非破坏性开放式激光剥蚀电感耦合等离子体质谱法原位测定大尺寸陶瓷样品主微量元素组成

激光剥蚀电感耦合等离子体质谱法(LA-ICP-MS)通常采用体积固定的封闭剥蚀池,大尺寸样品要经过切割或破碎,能够放入剥蚀池后才可以再进行LA-ICP-MS分析,因此,这种常规密闭式LA-ICP-MS难以应用于无法破碎的珍稀大尺寸样品分析.为实现大尺寸样品的非破坏性微区原位主微量元素分析,本文基于自行设计的开放式样品采...

In-situ Non-destructive Determination of Major and Trace Elements in Large Size Ceramic Samples by Open Laser Ablation Inductively Coupled Plasma-Mass Spectrometry

BACKGROUND: Usually, laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) analysis is equipped with a closed ablation cell. It cannot be used for non-destructive analysis of the large-size samples which exceeds the size of the cell.
OBJECTIVES: To realize directly in situ non-destructive analysis of major and trace elements in the large-size samples.
METHODS: Based on the self-designed open sample collection port, combined with the gas exchange device, an open LA-ICP-MS analysis method was established. Taking the large-size ceramic disc sample as an example, samples can be directly determined for major and trace elements in an air environment without being broken.
RESULTS: Analyte aerosols produced by laser ablation were collected and sucked by open sample collector. The air in the aerosols was replaced via transfer tube by high purity argon in a gas exchange device, the analyte aerosols were then transferred into ICP-MS for detection. After non-destructive analyses by this method, large-size ceramic samples were broken and analyzed by traditional LA-ICP-MS. Relative deviations of most of 51 elements detected by the two methods were less than 10%. Only part of elements (such as P, Be, Sc, Y, La, Sm, Eu, Dy, Hf, W, etc.) had relative deviations higher than 20%, because of the extremely low contents.
CONCLUSIONS: The open LA-ICP-MS method is suitable for in situ non-destructive determination of major and trace elements in the large-size samples.