1H and 13C NMR were performed on a Bruker DPX‐400 spectrometer, at 400 MHz and 100 MHz, respectively. All chemical shifts were in parts per million (ppm) relative to the tetramethylsilane (TMS) internal standard (0.03% v/v, 0.00 ppm). Coupling constants (J) were expressed in Hertz (Hz). Infrared spectra were recorded on a Bruker ALPHA platinum ATR Fourier transform spectrometer. Absorptions were recorded in wavenumbers (cm−1). Mass spectrometry was achieved using an Agilent 6130B single Quad (ESI). GPC was performed on an Agilent 390‐MDS with autosampler using a PL gel 5.0 µm bead‐size guard column (50 × 7.5 mm), followed by two linear 5.0 µm bead‐size PL gel Mixed D columns (300 × 7.5 mm) and a differential refractive index detector. Using CHCl3 as eluent the system was calibrated using linear poly(styrene) Easi Vial standards (Agilent Ltd) range from 162 to 5×105 Da. Data were collected and analysed using Cirrus GPC/SEC (v. 3.3) and Agilent GPC/SEC software. TGA, DSC and melting points were carried out using Metler Toledo DSC1‐Star with 40 µL standard aluminium pans and autosampler. Samples heated from −100–70°C, cooled to −100 and heated from −100–600°C under N2 atmosphere for DSC and heated from 25–600°C for TGA.
390 mds
The 390-MDS is a laboratory instrument designed for the purpose of molecular detection and separation. It is a specialized piece of equipment used in analytical chemistry and life science research applications.
2 protocols using 390 mds
Comprehensive Analytical Characterization Protocol
1H and 13C NMR were performed on a Bruker DPX‐400 spectrometer, at 400 MHz and 100 MHz, respectively. All chemical shifts were in parts per million (ppm) relative to the tetramethylsilane (TMS) internal standard (0.03% v/v, 0.00 ppm). Coupling constants (J) were expressed in Hertz (Hz). Infrared spectra were recorded on a Bruker ALPHA platinum ATR Fourier transform spectrometer. Absorptions were recorded in wavenumbers (cm−1). Mass spectrometry was achieved using an Agilent 6130B single Quad (ESI). GPC was performed on an Agilent 390‐MDS with autosampler using a PL gel 5.0 µm bead‐size guard column (50 × 7.5 mm), followed by two linear 5.0 µm bead‐size PL gel Mixed D columns (300 × 7.5 mm) and a differential refractive index detector. Using CHCl3 as eluent the system was calibrated using linear poly(styrene) Easi Vial standards (Agilent Ltd) range from 162 to 5×105 Da. Data were collected and analysed using Cirrus GPC/SEC (v. 3.3) and Agilent GPC/SEC software. TGA, DSC and melting points were carried out using Metler Toledo DSC1‐Star with 40 µL standard aluminium pans and autosampler. Samples heated from −100–70°C, cooled to −100 and heated from −100–600°C under N2 atmosphere for DSC and heated from 25–600°C for TGA.
SEC Analysis of Polymer Molar Mass
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