Simultaneous ICP atomic emission spectrometry for accurate stoichiometric determination: application to a YNi2B2C superconducting material system

Abstract

For characterisation of the exact stoichiometry of semiconductor or superconductor compounds, the determination of major components with high precision and accuracy is necessary. In order to assess ICP-AES for this task, sophisticated procedures for sample preparation, measurement optimisation and data correction and evaluation, such as multi-line measurements for each analyte element, optimum calibration and recalibration, and internal standardisation, have been developed for simultaneous Echelle spectrometers with CID or CCD detectors. Procedures and results are demonstrated for superconducting materials of the YNi 2 B 2 C type. For the analyte elements Y, Ni and B, as well as for the internal standard element In, three optimum spectral lines were used. Calibration and external standardisation were carried out using different mixtures of mono-elemental standard solutions. The confidence intervals for the determination of Y, Ni and B were lowered to 0.17, 0.11 and 0.13% (w/w), respectively. Thus, the stoichiometric coefficients were determined with an error smaller than 0.002, 0.002 and 0.003 for Y, Ni and B, respectively. Using the F-test, the sample homogeneity was tested and, in this way, the presence of trace amounts of secondary phases were detected.

Atomic Spectroscopy

“…These applications range from the analysis of biological samples (animal tissue, plant materials, serum) over water, eventually with on-line preconcentration, to the analysis of metals and their alloys, crystal dopant determinations, and analyses of glasses and hard materials. Nevertheless, it is interesting to mention that work is being done on some challenging applications, such as the determination of metals in flue gases in waste incineration plants (119), determination of the exact stoichiometry of superconductor materials such as YNi 2 B 2 C with In as internal standard and CCD-based ICP-AES (120), and direct determination of Ca, Cl, K, Mg, Na, and P in biodiesel with the aid of an argon-oxygen mixed-gas ICP (121).…”

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

“…A YNi 2 B 2 C superconducting material has been analysed for the analytes B, Ni and Y, as well as the internal standard In, by ICP-AES. 297 The paper described procedures for sample preparation, measurement optimisation (including multi-line measurements for each analyte, optimum calibration and recalibration) and the use of echelle spectrometers with CID and CCD detectors. Under optimal conditions, the confidence intervals were 0.17, 0.11 and 0.13% w/w for Y, Ni and B, respectively.…”

Accurate determinations of Ge atom fractions in SiGe semiconductor chips using high performance ICP-OES

“…Kucharkowski et al 12,13 utilized ICP-OES to achieve similar measurements with superconducting materials. Multiple lines (typically 3) were selected for the analyte and internal standard elements in the determination of the stoichiometry.…”

“…Stoichiometric measurements on the SiGe semiconductors in the present study were performed using the high performance ICP-OES (HP-ICP-OES) approach. HP-ICP-OES and the approach used by Kucharkowski et al 12,13 are similar in principle but differ in execution. The approach of Kucharkowski et al utilizes volumetric measurements in the preparation of the standards and samples.…”