Optimization of a GFAAS method for determination of total inorganic arsenic in drinking water

The new 10 μg l⁻¹ arsenic standard in drinking water has been a spur to the search for reliable routine analytical methods with a limit of detection at the μg l⁻¹ level. These methods also need to be easy to handle due to the routine analyses that are required in drinking water monitoring. Graphite furnace atomic absorption spectrometry (GFAAS) meets these requirements, but the limit of detection is generally too high except for methods using a pre-concentration or separation step. The use of a high-intensity boosted discharge hollow-cathode lamp decreases the baseline noise level and therefore allows a lower limit of detection. The temperature program, chemical matrix modifier and thermal stabilizer additives were optimized for total inorganic arsenic determination with GFAAS, without preliminary treatment. The optimal furnace program was validated with a proprietary software. The limit of detection was 0.26 μg As l⁻¹ for a sample volume of 16 μl corresponding to 4.2 pg As. This attractive technique is rapid as 20 samples can be analysed per hour. This method was validated with arsenic reference solutions. Its applicability was verified with artificial and natural groundwaters. Recoveries from 91 to 105% with relative standard deviation <5% can be easily achieved. The effect of interfering anions and cations commonly found in groundwater was studied. Only phosphates and silicates (respectively at 4 and 20 mg l⁻¹) lead to significant interferences in the determination of total inorganic arsenic at 4 μg l⁻¹.     

Solvent-Free Green Synthesis of Azines and Their Conversion to 2,5-Disubstituted-1,3,4-thiadiazoles

A solvent-free, clean, and efficient method has been developed for the synthesis of 2,5-disubstituted-1,3,4-thiadiazoles via azines. This approach exploits the synthetic potential of clean reactions and offers many advantages such as excellent product yields, easy isolation of products, and ecofriendly benign reaction conditions. The newly synthesized compounds were analyzed by infrared, ¹H NMR, ¹³C NMR, and elemental analysis.     

The Oxalato-Titanium-Containing Tungstophosphate(V) Dimers, [Ti8(C2O4)8P2W18O76(H2O)4]18− and [Ti6(C2O4)4P4W32O124]20−

The oxalato-titanium(IV)-containing, dimeric 18-tungsto-2-phosphate [Ti₈(C₂O₄)₈P₂W₁₈O₇₆(H₂O)₄]^18? (1) and the 32-tungsto-4-phosphate [Ti₆(C₂O₄)₄P₄W₃₂O₁₂₄]^20? (2) are formed upon reaction of the oxalato-titanium complex [TiO(C₂O₄)₂]^2? with the trilacunary Keggin precursor [A-α-PW₉O₃₄]^9? and the hexalacunary Wells–Dawson precursor [H₂P₂W₁₂O₄₈]^12?, respectively. Polyanion 1 consists of two {PW₉} units encapsulating eight titanium centers and connected to each other via two Ti–O–Ti bridges, and crystallizes as a mixed potassium-sodium-lithium salt in the triclinic space group $P{\bar{1}}$ . Polyanion 2 comprises two {P₂W₁₆} units containing each two titanium atoms, and the two half-units are connected via two titanium atoms decorated by two oxalate groups each, and crystallizes as a mixed potassium-lithium salt in the rhombohedral space group $R{\bar{3}}c$ . Polyanions 1 and 2 were characterized in the solid state by single-crystal XRD, FT-IR, and TGA, whereas polyanion 2 was also investigated by ³¹P and ¹⁸³W NMR.     

