Determination of Trace Technetium-99 in Soil Samples by Isotope Dilution/Negative Thermal Ionization Mass Spectrometry
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Graphical Abstract
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Abstract
As an important long-lived and high-abundance fission product, 99Tc dispersed into the environment because of the nuclear test in atmosphere, the nuclear fuel cycle and nuclear medicine.The isotope dilution mass spectrometry (IDMS)technology of measuring 99Tc using 97Tc as the spike was developed. The chemical separation procedure of Tc is established, and the recovery rate is more than 71% for the overall process. 97Tc (97Tc, 84.77%; 98Tc, 15.03%; 99Tc, 0.20%)was prepared by irradiation of natural ruthenium metal, then was calibrated by IDMS with 99Tc standard material as the spike. The conventional positive thermal ionization mass spectrometry(TIMS) was inapplicable due to the high ionization potential of 7.3 eV for technetium, therefore based on MgCl2+Ba(OH)2 as the loading reagent, the negative thermal ionization mass spectrometry of technetium was established, and the ion current indensity of 99TcO4-(M/z=163) reached 1.7×10-12A. Then, 99Tc in the soil samples was quantitatively determined by negative thermal ionization mass spectrometry and isotope dilution method. The combined standard uncertainty is better than 3%.
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