Perkin-Elmer thermogravimetric

TGA analysis was carried out on a Perkin-Elmer Thermogravimetric analyzer, model TGS-2 at a heating rate of 10°min. 

The thermal stability of PEtG was obtained using a Perkin Elmer thermogravimetric analyzer (TGA7) at the heating flow of lOX/min and under N2. 

A Perkin-Elmer thermogravimetric analyzer (TGA) was used to determine the hydrogen desorption kinetics at atmospheric pressure. This instruntent was located in another glove box under nitrogen atmosphere to prevent any exposure of the samples to air and moisture. Samples were heated to 2S0°C at a ramping rate of S°C/min under 1 atm of He, using an initial 1 minute delay to ensure an environment of pure He. Approximately 10 mg of sample were used in the TGA. 

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. 

S.3 Thermogravimetric Analysis The thermal properties of the membranes were evaluated using a Perkin-Elmer thermogravimetric analyzer (TGA-7) interfaced... 

Dynamic mechanical anlaysis (DMA) measurements were done on a Rheometrics RDS-7700 rheometer in torsional rectangular geometry mode using 60 x 12 x 3 mm samples at 0.05% strain and 1 Hz. Differential scanning calorimetry (DSC), thermomechanical analysis (TMA), and thermogravimetric analysis (TGA) were performed on a Perkin-Elmer 7000 thermal analysis system. 

Thermal stabilities were assessed by thermogravimetric analysis (TGA). Samples were held at constant temperature (290°C) for 1 h in air in a Perkin-Elmer TGA. Much of the weight loss, particularly for Kel-F 6060, is suspected to be emulsifier used during polymerization. 

The XPS data were acquired on a Physical Electronics model 5400 XPS system using a Mg anode. For survey spectra, the pass energy was 44.75 eV with a step size of 0.5 eV. The time per step was 50 msec. High resolution spectra were acquired with a pass energy of 35.75 eV and step size of 0.1 eV, The time per step was 50 msec. Thermogravimetric data were obtained on a Perkin-Elmer, Diamond Thermogravimetric/ Differential Thermal Analyzer (TG/DTA) with Pyris software, version 7.0-0.0110. 

ThermoGravimetric Analysis (TGA) was performed on TGAQ50 (TA Instruments) under air up to 800°C. FTIR spectra were obtained on a Spectrum One from Perkin Elmer Instruments. Elemental Analysis was performed by Service Central d Analyse from CNRS located at Vemaison (France). Con-ductimetry back-titration of amine functions (after contact with HCL 0.1 N in excess) was performed using a Tacussel conductimetry probe by a 0.1M NaOH solution. Porosimetry measurements were performed on a SORPTOMATIC 1990 from CE Instruments specific surface areas were calculated using BET model between P/P =0 and P/P =0.4 and pore size repartitions were determined using BJH model. SEM photos were obtained on an Ultra 55 (Zeiss). 

The compositions of the products were determined by inductively coupled plasma (ICP) with a Perkin-Elmer plasma 40 emission spectrometer. Simultaneous differential thermal analysis and thermogravimetric (DTA-TG) curves were carried out by using Perkin-Elmer DTA-7000, TGA-7 PC series thermal analysis instrument in air with a heating rate of 10 °C /min. The infrared (IR) spectra were recorded on an Impact 410 IR spectrometer on samples pelletized with KBr powder. Valence states were determined by X-ray photoelectron spectroscopy (XPS). The XPS for powder samples fixed on double sided tapes was measured on an ESCA-LAB MKII X-ray photoelectron spectrometer. The Cis signal was used to correct the charge effects. 

The sample particles of the precursor used here are about 10 pm in size. Its composition was confirmed with its molecular formula. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were simulteineously conducted on a PCT-1 type thermoanalysis meter in H2 (99.999%), and were respectively completed on a Perkin-Elmer TGS-2 and a Perkin-Elmer DTA-1700 in N2(99.99%) or air, with 5 °C min heating rate and a gas flow rate of 15 mL min . 

