应用X射线荧光光谱法测定了海洋沉积物中12种元素(即硫、铝、铁、钙、钾、磷、钛、锰、氯、硅、钠及镁)。样品预先在120 ℃烘8 h后,称取0.500 0 g与5.000 g混合熔剂(四硼酸锂67 g与偏硼酸锂33 g混合)置于铂-金坩埚中混匀后,先在600 ℃预氧化200 s,使还原性物质充分氧化,随即升温至1 000 ℃熔融9 min。熔融物自动在坩埚内成型为样品,自动脱出后即可用于X射线荧光光谱法测定。用理论α系数法校正基体效应及元素间谱线重叠干扰。应用此方法分析了2个深海沉积物标准物质,所测得12种组分的结果与标准值一致。

XRFS was applied to the determination of 12 elements in sea sediments (including S, Al, Fe, Ca, K, P, Ti, Mn, Cl, Si, Na and Mg) with preparation of sample piece by fusion with mixed flux of Li2B4O7 and LiBO2 (67+33). A portion (0.500 0 g) of sample after dried at 120 ℃ for 8 h was mixed with 5.000 g of the flux in a Pt-Au crucible, pre-oxidized at 600 ℃ for 200 s and then fused at 1 000 ℃ for 9 min. The melt in the crucible was cooled and a disc-shaped sample piece was formed which after demoulding was used for XRFS determination of the elements. Matrix effect and interferences due to overlapping of spectral lines of co-existing elements were elininated by applying the theoratical α coefficient method. Two CRM′s of sea sediments were analyzed by the proposed method, giving results of 12 components in consistency with the certified values.