Split-Split-Plot Experimental Design in a High-Throughput Reactor

ABSTRACT

In the last few years, high-throughput (HT) reactors have received significant attention due to the potential for fast material development. Split-plot experimental design plays a critical role in this type of application given randomization restrictions often imposed by equipment constraints. A case study in a parallel polymerization reactor is presented.

KEYWORDS:

• combinatorial experimentation
• high-throughput experimental design
• randomization restrictions
• split-split-plot

ACKNOWLEDGMENTS

The author thanks Professor Soren Bisgaard for his feedback and encouragement to publish the work reported in this article.

Notes

¹Here, the designation well is used for individual reaction or synthesis chambers that are chemically isolated from other chambers and form the basic experimental unit of high-throughput experimentation.

²A module is a block of wells tied together by engineering constraints, such as a common pressure control unit or a common heater block.

³PPR is a registered trademark of Symyx Technologies, Santa Clara, California.

⁴ T = temperature, P = pressure, C = catalyst type, D = catalyst concentration.

⁵ز is used to represent a fixed effect that is the sum squares of the model component associated with the particular factor divided by its degrees of freedom: is the fixed effect for catalyst type (C).