Anthemidis Aristidis N, Martavaltzoglou Evdoxia K
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124, Greece.
Anal Chim Acta. 2006 Jul 28;573-574:413-8. doi: 10.1016/j.aca.2005.12.055. Epub 2006 Feb 8.
A novel flow injection (FI) solid phase extraction method for the determination of arsenic(III) at trace levels was developed, using on-line hydride generation atomic absorption spectrometry (HG-AAS). Selective determination of As(III) was achieved by on-line formation and retention of the pyrrolidine dithiocarbamate arsenic complex As(III)-PDC on the PTFE turnings which are packed in the preconcentration micro-column. The retained complex was eluted by 2 ml 2 mol l(-1) HCl and subsequently introduced on-line into the integrated reaction chamber/gas-liquid separator (RC-GLS). A 1.5% (m/v) NaBH4 solution was used for arsine generation, while a gas stream of N2 was employed for flash release and transportation towards the atomic absorption flow through cell (AAC) for atomization and measurement. The excellent performance of PTFE turnings as sorbent material and the compact design of the RC-GLS result to high sensitivity, selectivity and sampling frequency. For 60s preconcentration time and sample consumption 10.4 ml a sampling frequency of 25 h(-1) and a detection limit of c(L)=0.02 microg l(-1) were obtained. The repeatability, expressed as relative standard deviation (R.S.D.), at 1.0 microg l(-1) As(III), was s(r)=2.8%. The proposed method was successfully applied to the selective determination of As(III) in natural waters and total arsenic determination in certified reference material.
建立了一种使用在线氢化物发生原子吸收光谱法(HG-AAS)测定痕量砷(III)的新型流动注射(FI)固相萃取方法。通过在预浓缩微柱中填充的聚四氟乙烯车削屑上在线形成并保留吡咯烷二硫代氨基甲酸酯砷络合物As(III)-PDC,实现了对As(III)的选择性测定。保留的络合物用2 ml 2 mol l(-1) HCl洗脱,随后在线引入集成反应室/气液分离器(RC-GLS)。使用1.5%(m/v)NaBH4溶液产生砷化氢,同时采用N2气流进行快速释放并输送至原子吸收流通池(AAC)进行雾化和测量。聚四氟乙烯车削屑作为吸附材料的优异性能以及RC-GLS的紧凑设计导致了高灵敏度、选择性和采样频率。对于60 s的预浓缩时间和10.4 ml的样品消耗量,获得了25 h(-1)的采样频率和c(L)=0.02 μg l(-1)的检测限。在1.0 μg l(-1) As(III)时,以相对标准偏差(R.S.D.)表示的重复性为s(r)=2.8%。所提出的方法成功应用于天然水中As(III)的选择性测定以及标准参考物质中总砷的测定。