流动注射微柱预富集-火焰原子吸收光谱法测定海水中铅(Ⅱ)  

FAAS Determination of Lead(Ⅱ) in Sea Water with FI-Pre-enrichment on Micro-column

作　　者：童颖[1] 徐芳[2] 刘志高 印春生[1] 杨红[1] 

机构地区：[1]上海海洋大学环境科学系,上海201306 [2]上海交通大学环境科学与工程学院,上海200240 [3]上海光谱仪器有限公司,上海200233

出　　处：《理化检验（化学分册）》2012年第3期269-271,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海市教委重点学科(No.J50702);国家海洋公益项目(201005026);上海市科委项目(08142200202;10142201800)

摘　　要：应用流动注射技术,用D412螯合树脂微柱富集海水中的铅(Ⅱ),并与火焰原子吸收光谱法相结合测定海水中铅(Ⅱ)。20mL海水样品以3mL.min-1流量进柱,被树脂螯合吸附富集,以0.2mol.L-1乙酸铵溶液5mL淋洗柱体去除干扰物,以4mol.L-1硝酸溶液4mL为洗脱剂(流量为7mL.min-1),洗脱液直接引入火焰原子吸收光谱仪雾化器,在线检测。当海水样进样20mL时,铅(Ⅱ)测定灵敏度可提高约35倍;检出限(3s)为1.3μg.L-1。实际应用于海水样品分析,加标回收率为94.5%,测定值的相对标准偏差(n=6)为2.2%。Trace amount of lead（Ⅱ） in sea water was pre-enriched on a micro-column packed with D412 chelate resin in a FI-system.Twenty mL of sea water sample was injected into the micro-column by wriggling pump at a rate of 3 mL·min-1,and Pb（Ⅱ） in the sample solution was adsorbed on the chelate resin.The micro-column was washed with 5 mL of 0.2 mol·L-1 NH4OAc solution to remove residual seawater.Pb（Ⅱ） was stripped from the micro-column with 4 mL of 4 mol·L-1 HNO3 solution at the rate of 7 mL·min-1.The eluate was transferred directly to the atomizer of the instrument.Peak-shaped absorption signal was recorded and the value of peak height was taken as parameter for quantification.By the enrichment procedure mentioned above,sensitivity for determination of the Pb（Ⅱ） was raised 35 times as compared with the procedure without pre-enrichment.Detection limit（3s） of the method was 1.3 μg·L-1.Test for recovery was made by standard addition method,giving value of recovery of 94.5% with RSD（n=6） of 2.2%.

关 键 词：火焰原子吸收光谱法 在线流动注射 微柱预富集 螯合树脂 海水 铅(Ⅱ) 

分 类 号：O657.31[理学—分析化学]