Rapid Analysis of Feldspar by X-ray Diffractometry Rietveld Refinement Method
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摘要: 长石中矿物的含量需要根据化学分析结果计算获得，分析流程长、计算复杂，而光学显微镜测定长石含量易受切片位置的影响。本文利用HighScore软件对长石样品进行X射线衍射全谱拟合分析，能有效降低衍射峰重叠影响，修正择优取向造成的衍射强度误差，方法的准确度优于参比法（RIR法）；样品定量分析结果与绝热法结果接近，相对偏差小于1.69%；与化学分析结果换算的矿物含量比较，绝对误差小于5%，满足了DZ/T 0130-2006所规定的绝对误差允许限。采用钾长石国家一级标准物质进行验证，主要矿物成分的分析误差小于1.34%，与钾长石化学成分标准值相比，绝对误差均小于1%。对长石物相进行定量分析的结果表明：X射线衍射全谱拟合法操作简单，分析质量能够满足相关标准对衍射分析的要求，用于地质实验中岩石矿物物相含量分析是可行的。Abstract: The content of minerals in feldspar can be calculated by chemical analytical results, but the analytical process is long and the calculation process is complex. Moreover, slice position could affect the result of feldspar content determined by optical microscopy. Feldspar samples were quantitatively analyzed using the Rietveld method in HighScore software. This method can effectively reduce the effect of diffraction peak overlap and correct the diffraction intensity error caused by the preferred orientation. The accuracy of the method is superior to the reference method (RIR method). The quantitative analysis results of the samples are close to the results of the adiabatic method, and the relative deviation is less than 1.69%. Compared to the mineral content by conversion from chemical composition, the absolute error is less than 5%, which meets the allowable error provided by DZ/T 0130-2006. As proved by first grade standard materials of potassium feldspar, the absolute error is less than 1%. The results of quantitative analysis of the feldspar show that the X-ray diffraction full-spectrum fitting method is simple and the analytical quality meets the quality requirements of the relevant standard for the diffraction analysis. It is feasible to analyze rock mineral content in geological samples using this method.
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Key words:
- X-ray Diffractometry /
- Rietveld refinement method /
- quantitative analysis /
- feldspar /
- phase composition
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表 1 样品Rietveld定量相分析结果和组成相的结构参数
Table 1. Rietveld quantitative phase analysis results and crystal structure data of samples
矿物名称 化学结构式 结构参数 含量 数据来源 a(Å) b(Å) c(Å) α(°) β(°) γ(°) Rietveld法 参比法(RIR法) 微斜长石 Al1K1O8Si3 7.2230 7.6230 7.9190 113.075 104.240 103.651 75.34 84 ICSD 7.2229 7.6352 7.9129 113.026 104.267 103.704 本研究 钠长石 Al0.91 Na1O8 Si3 7.1580 7.4370 7.7140 115.080 107.329 100.419 24.66 16 ICSD 7.1576 7.4456 7.7161 115.106 107.305 100.432 本研究 
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表 2 X射线衍射全谱拟合法与化学分析结果的比较
Table 2. A comparison of analytical results of ore determined by XRD and chemical analysis
矿物名称 全谱拟合分析结果(%) 化学分析结果换算(%) 绝对误差允许限(%) 绝对误差(%) 微斜长石 75.34 70.76 5.86 4.58 钠长石 24.66 24.86 2.04 0.20
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表 3 钾长石标准物质物相分析结果
Table 3. Phase analysis results of potassium feldspar standards
矿物名称 参考卡片 化学结构式 全谱拟合分析含量(%) 标准值换算含量(%) 绝对误差(%) 绝对误差允许限(%) 钾长石 01-072-1114 KAlSi3O8 56.6 56.74 0.14 4.24 钠长石 98-001-8020 (Na0.84Ca0.16)Al1.16Si2.84O8 36.2 37.54 1.34 2.73 石英 98-004-6143 SiO2 7.2 - - -
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表 4 GBW03116化学成分分析结果比较
Table 4. A comparison of analytical resuts of the chemical components in GBW03116 standard material
标准物质成分 化学成分标准值(%) 全谱拟合结果计算化学成分含量(%) 绝对误差(%) SiO2 66.26 67.19 0.93 Al2O3 18.63 18.45 0.18 K2O 9.60 9.58 0.02 Na2O 3.69 3.56 0.13 CaO 0.76 1.23 0.47
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