Fluid catalytic cracking (FCC) is the major conversion process used in oil refineries to produce valuable hydrocarbons from crude oil fractions. Because the demand for oil-based products is ever increasing, research has been ongoing to improve the performance of FCC catalyst particles, which are complex mixtures of zeolite and binder materials. Unfortunately, there is limited insight into the distribution and activity of individual zeolitic domains at different life stages. Here we introduce a staining method to visualize the structure of zeolite particulates and other FCC components. Brønsted acidity maps have been constructed at the single particle level from fluorescence microscopy images. By applying a statistical methodology to a series of catalysts deactivated via industrial protocols, a correlation is established between Brønsted acidity and cracking activity. The generally applicable method has clear potential for catalyst diagnostics, as it determines intra- and interparticle Brønsted acidity distributions for industrial FCC materials.

Raman microscopy has been applied to study the preparation of shaped Mo/Al2O3 catalysts. The speciation of different Mo complexes over γ-Al2O3 support bodies was followed in time after pore volume impregnation with aqueous solutions containing different Mo complexes. The addition of NO3 -to the impregnation solutions allows for a quantitative Raman analysis of the distribution of different complexes over the catalyst bodies as this ion can be used as an internal standard. After impregnation with an acidic ammonium heptamolybdate (AHM) solution, the strong interaction between Mo7O24 6-and Al2O3 results in slow transport of this complex through the support and extensive formation of Al(OH)6Mo6O18 3-near the outer surface of the support bodies. This may be prevented by decreasing the interaction between Mo and Al2O3. In this way, transport is facilitated and a homogeneous distribution of Mo is obtained on a reasonable time scale. A decrease in interaction between Mo and Al2O3 can be achieved by using alkaline impregnation solutions or by the addition of complexing agents, such as citrate and phosphate, to the impregnation solution. In general, time-resolved in situ Raman microscopy can be a valuable tool to study the physicochemical processes during the preparation of supported catalysts.

Temperature dependent luminescence and luminescence lifetime measurements are reported for nanocrystalline ZnS:Cu 2+ particles. Based on the variation of the emission wavelength as a function of particle size (between 3.1 and 7.4 nm) and the low quenching temperature (T q ¼ 135 K), the green emission band is assigned to recombination of an electron in a shallow trap and Cu 2+ . The reduction in lifetime of the green emission (from 20 ms at 4 K to 0.5 ms at 300 K) follows the temperature quenching of the emission. In addition to the green luminescence, a red emission band, previously only reported for bulk ZnS:Cu 2+ , is observed. The red emission is assigned to recombination of a deeply trapped electron and Cu 2+ . The lifetime of the red emission is longer (about 40 ms at 4 K) and the quenching temperature is higher. r

The physicochemical processes that occur during the preparation of CoMo–Al2O3 hydrodesulfurization catalyst bodies have been investigated. To this end, the distribution of Mo and Co complexes, after impregnation of γ‐Al2O3 pellets with different CoMoP solutions (i.e., solutions containing Co, Mo, and phosphate), was monitored by Raman and UV‐visible‐NIR microspectroscopy. From the speciation of the different complexes over the catalyst bodies, insight was obtained into the interaction of the different components in the impregnation solution with the Al2O3 surface. It is shown that, after impregnation with a solution containing H2PMo11CoO405−, the reaction of phosphate with the Al2O3 leads to the disintegration of this complex. The consecutive independent transport of Co2+ complexes (fast) and Mo6+ complexes (slow) through the pores of the Al2O3 is envisaged. By the addition of extra phosphate and citrate to the impregnation solution, the formation of the desired heteropolyanion can be achieved inside the pellets. Ultimately, the H2PMo11CoO405− distribution could be controlled by varying the aging time applied after impregnation. The power of a combination of spatially resolved spectroscopic techniques to monitor the preparation of supported catalyst bodies is illustrated.