This file Data was updated on 2024-17-04 by Aristotelis Zografos Recommended citation for the data: Zografos, Aristotelis; Maines, Erin, M; Hassler, Joseph, F; Bates, Frank, S; Hillmyer, Marc, A. (2024). Supporting data for Preparation and characterization of H-shaped polylactide. Retrieved from the University Digital Conservancy, https://doi.org/10.13020/3xyj-va41 ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Supporting data for Preparation and characterization of H-shaped polylactide Author Information: Principal Investigator Contact Information Name: Aristotelis Zografos Institution: University of Minnesota Address: Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: zoga005@umn.edu ORCID: https://orcid.org/0000-0001-9612-091X Associate or Co-investigator Contact information Name: Erin M. Maines Institution: University of Minnesota Address: Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: maine030@umn.edu ORCID: https://orcid.org/0009-0002-8416-6333 Associate or Co-investigator Contact Information Name: Joseph F. Hassler Institution: University of Minnesota Address: Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: hassl025@umn.edu ORCID: https://orcid.org/0000-0003-0904-2314 Associate or Co-investigator Contact Information Name: Frank S. Bates Institution: University of Minnesota Address: Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: bates001@umn.edu ORCID: https://orcid.org/0000-0003-3977-1278 Associate or Co-investigator Contact Information Name: Marc A. Hillmyer Institution: University of Minnesota Address: Chemistry, 225 Pleasant St SE, Minneapolis, Minnesota 55455 Email: hillmyer@umn.edu ORCID: https://orcid.org/0000-0001-8255-3853 Date of data collection: November 2022 - August 2023 Geographic location of data collection: University of Minnesota Information about funding sources that supported the collection of the data: This research was supported by a grant from the National Science Foundation through the Center for Sustainable Polymers (grant CHE-1413862) and the Graduate Research Fellowship Program (DGE-1839286). 1H-NMR experiments were conducted at the University of Minnesota Nuclear Magnetic Resonance Laboratory using an instrument that is supported by the Director, National Institutes of Health (S10OD011952). The content of this work is solely the responsibility of the authors and does not necessarily represent the official views of the National Institutes of Health. -------------------------- SHARING/ACCESS INFORMATION -------------------------- 1. Licenses/restrictions placed on the data: CC0 1.0 Universal 2. Links to publications that cite or use the data: Zografos, A., Maines, E. M., Hassler, J. F., Bates, F. S., & Hillmyer, M. A. (2024). Preparation and Characterization of H-Shaped Polylactide. ACS Macro Letters, 13, 695-702. https://doi.org/10.1021/acsmacrolett.4c00217 3. Links to other publicly accessible locations of the data: None 4. Links/relationships to ancillary data sets: None 5. Was data derived from another source? No. --------------------- DATA & FILE OVERVIEW --------------------- Purpose Statement: This document describes all necessary information relevant to the dataset used in the publication, including supplementary data. General Notes: All data is categorized according to the corresponding manuscript figure. For example, the folder "Figure 1" contains all data used in Figure 1 of the manuscript. Files Contained: +---Figure1 | | Figure1C.txt | | | +---Figure1A_inset_PLAbb_8kDa_OH | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram1309 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1A_PLAbb_8kDa_prot-OH2 | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram31249 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_120m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_15m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_240m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_30m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_5m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_60m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_anhydride_110m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_anhydride_160m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_anhydride_240m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure1B_HNMR_anhydride_65m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram16742 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | \---Figure1B_HNMR_anhydride_80m | \---10 | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram16742 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---Figure2 | Figure2_MALDI_PLAbb_8kDa_OH.txt | Figure2_MALDI_PLAbb_8kDa_OH2.txt | Figure2_MALDI_PLAbb_8kDa_prot-OH2.txt | +---Figure3 | | Figure3A,B_SECData.csv | | Figure3C_SEC_Data.csv | | | +---Figure 3A_HNMR_0m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure 3A_HNMR_1hr | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure 3A_HNMR_1hr45m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure 3A_HNMR_1m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure 3A_HNMR_20m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---Figure 3A_HNMR_3hr | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | \---Figure 3A_HNMR_5m | \---10 | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram3734 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---Figure4 | Figures_4A,B,C,D_HPLA_120kDa.csv | Figures_4A,B,C,D_HPLA_34kDa.csv | Figures_4A,B,C,D_linearPLA.csv | +---FigureS10_SEC_Products3and4_8kDa | FigureS9_Macroinitiators.csv | +---FigureS11_SEC_Products3and4_25kDa | FigureS11_Macroinitiators.csv | +---FigureS13_DSC | FigureS13_DSC_HPLA_120kDa.txt | FigureS13_DSC_HPLA_34kDa.txt | FigureS13_DSC_LPLA.txt | +---FigureS1_Product1 | \---10 | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram1309 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---FigureS2,S4_protectedBisMPA | +---FigureS2_HNMR | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram23887 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | \---FigureS4_CNMR | | acqu | | acqus | | audita.txt | | cpdprg2 | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram23887 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---FigureS3,S4_Product2 | +---FigureS3_HNMR | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram23887 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | \---FigureS4_CNMR | | acqu | | acqus | | audita.txt | | cpdprg2 | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram23887 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---FigureS5_PLA_Product3_25kDa | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | pulseprogram | | scon2 | | shimvalues | | specpar | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | 1i | 1r | auditp.txt | integrals.txt | intrng | outd | proc | procs | thumb.png | title | +---FigureS7_DeprotectionKinetics_8kDa | +---FigureS7_HNMR_Deprotection_10equivH20_15m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_10equivH20_45m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_10equivH20_5m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_10equivH20_90m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram3734 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_1equivH20_1.5hr | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram31249 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_1equivH20_15m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram31249 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | +---FigureS7_HNMR_Deprotection_1equivH20_45m | | \---10 | | | acqu | | | acqus | | | audita.txt | | | fid | | | format.temp | | | fq1list | | | precom.output | | | prosol_History | | | pulseprogram | | | scon2 | | | shimvalues | | | specpar | | | stanprogram31249 | | | uxnmr.info | | | uxnmr.par | | | vtc_pid_settings | | | | | \---pdata | | \---1 | | outd | | proc | | procs | | title | | | \---FigureS7_HNMR_Deprotection_1equivH20__5m | \---10 | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram31249 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | +---FigureS8_Product4_8kDa | \---10 | | acqu | | acqus | | audita.txt | | fid | | format.temp | | fq1list | | precom.output | | prosol_History | | pulseprogram | | scon2 | | shimvalues | | specpar | | stanprogram3734 | | uxnmr.info | | uxnmr.par | | vtc_pid_settings | | | \---pdata | \---1 | outd | proc | procs | title | \---FigureS9_Product4_25kDa | acqu | acqus | audita.txt | fid | format.temp | fq1list | precom.output | pulseprogram | scon2 | shimvalues | specpar | uxnmr.info | uxnmr.par | vtc_pid_settings | \---pdata \---1 1i 1r auditp.txt integrals.txt intrng outd proc procs thumb.png title Additional related data collected that was not included in the current data package: None. Are there multiple versions of the dataset? No. -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection, generation, and processing of data: Proton nuclear magnetic resonance (1H-NMR) spectroscopy 1H-NMR spectroscopy measurements were made using either a Bruker Avance III HD 500 MHz spectrometer or a Bruker 900-MHz Avance III. The latter was used for analysis of polymers 3 and 4 (Scheme 1) with molar masses of 27 kg/mol. 13C-NMR data was collected using the Bruker Avance III HD 500 instrument. Data were collected at room temperature and chemical shifts were referenced to residual CHCl3 in CDCl3. Size exclusion chromatography (SEC) SEC experiments used either