Comments about sample treatment in the X-ray diffraction analysis of the oxidation products of lead

Timo Laitinen, Göran Sundholm (Corresponding Author), J. Vilhunen

Research output: Contribution to journalArticleScientificpeer-review

7 Citations (Scopus)

Abstract

The influence of different sample pretreatment methods in the period between switching off the potential control and the actual X-ray scan on the results of ex situ X-ray powder diffraction analysis of thin corrosion films of Pb anodized in H2SO4 has been studied. Washing the sample with a water (or acetone or ethanol) spurt and drying it rapidly with compressed air or nitrogen immediately after switching off the potential and removing the electrode from the solution, gave the most reliable and reproducible results. The washing was essential to prevent the discharge of PbO2 to PbSO4 on the electrode surface. The moisture remaining in the corrosion layer was found to render a self-discharge reaction inside the film possible, thus changing the original composition of the layer. It is concluded that more discussion is needed in the literature on sample pretreatment before ex situ analysis.
Original languageEnglish
Pages (from-to)71-80
JournalJournal of Power Sources
Volume32
Issue number1
DOIs
Publication statusPublished - 1990
MoE publication typeA1 Journal article-refereed

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Washing
X ray diffraction analysis
Lead
washing
Corrosion
pretreatment
Oxidation
oxidation
Electrodes
Compressed air
corrosion
products
Acetone
diffraction
X ray powder diffraction
compressed air
Drying
Ethanol
x rays
Nitrogen

Cite this

Laitinen, Timo ; Sundholm, Göran ; Vilhunen, J. / Comments about sample treatment in the X-ray diffraction analysis of the oxidation products of lead. In: Journal of Power Sources. 1990 ; Vol. 32, No. 1. pp. 71-80.
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Comments about sample treatment in the X-ray diffraction analysis of the oxidation products of lead. / Laitinen, Timo; Sundholm, Göran (Corresponding Author); Vilhunen, J.

In: Journal of Power Sources, Vol. 32, No. 1, 1990, p. 71-80.

Research output: Contribution to journalArticleScientificpeer-review

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AU - Sundholm, Göran

AU - Vilhunen, J.

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AB - The influence of different sample pretreatment methods in the period between switching off the potential control and the actual X-ray scan on the results of ex situ X-ray powder diffraction analysis of thin corrosion films of Pb anodized in H2SO4 has been studied. Washing the sample with a water (or acetone or ethanol) spurt and drying it rapidly with compressed air or nitrogen immediately after switching off the potential and removing the electrode from the solution, gave the most reliable and reproducible results. The washing was essential to prevent the discharge of PbO2 to PbSO4 on the electrode surface. The moisture remaining in the corrosion layer was found to render a self-discharge reaction inside the film possible, thus changing the original composition of the layer. It is concluded that more discussion is needed in the literature on sample pretreatment before ex situ analysis.

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