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同步辐射X射线荧光光谱测定沉积物中元素含量的归一方法研究——以四海龙湾纹层沉积物为例

DOI: 10.3969/j.issn.1001-7410.2014.06.22, PP. 1327-1335

Keywords: 同步辐射,X射线荧光光谱分析,归一方法,元素谱线强度,元素含量

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Abstract:

同步辐射X射线荧光光谱分析(SRXRF)是一种基于同步加速器光源与X射线荧光光谱分析(XRF)相结合的原位分析方法,可以直接对沉积物进行扫描获得每个点的能谱图,从而计算元素含量的相对变化。但是由于荧光光谱定性和定量分析中存在的问题,国内发表文献中各种XRF原位分析数据均以相对含量或者计数表示。本文通过对各种标准物质(土壤、沉积物和岩石)的SRXRF分析,结合标准样品的定量数据,对同步辐射X射线荧光光谱的定量方法进行了研究。鉴于元素质量数和谱线强度的差异,不同元素需要运用不同的归一方法。对于K和Ca元素,采用ROI0-195背景归一;Ti元素采用ROI293-303背景归一;Mn元素采用ROI214-222背景归一;而较高序数的元素Fe采用拟合康普顿散射峰归一。通过上述归一方法,我们获得了K、Ca、Ti、Mn和Fe元素的定量标准曲线,相关系数分别为0.89、0.98、0.96、0.93和0.98。运用标准样品对各元素的定量标准曲线进行检验,结果表明:Fe元素含量预测的平均相对偏差小于10%,K、Ca和Ti的平均相对偏差小于20%,Mn的相对偏差较大,为35.9%。从总体上看,SRXRF获得的数据可以基本满足湖泊沉积物中元素分析的定量化需求。为验证SRXRF方法能否揭示元素含量的季节性变化,我们对四海龙湾纹层沉积物进行了分析,按选定的归一方法计算样品中元素特征谱线的强度,利用各元素的标准曲线计算岩芯沉积物中元素含量。K、Ca、Ti、Mn和Fe元素含量具有明显的季节韵律变化,浅色碎屑微层中Ti和Ca含量较高,而Mn和Fe丰度的高值对应于暗色有机质-碎屑混合层。初步研究结果表明同步辐射X射线荧光光谱分析可以揭示湖泊中沉积的元素的季节性变化,对研究过去季节-年尺度的古气候、古环境变化具有重要的科学意义。

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