A simple spectrophotometric method for determination of carboxyhemoglobin (HbCO) in blood is described. Blood is dissolved in sodium carbonate solution at a dilution near 250-fold. The diluent contains sodium hydrosulfite providing the two-component system HbCO- reduced hemoglobin (HHb). The percentage of HbCO is calculated from absorbance values at 532 and 558 nm measured after the addition of sodium hydroxide, which makes the solution completely clear. Results obtained by the present method are in satisfactory agreement with those by the oxygen electrode method.