2023•SeparationsOpen access

Determination of Ultra-Trace Amounts of Copper in Environmental Water Samples by Dispersive Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry

Quan Han, Xiaohui Yang, Yanyan Huo, Jiale Lu, Yaqi Liu

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Abstract

A new method of dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of ultra-trace copper. It was based on the reaction of Cu(II) with the laboratory-prepared chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in a HAc-NaAc buffer solution at pH 5.0 to form stable hydrophobic chelates, which were separated and enriched by DLLME with chlorobenzene (C6H5Cl) and acetonitrile (CH3CN) as extraction and disperser solvents, respectively. The sedimented phase containing the chelates was then determined with GFAAS. Various operating variables that may be affected by the extraction process such as the pH of the solution, the concentration of the chelating agent 5-Br-PADMA, the types and volumes of extraction and disperser solvents, the extraction time, and the centrifugation time were investigated. Under optimum conditions, the calibration curve was linear in the range from 0.02 ng/mL to 0.16 ng/mL of copper with a correlation coefficient of r = 0.9961, and the detection limit was 0.01 ng/mL based on 3Sb. The relative standard deviation for six replicate measurements of 0.05 ng /mL of copper was 3.9%. An enrichment factor (EF) of 110 was obtained. The method has the advantages of low detection limit, high sensitivity, simple operation, less consumption of organic solvents, higher enrichment factor, and environmental friendliness and was applied to the determination of trace copper in environmental water samples with satisfactory results.

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A new method of dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of ultra-trace copper. It was based on the reaction of Cu(II) with the laboratory-prepared chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in a HAc-NaAc buffer solution at pH 5.0 to form stable hydrophobic chelates, which were separated and enriched by DLLME with chlorobenzene (C6H5Cl) and acetonitrile (CH3CN) as extraction and disperser solvents, respectively. The sedimented phase containing the chelates was then determined with GFAAS. Various operating variables that may be affected by the extraction process such as the pH of the solution, the concentration of the chelating agent 5-Br-PADMA, the types and volumes of extraction and disperser solvents, the extraction time, and the centrifugation time were investigated. Under optimum conditions, the calibration curve was linear in the range from 0.02 ng/mL to 0.16 ng/mL of copper with a correlation coefficient of r = 0.9961, and the detection limit was 0.01 ng/mL based on 3Sb. The relative standard deviation for six replicate measurements of 0.05 ng /mL of copper was 3.9%. An enrichment factor (EF) of 110 was obtained. The method has the advantages of low detection limit, high sensitivity, simple operation, less consumption of organic solvents, higher enrichment factor, and environmental friendliness and was applied to the determination of trace copper in environmental water samples with satisfactory results.

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Available abstract

A new method of dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of ultra-trace copper. It was based on the reaction of Cu(II) with the laboratory-prepared chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in a HAc-NaAc buffer solution at pH 5.0 to form stable hydrophobic chelates, which were separated and enriched by DLLME with chlorobenzene (C6H5Cl) and acetonitrile (CH3CN) as extraction and disperser solvents, respectively. The sedimented phase containing the chelates was then determined with GFAAS. Various operating variables that may be affected by the extraction process such as the pH of the solution, the concentration of the chelating agent 5-Br-PADMA, the types and volumes of extraction and disperser solvents, the extraction time, and the centrifugation time were investigated. Under optimum conditions, the calibration curve was linear in the range from 0.02 ng/mL to 0.16 ng/mL of copper with a correlation coefficient of r = 0.9961, and the detection limit was 0.01 ng/mL based on 3Sb. The relative standard deviation for six replicate measurements of 0.05 ng /mL of copper was 3.9%. An enrichment factor (EF) of 110 was obtained. The method has the advantages of low detection limit, high sensitivity, simple operation, less consumption of organic solvents, higher enrichment factor, and environmental friendliness and was applied to the determination of trace copper in environmental water samples with satisfactory results.

Key concepts: Graphite furnace atomic absorption, Detection limit, Chemistry, Enrichment factor, Extraction (chemistry), Copper, Calibration curve, Chromatography

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