Silicate analysis of carbonated rocks using ICP-AES with calibration by the concentration ratio

2020 ◽  
Vol 86 (5) ◽  
pp. 16-21
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder ◽  
S. V. Kachin
Keyword(s):  
Inductively Coupled Plasma ◽  
Concentration Ratio ◽  
Total Error ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Calibration Error ◽  
Plasma Atomic Emission Spectrometry ◽  
Standard Samples ◽  
Inductively Coupled ◽  
Carbonate Materials

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).

scholarly journals Determination of phosphorus mass fraction in steels of plasma atomic emission spectrometry

2021 ◽  
pp. 86-90
Author(s):  
V. A. Makarov ◽  
T. K. Savosteenko
Keyword(s):  
Inductively Coupled Plasma ◽  
Mass Fraction ◽  
Atomic Emission ◽  
Calibration Graph ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
Standard Samples ◽  
Inductively Coupled

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.

ANALYSIS OF GEOLOGICAL MATERIALS BY ICP-AES WITH CALIBRATION IN CONCENTRATION RATIO

2019 ◽  
Vol 85 (6) ◽  
pp. 24-29
Author(s):  
T. A. Karimova ◽  
G. L. Buchbinder
Keyword(s):  
Inductively Coupled Plasma ◽  
Concentration Ratio ◽  
Total Error ◽  
Internal Standard ◽  
Atomic Emission ◽  
Absolute Intensity ◽  
Emission Spectrometry ◽  
Calibration Error ◽  
Intermediate Precision ◽  
Geological Materials

A method of calibration in relative concentrations (concentration ratio) previously used only in analysis of non-ferrous and ferrous metals was first implemented when performing silicate analysis of geological materials using atomic emission spectrometry with inductively coupled plasma (AES-ICP). Prior to apply the Concentration Calibration Ratio to analysis of geological materials it is necessary to consider and address the following problems: some of the components are not determined by ICP-AES, matrix elements may be present in different oxidation states. Sample preparation of ores and geological materials was carried out in autoclaves heated at 180°C using HotBlock 200 system. A mixture HCl/HNO3/HF was used at the first step and then added with a 4% H3BO3 solution. The repeatability and intermediate precision of determination when using Concentration Ratio Calibration, calibration without internal standard and Calibration with In as internal standard are compared for determination of SiO2 (content 40 – 75%), Al2O3 (5 – 20%), CaO (0.25 – 15%), MgO (0.1 – 15%), Fe2O3 (0.5 – 15%), Na2O (0.5 – 10%), K2O (0.5 – 5%), P2O5 (0.01 – 0.3%), MnO (0.03 – 0.5%), and TiO2 (0.05 – 2%). The use of Concentration Ratio Calibration provides better metrological characteristics, repeatability and precision in analysis of geological materials compared to other calibration procedures due to elimination of the calibration error of balances and volumetric flasks from total error of analysis; measuring the large intensities of the base element; and better accuracy of measuring the intensity ratio compared to absolute intensity measurements.

scholarly journals Distribution and Mode of Occurrence of Co, Ni, Cu, Zn, As, Ag, Cd, Sb, Pb in the Feed Coal, Fly Ash, Slag, in the Topsoil and in the Roots of Trees and Undergrowth Downwind of Three Power Stations in Poland

Minerals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 133
Author(s):  
Henryk R. Parzentny ◽  
Leokadia Róg
Keyword(s):  
Inductively Coupled Plasma ◽  
Coal Fly Ash ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
X Ray ◽  
Inductively Coupled ◽  
Power Stations ◽  
Mode Of Occurrence ◽  
Feed Coal

It is supposed that the determination of the content and the mode of occurrence of ecotoxic elements (EE) in feed coal play the most significant role in forecasting distribution of EE in the soil and plants in the vicinity of power stations. Hence, the aim of the work was to analyze the properties of the feed coal, the combustion residues, and the topsoil which are reached by EE together with dust from power stations. The mineral and organic phases, which are the main hosts of EE, were identified by microscopy, X-ray powder diffraction, inductively coupled plasma atomic emission spectrometry, and scanning electron microscope with an energy dispersive X-ray methods. The highest content of elements was observed in the Oi and Oe subhorizons of the topsoil. Their hosts are various types of microspheres and char, emitted by power stations. In the areas of long-term industrial activity, there are also sharp-edged grains of magnetite emitted in the past by zinc, lead, and ironworks. The enrichment of the topsoil with these elements resulted in the increase in the content of EE, by between 0.2 times for Co; and 41.0 times for Cd in the roots of Scots pine, common oak and undergrowth, especially in the rhizodermis and the primary cortex and, more seldom, in the axle roller and cortex cells.

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