Gas physisorption is an experimental technique based on equilibrium Van der Waals interactions between gas molecules and solid particles, that quantifies the specific surface area (SSA), pore size distribution (PSD), and pore volume of solids and powders. The performance of catalysts, absorbents, chromatography column materials, and polymer resins depends on these morphological properties. Here we introduce the basic principles and procedures of physical adsorption, especially nitrogen physisorption, as a guide to students and researchers unfamiliar with the field. The Brunauer‐Emmett‐Teller theory (BET) is a common approach to estimate SSA that extends the Langmuir monolayer molecular adsorption model to multilayer layers. It relies on an equilibrium adsorption isotherm, measured at the normal boiling point of the adsorbate, eg, 77 K or 87 K for N2 and Ar, respectively. Web of Science indexed 45 400 articles in 2016 and 2017 that mentioned N2 adsorption porosimetry—BET and BJH (Barrett‐Joyner‐Halenda) keywords. The VOSViewer bibliometric tool grouped these articles into four research clusters: adsorption, activated carbon in aqueous solutions for removal of heavy metal ions; synthesis of nanoparticles and composites; catalysts performance in oxidation and reduction processes; and photocatalytic degradation with TiO2. According to the literature, the accuracy of the density function theory (DFT) method is higher than with the BJH theory and it is more reliable.

Any vessel in which solids are transported upward by a gas stream and then recycled to the bottom may be classified as a Circulating Fluidized Bed (CFB). We describe possible CFB operating regimes in the context of this broad classification and highlight commercial processes that employ CFB technology and potential applications. Process design and development require a fundamental understanding of gas and solids hydrodynamicssolids hold-up, mixing and velocity distribution. We discuss techniques used to measure solids mass flux, which is a critical parameter for both design and control. In the last decade, significant research efforts have been devoted to new experimental techniques to measure both gas and solids spatial and temporal distribution. We list these techniques and detail the different modelling approaches that have emerged based on the new data. Characterization of the data is still incomplete and the available models require further refinement to reliably predict the effect of scale, operating conditions and particle characteristics on hydrodynamics. N'importe quel contenant dans lequel des particules sont emportks dans la direction ascendante par un courant gazeux puis recyclkes par le bas peut Stre class6 c o m e un Lit Fluidisk Circulant (LFC). Nous dkrivons les rkgimes possibles des op6rations dans ces LFC en tenant compte de cette dkfinition ktendue et les prockddcs industriels existants et potentiels qui utilisent cette technologie des LFC. La conception et le dkveloppement des proctklks exigent une comprkhension fondamentale des hydrodynamics du gaz et des particulesrktention de solides, degrk de mklange et distribution des vitesses. Nous discutons les diffkrentes techniques utiliskes pour mesurer le taux de circulation de solide qui est un paramttre critique pour aussi bien le design que le contr6le. Durant le dernitres mks, un effort significatif'de recherche a kt6 consenti au dkveloppement de nouvelles techniques exp6rimentales pour mesurer les distributions temporelle et spatiale des diffkrentes caractkristiques du gaz et du solide. Nous reportons ces techniques et nous dktaillons le diffkrentes approches de modklisation qui ont kt6 introduites en se basant sur ces nouvelles donnks.La caradrisation de ces donnks est encore incompltte et les modkles existants doivent Stre encore raflids afin de pddire ad6quatement les effets d'khelle, des conditions @ratoires et des mactkristiques des particules sur I'hydrodynamique.

Chemical Looping Combustion technology involves circulating a metal oxide between a fuel zone where methane reacts under anaerobic conditions to produce a concentrated stream of CO 2 and water and an oxygen rich environment where the metal is reoxidized. Although the needs for electrical power generation drive the process to high temperatures, lower temperatures (600-800 C) are sufficient for industrial processes such as refineries. In this paper, we investigate the transient kinetics of NiO carriers in the temperature range of 600 to 900 C in both a fixed bed microreactor (WHSV ¼ 2-4 g CH 4 /h/g oxygen carrier) and a fluid bed reactor (WHSV ¼ 0.014-0.14 g CH 4 /h per g oxygen carrier). Complete methane conversion is achieved in the fluid bed for several minutes. In the microreactor, the methane conversion reaches a maximum after an initial induction period of less than 10 s. Both CO 2 and H 2 O yields are highest during this induction period. As the oxygen is consumed, methane conversion drops and both CO and H 2 yields increase, whereas the CO 2 and H 2 O concentrations decrease. The kinetics parameter of the gas-solids reactions (reduction of NiO with CH 4 , H 2 , and CO) together with catalytic reactions (methane reforming, methanation, shift, and gasification) were estimated using experimental data obtained on the fixed bed microreactor. Then, the kinetic expressions were combined with a detailed hydrodynamic model to successfully simulate the comportment of the fluidized bed reactor.

