, S. P. Ertem, S. Morozova, Y. Talmon, F. S. Bates, T. P. Lodge, Macromolecules 2022, 54, 2090-2100. https://pubs.acs.org/doi/abs/10.1021/acs.macromol.0c02429 3. Links to other publicly accessible locations of the data: Not applicable. 4. Links/relationships to ancillary data sets: Not applicable. 5. Was data derived from another source? No If yes, list source(s): --------------------- DATA & FILE OVERVIEW --------------------- 1. File List General Notes: Data files are grouped by manuscript and supplementary information figure number. 1. Filename: 020720_MC300_1%_NoSalt_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 without salt. Data was used to generate the No Salt data points in Figure 1. 1a_1. Filename: MC300_1%_NaCl_2%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% NaCl. Data was used to generate the 2 wt% data points in Figure 1a. 1a_2. Filename: MC300_1%_NaCl_4%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% NaCl. Data was used to generate the 4 wt% data points in Figure 1a. 1a_3. Filename: MC300_1%_NaCl_6%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% NaCl. Data was used to generate the 6 wt% data points in Figure 1a. 1a_4. Filename: MC300_1%_NaCl_8%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 8 wt% NaCl. Data was used to generate the 8 wt% data points in Figure 1a. 1b_1. Filename: MC300_1%_NaI_2%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% NaI. Data was used to generate the 2 wt% data points in Figure 1b. 1b_2. Filename: MC300_1%_NaI_4%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% NaI. Data was used to generate the 4 wt% data points in Figure 1b. 1b_3. Filename: MC300_1%_NaI_6%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% NaI. Data was used to generate the 6 wt% data points in Figure 1b. 1b_4. Filename: MC300_1%_NaI_8%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 8 wt% NaI. Data was used to generate the 8 wt% data points in Figure 1b. 1c_1. Filename: 02262020_MC300_1%_NH4Cl_2%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% NH4Cl. Data was used to generate the 2 wt% data points in Figure 1c. 1c_2. Filename: 07162020_MC300_1%_NH4Cl_4%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% NH4Cl. Data was used to generate the 4 wt% data points in Figure 1c. 1c_3. Filename: 07162020_MC300_1%_NH4Cl_6%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% NH4Cl. Data was used to generate the 6 wt% data points in Figure 1c. 1c_4. Filename: 07162020_MC300_1%_NH4Cl_8%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 8 wt% NH4Cl. Data was used to generate the 8 wt% data points in Figure 1c. 1d_1. Filename: 03122020_MC300_1%_CaCl2_2%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% CaCl2. Data was used to generate the 2 wt% data points in Figure 1d. 1d_2. Filename: 08032020_MC300_1%_CaCl2_4%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% CaCl2. Data was used to generate the 4 wt% data points in Figure 1d. 1d_3. Filename: 08032020_MC300_1%_CaCl2_6%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% CaCl2. Data was used to generate the 6 wt% data points in Figure 1d. 1d_4. Filename: 03122020_MC300_1%_CaCl2_8%_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 8 wt% CaCl2. Data was used to generate the 8 wt% data points in Figure 1d. 2. Filename: Tgel_Tcloud_NaCl_NaI_NH4Cl_CaCl2_NoSalt.xlsx Short description: Cloud point from transmittance and gelation point from SAOS rheology measurements as a function of salt molar concentration of 1 wt% MC300 without salt and with NaCl, NaI, NH4Cl, and CaCl2. Data was used to generate Figures 2a and 2b. 3a. Filename: MC300_1%_NoSalt_SAXS.xslx Short description: 1D SAXS data of 1 wt% MC300 gel without salt at 30, 40, 50, 60, 70, and 80C. Data was used for Figure 3a. 3b. Filename: MC300_1%_NaCl_8%_SAXS.xslx Short description: 1D SAXS data of 1 wt% MC300 gel with 8 wt% NaCl at 30, 40, 50, 60, 70, and 80C. Data was used for Figure 3b. 3c. Filename: MC300_1%_NaI_8%_SAXS.xslx Short description: 1D SAXS data of 1 wt% MC300 gel with 8 wt% NaI at 30, 40, 50, 60, 70, and 80C. Data was used for Figure 3c. 3d. Filename: MC300_1%_NH4Cl_8%_SAXS.xslx Short description: 1D SAXS data of 1 wt% MC300 gel with 8 wt% NH4Cl at 30, 40, 50, 60, 70, and 80C. Data was used for Figure 3d. 3e. Filename: MC300_1%_CaCl2_8%_SAXS.xslx Short description: 1D SAXS data of 1 wt% MC300 gel with 8 wt% CaCl2 at 30, 40, 50, 60, 70, and 80C. Data was used for Figure 3e. 4a. Filename: Conv_to_Fibrils_NaCl_NaI_NoSalt.xslx Short description: Data used to determine conversion into fibrils from G* (SAOS rheology) and from the average of the relative SAXS intensity over q SAXS without the addition of salt and with the addition of NaCl and NaI. Data was used for Figure 4a. 4b. Filename: Conv_to_Fibrils_NH4Cl_CaCl2_NoSalt.xslx Short description: Data used to determine conversion into fibrils from G* (SAOS rheology) and from the average of the relative SAXS intensity over q SAXS without the addition of salt and with the addition of NH4Cl and CaCl2. Data was used for Figure 4b. 5. Filename: FibrilDiameter_vs_SaltConc_80C_SAXSFitting.xslx Short description: Fibril diameter fitting data obtained from fitting the 1 wt% MC300 data obtained at 80C, used to determine the effect of the addition of salt on fibril diameter. Data was used for Figure 5. 