The use of a specially designed coulometer and a high accuracy cou lometric circuit re s ulted in tllf' accurate mea surem e nt of the electrochemical equivalent and atomic weight of zinc. The experi· mental (,onditions to make possible the final preci se and accurate measul'e ments were ('stablished. Th,.,,· includ,. a study of mechanical lo" ses from the anode during the e lectrolys is and th e co rrosion of ,inc in various media '''ed in the determination. Th e effects of both of these so urc es of erro r may be ('ontrolled. :Vlechanical lo sses are minimized when an amalgamated electrode is used: corrosion. when an amalgamatt'C1 electrode is used in an air free system. An e lec trolyt e. 25 wl. percent NH ,Ci and 3 molal I:nCI , . was used in the se determinations. This report prese nt s th e account of resea rch which was prf'l'equi s it e to ,u bsequent a('('urat,. d e te rmination of the e lec trochemical equiva lent and th e atomic w{'i~ht of zinc.