Wang Yang, Wang Jian-Hua, Fang Zhao-Lun
Research Center for Analytical Sciences, Northeastern University, Box 332, Shenyang 110004, China.
Anal Chem. 2005 Aug 15;77(16):5396-401. doi: 10.1021/ac050638z.
Octadecyl immobilized surface was, for the first time, proved to be a superb precipitate-collecting medium. Surface charge effect was assumed to dominate the adsorption of cadmium hydroxide precipitate, facilitated by electrostatic interaction between the negatively charged C18 bead surface and positively charged cadmium hydroxide clusters. Residual silanol groups on the C18-immobilized silica surface did not contribute to precipitate adsorption. A novel procedure for ultratrace cadmium preconcentration was proposed by incorporating a renewable microcolumn in a lab-on-valve system. Cd(OH)(2) precipitate was adsorbed onto the C18 surface, which was afterward eluted with 20 microL of nitric acid (1%) and quantified with detection by electrothermal atomic absorption spectrometry. An enrichment factor of 28 and a limit of detection of 1.7 ng L(-1), along with a sampling frequency of 13 h(-1) were obtained with a sample consumption of 600 microL within the concentration range of 0.01-0.2 microg L(-1), achieving a precision of 2.1% RSD at the 0.05 microg L(-1) level. The enrichment factor was further enhanced to 44 by increasing the sample volume to 1200 microL. The procedure was validated by analyzing cadmium in three certified reference materials, that is, river sediment (CRM 320), sea lettuce (CRM 279), and frozen cattle blood (GBW 09140). Good agreement between the obtained results and the certified values was achieved.
首次证明十八烷基固定化表面是一种出色的沉淀物收集介质。表面电荷效应被认为主导了氢氧化镉沉淀物的吸附,这是由带负电荷的C18珠粒表面与带正电荷的氢氧化镉簇之间的静电相互作用促成的。C18固定化硅胶表面上的残留硅醇基团对沉淀物吸附没有贡献。通过在阀上实验室系统中加入可再生微柱,提出了一种超痕量镉预富集的新方法。Cd(OH)₂沉淀物吸附到C18表面,随后用20 μL硝酸(1%)洗脱,并用电热原子吸收光谱法进行检测定量。在0.01 - 0.2 μg L⁻¹的浓度范围内,进样量为600 μL时,获得了28的富集因子、1.7 ng L⁻¹的检测限以及13 h⁻¹的采样频率,在0.05 μg L⁻¹水平下实现了2.1%的相对标准偏差精密度。通过将样品体积增加到1200 μL,富集因子进一步提高到44。通过分析三种有证标准物质,即河流沉积物(CRM 320)、海莴苣(CRM 279)和冻牛血(GBW 09140)中的镉,验证了该方法。所获结果与认定值之间达成了良好的一致性。