We describe a method for rapid and specific measurement of thiocyanate in serum or urine. We separate thiocyanate from interfering compounds by adsorbing it on an anion-exchange resin that has special affinity for thiocyanate, then eluting with sodium perchlorate. The eluted thiocyanate is quantified by a modified König reaction, sodium hypochlorite being used as the chlorinating reagent. Analytical recovery of thiocyanate added to serum and urine was quantitative; the coefficient of variation was 2.3% for both within-day and between-day precision. Cyanide and certain antibiotics interfere, but may be eliminated by including additional washing steps in the usual procedure. The proposed procedure was compared with another method, based on the oxidation of thiocyanate to cyanide. Agreement was satisfactory, both for serum and urine.