Using temperature programmed desorption tpd or thermal desorption spectrometry tds, the surface composition of a substrate can be characterized. The application of flash desorption spectroscopy to chemical reactions on surfaces. Temperature programmed desorption is a powerful tool for materials analysis based on the release of impurities to the gas phase when a specimen is heated. Temperature programmed desorption system consisting of a hiden 200 amu rga, a molybdenum sample holder with a selfassemble monolayer of dodecanethiol grown on a thin film of silver on silicon substrate, and a thermocouple mounted on a tungsten spring to read the temperature on the surface of the sample. Temperatureprogrammed desorption mass spectrometry tpdms is discussed with reference to studies of modified pyrogenic oxides. The construction of a modified tpd instrument from. This study evaluated the application of a versatile optical technique to study the adsorption and desorption of model adsorbates representative of volatile polar acetone and nonpolar propane organic compounds on a model carbonaceous surface under ultra high vacuum uhv conditions. During temperatureprogrammed desorption tpd, a molecule is adsorbed on a solid surface, the temperature is ramped linearly with time and the rate of desorption is measured. Temperature programmed desorption university of toronto. Analysis of temperature programmed desorption tpd data for the characterization of catalysts containing a distribution of adsorption sites patrick j. Temperature programmed desorption tpd experimental setup.
The temperature programmed desorption is easily performed by ramping the sample temperature at 10cminute to 500c. This part of the work was done using reference catalysts of the catalysis society of japan. Temperature programmed desorption study of c6h12zr0001. A statistical rate theory approach article pdf available in the journal of chemical physics 106. Temperatureprogrammed desorption studies of nh3 and h2o. Download hires imagedownload to mspowerpointcite this. Temperature programmed desorption spectra of systems with concentration gradients in the solid lattice.
This technique is performed by linearly increasing the temperature of a sample while measuring the partial pressures of the desorbing gas species. Temperatureprogrammed desorption mass spectrometry tpdms is. Pdf the grammed desorption technique, widely used in the fields of surface science and catalysis, was adapted to. This type of analysis allows the user to investigate the kinetics of adsorption through the dissociation of gases adsorbed on surfaces. Simulating temperature programmed desorption of oxygen on pt111 using dft derived coverage dependent desorption barriers kitchinhubkitchingroup43. The unimolecular decomposition of alkoxide groups was studied. Temperature programmed desorption distribution of acid sites nh 3tpd which sites are present. Abstract in a typical temperatureprogrammed desorption tpd experiment on a supported metal catalyst, a small amount of catalyst 10200 mg is contained in a reactor that can be heated by a furnace.
Temperatureprogrammed desorption tpd of bases is again designed to furnish information on both the density and strength of acid sites on the surface of a solid see also chapter 17. The results showed the strong correlation between optical differential reflectance odr and adsorbate. The theoretical equation for the tpd with free readsorption of ammonia was then. Temperatureprogrammed desorption tpd is one of the powerful. It is a good rule of thumb that the end temperature during the tpd not exceed the maximum temperature used in the preparation of the sample. When experiments are performed using welldefined surfaces of singlecrystalline samples in a continuously pumped ultrahigh vacuum uhv chamber, then this experimental technique is often also referred to as thermal desorption spectroscopy or thermal. Independent of the ice morphology, the desorption of o2 is found to follow 0thorder kinetics. An inert gas, usually helium at atmospheric pressure, flows over the catalyst. Unlimited viewing of the articlechapter pdf and any associated supplements and figures.
Theoretical parameterfree analysis model for temperature. Principles, instrument design, and demonstration with naalh4 showing 14 of 5 pages in this article. It has been established3 that this equation, which is based on absolute rate theory,4 does not give explicitly the coverage and temperature dependence necessary to predict tpd spectra in several important sys. Tpd in the temperature range between 300 and 500 k results in desorption profiles of different intensities depending on the kind of cation and the aluminium content of zeolites. The adsorption of c2h6, and the cycloparaffins c3h6, c6h12, and c8h16 on ru001 at 80 k has been studied using leed, temperature programmed desorption, and. Following pretreatment to obtain a reduced catalyst, a gas is adsorbed on the surface, usually by pulse. Temperature programmed desorption spectra of systems with. Thermal desorption researchers have demonstrated that contaminant removal is highly dependent on. Pdf temperature programmed desorption of carbon dioxide. Ying tang, tianlan yan, bo shen, huafeng li, ayodeji jeje. Using temperatureprogrammed desorption tpd, we have investigated the interaction of carbon dioxide with alkalimetal cationexchanged faujasite type zeolites lsx, x and y. The influence of the experimental conditions of the tpd temperatureprogrammed desorption of ammonia on the measurement of acidity of mordenites and y zeolites was studied.
