微柱固相萃取-电感耦合等离子体质谱联用技术用于测定高盐样品中痕量的铅

Determination of Trace Lead in High Salt-ContainingSamples by Solid Phase Extraction Column(SPE)Hyphenated with Inductively Coupled PlasmaMass Spectrometer(ICP-MS)

建立了微柱固相萃取 -电感耦合等离子体质谱联用系统 .对萃取体系的 p H、洗脱液酸度及流速进行了优化选择 .在最佳的分离条件下 Pb的检测限 (3σ,n=6)为 0 .0 3ng/ m L,测定海水的铅的RSD为 2 .6% .该系统成功地应用于实际样品和标准参考物的在线分离富集和测定 .

A Solid Phase Extraction Column(SPE) Inductively Coupled Plasma Mass Spectromet er(ICP MS) hyphenation system was established. The parameters of extraction sys tem such as pH condition, the concentration of nitric acid in eluant and the flo w rate of eluant were optimized. Under optimized conditions, the determination l imit of lead (3σ, n =6) is 0.03 ng/mL.The RSD of measurements for four i ndividual seawaters was 2.6%. The accuracy of the method was assessed by the ana lysis of a certified reference material. Lead recovery from CRM and spiked seawa ter were in the range of 98% and 99.6%.