以表面浸渍固载有疏水性室温离子液体—1-己基-3-甲基咪唑六氟磷酸盐(1-hexyl-3-methylimidazolium hexafluorophosphate,[C6mim]PF6)的Amberlite XAD-7大孔树脂为固相萃取微柱的吸附剂,建立了微柱在线富集和流动注射-分光光度法测定废水中痕量游离态汞的新方法。在酸性介质中和十六烷基三甲基溴化铵(CTMAB)存在下,Hg2+与双硫腙反应生成红色的中性配合物可被微柱有效地定量富集。在优化的实验条件下,方法的线性范围为0.35~50 μg·L^-1 Hg^2+,检出限为0.067 μg·L^-1 Hg^2+。进样体积为50 mL时,Hg2+的富集因数为25倍。对环境水质汞标准样品(GSBZ50016-90)和加标废水样品的测定,回收率在99%~103%。
Amberlite XAD-7 resin was modified by room temprature ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate, [C4 mim]PF6 ) coating through a maceration method, gaining a new sort of hydrophobie adsorbent for the solid phase extraction mini-column. Trace inorganic mercury in wastewater samples was preconeentrated and determined by flow injection online mini-column sampling coupled with spectrophotometric determination. In acid medium, dithizone was employed as chelator with cetyhrimethylammonium bromide (CTMAB) to form a red neutral mereury-dithizone complex, which could be extracted quantificationally by solid phase extraction technique on the mini-column. Under the optimized conditions, the linearity and the detection limit of the proposed method were found to be 0.35 to 50. 0 μg · L^-1 Hg^2+ and 0. 067μg · L^-1 Hg^2+, respectively. The enrichment factor of 25 times could be achieved with a 50 mL sampling volume and the developed procedure was successfully applied for the determination of mercury in the certified reference material (GSBZ50016-90) and the spiked dock wastewater samples with the recovery of 99%-103%.