Chelate-exchange titrimetry has been applied to the determination of μg amounts of some metal 8-quinolinates in benzene. The titrant was a standard solution of diphenylthiocarbazone in benzene. Accuracy and precision were good in the cases of Pb, Cu(II), Cd, Zn, and In. Very slow reaction rates made titrations of Ag and Ni impracticable, and chelate-exchange was negligible in the case of Co(II). A new titrimetric method is also shown to be precise and accurate for the determination of free 8-quinolinol in benzene; the titrant was a standard solution of Cu(NO3)2 in ethanol.