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A dedicated CPC prototype permits direct flow pattern visualization in the partition cells of a CPC column. It was used to understand “flooding”, a frequent phenomenon associated with large injections. A general strategy was developed to optimize the injection step in the framework of a particular preparative separation: the purification of 5-n-alkylresorcinols from a wheat bran lipid extract on a several hundred milligram scale. The construction of the “mobile phase/stationary phase/sample” pseudo ternary diagram characterizes the effect of the injected solution on mobile and stationary phases. The position of the binodal curve maximum indicates if the biphasic system is “robust” towards a large injection or not, and can be used for optimum mass load determination.