N-compounds speciation analysis in environmental samples using ultrasound-assisted solid-liquid extraction and non-chromatographic techniques.

A fast, efficient, and non-chromatographic method was presented in this study for nitrite, nitrate, and p-nitrophenol (N-compounds) extraction and speciation analysis of environmental samples. By applying ultrasound-assisted solid-liquid extraction (USLE), analytes were efficiently extracted from water, soil, or sediment collected in areas of environmental disaster. These analytes were selectively converted to NO(g) through UV photolysis (NO3-), H2O2/UV photocatalysis (PNP), and direct conversion (NO2-). Following conversion, NO(g) was separated from the liquid phase and determined by high-resolution continuum source molecular absorption spectrometry (HR-CS MAS). The LODs obtained were 0.097 ± 0.004 mg L-1 for nitrite, 0.119 ± 0.004 mg L-1 for nitrate, and 0.090 ± 0.006 mg L-1 for p-nitrophenol. On applying this speciation method to environmental samples, concentrations were found to be up to 0.99 ± 0.03 mg L-1 (NO2-), 49.80 ± 2.5 mg L-1 (NO3-), and 0.10 ± 0.02 mg L-1 (PNP). Finally, addition/recovery study of real water, soil, and sediment samples showed 101 ± 2% recovery for NO2-, 100 ± 1% for NO3-, and 96 ± 5% for PNP.

UV photochemical hydride generation using ZnO nanoparticles for arsenic speciation in waters, sediments, and soils samples.

The environmental disasters that occurred due to the leakage of mining waste in Mariana-MG (2015) and Brumadinho-MG (2019), located in Brazil, attracted the attention of the scientific community. This designated efforts to investigate the environmental consequences of toxic waste in the affected ecosystem. Therefore, a simple, easily executed and accessible method was presented for arsenic speciation [As(III), As(V), and DMA]. Using an atomic absorption spectrometer coupled to the hydride generation system, the heterogeneous photocatalysis was applied in the reduction of As(V) and DMA to As(III). After the optimization, a calibration curve was constructed, with LODs equivalent to 3.20 µg L-1 As(III), 3.86 µg L-1 As(V), and 6.68 µg L-1 DMA. When applying the method for quantification in environmental samples, a concentration of up to 103.1 ± 9.4 µg L-1 As(V) was determined for surface water samples. The soil samples, 84.1 ± 3.6 µg L-1 As(III) and 112.4 ± 9.9 µg L-1 As(V) were quantified, proving the contamination of the ecosystems impacted by the environmental disasters. We proceeded the study through an addition/recovery method with samples of water, soil, and sediments (collected from impacted environments). Recovery values were equivalent to 99.0% for As(III), 93.8% for As(V), and 99.2% for DMA. Graphical abstract Photocatalytic reduction mechanism of As(V) and DMA to As(III) by heterogeneous photocatalysis.