Wei W C, Yang M H
Institute of Nuclear Science, National Tsing Hua University, Kuang-Fu Road, 30043, Hsinchu, Taiwan.
Anal Bioanal Chem. 1995 Sep;353(2):167-70. doi: 10.1007/s0021653530167.
A method for the determination of trace impurities of phosphorus and arsenic in trichlorosilane with prior separation followed by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) has been developed. The preconcentration of the analytes from the sample matrix was made by adding cuprous chloride to a 10 mL trichlorosilane sample for the formation of non-volatile compounds with the elements of interest. Upon evaporation of trichlorosilane, the analytes retained in the residue were then determined in the presence of copper as modifier by ETV-ICP-MS. The dual role of cuprous chloride both in the preconcentration and instrumental determination was investigated and discussed. By meticulous control of experimental conditions, limits of detection for these two elements as low as sub-ng/g can be achieved. The method was applied to the determination of phosphorus and arsenic in a commercially available trichlorosilane sample.
建立了一种先分离后用电热蒸发电感耦合等离子体质谱法(ETV-ICP-MS)测定三氯硅烷中痕量磷和砷杂质的方法。通过向10 mL三氯硅烷样品中加入氯化亚铜,使其与目标元素形成非挥发性化合物,从而实现从样品基质中预富集分析物。三氯硅烷蒸发后,在有铜作为改性剂的情况下,通过ETV-ICP-MS测定残留在残渣中的分析物。研究并讨论了氯化亚铜在预富集和仪器测定中的双重作用。通过精心控制实验条件,可实现这两种元素低至亚纳克/克的检测限。该方法应用于市售三氯硅烷样品中磷和砷的测定。