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Parametric optimization and spectral line selection for liquid sampling-atmospheric pressure glow discharge – optical emission spectroscopy†
Journal of Analytical Atomic Spectrometry ( IF 3.4 ) Pub Date : 2019-11-07 , DOI: 10.1039/c9ja00325h
Katja A. Hall 1, 2, 3, 4, 5 , R. Kenneth Marcus 1, 2, 3, 4, 5
Affiliation  

A design-of-experiment (DOE) parameterization was performed with the liquid sampling-atmospheric pressure glow discharge (LS-APGD) optical emission spectroscopy (OES) system to establish the optimal powering mode and operating conditions that allow for maximum signal intensity, signal-to-background (S/B) ratio, and signal-to-noise (S/N) ratio. Different from other APGD sources, the operation principles of the LS-APGD provide alternative means of applying the discharge potential. As a result of this parameterization, the sensitivity of the LS-APGD was dramatically improved, as noted by the ∼30× improvement in limit of detection (LOD), now 0.8 μg mL−1 for 20 μL injections, versus earlier reports, with the solution-grounded cathode (SGC) found to be the preferred powering mode. Using the parameters from the DOE analysis, a line selection evaluation was performed for Ag, Ca, Cr, Cu, K, Mg, Na, and Zn as test elements. The best emission lines for analytical performance determination and future works were determined by measuring the stability and signal intensity for all observed lines. The chosen lines were probed for sensitivity by acquiring calibration curves for each of the analytes' transitions. When single-element solutions were used, the LODs acquired for many of the analytes were superior to previously reported LS-APGD results. While the sensitivity of the LS-APGD-OES is lower than that of an ICP-OES, the LODs for the LS-APGD are likely acceptable for those applications where portability and low-cost instrumentation are desired.

中文翻译:

液体采样-大气压辉光放电的参数优化和光谱线选择–发射光谱

利用液体采样-大气压辉光放电(LS-APGD)光学发射光谱(OES)系统进行了实验设计(DOE)参数化,以建立最佳的供电模式和操作条件,以实现最大的信号强度,信号与背景(S / B)的比率以及信噪比(S / N)的比率。LS-APGD的工作原理与其他APGD来源不同,它提供了施加放电电势的替代方法。作为该参数的结果,LS-APGD的灵敏度显着提高,如通过在检测限(LOD)的极限的约30×改善所指出的,现在0.8微克毫升-1 20μL注射剂,较早的报道中,溶液接地阴极(SGC)被认为是首选的供电方式。使用来自DOE分析的参数,对Ag,Ca,Cr,Cu,K,Mg,Na和Zn作为测试元素进行了线选择评估。通过测量所有观察到的谱线的稳定性和信号强度,可以确定用于分析性能确定和未来工作的最佳发射谱线。通过获取每个分析物的跃迁的校准曲线,对选定的谱线进行灵敏度检测。当使用单元素溶液时,许多分析物获得的LOD优于先前报道的LS-APGD结果。尽管LS-APGD-OES的灵敏度低于ICP-OES,
更新日期:2019-11-28
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