A Correction Method and Affecting Factors on Element Analysis Results with Varied Diameters of Round-Bar Specimens by Electric Spark-Direct Reading Spectrometry
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摘要: 在实际工作中发现，电火花直读光谱法直接分析圆棒试样时，圆棒试样直径的大小会对各元素测定结果产生影响。本文在40 mm厚合金钢板上制备出直径为Φ25 mm、Φ12 mm、Φ8 mm、Φ6 mm、Φ4 mm、Φ3 mm等系列试样，采用电火花直读光谱法研究了圆棒试样直径对元素测定的影响。结果表明，随着圆棒试样直径的减小，碳硫锰磷铬镍铜和锡的测定值偏大，硅的测定值略偏小，钼和钒的测定值偏小；各元素测定结果的变化与其挥发性和存在形态相关。为了校正各元素的测定结果，本文提出曲线插入法的校正方法，采用标准物质进行测定，各元素经过校正的测定值与标准值的绝对差值都小于相应方法规定的实验室间允差(R)，证明了曲线插入校正方法的可行性，改善了直读光谱分析的准确度，可以适用于直径Φ3 mm以上圆棒试样的直接分析。Abstract: The variation of element analysis results related to the diameter of round-bar specimens by Electric Spark-Direct Reading Spectrometry was uncovered during experimental work. A series of specimens, with diameters of Φ25 mm, Φ12 mm, Φ8 mm, Φ6 mm, Φ4 mm and Φ3 mm, were prepared from a 40 mm thick alloy steel plate. All the round-bar specimens were analyzed by using direct-reading spark spectrometry. The results indicate that the specimen with the smallest diameter has the highest content reading of C, S, Mn, P, Cr, Ni, Cu and Sn, slightly lower content reading of Si and low content reading of Mo and V. The variation of content readings is related to the volatility and occurrence form of the target element. In order to correct the results, a curve interpolation method was applied. A CRM was analyzed and corrected, the element deviation between the content result and certified value was less than the tolerance between laboratories (R), and the feasibility of the method was confirmed. This method is suitable for round-bar specimens with more than Φ3 mm in diameter.
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表 1 分析元素及测定范围
Table 1. Analytical element and its determination range
分析元素 分析线
(nm)内参比线
(nm)测定范围
(%)组合光源 C 165.812Ⅰ Fe1 163.5Ⅰ 0.00050～2.50 火花放电1 Si 288.160Ⅰ Fe3 282.3Ⅰ 0.00060～1.60 火花放电3 Mn 293.306Ⅱ Fe3 297.1Ⅱ 0.00020～1.50 火花放电3 P 178.287Ⅰ Fe1 217.8Ⅰ 0.00030～0.150 火花放电1 S 180.731Ⅰ Fe1 217.8Ⅰ 0.00020～0.330 火花放电1 Cr 312.260Ⅱ Fe3 297.1Ⅱ 2.00～30.00 火花放电3 Ni 231.604Ⅱ Fe1 163.9Ⅱ 0.00040～1.00 火花放电3 Mo 281.615Ⅱ Fe3 239.1Ⅱ 0.00080～2.50 火花放电3 Cu 324.754Ⅰ Fe3 281.3Ⅰ 0.0001～0.20 火花放电2 V 310.230Ⅱ Fe2 297.1Ⅱ 0.0002～0.60 火花放电2 Al 396.153Ⅰ Fe3 281.3Ⅰ 0.00010～0.300 火花放电3 Co 345.351Ⅰ Fe3 281.3Ⅰ 0.000040～0.100 火花放电2 Sn 147.515 Ⅰ Fe4 149.7Ⅰ 0.0002～0.20 火花放电4 
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表 2 圆棒试样的分析结果
Table 2. Analytical results of round-bar specimens
直径
(mm)各元素的含量
(%)C S Si Mn P Cr Ni Mo Cu V Sn Φ25 0.885 0.0029 0.920 0.528 0.0146 7.702 0.103 2.51 0.060 0.513 0.0018 Φ12 0.889 0.0027 0.921 0.532 0.0144 7.704 0.101 2.50 0.061 0.513 0.0017 Φ8 0.931 0.0034 0.924 0.541 0.0167 7.749 0.104 2.37 0.064 0.512 0.0023 Φ6 0.950 0.0033 0.908 0.547 0.0168 7.898 0.104 2.23 0.067 0.501 0.0026 Φ4 0.977 0.0037 0.894 0.579 0.0171 7.942 0.111 2.05 0.073 0.468 0.0033 Φ3 1.005 0.0044 0.904 0.585 0.0194 7.972 0.116 1.81 0.083 0.465 0.0040
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表 3 标准物质分析
Table 3. Analysis results of certified reference materials
项目 各元素的含量(%) C S Si Mn P Cr Ni Mo Cu V 标准物质的测定值 0.386 0.0079 0.715 0.806 0.0309 9.70 0.528 0.191 0.423 0.193 校正因子(f) 0.9059 0.7871 1.0299 0.9120 0.8551 0.9698 0.9293 1.3124 0.8165 1.0965 校正后的报出值 0.350 0.0062 0.736 0.735 0.0264 9.40 0.490 0.250 0.345 0.211 标准物质的标准值 0.340 0.0054 0.772 0.740 0.0262 9.37 0.461 0.244 0.374 0.201 报出值与标准值的绝对差值 0.010 0.0008 0.036 0.005 0.0002 0.03 0.029 0.006 0.029 0.010 实验室间允差(R) 0.063 0.0023 0.042 0.040 0.0044 0.26 0.046 0.018 0.030 0.017
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