Platelets, mononucleated cells, polymorphonucleated cells, and erythrocytes were separated from whole blood by use of discontinuous gradients of colloidal polyvinylpyrrolidone-coated silica ("Percoll"). We measured the zinc content of these cells by flame atomic absorption spectrophotometry, using a modified technique for micro-samples that obviated matrix interferences. Thus, results obtained by conventional flame atomic absorption and by the micro-method were identical. Inter-comparisons of separation methods indicated that separation of platelets and mononucleated cells by a two-gradient system of "Ficoll-Hypaque" (a synthetic polymer of sucrose) or Percoll was relatively poor, whereas there was a good separation when a tertiary gradient system of Percoll was used. The apparent zinc content of mononucleated cells depended on the degree of separation from the platelets, with contamination by platelets resulting in artificially high values for mononucleated cells.