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Determination of ultra-trace level of 232 Th in seawater by ICP-SFMS after matrix separation and preconcentration.

Analytica Chimica Acta 2018 Februrary 14
This article describes the development and validation of an analytical procedure for the matrix separation, preconcentration and determination of sub-ng kg-1 levels232 Th in a small volume (20 mL) of seawater samples. The matrix separation and Th preconcentration was carried out using a commercially available ion-chelation system seaFAST-pico. The acidified to pH < 2 seawater samples were mixed on-line with the ammonium acetate buffer (pH of 6.0 ± 0.2) before loading on the column containing resin with iminodiacetic and ethylenediaminetriacetic functional groups. At this pH,232 Th was quantitatively retained on the resin, demonstrating a good affinity (selectivity) for Th in seawater matrix. The element retained on the resin was eluted using only 0.2 mL of 1.8 M HNO3 enabling to achieve high preconcentration factor. The pretreatment procedure, with two sample loading cycles (each one 10 mL), was accomplished in about 25 min. Determining232 Th mass fraction in seawater samples was based on isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) method, which was considered as the most accurate calibration strategy for precise quantification of232 Th mass fraction in seawater samples. ISO/IEC17025 and Eurachem guidelines were followed to perform the validation of the developed in this study procedure. In the case of seawater samples with natural level of thorium the major contributions to the expanded uncertainty arose from the uncertainty associated with isotopic ratio measurements in the isotopically spiked sample, followed by the correction for procedural blank and the correction for mass discrimination effect. The estimated method detection limit for232 Th was 0.005 ng kg-1 . The developed method was successfully applied to the determination of232 Th mass fraction in seawater reference samples: IAEA-443, SLEW-3, NASS-4, NASS-6, and CASS-5. Although232 Th is not certified in any of the seawater reference materials, a good agreement was obtained between the results in this study and data published elsewhere.

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