6a. Filename: MC300_0.05%_NoSalt_60C_CryoTEM.xslx Short description: Raw cryo-TEM data of 0.05 wt% MC300 without salt vitrified at 60C after 30 min. Data was used for Figure 6a. 6b. Filename: MC300_0.05%_NaCl_8%_30C_CryoTEM.xslx Short description: Raw cryo-TEM data of 0.05 wt% MC300 with 8 wt% NaCl vitrified at 30C after 30 min. Data was used for Figure 6b. 6c. Filename: MC300_0.05%_NaI_8%_60C_CryoTEM.xslx Short description: Raw cryo-TEM data of 0.05 wt% MC300 with 8 wt% NaI vitrified at 60C after 30 min. Data was used for Figure 6c. 7. Filename: MC300_3%_Salts_8%_MAXS_WAXS_80C.xslx Short description: MAXS and WAXS data of 3 wt% MC300 without salt and with the addition of 8 wt% of NH4Cl, CaCl2, NaCl, and NaI. Data was used for Figure 7. 8. Filename: MC300_1%_salts_OsmoticStress_vs_CompressiveStrain.xslx Short description: Data used to determine the osmotic pressure as a function of compressive strain with the addition of salt. Data was used for Figure 8. S1. Filename: 020720_MC300_1%_NoSalt_Rheo.txt Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 without salt. Data was used to generate the No Salt data points in Figure S1. S1a_1. Filename: MC300_1%_LiCl_2%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% LiCl. Data was used to generate the 2 wt% data points in Figure S1a. S1a_2. Filename: MC300_1%_LiCl_4%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% LiCl. Data was used to generate the 4 wt% data points in Figure S1a. S1a_3. Filename: MC300_1%_LiCl_6%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% LiCl. Data was used to generate the 6 wt% data points in Figure S1a. S1a_4. Filename: MC300_1%_LiCl_8%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 8 wt% LiCl. Data was used to generate the 8 wt% data points in Figure S1a. S1b_1. Filename: MC300_1%_KCl_2%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 2 wt% KCl. Data was used to generate the 2 wt% data points in Figure S1b. S1b_2. Filename: MC300_1%_KCl_4%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 4 wt% KCl. Data was used to generate the 4 wt% data points in Figure S1b. S1b_3. Filename: MC300_1%_KCl_6%_Rheo.xlsx Short description: Raw rheological SAOS data upon heating and cooling of 1 wt% MC300 with 6 wt% KCl. Data was used to generate the 6 wt% data points in Figure S1b. S2. Filename: Tgel_Tcloud_LiCl_KCl_NoSalt.xlsx Short description: Cloud point from transmittance and gelation point from SAOS rheology measurements as a function of salt molar concentration of 1 wt% MC300 without salt and with LiCl and KCl. Data was used to generate Figures S2. S3a. ConvChains_to_Fibrils_SAXS_NoSalt.xlsx Short description: Data used to determine the conversion of free chains in solution into fibrils at temperatures ranging between 30-80C for 1 wt% MC300 without salt. Data was used to generate Figure S3a. S3b. ConvChains_to_Fibrils_SAXS_NaCl_8%.xlsx Short description: Data used to determine the conversion of free chains in solution into fibrils at temperatures ranging between 30-80C for 1 wt% MC300 with 8% NaCl. Data was used to generate Figure S3b. S3c. ConvChains_to_Fibrils_SAXS_NaI_8%.xlsx Short description: Data used to determine the conversion of free chains in solution into fibrils at temperatures ranging between 30-80C for 1 wt% MC300 with 8% NaI. Data was used to generate Figure S3c. S3d. ConvChains_to_Fibrils_SAXS_NH4Cl_8%.xlsx Short description: Data used to determine the conversion of free chains in solution into fibrils at temperatures ranging between 30-80C for 1 wt% MC300 with 8% NH4Cl. Data was used to generate Figure S3d. S3e. ConvChains_to_Fibrils_SAXS_CaCl2_8%.xlsx Short description: Data used to determine the conversion of free chains in solution into fibrils at temperatures ranging between 30-80C for 1 wt% MC300 with 8% CaCl2. Data was used to generate Figure S3e. S4a. RadiusDispersity_SAXSFittings.xlsx Short description: Data used to estimate fibril radius dispersity from fitting of the SAXS data obtained at 80C. Data was used to generate Figure S4a. S4b. Scale_vs_SaltConc_80C_SAXSFitting.xlsx Short description: Data used to estimate the scale parameter from fitting of the SAXS data obtained at 80C. Data was used to generate Figure S4b. S4c. KuhnLength_vs_SaltConc_80C_SAXSFitting.xlsx Short description: Data used to estimate the fibril Kuhn length from fitting of the SAXS data obtained at 80C. Data was used to generate Figure S4c. 2. Relationship between files: All files are used to generate the figures in the manuscript and supplementary information. Files are grouped by figure number. 