Sta 449 f1 jupiter thermobalance

The thermal properties of the copolymer sample were investigated using the TG/FTIR/MS thermal analysis system consisting of an STA 449 F1 Jupiter thermobalance, Netzsch, Selb, Germany, coupled online with a Vertex 70 FTIR spectrometer (Ettlingen, Germany) and with an Aëolos QMS 403C mass spectrometer from Netzsch. Briefly, 14 mg of freeze-dried sample was placed in an open Al₂O₃ crucible and heated in a nitrogen-inert atmosphere (50 mL/min gas flow) up to 675 °C. Measurement was achieved in dynamic mode with a heating rate of 10 °C/min using Proteus 5.0.1 software. Gases evolved during the decomposition process were transferred through a heated Teflon line (190 °C) to the TGA-IR external modulus fitted with an MCT (Mercury Cadmium Telluride) detector. FTIR spectra were registered between 4000 and 600 cm⁻¹ in 3D size with OPUS 6.5 software. The gases were also transferred to the Aëolos mass spectrometer using a 75 μm quartz capillary maintained at 260 °C. MS spectra ranging from 1 to 200 m/z were obtained using ionization energy with an electron impact of 70 eV and a vacuum of 10⁻⁵ mbar. Aëolos 32 software was employed in MS data acquisition and processing.

The synthesized copolymer was investigated from the viewpoint of the thermal behavior. Simultaneous analysis TG/FTIR/MS was used to study the weight losses and identify the main released gases composition. The following system has been used: STA 449 F1 Jupiter thermobalance (Netzsch, Selb, Germany) coupled online with a mass spectrometer Aeolos QMS 403C (Netzsch, Selb, Germany) and FTIR spectrophotometer Vertex 70 (Bruker, Kloten, Switzerland) equipped with TGA-IR external module. The samples weighed up to 10–15 mg, were placed into Al₂O₃ crucible and heated under nitrogen flow of 40 mL min⁻¹ from room temperature up to 650 °C with a heating rate of 10 °C min⁻¹ in the presence of Al₂O₃ crucible as reference material. The resulted gases were transferred to mass spectrometer through a quartz capillary of 70 µm maintained at 290 °C. The MS spectra were registered with the aid of Aeolos 7.0 software (Selb, Germany) on the range of m/z of about 1 up to 200.
Additionally, the gases are transferred through a poly(tetrafluoroethylene) tube maintained at 190 °C, to the TGA-IR external modulus where the FT-IR spectra were recorded on the 600–4000 cm⁻¹ interval, at a resolution of 4 cm⁻¹ using OPUS 6.5 software.

Transmission electron microscopy (TEM) images were carried out using a FE-TEM Libra 120 Carl Zeiss microscope at a 120 kV acceleration voltage. The samples were placed onto a carbon coated copper microgrid (400 mesh) that was dried overnight. At least 5 different sample of nanoparticles were prepared, and from each grid at least 3 pictures were taken. The diameters of the cores of the nanoparticles were determined for at least 300 nanoparticles in each image.
The UV-Vis spectra were recorded using a Perkin Elmer Lambda 25 UV-Vis spectrophotometer.
Thermogravimetric measurements (TG) were carried out using a Netzsch STA 449 F1 Jupiter thermobalance. All samples were heated at a rate of 5°C min⁻¹ up to 760 °C in an argon atmosphere. Argon (99.5%) was obtained from Air Products (Poland).
The electrochemical experiments were performed using a CHI 750D electrochemical workstation (CHI Instruments Inc., Austin, Texas) in the three-electrode arrangement employing a platinum foil counter electrode, an Ag/AgCl (KCl sat.) reference electrode and a glassy carbon disc electrode (BASI) as a working electrode.
All ¹H and ¹³C NMR spectra were performed using a Bruker AVANCE 300 MHz spectrometer and the mass spectra were recorded with a Quattro LC mass spectrometer.