A Method for Estimating Micro-area Composition of Quartz-diorite Based on Quantitative Mapping of Electron Probe Microanalysis
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摘要:
岩石的微区成分特征是精细化反演岩石演化的重要依据，而常规的电子探针面扫描分析方法无法提供面扫描区域的定量分析结果。本文使用矿物分布相对均匀的代表性岩石样品开展了岩石薄片的面扫描和矿物的定量分析。通过对常规测试的主量元素的面扫描进行图像校正，并利用ZAF校正后的点分析数据与面扫描图像的灰度值进行最小二乘法曲线拟合的方式，实现了X射线强度与质量浓度的转换。对比全岩X射线荧光光谱(XRF)测试数据，电子探针面扫描定量化方法的主量元素SiO2、CaO、FeO、Al2O3、TiO2的相对误差在10%以内，且相对标准偏差(RSD)不高于12%，具有良好的一致性；MgO和Na2O的相对误差与标准偏差略大，可通过多次测量加以改善；K2O由于缺乏富钾硅酸盐矿物的定量分析数据，导致结果不精确。研究表明，在仪器测试条件良好的情况下使用电子探针定量数据校正面扫描图像，可对矿物分布较均匀的岩石开展微区成分分析，给出估计结果，并通过多个切面的多次测量等方式，减少来自矿物形态、粒径大小、分布的影响。
Abstract:BACKGROUND The estimation of bulk composition of the micro-area of a rock is an important basis of tracing rock evolution. The conventional electron probe microanalysis (EPMA) mapping method cannot provide quantitative analysis results of the surface scanning area.
OBJECTIVES In order to estimate the composition of the micro-area by quantitative mapping of EPMA.
METHODS The mapping and point analyses were carried out to determine the composition of the micro-area of a homogeneous quartz-diorite. By performing image correction of the pixels of the mapping of the major elements, and using the point analysis data after ZAF correction and the gray value of the surface scan image to perform the least square curve fitting method, the X-ray intensity and concentration were converted.
RESULTS By comparing to X-ray fluorescence spectrometry (XRF), the relative errors of SiO2, CaO, FeO, Al2O3 and TiO2 of EPMA method were within 10%, and the relative standard deviation was less than 10%. The relative error and standard deviation of MgO and Na2O were slightly larger, which can be improved by multiple measurements. The K2O content were not accurate due to lack of K-rich silicate minerals' point analysis.
CONCLUSIONS The results show that the estimation of micro-area composition of a rock with relatively homogeneous mineral distributions can be carried out by using point analyses of EPMA to correct the mapping under good instrument conditions, and the influence of mineral morphology, particle size, and distribution can be reduced by multiple measurements on different sections.
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表 1 斜长石和角闪石电子探针分析结果
Table 1. Electron probe microanalysis results of plagioclase and amphibole
成分 斜长石不同测试点位的分析结果(%) 角闪石不同测试点位的分析结果(%) 1 2 11 13 17 18 23 24 3 4 5 7 8 9 15 16 19 25 26 SiO2 57.83 56.74 56.74 56.54 56.89 57.67 57.78 57.25 45.82 47.71 47.08 46.36 47.17 46.72 46.50 45.66 46.68 47.66 45.85 TiO2 0.00 0.00 0.00 0.08 0.00 0.00 0.00 0.00 2.28 1.03 1.14 1.28 1.31 1.47 1.95 2.39 1.85 1.19 2.26 Al2O3 27.03 27.80 28.07 28.28 28.28 28.28 27.57 25.23 8.30 7.33 7.64 7.20 7.63 7.82 8.00 8.58 7.80 7.17 8.35 FeO 0.19 0.13 0.18 0.08 0.11 0.10 0.10 0.04 15.22 15.12 15.35 15.01 14.44 15.49 14.88 14.27 14.66 14.63 14.88 MnO 0.00 0.02 0.00 0.00 0.01 0.00 0.02 0.00 0.47 0.44 0.38 0.48 0.50 0.48 0.45 0.48 0.45 0.50 0.49 MgO 0.02 0.03 0.00 0.00 0.02 0.02 0.01 0.00 12.24 12.54 12.47 12.76 12.41 12.32 11.92 12.27 12.49 12.64 12.29 CaO 8.49 9.47 9.47 9.91 9.59 8.88 8.62 6.96 11.10 11.74 11.73 11.34 11.35 11.24 11.28 11.41 11.16 11.68 10.94 Na2O 6.44 6.26 6.17 5.71 6.08 6.18 6.37 7.41 1.23 0.85 0.74 1.00 1.06 1.05 1.23 1.17 1.16 0.92 1.39 K2O 0.19 0.16 0.17 0.08 0.13 0.21 0.11 0.08 0.49 0.50 0.52 0.44 0.47 0.49 0.49 0.54 0.44 0.49 0.49 总含量 100.19 100.61 100.80 100.67 101.11 101.33 100.57 96.98 97.14 97.26 97.05 95.86 96.33 97.08 96.70 96.76 96.69 96.87 96.94 O 8.02 7.99 8.00 8.03 8.00 8.02 8.02 7.98 23.00 23.00 23.00 23.00 23.00 23.00 