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李迎春, 张磊, 周伟, 尚文郁. 熔融制样-波长色散和能量色散X射线荧光光谱仪应用于硅酸盐类矿物及疑难样品分析[J]. 岩矿测试, 2020, 39(6): 828-838. DOI: 10.15898/j.cnki.11-2131/td.201912250178
引用本文: 李迎春, 张磊, 周伟, 尚文郁. 熔融制样-波长色散和能量色散X射线荧光光谱仪应用于硅酸盐类矿物及疑难样品分析[J]. 岩矿测试, 2020, 39(6): 828-838. DOI: 10.15898/j.cnki.11-2131/td.201912250178
LI Ying-chun, ZHANG Lei, ZHOU Wei, SHANG Wen-yu. Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling[J]. Rock and Mineral Analysis, 2020, 39(6): 828-838. DOI: 10.15898/j.cnki.11-2131/td.201912250178
Citation: LI Ying-chun, ZHANG Lei, ZHOU Wei, SHANG Wen-yu. Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling[J]. Rock and Mineral Analysis, 2020, 39(6): 828-838. DOI: 10.15898/j.cnki.11-2131/td.201912250178

熔融制样-波长色散和能量色散X射线荧光光谱仪应用于硅酸盐类矿物及疑难样品分析

Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling

  • 摘要: 目前硅酸盐类样品中主量元素一般采用熔融制样X射线荧光光谱法(XRF)测定,不仅单元素测定结果不能超差,而且百分数加和也要满足要求。但对于矿化样品,由于微量元素较高,往往造成不能满足加和质量要求。充分利用波长色散(WD)和能量色散(ED)复合式X射线荧光光谱仪同时波谱、能谱测定的优势,可使分析人员快速掌握样品组成信息,对评估矿化样品数据质量具有重要意义。本文利用波长-能量色散X射线荧光光谱仪,可在测定主量元素的同时加入更多的微量元素进行测定,而分析时间不延长。主量元素采用波长色散定量,次量元素主要采用能量色散测定,在保证主量元素准确度的情况下,合理设置测量条件,延长能谱测量时间,实现在波长色散12min左右测定主量元素的同时,能够提供14个微量元素如Rb、Sr、Y、Zr、Ba、Cu、Zn的测定结果和10个线性范围较窄或含量较低元素如Co、Ge、Pr、Ta的参考结果,24个微量元素最大检出限为16.76μg/g。通过准确度考核,主量元素测定结果与认定值基本一致,高含量微量元素测定结果亦满足定量分析要求。该方法可使分析人员快速掌握样品组成信息,为提供更加准确、可靠的数据奠定基础,有效地解决矿化疑难样品主量元素测定问题。

     

    Abstract:
    BACKGROUNDAt present, the major elements in silicate samples are generally determined by X-ray fluorescence spectrometry with fusion sample preparation. Not only can the single element determination results not exceed the limit, but also the percentage sum must meet the requirements of sum quality (99.3%-100.7%). However, for the analysis of mineralized samples, due to the high content of trace elements, it is often not possible to meet the requirements of sum quality. The wavelength and energy dispersive X-ray fluorescence spectrometer are fully utilized. The advantages of the determination can make the analysts to get the information of sample composition as soon as possible, which is of great significance to evaluate the data quality of mineralized samples.
    OBJECTIVESTo develop a method for determination of major elements in mineralized samples.
    METHODSThe wavelength-energy dispersive X-ray fluorescence spectrometer was used to determine the major elements while adding more minor elements to the determination without prolonging the analysis time. The main elements were quantified by wavelength dispersion, while the minor elements were mainly determined by energy dispersion. Under the condition of ensuring the accuracy of the major elements, the measurement conditions were reasonably set and the energy spectrum measurement time was extended.
    RESULTSThe method achieved the measurement of the major elements within 12 minutes using wavelength dispersion, and also provided results of 14 minor elements such as Rb, Sr, Y, Zr, Ba, Cu, Zn and the semi-quantitative results of 10 elements with narrow linear range or low content such as Co, Ge, Pr and Ta. The maximum limit of detection of 24 minor elements was 16.76μg/g.
    CONCLUSIONSThrough the accuracy assessment, the determination results of major elements are consistent with the certified values, and the determination of minor elements with high content also meets the requirements of quantitative analysis. This method makes the analysts to get the information of sample composition quickly, provides a basis for more accurate and reliable data, and effectively solves the determination of major elements in complex mineralized samples.

     

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