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Determination of the Stoichiometric Composition of High-Temperature Superconductors by ICP-OES for Production Control
Authors:Dirk Geilenberg  Michael Gerards  José A. C. Broekaert
Affiliation:Analytische Chemie, FB Chemie, Universit?t Dortmund, D-44221 Dortmund, Germany, DE
Merck KGaA, Werk Gernsheim, Mainzer Stra?e 41, D-64579 Gernsheim, Germany, DE
Universit?t Leipzig, Institut für Analytische Chemie, Linnéstra?e 3, D-04103 Leipzig, Germany, DE
Abstract: A procedure to dissolve and analyse different types of high-temperature superconducting materials in order to determine their stoichiometric com- position is described. As sample materials Y-Ba-Cu-O and (Pb)Bi-Sr-Ca-Cu-O were analysed. They were dissolved with hydrochloric acid and analysed by simultaneous ICP-OES, which fits best for this analytical task because of its multielement capacity, its high precision of determination and accuracy. Each of the relevant metals (Pb, Bi, Sr, Ca, Y, Ba, Cu) could be determined successfully. The precision of the determination was found to be better than 2% relative standard deviation and usually even below 1%. The sample preparation and determination procedure described allows a high sample throughput, which is essential for production control. Also precursors of the superconducting materials (e.g. nitrate solutions) could be analysed by the procedure described.
Keywords::   High-temperature superconducting materials   simultaneous ICP-OES   stoichiometry   main components.
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