Coprecipitation of Ti, Mo, Sn and Sb with fluorides and application to determination of B, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by ICP-MS

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We examined the coprecipitation behavior of Ti, Mo, Sn and Sb in Ca-Al-Mg fluorides under two different fluoride forming conditions: at < 70 °C in an ultrasonic bath (denoted as the ultrasonic method) and at 245 °C using a Teflon bomb (denoted as the bomb method). In the ultrasonic method, small amounts of Ti, Mo and Sn coprecipitation were observed with 100% Ca and 100% Mg fluorides. No coprecipitation of Ti, Mo, Sn and Sb in Ca-Al-Mg fluorides occurred when the sample was decomposed by the bomb method except for 100% Ca fluoride. Based on our coprecipitation observations, we have developed a simultaneous determination method for B, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by Q-pole type ICP-MS (ICP-QMS) and sector field type ICP-MS (ICP-SFMS). 9-50 mg of samples with Zr-Mo-Sn-Sb-Hf spikes were decomposed by HF using the bomb method and the ultrasonic method with B spike. The sample was then evaporated and re-dissolved into 0.5 mol l- 1 HF, followed by the removal of fluorides by centrifuging. B, Zr, Mo, Sn, Sb and Hf were measured by ID method. Nb and Ta were measured by the ID-internal standardization method, based on Nb/Mo and Ta/Mo ratios using ICP-QMS, for which pseudo-FI was developed and applied. When 100% recovery yields of Zr and Hf are expected, Nb/Zr and Ta/Hf ratios may also be used. Ti was determined by the ID-internal standardization method, based on the Ti/Nb ratio from ICP-SFMS. Only 0.053 ml sample solution was required for measurement of all 9 elements. Dilution factors of ≤ 340 were aspirated without matrix effects. To demonstrate the applicability of our method, 4 carbonaceous chondrites (Ivuna, Orgueil, Cold Bokkeveld and Allende) as well as GSJ and USGS silicate reference materials of basalts, andesites and peridotites were analyzed. Our analytical results are consistent with previous studies, and the mean reproducibility of each element is 1.0-4.6% for basalts and andesites, and 6.7-11% for peridotites except for TiO2.

Original languageEnglish
Pages (from-to)13-26
Number of pages14
JournalChemical Geology
Issue number1-2
Publication statusPublished - Jan 15 2007



  • Coprecipitation
  • Determination
  • Fluoride compounds
  • HFSE
  • ICP-MS
  • Silicate materials

ASJC Scopus subject areas

  • Geology
  • Geochemistry and Petrology

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