Abstract:
This dataset contains vertically offset XRD patterns at 22 degrees C of neat HS-n-OH and their isostearyl alcohol gels, log-log plot of SANS intensity versus Q profile, log-log frequency and strain sweeps, and storage (G') and loss (G") moduli values versus time of various strains and frequencies. Also included are polarized optical microscopy images at 25 degrees C of 2 wt% HS-2-OH in isostearyl alcohol solution at different times after being fast-cooled.
Suggested Citation:
Richard Weiss. 2016. Dataset for: Structural bases for mechano-responsive properties in molecular gels of (R)-12-hydroxy-N-(ω-hydroxyalkyl)octadecanamides. Rates of formation and responses to destructive strain.. Distributed by: GRIIDC, Harte Research Institute, Texas A&M University–Corpus Christi. doi:10.7266/N7ZW1HXR
Data Parameters and Units:
PNG Image files: Image 1. AFM image of a 2 wt% HS-2-OH in silicone oil gel Image 2. Polarized optical microscopy OM images at 25 1C of a 2 wt% HS-2-OH in isostearyl alcohol sol at different times after being fast-cooled from 110 to 25 0 C (at approximately 20 0C/min): Image taken at 0 min; The images were taken with a full-wave plate Image 3. Polarized optical microscopy OM images at 25 1C of a 2 wt% HS-2-OH in isostearyl alcohol sol at different times after being fast-cooled from 110 to 25 0 C (at approximately 20 0C/min): Image taken at 7 min. The images were taken with a full-wave plate Image 4. Polarized optical microscopy OM images at 25 1C of a 2 wt% HS-2-OH in isostearyl alcohol sol at different times after being fast-cooled from 110 to 25 0 C (at approximately 20 0C/min): Image taken at 15 mins. The images were taken with a full-wave plate Image 5. Polarized optical microscopy OM images at 25 1C of a 2 wt% HS-2-OH in isostearyl alcohol sol at different times after being fast-cooled from 110 to 25 0 C (at approximately 20 0C/min): Image taken at 110 mins. The images were taken with a full-wave plate Spreadsheet of data.xml: Figure 2A: Vertically offset XRD patterns at 22 oC of neat HS-2-OH (crystallized from ethyl acetate) and 4.8 wt% HS-2-OH isostearyl alcohol gel. Figure 2B: Vertically offset XRD patterns at 22 oC of neat HS-3-OH (crystallized from ethyl acetate) and 5.1 wt% HS-3-OH isostearyl alcohol gel. Figure 2C: Vertically offset XRD patterns at 22 oC of neat HS-4-OH (crystallized from ethyl acetate) and 5.0 wt% HS-4-OH isostearyl alcohol gel. Figure 2D: Vertically offset XRD patterns at 22 oC of neat HS-4-OH (crystallized from ethyl acetate) and 5.3 wt% HS-5-OH isostearyl alcohol gel. Figure 3: Log–log plot of SANS intensity (I) versus Q profile of a fast-cooled 2 wt% HS-2-OH in toluene-d8 gel. Figure 6: G’ and G” at 25 oC as a function of time and application of different strains and frequencies to a fast-cooled 2.0 wt% HS-3-OH in isostearyl alcohol gel. Linear viscoelastic region (LVR): = 0.05%, ω= 100 rad s-1 Destructive strain (DS): = 30%, ω = 1 rad s-1, rotational strain was kept at 0% for 0.05 s before changing from DS to LVR conditions. Figure S13: Log-log strain sweep (1.0 rad/sec) at 25 oC for a fast-cooled 2.0 wt % HS-2-OH in isostearyl alcohol gel: G’, black squares; G’’, red circles. Figure S14: Log-log frequency sweep (0.05 % strain) at 25 oC for a fast-cooled 2 wt % HS-2-OH in isostearyl alcohol gel. Figure S15: Log-log strain sweep (1.0 rad/sec) at 25 oC for a 2.0 wt % fast-cooled HS-3-OH in isostearyl alcohol gel. Figure S16: Log-log frequency sweep (0.05 % strain) at 25 oC for a fast-cooled 2.0 wt % HS-3- OH in isostearyl alcohol gel. Figure S17: Log-log strain sweep (1.0 rad/sec) at 25 oC for a 2.0 wt % fast-cooled HS-4-OH in isostearyl alcohol gel. Figure S18: Log-log frequency sweep (0.05 % strain) at 25 oC for a 2 wt % fast-cooled HS-4-OH in isostearyl alcohol gel. Figure S19A: Log-log strain sweep (1.0 rad/sec) at 25 oC for a 2.0 wt % fast-cooled HS-5-OH in isostearyl alcohol gel. Figure S19B: Log-log frequency sweep (0.05 % strain) at 25 oC for a 2 wt % fast-cooled HS-5-OH in isostearyl alcohol gel. Figure S20: Log-log frequency sweep (0.05 % strain) at 25 oC for a 2 wt % S-3-OH in isostearyl alcohol gel. Figure S28: Plots of G’ and G” versus time for a 2 wt % HS-2-OH in isostearyl alcohol gel sample starting immediately upon reaching 25 oC after its sol was cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency. Figure S29: Plots of G’ and G” versus time for a 2 wt % HS-3-OH in isostearyl alcohol gel sample starting immediately upon reaching 25 oC after its sol was cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency. Figure S30: Plots of G’ and G” versus time for a 2 wt % HS-4-OH in isostearyl alcohol gel sample starting immediately upon reaching 25 oC after its sol was cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency Figure S31: Plots of G’ and G” versus time for a 2 wt % HS-5-OH in isostearyl alcohol gel sample starting immediately upon reaching 25 oC after its sol was cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency. Figure S32A: Plots of G’ and G” versus time for gels consisting of 2 wt % S-3- OH in isostearyl alcohol gel. Measurements commenced immediately upon reaching 25 oC after the sols were cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency. Figure S32B: Plots of G’ and G” versus time for gels consisting of 2 