23.00 23.00 23.00 23.00 23.00 Si 2.59 2.53 2.53 2.53 2.53 2.56 2.58 2.63 6.55 6.79 6.71 6.70 6.77 6.67 6.67 6.55 6.68 6.80 6.57 Ti 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.25 0.11 0.12 0.14 0.14 0.16 0.21 0.26 0.20 0.13 0.24 Al 1.42 1.46 1.47 1.49 1.48 1.48 1.45 1.37 1.40 1.22 1.28 1.23 1.29 1.32 1.35 1.45 1.32 1.21 1.40 Fe 0.01 0.01 0.01 0.00 0.04 0.00 0.00 0.01 1.82 1.80 1.83 1.82 1.73 1.85 1.78 1.71 1.75 1.75 1.78 Mn 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.06 0.05 0.05 0.06 0.06 0.06 0.05 0.06 0.05 0.06 0.06 Mg 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 2.60 2.66 2.65 2.75 2.65 2.62 2.55 2.62 2.67 2.69 2.62 Ca 0.41 0.45 0.45 0.48 0.46 0.42 0.41 0.34 1.70 1.80 1.80 1.76 1.74 1.72 1.73 1.75 1.71 1.79 1.69 Na 0.56 0.54 0.53 0.50 0.52 0.53 0.55 0.66 0.34 0.24 0.20 0.28 0.30 0.30 0.34 0.32 0.32 0.26 0.39 K 0.01 0.01 0.01 0.00 0.01 0.01 0.01 0.01 0.09 0.09 0.10 0.08 0.09 0.09 0.09 0.10 0.08 0.09 0.09 总阳离子数 5.00 5.00 5.00 5.00 5.04 5.00 5.00 5.01 16.81 16.75 16.75 16.81 16.77 16.78 16.77 16.83 16.79 16.77 16.83 An 41.64 45.13 45.46 48.74 46.20 43.73 42.52 34.01 Ab 57.22 53.96 53.56 50.81 53.03 55.04 56.85 65.51 Or 1.13 0.90 0.98 0.45 0.77 1.23 0.63 0.48 
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表 2 石英、磁铁矿、磷灰石、绿帘石和黑云母电子探针分析结果
Table 2. Electron probe microanalysis results of quartz, magnetite, apatite, epidote and biotite
成分 石英不同测试点位分析结果(%) 磁铁矿不同测试点位分析结果(%) 磷灰石不同测试点位分析结果(%) 绿帘石不同测试点位分析结果(%) 黑云母不同测试点位分析结果(%) 10 6 12 14 20 21 22 27 28 29 SiO2 99.77 0.04 0.04 0.05 0.06 0.06 0.11 36.52 35.49 34.87 TiO2 0.00 0.06 0.01 0.01 0.02 0.00 0.00 0.00 2.831 2.59 Al2O3 0.00 0.04 0.06 0.07 0.18 0.00 0.01 20.97 15.79 15.83 FeO 0.06 95.10 96.12 95.98 95.44 0.00 0.05 17.22 17.57 18.30 MnO 0.00 0.05 0.07 0.12 0.14 0.04 0.06 0.00 0.00 0.00 MgO 0.00 0.00 0.00 0.04 0.03 0.02 0.00 0.00 12.12 12.24 CaO 0.02 0.00 0.00 0.00 0.00 53.01 53.06 23.05 0.03 0.09 Na2O 0.01 0.03 0.01 0 0.04 0.09 0.14 0.00 0.08 0.09 K2O 0.00 0.01 0.00 0.00 0.00 0.00 0.01 0.00 9.14 8.36 P2O5 - - - - - 46.77 46.56 - - - 总含量 99.86 95.32 96.30 96.27 95.90 99.99 100.00 97.76 93.05 92.37 O 2.00 4.00 4.00 4.00 4.00 12.00 12.00 12.50 12.00 12.00 Si 0.997 0.002 0.002 0.003 0.003 0.004 0.008 2.92 2.73 2.73 Ti 0.000 0.002 0.000 0.000 0.001 0.000 0.000 0.00 0.15 0.15 Al 0.000 0.002 0.004 0.004 0.010 0.000 0.001 1.98 1.46 1.46 Fe 0.000 3.984 3.987 3.981 3.967 0.000 0.003 1.15 1.20 1.20 Mn 0.000 0.002 0.003 0.005 0.006 0.003 0.004 0.00 0.00 0.00 Mg 0.000 0.000 0.000 0.003 0.003 0.002 0.000 0.00 1.43 1.43 Ca 0.000 0.000 0.000 0.000 0.000 4.367 4.377 1.97 0.01 0.01 Na 0.000 0.002 0.001 0.000 0.004 0.013 0.021 0.00 0.01 0.01 K 0.000 0.001 0.000 0.000 0.000 0.000 0.001 0.00 0.83 0.83 P - - - - - 3.045 3.035 - - - 总阳离子数 1.00 4.00 4.00 4.00 3.99 7.43 7.45 9.02 7.82 7.82
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表 3 面扫描定量化微区分析结果与全岩XRF分析结果对比
Table 3. Comparison between estimated results from quantified mapping and bulk XRF data
原样品号 SiO2 CaO K2O TFe2O3 Na2O MgO Al2O3 TiO2 XRF：全岩GC01-1(%) 52.12 7.20 1.50 8.72 4.28 4.75 18.16 1.16 XRF：全岩GC01-3(%) 57.09 6.72 1.15 6.98 4.19 3.38 16.95 0.99 电子探针面扫描定量化(%) 56.10 7.40 0.66 7.38 3.50 3.52 16.80 0.93 相对误差(%) 1.81 4.13 -40.18 -4.07 -12.28 -9.36 -2.91 -9.42 RSD(%) 4.77 4.92 38.24 11.85 10.70 19.41 4.31 11.62 注：相对误差=(实际值-真实值)/真实值×100；标准偏差： $ s = \sqrt {\sum {{({x_i} - x)}^2}/(n{\rm{ - }}1)} $ ；相对标准偏差(RSD)＝标准偏差/平均值×100；FeO=0.9×Fe2O3。
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表 4 定量化面扫描与面扫描定量化处理方式的对比
Table 4. Comparison of different processing methods of quantitative mapping
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