TITLE

Determination of ultra-trace amounts of Fe in AgNO3 solutions by means of isotope dilution analysis applying an inductively coupled plasma mass spectrometer equipped with a dynamic reaction cell

AUTHOR(S)
Balcaen, Lieve; Geuens, Ingrid; Moens, Luc; Vanhaecke, Frank
PUB. DATE
November 2003
SOURCE
Analytical & Bioanalytical Chemistry;Nov2003, Vol. 377 Issue 6, p1020
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
The development of an ICP-MS method for the determination of ultra-trace amounts of Fe in AgNO3 solutions using isotope dilution for calibration is described. AgNO3 solutions are used as raw materials in the production of traditional photographic materials, and it is known that contamination with metal traces can influence the quality of the films thus produced. After adding an appropriate amount of an 54Fe-enriched spike and permitting isotopic equilibration to take place, Ag was selectively removed from the solutions by precipitation as AgBr. Although to some extent, co-precipitation of Fe is possible under the given circumstances, an incomplete recovery of the analyte element did not affect the accuracy of the results, owing to the use of isotope dilution for calibration. NH3 was used as a reaction gas in a quadrupole-based ICP-MS instrument, equipped with a dynamic reaction cell (DRC), providing interference-free measurement of the 54Fe/56Fe ratio. The limit of detection (LOD) obtained using this procedure was approximately 0.01 �g g-1. This is an excellent value in comparison with the detection limit obtained with the more traditional approach: sample dilution and external calibration with a Fe standard solution (LOD ~1 �g g-1). To validate the method, recovery experiments were carried out. In all instances, a quantitative recovery was established. Finally, the method was applied to the analysis of AgNO3 solutions. A large variation in Fe concentration was observed. Depending on the Fe content in the samples, relative standard deviations typically ranged between 1 and 14%.
ACCESSION #
15124801

 

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