Tyson J F, Palmer C D
Department of Chemistry, University of Massachusetts, 710 North Pleasant Street, Amherst, MA 01003, USA.
Anal Chim Acta. 2009 Oct 12;652(1-2):251-8. doi: 10.1016/j.aca.2009.07.002. Epub 2009 Jul 8.
An inductively coupled plasma atomic fluorescence spectrometry (ICP-AFS) instrument, was modified so that it was capable of monitoring transient chromatographic or flow-injection profiles and that sulfur molecular emission and selenium atomic fluorescence could be monitored simultaneously in an argon-hydrogen diffusion flame on a glass burner. The analytes were introduced as hydrogen selenide and hydrogen sulfide, generated on a flow-injection manifold. Selenate was reduced to hydride-forming selenite by microwave-assisted on-line reaction with hydrochloric acid, and sulfate, or sulfite, was reduced to hydride-forming sulfide by a mixture of hydriodic acid, acetic acid and sodium hypophosphite. The effects of the nature of reducing agent, flow rate, microwave power and coil length were studied. The limit of detection (3s) for selenium was 10microgL(-1), and for sulfide was 70microgL(-1) (200-microL injection volume). The calibration was linear for selenium up to 2mgL(-1) and to 10mgL(-1) for sulfide. The throughput was 180h(-1). The three sulfur species could be differentiated on the basis of reactivity at various microwave powers.
对一台电感耦合等离子体原子荧光光谱仪（ICP-AFS）进行了改进，使其能够监测瞬态色谱或流动注射曲线，并能在玻璃燃烧器的氩-氢扩散火焰中同时监测硫分子发射和硒原子荧光。分析物以在流动注射歧管上生成的硒化氢和硫化氢形式引入。通过与盐酸的微波辅助在线反应，将硒酸盐还原为可形成氢化物的亚硒酸盐，而硫酸盐或亚硫酸盐则通过氢碘酸、乙酸和次磷酸钠的混合物还原为可形成氢化物的硫化物。研究了还原剂性质、流速、微波功率和线圈长度的影响。硒的检测限（3s）为10μg L⁻¹，硫化物的检测限为70μg L⁻¹（进样体积200μL）。硒的校准曲线在高达2mg L⁻¹范围内呈线性，硫化物在高达10mg L⁻¹范围内呈线性。分析通量为180 h⁻¹。根据在不同微波功率下的反应性，可以区分三种硫物种。
