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The tuning of selectivity by changing the flow rate has been investigated in HPLC: two columns with different retention characteristics were coupled in series via a T-piece and the relative retention of components chromatographed on the system were changed by varying the individual flow rates in the coupled columns. The flow rate alteration was performed by adding a second flow after the first column.The flow rate ratio necessary for optimum resolution can be easily calculated on the basis of the capacity factors measured on the individual columns. The performance of this method for adjusting selectivity has been demonstrated by using different column combinations to separate several mixtures containing chlorophenols, nitroaromatic compounds, and aromatic hydrocarbons.