Dtg 60h thermal analyzer

Scanning electron microscopy was performed using a Hitachi S-3400 scanning electron microscope in backscattered electron mode under high vacuum. Elemental analysis in the scanning electron microscope was performed using an Ametek EDAX energy dispersive X-ray analyzer. Crystallographic analysis was performed using a Shimadzu XRD-6000 X-ray diffractometer with CuKα radiation (λ = 0.15418 nm). To investigate the optical response of the samples by diffuse reflectance spectral measurements, a JASCO V-560 UV–Vis-NIR absorption spectrophotometer equipped with a JASCO ISV-469 type integrating sphere was used. A solid sample cell with a quartz window was used for the measurements. Barium sulfate powder was used as the white light reference standard. A Shimadzu Biospec-1600 UV–visible absorption spectrophotometer was used for determination of the methylene blue concentration in aqueous solution. The concentration was determined using a calibration curve prepared from the absorbance of methylene blue standard solutions at 665 nm. For thermal analysis, a Shimadzu DTG-60H thermal analyzer was used to record the differential heat and thermogravimetric changes with increasing temperature.

The FTIR spectra of the ligand and its metal complexes in the solid state were measured using Agilent technologies/Gladi-ATR, USA) Cary 600 Series FTIR Spectrometer in the wave range 400–4000 cm⁻¹. The carbon, hydrogen, and nitrogen contents were determined for the prepared ligand and its metallic complexes using a Eurovector CHN (EA3000, Italy) analyzer. Magnetic moments were measured using a Sherwood Scientific magnetic susceptibility balance (MSB-Auto) (UK). Electron-visible and UV-visible absorption spectra of (DMSO, 1 × 10⁻³ M) solutions were also recorded on a Shimadzu 1650-Spec UV-Vis spectrometer (Shimadzu, Duisburg, Germany). Thermal analysis of the compounds was carried out in dynamic air on a Shimadzu (DTG 60-H) thermal analyzer at a heating rate of 10 °C/min, the temperature range was 20–600 °C. XRD Model (PW 1710) control unit Philips with a Cu Kα (l = 1.54180 Å) anode at 40 K.V 30 M. A scanning electron microscopy (SEM) was used to examine the morphology of the complexes (JEOL JSM-5400-LV Field Emission SEM, Tokyo, Japan).

The infrared measurements (KBr discs) were recorded on a Perkin-Elmer BX FTIR spectrometer (4000–400). The UV-visible spectra were recorded on a SM-1600 Spectrophotometer. Molar conductance of the complexes was recorded at room temperature in 1.0 × 10-3 M in DMSO solution using electrical conductometer (AD8000). The thermogravimetric/differential thermal analyses (TGA/DTA) data were recorded from 25–800 C with a heating rate of 10°C/min under nitrogen-atmosphere (20 ml/min) by a Shimadzu DTG-60H thermal analyzer. The high-resolution mass spectra were obtained with a Waters-LCT-Premier mass spectrometer using 2 ng/μl of sample concentration with a capillary voltage of 2500 V and a desolvation temperature of 250°C using nitrogen gas at 250 L/h, Bruker APEX II CCD area detector diffractometer, with graphite monochromated Mo K3 radiation (50 kV, 30 mA) and temperature of measurement at 173 (2) K coupled with APEX 2 data collection software. Four scans of width 0.5 and 512 × 512 bit data frames were involved for data collection, SAINT + program was used to achieve the data reduction, and face indexed absorption corrections were made using XPRE.

Melting points were measured on an electrothermal digital microscopic melting point apparatus and recorded without modification. The reaction was followed by thin layer chromatography on silica. ¹H NMR and ¹³C NMR spectra were recorded with tetramethylsilane as standard in CDCl₃ or DMSO-d6 solution, respectively, using a Bruker AMX 500-MHz spectrometer at 500 and 125 MHz. Chemical shifts were measured in parts per million (ppm) and coupling constants (J), hertz (Hz).
Low resolution mass spectrographic analyses were measured using the electrospray ionization technique on a Bruke Esquire 3000 spectrometer. Thermogravimetry (TG), differential thermogravimetry (DTG), and differential thermal analysis (DTA) curves were obtained simultaneously using a Shimadzu DTG-60H thermal analyzer. The air atmosphere was selected and the flowing rate was adjusted as 25 mL min^–1, since the potential applications of these compounds were carried out in air. All compounds were heated from room temperature to 800 °C with using 10 °C min^–1 heating rate. Silver was used to calibrate the balance for buoyancy effects for the quantitative estimation of mass change. The melting points indium of tin (provided by Shimadzu) were used to calibrate the temperature. Four different compounds (1a, 1b, 1d, 1h) were selected for thermal investigation. These compounds were chosen due to the varied functional groups.

The attempted materials were characterized by means of various analysis as follows. XRD (D8Discover with GADDS, Bruker AXS) was carried out over the 2θ range of 10–80°, using a CuKα radiation source (λ = 1.5406 Å). XPS analysis was carried out using a K-Alpha model (Thermo Electron). Other characterization techniques included FE-SEM (Leo Supra 55, Genesis 2000, Carl Zeiss), FE-TEM JEM-2100F, JEOL) with elemental mapping, TGA (DTG-60H thermal analyzer, Shimadzu), high-resolution Raman spectroscopy (HR-Raman, inVia), EIS (IVIUM), and electrochemical (Arbin).

Approximately 16 mg of powder for each set of sealers was obtained by grinding using an agate mortar and pestle (Nahita, Istanbul, Turkey). Sample powders were analyzed to evaluate the thermal stability of each sealer using Thermogravimetric analysis (TGA) and Differential thermal analysis (DTA) using a TGA/DTA Thermal Analyzer (Shimadzu DTG-60H Thermal Analyzer, Kyoto, Japan). Thermal measurements were performed under the flow of nitrogen atmosphere with a flow rate of 100 ml min⁻¹ in the temperature range from ambient to 250 °C. The heating rate was 20 °C per minute. Highly sintered α-Al₂O₃ was used as the reference material. Thermo-analytical TGA and DTA curves were obtained simultaneously. The data were analyzed using the TGA software (CDSS, v1.1).