Effect of Ho3+ Substitution on Magnetic Properties of ZnCr2Se4.

A series of ZnCr2-xHoxSe4 microcrystalline spinels (where x = 0.05, 0.075, and 0.10) containing holmium ions in octahedral coordination were obtained by sintering of adequate reactants at high temperatures. The obtained doped materials were characterized by X-ray diffraction, Scanning Electron Microscopy, UV-Vis-NIR, molecular field approximation, and XPS spectroscopies. Their thermal properties were also investigated. The doping of the ZnCr2S4 matrix with paramagnetic Ho3+ ions with a content of not more than 0.1 and a screened 4f shell revealed a significant effect of orbital and Landau diamagnetism, a strong reduction in short-range ferromagnetic interactions, and a broadening and shift of the peak of the first critical field by simultaneous stabilization of the sharp peak in the second critical field. These results correlate well with FPLO calculations, which show that Cr sites have magnetic moments of 3.19 µB and Ho sites have significantly larger ones with a value of 3.95 µB. Zn has a negligible magnetic polarization of 0.02 µB, and Se induces a polarization of approximately -0.12 µB.

Ultrasound-assisted dispersive micro-solid phase extraction using molybdenum disulfide supported on reduced graphene oxide for energy dispersive X-ray fluorescence spectrometric determination of chromium species in water.

Molybdenum disulfide (MoS2) was supported on graphene oxide (GO) by hydrothermal method. The resulting nanocomposite (MoS2-rGO) was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The experiments show that at pH 2, MoS2-rGO has a great affinity for adsorption of hexavalent chromium ions while Cr(III) ions remain in aqueous sample. In the adsorption process, the dominant role plays chemisorption. The determined adsorption capacity is 583.5 mg g-1. Parameters affecting the extraction process, namely sample pH, sample volume, contact time, and matrix ions, were investigated by sequential batch tests. Under optimal conditions (pH 2, sample volume 50 mL, sonication time 10 min, adsorbent mass 1 mg), the calibration curve covers the 1-200 ng mL-1 range with a correlation coefficient (R2) of 0.998. The recovery of the method is 97 ± 3%. Other data of merit include a relative standard deviation of < 3.5%, enrichment factor of 3350, and detection limit of 0.050 ng mL-1. The accuracy of the method was confirmed by analysis of the reference materials QC1453 (chromium VI in drinking water) and QC3015 (chromium VI in seawater). The method was successfully applied to chromium speciation in water samples, including high salinity ones. The concentration of Cr(III) was calculated as the difference between the total concentration of chromium (after oxidation of Cr(III) to Cr(VI) with potassium permanganate) and the initial Cr(VI) content.Graphical abstract Schematic presentation of a method for determination of chromium species by energy dispersive X-ray fluorescence spectrometry after preconcentration on molybdenum disulfide supported on reduced graphene oxide.

Graphene oxide chemically modified with 5-amino-1,10-phenanthroline as sorbent for separation and preconcentration of trace amount of lead(II).

Graphene oxide (GO) was chemically functionalized with 5-amino-1,10-phenanthroline. The resulting conjugate (phen-GO) was characterized by scanning electron microscopy and X-ray photoelectron spectroscopy. The experiments show that phen-GO has a high affinity for extraction of Pb(II) ions. Isotherms and kinetics fit the Langmuir model and pseudo-second-order equations. By using phen-GO as a sorbent, Pb(II) ions can be quantitatively adsorbed at pH 6.0. The adsorption capacity is 548 mg g-1. Following desorption with 2 mol L-1 HNO3, Pb(II) was quantified by inductively coupled plasma optical emission spectrometry. The effects of pH value, eluent type, sorption time, sample volume, and matrix ions were optimized. The accuracy of the method was validated by analysis of the reference materials DOLT-3 (dogfish liver) and SRM 1640a (natural water). Under optimal conditions, the calibration plots cover the 0.25 to 500 ng mL-1 Pb(II) concentration range. The method was successfully applied to the analysis of spiked water and biological samples. Other figures of merit include a preconcentration factor of 250, a detection limit of 46 ng L-1, and a relative standard deviation of <5%. Graphical abstract Schematic presentation of the dispersive solid-phase extraction of lead(II) ions using graphene oxide modified with 5-amino-1,10-phenanthroline, followed by their determination by inductively coupled plasma optical emission spectrometry (ICP OES).