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Internal standardization and least-squares background correction in high-resolution continuum source flame atomic absorption spectrometry to eliminate interferences on determination of Pb in phosphoric acid
Authors:Jorge L Raposo Jr  Silvana R Oliveira  Joaquim A Nóbrega  José A Gomes Neto
Institution:1. São Paulo State University, UNESP, Institute of Chemistry, Analytical Chemistry Department, P.O. Box 355, 14801-970 Araraquara — SP, Brazil;2. Universidade Federal de São Carlos, Departamento de Química, 13560-970 São Carlos — SP, Brazil
Abstract:In this work the least-squares background correction (LSBC) and internal standardization (IS) techniques were combined to eliminate spectral and transport interferences in the determination of Pb in phosphoric acid by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). Blanks, samples and reference solutions 0.10–1.00 mg L− 1 Pb in 1% (v/v) HNO3] were spiked with 4.00 mg L− 1 Co used as internal standard. For absorbance measurements at the wavelength integrated absorbance equivalent to 9 pixels, correlations between the ratio of absorbance of Pb to absorbance of Co and the analyte concentration were close to 0.9992. Relative standard deviations of measurements varied from 0.6 to 4% and 1 to 7% (n = 12) without and with IS/LSBC techniques, respectively. Recoveries for Pb spikes were in the 96–104% and 76–180% range with and without IS/LSBC, respectively. The limit of detection improved with IS/LSBC techniques. Accuracy of the proposed method was checked for the determinations of Pb in commercial phosphoric acid samples and results obtained with IS were better than those without IS.
Keywords:Lead  Phosphoric acid  Least Least-squares background correction  Internal standardization  High-resolution continuum source atomic absorption spectrometry
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