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The influence of change in water cocatalyst concentration on polymer yield and composition, and on reaction rate was investigated in the benzene‐ferric chloride system. For short reaction times, polymer yield passes through a maximum at a H2O/FeCl3 molar ratio of 1. The most rapid rate of hydrogen chloride evolution was observed at this same ratio. The data suggest that ferric chloride monohydrate constitutes the active catalyst‐cocatalyst complex. With more prolonged reaction times, the yield maximum shifted to lower values of H2O/FeCl3, accompanied by a progressive increase in polymer yield. As evidenced by the C/(H + Cl) atomic ratio, p‐polyphenyl formation is favored by short reaction times at H2O/FeCl3 ratios of 0, 1, and 2. Longer reaction times, gave C/(H + Cl) ratios greater than 1.5 for the polymer, indicating the presence of polynuclear structures. An increase in chlorine content attended the rise in C/(H + Cl) ratio. Interpretations of the data are presented.