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采用激光剥蚀电感耦合等离子体质谱法(LA-ICP-MS),以NIST玻璃标准物质制作校准曲线,29Si为内标,相对灵敏度因子(RSF)校准标样和样品间的基体效应,对碳化硅陶瓷器件中9种痕量元素(B,Ti,Cr,Mn,Fe和Ni等)进行定量测定。选择线性扫描方式,激光剥蚀孔径为150μm,氦气和氩气流量为0.7 L/min时,信号稳定性和灵敏度最佳。经内标校准后,各元素标准曲线的线性有较大改善,线性相关系数为0.9981~0.9999。以建立的方法对碳化硅标准参考物质(BAM-S003)中的痕量元素进行测定,并与标准参考值进行对比,结果一致,证实了LA-ICP-MS方法应用于碳化硅样品检测的准确性和有效性。采用本方法定量测定碳化硅器件中痕量元素,结果与辉光放电质谱法(GD-MS)测定的结果比较一致。元素B,Ti,Cr,Mn,Fe,Ni,Cu,Sr和La的检出限为0.004~0.08 mg/kg,相对标准偏差(RSD)小于5%。
The calibration curves were prepared by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with NIST glass standard, 29Si was the internal standard, the relative sensitivity factor (RSF) calibration standard and the matrix effect between samples, Nine kinds of trace elements (B, Ti, Cr, Mn, Fe and Ni) in ceramic devices were quantitatively determined. Select the linear scan mode, laser ablation aperture of 150μm, helium and argon flow rate of 0.7L / min, the signal stability and sensitivity of the best. After the internal standard calibration, the linearity of each standard curve has been greatly improved, the linear correlation coefficient of 0.9981 ~ 0.9999. The established method for the determination of trace elements in the standard reference material of silicon carbide (BAM-S003) was compared with the standard reference values and the results were consistent, confirming the accuracy of LA-ICP-MS method for the detection of silicon carbide samples Sexuality and effectiveness. The method of quantitative determination of trace elements in silicon carbide devices, the results and glow discharge mass spectrometry (GD-MS) measured the results are more consistent. The detection limits of elemental B, Ti, Cr, Mn, Fe, Ni, Cu, Sr and La were 0.004-0.08 mg / kg and the relative standard deviations (RSDs) were less than 5%.