Chapters authored
A Simple and Highly Structured Procaine Hydrochloride as Fluorescent Quenching Chemosensor for Trace Determination of Mercury Species in Water
An ultrasensitive, simple and highly selective spectrofluorometric strategy for quantifying traces of mercury(II) in environmental water has been established using the fluorescent probe procaine hydrochloride (PQ+.Cl−). The procedure was based upon the formation of the ternary ion associate complex [(PQ+)2.(HgI4)2−] between PQ+.Cl− and mercury(II) in iodide media at pH 9.0–10.0 with its subsequent extraction onto dichloromethane accompanied by a change in fluorescence intensity at λex/em = 268/333 nm. The developed strategy exhibited a linear range of 1–114 μg L−1 with lower limit of detection (LOD) and quantification (LOQ) of mercury(II) 1.3 and 3.98 nM, respectively. Intra and inter-day laboratory accuracy and precision for trace analysis of mercury(II) in water were performed. Complexed mercury(II) in environmental water, chemical speciation and successful literature comparison was performed. The proposed system offered excellent selectivity towards mercury(II) ions examined in the presence of competent ions in excess, relevant to real water samples. The method was applied for analysis of mercury(II) in tap water samples. Statistical comparison (Student’s t and F tests) of the proposed method with the reference ICP-OES method revealed no significant differences in the accuracy and precision.
Part of the book: Trace Elements
Chromatographic Separation, Total Determination and Chemical Speciation of Mercury in Environmental Water Samples Using 4-(2-Thiazolylazo) Resorcinol-Based Polyurethane Foam Sorbent-Packed Column
A simple method has been developed for quantitative retention of traces of mercury(II) ions from aqueous media using polyurethane foams (PUFs) loaded with 4-(2-thiazolylazo) resorcinol (TAR). The kinetics and thermodynamics of the sorption of mercury(II) ions onto PUFs were studied. The sorption of mercury(II) ions onto PUF follows a first-order rate equation with k = 0.176 ± 0.010 min−1. The negative values of ΔH and ΔS may be interpreted as the exothermic chemisorption process and indicative of a faster chemisorption onto the active sites of the sorbent. The sorption data followed Langmuir, Freundlich and Dubinin-Radushkevich (D–R) isotherm models. The D-R parameters β, KDR and E were 0.329 mol2 kJ−2, 0.001 μmol g−1 and 1.23 ± 0.07 kJ/mol for the TAR-loaded PUFs, respectively. An acceptable retention and recovery (99.6 ± 1.1%) of mercury(II) ions in water at ≤10 ppb by the TAR-treated PUFs packed columns were achieved. A retention mechanism, involving absorption related to “solvent extraction” and an “added component” for surface adsorption, was suggested for the retention of mercury(II) ions by the used solid phase extractor. The performance of TAR-immobilized PUFs packed column in terms of the number (N), the height equivalent to a theoretical plate (HETP), the breakthrough and critical capacities of mercury(II) ion uptake by the sorbent packed column were found to be 50.0 ± 1.0, 1.01 ± 0.02 mm, 8.75 and 13.75 mg/g, respectively, at 5 mL/min flow rate.
Part of the book: Chemometrics and Data Analysis in Chromatography