Study on ICP Mass Spectrometry with Solutions capturing Solid-Sample Particles generated by Laser Ablation

为了提高激光烧蚀（LA）/ICP-MS定量分析的特性，我们研究了利用溶液中的固体样品颗粒收集由LA产生。在我们的第一种方法中，通过在纯水中的一系列标准钢样品的表面上照射激光脉冲来制备样品溶液。当样品溶液中分析物的离子强度对标准钢样品的每个浓度作图时，可以获得良好的线性。但与用试剂配制的标准溶液相比，样品和标准溶液的校准曲线斜率存在差异，沸点较高的元素，其差异增大;例如，确认了元素之间的选择性蒸发。另一种方法是用常规的LA系统产生固体样品颗粒，用载气将其转移到0.1mol/LHNO_3溶液中。校准曲线通过绘制样品溶液中分析物的离子强度对标准钢样品的每个浓度来获得。然而，校准曲线在斜率方面与标准品溶液的校准曲线不同，此外，绘制的点分散。通过应用内标法，Co和Mo的校准曲线在样品和标准溶液之间重叠。在烧结氮化硅标准样品分析中的应用。准确度和精密度几乎令人满意。发现了在极短时间内分析烧结精细陶瓷的可能性。

In order to improve the characteristics of quantitative analysis in laser ablation (LA)/ICP-MS, we investigated the utilization of solutions in which solid-sample particles generated by LA were collected. In our first method, sample solutions were prepared by irradiating laser pulses on the surface of a series of standard steel samples in pure water. A good linearity could be obtained when ion intensities of analytes in sample solutions were plotted against each concentration for standard steel samples. Compared to standard solutions prepared from reagents, however, the differences in the slope of calibration curves between sample and standard solutions were found. An increase in the difference was observed for elements with higher boiling points ; i. e., selective vaporization between elements was recognized. By using predetermined factors for compensating the selective vaporization another steel samples could be analyzed only with standard solutions.As a second method, solid-sample particles, which were generated by a conventional LA system, were transferred into 0.1 mol/L HN0_3 solution with carrier gas. Calibration curves were obtained by plotting ion intensities of analytes in sample solutions against each concentration for standard steel samples. The calibration curves, however, differed from those for standard solutions in terms of the slope, and furthermore, the plotted points scattered. By applying an internal standard method, the calibration curves for Co and Mo overlapped between sample and standard solutions. In an application to the analysis for a standard sample of sintered silicon nitride. both accuracy and precision were almost satisfactory. The possibility of analyzing sintered fine-ceramics in an extremely short time was found.