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2个富钴结壳铂族元素(PGEs)标准物质MCPt-1和MCPt-2的原样分别由中国和俄罗斯取自中太平洋海山和西太平洋麦哲伦海山区。样品经风干、选配,先经球磨制备成74μm(200目)粉体样品,再用气流磨将其进一步加工成具有超细粒度的均匀样品。采用激光粒度仪检测样品的粒度分布,其平均粒度分别为1.8和1.5μm(约2 000目)。采用高精度的X射线荧光光谱法(XRF)和电子探针方法分别检验了6个主、次元素在mg和μg取样量水平上的均匀性,用LA-ICP-MS检验了包括Pt在内的40多个痕量元素在μg量水平上的均匀性。样品采用锍镍火试金和Carius管预富集和酸溶消解,除Rh外均采用同位素稀释电感耦合等离子体质谱测定(ID-ICP-MS),确定了MCPt-1和MCPt-2中6个铂族元素的标准值;采用XRF和ICP-AES、ICP-MS方法相结合给出了62个主、次和痕量元素的信息值。最小取样量分别为1 g(测定PGEs)和2mg(测定其他元素)。
Two samples of cobalt-rich crusts PGEs MCPt-1 and MCPt-2 were taken from China and Russia from the seamounts of the Seashore in the Central Pacific and the Magellan Seas in the western Pacific. Samples were air-dried, optional, first prepared by ball milling 74μm (200 mesh) powder samples, and then jet mill further processed into a uniform sample with ultra-fine particle size. The particle size distribution of the samples was measured by laser particle sizer. The average particle sizes were 1.8 and 1.5 μm (about 2,000 mesh), respectively. High-precision X-ray fluorescence (XRF) and electron probe methods were used to examine the homogeneity of the six major and minor elements at the mg and μg sampling levels, respectively. The results of LA-ICP-MS including Pt Of more than 40 trace elements in the amount of μg level of uniformity. The samples were pre-enriched with sulfoniumbromide and Carius tubes and digested with acid. All samples except for Rh were identified by isotope dilution ICP-MS (Isotopically Coupled Plasma Mass Spectrometry) Platinum group elements of the standard value; using XRF and ICP-AES, ICP-MS method gives the information of 62 primary, secondary and trace elements. The minimum sampling volume was 1 g (PGEs) and 2 mg (other elements were measured).