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Synthesis of α-Nitroso-β-Naphthol Modified Amberlite XAD-2 Resin and its Application in On-Line Solid Phase Extraction System for Cobalt Preconcentration

Valfredo Azevedo Lemos, Juracir Silva Santos, Patrícia Xavier Baliza

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Abstract

In this work, an on-line system for preconcentration and determination of cobalt at μg1−1 level is proposed. Amberlite XAD-2 functionalized with α-nitroso-β-naphthol (NN-XAD) packed in a minicolumn was used as sorbent. Cobalt (II) ions were sorbed in the minicolumn, from which it could be eluted by hydrochloric acid solution. This eluate reacted with Nitroso Salt R and the absorbance of the complex was read at 510 nm in a spectrophotometer. Signals were measured as peak height by using instrument software. Achieved sampling rate was 45 samples per hour. Analytical parameters were evaluated and the results demonstrated that cobalt can be determined, with sample pH in the range of 7.0–8.5, preconcentration time of 60s with a sample flow rate of 5.0mL min−1. The detection limit (3 s) was 6.0 μg1−1 and the precision (assessed as the relative standard deviation) reached values of 6.1 to 1.9% in cobalt solutions of 10 to 300 μg1−1 concentration, respectively. The proposed procedure was applied in natural waters. Recoveries of spike additions (10, 25, or 50 μg1−1) to natural water samples were quantitative (92–106%).

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What this paper is about

In this work, an on-line system for preconcentration and determination of cobalt at μg1−1 level is proposed. Amberlite XAD-2 functionalized with α-nitroso-β-naphthol (NN-XAD) packed in a minicolumn was used as sorbent. Cobalt (II) ions were sorbed in the minicolumn, from which it could be eluted by hydrochloric acid solution. This eluate reacted with Nitroso Salt R and the absorbance of the complex was read at 510 nm in a spectrophotometer. Signals were measured as peak height by using instrument software. Achieved sampling rate was 45 samples per hour. Analytical parameters were evaluated and the results demonstrated that cobalt can be determined, with sample pH in the range of 7.0–8.5, preconcentration time of 60s with a sample flow rate of 5.0mL min−1. The detection limit (3 s) was 6.0 μg1−1 and the precision (assessed as the relative standard deviation) reached values of 6.1 to 1.9% in cobalt solutions of 10 to 300 μg1−1 concentration, respectively. The proposed procedure was applied in natural waters. Recoveries of spike additions (10, 25, or 50 μg1−1) to natural water samples were quantitative (92–106%).

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Available abstract

In this work, an on-line system for preconcentration and determination of cobalt at μg1−1 level is proposed. Amberlite XAD-2 functionalized with α-nitroso-β-naphthol (NN-XAD) packed in a minicolumn was used as sorbent. Cobalt (II) ions were sorbed in the minicolumn, from which it could be eluted by hydrochloric acid solution. This eluate reacted with Nitroso Salt R and the absorbance of the complex was read at 510 nm in a spectrophotometer. Signals were measured as peak height by using instrument software. Achieved sampling rate was 45 samples per hour. Analytical parameters were evaluated and the results demonstrated that cobalt can be determined, with sample pH in the range of 7.0–8.5, preconcentration time of 60s with a sample flow rate of 5.0mL min−1. The detection limit (3 s) was 6.0 μg1−1 and the precision (assessed as the relative standard deviation) reached values of 6.1 to 1.9% in cobalt solutions of 10 to 300 μg1−1 concentration, respectively. The proposed procedure was applied in natural waters. Recoveries of spike additions (10, 25, or 50 μg1−1) to natural water samples were quantitative (92–106%).

Key concepts: Amberlite, Chemistry, Detection limit, Cobalt, Elution, Chromatography, Solid phase extraction, Absorbance

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Synthesis of α-Nitroso-β-Naphthol Modified Amberlite XAD-2 Resin and its Application in On-Line Solid Phase Extraction System for Cobalt Preconcentration — Research Paper | ScholarLens