Advance dpx 400 mhz spectrometer

¹H NMR spectra were obtained on an Advance DPX 400 MHz spectrometer (Bruker, Karlsruhe,, Germany). The samples were dissolved either in deuterated chloroform (CDCl₃) or dimethylsulfoxide (DMSO-d₆) with tetramethylsilane (TMS) used as internal standard. Thermogravimetric analysis (TGA) was performed using a Labsys TG (Setaram Instrumentation, Caluire-et-Cuire, France). The samples were heated at 20 °C min⁻¹ to 800 °C under nitrogen atmosphere. ATR-IR spectra were recorded on Platinum ATR spectrometer (Bruker, Ettlingen, Germany). The surface and the cross-sectional morphology of the membranes were studied by SEM using a LEO Supra 35VP microscope (Zeiss, Oberkochen, Germany). The specimens for the cross-section study were prepared by fracturing the membranes in liquid nitrogen. Differential Scanning Calorimetry analyses were performed on a DSC instrument from Perkin Elmer (DSC Q100, Waltham, MA, USA) over a temperature range from −100 to 300 °C (including heating and cooling cycles) under nitrogen flow at a scan rate of 10 °C/min. The first heating run was conducted in order to remove the thermal history and traces of absorbed water and residual solvents from the samples. The glass transition temperatures were recorded in the second heating run.

5,10,15,20-tetrakis(3-pyridyl)porphyrin, TPyP was prepared using Adler-Longo method with modifications, which was further methylated to produce 5,10,15,20-tetrakis (3-methyl pyridyl) porphyrin (TMePyP) [47 (link),48 (link)]. Initially, TPyP was synthesized by mixing 3.76 mL (0.04 mol) of 3-pyridylcarboxaldehyde and 2.8 mL (0.04 mol) of freshly distilled pyrrole in a flask containing 150 mL of propionic acid under reflux conditions. After ca. 30 min, the flask was cooled to room temperature, and distilled water (150 mL) was added to the reaction mixture. The product was extracted using 150 mL of dichloromethane. After removal of the solvent, the product was purified by column chromatography using dichloromethane, n-hexane, and methanol (1:1:1) as eluents to give 350 mg of TPyP yield.
For the methylation of TPyP, 330 mg of the as-synthesized TPyP was mixed with 30 mL of MeI in CHCl₃ at room temperature and stirred. After 6 h, the solution was filtered and washed with diethyl ether, and the filtrate was air-dried. ¹H NMR spectra and ¹³C-NMR spectra were recorded on a Bruker Advance DPX-400 MHz spectrometer (Karlsruhe, Germany). The absorption spectra were recorded on a UV-Vis-NIR JASCO V-770 spectrophotometer (JASCO Corp., Tokyo, Japan).

The ¹HNMR and Fluorine Nuclear Magnetic Resonance (¹⁹FNMR) spectra were recorded on an Advance DPX 400 MHz spectrometer (Bruker, Karlsruhe, Germany). All solutions were made either in deuterated chloroform (CDCl₃) or dimethylsulfoxide (DMSO-d₆) and tetramethylsilane (TMS) was used as internal standard.
Thermogravimetric analysis (TGA) was conducted in the temperature range from room temperature to 800 °C under nitrogen atmosphere and a heating rate 20 °C min⁻¹ using a Labsys TG (Setaram Instrumentation, Caluire-et-Cuire, France).
Attenuated Total Reflection Fourier Transform Infra Red (ATR-FT-IR) spectra were collected on a Platinum ATR spectrometer (Bruker, Ettlingen, Germany).
Scanning Electron Microscopy (SEM) was conducted on a LEO Supra 35VP microscope (Zeiss, Oberkochen, Germany). Membrane cross-sections for SEM imaging were prepared by freeze-fracturing the samples after immersion in liquid nitrogen.
Differential Scanning Calorimetry (DSC) was carried out on a Perkin Elmer DSC instrument (DSC Q100, Waltham, MA, USA) from −100 to 300 °C with a heating rate of 10 °C/min under a nitrogen flow. The effect of water and previous thermal history was erased by the first heating run while the glass transition temperatures were recorded in the second heating run.