Spark ablation inductively coupled plasma mass spectrometry analysis of minor and trace elements in low and high alloy steels using single calibration curves
Spark ablation inductively coupled plasma mass spectrometry analysis of minor and trace elements in low and high alloy steels using single calibration curves
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DOI：
10.1039/a901650c
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发表时间：
1999
影响因子：
3.4
通讯作者：
R. Maibusch;H. Kuss;A. G. Coedo;T. Dorado;I. Padilla
中科院分区：
文献类型：
--
作者：
R. Maibusch;H. Kuss;A. G. Coedo;T. Dorado;I. Padilla
单向大电流脉冲火花具有很快的上升时间，确保了能量快速和完整地传递到样品，作为采样系统，在相同的操作条件下分析了碳钢和高合金钢。优化了点火操作条件，并设计了一条限制路径，以减少到达等离子体的侵蚀物质的数量，以防止材料沉积在火炬喷射器中，并将采样锥体堵塞和漂移影响降至最低。对火花消融采样效率和受限路径的有效性进行了评估。为了补偿材料烧蚀量的差异或漂移的变化，使用57Fe和55Mn作为内标。校准程序用于分析下列标准物质中存在的元素Al、B、Co、Cu、Mn、Nb、P、Si和V：BCS(分析样品局)SS-456至SS-460(残留系列)；CRMS(欧洲钢铁标准化委员会)编号285-2(马氏体时效钢)、编号292-1(Nb稳定化钢)、编号295-1(高合金钢)和编号296-1(杰特钢)。当绘制强度比(Ix/Iis)与浓度比(Cx/Cis)时，得到了在整个测试浓度范围内的线性校准曲线，相关系数大于0.999。方法的检出限低于1µg g-1，精密度优于2.8%。它还被证明在浓度水平大于0.03%的情况下测定碳含量，RSD值低于3%。对于只存在于一种或两种标准物质中的元素As、Sn、Ti、W和Zr，也进行了灵敏度评估。此外，还证明了从仅几秒的火花周期中获得可重现的瞬时信号的可能性。
A unidirectional high current pulse spark with a very fast rise-time, ensuring a rapid and complete transfer of energy to the sample, was used as the sampling system for the analysis of carbon steels and highly alloyed steels with the same operating conditions. The sparking operating conditions were optimised and a restrictive path was designed to decrease the quantity of eroded material reaching the plasma, in order to prevent deposition of material in the torch injector, and to minimise sampling cone blockage and drift effects. Spark ablation sampling efficiency and effectiveness of the restrictive path were evaluated. To compensate for differences in the amount of material ablated or for a variation in drift, 57 Fe and 55 Mn were used as internal standards. The calibration procedure was applied to the analysis of the elements Al, B, Co, Cu, Mn, Nb, P, Si, and V, present in the following certified reference materials: BCS (Bureau of Analysed Samples) SS-456 to SS-460 (residual series); CRMs (European Committee for Iron and Steel Standardisation) No 285-2 (Maraging steel), No 292-1 (niobium stabilised steel), No 295-1 (highly alloyed steel), and No 296-1 (jethete steel). When plotting intensity ratios (I X /I IS ) versus concentration ratios (C X /C IS ) linear calibration curves over the entire range of tested concentrations, with correlation coefficients better than 0.999, were obtained. Determination limits below 1 µg g –1 were found and the precision was better than 2.8%. It has also been shown to determine carbon contents at concentration levels greater than 0.03% with RSD values below 3%. For the elements As, Sn, Ti, W and Zr, only present in one or two of the Standard Materials, the sensitivity was also evaluated. Furthermore, the possibility of obtaining reproducible transient signals from sparking periods of only a few seconds was demonstrated.