Abstract
A method of determination of palladium is developed which combines precipitation of palladium with dimethylglyoxime, recovery of weighed form of metallic palladium, and subsequent determination of coprecipitated impurities in an isolated precipitate by atomic emission spectrometry with inductively coupled plasma and arc sources of excitation with the aim of introducing a correction into the results of gravimetric analysis. The evaluation of the error of palladium determination by the proposed scheme characterized as the total error of two independent stages of analysis (gravimetry and atomic emission spectrometry), which have different metrological characteristics, is performed. The total error of analysis in determination of the threshold concentrations of impurities in the separated palladium precipitate does not exceed the error characteristic of gravimetric analysis (RSD ≈ 0.2–0.5%). The given scheme makes it possible to substantially reduce the labor intensity and time of analysis compared to the classical scheme of gravimetric analysis.
This is a preview of subscription content, access via your institution.
References
Shneider, B.V., Malyutina, T.M., Alekseeva, T. Yu., Karpov, Yu.A., and Bukhryakova, S.K., Determination of macro concentrations of platinum by combined application of gravimetry and inductively coupled plasmaatomic emission spectrometry, Zavod. Lab., Diagn. Mater., 2009, vol. 75, no. 10, pp. 9–13.
Ginzburg, S.I., Ezerskaya, N.A., Prokof’eva, I.V., Fedorenko, N.V., Shlenskaya, V.I., and Bel’skii, N.K., Analiticheskaya khimiya platinovykh metallov (Analytical Chemistry of Platinum Metals), Moscow: Nauka, 1972.
Beamish, F.V., Analytical Chemistry of the Noble Metals, Pergamon Press, 1966.
Zhitenko, L.P., Obrezumov, V.P., Bukhryakova, S.K., Gorbatova, L.D., Il’yusha, T.G., Zemlyanko, T.P., and Khabeev, I.A., The current state and problems of determination of high concentrations of platinum metals in alloys and products, Zavod. Lab., Diagn. Mater., 2008, vol. 74, no. 8, pp. 4–14.
GOST (State Standard) 12564.1-83: Gold-Palladium-Platinum Alloys. Method of Determination of Gold, Palladium, and Platinum, 1983.
ISO 11490:1995(E). Determination of palladium in palladium jewellery alloys. Gravimetric determination with dimethylglyoxime. ISOTC 174. Moscow: Yuvelirnoe delo. 1995. 8 s.
GOST R (State Standard) 52244-2004. (GOSTR 522442004) Affined Palladium. Technical Specifications 2004.
GOST (State Standard) 12225-80: Palladium. Methods of Analysis, 1980.
Author information
Authors and Affiliations
Corresponding author
Additional information
Original Russian Text © T.M. Malyutina, B.V. Shneider, T.Yu. Alekseeva, Yu.A. Karpov, 2012, published in Zavodskaya Laboratoriya. Diagnostika Materialov, 2012, Vol. 78, No. 4, pp. 4–9.
Rights and permissions
About this article
Cite this article
Malyutina, T.M., Shneider, B.V., Alekseeva, T.Y. et al. Determination of high concentrations of palladium by combined use of gravimetric and spectral analysis. Inorg Mater 49, 1277–1282 (2013). https://doi.org/10.1134/S0020168513140070
Received:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168513140070
Keywords
- palladium
- gravimetric analysis
- dimethylglyoxime
- inductively coupled plasma atomic emission spectrometry
- arc atomic emission spectrometry