In this procedure hemoglobin is converted to its reduced form and the magnitude of the zero-order spectral shift of the reduced hemoglobin peak at 430 nm to the carboxyhemoglobin peak at 418 nm is determined by second-derivative spectrum analysis. The method is simple, straightforward to set up, and rapid. A result may be obtained within 15 min of receiving the sample. It is sufficiently sensitive to differentiate carboxyhemoglobin concentration in the blood of smokers and nonsmokers.