将多孔石墨化炭黑与5-硫代-15-冠-5的乙醚溶液混合后,蒸干溶剂乙醚.将所得的混合物填入聚四氟乙烯柱中,制得固相萃取柱.萃取柱经0.1 mol·L-1的硫代硫酸钠和pH 3.5的乙酸盐缓冲溶液洗涤后,用0.1 mol·L-1的硫代硫酸钠溶液反向洗脱小柱上富集的金,洗脱液供火焰原子吸收光谱法测定.方法用于矿石和环境水样中金的实际测定,结果与电感耦合等离子体质谱法的结果一致,相对标准偏差(n=5)在2.4%~3.4%之间,回收率在92.6%~97.8%之间.

To prepare the SPE column,ether solution of 5-thio-15-crown-5 (5-T-15-CR-5) was first mixed with porous graphitized carbon black,and the solvent ether was removed by evaporation.The dried mixture was then filled into a PTFE column which was rinsed successively with 0.1 mol·L-1 Na2S2O3 solution and acetate buffer solution of pH 3.5,and was ready for enrichment of auric ion.Gold(Ⅲ) in sample solution of acetate buffer medium of pH 3.5 was enriched on the SPE column and eluted from the column by reverse elution with definite amount of 0.1 mol·L-1 Na2S2O3 solution and the eluate obtained was used for FAAS determination.The proposed method was applied to the determination of gold in samples of environmental water and ores,giving results in consistency with the results obtained by ICP-MS method.Values of RSD′s (n=5) were in the range of 2.4%-3.4% and results of recovery were in range of 92.6%-97.8%.