A 6sulfanilic acid of known concentration was prepared by diazotization and used as eruch. Previously the solid compound was isolated and weighed out for each run. The explosive character of the diazo salt made the use of a solution much more convenient. The reproducibility of the data was unaffected by the change and remained of the order 570, with the greatest spread being 770. In those cases where quenching of the reaction mixture in sulfuric acid resulted in a precipitate-( a.g., calcium sulfate)-it waa merely necessary to centrifuge the sample to obtain a clear supernatant liquid which could be used for the spectrophotometric estimation of the dye. The metals were added as their chloride or sulfate salts.Rate Constants.-The rate constants are pseudo first-order rate constants obtained from the expression:The constant kl incorporates the product kn(RX*+), where (RNz+) is a constant excess of the diazonium salt and kz is the second order rate constant. This diazonium salt was present in fifty-fold excess. The concentration of the diazonium salt was 5.0 X 10-8 M while that of the phenol was 9.26 X 10-6 M in all of the runs.The second-order rate constants may be obtained from the relationship between the two rate constants and the concentration of diazonium salt.