Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca, Romania.
Research Center for Advanced Chemical Analysis, Instrumentation and Chemometrics-Analytica, Babes-Bolyai University, Arany Janos 11, 400028 Cluj-Napoca, Romania.
Molecules. 2021 Apr 30;26(9):2642. doi: 10.3390/molecules26092642.
The simultaneous determination of chemical vapor-generating elements involving derivatization is difficult even by inductively coupled plasma optical emission spectrometry or mass spectrometry. This study proposes a new direct liquid microsampling method for the simultaneous determination of As, Bi, Se, Te, Hg, Pb, and Sn, using a fully miniaturized set-up based on electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry. The method is cost-effective, free from non-spectral interference, and easy to run by avoiding derivatization. The method involves the vaporization of analytes from the 10 µL sample and recording of episodic spectra generated in low-power (15 W) and low-Ar consumption (150 mL min) plasma microtorch interfaced with low-resolution microspectrometers. Selective vaporization at 1300 °C ensured the avoidance of non-spectral effects and allowed the use of external calibration. Several spectral lines for each element even in the range 180-210 nm could be selected. Generally, this spectral range is examined with large-scale instrumentation. Even in the absence of derivatization, the obtained detection limits were low (0.02-0.75 mg kg) and allowed analysis of environmental samples, such as cave and river sediments. The recovery was in the range of 86-116%, and the accuracy was better than 10%. The method is of general interest and could be implemented on any miniaturized or classical laboratory spectrometric instrumentation.
即使通过电感耦合等离子体光发射光谱法或质谱法,涉及衍生化的化学蒸气生成元素的同时测定也很困难。本研究提出了一种新的直接液体微采样方法,用于同时测定砷、铋、硒、碲、汞、铅和锡,使用基于电热蒸气化电容耦合等离子体微火炬光发射光谱法的完全小型化装置。该方法具有成本效益,无光谱干扰,通过避免衍生化,易于运行。该方法涉及从 10 µL 样品中蒸发分析物,并记录在低功率(15 W)和低氩气消耗(150 mL min)等离子体微火炬中产生的间歇性光谱,该微火炬与低分辨率微光谱仪接口。在 1300 °C 下选择性蒸发可确保避免非光谱效应,并允许使用外部校准。甚至可以选择每个元素的多个谱线,即使在 180-210 nm 范围内也是如此。通常,这个光谱范围是用大型仪器进行检查的。即使没有衍生化,也可以获得低检测限(0.02-0.75 mg kg),并且可以分析环境样品,如洞穴和河流沉积物。回收率在 86-116%之间,准确度优于 10%。该方法具有普遍意义,可以在任何小型化或经典的实验室光谱仪器上实施。