Thermal behavior of the investigated compound was determined using Setaram Setsys (Setaram Instrumentation, Ratingen, Germany)16/18 derivatograph, registering TG, DTG and DSC curves. The sample (3.96 mg) was heated in a Al2O3 crucible between 30 and 1000 °C in flowing air atmosphere (v = 0.75 dm3 h−1) with a heating rate of 10 °C min−1. The temperature and heat flow of the instrument were calibrated by the melting point and enthalpy of indium standard. TG-infrared spectrometry (TG-FTIR) of the title compound was performed using the TGA Q5000 analyzer (TA Instruments, New Castle, DE, USA) interfaced to the Nicolet 6700 FTIR spectrophotometer (Thermo Scientific, Waltham, MA, USA) in oxidizing and inert atmospheres. The samples of 10.65 mg (air atm.) and 19.09 mg (N2 atm.) were put in an open platinum crucible and heated from an ambient temperature (~25 °C) to 700 °C with a heating rate of 20 °C min−1 (at a flow rate of 25 mL min−1). In order to reduce the possibility of gases condensing along the transfer line, the temperature in the gas cell and transfer line were set to 250 and 240 °C, respectively. The FTIR spectra were recorded in the spectral range of 600–4000 cm−1 with a resolution of 4 cm−1 and 6 scans per spectrum. Thermal decomposition of compound in air atmosphere using TGA Q5000 analyzer was also performed with a heating rate of 10 °C min−1 in the range 25–700 °C.
Do you have any questions about this protocol?
Post your question to gather feedback from the community. We will also invite the authors of this article to respond.