scholarly journals Analysis of surfacing materials from cast carbide alloys using inductively coupled plasma atomic emission spectrometry (ICP-AES)

2018 ◽  
Vol 84 (6) ◽  
pp. 5-10
Author(s):  
A. V. Vyacheslavov ◽  
V. V. Tsepkova ◽  
A. D. Titova ◽  
T. N. Ermolaeva
Keyword(s):  
Sample Preparation ◽  
Inductively Coupled Plasma ◽  
Analytical Form ◽  
Emission Spectrometry ◽  
Acid Mixture ◽  
Volatile Components ◽  
Single Element ◽  
Plasma Atomic Emission Spectrometry ◽  
Standard Samples ◽  
Weight Variation

A technique for analysis of surfacing materials (cast cobalt-based carbide alloys) using by ICP-AES in combination with microwave autoclave sample preparation is developed. Composition of the acid mixture, temperature and time parameters of the sample preparation under microwave heating in an autoclave are specified, thus ensuring complete quantitative transfer of the sample into a convenient analytical form without losses of volatile components for the subsequent ICP-AES analysis. Analytic lines of the elements free from spectral interference were chosen to determine all the rated components in the casting materials from cast carbide alloys. Study of surfacing materials was carried out using alloys Pr-B3K-PrH-U10Kh63B5, Pr-B3K-P-PrN-U20Kh57B10 and TsN-2-E-190K62X29B5C2, containing the alloying elements (% wt.): Co (up to 65); Cr (28.0 – 32.0); W (4.0 – 11.0); Si (1.0 to 3.0); C (1.0 – 2.0); Ni (0.1 – 2.0); Mn (0.3 – 0.6) and Fe (up to 2.0). The correctness of determining rated element was confirmed in analysis of standard samples using sample weight variation. The developed technique was tested on industrial prototypes of surfacing materials made of cobalt-based cast carbide alloys of tested grades. The method is rapid (11-fold reduction in the time of analysis) and reagent-saving (by 12.5 times) procedure compared to single-element methods by 11 times and reduction of the volume of applied reagents. Combination of the multielement ICP-AES method with microwave sample preparation provides an increase in the accuracy of Si, Cr, Mn, Fe, Ni, and W determination in surfacing materials of cast carbide alloys within a range of rated concentrations.

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.

scholarly journals DETERMINATION OF REM IN URANIUM ORES OF THE SHU-SARYSU URANIUM-ORE PROVINCE BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

2021 ◽  
Vol 2 (446) ◽  
pp. 29-35
Author(s):  
А. К. Тorebekov ◽  
M. S. Kalmakhanova ◽  
B. K. Massalimova
Keyword(s):  
Sample Preparation ◽  
Inductively Coupled Plasma ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Uranium Ore ◽  
Inductively Coupled

This article discusses the features of the determination of elements in uranium ores of the Shusarysu uranium-ore province by inductively coupled plasma atomic emission spectrometry in comparison with the ore standard of Ore Research & Exploration (Australia). A multi-stage method of sample preparation for measurement is considered. The existing and developed methods for determining the elemental composition of uranium ores are focused, as a rule, on the determination of specific elements using regulated analysis procedures. However, during routine analysis, we need to quickly and efficiently determine a larger list of elements available with one instrumental method. Various methods are used to obtain multielement analysis, among which mass spectrometry and inductively coupled plasma atomic emission analysis are most popular due to their high performance and low detection limits. The listed methods work with solutions, therefore, it is necessary to pay great attention to sample preparation and instrument calibration. The invention relates to a method for preparing samples for the study of materials by determining their chemical properties in a liquid state, for example, using inductively coupled plasma spectrometry. The method for preparing silicate and carbonate rock samples for spectrometric analysis includes autoclave decomposition of samples in a mixture of concentrated acids in a microwave oven at temperature and pressure and cooling the samples. Then carry out the introduction of the internal standard and bringing to the standard volume.

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