Temperature Programmed Analytical OptionsTemperature Programmed Desorption (TPD)Temperature Programmed Reduction (TPR)Temperature Programmed Oxidation (TPO)Temperature programmed analyses are part of our suite of chemisorption options, used to investigate reduction, oxidation, desorption and decomposition as a function of temperature. Traditionally these have been applied to the catalysis sector where the understanding of surface reactions are fundamental to the development and regeneration of high efficiency systems. The use of these techniques is often extended to other sectors and applications, wherever the behaviour of oxidisable or reducible species is of importance or for the study and development of adsorbents and filter materials. Temperature programmed analyses at MCA Services are undertaken using our state-of-the-art Micromeritics AutoChem instrument, capable of analyses from sub-ambient temperature to 1100 °C. Furthermore, this instrument provides tremendous scope for accurate selection and control over analytical parameters such as gas flow rate, temperature ramp rate and temperature holding ranges. The instrument detector is always calibrated to match specific analytical parameters, ensuring the accurate calculation of specific active gas consumption.
Temperature Programmed Desorption (TPD)Temperature programmed desorption is used to study the temperature dependence and strength of interaction between a sample surface and a probe molecule. Typical probe molecules include H2, CO and NH3, although others, including vapours, can also be applied in order to investigate specific systems. Initial adsorption, either physical or chemical, is usually conducted at ambient temperature, although sub-ambient conditions can also be applied. The desorption process is then measured with steady increasing sample temperature under inert gas flow. Recording the temperature at which desorption occurs and accurately measuring the volume of gas desorbing allows for the determination of the number and strength of active adsorption sites on a sample surface. Temperature programmed desorption can also be extended to investigate sample materials when the adsorption / desorption processes are significant to performance, for example effectiveness and regeneration of adsorbents, filter materials and catalysts.
Temperature Programmed Reduction (TPR) Temperature programmed reduction is used to investigate the reducibility of a species and can be applied to metals and metal compounds such as oxides in both supported and un-supported forms. Historically very important to the study of catalysts, TPR can be applied to a wide variety of metallic and supported metallic species when reduction behaviour requires understanding. The analytical process involves heating a sample at a steady rate, to a maximum of 1100 °C, in a stream of reducing gas, typically low concentration hydrogen or carbon monoxide balanced with an inert carrier. Reduction of the sample is then recorded using a thermal conductivity detector (TCD) as the concentration of the reducing gas component falls as it is consumed during reduction of the sample. At MCA Services, the TCD is calibrated with respect to reducing gas concentration which allows for the calculation of active gas consumption during the reduction process. Results then include quantified graphical representations of the reduction process in relation to temperature and numerical reducing gas consumption data. TPR, therefore, provides important information regarding reduction temperature and gas consumption which can be extended to the identification of the number of reducible species and insight into the reduction sequence via intermediate species. This information is important to many process during application and regeneration and to the understanding of support materials, which can profoundly affect reduction behaviour.
Temperature Programmed Oxidation (TPO)Analogous to TPR, temperature programmed oxidation is applied to the study of oxidisable species on a material surface. The analytical process is very similar to that of TPR with oxygen replacing the reducing gas species in the carrier stream. Similar data is also obtained, the TCD again being accurately calibrated for oxygen consumption, allowing for the quantified determination of the number and extent of oxidisable species on the sample surface. Classic applications of TPO are within the catalysis and electro-catalysis sectors, whereby it is very useful for investigating coking during use for many processes involving hydrocarbons. TPO also can be applied to many systems when the process of oxidation is of importance, including stages of chemical product and process development in order to maximise efficiency and yield.
At MCA Services we have decades of experience in the analysis and characterisation of materials by chemisorption techniques and are always happy to discuss specific samples and applications. The flexibility of our analytical options combined with our expertise ensures that the most appropriate analytical test, or combination of tests, are selected for your particular sample, application and requirements. We also provide assistance with the interpretation of results and more information about these analytical options and the background operation and theory can be found on our YouTube channel.
