In this study, a switchable solvent was used to preconcentrate trace amounts of Cd from aqueous solution for its determination by flame atomic absorption spectrometry (FAAS). Protonation of N,N-dimethylbenzylamine by dry ice (solid CO) made it water soluble, and addition of sodium hydroxide converted it back to its original nonionic state for phase separation and subsequent extraction of Cd. A slotted quartz tube (SQT) was attached to the flame burner head to increase the residence time of Cd atoms in the light path. Under the optimum conditions, limits of detection and quantification were determined as 0.7 and 2.6 μg L, respectively. Low relative standard deviations calculated from seven replicate measurements of the lowest concentration indicated high precision. Accuracy of the developed method was checked by using a standard reference material (SRM 1633c). Spiked recovery tests were also performed on lake water and wastewater samples at different concentrations to check the applicability of the developed method, and the results obtained (90-103%) established high recovery.
Switchable solvent liquid-phase microextraction was combined with gas chromatography and mass spectrometry to improve the sensitivity and accuracy for the determination of selected endocrine disruptors, pesticides, and hormones. The extraction method was used to complement gas chromatography with mass spectrometry by preconcentrating analytes for trace determinations. A Box-Behnken experimental design was used to evaluate the main variables and their interaction effects, and optimum parameters were selected based on the model of experimented results. Application of optimum extraction conditions to mixed standard solutions yielded limits of detection and quantitation values between 0.20-13 and 0.90-46 ng/mL, respectively. The accuracy and the applicability of the developed method was checked in tap water and two different wastewater samples by spiked recovery tests. The percent recoveries recorded for the analytes were between 91 and 110%, and percent relative standard deviation values were all below 10%. The results indicate that the method can be used for the accurate and sensitive determination of these analytes in the presented matrixes.
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