Abstract

A simple rapidly synergistic cloud point extraction procedure has been developed for the separation and preconcentration of trace amounts of lead from food and water samples by flame atomic absorption spectrometry (FAAS). Rapidly synergistic cloud point extraction (RS-CPE) greatly simplified and accelerated the procedure of traditional cloud point extraction (CPE). This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent which lowered the cloud point temperature of Triton X-114 and assisted the subsequent extraction process. Some parameters that influenced cloud point extraction and subsequent determination were evaluated in detail, such as sample pH, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time and ionic strength, as well as interferences. Under optimized conditions (pH 8.5, octanol: 10 µL, Triton X-114: 0.04% w/v and diluting solvent: 1 mol L-1 HNO3 in methanol), an enhancement factor of 40 could be obtained, and the detection limit (LOD) for lead was 1.6 µg L-1. Relative standard deviation for ten replicate determinations of the standard solution containing 100 µg L-1 lead was 2.1%. The proposed method was applied for the determination of lead in food (spinach, rice and black tea bag) and water samples and satisfactory results were obtained.

Highlights

  • The environment and all the life on earth face a very serious threat due to heavy metal pollution resulting from rapid industrialization and increase in world population

  • In 1991, the United States Environmental Protection Agency (USEPA) published a regulation to control lead in drinking water, which included an action level of 0.015 mg L−1.5 The World Health Organization (WHO) has released the guidelines for drinking water quality containing the guideline value 0.01 mg Pb L−1.6 the accurate determination of lead at trace levels in environmental samples is a subject of great concern

  • The effect of octanol amounts In rapidly synergistic cloud point extraction (RS-cloud point extraction (CPE)), octanol worked as cloud point revulsant and synergic reagent as mentioned before, which lowered the cloud point of the surfactant below room temperature and assisted the subsequent extraction process

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Summary

Introduction

The environment and all the life on earth face a very serious threat due to heavy metal pollution resulting from rapid industrialization and increase in world population. 500.0 mg of spinach was transferred into a 250 mL beaker and 5 mL of 0.5 mol L−1 HNO3 was added to moisten the sample thoroughly. This was followed by adding 10 mL of concentrated HNO3 and heating it on a hot plate at 130 °C for 3 h. The mixture was heated gently until the completion of sample decomposition In this step, a clear solution was obtained. 5.0 grams of powdered rice sample was dissolved in 25 mL concentrated HNO3 and heated on a hot plate at a low temperature. Before doing the CPE procedure, the digested samples were neutralized with NaOH and the pH was reached to 8.5 by adding buffer

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