Film thicknesses were assessed using variable angle spectroscopic ellipsometry (VASE, J.A. Woollam, USA). Thermal cross-linking was produced using FP82HT Hot stage with FP90 Central Processor (Mettler Toledo, USA). Photo-cross-linking reactions were performed using Omnicure series-1000 UV lamp at the wavelength of 360 nm (Lumen Dynamics, USA). The intensity of UV light was measured employing ILT-1400-A radiometer–photometer (International Light Technology, USA). In all experiments, the UV lamp was allowed to warm for about 20–30 min prior to the cross-linking reactions for better reproducibility (cf. Figure S7 ). Dip-coater (KSV-NIMA, USA) was used to move the sample under the UV light for making photogradient surfaces. The polymer film was deposited using spin coater (PNM32 model, Headway Research, Inc., USA). The molecular weight of the polymer was determined using size exclusion chromatography (SEC, Wyatt Optilab rex detector along with Alliance waters 2695 separation module, USA). Functionality of the monomer and polymer was examined using 300 MHz 1H NMR and 13C NMR (Varian, USA).
13c nmr
Manufactured by Agilent Technologies
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The 13C NMR (Carbon-13 Nuclear Magnetic Resonance) is a laboratory equipment used to analyze the chemical structure of organic compounds. It detects the magnetic properties of carbon-13 isotopes within a sample, providing information about the chemical environment and connectivity of carbon atoms.
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Lab products found in correlation
3 protocols using 13c nmr
1
Photocrosslinking Polymer Thin Films
2
Characterization of Synthesized Compounds
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Chemicals were obtained from Sigma-Aldrich (Aldrich chemical Co., Milwaukee, WI, USA). A Griffin melting point apparatus (Griffin, Valdosta, GA, USA) was used to measure melting points (m.p.). A Nicolet IR 300 (Thermo Fisher Scientific, Barrington, RI, USA) was used to measure the infrared spectra. 1H- NMR and 13C- NMR (Varian, Palo Alto, CA, USA) were performed in deuterated dimethyl sulfoxide (DMSO-d6) using a Varian 300 MHz instrument. Tetramethylsilane (TMS) was used as internal standard. MS spectra were measured using a JEOL-SX-102 electron impact ionization instrument (Joel, Peabody, MA, USA). Evaporation processes were performed under reduced pressure by using a Buchi rotary evaporator (Buchi, Postfach, Flawil, Switzerland). Elemental analyses (C, H, N) were accomplished using a Perkin-Elmer 240C analyzer (Perkin-Elmer, Norwalk, CT, USA). The synthesized compounds were within ±0.4% of the theoretical values. Purity of the newly-synthesized compounds was above 99.6%.
3
Isolation and Purification of Compounds
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ACS reagent grade solvents were purchased from Sigma–Aldrich Chemical Company (St. Louis, MO, USA) and used for all isolation and purification steps. Merck silica gel (60 mesh size, 35−70 μm) with particle size of 60 μm was used for preparative medium-pressure liquid chromatography (MPLC). Silica gel plates (250 μm; Analtech, Inc., Newark, DE, USA) were used for preparative thin-layer chromatography (TLC). After developing, TLC plates were observed under UV light at 254 and 366 nm in a Spectroline CX-20 ultraviolet fluorescence analysis cabinet (Spectroline Corp., Westbury, NY, USA) and sprayed with 10% sulfuric acid solution. NMR spectra were recorded on 500 MHz (Varian Unity ±500, 1H NMR) and 125 MHz (Varian Unity ±500, 13C NMR) VRX instruments. ESIMS spectra were recorded on a Waters Xevo G2-S Q-TOF LC mass spectrometer (Waters Corporation, Milford, MA, USA) and GCMS on Thermo DSQ-II GC/single quadrupole mass spectrometer (Thermo Electron Corporation, Austin, TX USA).
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