ABSTRACT

A new preconcentration technique of Zr, Nb, Mo, Hf, Ta and W has been invented employing coprecipiation with Ti compounds. Silicate samples were digested by HF with addition of Ti. Subsequent drying with HClO₄ resulting in complete elimination of fluorine produces Ti compounds (oxide/hydroxides). The sample was then dissolved with dilute nitric acid and centrifuged, and the residual Ti compounds were collected. The Ti compounds forming from 2 mg of Ti without matrix elements concentrate 84-98% of Zr, Nb, Mo, Hf, Ta and W. In 20 mg basaltic and 50 mg peridotitic matrices, the addition of 1 mg of Ti was appropriate and gave yields of 46-69 and 54-79%, respectively, for Zr, Nb, Mo, Hf, Ta and W. Exploiting this preconcentration, sequential separation protocols of Hf, Pb, Sr, Lu, Nd and Sm for isotope analysis are developed with total blanks of 16, 11, 60, 2.4, 3 and 0.4 pg, respectively. The method is suitable for Lu-Hf system studies with capability of simultaneous separation of Pb, Sr, Nd and Sm from the same sample digest as well as isotopic anomaly studies of Zr, Mo and W. As application examples, accurate Lu-Hf data and Pb isotope ratios were obtained for basalt (JB-3) and peridotite (JP-1) by MC-ICP-MS.