Methyl methacrylate (MMA) is a specialty monomer for poly methyl methacrylate (PMMA) and the increasing demand for this monomer has motivated industry to develop clean technologies based on renewable resources. The dominant commercial process reacts acetone and hydrogen cyanide to MMA (ACH route) but the intermediates (hydrogen cyanide, and acetone cyanohydrin) are toxic and represent an environmental hazard. Esterification of methacrylic acid (MAA) to MMA is a compelling alternative together with ethylene, propylene, and isobutene/t-butanol as feedstocks. Partially oxidizing isobutane or 2-methyl-1,3-propanediol (2MPDO) over heteropolycompounds to MAA in a single-step is nascent technology to replace current processes. The focus of this review is on catalysts and their role in the development of processes herein described. Indeed, in some cases remarkable catalysts were studied that enabled considerable steps forward in both the advancement of catalysis science and establishing the basis for new technologies. An emblematic example is represented by Keggin-type heteropolycompounds with cesium and vanadium, which are promising catalysts to convert isobutane and 2MPDO to MAA. Renewable sources for the MMA or MAA route include acetone, isobutanol, ethanol, lactic, itaconic, and citric acids. End-of-life PMMA is expected to grow as a future source of MMA.

Databases catalogue the corpus of research literature into scientific categories and report classes of bibliometric data such as the number of citations to articles, the number of authors, journals, funding agencies, institutes, references, etc. The number of articles and citations in a category are gauges of productivity and scientific impact but a quantitative basis to compare researchers between categories is limited. Here, we compile a list of bibliometric indicators for 236 science categories and citation rates of the 500 most cited articles of each category. The number of citations per paper vary by several orders of magnitude and are highest in multidisciplinary sciences, general internal medicine, and biochemistry and lowest in literature, poetry, and dance. A regression model demonstrates that citation rates to the top articles in each category increase with the square root of the number of articles in a category and decrease proportionately with the age of the references: articles in categories that cite recent research are also cited more frequently. The citation rate correlates positively with the number of funding agencies that finance the research. The category h-index correlates with the average number of cites to the top 500 ranked articles of each category (R2=0.997). Furthermore, only a few journals publish the top 500 cited articles in each category: four journals publish 60% (σ=±20%) of these and ten publish 81% (σ=±15%).

Thermogravimetric analysis (TGA) is a quantitative analytical technique that monitors the mass of a sample from 1 mg to several g as a furnace ramps temperature to as high as 1600°C under a stable or changing gas flow. The first gravimetric test was in 27 BC when Vitruvius measured limestone's change of mass as it calcined to lime. In modern chemical engineering, researchers apply the technique to derive conversions, kinetics, and mechanisms for any process with a change of mass by isothermal, non‐isothermal, and quasi‐isothermal methods. The mass drops as the sample decomposes, volatile compounds evaporate, or the oxidation state decreases, while in reactive environments (with O2, for example), the mass of transition metals may increase. TGA is incapable of detecting phase transitions, polymorphic transformations, or reactions for which mass is invariant. DSC or DTA couple with TGA to help deconvolute a DSC plot by separating physical changes from chemical changes. Evolved gas analysis techniques monitor the gaseous products exiting the TGA furnace on‐line as the temperature ramps. A bibliometric map of keywords from articles citing TGA indexed by Web of Science in 2016 and 2017 identified five research clusters: nanoparticles, performance, and films; crystal structures, acid, and oxidation; composites, nanocomposites, and mechanical properties; kinetics, pyrolysis, and temperature; and adsorption, water and wastewater, and aqueous solutions. This review provides an overview of the basic principles of modern TGA.

X-ray diffraction (XRD) analysis identifies the long-range order (ie, the structure) of crystalline materials and the short-range order of non-crystalline materials. From this information we deduce lattice constants and phases, average grain size, degree of crystallinity, and crystal defects. Advanced XRD provides information about strain, texture, crystalline symmetry, and electron density. When radiation impinges upon a solid, coherent scattering of the radiation by periodically spaced atoms results in scattered beams that produce spot patterns from single crystalline samples and ring patterns from polycrystalline samples. The pattern, intensities of the diffraction maxima (peaks or lines), and their position (Bragg angle θ or interplanar spacing d hkl ), correlate to a specific crystal structure. In 2016 and 2017 close to 100 000 articles mention XRD-more than any other analytical technique, and it was the top analytical technique of researchers that published in Can. J. Chem. Eng. A bibliographic analysis based on the Web of Science groups articles referring to XRD into five clusters: the largest cluster includes research on nanoparticles, thin films, and optical properties; composites, electro-chemistry, and synthesis are topics of the second largest cluster; crystal morphology and catalysis are next; photocatalysis and solar cells comprise the fourth largest cluster; and, waste water is among the topics of the cluster with the least number of occurrences. Researchers publishing in Can. J. Chem. Eng. focus most of the XRD analyses to characterize polymers, nanocomposite materials, and catalysts. K E Y W O R D Scrystallinity, Debye-Scherrer method, limit of quantification, nanoparticle, XRD

No abstract