Temperature programmed desorption analysi

Temperature programmed desorption analysis was also performed over the heteropolyacids without previous thermal treatments in order to identify the... 

Temperature programmed desorption analysis gave insights on the species evolved upon heating of the heteropolyacids that were synthesized through ion exchange... 

Nishide, T., T. Tanaka, T. Yabe (2004) Temperature programmed desorption analysis of sol-gel-derived titania films. Journal of thermal analysis and calorimetry. 90,373-378. 

Temperature-programmed desorption (TPD) is amenable to simple kinetic analysis. The rate of desorption of a molecular species from a uniform surface is given by Eq. XVII-4, which may be put in the form... 

Temperature programmed desorption, TPD detection of backspillover species, 228 of oxygen, 228 Thermodynamics of adsorption, 306 of spillover, 104, 499 Three phase boundaries charge transfer at, 114 electrocatalysis at, 115 length, measurement of, 243 normalized length, 243 Time constants ofNEMCA analysis of, 198 and backspillover, 198 prediction of, 200... 

The scanning transmission electron microscope (STEM) was used to directly observe nm size crystallites of supported platinum, palladium and first row transition metals. The objective of these studies was to determine the uniformity of size and mass of these crystallites and when feasible structural features. STEM analysis and temperature programmed desorption (TPD) of hydrogen Indicate that the 2 nm platinum crystallites supported on alumina are uniform In size and mass while platinum crystallites 3 to 4 nm in size vary by a factor of three-fold In mass. Analysis by STEM of platinum-palladium dn alumina established the segregation of platinum and palladium for the majority of crystallites analyzed even after exposure to elevated temperatures. Direct observation of nickel, cobalt, or iron crystallites on alumina was very difficult, however, the use of direct elemental analysis of 4-6 nm areas and real time Imaging capabilities of up to 20 Mx enabled direct analyses of these transition metals to be made. Additional analyses by TPD of hydrogen and photoacoustic spectroscopy (PAS) were made to support the STEM observations. 

This study presents kinetic data obtained with a microreactor set-up both at atmospheric pressure and at high pressures up to 50 bar as a function of temperature and of the partial pressures from which power-law expressions and apparent activation energies are derived. An additional microreactor set-up equipped with a calibrated mass spectrometer was used for the isotopic exchange reaction (DER) N2 + N2 = 2 N2 and the transient kinetic experiments. The transient experiments comprised the temperature-programmed desorption (TPD) of N2 and H2. Furthermore, the interaction of N2 with Ru surfaces was monitored by means of temperature-programmed adsorption (TPA) using a dilute mixture of N2 in He. The kinetic data set is intended to serve as basis for a detailed microkinetic analysis of NH3 synthesis kinetics [10] following the concepts by Dumesic et al. [11]. 

N2-BET analysis and porosity measurements were done on a Micrometries ASAP 2000 apparatus at liquid nitrogen temperature. Temperature-programmed desorption of ammonia (NH3-TPD) and temperature-programmed reduction by H2 (H2-TPR) were performed with a Micromeritics AutoChem 2910 apparatus. 

For this purpose, all three catalyst supports were initially synthesized by a chemical vapor deposition (CVD) process and thereafter, using a wet impregnation method, loaded with cobalt as the active component for FTS. The as-synthesized Co/nanocatalysts were then characterized by applying electron microscopic analysis as well as temperature-programmed desorption, chemi- and physisorption measurements, thermogravimetric analysis, and inductively coupled plasma... 

Katada, N., Igi, H., Kim, J.H., and Niwa, M. (1997) Determination of the acidic properties of zeolite by theorecti-cal analysis of temperature programmed desorption of ammonia based on adsorption equilibrium. J. Phys. Chem. B, 101, 5969-5977. 

Temperature programmed desorption (TPD) is an experimental technique to measure surface kinetic parameters. The most straightforward analysis of TPD is due to Redhead [331], Assuming that the surface has some fractional coverage 0 of adsorbed A molecules, the desorption rate of A from the surface r(j (1/s) is taken to be... 

The surface structure and acid sites of alumina-supported molybdenum nitride catalysts have been studied using temperature-programed desorption (TPD), and reduction (TPR), diffuse reflectance infrared spectroscopy, and X-ray diffraction (XRD) analysis. The nitride catalysts were prepared by the temperature-programmed reaction of alumina-supported molybdenum oxide (12.5% and 97.1%) with NH3 at temperatures of 773, 973, and 1173 K. TPR and XRD analyses showed that y-Mo2N was already formed at 973 K. On the basis of NH3-TPD measurements and IR spectroscopy, it was found that Lewis acid sites were predominant over Bronsted acid sites on the surface of Mo2N/A1203. 

Two amorphous Si02-Al203 (ASA) supports with different Si/Al-ratios were used. One ASA had a Si/Al ratio of 2.5 (Engelhard, BET surface area 320 m2/g, pore volume 0.50 ml/g), the other of 11.3 (Ketjen, HA 100 5P, 355 m /g, 0.59 ml/g). The supports and corresponding catalysts are further coded ASA [. ], where. represents the above mentioned Si/Al ratio. For both supports, the number of acid sites was determined with the combination of thermographic analysis and temperature programmed desorption of isopropylammine29. The number of acid sites was 1.2 mmol/g for ASA [2.5] and 0.28 mmol/g for ASA [11.3], See Table 1. 

Temperature-programmed desorption (or decomposition) with quantitative analysis of gas-phase products (usually by mass spectrometry) has been used to help identify the ligands bonded to a metal in a supported complex. Complications such as reaction of desorbed ligands (e.g., CO) with support groups (e.g., OH) may complicate interpretation of the data (Brenner, 1986). 

Finally, new methods of analysis have recently been developed that may allow characterization of single atoms on surfaces such as atomic force microscopy.9 In certain cases, in situ experiments can be done such as the study of electrodes, enzymes, minerals and biomolecules. It has even been shown that one atom from a tip can be selectively placed on a desired surface.10 Such processes may one day be used to prepare catalysts that may enhance selectivity. Other methods that show promise as regards detection of surface catalytic intermediates are temperature programmed desorption techniques.11 Selective poisoning of some surface intermediates with monitoring via temperature programming methods may also allow the preparation of more selective catalysts. 

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