Cherkashina T Yu, Shtel'makh S I, Pashkova G V
Institute of the Earth's Crust, SB RAS, 128 Lermontov St., Irkutsk 664033, Russia.
Institute of the Earth's Crust, SB RAS, 128 Lermontov St., Irkutsk 664033, Russia.
Appl Radiat Isot. 2017 Dec;130:153-161. doi: 10.1016/j.apradiso.2017.09.038. Epub 2017 Sep 23.
A simple, rapid and non destructive Wavelength Dispersive X-ray Fluorescence Spectrometry (WDXRFS) was developed for the determination of trace elements such as V, Cr, Co, Ni, Cu, Zn, Pb, Ba, La, Ce, Nd, Rb, Sr, Y, Zr, and Nb in carbonate rocks with high calcium content. Samples of marble, limestone, fluorite ore and carbonatite-like rocks were chosen as objects under investigation. These samples have wide ranges of major and trace element contents, and high concentration of calcite (70-98%) in calcium rich carbonates. The sample mass required for infinite thickness was calculated for each element. In order to determine V, Cr, Co, Ni, Cu, Zn, Ba, La, Nd, Ce, sample weighting 1g was pressed with a pressure of 100kN. For the determination of Rb, Sr, Y, Zr, Nb, Pb, the sample mass was increased up to 5g. The calibration curves were constructed by employing the International Certified reference materials (ICRMs) and in-house standard reference materials (HSRMs) of various types of rocks and sediments, and the matrix effects were taken into account using the influence coefficients (α-correction equations). Analytical figures of merit have also been assessed. The calculated values of the instrumental limit of the detection were within the interval from 0.5 to 4.0mgkg. The repeatability and reproducibility were found to be satisfactory with the relative standard deviations lower than 5%. The accuracy was evaluated by the analysis of two reference materials and the comparison with the ICP-MS results. A good agreement was achieved between the reference and measured values with recoveries ranging from 85% to 115%. The relative disagreements between the XRF and ICP-MS results were less than 10%.
开发了一种简单、快速且无损的波长色散X射线荧光光谱法（WDXRFS），用于测定高钙含量碳酸盐岩中的痕量元素，如V、Cr、Co、Ni、Cu、Zn、Pb、Ba、La、Ce、Nd、Rb、Sr、Y、Zr和Nb。选取大理石、石灰石、萤石矿和类碳酸岩岩石样品作为研究对象。这些样品的主量和痕量元素含量范围广泛，富钙碳酸盐中方解石浓度较高（70 - 98%）。计算了每种元素达到无限厚度所需的样品质量。为了测定V、Cr、Co、Ni、Cu、Zn、Ba、La、Nd、Ce，称取1g样品，在100kN压力下压片。对于Rb、Sr、Y、Zr、Nb、Pb的测定，样品质量增加至5g。采用各种类型岩石和沉积物的国际认证参考物质（ICRM）和内部标准参考物质（HSRM）构建校准曲线，并使用影响系数（α校正方程）考虑基体效应。还评估了分析性能指标。计算得到的仪器检测限数值在0.5至4.0mg/kg范围内。发现重复性和再现性令人满意，相对标准偏差低于5%。通过分析两种参考物质并与ICP-MS结果进行比较来评估准确性。参考值与测量值之间达成了良好的一致性，回收率在85%至115%之间。XRF和ICP-MS结果之间的相对偏差小于10%。
