Optimal design of a liquid‐liquid settler requires experimental investigation on phase separation behavior of the used material system under the same operating conditions as in the technical application. Performing these experiments and evaluating the obtained data is highly time‐consuming. To reduce manual effort, the procedure was largely automated. In this work, the experimental setup, the automated procedure, and its validation results at various operating temperatures are presented. The results show the suitability of the automated procedure and the influence of temperature on phase separation behavior of the liquid‐liquid system 1‐octanol/water.