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詹秀春, 樊兴涛, 李迎春, 王袆亚. 直接粉末制样-小型偏振激发能量色散X射线荧光光谱仪分析地质样品中多元素[J]. 岩矿测试, 2009, 28(6): 501-506.
引用本文: 詹秀春, 樊兴涛, 李迎春, 王袆亚. 直接粉末制样-小型偏振激发能量色散X射线荧光光谱仪分析地质样品中多元素[J]. 岩矿测试, 2009, 28(6): 501-506.
ZHAN Xiuchun, FAN Xingtao, LI Yingchun, WANG Yiya. Multi-element Determination in Geological Materials by Bench-top Polarized Energy Dispersive Xray Fluorescence Spectrometer Coupled with Direct Powder Sample Preparation[J]. Rock and Mineral Analysis, 2009, 28(6): 501-506.
Citation: ZHAN Xiuchun, FAN Xingtao, LI Yingchun, WANG Yiya. Multi-element Determination in Geological Materials by Bench-top Polarized Energy Dispersive Xray Fluorescence Spectrometer Coupled with Direct Powder Sample Preparation[J]. Rock and Mineral Analysis, 2009, 28(6): 501-506.

直接粉末制样-小型偏振激发能量色散X射线荧光光谱仪分析地质样品中多元素

Multi-element Determination in Geological Materials by Bench-top Polarized Energy Dispersive Xray Fluorescence Spectrometer Coupled with Direct Powder Sample Preparation

  • 摘要: 采用小型偏振激发能量色散X射线荧光光谱仪,直接粉末制样法,分析了硅酸盐类岩石、土壤、沉积物样品。实验结果表明,主量元素的总分析精度优于2%(RSD),主要受制样精度控制。不同含量的痕量元素的总分析精度一般优于5%(RSD),含量低时可达约20%(RSD)。制样精度(方差)在分析总精度(方差)中所占的比例一般大于50%,且元素原子序数越小、含量越高(计数统计涨落小),所占的比例越大。实验还表明,对于大多数元素,在样品量大于1 g后,分析结果变化不显著;但Ba等重元素在样品量小于5 g时结果受样品量影响显著;实际分析中可以不必称量样品,但应保证所使用的样品量大于5 g。通过作为未知样品分析的标准参考物的分析结果和参校标准物质的回算结果的综合考察,并参照中国地质调查局多目标地球化学调查规范(1∶25万),作者认为,该方法在常规情况下可定量分析K、Ca、Ti、V、Cr、Mn、Fe、Ni、Cu、Zn、Ga、As、Rb、Sr、Y、Zr、Nb、Ba、Pb、Th等20种元素,过渡金属元素的测定限在10 mg/kg左右。由于制样方法简单,无需制样设备,该方法适合于车载野外现场快速分析。

     

    Abstract: A benchtop type Polarized Energy dispersive X-ray fluorescence spectrometer coupled with direct powder sample preparation technique has been used to analyze silicate rocks, soils and sediments. About 50 elements can be simultaneously monitored, among which 20 elements (including K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, As, Rb, Sr, Y, Zr, Nb, Ba, Pb, Th) can be quantified in accordance with the regulation on mulitipurpose geochemical survey (1∶250000) issued by China Geological Survey and about 10 more elements can also be determined with less accuracy. Repeated sampling experiments showed that the analysis precisions for major elements were better than 2%(RSD) and mainly affected by sample preparation. For trace elements, the analysis precisions were generally better than 5%(RSD) and would be worse (up to 20%RSD) for very low concentrations. Generally, sample preparation contributed more than 50% to the total analysis variations. And this contribution increased with lower atomic numbers and higher concentrations. Different sampling mass would cause obvious result changes for such elements as Sn and Ba whose high energy K lines were used for measurements, but would not when sampling mass exceeded 1 g for elements with analysis line energies less than that of the Compton lines of Mo Ka which was used as the internal standard. Sampling mass need not be controlled if ensured to exceed 5 g. The method is suited for onsite geochemical analysis for its simplicity and its powerful measurement capability.

     

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