Cxp 200

IR spectra of the samples were recorded in potassium bromide pellets using a Nicolet 380 spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). ¹H NMR spectra were registered on Bruker CXP 200, Chemical shifts in ¹H spectra were measured relative to the signal of (CH₃)₄Si. Micro photo images were processed using the MCview (Lomo Microsystems, St-Petersburg, Russia) software package via Lomo MSP-2-2SD stereoscopic microscope equipped with an MC-5 electronic camera (Lomo Microsystems, Russia). MALDI spectra were recorded on an Ultraflex II mass spectrometer (Bruker, Karlsruhe, Germany) with an accelerating voltage of 25 kV with Nd: YAG laser (355 nm) desorption from a DHB matrix.

0.2 mL of a solution of 1,3-dimethylimidazolium (phosphonooxy-)oligosulphanide, obtained according to the previously described method [21 (link)], was added to a solution of 0.5 g of acrylamide (“Sigma-Aldrich”, purity over 99%, St. Louis, MI, USA) in 2 mL of water (bidistillate), followed by stirring for 20 min. Then the reaction mixture was left at a temperature of 298 K (25 °C) and dried. The structure of the obtained polyacrylamide was characterized by XRD (Benchtop X-ray Diffractometer, Malvern Panalytical Aeris XRD) and X-ray fluorescent analysis (Bruker Kappa APEX DUO).
The dynamics of acrylamide polymerization was investigated in situ in an open ampoule, daily recording the ¹H NMR spectrum (Bruker CXP 200) of the reaction system. For the sample isolated four days after the start of the reaction and washing with methanol (in the calculation of 10 mL of CH₃OH (“Sigma-Aldrich”, purity over 99%) per 1 g of gel), the ¹³C NMR spectrum was recorded.