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Analysis of 14C-bearing compounds released by corrosion of irradiated steel using accelerator mass spectrometry


The combination of ion chromatography (IC) with accelerator mass spectrometry (AMS) was developed to determine the speciation of 14C-(radiocarbon) bearing organic compounds in the femto to pico molar concentration range. The development of this compound-specific radiocarbon analysis (CSRA) of carboxylic acids is reported and the application of the method on a leaching solution from neutron-irradiated steel is demonstrated. Background and dynamic range of the AMS-based method were quantified. Using 14C-labelled standards, the measurements demonstrate the repeatability of the analytical method and the reproducible recovery for the main target carboxylic acids (i.e., acetate, formate, malonate, and oxalate). The detection limit was determined to be in the mid fmol 14C/L level while the dynamic range of the analytical method covers three orders of magnitude from the low fmol to mid pmol 14C/L level. Cross contamination was found to be negligible during IC fractionation and was accounted for during eluate processing and 14C detection by AMS. The 14C-bearing carboxylates released from an irradiated steel nut into an alkaline leaching solution were analysed using the CSRA-based analytical method with the aim to check the applicability of the approach and develop appropriate sample preparation. The concentrations of 14C-bearing formate and acetate, the main organic corrosion products, were at low pmol 14C/L level for convenient dimensions of the alkaline leaching experiment which demonstrates that compound-specific 14C AMS is an extremly sensitive analytical method for analysing 14C-bearing compounds. The content of total organic 14C in solution (TO14C) determined by direct meassurement of an aliquot of the leaching solution agrees well with the sum of the 14C concentrations of the individual carboxylates within the uncertainty of the data. The TO14C content further is in good agreement with the calculated value using the corrosion rate determined from 60Co release and the 14C inventory of the irradiated steel specimen.

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Publication details

The article was received on 06 Feb 2018, accepted on 03 May 2018 and first published on 07 May 2018

Article type: Paper
DOI: 10.1039/C8AN00237A
Citation: Analyst, 2018, Accepted Manuscript
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    Analysis of 14C-bearing compounds released by corrosion of irradiated steel using accelerator mass spectrometry

    B. Z. Cvetković, G. Salazar, D. Kunz, S. Szidat and E. Wieland, Analyst, 2018, Accepted Manuscript , DOI: 10.1039/C8AN00237A

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