We developed an ion-associate phase (IAP)-extraction / acid back-extraction system for the pre-concentration and atomic spectrometric determination of lithium trace amounts in water.The chelating reagent for lithium works also as a constituent of the extraction phase.The lithium in a 10 mL sample solution was converted through a chelate complex reaction with 2,2,6,6-tetramethyl-3,5-heptanedione (HDPM). Addition of a benzyldimethyltetradecylammonium ion caused the formation of an IAP suspension in the solution. Centrifugation of the solution led to the isolation of a liquid organic phase and the lithium complex was extracted as the upper phase from the centrifuge tube. After the aqueous phase was removed, lithium was back-extracted with a 400 µL nitric acid solution from the IAP.The acid phase was measured using liquid-electrode-plasma atomic-emission-spectrometry (LEP-AES) or graphite-furnace atomic-absorption spectroscopy (GF-AAS). The detection limits were 0.02 mg/L for LEP-AES and 0.02 g/L for GF-AAS. This system was applied to the determination of environmental waters.The HDPM in the organic phase was reusable.requires only 20 L of sample. Like many atomic spectroscopic methods, both LEP-AES and GF-AAS are affected by the matrix, so some pretreatment such as separation and concentration is required.Separation and pre-concentration methods that take advantage of the small sample volume required by both LEP-AES and GF-AAS include cloud point extraction, 7, 8 dispersive liquid−liquid extraction, 9, 10 thermoresponsive polymer-mediated extraction, 11 and homogeneous liquid-liquid extraction. 12,13 These techniques are based on the dependence between equilibration temperature and time, 7, 8 the use of chloroform or chlorobenzene as an extraction solvent, 9, 10 the application of heat, 11 or the use of a fluorine-based surfactant. 12,13 In this study, we develop an ion-associate phase extraction method 14 with improved sensitivity and discerning ability against the matrix, and apply it to atomic spectroscopy. 15 This technique converts the analyte in the environmental water into an appropriate form, if necessary, and adds an organic anion and an organic cation to form an ion-associate. The resulting ion-associate phase (IAP) is separated by centrifugation and the aqueous phase is discarded. The
Analytical SciencesIAP is dissolved in an organic solvent, 15 and a mixed solution consisting of an organic solvent and acid, 6 back-extracted with acid, 16 and the analyte is then measured through atomic spectroscopic methods.The hydrophobic chelating agent, DPM, acts as the organic anion in the developed IAP.The combination of IAP extraction and back extraction is the best combination for lithium pre-concentration and LEP-AES measurement. Therefore, we used this method to measure lithium in seawater by LEP-AES and in river water and spring water by GF-AAS. River water and spring water were measured by GF-AAS because the concentration of lithium is more than an order of magnitude lower than seawater and cannot be measured...