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首页> 外文期刊>Journal of Alloys and Compounds: An Interdisciplinary Journal of Materials Science and Solid-state Chemistry and Physics >Trace element analysis by means of synchrotron radiation, XRF, and PIXE: selection of sample preparation procedure
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Trace element analysis by means of synchrotron radiation, XRF, and PIXE: selection of sample preparation procedure

机译：通过同步辐射，XRF和PIXE进行痕量元素分析：选择样品制备程序

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摘要

When it comes to biological samples, trace element (TE) determination has to cope with very low concentrations, sometimes even below the minimum detectable limit (MDL). This is why special sample preparation procedures have to be employed so that the TE concentration in the specimen is effectively enhanced in a known way. The aim of this study was the selection of a proper sample preparation procedure by determination of selected element concentrations in different types of biological samples. In this work several sample preparation procedures were applied in order to choose the best one for specific experimental needs. The methods included: (a) tissue sectioning method (if appropriate); (b) dry method without chemical treatment - the samples were dried, homogenized and pressed into pellet; (c) wet method with chemical treatment - the samples were mineralized. The analyses were performed with different analytical methods in order to confirm the results obtained and in order to determine the influence of target preparation procedure on the level of elemental concentrations determination. The measurements were done by means of SRIXE (synchrotron radiation induced X-ray emission), EDXRF (energy dispersive X-ray fluorescence), TR-XRF (total reflection X-ray fluorescence), and PIXE (proton-induced X-ray emission). The above methods are described and the analytical results discussed. The results of the elemental analyses performed with different techniques show a good agreement only for some elements. The mineralization process increases the sensitivity of elemental determination only for selected elements. In other cases one could observe decreasing of elemental concentration in respect to non mineralized samples. Selection of sample preparation procedure depends on analytical requirements.
机译：对于生物样品，痕量元素（TE）的测定必须处理非常低的浓度，有时甚至低于最低可检测限（MDL）。这就是为什么必须采用特殊的样品制备程序，以便以已知方式有效提高样品中TE浓度的原因。这项研究的目的是通过确定不同类型的生物样品中所选元素的浓度来选择合适的样品制备程序。在这项工作中，采用了几种样品制备程序，以便为特定的实验需求选择最佳的程序。这些方法包括：（a）组织切片法（如果适用）; （b）未经化学处理的干燥方法-将样品干燥，均质并压成颗粒; （c）湿法化学处理-将样品矿化。为了确认获得的结果并确定目标制备程序对元素浓度测定水平的影响，使用了不同的分析方法进行了分析。测量是通过SRIXE（同步辐射诱发的X射线发射），EDXRF（能量分散X射线荧光），TR-XRF（全反射X射线荧光）和PIXE（质子诱发的X射线发射）完成的）。描述了上述方法并讨论了分析结果。使用不同技术进行的元素分析结果仅对某些元素显示出良好的一致性。矿化过程仅对选定元素增加了元素测定的灵敏度。在其他情况下，可以观察到相对于非矿化样品而言元素浓度降低。样品制备程序的选择取决于分析要求。

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