二溴羟基苯基荧光酮分光光度法测定汞(Ⅱ)-经巯基葡聚糖凝胶柱分离富集
Spectrophotometric Determination of Mercury(Ⅱ) with Color Reagent DBHPF After Separation and Enrichment on Sulfhydryl Dextran Gel Column
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摘要: 在以硼酸盐缓冲溶液控制于pH 9.1的由十六烷基三甲基溴化铵(CTMAB)、正丁醇、正庚烷和水以1.0比0.9比0.1比9.8的质量比配制的微乳溶液中,汞(Ⅱ)与二溴羟基苯基荧光酮(DBHPF)反应形成1比2的橙色络合物,络合物的最大吸收峰位于570 nm波长处,表观摩尔吸光率为3.2×105L·mol-1·cm-1.汞(Ⅱ)的质量浓度在6~550 μg·L-1范围内符合比耳定律,检出限(3S/N)为2 μg·L-1.据此提出了测定痕量汞(Ⅱ)的方法.应用此方法测定了水样中汞(Ⅱ)并作方法的回收率及精密度试验,测得平均回收率为104%,相对标准偏差(n=6)为2.7%(两个样品的平均值).对水样中痕量汞(Ⅱ)的分离和富集,建议采用巯基葡聚糖凝胶吸附分离法,吸附于凝胶柱上的汞(Ⅱ)用氯化钠饱和的8 mol·L-1盐酸溶液洗脱后按上述光度法测定.Abstract: In a microemulsoid medium containing CTMAB,n-butanol,n-heptane and water,mixed in the mass ratio of 1.0 to 0.9 to 0.1 to 9.8,and buffered at pH 9.1 with borax buffer solution,an orange colored complex (Hg∶R=1∶2) was formed by the reaction of Hg(Ⅱ) ion with dibromohydroxyphenylfluorone (DBHPF),having its absorption maximum at the wavelength of 570 nm and its apparent molar absorptivity (ε570) of 3.2×105L·mol-1·cm-1.Beer′s law was kept in the range of 6-550 μg·L-1 of Hg(Ⅱ).Detection limit (3S/N) of the method was found to be 2 μg·L-1.Based on these facts,a method for determination of traces of Hg(Ⅱ) was proposed.Tests for recovery and precision were made by analyzing 2 water samples,giving values of average recovery and average RSD′s (n=6) to be 104% and 2.7% respectively.Procedure for enrichment of traces of Hg(Ⅱ) in water sample by adsorption on sulfhydryl dextran gel (SDG) column and elution from the column by 8 mol·L-1 HCl saturated with NaCl was given in detail.