Analysis of iron ores by ICP-AES

2021 ◽  
Vol 87 (6) ◽  
pp. 20-24
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder ◽  
N. Romanov ◽  
S. V. Kachin

A method for the analysis of iron ore raw materials (IORM) using inductively coupled plasma atomic- emission spectrometry (ICP-AES) and Concentration Ratio Calibration (CRC) has been developed. However, the general eq. for calibration by concentration ratios used in analysis of metals and alloys was modified with allowance for the IORM characteristics: all the elements, except sulfur, were represented as oxides, iron was represented as FeO and Fe2O3, and the total of 100% included ignition losses (LOI). A variant of solving the equation is proposed, which allowed us to relate the relative concentrations of the components (the ratios of the mass fraction of the determined components to the mass fraction of iron oxide) to the ratio of the line intensities of the certain element and iron line measured on a spectrometer. The equation takes into account the content of FeO and LOI, which are determined by standard methods of analysis. A method for acid decomposition of the samples in autoclaves heated in a HotBlock 200 system is proposed: a sample weight of 0.25 g was decomposed in closed vessels at a temperature of 150 – 180°C in the mixture of HCl, HF and HNO3. The following components were determined in concentrates and pellets: Fe2O3, Fetot, Al2O3, CaO, Cr2O3, K2O, MgO, MnO, Na2O, P2O5, SiO2, TiO2, Co, Cu, Mo, Ni, Pb, S, V, Zn. The correctness of the developed method is confirmed by the analysis of SS of iron ore and iron concentrates, as well as by comparison with the results obtained by standardized methods. The proposed technique provides iron determination in iron ore raw materials with an accuracy no worse than that specified in GOST 23581, all other components are determined in a wider range of contents and with a higher accuracy.

1995 ◽  
Vol 49 (10) ◽  
pp. 1478-1484 ◽  
Author(s):  
Luc Soudier ◽  
Jean-Michel Mermet

A procedure is described to conduct qualitative analysis in inductively coupled plasma atomic emission spectrometry even in the presence of spectral interferences. This procedure is based on the use of both line correlation and normalized relative line intensities of given elements. When spectral interferences due to a major element are observed for an analyte, use of multiple linear regression of the normalized relative line intensities of both the analyte and the major element provides information about the certainty of the presence of the analyte and the relative concentration between the major element and the analyte. Direct peaking and automatic background correction are required for this procedure. In this instance, no information is necessary about the shape of the line profile. This procedure has been tested with an echelle grating-based dispersive system equipped with a custom segmented-array charge-coupled device detector.


Author(s):  
V. A. Makarov ◽  
T. K. Savosteenko

A method for measuring the mass fraction of phosphorus in steels by atomic emission spectrometry with the inductively coupled plasma (AES-ICP) has been developed. Possibilities of atomic emission spectrometers of iCAP series for determination of phosphorus in steels allowing to reduce considerably duration of the analysis and to increase its profitability in comparison with chemical methods of the analysis are investigated. A method of decomposition of steel for the complete transfer of phosphorus into solution is proposed. The possibility of software spectrometers “iTeva” in the analysis by the method of relative concentrations. Calibration of the spectrometer was carried out on aqueous solutions with a known concentration of phosphorus using the method of relative concentrations. For the preparation of calibration solutions, chemically pure salt was used. The analytical line free from spectral overlays is selected. A good correlation of the calibration graph is obtained. The correctness of the determination is confirmed by the analysis of standard samples and comparison with the results of the determination in accordance with the chemical method. The developed technique is used in determining the mass fraction of phosphorus in steels. Validation of the methodology was carried out. iCAP spectrometers can be used to determine the mass fraction of phosphorus in steels.


2017 ◽  
Vol 2017 ◽  
pp. 1-8 ◽  
Author(s):  
Fuad A. Ababneh

54 samples belonging to 23 herbal species (15 individuals and 8 mixtures) were analyzed for their contents of heavy metals in the raw materials and in their water infusions. Trace and toxic elements in these samples were determined by using inductively coupled plasma-atomic emission spectrometry (ICP-OES) following acid digestion. The order of decreasing mean metal concentrations in raw materials (mg/kg) was found to be as follows: Fe (440) > Mn (162) > Zn (45.8) > Cu (12) > Pb (10.4) > Ni (5.4) > Cr (2.9) > Co (0.91) > Cd (0.5). It was found that 21% of the analyzed samples contain both Cd and Pb above their permissible limits. However, the infusions produced from these plants were found to contain fewer amounts of metals than the raw materials. Studied metals had the following mass transfer percentages to the infusion solutions (Fe: 3.5%, Cd: 14%, Cr: 15%, Pb: 20%, Co: 29%, Ni: 31%, Zn: 36%, Cu: 48%, and Mn: 53%). The estimated daily intake calculated for the toxic elements Pb and Cd through the consumption of herbal infusions was far below the tolerable daily intake set by the World Health Organization (WHO).


1987 ◽  
Vol 41 (3) ◽  
pp. 391-395 ◽  
Author(s):  
R. S. Houk ◽  
B. R. Lafreniere ◽  
H. B. Lim ◽  
V. A. Fassel

A supplementary electrical discharge is generated by extraction of the axial channel of an Ar inductively coupled plasma (ICP) into a small vacuum chamber. The spectral background levels and background noise emitted by this discharge are similar to those from the ICP alone. The discharge enhances the intensities of ion lines by factors of up to 13 relative to intensities observed from the ICP alone. Neutral atom lines from elements with high ionization energies (≤9 eV) are also enhanced but by less than ion lines; neutral atom lines from easily ionized elements are suppressed by the discharge. Metal oxides in the ICP can be seen to dissociate into atomic species as they enter the discharge. These effects are attributed to more efficient atomization, excitation, and ionization in the discharge and to the tendency of analyte species to be constricted or concentrated closer to the central axis of the ICP as they flow into the discharge. Under the same operating conditions a 40-MHz plasma generates a more intense discharge and yields higher intensity enhancements than does a 27-MHz plasma.


1996 ◽  
Vol 50 (8) ◽  
pp. 959-964 ◽  
Author(s):  
Cedric Rivier ◽  
Jean-Michel Mermet

In a previously published work, a procedure was described to conduct qualitative analysis in inductively coupled plasma atomic emission spectrometry, keeping in mind the possibility of spectral interferences. This procedure is based on the use of both line correlation and normalized relative line intensities of given elements. When spectral interferences due to a single or two major elements are observed for an analyte, use of multiple linear regression of the normalized relative line intensities of both the analyte and the major element provides information about the certainty of the presence of the analyte. This procedure has been used with an echelle grating-based dispersive system equipped with a custom segmented-array charge-coupled device detector and evaluated with the use of line-rich matrices such as Fe, Cr, and Ni. Satisfactory results were obtained even when several lines of the analyte suffered from interference. The only limitation was the number of available lines for a given analyte.


2020 ◽  
Vol 86 (5) ◽  
pp. 16-21
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder ◽  
S. V. Kachin

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).


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