Secondary ion mass spectrometric investigation of Au-based composites.

The electrodeposition of thick gold layers plays an important role both in traditional and high-tech productions, such as jewelry and microelectronics, respectively. In this work a secondary ion mass spectrometric study will be presented on Au co-deposits with (sub-)micrometric ceramic powders, in order to harden gold. Mass spectra are used to identify the components deposited, providing evidence of the additives and/or eventual contaminants introduced during electrolysis. Furthermore, analysis of ion depth profiles and the intensity distribution of ionic species along the film were studied.

Secondary ion mass spectrometry in the characterisation of boron-based ceramics.

A secondary ion mass spectrometry (SIMS) study of Zr- and Ti-based borides is reported: ZrB2 ceramic samples (with and without nickel addition) and a TiB2-Ni-B4C/Cu joint were investigated. For Zr-based samples, SIMS measurements show evidence for induced effects by the presence of nickel with regard to oxygen and hydrogen absorption and zirconia formation. In the case of the TiB2-Ni-B4C/Cu joint, the ceramic-metal interface region was analysed and the extent of Cu diffusion into the ceramic material was established. SIMS results were in agreement with previously obtained SEM-EDS data.

Surface chemistry of RuO(2)/IrO(2)/TiO(2) mixed-oxide electrodes: secondary ion mass spectrometric study of the changes induced by electrochemical treatment.

The IrO(2)/RuO(2)/TiO(2) ternary system is well known for its electrocatalytic activity towards oxygen- and chlorine-evolution reactions. Electrochemical processing induces noticeable chemical and morphological modifications on these electrodes, depending on the noble metal oxide content. In this work, cathodic/anodic polarization and the oxygen-evolution reaction were studied in order to evaluate the electrocatalytic activity at various noble metal oxide percentages. The best performing electrode (30 mol% noble metal oxides) was analyzed before and after electrochemical tests by means of secondary ion mass spectrometry (SIMS) in order to determine the chemical composition modification which occurred on the surface and in deeper regions of the mixed-oxide film.

Secondary ion mass spectrometric investigation on ruthenium oxide systems: a comparison between poly- and nanocrystalline deposits

The influence of different RuO(2) crystallite sizes was investigated by secondary ion mass spectrometry (SIMS) on the oxide deposited on various support materials (Ni, Ti, Al(2)O(3), oxidized Si(100)). In order to examine the effect of an oxidic environment on the film structure, RuO(2) 20%-TiO(2) 80% at. mixed oxide was deposited on Ti. The polycrystalline coatings were prepared by heating the Ru (and Ti)-containing solution dropped on the supports.1 RuO(2) nanocrystalline coatings were grown by chemical vapor deposition (CVD) from Ru(COD)(eta(3)-allyl)(2).2 The identification of mixed oxide clusters showed the higher reactivity of Ni and Al(2)O(3) over the other substrates. Diffusion and migration characteristics were observed to be influenced by the nature of the support. The results are complementary to those of a previous SIMS investigation.3 Copyright 2000 John Wiley & Sons, Ltd.

Ni-Zr alloys: relationship between surface characteristics and electrocatalytic behavior

A relationship between electrocatalytic activity for the hydrogen evolution reaction and the surface composition of the electrode was established for Ni-Zr crystalline and amorphous alloys by means of secondary ion mass spectrometry (SIMS). Electrocatalytic activity was tested by means of cathodic polarization in 1 M KOH at 25 degrees C and the resulting exchange current density has been taken as a measure of catalytic efficiency. Surface activation treatment involved chemical etching in HF solutions; the consequent morphological and compositional surface changes were studied by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical behavior of the pure elements (Ni and Zr) was also considered for comparison. All samples submitted to chemical etching in HF solutions showed an increase in electrocatalytic activity, particularly the alloy with the highest Ni content. The beneficial effect of chemical etching is due to dissolution of the zirconium oxide layer and to the formation of nanocrystalline Ni on the surfaces.

Rapid, sensitive and specific determination of oxytetracycline residues in bovine milk and meat by CAD MIKEs analysis at the 1 ppb level.

A rapid and sensitive method for the selective detection and quantification of oxytetracycline residues at the ppb level in crude extracts of bovine milk and meat is described. The technique employed is a tandem mass spectrometric method: CAD MIKE spectrometry (collisionally activated decomposition mass-analysed ion kinetic energy spectrometry). Quantification is performed by single ion monitoring of CAD species of oxytetracycline and of its internal standard.

Hydroxyl negative chemical ionization mass spectrometry linked with collisionally activated decomposition. A modern analytical tool in inborn errors of metabolism.

Two kinds of inborn errors of metabolism, dicarboxylic aciduria and hyperoxaluria, have been studied by means of hydroxyl negative ion chemical ionization [NICI(OH-)], linked with collisionally activated decomposition experiments on the [M-H]- species of the pathognomonic organic acids. This method has led to non-controversial qualitative determinations of C4-C10 dicarboxylic acids and oxalic, glyceric and glyoxylic acids. NICI(OH-) linked with collisionally activated decomposition mass analysed ion kinetic energy spectrometry (CAD MIKES) is proposed herein for diagnostic purposes, as a valid mass spectrometric alternative to standard gas chromatographic/mass spectrometric analysis. The procedure is characterized by simplified sample treatment and by fast execution.

CAD MIKES: a new method for a rapid and unequivocal structural identification of organic acids in biological fluids. A first application to a case of methylmalonic aciduria.

A novel application of Collisionally Activated Decomposition Mass analysed Ion Kinetic Energy (CAD MIKE) spectrometry to separation and positive structural identification of urinary methylmalonic acid (MMA) (the pathognomonic compound for the diagnosis of methylmalonic acidurias) is presented. CAD MIKES scans of EI ionic species at m/z 119 ([M + H]+) and m/z 101 ([M-OH]+) have been obtained from a pure standard of MMA and from crude urinary acid fractions. With reference to the procedures employed so far, the advantages of the proposed method lie in fast and simplified sample pretreatment and in a quick non-controversial response to a clinical suspicion of serious, life-threatening inherited metabolic diseases.