RESUMEN
An effervescent tablet-assisted switchable solvent based liquid phase microextraction (EA-SS-LPME) was developed for multi-element determination of Pb and Cd in various samples using high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS). The effervescent tablets were used for improving the extraction efficiency. Triethylamine as a hydrophobic solvent was switched to protonated triethylamine carbonate by CO2 and used to extract dithizone complexes from samples. Calibration linearities were obtained from 0.06 to 10.0 mg L-1 (Pb) and 0.02 to 1.50 mg L-1 (Cd). LODs of the proposed method were 0.0195 (Pb) and 0.0068 (Cd). LOQs were 0.0649 mg L-1 (Pb) and 0.0228 mg L-1 (Cd) with %RSDs of 1.25%-1.69% (Pb) and 1.07%-1.64% (Cd). The proposed method was applied for the determination of Pb and Cd in water and canned food samples. The spiked recoveries were 82.3-119.0% (Pb) and 81.7-120.0% (Cd). In addition, the PF was 3.3, with EF at 1.4 (Pb) and 2.6 (Cd) obtained after extraction for under 8 min.
Asunto(s)
Microextracción en Fase Líquida , Contaminantes Químicos del Agua , Cadmio/análisis , Alimentos en Conserva , Solventes , Espectrofotometría Atómica , Comprimidos , Contaminantes Químicos del Agua/análisisRESUMEN
Magnetic dispersive solid phase extraction (MdSPE) was developed to determine the concentration of lead (Pb) in real water samples, while graphene oxide-magnetite-dithizone (GO-Fe3O4-DTZ) from the used graphite tubes (recycled graphite) of electrothermal technique was simply employed as a new sorbent to improve extraction efficiency, separated by external magnetic field and analyzed with FAAS. The synthesized sorbent was evaluated for its surface property, functional group and surface morphology by Zeta potential, Fourier transform infrared spectrophotometer (FTIR), and scanning electron microscope (SEM), respectively. The relevant measurement parameters, such as pH, extraction time, type and concentration of eluent, sample volume and reusability, were optimized. Under the optimal conditions, preconcentration factor was 13.33. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 0.070 and 0.23 mg/L, respectively. The relative standard deviation (%RSD) was 3.41%. Recovery values were 90.1 - 123%. In addition, the robustness of the method was affirmed in terms of tolerance limit obtained from interference studies.