Department of Chemistry, Faculty of Science, Masaryk University, Kotlárská 2, 611 37 Brno, Czech Republic.
Talanta. 2010 Mar 15;80(5):1862-7. doi: 10.1016/j.talanta.2009.10.035. Epub 2009 Oct 24.
A study of LA-ICP-MS analysis of pressed powdered tungsten carbide precursors was performed to show the advantages and problems of nanosecond laser ablation of matrix-unified samples. Five samples with different compositions were pressed into pellets both with silver powder as a binder serving to keep the matrix unified, and without any binder. The laser ablation was performed by nanosecond Nd:YAG laser working at 213 nm. The particle formation during ablation of both sets of pellets was studied using an optical aerosol spectrometer allowing the measurement of particle concentration in two size ranges (10-250 nm and 0.25-17 microm) and particle size distribution in the range of 0.25-17 microm. Additionally, the structure of the laser-generated particles was studied after their collection on a filter using a scanning electron microscope (SEM) and the particle chemical composition was determined by an energy dispersive X-ray spectroscope (EDS). The matrix effect was proved to be reduced using the same silver powdered binder for pellet preparation in the case of the laser ablation of powdered materials. The LA-ICP-MS signal dependence on the element content present in the material showed an improved correlation for Co, Ti, Ta and Nb of the matrix-unified samples compared to the non-matrix-unified pellets. In the case of W, the ICP-MS signal of matrix-unified pellets was influenced by the changes in the particle formation.
采用 LA-ICP-MS 分析了压制粉末状碳化钨前驱体,以展示纳秒激光烧蚀基体统一样品的优势和问题。将五种不同成分的样品分别压制成两个系列的样品,其中一组样品加入了银粉作为保持基体统一的粘结剂,另一组样品则没有加入任何粘结剂。纳秒 Nd:YAG 激光在 213nm 波长下进行激光烧蚀。采用光学气溶胶光谱仪研究了两组样品的颗粒形成过程,该光谱仪能够测量两个粒径范围(10-250nm 和 0.25-17μm)的颗粒浓度以及 0.25-17μm 粒径范围内的颗粒分布。此外,还使用扫描电子显微镜(SEM)研究了收集在滤纸上的激光生成颗粒的结构,并使用能谱仪(EDS)确定了颗粒的化学成分。实验证明,对于粉末材料的激光烧蚀,使用相同的银粉粘结剂来制备压片可以减少基体效应。与非基体统一的压片相比,基体统一样品的 LA-ICP-MS 信号与材料中存在的元素含量的相关性得到了改善,其中 Co、Ti、Ta 和 Nb 的改善更为显著。对于 W,基体统一压片的 ICP-MS 信号受到颗粒形成变化的影响。