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Two head-space gas chromatographic methods for the determination of hydrogen cyanide (HCN) in blood were demonstrated using electron capture detector (ECD). One was the double head-space gas sampling technique and the other used the reaction pre-column packed with Chloramine-T for the conversion of HCN into cyanogen chloride (CNC1). In the former method, HCN in blood was firstly released by acidification, and then the HCN gas was replaced into the another vial in which Chloramine-T solution had been placed. The head-space gas in the second vial was analyzed by gas chromatograph (GC). In the latter, HCN gas released was directly injected into the GC pre-connected the reaction column. The conversion of HCN into CNC1 was easily achieved by both methods. The use of dichloromethane as an internal standard and PTFE-faced septum for the sealing of vial greatly improved the precision and reliability of these analytical methods. The calibration curves by these methods gave good linearity and the lower detection limit taken from these plots was ca. 0.05 micrograms/ml. In particular, the reaction pre-column method, by which blood cyanide can be analyzed rapidly and accurately with only simple alteration of apparatus, is superior in the routine analysis of blood cyanide.