Spark Ablation Inductively Coupled Plasma Mass Spectrometry Applied to the Semi-Quantitative Panoramic Analysis of Ferroalloys

Abstract

The coupling of inductively coupled plasma mass spectrometry (ICP-MS) with spark ablation (SA) was applied for the semi-quantitative determination of impurities in different types of ferroalloys. The sparking operating conditions were optimized, and a restrictive path including a cyclone and a spray chamber was used to decrease the quantity of sparked material reaching the plasma, to prevent torch injector and sampling cone blockage. Samples were mixed in a 1:2 sample-to-graphite ratio and pressed into pellets for direct solid sampling by the spark. The advantage of the technique includes the benefit of easily determining some refractory elements that are very difficult to dissolve. The method was tested on three different types of ferroalloys: Fe-Ti, Fe-Nb, and Fe-V. A single standard ferroalloy sample was used as an external calibration sample to create a complete response curve for each type of ferroalloy base. Industrial ferroalloys, chemically characterized by using different analytical methods, were applied as calibration samples. The use of a calibration sample closely matching the ferroalloy material to be analyzed was found to be essential if accurate analyses were to be obtained. Certified Reference Materials of the three ferroalloys types tested—BAS (Bureau of Analyzed Samples) 579-1 (Fe-Nb alloy); BAM (Bundesanstalt für Materialprüfung) 589-1 (Fe-Ti alloy); and BAS 577-1 (Fe-V alloy)—were analyzed to evaluate the accuracy attainable in this panoramic mode. Most of the results, ranging from 0.05% to 5% m/m, were observed to be accurate to within 6–18.6% of the certified value, and the precision was better than 17.8% relative standard deviation. Determination limits based on 10 times the standard deviation of six replicates of a blank graphite pellet were on the μg g−1 level.

Effect of Magnesium Deficiency on Various Mineral Concentrations in Rat Liver

“…It is suitable for multielement analysis because of the simplicity of the spectra, the excellent detection limits, and the large linear dynamic range. The semiquantitative analysis using ICP-MS simultaneously provides approximate concentrations of many trace elements in one sample; this method is not necessary to specify the individual elements to be determined because ICP-MS can measure the entire mass spectrum, and then a software automatically corrects for isotopic interferences and interfering molecular species, producing a comprehensive report which lists each element present in the sample along with its concentration [9].…”

Direct Determination of Zinc in Steel Samples by Electrothermal Vaporization Inductively Coupled Plasma Atomic Emission Spectrometry

“…However, the relative errors increased to 6-12%. 8 When powdered samples are analyzed by the ETV method, alternative difficulties still remain, such as introducing preweighed small amounts of finely powdered samples into the ETV device, removing the residues from it easily, and finding an accurate calibration method. In order to overcome these difficulties, as a sample introduction technique, slurry sampling ETV and/or slurry sampling nebulization are used for the analysis of finely powdered samples.…”

Plasma parameter and film casting optimization for the determination of particulate matter in a sol–gel matrix by radiofrequency glow discharge optical emission spectrometry (rf-GD-OES)

“…[5][6][7][8] In addition, excess levels of some transition metals have been shown to act as catalysts for enzyme activity. 3,4 Analysis of solid particulate material typically involves a dissolution process followed by elemental determination by solution-based methods (e.g., atmospheric pressure flames and plasmas) or binding the powdered form with a chemical binder into a pellet and subsequent analysis by scanning electron microscopy with energy dispersive X-ray (SEM/EDX), [9][10][11][12][13] laser ablation (LA) [14][15][16][17][18] and spark ablation (SA) 19,20 inductively coupled plasma spectroscopies, [21][22][23][24] direct current glow discharge (dc-GD) spectrometries, [25][26][27] or X-ray fluorescence (XRF). [28][29][30][31][32][33][34] However, SEM/EDX, SA, and dc-GD methods require the sample to be electrically conductive for proper operation.…”