Meisel T, Moser J, Fellner N, Wegscheider W, Schoenberg R
General and Analytical Chemistry, University of Leoben, Franz-Josef-Str. 18, A-8700 Leoben, Austria.
Analyst. 2001 Mar;126(3):322-8. doi: 10.1039/b007575m.
A method for the determination of low Ru, Pd, Re, Os, Ir and Pt abundances in geological reference materials by isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) after acid digestion in a high pressure asher (HPA-S) is presented. The digestion technique is similar to that using Carius tubes but easier to handle and reaches higher temperatures. Osmium can be determined as OsO4 with ICP-MS directly after digestion through a sparging technique. The remaining elements are preconcentrated by means of anion column chromatography. The resin is digested directly without elution leading to high yields but this causes problems if Zr is present at higher levels in the silicate rich materials. The analytical results for international platinum group element (PGE) reference materials, chromitite CHR-Bkg, basalt TDB-1 and gabbro WGB-1, are presented and compared with literature data, demonstrating the validity of the described method. Although higher in concentration, PGEs determined for reference material WGB-1 were worse than for TDB-1 indicating a more inhomogeneous distribution of the platinum group mineral phases. The low PGE abundance chromitite standard, CHR-Bkg, is likely to be homogeneous for Ru, Re, Os and Ir and is recommended as a reference material for the study of chromitites. Detection limits (3s x total procedure blank) range from 0.012 ng (Re and Os) to 0.77 ng (Pt), which could be further improved by applying higher quality acids.
介绍了一种通过在高压灰化器(HPA-S)中酸消解后,采用同位素稀释电感耦合等离子体质谱法(ICP-MS)测定地质标准物质中低含量钌(Ru)、钯(Pd)、铼(Re)、锇(Os)、铱(Ir)和铂(Pt)的方法。该消解技术与使用卡里乌斯管的技术类似,但更易于操作且能达到更高的温度。消解后,锇可通过鼓泡技术直接用ICP-MS测定为OsO4。其余元素通过阴离子柱色谱法进行预富集。树脂无需洗脱直接消解,回收率高,但如果富含硅酸盐的物质中锆含量较高,会产生问题。给出了国际铂族元素(PGE)标准物质铬铁矿CHR-Bkg、玄武岩TDB-1和辉长岩WGB-1的分析结果,并与文献数据进行了比较,证明了所述方法的有效性。尽管参考物质WGB-1中测定的PGE浓度较高,但其结果比TDB-1的差,表明铂族矿物相的分布更不均匀。低PGE含量的铬铁矿标准物质CHR-Bkg在Ru、Re、Os和Ir方面可能是均匀的,推荐作为铬铁矿研究的参考物质。检测限(3s×全程序空白)范围为0.012 ng(Re和Os)至0.77 ng(Pt),通过使用更高质量的酸可进一步提高检测限。