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A comparison of signal suppression and particle size distributions for ns- and fs-LA of metallic samples by LA-ETV-ICPMS
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2017-08-08 00:00:00 , DOI: 10.1039/c7ja00176b Hale Ceren Yilmaz 1, 2, 3, 4 , Bodo Hattendorf 1, 2, 3, 4
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2017-08-08 00:00:00 , DOI: 10.1039/c7ja00176b Hale Ceren Yilmaz 1, 2, 3, 4 , Bodo Hattendorf 1, 2, 3, 4
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The influence of thermal treatment of laser-generated aerosols in a graphite furnace electrothermal vaporization (ETV) unit was investigated. Changes in the chemical composition and particle size distribution (PSD) of aerosols generated by nanosecond (ns-LA) and femtosecond (fs-LA) ablation of Cu, Zn, brass and Ta were monitored as a function of the graphite furnace temperature via inductively coupled plasma mass spectrometry (ICPMS) and with an optical particle counter (OPC). Morphology changes were investigated by recording SEM images of filter-collected material. With increasing furnace temperature, the ICPMS signals of all elements decreased and the onset temperatures of the suppression followed the order of the boiling points of the elements. Ablation with fs-LA generally showed a continuous signal decrease with increasing temperature. When ablating Zn with ns-LA, a discontinuity was introduced in the suppression profile, which was related to the PSDs of the original aerosols. Between 60 nm and 1 μm, they were generally broader when using fs-LA for the ablation of Zn, Cu and brass. When heating the aerosols, the morphology and PSD of the aerosols indicated that melting causes the nanoparticles' agglomerate to collapse into lumps of spherical shape. The discontinuity in the suppression profiles is interpreted to originate from the contribution of the large particles that do not evaporate and give a continuous contribution to the ion signals. Heating of the Ta-aerosols only resulted in a slight signal suppression, while SEM images revealed the presence of particles of larger sizes that were most likely formed from molten NPs and agglomerates. The thermal treatment opens a unique way for selective removal of elements forming spectral interference when using LA-ICPMS for spatially resolved solid sampling. In this study, the Zn-signal from the brass sample could be lowered by selective evaporation by more than 3 orders of magnitude, while Cu was still quantitatively retained in the aerosol. This separation was slightly more efficient when using fs-LA, which is most likely the result of the larger fraction of μm-sized particles in the ns-LA aerosols studied here.
中文翻译：
LA-ETV-ICPMS对金属样品中ns-和fs-LA的信号抑制和粒径分布的比较
研究了石墨炉电热汽化（ETV）单元中激光产生的气溶胶热处理的影响。通过石墨炉温度的函数，通过纳秒（ns-LA）和飞秒（fs-LA）烧蚀Cu，Zn，黄铜和Ta产生的气溶胶的化学成分和粒径分布（PSD）的变化通过石墨炉温度进行监测电感耦合等离子体质谱（ICPMS）和光学粒子计数器（OPC）。通过记录过滤器收集材料的SEM图像来研究形态变化。随着炉温的升高，所有元素的ICPMS信号均降低，抑制的起始温度遵循元素沸点的顺序。用fs-LA消融通常显示随着温度的升高信号持续降低。当用ns-LA烧蚀Zn时，抑制谱中引入了不连续性，这与原始气溶胶的PSD有关。当使用fs-LA烧蚀Zn，Cu和黄铜时，它们通常在60 nm和1μm之间，更宽。加热气溶胶时，气溶胶的形态和PSD表明，熔化会导致纳米颗粒 凝聚成球状的块状。抑制曲线中的不连续性被解释为源自大颗粒的贡献，这些大颗粒没有蒸发，并且对离子信号产生了连续的贡献。Ta气溶胶的加热仅导致轻微的信号抑制，而SEM图像显示存在较大尺寸的颗粒，该颗粒最有可能是由熔融NP和附聚物形成的。当使用LA-ICPMS进行空间分辨固体采样时，热处理为选择性去除形成光谱干扰的元素开辟了一条独特的途径。在这项研究中，通过选择性蒸发可将黄铜样品中的Zn信号降低3个数量级以上，而Cu仍被定量保留在气溶胶中。
更新日期：2017-08-25
中文翻译：
LA-ETV-ICPMS对金属样品中ns-和fs-LA的信号抑制和粒径分布的比较
研究了石墨炉电热汽化（ETV）单元中激光产生的气溶胶热处理的影响。通过石墨炉温度的函数，通过纳秒（ns-LA）和飞秒（fs-LA）烧蚀Cu，Zn，黄铜和Ta产生的气溶胶的化学成分和粒径分布（PSD）的变化通过石墨炉温度进行监测电感耦合等离子体质谱（ICPMS）和光学粒子计数器（OPC）。通过记录过滤器收集材料的SEM图像来研究形态变化。随着炉温的升高，所有元素的ICPMS信号均降低，抑制的起始温度遵循元素沸点的顺序。用fs-LA消融通常显示随着温度的升高信号持续降低。当用ns-LA烧蚀Zn时，抑制谱中引入了不连续性，这与原始气溶胶的PSD有关。当使用fs-LA烧蚀Zn，Cu和黄铜时，它们通常在60 nm和1μm之间，更宽。加热气溶胶时，气溶胶的形态和PSD表明，熔化会导致纳米颗粒 凝聚成球状的块状。抑制曲线中的不连续性被解释为源自大颗粒的贡献，这些大颗粒没有蒸发，并且对离子信号产生了连续的贡献。Ta气溶胶的加热仅导致轻微的信号抑制，而SEM图像显示存在较大尺寸的颗粒，该颗粒最有可能是由熔融NP和附聚物形成的。当使用LA-ICPMS进行空间分辨固体采样时，热处理为选择性去除形成光谱干扰的元素开辟了一条独特的途径。在这项研究中，通过选择性蒸发可将黄铜样品中的Zn信号降低3个数量级以上，而Cu仍被定量保留在气溶胶中。
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