The green synthesis of magnesium oxide nanocomposite-based solid phase for the extraction of arsenic, cadmium, and lead from drinking water.

Solid-phase extraction (SPE) has attracted the attention of scientists because it can increase the selectivity and sensitivity measurements of analytes. Therefore, this study is designed to synthesise magnesium oxide nanoparticles (D-MgO-NPs) by an eco-friendly method using biogenic sources Duranta erecta followed by fabricating its chitosan-based polymeric composite (D-MgO-NC) for the SPE of heavy metals (HMs), i.e., arsenic (As), cadmium (Cd), and lead (Pb) from drinking water. Various analytical techniques were used for the surface characterization of D-MgO-NPs and D-MgO-NC. FTIR findings confirmed the formation of D-MgO-NC based on MgO association with the -OH/-NH2 of the chitosan. D-MgO-NC showed the smallest size of particles with rough surface morphology, followed by the crystalline cubic structure of MgO in its nanoparticle and composites. The synthesised D-MgO-NC was used as an adsorbent for the SPE of HMs from contaminated water, followed by their detection by atomic absorption spectrometry. Various experimental parameters, including pH, flow rate, the concentration of HMs, eluent composition, and volume, were optimised for the preconcentration of HMs. The limits of detection for As, Cd, and Pb of the proposed D-MgO-NC-based SPE method were found to be 0.008, 0.006, and 0.012 µm L-1, respectively. The proposed method has an enrichment factor and relative standard deviation of >200 and <5.0%, respectively. The synthesised D-MgO-NC-based SPE method was successfully applied for the quantitative detection of As, Cd, and Pb in groundwater samples, which were found in the range of 18.3 to 15.2, 3.20 to 2.49, and 8.20 to 6.40 µg L-1, respectively.

Biosynthesis and Analytical Characterization of Iron Oxide Nanobiocomposite for In-Depth Adsorption Strategy for the Removal of Toxic Metals from Drinking Water.

The biosynthesis of the iron oxide nanoparticles was done using Ixoro coccinea leaf extract, followed by the fabrication of iron oxide nanobiocomposites (I-Fe3O4-NBC) using chitosan biopolymer. Furthermore, the synthesized I-Fe3O4-NPs and I-Fe3O4-NBC were characterized, and I-Fe3O4-NBC was applied to remove toxic metals (TMs: Cd, Ni, and Pb) from water. The characterization study confirmed that the nanostructure, porous, rough, crystalline structure, and different functional groups of chitosan and I-Fe3O4-NPs in I-Fe3O4-NBCs showed their feasibility for the application as excellent adsorbents for quantitative removal of TMs. The batch mode strategy as feasibility testing was done to optimize different adsorption parameters (pH, concentrations of TMs, dose of I-Fe3O4-NBC, contact time, and temperature) for maximum removal of TMs from water by Fe3O4-NBC. The maximum adsorption capacities using nanocomposites for Cd, Ni, and Pb were 66.0, 60.0, and 66.4 mg g-1, respectively. The adsorption process follows the Freundlich isotherm model by I-Fe3O4-NBC to remove Cd and Ni, while the Pb may be adsorption followed by multilayer surface coverage. The proposed adsorption process was best fitted to follow pseudo-second-order kinetics and showed an exothermic, favorable, and spontaneous nature. In addition, the I-Fe3O4-NBC was applied to adsorption TMs from surface water (%recovery > 95%). Thus, it can be concluded that the proposed nanocomposite is most efficient in removing TMs from drinking water up to recommended permissible limit.

Use of an aminated Amberlite XAD-4 column coupled to flow injection cold vapour generation atomic absorption spectrometry for mercury speciation in water and fish tissue samples.

An aminated Amberlite XAD-resin as a solid phase extractant was tested for speciation of inorganic mercury, Hg(II) and methylmercury, MeHg(I) in water and fish tissue samples. It was found that Hg(II) and MeHg(I) ions could be simultaneously retained by a column filled with AAXAD-4 resin at pH 4 and the sequential quantitative elutions of Hg(II) and MeHg(I) were achieved using 10 mL of 0.1%(m/v) thiourea in 3%(v/v) HCl and 10 mL of 6 mol L-1 HCl, respectively. Hg(II) in the eluent was directly determined and MeHg(I) in the second eluent is quantified using FI-CVG-AAS after its oxidative digestion with KMnO4. The limits of detection for Hg(II) and MeHg(I) ions were found to be 0.148 and 0.157 µg L-1, respectively. The method was validated by analysing a certified reference material. The relative errors for Hg(II), MeHg(I) and T-Hg were in range of -1.8% and -3.2%.

