Methods and Procedures for Catalyst Characterization

The sections in this article are Introduction Catalyst Preparation Preparation of the Primary Solid Deposition Impregnation Impregnation by soaking, or with an excess of solution [2] Impregnation by soaking, or with an excess of solution Dry or pore-volume impregnation Incipient wetness impregnation Deposition by selective reaction with the surface of the support Impregnation by percolation Co-impregnation Successive impregnation Ion exchange Gas-phase deposition Solid–solid reactions Wash coat Precipitation and Coprecipitation Synthesis of Zeolites and Related Materials Precipitation–Deposition Gel Formation and Related Processes Selective Removal Pillared Layer Compounds Treatment of Intermediate Solids or Precursors Activation of the Precursor (see Chapter Reactions During Catalyst Activation) Activation of the Precursor (see Chapter ) Forming Methods Powder: Preparation, Crushing and Grinding Forming by Crushing Spray Drying Oil Drop Granulation Tabletting Extrusion Stability During Handling and Storage Passivation Protection by an Inert Gas Protection by a condensed phase Characterization of Surface Properties by Adsorption Methods Methodology Static Methods Dynamic Methods Desorption Precautions Categories of Catalysts Metals [13-16] Metals Acidic Amorphous Oxides and Zeolites Sulfides Fine Structure of Catalysts [12, 20] Fine Structure of Catalysts Surface Structure and Chemical Composition Surface Structure and Topography Electron Microscopy Conventional Transmission Electron Microscopy (CTEM) Techniques Related to CTEM Dark-field methods High-resolution electron microscopy (HREM) Reflection electron microscopy (REM) and reflection high energy electron diffraction (RHEED) Scanning electron microscopy (SEM) [21] Scanning electron microscopy (SEM) Scanning transmission electron microscopy (STEM) [22] Scanning transmission electron microscopy (STEM) Selected area diffraction (also called: microdiffraction) X-Ray and Neutron Methods for Structure Determination X-Ray Diffraction and Diffusion Radial Electron Distribution (RED) Extended X-Ray Absorption Fine Structure (EXAFS) [20] Extended X-Ray Absorption Fine Structure (EXAFS) Techniques Related to EXAFS Neutron Diffraction Ion Scattering Techniques Electron State and Local Environment of Elements [20-31] Electron State and Local Environment of Elements Nuclear Magnetic Resonance (NMR) [20] Nuclear Magnetic Resonance (NMR) Electron Spin Resonance (ESR) Mössbauer Spectroscopy (see Chapter Gamma Spectroscopy) Mössbauer Spectroscopy (see Chapter ) Vibrational Spectroscopies Transmission Infrared Spectroscopy (IR) Infrared Emission Spectroscopy Diffuse Reflectance Spectroscopy (DRS) Internal Reflectance Spectroscopy Photoacoustic Spectroscopy (PAS) Others Raman Spectroscopy Inelastic Neutron Scattering Spectroscopy (INS) Electron Spectroscopies Photoelectron Spectroscopy (XPES, UPES) Auger Electron Spectroscopy (AES) Determination of Spatial Distribution of Elements Analytical Electron Microscopy Energy Dispersive X-Ray Spectroscopy (EDS, EDX) Electron Energy Loss Spectroscopy (EELS) Scanning Auger Microscopy (SAM) Secondary Ion Mass Spectroscopy (SIMS) Ion Beam Techniques Depth Profiling Catalytic Properties Reactor Types and Measurement Methods [38] Reactor Types and Measurement Methods Plug-Flow Reactor Continuous Stirred-Tank Reactor (CSTR) Fluidized-Bed Reactor Batch Reactor Discontinuous Flow Reactor Reactant Introduction Methods Typical Experimental Parameters Used in Catalyst Testing Reactor Reactants Catalyst Problems of Heat and Mass Transfer Kinetic Analysis [39-47] Kinetic Analysis Determination of the Reaction Rate Rate Equations Selection of a Suitable Form of the Rate Equation and Evaluation of Constants Heat and Mass Transfer Effects (see Part 6) Internal Mass and Heat Transfer External Mass and Heat Transfer Inhibition of Catalytic Action Identification of the Inhibiting Substances Identification of the Mode of Action of the Inhibiting Substances Characterization of Catalysts with Respect to Their Response to IS Poisons Inhibitors Fouling Agents Deactivation of Catalysts and Time-Dependent Effects Deactivation: Overall Characterization Physicochemical Characterization in Deactivation Studies Accelerated Tests Regeneration Preliminary Treatment Removal of Inhibitory Substances (IS) Removal of Coke Removal of Foulants Redispersion General