uninhibited tetrahydrofuran (THF-SEC) or dimethylformamide with 0.05 M LiBr (DMF-SEC) as eluents. Each analysis method used a flow rate of 1 mL/min. THF-SEC analysis was conducted using a Viscotek GPCMax VE 2001 instrument equipped with three Agilent Technologies PLgel 5μm Mixed-C 300 x 7.5 mm columns, connected in series with an eluent temperature of 22 °C. An in-line Viscotek VE 3580 refractometer was used to characterize the elution profile. The columns enabled better molar mass resolution, compared to those of the DMF-SEC instrument. DMF-SEC analysis was conducted using an Agilent 1200 pump/autosampler system with two Viscotek (Model I-MBMMW-3078) columns connected in series. Wyatt miniDAWN (MALS) and Wyatt Optilab T-rEX (dRI) detectors are both connected in-line with the columns. The columns are operated at 50 °C and the MALS and dRI detector flow cells are operated at 25 °C. The absolute weight average molar mass of each polymer was determined using this instrument. The analysis uses a pre-programed method for calculating the dn/dc via ASTRA software. This calculation assumes that the polymer concentration at the detector is equal to the injection concentration (i.e., 100% mass recovery assumed). Matrix assisted laser desorption/ionization (MALDI) spectroscopy MALDI measurements were performed on a Bruker Daltonics Autoflex Speed MALDI-TOF/TOF instrument operating in linear mode. The instrument was calibrated with a solution of protein standards prior to every experiment. All data were acquired with ~30% laser power, near the minimum intensity required to make the samples fly. Samples were made by preparing stock solutions of (trans-2-[3-(4-tert-butylphenyl)-2-methyl-2-propenylidene]malononitrile) (DCTB) (matrix), sodium iodide (counterion), and polymer, which were prepared in THF at concentrations of 150 mg/mL, 50 mg/mL, and 10 mg/mL, respectively. The stock solutions were then combined in a 3:1:1 matrix:counterion:sample (vol:vol:vol) and 1 μL was spotted onto the plate.3 Differential scanning calorimetry (DSC) Thermal measurements were made using a Mettler Toledo DSC 1 instrument, using a nitrogen gas environment and aluminum sample pans. All cooling and heating rates were at 10 °C/min. The sample was heated to 150 °C, held isothermally for 5 minutes, cooled to 25 °C, held isothermally for 2 minutes, and then heated to 200 °C. The reported data uses the second heating trace. Sample preparation for rheology A Wabash Genesis Series hydraulic press was used to create polymer films. To do this, the polymer was pressed between two Teflon-lined aluminum foil sheets at 500 lb-force for 1.5 minutes to allow the material to come to temperature, followed by 1000 lb-force for 1 minute. This was done at 85 < T < 150 °C, where T was selected based on the polymer viscosity. Metal shims were used to achieve a sample thickness of 0.5 mm. From the films, samples were cut for small amplitude oscillatory shear (SAOS) and extensional rheology. Care was made to limit defects in the films (e.g., air bubbles). Small-amplitude oscillatory shear rheology Rheology measurements used an ARES-G2 rheometer. SAOS was conducted using 8 mm parallel plates. The polymer was loaded onto the instrument and then trimmed to achieve a gap height of ~0.7 mm. Frequency sweeps used a strain that was within the bounds of linear viscoelasticity, which was selected based on strain amplitude sweeps. Frequency sweeps were conducted between 0.1 and 100 rad/second. Temperatures between Tg < T < 140 °C were probed to construct master curves for each melt. Data analysis was conducted using either TRIOS or IRIS Rheo-Hub software. Derivative curves of the tan(δ) data were smoothed using TRIOS software. Extensional rheology Extensional measurements were made using an extensional viscosity fixture. These were conducted at the temperatures specified in Figure 4D. From the polymer sheets mentioned above, 15mm x 10mm x 0.5 mm samples were created for this analysis. Hencky strain rates < 10 s-1 were probed, which is the upper limit of the instrument. Hencky strains < 4 were probed, which is the upper limit of the instrument. Note, the rheometer can go past this strain but doing so causes the sample to wrap onto itself, distorting the measurement. People involved with sample collection, processing, analysis and/or submission: Aristotelis Zografos collected or helped collect all data. Analyzed all data. Erin M. Maines collected rheology data for the 120 kg/mol H-polymer. Joseph F. Hassler developed method used to collect all MALDI data and helped with MALDI data analysis. Marc A. Hillmyer was involved in data analysis and interpretation. Frank S. Bates was involved in data analysis and interpretation.