Development of a Methodology Based on Extraction Induced by Emulsion Breaking for Copper Determination in Gasohol by Graphite Furnace Atomic Absorption Spectrometry
The development of a method based on extraction induced by emulsion breaking (EIEB) aiming copper determination in gasohol using graphite furnace atomic absorption spectrometry (GF AAS) is reported. Emulsification of the gasohol samples was carried out using nitric acid solution, (1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol surfactant (Triton X-114), and ultrasound energy. The variables related to the extraction efficiency were optimized by multivariate approaches (two-level factorial fractional design and Doehlert design). The best results were obtained when the emulsion was formed with 5.0 mL of the sample, 0.200 mL of 2.4 mol L-1 HNO3, 0.100 mL of 10% Triton X-114 and 10 min of sonication. A fast and efficient emulsion breaking was performed at 90 ºC. A volume of 6.65 mL of the copper-rich hydroalcoholic phase was extracted, separated from the organic phase and analyzed. Under these conditions, the following analytical characteristics were obtained: 0.61 and 2.0 µg L-1 for limits of detection and quantification, respectively; precision (percentage of relative standard deviation, 10 µg L-1) of 2.8%; and analytical sensitivity of 0.011 L µg -1. Accuracy was assessed by spike tests, and values in the range of 95-110% were achieved. The method was applied in the determination of copper in Brazilian gasoline samples (gasohol with 27% ethanol).
| Main Authors: | , , , , |
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| Format: | Digital revista |
| Language: | English |
| Published: |
Sociedade Brasileira de Química
2021
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| Online Access: | http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532021000200329 |
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| Summary: | The development of a method based on extraction induced by emulsion breaking (EIEB) aiming copper determination in gasohol using graphite furnace atomic absorption spectrometry (GF AAS) is reported. Emulsification of the gasohol samples was carried out using nitric acid solution, (1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol surfactant (Triton X-114), and ultrasound energy. The variables related to the extraction efficiency were optimized by multivariate approaches (two-level factorial fractional design and Doehlert design). The best results were obtained when the emulsion was formed with 5.0 mL of the sample, 0.200 mL of 2.4 mol L-1 HNO3, 0.100 mL of 10% Triton X-114 and 10 min of sonication. A fast and efficient emulsion breaking was performed at 90 ºC. A volume of 6.65 mL of the copper-rich hydroalcoholic phase was extracted, separated from the organic phase and analyzed. Under these conditions, the following analytical characteristics were obtained: 0.61 and 2.0 µg L-1 for limits of detection and quantification, respectively; precision (percentage of relative standard deviation, 10 µg L-1) of 2.8%; and analytical sensitivity of 0.011 L µg -1. Accuracy was assessed by spike tests, and values in the range of 95-110% were achieved. The method was applied in the determination of copper in Brazilian gasoline samples (gasohol with 27% ethanol). |
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