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Direct determination of metallic impurities in nuclear-grade boron carbide by slurry sampling total reflection X-ray fluorescence spectrometry and ICP atomic emission spectrometry subsequent to ultra-high-pressure sample digestion

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Abstract

Slurry sampling-TXRF and ultra-high-pressure digestion ICP-OES methods were developed for the direct determination of Ca, Co, Cr, Al, Cu, Fe, Mn, Na, Ni, Ti in different particle size nuclear-grade boron carbide powders. The dispersive effect of polacrylateamine (NH4PAA) was used as a dispersion agent. Different zeta potential values and NH4PAA concentrations could get stable and homogeneous slurries. It was found that pH at 6.0 and NH4PAA 0.5 wt% provided the best conditions. Optimization of the slurry concentration of TXRF was performed for the net elemental intensity of Ca, Ti, Fe, and the internal standard element Ga. Through experimental results, we used the 10 mg·mL−1 as a suitable slurry concentration. The analytical results obtained using TXRF and ultra-high-pressure digestion ICP-OES methods were in good agreement with the recommended method DC-arc-OES. Besides, the detection limit of TXRF and ICP-OES is in the range of 0.1–1.0 μg·g−1 (expect Al and Na) which was lower than the DC-arc-OES method. The reference material of ERM 102 was used to validate the accuracy and get good results. The recovery rates of TXRF are between 83% and 115% for Cu (2.4–25 μg·g−1), Cr (12–234 μg·g−1), Ca (158–211 μg·g−1), Co (2.9–6.5 μg·g−1), Fe (965–1547 μg·g−1), Mn (17–24 μg·g−1), Ni (56–128 μg·g−1), and Ti (12–80 μg·g−1).

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Acknowledgements

The authors thank Dr. Junjie Li for his valuable guidance in the preparation of this manuscript. The financial support of the NSFC (41973051) is gratefully acknowledged.

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Authors and Affiliations

  1. Beijing Research Institute of Uranium Geology, Beijing, 100029, China

    Jian Yuan, Shuo Feng, Jianyong Cui, Apeng Yu & Yang Chang

  2. Institute for Advanced Study, Chengdu University, Chengdu, 610106, China

    Shouhua Sun

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  1. Jian Yuan
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  2. Shuo Feng
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  3. Jianyong Cui
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  4. Shouhua Sun
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  5. Apeng Yu
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Correspondence to Jian Yuan or Shouhua Sun.

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Yuan, J., Feng, S., Cui, J. et al. Direct determination of metallic impurities in nuclear-grade boron carbide by slurry sampling total reflection X-ray fluorescence spectrometry and ICP atomic emission spectrometry subsequent to ultra-high-pressure sample digestion. J IRAN CHEM SOC 19, 589–597 (2022). https://doi.org/10.1007/s13738-021-02332-7

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