A Simple Method for the Determination of Lead Isotope Ratios in Ancient Glazed Ceramics Using Inductively Coupled Plasma-Quadrupole Mass Spectrometry

Content Provider	Semantic Scholar
Author	Marzoa, P. Labordaa, F. Pérez-Aranteguia, J.
Copyright Year	2008
Abstract	A simple method of singledrop microextraction (SDME) combined with electrothermal atomic absorption spectrometry is proposed for the determination of trace Pb using dithizone as the extractant. Several factors influencing the microextraction efficiency (pH, extraction time, dithizone concentration, organic drop volume, stirring rate, and sample volume) were investigated and optimized. Under the optimized conditions, a detection limit (3σ) of 0.73 ng mL–1 and an enrichment factor of 74 were achieved. The relative standard deviation was 7.7% (c=10 ng mL–1, n=5). The developed method was applied to the determination of trace Pb in water samples with satisfactory results. difficult because the low concentrations present fall below the detection limits of conventional analytical techniques and because of matrix effects. Hence, preconcentration and separation techniques are still necessary. Solid-phase extraction (8–11) and liquid-liquid extraction (LLE) (12–15) are classic pretreatment techniques that have been widely employed in analytical chemistry. However, conventional LLE consumes large amounts of expensive and potentially hazardous organic solvents, the disposal of which is problematic and very time-consuming to perform. INTRODUCTION It is now known that Pb has serious influences on the environment and human health. Its influence on the environment is through contamination of the air and water. Lead accumulates in the body, including the brain, liver, kidney, and heart and has a high potential for toxicity. Inorganic lead, in particular, can be absorbed into the bloodstream where it is distributed to soft tissues, bones, and teeth (95% in bones and teeth) (1). In addition, it also can destroy the central nervous and reproductive systems. Therefore, the ability to determine trace amounts of Pb is of great importance. For the determination of trace Pb in a variety of materials, highly sensitive and selective analytical techniques have been used including inductively coupled plasma atomic emission spectrometry (ICPAES) (2), atomic fluorescence spectrometry (AFS) (3), atomic absorption spectrometry (AAS) (4–6), and inductively coupled plasma mass spectrometry (ICP-MS) (7). In particular, electrothermal atomic absorption spectrometry (ETAAS) has long been considered one of the most suitable instrumental techniques for the determination of trace Pb in different samples due to its excellent analytical performance, simple operating procedures, low cost of instrumentation, high sensitivity and selectivity. However, the determination of trace Pb in natural water samples is Recently, liquid-liquid microextraction (LPME) (16–19) has attracted increasing attention as a novel technique for sample preparation. Jeannot and Cantwell (20) were first to report a novel singledrop microextraction (SDME) technique. In their report, a small organic solvent drop that was immiscible with water was held at the end of a Teflon® rod, which was immersed in a stirred aqueous sample solution. After extracting for a prescribed period of time, the micro-drop was retracted back into the microsyinge and transferred to a gas chromatograph for further analysis. This technique is simple, inexpensive, and employs a minimal amount of toxic organic solvents. Therefore, further studies have exploited the analytical application of SDME (21,22). In the past few years, this method was primarily applied to the determination of organic compounds in water and various environmental and biological samples. Recently, there have been several reports on the study of single-drop microextraction for inorganic analytes (23,24). However, few analytical applications of the SDME method for extraction and preconcentration of metal ions have been reported. SDME is a miniaturized sample pre-treatment technique and ETAAS is a microvolume sample analysis technique. Therefore, it will be a perfect combination if SDME is combined with ETAAS. In this work, a dithizone-carbon tetrachloride single-drop microextraction system is combined with electrothermal atomic absorption spectrometry for the determination of trace Pb in water samples.
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