The zirconium/nickel alloy-potassium perchlorate-nitrocellulose pyrotechnic system has been studied using differential scanning calorimetry, simultaneous TG-DTA-mass spectrometry and chemical analysis using ion-specific electrodes. Quantitative measurements on the solid state reaction, in the region of 400 degrees C, between zirconium/nickel alloy and potassium perchlorate have shown that a major component of the solid state reaction may be represented by the equation 9Zr + 14Ni + 8KClO(4) = 9ZrO(2) + 14NiO + 8KCl. DSC has been confirmed as an excellent ancillary method for the determination of the amount of potassium perchlorate reacted.