Equilibrium and kinetic studies for the adsorption of benzene and toluene by graphene nanosheets: a comparison with carbon nanotubes

In this study, graphene nanosheets (GNSs) were adopted as an adsorbent to investigate their characterizations and performance for adsorbing benzene and toluene in aqueous solutions. In order to determine the best fit model for each considered system, nonlinear regressions were used. Experimental data of adsorption were corroborated by the combined Langmuir–Freundlich (Sips) models for the isotherms and pseudo‐first‐order model for the kinetics. As a result, GNSs displayed high affinity to the aromatic hydrocarbons such as benzene and toluene. The high affinity was dominated by π–π interactions to the flat surface and the sieving effect of the powerful groove regions formed by wrinkles on GNS's surfaces. Hydrophobic properties and molecular sizes of benzene and toluene affected the adsorption of GNS. In addition, the favorable adsorption of toluene possibly was due to the increase in the molecular weight, decrease in the solubility, and the increase in the boiling point. A comparative study on the benzene and toluene adsorption revealed that favorable adsorption of GNSs compared with that of carbon nanotubes was consistent with the order of physical properties such as specific surface area and pore's volume. Copyright © 2016 John Wiley & Sons, Ltd.     

Dynamic arsenic removal on a MnO2-loaded resin

Previous batch studies on a polystyrene matrix loaded with manganese dioxide, synthesized from an anionic commercial resin in chloride form, have proven the efficiency of this sorbent in As(V) and As(III) removal. This solid is now tested with column experiments to predict its behavior in a treatment process. An artificial water, with a composition in major ions similar to that of granitic water, often contaminated with arsenic, was prepared. This artificial water was used to simulate arsenic removal processes under near-natural conditions and with a stable composition. Furthermore, the hydride generation AAS analytical method was optimized to measure low arsenic concentrations (1 to 20 microg/L).     

Periodic solutions of nonlinear systems of differential-operator equations with impulse action

Numerical-analytic methods are considered for the investigation of the existence and the approximate construction of periodic solutions of nonlinear differential-operator equations, subjected to an impulse action.Translated from Ukrainskii Matematicheskii Zhurnal, Vol. 43, No. 9, pp. 1260–1264, September, 1991.     

Optimization of NMR receiver bandwidth by inductive coupling.

We show, by theory and experiment, that inductive coupling can be used in overcoupled mode to widen the bandwidth of a high-Q NMR coil with only a negligible degradation of signal-to-noise ratio over the bandwidth of interest. The receiver bandwidth depends on the coupling coefficient between the NMR coil and the coupling coil rather than on the quality factor of the NMR coil alone. The overall bandwidth can be optimized by a judicious choice of the coupling coefficient. Moreover, this method permits wireless reception without the need for retuning and rematching despite changes of NMR coils or samples. This technique has been incorporated in a 0.1-T imager for clinical routine. It achieves a typical bandwidth five times greater than that using a classic 50-omega matching method.     

Polyaniline-coated cerium oxide nanoparticles as an efficient adsorbent for preconcentration of ultra-trace levels of cadmium (ІІ) followed by electrothermal atomic absorption spectrometry

For the first time, polyaniline-coated cerium oxide nanoparticles were synthesized in alkaline media and applied for preconcentration of ultra-trace levels of cadmium (??) in different real samples followed by electrothermal atomic absorption spectrometry. Cerium oxide nanoparticles were synthesized by a microwave method and modified by polyaniline to produce polyaniline-coated cerium oxide nanoparticles. Fourier-transform infrared spectroscopy and scanning electron microscopy were used to characterize the synthesized adsorbent. To optimize the critical experimental conditions; surface response methodology—Box–Behnken experimental design was used. On the basis of the results, pH 8.4, 10?mg of polyaniline-coated cerium oxide nanoparticles, 14.4?min extraction time, and 4.3?min desorption time were selected as the optimum conditions. Under the optimum conditions the calibration curve of cadmium (??) was linear in the range of 0.02–0.4?ng?mL^?1 with a correlation coefficient of 0.9976. The relative standard deviation based on seven replicate analysis of 0.1?ng?mL^?1 cadmium (??) was 4.2% and limit of detection was 0.005?ng?mL^?1 cadmium (??). The analysis of certified reference material shows very good agreement with the certified value. Finally, the proposed method was applied for the determination of ultra-trace levels of cadmium (??) in different water, rice, and tea samples.