3. Additional related data collected that was not included in the current data package: No additional data was collected that was not included in the current data package. 4. Are there multiple versions of the dataset? no -------------------------- METHODOLOGICAL INFORMATION -------------------------- 1. Description of methods used for collection/generation of data: A. Phase-Plate Cryo-TEM: Cryo-TEM specimens were prepared in a controlled environment vitrification system at 60 °C and 100% relative humidity (https://onlinelibrary.wiley.com/doi/abs/10.1002/jemt.1060100111). The specimens were blotted manually and plunged into liquid ethane at its freezing point. The cryo-specimens were loaded into a Gatan 626 cryo-holder and kept in an FEI Talos 200C high-resolution TEM equipped with a Schottky field-emission gun at −180 °C. The image contrast was enhanced by a Volta “phase-plate” that converts image phase differences into amplitude difference (https://www.jstage.jst.go.jp/article/biophysics/2/0/2_0_35/_article). Images were recorded at an acceleration voltage of 200 kV by an FEI Falcon III direct-imaging camera, using very low electron exposure, below 10 e−/Å2. B. Small-angle X-ray scattering (SAXS): Experiments were conducted at the DND-CAT, Sector 5-ID-D of the Advanced Photon Source at Argonne National Laboratory. Two-dimensional (2D) scattering patterns were collected during 1 s exposures to 0.0729 nm wavelength X-rays on a Rayonix MX170-HS CCD detector, at a sample-to- detector distance of 8.5 m. The detector readout was binned to 4 × 4 pixels to decrease the detector readout noise. The 2D SAXS data were integrated azimuthally yielding one-dimensional (1D) scattering patterns of intensity versus the scattering wave vector q. At the X-ray wavelength and detector distance used, the q range accessed was 2.35 × 10−3 to 0.137 Å−1. Samples were prepared by loading 1 wt% solutions into 1.5 mm diameter quartz capillaries, which were subsequently sealed with epoxy and placed into a custom-fabricated eight-capillary heating stage. Each set of eight samples was heated stepwise by 10 °C for 10 min to approximate a 1 °C/min temperature ramp. C. Mid- and wide-angle X-ray scattering (MAXS and WAXS): Experiments were conducted at the DND-CAT, Sector 5-ID-D of the Advanced Photon Source at Argonne National Laboratory. 0.001 in. thick films were secured in a nylon washer by Kapton tape and placed in the path of the beam. 2D data were collected with a 1 s exposure with a SAXS, MAXS, and WAXS detector simultaneously. The 2D data were integrated azimuthally yielding one-dimensional (1D) scattering patterns of intensity versus the scattering wave vector q. Rayonix LX170-HS CCD detectors were employed for the MAXS and WAXS measurements at sample-to-detector distances of 1.01 and 0.2 m, respectively, and were generally binned at 2 × 2 pixels. The q values accessed for these detectors were from q = 0.13 to 0.86 Å−1 for MAXS and 0.68−4.5 Å−1 for WAXS. D. SAOS Rheology: Small-amplitude oscillatory shear rheology (SAOS)measurements were conducted on a TA Instruments AR-G2 with the Couette geometry (inner cylinder diameter 14 mm, outer diameter 15 mm, immersed height 42 mm). Low-viscosity silicone oil was floated above the solution to prevent evaporation during testing. Temperature ramps were conducted at 1 °C/min, with a frequency of 1 rad/s and a constant strain amplitude of 5%. E. Optical turbidity: Cloud-point measurements were conducted with a home-built transmittance setup. A HeNe laser (λ = 633 nm) beam was passed through a sample contained in an ampoule. The intensity was measured using a photometer. The temperature was controlled by a heating block heated at a rate of 1 °C/min to locate the transition from a clear solution to turbid hydrogel. The gel point was assigned to the temperature at which the transmission dropped to 86% of the maximum transmittance. 2. Methods for processing the data: A. Cryo-TEM images were processed using Image-J software. B. 1D SAXS patterns were analyzed using IgorPro software. A power law background was subtracted from each sample to account (approximately) for water and quartz scattering. A form factor for a semiflexible cylinder with a disperse radius was used to fit the SAXS patterns. The scattering length density and scale terms (volume fraction of polymer, φ, multiplied by the fibril volume) were combined into a single fitting term, A_scale. C. All plots in the manuscript were made using OriginPro 8. 3. Instrument- or software-specific information needed to interpret the data: 4. Standards and calibration information, if appropriate: 5. Environmental/experimental conditions: 6. Describe any quality-assurance procedures performed on the data: 7. People involved with sample collection, processing, analysis and/or submission: Lucy Liberman, Peter W. Schmidt, McKenzie L. Coughlin, Asia Matatyaho Ya’akobi, Irina Davidovich, Jerrick Edmund, S. Piril Ertem, and Svetlana Morozova were all involved with sample collection, processing, analysis, and/or submission.