Abstract: Sample of low smoke HFFR cable was combusted in oxygen flask and the gaseous HCl liberated was absorbed in deionized water. The content of total chlorine in the water solution was determined by mercury thiocyanate-spectrophotometry. Linear relationship between values of absorbance and mass concentration of Cl- was obtained in the range of 0.20-5.00 mg·L-1. The proposed method was applied to the determination of chlorine in low smoke HFFR cable; values of recovery found by standard addition method were in the range of 96.0%-103% with RSD′s (n=5) less than 4.5%.