Interference-free, green microanalytical method for total mercury and methylmercury determination in biological and environmental samples using small-sized electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry

Simultaneous Determination of As, Bi, Sb, Se, Te, Hg, Pb and Sn by Small-Sized Electrothermal Vaporization Capacitively Coupled Plasma Microtorch Optical Emission Spectrometry Using Direct Liquid Microsampling

“…The SSETV-µCCP-OES method was characterized in terms of analytical performance, namely, LODs, parameters of the calibration curves established by the net peak area of transient signals and their maximum height ( Table 2 and Table 3 ), accuracy by analyzing several CRMs ( Table 4 and Table 5 ), non-spectral effects of the multimineral matrix and precision in measuring test samples of cave and river sediment. The limits of detection in liquid were calculated using the standard deviation of residuals (s y/x ) and calibration slope (m) [ 67 ], while in the solid based on the sample preparation procedure. The accuracy was estimated by comparing the certified concentrations with found values, for the 95% confidence level.…”

“…The UV background spectrum emitted by the low power and low Ar consumption µCCP consists of molecular emission from NO (A 2 Σ + →X 2 Π; E ex = 5.45 eV; 205.28 nm (2,2); 215.49 (9,1); 226.94 nm (0,0); 237.02 nm (1,0); 247.87 nm (2,0); 250.60 nm (5,0)) and OH (A 2 Σ + →X 2 Π; E ex = 4.05 eV; 269.11 nm (1,3); 282.90 (0,1); 289.27 nm (1,2); 296.24 nm (2,3); and 308.90 nm (0,0)). In a recent study aiming to determine total Hg and CH 3 Hg + in food and river sediment by SSETV-µCCP-OES, it was remarked the capability of microplasma to provide several emission lines of Fe, S, and P in the range 180–200 nm [ 67 ]. In another study on the simultaneous determination of Ag, As, Cd, Cu, Hg, Pb, Sn, and Zn in soil, it was achieved a selective vaporization of Hg and Ag at 1200–1300 °C, while for the less volatile elements such as Cu and Zn, it was necessary a vaporization temperature of at least 1500 °C [ 66 ].…”

“…Based on these considerations, the present study tries to answer the question of whether the SSETV-µCCP-OES could be useful for the simultaneous determination of the common chemical vapor-generating elements by selective vaporization from liquid microsamples without derivatization. Previously, the same approach was found convenient for the determination of total mercury and CH 3 Hg + [ 67 ]. The answer is provided in the emission spectra of elements recorded with two low resolution microspectrometers, Maya2000 Pro and QE65 Pro ( Figure 1 and Figure 2 ), and the characteristics of the identified lines ( Table 1 ).…”

“…The prototype experimental set-up ( Figure 6 ) for SSETV-µCCP-OES used in this study was previously described [ 63 , 64 , 65 , 66 , 67 ] and patented [ 69 ]. The analytical system is fully miniaturized and its constructive features and operation conditions are given in Table 7 .…”

“…To avoid the matrix interference, quantification was performed using the standard addition. However, heating the filament to a lower temperature (1300 °C) provided a selective vaporization of Hg and thus, a new opportunity for the determination of total Hg and CH 3 Hg + by SSETV-µCCP-OES using external calibration [ 67 ]. New validated methods, free from non-spectral interference using miniaturized instrumentation incorporating plasma sources continue to be a challenge and a necessity.…”