研究了流动注射在线置换吸附预富集-火焰原子吸收(FAAS)联用技术测定复杂样品中痕量铅的方法。首先使Zn(Ⅱ)与二乙基二硫代氨基甲酸钠(DDTC)在线配合形成Zn-DDTC并预先吸附在香烟过滤嘴填充柱上,然后使含Pb(Ⅱ)的标准溶液或样品溶液流经填充柱与Zn-DDTC发生置换反应而被填充柱富集。被吸附的分析物用乙醇定量洗脱至FAAS进行在线检测。此在线置换吸附预富集过程有效地消除了与DDTC的配合物稳定性较Zn-DDTC弱的共存金属离子的干扰。在样品流速为5.0mL/min和置换吸附预富集90s的条件下,得到铅的吸收信号的增感因子为33,检出限为2.0μg/L。浓度为100μg/L的铅标准溶液11次平行测定的精密度(RSD)为1.2%。本方法已应用于生物样品的分析。
A flow injection (FI) on-line displacement sorption preconcentration coupled with flame atomic absorption spectrometry (FAAS) for selective preconcentration and separation of trace lead in biological samples was developed. The method involved on-line formation of the Zn-sodium diethylammonium diethyldithiocarbanate ( DDTC ) complex and its presorption onto the microcolumn packed with cigarette filter, retention of the analyte Pb(Ⅱ) onto the cigarette filter through a displacement reaction between the Pb(Ⅱ) and the pre-sorbed Zn-DDTC, elution of the retained analyte with ethanol, and on-line detection by FAAS. Interferences from coexisting ions with lower stability of their DDTC complexes relative to Zn-DDTC were eliminated because they could not displace the Zn(Ⅱ) from the presorbed Zn-DDTC. With a 90-s displacement sorption at a flow rate of 5.0 mL/min, an enhancement factor of 33 with a detection limit ( 3s ) of 2.0 μg/L was obtained. The precision ( RSD, n = 11 ) was 1.2% at the level of 100 μg/L. The developed method was successfully applied to selective determination of trace lead in biological materials.