wt % HS-3 in isostearyl alcohol gel. Measurements commenced immediately upon reaching 25 oC after the sols were cooled from 110 oC over ca. 5 min; 0.05 % strain and 1 rad/sec angular frequency. Figure S42A: G' and G" versus time for gels consisting of 2 wt% HS-2-OH in toluene gel. Linear viscoelastic region: 0.03 % strain and 100 rad/sec angular freqency. Destructive strain: 50 % strain and 1 rad/sec angular frequency. Figure S42B: G' and G" versus time for gels consisting of 2 wt% HS-2-OH in silicone oil gel. Linear viscoelastic region: 0.1 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 rad/sec angular freqency. Figure S47: G' and G" versus time for gels consisting of 2 wt% HS-2-OH in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 rad/sec angular frequency. Figure S48: G' and G" versus time for gels consisting of 2 wt% HS-2-OH in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Figure S50: G' and G" versus time for gels consisting of 2 wt% HS-4-OH in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 rad/sec angular frequency. Figure S51: G' and G" versus time for gels consisting of 2 wt% HS-5-OH in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 rad/sec angular frequency. Figure S54: G' and G" versus time for gels consisting of 2 wt% 12-hydroxy-N-propyloctadecanamide/isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 /rad/sec angular frequency. Figure S55: G' and G" versus time for gels consisting of 2 wt% 12-hydroxy-N-propyloctadecanamide in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 /rad/sec angular frequency. Figure S57: G' and G" versus time for gels consisting of 2 wt% S-3-OH in isostearyl alcohol gel. Linear viscoelastic region: 0.05 % strain and 100 rad/sec angular frequency. Destructive strain: 30 % strain and 1 rad/sec angular frequency. Figure S58: Log-log plot of time versus Avrami parameter K and destructive strain for 2 wt % isostearyl alcohol gels of HS-n-OH, S-3-OH, and HS-3.
Instruments:
1. Atomic force microscopy (AFM) imaging was accomplished on a Bruker Bio Scope Catalyst microscope with peak force tapping using a Scan Asyst-Air probe (k B 0.4 N m_1 and tip radius o10 nm) or NTEGRA Prima scanning probe microscope (NT-MDT) mounted on an inverted Nikon Eclipse Ti–S fluorescence microscope with peak force tapping using a probe (NSG 10, k = 3.7–37.6 N/m, tip radius= B10 nm). 2. Optical microscopy The gel samples were prepared on glass micro slides (Corning 75x25x1 mm) using the fast-cooling protocol. Images were analyzed using Research Nanoscope 8.15 or Image Analysis 3.50.2090 NTMDT software. 3. 1H NMR spectra were recorded on a Varian 300 MHz spectrometer and chemical shifts were referenced to an internal standard, tetramethylsilane (TMS). 4. Elemental analyses were performed on a Perkin-Elmer 2400 CHN elemental analyzer using acetanilide as a calibration standard. 5. Melting points and polarized optical micrographs (POMs) were recorded on a Leitz 585 SM-LUX-POL microscope equipped with crossed polars, a Leitz 350 heating stage, a Photometrics CCD camera interfaced to a computer, and an Omega HH503 microprocessor thermometer connected to a J-K-T thermocouple. The samples for POM analyses were flamesealed in 0.4 or 0.5 mm path-length, flattened Pyrex capillary tubes (VitroCom, Inc.), heated to their liquid phase in a boiling water bath, and cooled according to protocols described below. 6. Powder X-ray diffraction (XRD) patterns of samples were obtained on a Rigaku R-AXIS image plate system with Cu K X-rays ( = 1.54 Å) generated by a Rigaku generator operating at 46 kV and 40 mA with the collimator at 0.5 mm.1 Data processing and analyses were performed using Materials Data JADE (version 5.0.35) XRD pattern processing software. Samples were sealed in 0.5 mm glass capillaries (W. Müller, Schönwalde, Germany) and diffraction data were collected for 2 h (neat powders) or 10 h (gels). 7. Differential scanning calorimetry (DSC) were performed on a TA 2910 differential scanning calorimeter interfaced to a TA Thermal Analyst 3100 controller under a slow stream of nitrogen flowing through the cell. 8. Small-angle neutron scattering (SANS) experiments, using neutrons of wavelength = 6 Å, were conducted at the Center for Neutron Research at the National Institute of Standards and Technology (NIST, Gaithersburg, MD, USA) using the NG7 30 m instrument2 over a set of 3 detector distances (13, 6, and 1 m), providing an overlap between the 3 configurations and, at the end, a range of scattering vectors Q from 0.004 to 0.45 Å-1.Radial averaging of the isotropic 2D arrays was performed using the NIST software package. 9. Rheological measurements were obtained at 25 oC on an Anton Paar Physica MCR 301 strain-controlled rheometer using a Peltier temperature-controller and parallel plates (25 mm diameter). The gap between the plates was 0.5 mm and the data were collected using Rheoplus/32 Service V3.10 software. Before recording data, each sample was placed between the plates of the rheometer and heated to 110 oC to ensure that a solution/sol was present. It was cooled to 10 oC (~20 oC/min) and the temperature was increased to 25 oC and incubated there for 15 min to reform the gel and remove any shearinduced alignment of the fibers.
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