Determination of Pt, Pd, Ru and Ir in geological samples by ID-ICP-MS using sodium peroxide fusion and Te co-precipitation
Determination of Pt, Pd, Ru and Ir in geological samples by ID-ICP-MS using sodium peroxide fusion and Te co-precipitation
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DOI：
10.2343/geochemj.37.557
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发表时间：
2003-10
影响因子：
0.8
通讯作者：
L. Qi;D. Grègoire;Mei‐Fu Zhou;J. Malpas
中科院分区：
文献类型：
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作者：
L. Qi;D. Grègoire;Mei‐Fu Zhou;J. Malpas
建立了同位素稀释-电感耦合等离子体质谱（ICP-MS）测定地质样品中铂、钯、钌、铱的方法。以Lu为内标，外标法测定单一同位素Rh和Au。采用过氧化钠熔融法在石墨坩埚（而不是玻璃碳或锆坩埚）中分解样品。在将熔融滤饼溶解在水中之后，向溶液中加入富集的Pt、Pd、Ru和Ir的稳定同位素，然后用HCl酸化。然后将该溶液蒸发至干，促进由胶体材料形成无水硅酸盐。然后通过Te共沉淀预浓缩PGE和Au。通过Te共沉淀纯化试剂HCl和SnCl 2。因此，PGE空白水平仅来自PGE浓度<0.02 ng/g的Na 2 O2。加入镥作为内标，以校正仪器漂移和基质抑制效应，用于测定单一同位素元素。方法检测限范围为0.02 - 0.3 ng/g。CCRMP（CANMET，渥太华，加拿大）认证的标准物质WGB-1（辉长岩）、TDB-1（辉长岩）、UMT-1（超镁铁尾矿）、WPR-1（蚀变橄榄岩）、WMG-1（矿化辉长岩）和WMS-1（块状硫化物）的结果与认证值一致。
A method is proposed for the determination of Pt, Pd, Ru and Ir in geological samples by isotope dilution-inductively coupled plasma mass spectrometry (ICP-MS). Mono-isotopic elements Rh and Au are determined by external calibration using Lu as the internal standard. Sodium peroxide fusion in corundum crucibles (instead of glassy carbon or zirconium crucibles) is used to decompose the samples. After dissolution of the fused cake in water, the solution is spiked with enriched stable isotopes of Pt, Pd, Ru and Ir, and then acidified with HCl. This solution is then evaporated to dryness promoting the formation of anhydrous silicate from colloidal material. PGEs and Au are then pre-concentrated by Te co-precipitation. The reagents HCl and SnCl2 are purified by Te co-precipitation. PGE blank levels are thus only derived from the Na2O2 which has PGE concentrations of <0.02 ng/g. Lutetium is added as the internal standard to correct for instrument drift and matrix suppression effects for the determination of the mono-isotopic elements. Method detection limits range from 0.02 to 0.3 ng/g. The results obtained for the CCRMP (CANMET, Ottawa, Canada) certified reference materials WGB-1 (gabbro), TDB-1 (diabase), UMT-1 (ultramafic ore tailings), WPR-1 (altered peridotite), WMG-1 (mineralized gabbro), and WMS-1 (massive sulphide) are in good agreement with certified values.