Oxford inca 350

Mineralogical identification of suspended particles and sediments at different intervals was performed by different techniques at SGIker analytical services (UPV/EHU). X-ray Diffraction (XRD) was carried out on a PANalytical X’Pert Pro Malvern Panalytical, Almelo, Netherlands diffractometer and interpreted using High Score X’Pert software pack. In order to prevent the artificial formation of minerals (e.g., salts) during sample preparation, suspended particulate matter and sediment samples were washed with MilliQ water in several cycles (repeated centrifugation at 4,400 rpm, Eppendorf 5702 or 13,200 rpm, Eppendorf 5415D) (Eppendorf, Hamburg, Germany), liquid phase elimination, water addition and re-suspension), all performed in the metal-free ISO seven clean room. These samples were mounted on 25 mm C (graphite) stub, subjected to plasma cleaning and coated with C layer. These stubs were examined under a Scanning Electron Microscope (SEM) with field emission source JEOL JSM-7000F (JEOL, Tokyo, Japan) (10 mm working distance, 20 kV, 1 nA) coupled with Oxford INCA 350 (Oxford Instruments, Abindon, United Kingdom) energy dispersive X-ray spectroscopy (EDX) for semi-quantitative point chemical analysis.

The MnFCN thin film was characterized using scanning electron microscopy (SEM) on a Tescan Vega 3 SBH microscope (Tescan, Brno, Czech Republic) to reveal its surface morphology, using an energy-dispersive X-ray (EDX) spectrometer attached to an Oxford INCA 350 (Oxford Instruments, Abingdon, UK) to detect the elements and the surface distribution of Mn and Fe, and using X-ray diffraction (XRD) with Cu Kα radiation (λ = 0.1542 nm) on a Rigaku SmartLab 3 Powder X-ray diffractometer (Rigaku, Tokyo, Japan) to display the crystalline phases. The qualitative and quantitative analysis of the samples was characterized via X-ray photoelectron spectroscopy (XPS) using an ESCALAB 250Xi electron spectrometer (ThermoFisher Scientific, Waltham, MA, USA).

The Al and Fe-based NPs were characterized by FTIR spectroscopy (Shimadzu IR Prestige−21, FTIR-8400S spectrophotometer, Kyoto, Japan) and PXRD measurements (Empyrean X-ray diffractometer with Cu Kα1 radiation, λ = 1.5406 Å, Malvern Panalytical Ltd. Malvern, Worcestershire, UK). Samples were scanned over a 2θ range between 10° and 75° with a scan step of 0.013°. Crystallite size information was extracted from the phase fitting method based on the change in profile widths compared to a standard sample. For insight into nanoparticles morphology, thermal field-emission scanning electron microscope ((FE-SEM), model JSM-7000F, manufactured by Jeol Ltd., Tokyo, Japan) was used, while the composition of the samples was checked with an energy dispersive spectrometer (EDS, model Oxford Inca 350, manufactured by Oxford Instruments, Abingdon, UK)