Univariate Optimization of Dispersive LiquideLiquid Micro-extraction for Pre-concentration of Lead From Environmental Matrices, Samawah Region Prior to Quantification Using Flame Atomic Absorption Spectroscopy

Abstract

In this work, a procedure based on dispersive liquid₋liquid micro-extraction for lead (Pb) pre-concentration andquantification in an environmental matrix by flame atomic absorption spectroscopy (FAAS) was applied. A case-studyapproach was chosen to obtain further in-depth information on the Pb levels. The green chemistry principles have beenapplied for the pretreatment and preparation of real samples by focusing on some features such as the volume ofreagents/sample, employ of energy efficient equipment, and production of waste. A univariate strategy was utilized toachieve the optimum extraction conditions. 1750 mL of acetonitrile containing 100 mL of carbon tetrachloride, were rapidinjection into: 12.0 mL of a sample solution adjusted the pH at 9.0 and 0.07% (m v¡1) Dithizone. The estimated limits ofdetection (LOD) and quantification (LOQ) under optimum conditions were 2.85 and 9.5 mg L¡1, respectively. Theenrichment factors EFs were found to be 60.6 (aqueous standards/DLLME₋FAAS) and 30.8 (matrix matched/DLLME₋-FAAS). It was applied for the analyzing eleven environmental samples. The detectable Pb levels for water samples wereranged from 1.87 to 8.11 mg L¡1, while in solid samples were ranged 0.39e4.66 mg g¡1. The relative standard deviation forthree concentrations (low, medium, and high) were found to be 10.64, 6.87, and 2.7, respectively. The presented systemwas validated by analyzing eleven environmental samples (water, bivalve molluscs, lettuce, and medicinal plants). Theresults indicated that high recoveries were obtained in the range of 92e104 %. The lead concentration was found in thesesamples always lower than permissible maximum levels stipulated by Iraqi Standards Specifications 2009 (number 417)for neutral water. The DLLME/FAAS procedure has proven to be a fast, simple, low-cost, and efficient analytical protocol, therefore allowing for employing this protocol in routine analysis of trace metals in such matrixes