Direct and simultaneous determination of metal impurities in catalysts based on platinum group elements

• Authors: Ashraf Abusenaina , Viera Vojteková , Karol Flórián , Zuzana Poperníková , Vladislava Mičková , Miroslava Hámborská , Silvia Ružičková
• Languages of publication: EN

Abstracts

EN

Production of new catalysts requires effective analytical quality control. The study of trace element composition of heterogeneous catalysts, based on C+PdO, using atomic emission spectrometry (AES) was carried out. A new method for the direct solid-state analysis by means of AES with direct current arc discharge was developed. On the basis of the qualitative analysis of elements, Al, Fe, Ni, Si and Ti have been identified, and for these elements, the quantitative method of determination has been developed. Optimization of excitation parameters and validation of the analytical method are presented. Calibration samples of the following composition were prepared: graphite powder (as a matrix), 3% of PdO and increasing contents of determined element oxides (spectrally pure). Calibrations were calculated by means of the least squares method. Working range for element impurities was from 1% to 0.0003%, and the limits of quantification - LOQ, (10-σ criterion) varied in the range from 0.002% (Ti) to 0.0038% (Si). For the control of active component, palladium was calibrated (working range - 0.01%–10.00%; LOQ −0.027%). The developed method can be used, also, for the elemental determinations of the other carbon based catalysts with the different active components (of platinum group elements).

Keywords

EN

Palladium catalysts; Trace element composition; Solid-state analysis; DC arc spectrometry

• Publisher: De Gruyter Open
• Journal: Open Chemistry
• Year: 2014
• Volume: 12
• Issue: 6
• Pages: 678-686

Dates

published

1 - 6 - 2014

online

13 - 3 - 2014

Contributors

author

Ashraf Abusenaina

• Pavol Jozef Šafárik University in Košice

author

Viera Vojteková

• Pavol Jozef Šafárik University in Košice

author

Karol Flórián

• Technical University of Košice

author

Zuzana Poperníková

• Pavol Jozef Šafárik University in Košice

author

Vladislava Mičková

• Technical University of Košice

author

Miroslava Hámborská

• Technical University of Košice

author

Silvia Ružičková

• Technical University of Košice

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Identifiers

DOI

10.2478/s11532-014-0519-1