期刊
ANALYTICAL LETTERS
卷 55, 期 5, 页码 741-754出版社
TAYLOR & FRANCIS INC
DOI: 10.1080/00032719.2021.1965154
关键词
Cadmium; cloud point extraction; flow-batch analysis; high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS); metal pre-concentration
资金
- FAPESP (Sao Paulo Foundation) [2011/19730-3, 2016/23878-0, 2015/11.523-0]
- CAPES (Coordination of Superior Level Staff Improvement) [001]
- CNPq (National Research Council) [308586/2018-2]
The study presents a computer-controlled multicommuted flow-batch system for the online cloud point extraction of metal ions followed by high-resolution continuum source flame atomic absorption spectrometric detection. By optimizing parameters, a wide linear range, low detection limit, low quantification limit, and low coefficient of variation were achieved.
A computer-controlled multicommuted flow-batch system is reported that allows for the online cloud point extraction of metal ions followed by high-resolution continuum source flame atomic absorption spectrometric (HR-CS GFAAS) detection. This approach combines reduced sample and reagent consumption and a short analysis time with the increased precision and sensitivity characteristic of flow-batch analysis and modern extraction techniques. As proof of concept, cadmium in aqueous solutions was determined by the formation of a hydrophobic complex [Cd(PAN)(2)]. Parameters related to complex formation (pH, pyridyl-azo-naphthol-PAN concentration, complexation time), cloud point extraction (Triton X-114 concentration, electrolyte composition, rich phase trapping), and the multicommuted flow-batch system (flow rates, timing control) were optimized. A small column packed with hydrophobic cotton was used as the interface between the extraction and detection stages to stack the cadmium-containing rich phase in a short plug. Optimized parameters led to a 5.0 to 75.0 mu g L-1 linear range, 1.3 mu g L-1 limit of detection, 4.3 mu g L-1 limit of quantification and 1.8% coefficient of variation (n = 12). Accuracy was evaluated by analyzing a certified reference material EP-H (drinking water) and by recovery tests employing tap water, groundwater, mineral water, and reuse water samples.
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