Furuta N, Shinofuji T
Department of Applied Chemistry, Faculty of Science and Engineering, Chuo University, 112, Kasuga, Bunkyo-ku, Tokyo, Japan.
Anal Bioanal Chem. 1996 Jun;355(5-6):457-60. doi: 10.1007/s0021663550457.
Recent regulation in Japan requires more sensitive trace analysis methods for the determination of arsenic and selenium and their oxidation states As(III) and (V), Se(IV) and (VI). The hydride generation (HG) technique is usually used in combination with AAS and ICP-AES to increase sensitivity. However, hydrochloric acid is mostly used to acidify the sample solution in HG. Isobaric interferences due to chlorine-related species cause mass spectral problems when the same solution is used for the determination of these elements by ICP-MS. In this study, different oxidation states of As and Se were determined by coupling ion chromatography (IC) to an ICP-AES instrument. An HG technique was used to introduce test samples into the ICP. Nitric acid was employed to acidify the samples for HG. The concentrations of acid and base were kept as low as possible to reduce contamination. The formation of As and Se hydrides could be achieved without HCl, if the concentrations of acid and alkaline solutions were optimized. However, HCl was necessary for additional reduction of Se(VI) to Se(IV).
日本最近的法规要求采用更灵敏的痕量分析方法来测定砷、硒及其氧化态(As(III) 和 As(V)、Se(IV) 和 Se(VI))。氢化物发生(HG)技术通常与原子吸收光谱法(AAS)和电感耦合等离子体发射光谱法(ICP - AES)联用,以提高灵敏度。然而,在氢化物发生过程中,盐酸大多用于酸化样品溶液。当使用相同溶液通过电感耦合等离子体质谱法(ICP - MS)测定这些元素时,与氯相关的物种产生的等压干扰会导致质谱问题。在本研究中,通过将离子色谱(IC)与 ICP - AES 仪器联用测定了砷和硒的不同氧化态。采用氢化物发生技术将测试样品引入 ICP。使用硝酸酸化样品以进行氢化物发生。酸和碱的浓度尽可能保持在低水平以减少污染。如果优化酸和碱溶液的浓度,则无需盐酸即可实现砷和硒氢化物的形成。然而,将 Se(VI) 进一步还原为 Se(IV) 需要盐酸。