Thermogravimetric analyzer heat measurements

Thermal Properties. The glass transition temperature (Tg) and the decomposition temperature (Td) were measured with a DuPont 910 Differential Scanning Calorimeter (DSC) calibrated with indium. The standard heating rate for all polymers was 10 °C/min. Thermogravimetric analysis (TGA) was performed on a DuPont 951 Thermogravimetric Analyzer at a heating rate of 20 °C/min. 

Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were performed in air at a heating rate of lOK/min. on a PTC-lOA thermogravimetric analyzer. The adsorption isotherms for vapor-phase water and ethanol were measured using the BET method. The saturation pressures, Pq, of water and ethanol at 299K are 758 mmHg. Prior to the adsorption experiments, the samples were dehydrated at 673K in air for 4 h. 

Temperature programmed reduction (TPR), temperature programmed Ar heating (TPAr) and extent of reduction experiments were all performed in a Perkin Elmer thermogravimetric analyzer (TGA) Model TGA 7 described elsewhere [22]. H2 chemisorption measurements were eonducted using a flow chemisorption method and apparatus described by Jones and Bartholomew [24]. Activity measurements and high-pressure steam treatments were conducted in a fixed-bed microreactor described elsewhere [22]. A Micromeritics Gemini 2360 surface analyzer was used to measure N2 adsorption at liquid N2 temperature for BET surface area measurements. A Micromeritics Tri-Star 3000 analyzer with N2 adsorption was used to obtain the pore size distribution. 

Thermogravimetric analyzer (TGA). TGA measures weight changes in a sample as the temperature is varied, providing a useful means to determine degradative processes and heat resistance in polymeric compounds. 

The thermal stability of nanobiocomposites was analyzed up to 500°C with a heating rate of 10°C/min under the atmosphere with flow rate of 100 ml/min. Changes in weight percentage and the decomposition temperatures of the samples were recorded with a thermogravimetric analyzer (TGA Q 500, TA Instruments). Approximately 10 mg of each sample were loaded for each measurement. 

Differential scanning calorimetry (DSC) was employed for the measurement of the Tg s and the detection of any other thermal transitions. For this purpose, a TA Instrument Model DSC 2910 was used with a heating rate of 10°C min for samples weighing 5-15 mg. An Auto TGA 2950HR V5.4A thermogravimetric analyzer... 

The TG measurements of the sample were carried out by a thermogravimetric analyzer (Model TGA/ SDTA 851e, Mettler Toledo, USA) under N2 with a flow rate of 40 ml-min-1 at the heating rate of 10 K-min-1 from 300 to 580 K, respectively. The sample about 10-15 mg was filled into alumina crucible without pressing. 

X-ray diffraction patterns were recorded on a Siemens D5000 diffractometer using CuKa radiation. Thermogravimetric and differential thermal analysis curves were recorded on a Setaram Setsys 12 thermal analysis station by heating in an argon atmosphere from 25 to 1200 -C at a rate of 5 min". Samples were used untreated. The Pt content was determined by the Service Central d Analyse, CNRS (Vernaison, France) and the microanalyses (C, H) were performed at Complutense University (Madrid, Spain). Na isotherms were determined on a Micromeritics ASAP 2000 analyzer. H MAS NMR, Si MAS NMR and C CP MAS NMR spectra were recorded at 400.13, 79.49 and 100.61 MHz, respectively, on a Broker ACP-400 spectrometer at room temperature. An overall 1000 free induction decays were accumulated. The excitation pulse and recycle time for H MAS NMR spectra were 5 ps and 3 s, respectively, those for Si MAS NMR spectra 6 ps and 60 s and those for C CP MAS NMR spectra 6 ps and 2 s. Chemical shifts were measured relative to a tetramethylsilane standard. Prior to measurement, if necessary, samples were dehydrated in a stove at 423 K for 24 h. 

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