The low toxicity and environmentally compatible ionic liquids (ILs) are alternatives to the toxic and harmful cyanide-based baths used in industrial silver electrodeposition. Here, we report the successful galvanostatic electrodeposition of silver films using the air and water stable ILs 1-ethyl-3-methylimidazolium trifluoromethylsulfonate ([EMIM]TfO) and 1-H-3-methylimidazolium hydrogen sulphate ([HMIM(+)][HSO4(-)]) as solvents and AgTfO as the source of silver. The electrochemical deposition parameters were thoughtfully studied by cyclic voltammetry before deposition. The electrodeposits were characterized by scanning electron microscopy coupled with X-ray energy dispersive spectroscopy and X-ray diffraction. Molecular dynamics (MD) simulations were used to investigate the structural dynamic and energetic properties of AgTfO in both ILs. Cyclic voltammetry experiments revealed that the reduction of silver is a diffusion-controlled process. The morphology of the silver coatings obtained in [EMIM]TfO is independent of the applied current density, resulting in nodular electrodeposits grouped as crystalline clusters. However, the current density significantly influences the morphology of silver electrodeposits obtained in [HMIM(+)][HSO4(-)], thus evolving from dendrites at 15 mA cm(-2) to the coexistence of dendrites and columnar shapes at 30 mA cm(-2). These differences are probably due to the greater interaction of Ag(+) with [HSO4(-)] than with TfO(-), as indicated by the MD simulations. The morphology of Ag deposits is independent of the electrodeposition temperature for both ILs, but higher values of temperature promoted increased cluster sizes. Pure face-centred cubic polycrystalline Ag was deposited on the films with crystallite sizes on the nanometre scale. The morphological dependence of Ag electrodeposits obtained in the [HMIM(+)][HSO4(-)] IL on the current density applied opens up the opportunity to produce different and predetermined Ag deposits.
An analytical method for multi-elementary determination in powder refreshment, based on sample digestion using dilute mineral acids and detection by inductively plasma coupled optical emission spectrometry (ICP OES) is proposed. Chemometric tools, such as fractional factorial design and principal component analysis (PCA) and hierarchical cluster analysis (HCA) were applied to optimize the sample preparation conditions in closed block digester, and Doehlert design for spectrometer operation. Addition and recovery tests and analyses of certified reference material were performed to evaluate the precision and accuracy, and the results confirm the reliability of the proposed method. Limits of quantification (LOQ) between 0.02 and 36 μg g−1 were obtained. The analytical method was applied for determination of 24 inorganic constituents in 20 powder refreshment samples. Calcium, K, Mg, Na, P, S and Ti presented the highest concentrations. The analytical method was adequate for the determinations of inorganic constituents in powder refreshment samples by ICP OES.
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