Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by flame atomic absorption spectrometry.
A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML(2)). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5x10(-2) mol L(-1), extraction temperature 40 degrees C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 microL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 microL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 microg L(-1), relative standard deviation (RSD) 5.5% and the working linear range 2-30 microg L(-1).
Carletto
Jeferson Schneider
JS
Departamento de Química-Universidade Federal de Santa Catarina, Florianópolis, 88040-900, Brazil.
Luciano
Raquel Medeiros
RM
Bedendo
Gizelle Cristina
GC
Carasek
Eduardo
E
D002104:Cadmium / Q000032:analysis* / Q000302:isolation & purification; D004129:Dimethylpolysiloxanes / Q000737:chemistry; D004492:Edetic Acid / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D063086:Organothiophosphates / Q000737:chemistry*; D015203:Reproducibility of Results; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013696:Temperature; D013997:Time Factors; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
D004129:Dimethylpolysiloxanes; D063086:Organothiophosphates; D014874:Water Pollutants, Chemical; D002104:Cadmium; C059015:O,O-diethyl dithiophosphate; C013830:baysilon; D004492:Edetic Acid