Quantitative surface chemical analysis of stainless steel 1.4301 using Surface Science Instruments XPS spectrometers: report on an interlaboratory comparison

Results of an interlaboratory comparison of XPS data obtained with stainless steel are presented. Only one photoelectron spectrometer model was used. The stainless‐steel sample surfaces were analysed in different states by XPS: ‘as received’, after sputtering to I(C 1s)/I(Fe 2p3/2) ∼0.025 and after...

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Bibliographic Details
Published in:Surface and interface analysis 2002-05, Vol.33 (5), p.426-432
Main Authors: Gross, Th, Unger, W. E. S., Patscheider, J.
Format: Article
Language:English
Subjects:
Analytical chemistry
Applied sciences
Chemistry
ESCA
Exact sciences and technology
interlaboratory comparison
Metals. Metallurgy
quantitative surface chemical analysis
Spectrometric and optical methods
stainless steel
XPS
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Summary:Results of an interlaboratory comparison of XPS data obtained with stainless steel are presented. Only one photoelectron spectrometer model was used. The stainless‐steel sample surfaces were analysed in different states by XPS: ‘as received’, after sputtering to I(C 1s)/I(Fe 2p3/2) ∼0.025 and after removing a chromium‐enriched oxide layer following a certain protocol. The Fe, Cr and Ni elemental concentrations were evaluated from the respective XPS data submitted by the participants of the interlaboratory test experiment. Total means, repeat standard deviations (sr) and reproducibility standard deviations (sR) are presented. The best reproducibility standard deviations were obtained for the XPS analysis after removal of a chromium‐enriched oxide layer and quantification of the XPS intensities without taking the contamination elements of carbon and oxygen into account. The absolute reproducibility standard deviation of the elemental concentrations in that case is as small as 1.1–1.5 at.%. This gives 2%, 6% and 16% for the relative reproducibility standard deviation of the concentrations of iron, chromium and nickel, respectively. The total means of the iron, chromium and nickel concentrations finally obtained agree within 2sR with bulk values determined by wavelength‐dispersive x‐ray fluorescence spectroscopy. Comparison to an earlier interlaboratory test experiment shows that using only one model of photoelectron spectrometer reduces the reproducibility standard deviations efficiently. Copyright © 2002 John Wiley & Sons, Ltd.
ISSN:0142-2421
1096-9918
DOI:10.1002/sia.1229