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Surface and subsurface examination of graphite tubes after electrodeposition of noble metals for electrothermal atomic absorption spectrometry

Bulska, Ewa and Thybusch, Brunhilde and Ortner, Hugo M. :
Surface and subsurface examination of graphite tubes after electrodeposition of noble metals for electrothermal atomic absorption spectrometry.
[Online-Edition: http://www.sciencedirect.com/science/article/B6THN-42XB6GV-4...]
In: Spectrochimica Acta Part B: Atomic Spectroscopy, 56 (4) pp. 363-373.
[Article] , (2001)

Official URL: http://www.sciencedirect.com/science/article/B6THN-42XB6GV-4...

Abstract

The modification phenomena of noble metals (Pd, Ir, Rh) electrodeposited onto the inner surface of pyrolytic graphite (PG) coated furnaces were investigated mainly by electron microprobe analysis with energy dispersive X-ray emission detection. The conditions of electrodeposition were optimized in order to achieve the best analytical performance of atomic absorption measurements. Investigations concerning the distribution of noble metals on the tube surface and in-depth were performed at different stages of the tube history. It was found that the noble metals used for the modification do not form a compact layer on the surface but penetrate into the pyrolytic graphite structure already at the deposition step. When two metals were deposited together, both penetrated into the graphite structure. The degree of penetration of the pyrolytic graphite at high temperature differs for various metals. It was also demonstrated that electrodeposited noble metals remain in sub-surface domains of the graphite for hundreds of atomization cycles, which means that they can be used as permanent modifiers.

Item Type: Article
Erschienen: 2001
Creators: Bulska, Ewa and Thybusch, Brunhilde and Ortner, Hugo M.
Title: Surface and subsurface examination of graphite tubes after electrodeposition of noble metals for electrothermal atomic absorption spectrometry
Language: English
Abstract:

The modification phenomena of noble metals (Pd, Ir, Rh) electrodeposited onto the inner surface of pyrolytic graphite (PG) coated furnaces were investigated mainly by electron microprobe analysis with energy dispersive X-ray emission detection. The conditions of electrodeposition were optimized in order to achieve the best analytical performance of atomic absorption measurements. Investigations concerning the distribution of noble metals on the tube surface and in-depth were performed at different stages of the tube history. It was found that the noble metals used for the modification do not form a compact layer on the surface but penetrate into the pyrolytic graphite structure already at the deposition step. When two metals were deposited together, both penetrated into the graphite structure. The degree of penetration of the pyrolytic graphite at high temperature differs for various metals. It was also demonstrated that electrodeposited noble metals remain in sub-surface domains of the graphite for hundreds of atomization cycles, which means that they can be used as permanent modifiers.

Journal or Publication Title: Spectrochimica Acta Part B: Atomic Spectroscopy
Volume: 56
Number: 4
Publisher: Elsevier
Uncontrolled Keywords: Noble metals modifier, Intercalation compounds, GF AAS, Electron probe microanalysis
Divisions: 11 Department of Materials and Earth Sciences > Material Science > Material Analytics
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences
Date Deposited: 03 Feb 2010 13:43
Official URL: http://www.sciencedirect.com/science/article/B6THN-42XB6GV-4...
Funders: This research was carried out in the framework of the project KBN 7 T09 A 053 from Committee for Scientific Research, Poland., E. Bulska thanks the DAAD of Germany for the grant of the research fellowship allowing the EPMA investigation in Darmstadt.
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