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Depth profile analysis of rare earth elements in corroded steels by pulsed glow discharge – time of flight mass spectrometry

机译:用脉冲辉光放电 - 飞行时间质谱法分析腐蚀钢中稀土元素的深度剖面

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摘要

Depth profiling of 304L stainless steel surfaces exposed to rare earth nitrate solutions over varying time lengths has been undertaken using the recently commercialized “PP-TOFMS Plasma Profiling Spectrometer” by Horiba. This combines a pulsed glow discharge source with a time-of-flight mass spectrometer (TOFMS) which allows elemental depth profiling with nanometric resolution of almost all elements of the periodic table. In this work special attention is paid first to the optimization of the new PP-TOFMS for depth profile analysis of low concentrations of rare earth elements (REE) in the samples. Sensitivity given in [(cps X × sputtering rate in μg s)/(μg g)], being the concentration of the element X (μg g) corrected by the abundance of the measured isotope, was in the order of 20 for all REEs under investigation. Moreover, a quantification strategy for these samples resembling the relative sensitive factors concept has been developed. Validation was done using a homogeneous reference material containing certified concentration values for La (6 ± 1 μg g), Ce (14 ± 1 μg g) and Nd (6 ± 1 μg g). Concentrations of 4 ± 1 μg g, 13 ± 1 μg g and 5 ± 1 μg g were calculated for La, Ce and Nd respectively with the proposed strategy. Quantitative depth profiles of the investigated samples have shown that the contaminants did not penetrate the substrate deeper than 80 nm even after a month of exposure to 12 M HNO.
机译:使用H场制作所最近商业化的“ PP-TOFMS等离子体轮廓光谱仪”,可以对在不同时间长度内暴露于稀土硝酸盐溶液的304L不锈钢表面进行深度剖析。它结合了脉冲辉光放电源和飞行时间质谱仪(TOFMS),该质谱仪可以对元素深度进行概要分析,并具有周期表几乎所有元素的纳米级分辨率。在这项工作中,首先要特别注意优化用于样品中低浓度稀土元素(REE)的深度剖面分析的新型PP-TOFMS。以[(cps X×以μgs为单位的溅射速率)/(μgg)]给出的灵敏度(通过所测同位素的丰度校正的元素X的浓度(μgg))对于所有稀土元素均为20量级。在调查中。此外,已经开发了类似于相对敏感因素概念的这些样品的定量策略。使用包含La(6±1μgg),Ce(14±1μgg)和Nd(6±1μgg)的认证浓度值的均质参考材料进行验证。用提出的策略分别计算出La,Ce和Nd的浓度分别为4±1μgg,13±1μgg和5±1μgg。所研究样品的定量深度曲线表明,即使在暴露于12 M HNO的一个月后,污染物也不会穿透基材深于80 nm。

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