Split‐Plot Experimental Designs for Combinatorial and High‐Throughput Experimentation

Abstract

In the last few years, high-throughput reactors have small received significant attention due to the potential they offer for fast material development. While many experimental design techniques are proposed, statistical issues related to experimentation in this type of equipment are emerging. One of the experimental design techniques needed is the split-plot approach, given the randomization restrictions imposed by the equipment. This paper presents the use of split-plot experimental designs in a high-throughput reactor. We discuss the unique error structure of these designs and the special statistical analysis that considers two different types of errors. A case study in the Dow Chemical Company is presented. The main advantage of the split-plot approach related to high throughput is that reactor-well utilization can be maximized, while randomization restrictions can be addressed correctly and simultaneously. The results obtained indicate the success of this strategy in maximizing the chance of detecting a lead and making the right conclusions, which is of key importance given the speed of data generation of high-throughput reactors.

Combinatorial and High‐Throughput Materials Science

“…A clear drawback is the large number of experiments to be carried out, which rapidly increases with the number of selected factors. Castillo et al [14] presented the use of a splitplot experimental design, developed for high-throughput studies of catalysts (see Figure 2 in Ref. [14]), but demonstrated this with only two catalysts.…”

“…Castillo et al [14] presented the use of a splitplot experimental design, developed for high-throughput studies of catalysts (see Figure 2 in Ref. [14]), but demonstrated this with only two catalysts. Here two levels of the parameters temperature (T) and pressure (p) were combined with the variation of two catalysts at two concentrations.…”

Recent advances and prospects of inkjet printing in heterogeneous catalysis

“…Several studies have been reported on the generation of catalyst libraries of multi-component catalysts for catalytic reaction explorations. [129][130][131][132] Among various techniques, inkjet printing has been reported to be a powerful tool for the rapid synthesis of catalyst nanomaterials. 94,133,134 Normally the catalyst species precursors are prepared in the form of inks and a variety of composition ratios can be produced by changing the gradient of designed patterns.…”

Kombinatorische und Hochdurchsatz‐Techniken in der Materialforschung

“…Ein offenkundiger Nachteil ist die große Zahl der auszuführenden Experimente, die mit der Anzahl der ausgewählten Parameter schnell ansteigt. Castillo et al [14] beschrieben die Verwendung eines experimentellen Split-Plot-Designs, das für HT-Studien an Katalysatoren (siehe Abbildung 2 in Lit. [14]) entwickelt wurde, demonstrierten dies jedoch anhand von nur zwei Katalysatoren.…”

“…Castillo et al [14] beschrieben die Verwendung eines experimentellen Split-Plot-Designs, das für HT-Studien an Katalysatoren (siehe Abbildung 2 in Lit. [14]) entwickelt wurde, demonstrierten dies jedoch anhand von nur zwei Katalysatoren. Hier werden zwei Werte der Parameter Temperatur (T) und Druck (p) mit der ¾nderung von zwei Katalysatoren in zwei Konzentrationen kombiniert.…”