A technique for analysis of secondary tungsten-containing raw materials (tungsten-containing sludge) using inductively coupled plasma atomic emission spectrometry in combination with microwave autoclave sample preparation has been developed. The composition of the acid mixture and algorithm of microwave heating of the autoclave are chosen to provide a complete quantitative transfer of the sample into a convenient analytical form for subsequent ICP-AES determination of the main components (heating of the sample to 220°C in the acid mixture of NH4F, HNO3, and HCl provides a quantitative transfer of its components to be determined into the solution). Analytical lines free from spectral interference were selected to determine Ti, Cr, Fe, Co, Ni, and W. We used real industrial samples of secondary raw materials obtained in product manufacture from VK-type hard alloys [solid solution of tungsten carbide grains (WC phase) in cobalt (Co phase)] in the form of tungsten-containing powders, grinding sludge of solid sintered alloys, dust waste, defective mixtures, waste of ventilation systems, and carbide powders. Correctness of the determination of elements was proved in analysis of ferrotungsten standard samples upon determination of the matrix component (tungsten) and by the methods of additives and sample weight variation upon determination of the alloying elements and impurities. The method of internal standard (with Sc as the element of comparison) was used to improve the precision and accuracy of the tungsten determination. The relative standard deviation was thus reduced from 0.03 to 0.004. The developed precise rapid technique was tested in analysis of industrial samples of secondary tungsten-containing sludge of hard alloys. The technique is recommended to control the composition of the secondary tungsten-containing sludge of hard alloys in a wide range of concentrations.
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The studies were performed on the equipment of the Center for the Collective Use of Scientific Equipment Composition, Structure, and Properties of Structural and Functional Materials of the National Research Center Kurchatov Institute—CRISM Prometey with financial support from the state represented by the Ministry of Education and Science within the framework of agreement no. 14.595.21.0004, unique identifier RFMEF159517X0004.
The authors declare that they have no conflicts of interest.
Translated by Sh. Galyaltdinov
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Vyacheslavov, A.V., Tsepkova, V.V., Titova, A.D. et al. Development of a Technique for Analysis of Tungsten-Containing Sludge Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). Inorg Mater 56, 1369–1373 (2020). https://doi.org/10.1134/S0020168520140150
- secondary tungsten-containing raw materials
- secondary tungsten-containing sludge of hard alloys
- microwave sample preparation