Powder X-ray diffraction (XRD) patterns of the samples were carried out on a Rigaku RTP300-RC X-ray diffractometer with Cu Ka ( =1.541 SA) radiation. Infrared spectra (IR) were recorded by the KBr method on a Perkin-Elmer 1600 Series FTIR infrared spectrometer. Thermogravimetric (TG) and differential thermal analysis (DTA) curves were obtained at a heating rate of 10°C/min in air on a Seiko SSC5200 thermal analyzer. Scanning electron microscopy (SEM) was performed on a Hitachi S-530 scanning electron microscope. 

Thermogravimetric analyses (TGA) were carried out with a Perkin-Elmer TGS-2 analyzer at a nitrogen flow rate of 50 cmmin. The temperature program for the analysis was 50 °C for 10 min followed by an increase of 5 °C/min to 600 °C. 

Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA) evaluations were performed using Perkin Elmer DSC-2C to obtain the T, T, and A/f. A Du Pont Model 2950 TGA was used to evaluate the total amount of carbon dioxide uptake in polymers. A constant heating rate of 20°C/min was used in both the DSC and TGA evaluations. 

X-ray powder diffraction patterns were obtained on oriented film specimens [7] (2 to 45° 2 , Philips PW 1120, monochromatized CuKa radiation, continuous peak registration). BET surface area and the pore volume distribution were determined from Nj adsorption-desorption isotherms at 77 K (degassing at 393 K, lO" mbar, 5h Sorptomatic 1900, Carlo Erba Instruments). The IR-spectra were recorded on KBr wafers [4] with a Specord 80M spectrometer. The XPS (X-ray photoelectron spectroscopy) spectra were obtained with VG ESCALAB 200 MKII spectrometer equipped with a twin anode AIKa source (1486 eV). The thermogravimetric (TGA) analyses were carried out with a Setaram TG 85 thermobalance at a heating rate of 6 K min in a helium flow of 30 ml min . The chromium content of the samples was determined by EPMA (JEOL 840 scanning electron microscope) with energy dispersive spectrometer (EDS, Tracer Northern) and by AAS (atomic absorption spectroscopy, Perkin Elmer 3030) analyses. 

Thermogravimetric Analysis (TGA) of diltiazem hydrochloride tested under a nitrogen atmosphere indicates no weight loss until a temperature of - 230°C is reached. Significant weight loss is observed above 230°C due to decompo-sition/vaporization. A typical TGA curve is shown in Figure 11. The curve was obtained using a Perkin Elmer Series 7 TGA... 

The solids were characterized by X-ray diffraction using a Siemmens D-500 diffractometer equipped with a copper anode and a nickel filter. The deposition of carbon was studied by thermogravimetric analysis (TGA) using a Perkin-Elmer 1700 TGA analyzer. For the TGA runs the sample was heated at 10°C/min in air (2.0 1/h) from ambient temperature (20 C) to 850°C the procedure was repeated to eliminate Ae effect of adsorbed water. 

General. Commercially available polyimides were used (see Table I). Solvents were reagent grade or better and were used as received. 1-Methylpiperazine (Aldrich Chemical Co.) was > 99.9% pure. Lactic acid (Aldrich) was reduced to 50% by weight in water and refluxed for an hour to hydrolyze esters. IR spectra were recorded on a Perkin-Elmer Model 1430 spectrometer. Thermogravimetric analysis was done on a P-E System 4/TGS-2 instrument. Size exclusion chromatography was done on a Perkin-Elmer Series 3B equipped with the LC-75 spectrophotometric detector. The column set used consisted of P-E 0258-2134, 2133, and 2131 columns (pore sizes 103, 104, and 106 A, respectively). For electrophoretic deposition experiments, a TCR Power Supply (Electronic Measurement Systems Inc.) was used. Temperatures are reported in °C throughout. 

A Perkin-Elmer TGA-7 instrument calibrated by Curie points of several metal standards has been employed for non-isothermal thermogravimetric analysis. The measurements were carried out at a desired heating rate (in the range of 3 - 40 K/min) in both inert (argon) and oxidizing (oxygen) atmospheres, as appropriate. 

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