MCA Services
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Temperature Programmed Analytical OptionsTemperature Programmed Desorption (TPD)Temperature Programmed Reduction (TPR)Temperature Programmed Oxidation (TPO)Temperature programmed analyses are part of our suite of chemisorption options, used to investigate reduction, oxidation, desorption and decomposition as a function of temperature. Traditionally these have been applied to the catalysis sector where the understanding of surface reactions are fundamental to the development and regeneration of high efficiency systems. The use of these techniques is often extended to other sectors and applications, wherever the behaviour of oxidisable or reducible species is of importance or for the study and development of adsorbents and filter materials. Temperature programmed analyses at MCA Services are undertaken using our state-of-the-art Micromeritics AutoChem instrument, capable of analyses from sub-ambient temperature to 1100 °C. Furthermore, this instrument provides tremendous scope for accurate selection and control over analytical parameters such as gas flow rate, temperature ramp rate and temperature holding ranges. The instrument detector is always calibrated to match specific analytical parameters, ensuring the accurate calculation of specific active gas consumption.
Temperature Programmed Desorption (TPD) Temperature programmed desorption is used to study the temperature dependence and strength of interaction between a sample surface and a probe molecule. Typical probe molecules include H2, CO and NH3, although others, including vapours, can also be applied in order to investigate specific systems. Initial adsorption, either physical or chemical, is usually conducted at ambient temperature, although sub-ambient conditions can also be applied. The desorption process is then measured with steady increasing sample temperature under inert gas flow. Recording the temperature at which desorption occurs and accurately measuring the volume of gas desorbing allows for the determination of the number and strength of active adsorption sites on a sample surface. Temperature programmed desorption can also be extended to investigate sample materials when the adsorption / desorption processes are significant to performance, for example effectiveness and regeneration of adsorbents, filter materials and catalysts.
Temperature Programmed Reduction (TPR)Temperature programmed reduction is used to investigate the reducibility of a species and can be applied to metals and metal compounds such as oxides in both supported and un-supported forms. Historically very important to the study of catalysts, TPR can be applied to a wide variety of metallic and supported metallic species when reduction behaviour requires understanding. The analytical process involves heating a sample at a steady rate, to a maximum of 1100 °C, in a stream of reducing gas, typically low concentration hydrogen or carbon monoxide balanced with an inert carrier. Reduction of the sample is then recorded using a thermal conductivity detector (TCD) as the concentration of the reducing gas component falls as it is consumed during reduction of the sample. At MCA Services, the TCD is calibrated with respect to reducing gas concentration which allows for the calculation of active gas consumption during the reduction process. Results then include quantified graphical representations of the reduction process in relation to temperature and numerical reducing gas consumption data. TPR, therefore, provides important information regarding reduction temperature and gas consumption which can be extended to the identification of the number of reducible species and insight into the reduction sequence via intermediate species. This information is important to many process during application and regeneration and to the understanding of support materials, which can profoundly affect reduction behaviour.
Temperature Programmed Oxidation (TPO) Analogous to TPR, temperature programmed oxidation is applied to the study of oxidisable species on a material surface. The analytical process is very similar to that of TPR with oxygen replacing the reducing gas species in the carrier stream. Similar data is also obtained, the TCD again being accurately calibrated for oxygen consumption, allowing for the quantified determination of the number and extent of oxidisable species on the sample surface. Classic applications of TPO are within the catalysis and electro-catalysis sectors, whereby it is very useful for investigating coking during use for many processes involving hydrocarbons. TPO also can be applied to many systems when the process of oxidation is of importance, including stages of chemical product and process development in order to maximise efficiency and yield.
At MCA Services we have decades of experience in the analysis and characterisation of materials by chemisorption techniques and are always happy to discuss specific samples and applications. The flexibility of our analytical options combined with our expertise ensures that the most appropriate analytical test, or combination of tests, are selected for your particular sample, application and requirements. We also provide assistance with the interpretation of results and more information about these analytical options and the background operation and theory can be found on our YouTube channel.