Temperatureprogrammed desorption of ammonia tpda from the silicoaluminophosphates hsapo5 a and. Measurements of acidic property of zeolites by temperature. Journal of thermal analysis and calorimetry 2016, 125 3, 12171224. The ami chemi family of instruments combines a variety of temperatureprogrammed techniques, including. Simple theoretical models are presented in order to allow an approximate analytical treatment of tpdms data. In order to overcome a serious disadvantage of the method i. The results showed that functionalitiesdefects sites on nanotube surfaces play an important role on the interaction between. Modern methods in heterogeneous catalysis research. The application of temperatureprogrammed desorption tpd to the characterization of porous, oxide catalysts is discussed. Temperatureprogrammed desorption for the characterization of. No x conversion % 300 400 500 600 700 800 0 25 50 75 100 greenhalg et al. The rates of desorption are plotted versus either temperature or time select with buttons for three heating rates 1, 3. Temperature programmed desorption tpd is the method of observing desorbed molecules from a surface when the surface temperature is increased. Temperatureprogrammed desorption mass spectrometry tpdms.
Temperature programmed desorption an overview sciencedirect. Thermal desorption spectroscopy tds, tpd tds system. It is a highperformance gas separation method that combines the simplicity of gaschromatographic separation with the advantages of gasspecific adsorption. Made by faculty at the university of colorado boulder, department of. Temperatureprogrammed desorption of ammonia on zeolites. Article information, pdf download for temperatureprogrammed desorption mass. It is used to determine the relative coverage and activation. Wed like to understand how you use our websites in order to improve them. View temperatureprogrammed desorption research papers on academia. The temperature of the first chamber is continuously monitored by means of 8 a thermocouple. Temperature programmed desorption tufts university. Temperature programmed desorption tpd is an experimental technique used to measure the desorption kinetics of molecules from surfaces. Initial adsorbed co2 could be assigned to carbonate species in different environments by drift spectroscopy.
Temperatureprogrammed desorption tpd of carbon dioxide. The desorption peaks were identified and the significance of readsorption of ammonia was pointed out for the first time. Explains temperatureprogrammed desorption tpd and solves the equations for firstorder desorption. Temperatureprogrammed desorption tpd thermal desorption spectroscopy tds sven l. The hiden tpd workstation is a complete experimental system for uhv temperature programmed desorption tpd studies. Adsorb fixed amount of molecules at surface gradually increased heating of surface leads to desorption desorbed particles analyzed by pressure gauge mass spectrometer information on.
Barrie department of chemical engineering, university of cambridge, pembroke street, cambridge cb2 3ra, u. The tpd workstation is provided with a multiport uhv chamber with a heated sample stage combined with a high precision triple filter analyser with digital pulse ion counting detector to offer users high level sensitivity and time resolution the hiden tpd workstation is a fullyfledged experimental system for uhv temperature programmed desorption tpd analysis. This study evaluated the environmental applications of carbon nanotubes through the adsorption and desorption of representative environmentally relevant adsorbates. Temperature programmed desorption tpd has been used to investigate the behavior of cyclohexane c6h12 on zr0001 and the effects of 500 ev electron bombardment on its desorption characteristics. Notes temperatureprogrammed desorption for catalyst. Storage of hydrogen in singlewalled carbon nanotubes nature. The principles and requirements of tpd are explained and the different components of a generic tpd apparatus are described. Temperatureprogrammed desorption wolfram demonstrations. Temperatureprogrammed desorption tpd is one of the most straightforward surface science experiments for the determination of the thermodynamic and kinetic parameters of a reaction. A temperature programmed desorption tpd technique has been developed especially in the field of catalysis, because the technique allows one to study the interaction of reaction gases with solid surfaces, thereby being a powerful tool for both the evaluation of active sites on catalyst surfaces and the understanding of the mechanisms of catalytic reactions including.
Temperatureprogrammed desorption mass spectrometry. Tpd for characterizing the acid sites on oxide surfaces. A temperature programmed desorption technique for investigation of practical catalysts. An introduction to direct temperature programmed desorption. The results were applicable to the measurements of the strength and the number of acid sites of zeolites. Temperature programmed desorption of carbon dioxide for activated carbon supported nickel oxide. Temperatureprogrammed desorption tpd of carbon dioxide on. Tpd infrared spectroscopymass spectrometrytemperature. Schroeder and michael gottfried june 2002 temperatureprogrammed desorption tpd techniques are important methods for the determination of kinetic and thermodynamic parameters of desorption processes or decomposition reactions. Temperature programmed desorption mass spectrometry used. Pdf a temperatureprogrammed desorption technique for. A thermal desorption study of the surface interaction between tritium and type 316 stainless steel. Temperature programmed desorption, reduction, oxidation. The overall view of the tpd of ammonia to measure the acidic property of zeolites is described.
The temperatureprogrammed desorption of oxygen from an. Numerical modeling of thermal desorption mass spectroscopy tds for the study of. Analysis of temperature programmed desorption tpd data. Surface area measurement from temperatureprogrammed desorption data temperatureprogrammed desorption experiments offer a means of obtaining quantitative information about the metallic surface area of supported metal catalysts along with a qualitative measure of the variation in strength of adsorption for different sites on the surface. Elementar has invented the patented direct temperature programmed desorption direct tpd technology. Temperature programmed desorption study of water adsorbed. Successive temperatureprogrammed desorption tpd after temperatureprogrammed reduction tpr combined tprtpd was performed in order to characterize supported platinum catalysts ptsio 2, ptal 2 o 3, ptzro 2 and pttio 2 as well as to judge the validity of the apparent tpr profiles. Surface area measurement from temperatureprogrammed. C, 20, 117, 666142, we proposed a model combining dft methods with microkinetics.
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