Fourier-transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were utilized to check comonomer incorporation in the synthesized gels. Attenuated total reflectance (ATR)-FTIR spectra were collected with a Varian 7000e FT-IR Spectrometer set to a resolution of 8 cm−1 co-added over 32 scans at a speed of 5 kHz. Elemental analysis was performed on each gel with a K-Alpha XPS (Thermo Scientific) using a spot size of 400 μm for a binding energy survey from −10 to 1,350 eV with a pass energy of 200 eV. The energy step size was held at 1 eV across 10 scans with a 10 ms dwell time. Two spots on opposite ends of each sample were captured to monitor intrabatch heterogeneity, and data represents the average and standard deviation from the two points for each gel between three gels synthesized identically. Linescans were drawn along the central z-axis of split T35.0 samples with a spot size of 30 μm. Six spots were planted equidistant from one another along the length of the scan, permitting three reflected points for each disk spanning from the thickness’s center. Parameters for surveys collected across the line scan were the same as those used for surface surveys.
7000e ft ir spectrometer
Manufactured by Agilent Technologies
The 7000e FT-IR Spectrometer is a laboratory instrument designed for the analysis of molecular compounds. It uses Fourier Transform Infrared (FT-IR) spectroscopy to identify and characterize the chemical composition of samples. The spectrometer measures the absorption of infrared radiation by the sample, producing a unique spectrum that can be used to identify the presence and concentration of various functional groups and molecular structures.
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4 protocols using 7000e ft ir spectrometer
1
Characterizing Copolymer Composition via FTIR and XPS
2
FTIR Analysis of Solid Samples
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The samples were in the form of a KBr pellet of a ~200-μm thickness and a 13-mm diameter. The samples were located in a cell composed of two circular KBr windows of a 25-mm diameter. The windows were separated by a 200-μm thick spacer with 25 and 20 mm outer and inner diameters, respectively. FTIR spectra were recorded by a Varian 7000e FTIR spectrometer. The samples with KBr windows were placed in a home-made oxygen-free high thermal conductivity (OFHC) copper cell, and the temperature of the samples was controlled and maintained in a variable temperature cell holder (GS21525, Specac, UK). Details of the temperature-controllable cell assembly have been reported elsewhere38 (link).
3
Measuring Hydrogel Monomer Conversion by FTIR
4
Characterization of Electrochemical Properties
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Instrumentation Ultraviolet-visible (UV-vis) spectra were recorded on an HP 8454 spectrophotometer in CH 2 Cl 2 . Cyclic voltammetry was carried out with an EG&G model 263A potentiostat equipped with a three-electrode system: a glassy carbon working electrode, a platinum wire counter electrode, and a saturated calomel reference electrode (SCE). Tetrabutylammonium perchlorate, recrystallized twice from absolute ethanol and dried in a desiccator for at least 2 weeks, was used as the supporting electrolyte. The reference electrode was separated from the bulk solution by a fritted-glass bridge filled with a solvent/supporting electrolyte mixture. All potentials were referenced to the SCE. A scan rate of 100 mV s -1 was used. The anhydrous CH 2 Cl 2 solutions were purged with argon for at least 5 min prior to the electrochemical measurements and an argon blanket was maintained over the solutions during the measurements. 1 H NMR spectra (400 MHz) were recorded in CDCl 3 (referenced to residual CHCl 3 at 7.26 ppm) at 298 K on a Varian Inova 400 spectrometer. High-resolution electrosprayionization (HR-ESI) mass spectra were recorded on an LTQ Orbitrap XL mass spectrometer. IR spectra were acquired as an average of 32 scans with a 1 cm -1 resolution on a Varian 7000e FT-IR spectrometer.
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