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Development of a versatile sample preparation method and its application for rare-earth pattern and Nd isotope ratio analysis in nuclear forensics.

Krajko J, Varga Z, Wallenius M, Mayer K - J Radioanal Nucl Chem (2014)

Bottom Line: An improved sample preparation procedure for trace-levels of lanthanides in uranium-bearing samples was developed.The method involves a simple co-precipitation using Fe(III) carrier in ammonium carbonate medium to remove the uranium matrix.The procedure is an effective initial pre-concentration step for the subsequent extraction chromatographic separations.

View Article: PubMed Central - PubMed

Affiliation: European Commission, Joint Research Centre, Institute for Transuranium Elements, Postfach 2340, 76125 Karlsruhe, Germany ; Faculty of Applied Sciences, Delft University of Technology, Mekelweg 15, 2629 JB Delft, Netherlands.

ABSTRACT

An improved sample preparation procedure for trace-levels of lanthanides in uranium-bearing samples was developed. The method involves a simple co-precipitation using Fe(III) carrier in ammonium carbonate medium to remove the uranium matrix. The procedure is an effective initial pre-concentration step for the subsequent extraction chromatographic separations. The applicability of the method was demonstrated by the measurement of REE pattern and (143)Nd/(144)Nd isotope ratio in uranium ore concentrate samples.

No MeSH data available.


Related in: MedlinePlus

Scheme of the procedure developed
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Fig1: Scheme of the procedure developed

Mentions: The Nd separation was performed in two steps: first a lanthanide group separation followed by the Nd separation. The Nd purification step is necessary for the removal of Sm, which interferes otherwise with the ICP-MS analysis. In the first step the lanthanide content of the sample aliquots was separated using extraction chromatography by the selective retention of trivalent lanthanides on the TRU™ resin in 3 mol L−1 nitric acid medium. In the second step, Ln resin was used in 0.05 mol L−1 HCl medium for the Nd separation. After Nd was stripped from the column with 0.2 mol L−1 HCl. This solution was evaporated to almost complete dryness and the residue was dissolved in nitric acid for mass spectrometric analysis. A method blank was processed through the entire dissolution and separation procedure parallel to the samples. The measured signal of the method blank was <2 % for all samples. The final Nd fractions were analysed by MC-ICP-MS. The simplified scheme of the entire separation procedure can be seen in Fig. 1. The detailed extraction chromatographic separation procedure can be found elsewhere [9, 16]. The method was validated by the measurement of reference material (Morille, Cetama), the recovery for the certified rare-earth elements (Sm, Eu, Gd, Dy) being better than 90 % [17].Fig. 1


Development of a versatile sample preparation method and its application for rare-earth pattern and Nd isotope ratio analysis in nuclear forensics.

Krajko J, Varga Z, Wallenius M, Mayer K - J Radioanal Nucl Chem (2014)

Scheme of the procedure developed
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4514581&req=5

Fig1: Scheme of the procedure developed
Mentions: The Nd separation was performed in two steps: first a lanthanide group separation followed by the Nd separation. The Nd purification step is necessary for the removal of Sm, which interferes otherwise with the ICP-MS analysis. In the first step the lanthanide content of the sample aliquots was separated using extraction chromatography by the selective retention of trivalent lanthanides on the TRU™ resin in 3 mol L−1 nitric acid medium. In the second step, Ln resin was used in 0.05 mol L−1 HCl medium for the Nd separation. After Nd was stripped from the column with 0.2 mol L−1 HCl. This solution was evaporated to almost complete dryness and the residue was dissolved in nitric acid for mass spectrometric analysis. A method blank was processed through the entire dissolution and separation procedure parallel to the samples. The measured signal of the method blank was <2 % for all samples. The final Nd fractions were analysed by MC-ICP-MS. The simplified scheme of the entire separation procedure can be seen in Fig. 1. The detailed extraction chromatographic separation procedure can be found elsewhere [9, 16]. The method was validated by the measurement of reference material (Morille, Cetama), the recovery for the certified rare-earth elements (Sm, Eu, Gd, Dy) being better than 90 % [17].Fig. 1

Bottom Line: An improved sample preparation procedure for trace-levels of lanthanides in uranium-bearing samples was developed.The method involves a simple co-precipitation using Fe(III) carrier in ammonium carbonate medium to remove the uranium matrix.The procedure is an effective initial pre-concentration step for the subsequent extraction chromatographic separations.

View Article: PubMed Central - PubMed

Affiliation: European Commission, Joint Research Centre, Institute for Transuranium Elements, Postfach 2340, 76125 Karlsruhe, Germany ; Faculty of Applied Sciences, Delft University of Technology, Mekelweg 15, 2629 JB Delft, Netherlands.

ABSTRACT

An improved sample preparation procedure for trace-levels of lanthanides in uranium-bearing samples was developed. The method involves a simple co-precipitation using Fe(III) carrier in ammonium carbonate medium to remove the uranium matrix. The procedure is an effective initial pre-concentration step for the subsequent extraction chromatographic separations. The applicability of the method was demonstrated by the measurement of REE pattern and (143)Nd/(144)Nd isotope ratio in uranium ore concentrate samples.

No MeSH data available.


Related in: MedlinePlus