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熔融制样-X射线荧光光谱法测定海洋沉积物中氯等元素 被引量:13

XRFS Determination of Chlorine etc Multi-Elements in Sea Sediments with Sample Preparation by Fusion
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摘要 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8h后,称取0.500 0g与5.000g混合熔剂(四硼酸锂67g与偏硼酸锂33g混合)置于铂-金坩埚中混匀后,先在600℃预氧化200s,使还原性物质充分氧化,随即升温至1 000℃熔融9min。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.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2011年第12期1420-1423,共4页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 X射线荧光光谱法 海洋沉积物 融熔法制样 理论α系数法 XRFS Sea sediments Sample preparation by fusion Theoratical α coefficient
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