High-temperature XRD study of thermally induced structural and chemical changes in iron oxide nanoparticles embedded in porous carbons

Magnetic carbon-based nanomaterials have promising applications in many fields owing to their biocompatibility and thermal/mechanical stability. This study describes a high-temperature X-ray diffraction (XRD) study of the chemical and structural transformations suffered by superparamagnetic iron oxide nanoparticles embedded in porous carbons. The nanoparticles were prepared from the decomposition of iron pentacarbonyl over porous carbons, resulting in nanometer-sized iron oxides homogeneously dispersed into the carbon matrix. The thermally induced changes in these materials were followed by in situ high-temperature XRD, using synchrotron radiation. The growing of the nanoparticles and of the carbon crystallites were first observed, followed by the reduction of the iron oxides to form α-Fe (at temperatures as low as 400 °C in some cases) and γ-Fe(C). The temperatures at which these chemical reactions occurred were dependent on the total time spent on heating and on the nature of the iron oxides formed in the as prepared materials. A noticeably large thermal expansion coefficient was also observed for the iron oxide nanocrystals. The formation of austenitic iron, stabilized by the presence of carbon, was found to be only partially reversible upon cooling.     

Pesticide residues in herbs and their transfer for infusions

In this work, a cost-effective gas chromatography-mass spectrometry method was validated for the analysis of twenty-five pesticide residues in herbs and infusions using a quick, easy, cheap, effective, rugged, and safe procedure or a dispersive liquid-liquid microextraction method, respectively. Figures of merit of the method showed good accordance with current guidelines. From the 58 herb samples studied (pertaining to 20 different species), 80% presented at least one detectable pesticide, with 62% of them above the maximum residual level. Results showed that pesticide residues from naturally contaminated herbs were not transferred at a significant rate to the herbal infusions. When a control assay was conducted by spiking a blank herb sample with a large amount of each pesticide (7 mg/L) 15 analytes were detected below the limit of quantification in the infusion.