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Capabilities of laser ablation inductively coupled plasma time-of-flight mass spectrometry
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2017-08-18 00:00:00 , DOI: 10.1039/c7ja00236j
Marcel Burger 1, 2, 3, 4 , Gunnar Schwarz 1, 2, 3, 4 , Alexander Gundlach-Graham 1, 2, 3, 4 , Debora Käser 1, 2, 3, 4 , Bodo Hattendorf 1, 2, 3, 4 , Detlef Günther 1, 2, 3, 4
Affiliation  

In this paper, we characterize an inductively coupled plasma time-of-flight mass spectrometry (ICP-TOFMS) instrument (icpTOF, TOFWERK AG, Thun, Switzerland) in combination with laser-ablation sample introduction. Three sample introduction approaches for LA-based ICP-TOFMS analysis are described: (1) steady-state LA with a conventional high-dispersion LA cell, (2) single-pulse analysis with large spot sizes (44 μm diameter) using a low-dispersion LA cell, and (3) pulse-resolved, high-speed, high-resolution (5 μm spot sizes) elemental imaging with the same low-dispersion LA cell. These sample-introduction schemes span the range of approaches most interesting for users of LA-ICP-TOFMS, from routine bulk quantification, to low-sample-consumption trace-element analysis, to demanding elemental imaging applications. From steady-state signal intensities, element concentrations in NIST SRM 612 and USGS BCR-2G were quantified within the uncertainty range of the preferred values when NIST SRM 610 was used as the external reference material. Relative deviations were less than 10% in most cases. When using a 44 μm diameter spot and a laser repetition rate of 10 Hz, limits of detection (LODs) were in the single digit ng g−1 range for the most sensitive isotopes. Isotope-ratio precision was in the sub per mill regime and governed by counting statistics. Similar accuracies were also achieved in low-dispersion LA-ICP-TOFMS experiments, when NIST SRM 612 and USGS BCR-2G element concentrations were quantified using signal intensities from single 44 μm diameter laser pulses. LODs were in the tens of ng g−1 range for most sensitive isotopes resulting in absolute LODs in the tens of attograms. Capabilities of the icpTOF for elemental imaging are demonstrated with pulse-resolved multi-elemental imaging of a multi-phase geological thin section. With the low-dispersion LA cell and a spot diameter of 5 μm, aerosol plumes were confined to less than 10 ms, which allowed elemental imaging at a laser repetition rate of 100 Hz with minimized pulse-to-pulse mixing and an adjacent-pixel dynamic range of greater than 102. Quantitative results for elements of major, minor and trace concentrations were in agreement with bulk composition of individual regions, which had been determined via petrographic microscopy and high-dispersion laser ablation inductively coupled plasma quadrupole mass spectrometry (LA-ICPQMS). LODs were in the single digit μg g−1 range for most sensitive isotopes.

中文翻译:

激光烧蚀电感耦合等离子体飞行时间质谱的能力

在本文中,我们结合激光烧蚀样品引入技术对电感耦合等离子体飞行时间质谱(ICP-TOFMS)仪器(icpTOF,TOFWERK AG,图恩,瑞士)进行了表征。描述了用于基于LA的ICP-TOFMS分析的三种样品引入方法:(1)具有常规高分散LA池的稳态LA,(2)具有大光点尺寸(直径为44μm)的单脉冲分析-色散LA细胞,以及(3)使用相同的低色散LA细胞进行脉冲分辨,高速,高分辨率(5μm光斑尺寸)的元素成像。这些样品引入方案涵盖了LA-ICP-TOFMS用户最感兴趣的方法范围,从常规的批量定量分析,低样品消耗的痕量元素分析到苛刻的元素成像应用。从稳态信号强度来看,当将NIST SRM 610用作外部参考材料时,NIST SRM 612和USGS BCR-2G中的元素浓度在优选值的不确定性范围内进行了定量。在大多数情况下,相对偏差小于10%。当使用直径为44μm的光斑且激光重复频率为10 Hz时,检出限(LOD)为单位ng g-1范围是最敏感的同位素。同位素比精度在每磨次制以下,并通过统计统计数据来控制。当使用来自单个44μm直径激光脉冲的信号强度对NIST SRM 612和USGS BCR-2G元素浓度进行定量时,在低分散LA-ICP-TOFMS实验中也获得了类似的精度。LOD处于数十ng g -1范围最敏感的同位素,导致绝对LOD达到数十个ATT图。icpTOF用于元素成像的功能已通过多相地质薄段的脉冲分辨多元素成像得以证明。使用低分散LA电池和5μm的光斑直径,气溶胶羽流被限制在小于10 ms的范围内,从而允许以100 Hz的激光重复频率进行元素成像,同时最大程度地减少了脉冲间的混合,并形成了一个相邻像素动态范围大于10 2。主要,次要和痕量浓度元素的定量结果与各个区域的总体组成相符,这是通过以下方法确定的岩相显微镜和高色散激光烧蚀电感耦合等离子体四极杆质谱(LA-ICPQMS)。对于大多数敏感同位素,LOD处于数位μgg -1范围内。
更新日期:2017-08-21
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