在大量氯酸盐存在下,确定了用硫酸亚铁使氯酸盐还原,当 pH=3—4时,用苯萃取 ClO_4~-——灿烂绿络合物,测定了高氯酸根。结果表明,在25毫升萃取液中,ClO_4~-于2—100微克范围内遵守比尔定律。大量 Li~+、Na~+、K~+、Mg~(++)、Mn~(++)、Pb~(++)、Fe~(+++)、F~-、Cl~-、SO_4~-、CH_3COO~-、和少量的 CrO_4~-不影响测定。方法可用于氯酸锂电解液中微量高氯酸根的测定,也可用于氯酸盐产品中微量高氯酸根的测定。 In the presence of a large amount of chlorate, chlorate was reduced with ferrous sulfate. When pH = 3-4, ClO 4 ~ --- brilliant green complex was extracted with benzene and the perchlorate was measured. The results show that Beer’s law is obeyed in the range of 2-100 micrograms ClO 4 ~ in 25 mL extract. A large number of Li ~ +, Na ~ +, K ~ +, Mg ~ (++), Mn ~ (++), Pb ~ (++) SO_4 ~ -, CH_3COO ~ -, and a small amount of CrO_4 ~ - does not affect the determination. The method can be used for the determination of trace perchlorate in lithium chlorate electrolyte and also for the determination of trace perchlorate in chlorate products.