Thermostar

The IR spectra of the coordination compounds were recorded on the Jasco FT/IR 6200 spectrophotometer (JASCO, Easton, MD, USA), in the spectral range 4000–400 cm⁻¹, in a form of KBr pellets. The UV-Vis diffuse reflectance spectra were recorded on the Jasco V-660 spectrophotometer (JASCO, Easton, MD, USA), in the spectral range 190–800 nm, using BaSO₄ as a standard with 100% reflectance. The thermal analyses were carried out in the TG/DTA-SETSYS-16/18 thermoanalyser (SETARAM Instrumentation, Caluire, France) coupled with the ThermoStar (Balzers) mass spectrometer. Samples were heated in platinum crucibles up to 1000 °C, with heating rate 5 °C∙min⁻¹ in synthetic air (21.0% O₂, 79.0% N₂) flow. Final products of decomposition were confirmed by X-ray powder diffraction (XRPD) using the Powder Diffraction File [44 ]. The X-ray powder diffraction (XRPD) patterns were measured in reflection mode on the XPert PRO XRPD system (Malvern Panalytical Ltd., Royston, UK) equipped with CuKα1 radiation, Bragg–Brentano PW 3050/65 high-resolution goniometer and PW 3011/20 proportional point detector. Surface morphologies of cobalt(II) oxide nanoparticles were characterized by the scanning electron microscope with energy dispersive X-ray spectrometer (SEM-EDS, HITACHI S-4700, EDS Thermo NORAN).

The thermogravimetric analyses (TGA) were performed with a TA Instruments TGA-DSC Simultaneous Analyzer, model SDT 2960. Two types of tests were carried out using 15 mg ionogel-based PIMs samples. The selected temperatures used for constant temperature tests were 60 °C and 90 °C, while for variable temperature tests a heating ramp of 10 °C/min was applied in a heating cycle set from 25 °C to 600 °C. All tests were conducted under an air atmosphere.
Longer duration tests were also performed for the same temperatures selected in the constant temperature tests discussed above, 60 °C and 90 °C. A 0.4 g sample of ionogel membrane was kept for 72 h at constant temperature in a Vaciotem-TV (J.P. Selecta) vacuum oven. To control the weight of the sample during the assay, the samples were removed from the oven in 24 h periods, allowed to temper in a desiccator for 1 h, and then they were weighed.
The thermogravimetric analyses (TGA) were performed with a TA Instruments TGA-DSC Simultaneous Analyzer, model SDT 2960.
In the case of thermogravimetric analysis coupled with mass spectrometry (TG-EM), the TG is coupled to a quadrupole mass spectrometer, “ThermoStar”, QMS 300M3, from Balzers, with a scanning range of 1 to 300 amu, from 0.2 to 10 s/uma. In this case, a heating ramp of 10 °C/min was applied in a heating cycle set from 30 °C to 800 °C.

Thermogravimetric (TG) analysis was carried out with a TGA 2050 (TA-Instruments, USA). Moreover, volatile products produced during thermal degradation were analyzed by mass spectrometry (MS). For this purpose, a thermogravimetric analyzer was coupled to the mass spectrometer (Thermostar, Balzers, Liechtenstein). Thermal analyses were made using samples of about 10 mg with a flow of air or nitrogen stream of 165 mL/min gas stream and a heating rate of 10 °C min⁻¹.