Manard Benjamin T, Konegger-Kappel Stefanie, Gonzalez Jhanis J, Chirinos Jose, Dong Meirong, Mao Xianglei, Marcus R Kenneth, Russo Richard E
Clemson University, Department of Chemistry, Biosystems Research Complex, 51 New Cherry Street, Clemson, SC 29634 USA.
Appl Spectrosc. 2015 Jan;69(1):58-66. doi: 10.1366/14-07585. Epub 2014 Dec 1.
Liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma is being developed as a secondary vaporization-excitation source for the optical emission analysis of laser ablation (LA)-generated particle populations. The practicalities of this coupling are evaluated by determining the influence of source parameters on the emission response and the plasma's robustness upon LA introduction of easily ionized elements (EIEs). The influence of discharge current (45-70 mA), LA carrier gas flow rate (0.1-0.8 L min(-1)), and electrode separation distance (0.5-3.5 mm) was studied by measuring Cu emission lines after ablation of a brass sample. Best emission responses were observed for high-discharge currents, low He carrier gas flow rates, and relatively small (<1.5 mm) electrode gaps. Plasma robustness and spectroscopic matrix effects were studied by monitoring Mg(II) : Mg(I) intensity ratios and N2-derived plasma rotational temperatures after the ablation of Sr- and Ca-containing pellets. Plasma robustness investigations showed that the plasma is not appreciably affected by the particle loadings, with the microplasma being slightly more ionizing in the case of Ca introduction. In neither case did the concentration of the concomitant element change the robustness values, implying a high level of robustness. Introduction of the LA particles results in slight increases in the rotational temperatures (∼10% relative), with Ca-containing particles having a greater effect than Sr-containing particles. The observed variation of 9% in the plasma rotational temperature is in the same order of magnitude as the short-term reproducibility determined by the proposed LA-LS-APGD system. The determined rotational temperatures ranged from 1047 to 1212 K upon introducing various amounts of Ca and Sr. The relative immunity to LA particle-induced matrix effects is attributed to the relatively long residence times and high power densities (>10 W mm(-3)) of the LS-APGD microplasma.
液体采样-大气压辉光放电(LS-APGD)微等离子体正被开发用作激光烧蚀(LA)产生的颗粒群发射光谱分析的二次蒸发-激发源。通过确定源参数对发射响应的影响以及引入易电离元素(EIEs)时LA对等离子体稳健性的影响,来评估这种耦合的实用性。通过测量黄铜样品烧蚀后的Cu发射线,研究了放电电流(45 - 70 mA)、LA载气流量(0.1 - 0.8 L min⁻¹)和电极间距(0.5 - 3.5 mm)的影响。在高放电电流、低氦载气流量和相对较小(<1.5 mm)的电极间隙下观察到最佳发射响应。通过监测含Sr和Ca颗粒烧蚀后的Mg(II) : Mg(I)强度比和N₂衍生的等离子体转动温度,研究了等离子体的稳健性和光谱基体效应。等离子体稳健性研究表明,等离子体不受颗粒负载的明显影响,在引入Ca的情况下微等离子体的电离作用稍强。在这两种情况下,伴随元素的浓度都没有改变稳健性值,这意味着具有很高的稳健性。引入LA颗粒会使转动温度略有升高(相对升高约10%),含Ca颗粒的影响比含Sr颗粒更大。观察到的等离子体转动温度9%的变化与所提出的LA-LS-APGD系统确定的短期重现性处于同一数量级。引入不同量的Ca和Sr后,确定的转动温度范围为1047至1212 K。对LA颗粒诱导的基体效应的相对免疫性归因于LS-APGD微等离子体相对较长的停留时间和高功率密度(>10 W mm⁻³)。