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Obtaining new nanocomposites with sorption properties towards chromium is highly important not only from the environmental point of view but also for developing eco-friendly methods of chromium determination. The potential use of aluminum oxide-coated nano-graphite (Al2O3/nano-G) as a new nanosorbent in ultrasound-assisted dispersive micro-solid-phase extraction (DMSPE) for rapid speciation of trace chromium(III) and chromium(VI) ions in natural water was evaluated. In the developed method, the crucial issue is the new nanocomposite synthesized by coating alumina on a nano-graphite surface with sorption properties. Structural researches of the nanocomposite were carried out by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and Raman spectroscopy. Maximum adsorption capacity of Al2O3/nano-G towards Cr(III) was 32.8 mg g−1. The influence of the method’s factors like pH, sample volumes, contact time, coexisting ions, and humic acid on the recovery of chromium was examined. The nanocomposites have been found to be stable and effective as a sorbent in water with high concentrations of selected cations and anions present in water as well as in water of various pH. Al2O3/nano-G is selective for Cr(III) in presence of Cr(VI). Cr(III) was determined by the developed method, total Cr after reduction of Cr(VI) to Cr(III), and Cr(VI) was calculated as the difference between total Cr and Cr(III). After sorption, the nanocomposite with chromium was collected on 5-mm diameter filters and analyzed by energy-dispersive X-ray fluorescence spectrometry (EDXRF) to determine the chromium concentration. The method was characterized by correlation coefficient 0.999, limit of detection (LOD) 0.04 ng mL−1, and relative standard deviation (RSD) 3.5%. Al2O3/nano-G combined with proposed DMSPE/EDXRF was verified by analysis of certificate reference material of natural water (NIST 1640a). Graphical abstractᅟ

A nanocomposite prepared from graphene nanosheets and cerium nanoparticles (G/CeO2) was applied to the extraction of Se(IV), As(V), As(III), Cu(II) and Pb(II). The structure of G/CeO2 was investigated by scanning electron microscopy, X-ray diffraction and Raman spectroscopy. The optimal pH values for extraction are 4.0 for As(V), 3.0 for Se(IV), and 6.0 for both Cu(II) and Pb(II). The maximum adsorption capacity of G/CeO2 (expressed as mg·g−1) were calculated by the Langmuir model and are found to be 8.4 for As(V), 14.1 for Se(IV), 50.0 for Cu(II) and 75.6 for Pb(II). The sorbent was applied to dispersive solid phase microextraction prior to direct quantitation by energy-dispersive X-ray fluorescence spectrometry without the need for prior elution. The limits of detection (in ng·mL−1 units) are 0.10 for As(V), 0.11 for Se(IV), 0.19 for Cu(II) and 0.21 for Pb(II). The precisions (RSDs) are

Graphene oxide decorated with cerium(IV) oxide (GO/CeO2) was synthesized and applied in adsorption of several metal ions such as As(III), As(V), Se(IV), Cu(II), and Pb(II) from aqueous samples. The important feature of GO/CeO2 nanocomposite is also its selectivity toward selenite in the presence of selenate. The structure of GO/CeO2 has been proven by microscopic and spectroscopic techniques. The maximum adsorption capacities of GO/CeO2 calculated by Langmuir model toward arsenic, selenium, copper, and lead ions are between 6 and 30 mg g–1. An interesting feature of this adsorbent is its excellent dispersibility in water. Thus, GO/CeO2 nanocomposite is ideal for fast and simple determination of heavy metal ions using dispersive microsolid phase extraction (DMSPE). Moreover, coupling DMSPE with energy-dispersive X-ray fluorescence spectrometry (EDXRF) is extremely beneficial because it allows direct analysis of adsorbent. Thus, the analyte elution step, as needed in many analytical techniques, was obviated...

Alumina supported on graphene oxide (Al2O3/GO) nanocomposite as new nanosorbent in dispersive micro-solid phase extraction (DMSPE) for As(V) and Cr(III) preconcentration is described. The crucial issue of the study is synthesis of novel nanocomposite suitable for sorption of selected species of arsenic and chromium. Al2O3/GO demonstrates selectivity toward arsenates in the presence of arsenites at pH 5 and chromium(III) ions in the presence of chromate anions at pH 6. The Al2O3/GO nanocomposite was characterized by scanning electron microscopy (SEM) transmission electron microscopy (TEM), powder X-ray diffraction (XRD) and the Raman spectroscopy. The maximum adsorption capacity calculated based on the Langmuir adsorption model were 43.9 mg g−1 and 53.9 mg g−1 for As(V) and Cr(III), respectively. The nanocomposite was used as solid sorbent in preconcentration of As(V) and Cr(III)_ions from water samples and their determination using energy dispersive X-ray fluorescence spectrometry (EDXRF). The As(V) and Cr(III) ions can be quantitatively preconcentrated from 25 to 100 mL aqueous samples within 5 min using DMSPE procedure and 1 mg of Al2O3/GO. The nanocomposite was also used for preparation of Al2O3/GO membrane. Then, As(V) and Cr(III)_ions can be retained under flow condition by passing analyzed solution through Al2O3/GO membrane. Under the optimized conditions, As(V) and Cr(III) ions can be determined with very good recovery (92–108%), precision (RSD 2.7–4.0%) and excellent limit of detection (0.02 ng mL−1 As and 0.11 ng mL−1 Cr). The accuracy of the method was studied by analyzing certified reference materials (NIST 1640a) and spiked real water samples.

We describe a novel solid phase sorbent that was synthesized by coupling graphene oxide (GO) to ethylenediamine (EDA). This nanomaterial (referred to as GO-EDA) is capable of adsorbing the ions of iron, cobalt, nickel, copper, zinc and lead. The ethylenediamine-modified graphene oxide was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy and Fourier transform infrared spectroscopy. The analytical procedure relies on (a) sorption of metal ions on GO-EDA dispersed in aqueous samples; (b) filtering, and (c) direct submission of the filter paper to energy-dispersive X-ray fluorescence spectrometry. This kind of dispersive micro-solid phase extraction was optimized with respect to pH values, concentration of GO-EDA, contact time, and the effects of interfering ions and humic acid on recovery of determined elements. Under optimized conditions, the recoveries of spiked samples range from 90 to 98 %. The detection limits are 0.07, 0.10, 0.07, 0.08, 0.06 and 0.10 ng mL−1 for Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Pb(II), respectively. The method has a relative standard deviation of