Vlasánkova R, Otruba V, Bendl J, Fisera M, Kanický V
Department of Analytical Chemistry, Masaryk University, CZ 611 37 Brno, Czech Republic.
Talanta. 1999 Apr;48(4):839-46. doi: 10.1016/s0039-9140(98)00100-3.
Modified silicagel (C18) was studied for separation and preconcentration of platinum group metals (Ru, Rh, Pd, Os, Ir and Pt) as ion associates of their chlorocomplexes with cation of onium salt N(1-carbaethoxypentadecyl)-trimethyl ammonium bromide. Sample containing HCl and the onium salt was pumped through the column. After elution with ethanol the eluate was evaporated in the presence of HCl. Resulting aqueous solutions were analysed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Recovery values of 1-20 mug Pt and Pd from 50 ml of synthetic pure solution were 100+/-3 and 100+/-1%, respectively, however, they diminished with increasing sample volume and in the presence of the real sample matrix or nitrate ions. Samples of engine soot (NIES No. 8), decomposed by low pressure oxygen high-frequency plasma, and airborne particulates from dust filters of meteorological stations, leached with HNO(3) and H(2)O(2), were analysed. A reasonable agreement was found between ICP-MS and ICP-AES results for airborne dust samples and the values comparable with those in literature were determined in NIES No. 8.
研究了改性硅胶（C18）对铂族金属（钌、铑、钯、锇、铱和铂）的分离和预富集作用，这些铂族金属以其氯配合物与鎓盐N-(1-羧乙氧基十五烷基)-三甲基溴化铵的阳离子形成的离子缔合物形式存在。将含有盐酸和鎓盐的样品泵入柱中。用乙醇洗脱后，在盐酸存在下将洗脱液蒸发。所得水溶液用感应耦合等离子体原子发射光谱法（ICP-AES）和感应耦合等离子体质谱法（ICP-MS）进行分析。从50毫升合成纯溶液中回收1-20微克铂和钯的回收率分别为100±3%和100±1%，然而，随着样品体积的增加以及在实际样品基质或硝酸根离子存在的情况下，回收率会降低。分析了通过低压氧气高频等离子体分解的发动机烟灰样品（NIES No. 8）以及用硝酸和过氧化氢浸出的气象站灰尘过滤器中的空气颗粒物。对于空气灰尘样品，ICP-MS和ICP-AES的结果之间存在合理的一致性，并且在NIES No. 8中测定的值与文献中的值相当。
