Zougagh M, de Torres A García, Cano Pavón J M
Department of Analytical Chemistry, Faculty of Sciences, University of Málaga, E-29071, Málaga, Spain.
Talanta. 2002 Mar 11;56(4):753-61. doi: 10.1016/s0039-9140(01)00605-1.
Two flow injection inductively coupled plasma atomic emission spectrometric methods for the preconcentration and determination of trace amounts of cadmium in sea-water and waste-water samples are described based on the adsorption of the metal ion on a micro-column placed in the injection valve of the FI manifold and packed with silica gel funtionalised with 1,5-bis(di-2-pyridyl) methylene thiocarbohydrazide (DPTH-gel) and silica gel functionalised with methylthiosalicylate (TS-gel), respectively. Various parameters and chemical variables affecting the preconcentration and determination of this metal by ICP-AES are evaluated. The DPTH-gel preconcentration method has a linear calibration range from 5 to at least 100 ng ml(-1) of cadmium, with a R.S.D. of 1.1% for ten independent analyses of 100 ng ml(-1), a detection limit of 1.1 ng ml(-1) and a throughput of 40 samples per hour using a 60 s preconcentration time. The TS-gel preconcentration method shows a linear range between 10 and 100 ng ml(-1), with a R.S.D. of 2.5% for ten independent analyses of 100 ng ml(-1), a detection limit of 4.3 ng ml(-1) and a sample throughput of 24 samples per hour for a preconcentration time of 120 s. Validation was carried out against a certified reference water sample and by determining the analyte content in spiked synthetic sea-water, sea-water and waste-water.
本文描述了两种流动注射电感耦合等离子体原子发射光谱法，用于海水和废水样品中痕量镉的预富集和测定。该方法基于金属离子分别吸附在流动注射进样阀中的微型柱上，微型柱分别填充有经1,5-双（二-2-吡啶基）亚甲基硫代氨基脲功能化的硅胶（DPTH-凝胶）和经甲基硫代水杨酸功能化的硅胶（TS-凝胶）。评估了影响电感耦合等离子体原子发射光谱法对该金属进行预富集和测定的各种参数和化学变量。DPTH-凝胶预富集方法的线性校准范围为5至至少100 ng ml⁻¹镉，对100 ng ml⁻¹进行十次独立分析时相对标准偏差为1.1%，检测限为1.1 ng ml⁻¹，使用60 s预富集时间时每小时可处理40个样品。TS-凝胶预富集方法的线性范围为10至100 ng ml⁻¹，对100 ng ml⁻¹进行十次独立分析时相对标准偏差为2.5%，检测限为4.3 ng ml⁻¹，预富集时间为120 s时每小时可处理24个样品。通过与有证标准水样对照以及测定加标合成海水、海水和废水中的分析物含量进行了方法验证。
