ABSTRACT

In view of the requirement of a well-characterized and easily available aquatic sediment reference material, a comprehensive analysis comprising of fifty major, minor and trace elements as well as Sr-Nd-Pb-Hf isotopes were carried out in the stream sediment reference material, JSd-1, issued by the Geological Survey of Japan. The data for marine sediment reference material, MAG-1, issued by U.S. Geological Survey is also obtained for comparison. The elements were divided into two groups: Group I and Group II. Elements in Group I form stable soluble ions in HNO₃; and those in Group II form soluble oxo- and fluoro-complexes in HF, such as Zr, Nb, Hf, Ta, etc. For Group I, the sample was decomposed with HF in a tetra fluoro ethylene (TFE) bomb at 245°C for 96 hrs with Mg addition. The elemental concentration was measured by quadrupole type inductively coupled plasma source mass spectrometry (ICP-QMS) and sector field type ICP-MS (ICP-SFMS) using isotope dilution-internal standardization (ID-IS) methods. The aliquot of the sample solution was passed through 3-step column chemistry for isotope ratio determination of Pb by multiple collector (MC) ICP-MS and thermal ionization mass spectrometry (TIMS), and Sr and Nd by TIMS. For Group II elements, the sample was decomposed with HF in a TFE bomb with the same time and temperature settings. Zr, Mo, Sn, Sb and Hf were determined by ID, and Nb and Ta by ID-IS using ICP-QMS. The original JSd-1 powder showed heterogeneity for Group II elements, indicating insufficient pulverization and distribution. Thus, we further pulverized the powder and measured the concentration, which showed improved homogeneity. The aliquot for the re-pulverized powder was passed through 2-step column chemistry, and the Hf isotope ratio was determined by MC-ICP-MS. Thus a new data on the trace elements as well as Sr-Nd-Pb-Hf isotope ratios is provided for JSd-1 and MAG-1 in this paper.