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李大勇, 朱志雄, 李靖, 王亮. X射线荧光光谱法半定量分析高烧失量矿物的准确度研究[J]. 岩矿测试, 2020, 39(1): 135-142. DOI: 10.15898/j.cnki.11-2131/td.201903080034
引用本文: 李大勇, 朱志雄, 李靖, 王亮. X射线荧光光谱法半定量分析高烧失量矿物的准确度研究[J]. 岩矿测试, 2020, 39(1): 135-142. DOI: 10.15898/j.cnki.11-2131/td.201903080034
LI Da-yong, ZHU Zhi-xiong, LI Jing, WANG Liang. Accuracy Research of Minerals with High Loss of Ignition during X-ray Fluorescence Spectrometry Semi-quantitative Analysis[J]. Rock and Mineral Analysis, 2020, 39(1): 135-142. DOI: 10.15898/j.cnki.11-2131/td.201903080034
Citation: LI Da-yong, ZHU Zhi-xiong, LI Jing, WANG Liang. Accuracy Research of Minerals with High Loss of Ignition during X-ray Fluorescence Spectrometry Semi-quantitative Analysis[J]. Rock and Mineral Analysis, 2020, 39(1): 135-142. DOI: 10.15898/j.cnki.11-2131/td.201903080034

X射线荧光光谱法半定量分析高烧失量矿物的准确度研究

Accuracy Research of Minerals with High Loss of Ignition during X-ray Fluorescence Spectrometry Semi-quantitative Analysis

  • 摘要: 应用X射线荧光光谱半定量分析软件(SQX)分析未知样品时,SQX软件可对样品中的9F~92U元素进行半定量分析,而对H2O、C这些参数不能直接测定。对于烧失量和结晶水含量较高的铝土矿、CO2含量较高的碳酸盐矿物、硫碳含量较高的硫化物金属矿等样品,平衡归一化计算时,未测定参数对样品中的Al2O3、SiO2、CaO、MgO、Fe等主要元素分析结果影响较大,半定量分析数据的准确度较低。本文通过试验研究,提出了一种校正模式。该校正模式根据XRF半定量分析初步结果,选择性地对未知样品中的烧失量、结晶水、二氧化碳、硫等参数进行化学定量分析,将化学定量分析结果输入SQX,二次平衡归一计算得出新的半定量分析结果。实验结果表明,使用该校正模式分析铝土矿、碳酸盐矿物、硫化物金属矿中的多元素,平均准确度提高了2.6~4.5倍。本方法可快速、较为准确地测定铝土矿、碳酸盐矿物、硫化物金属矿等高烧失量矿物中的多元素。

     

    Abstract:
    BACKGROUNDThe SQX, X-ray fluorescence spectrometry semi-quantitative analysis software, was used to analyze an unknown sample. The software can analyze the range of 9F-92U elements, but cannot directly analyze the parameters such as H2O and C. Employing the balanced normalized calculation to test a special sample, such as bauxite with high loss of ignition and high crystalliferous water content, carbonate minerals with higher CO2 content, sulfide metal minerals with higher sulfur and carbon content, the analysis results for main elements like Al2O3, SiO2, CaO, MgO and Fe are largely affected by undetermined parameters resulting in low accuracy of semi-quantitative analysis data.
    OBJECTIVESTo propose a new calibration mode through experimental research.
    METHODSThe calibration mode quantitatively and selectively analyzes the parameters such as loss of ignition, crystalliferous water, carbon dioxide and sulfur of an unknown sample, based on the preliminary results of semi-quantitative analysis. By putting the quantitative analysis result into SQX, the new semi-quantitative analysis results were obtained by using the second equilibrium normalization calculation.
    RESULTSThe experimental results show that the average accuracy of multi-element in bauxite, carbonate minerals and sulfide metal minerals was increased by 2.6 to 4.5 times using this calibration mode.
    CONCLUSIONSThe method can quickly and accurately determine multi-element in minerals with high loss of ignition, including bauxite, carbonate minerals, and sulfide metal minerals.

     

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