Ion pair-dispersive liquid-liquid microextraction coupled to microsample injection system-flame atomic absorption spectrometry for determination of gold at trace level in real samples.

A novel ion pair-dispersive liquid-liquid microextraction (IP-DLLME) of gold followed by its determination with microsample injection system-flame atomic absorption spectrometry (MIS-FAAS) detection was developed. The extraction method was based on the reaction of anionic tetrachloro gold(III) complex with the cationic form of Rhodamine B to give a violet ion pair complex, which is extracted from 1.0 mol L(-1) HCl solution of 8.0 mL to fine droplets of chloroform of 500 µL. A Plackett-Burman experimental design of MINITAB statistical program was employed to optimize the influence of main parameters to be controlled in DLLME. After optimizing the extraction conditions, gold was quantitatively recovered by preconcentration factor of 40, limit of detection (LOD) of 1.8 µg L(-1) and relative standard deviation of less than 6.8%. The proposed method was successfully applied to the preconcentration and determination of gold in some samples such as tap water, waste water, copper electrolysis solution and copper wire coated nickel.

Solid-phase chelate extractive preconcentration of heavy metal ions prior to their ultratrace determination by microsample injection system coupled flame atomic absorption spectrometry.

Chromosorb-105 resin/1-(2-pyridylazo)-2-naphthol (PAN) system was developed for solid phase chelate extractive preconcentration of heavy metal ions. The metal ions on Chromosorb-105 resin column were eluted with 3.0 mL of 2.0 mol L-1 HNO3 and determined by microsample injection system coupled flame atomic spectrometry (MIS-FAAS) using 75.0 µL of sample solution for single element determination. The influence of pH, resin amount, reagent amount, flow rate and volume of eluent and sample solution was optimized. The quantitative recoveries (≥95%) of Fe(III), Zn(II), Cu(II) and Pb(II) ions were achieved at pH 9; resin amount, 700 mg; reagent amount, 6.0 µmol; flow rate of eluent and sample solution, 1.0 mL min-1 and 5.0 mL min-1, respectively. The limit of detection and limit of quantification of understudied analytes were found to be 0.17-1.74 µg L-1 and 0.40-2.98 µg L-1, respectively with preconcentration factor of 150-300. The proposed method was validated by analysis of waste water (BCR-715) as a certified reference material. The method was applied successfully for ultratrace determination of studied metal ions in tap water and hot spring water samples.

Determination of cobalt, nickel and iron at trace level in natural water samples by in-column chelation-reversed phase high-performance liquid chromatography.

This paper reports the utilization of 4-(2-pyridylazo) resorcinol (PAR) as a chelating reagent for in-column derivatization and the determination of trace Co, Fe, and Ni ions by reversed-phase high-performance liquid chromatography with photodiode array detector. A good separation of Co, Fe, and Ni chelates were achieved by using an Inertsil ODS-3 column and a mobile phase, consisted of methanol-THF-water mixture (50:5:45) containing ammonium acetate buffer (pH 5.0) and PAR. After full optimization, good repeatability of retention times (relative standard deviation (RSD) < 0.05%) and peak areas (RSD < 1.7%) was achieved as well as a good linearity (r (2) > 0.9991). The detection limits (S/N = 3), expressed as micrograms per liter, were 0.50 (Co), 9.07 (Fe), and 2.00 (Ni). The applicability and the accuracy of the developed method were estimated by the analysis of spiked water samples and certified reference material BCR 715 wastewater-SRM.

Selective extraction of chromium(VI) using a leaching procedure with sodium carbonate from some plant leaves, soil and sediment samples.

Speciation of chromium in some plant leaves, soil and sediment samples was carried out by selective leaching of Cr(VI) using a sodium carbonate leaching procedure. Total chromium from the samples was extracted using aqua regia and oxidative acid digestion, respectively. The concentrations of chromium species in the extracts were determined using by graphite furnace atomic absorption spectrometry (GFAAS). Uncoated graphite furnace tubes were used as an atomizer. Due to the presence of relatively high amounts of Na(2)CO(3) in the resulting samples, the possible influences of Na(2)CO(3) on the absorbance signals were checked. There is no interference of Na(2)CO(3) on the chromium absorbance up to 0.1 mol L(-1) Na(2)CO(3). A limit of detection (LOD) for determination of Cr(VI) in 0.1 Na(2)CO(3) solution by GFAAS was found to be 0.93 microg L(-1). The procedure was applied to environmental samples. The relative standard deviation, R.S.D. as precision for 10 replicate measurements of 20 microL(-1) Cr in processed soil sample was 4.2%.