Perchlorate and tetrafluoroborate have been determined at low concentrations by precipitation titration with tetraphenylarsonium chloride, the appropriate anionselective electrodes being used to follow the course of the titration potentiometrically. A low temperature, 2°, was employed to sharpen the titration curves, thus resulting in greater accuracy and lower limits of analysis. As little as 0.05 mmol of perchlorate and 0.25 mmol of tetrafluoroborate have been determined to within 1% relative accuracy. These limits could easily be extended by a factor of 10 by using a miniaturized titration apparatus. © 1969.