Application of bias correction methods to improve U3Si2 sample preparation for quantitative analysis by WDXRF

Marcos Antonio Scapin

doi:10.15392/bjrs.v7i2A.582

Authors

Marcos Antonio Scapin Instituto de Pesquisas Energéticas e Nucleares

DOI:

https://doi.org/10.15392/bjrs.v7i2A.582

Keywords:

U3Si2, XRF, WDXRF.

Abstract

The determination of silicon (Si), total uranium (U) and impurities in uranium-silicide (U₃Si₂) samples by wavelength dispersion X-ray fluorescence technique (WDXRF) has been already validated and is currently implemented at IPEN’s X-Ray Fluorescence Laboratory (IPEN-CNEN/SP) in São Paulo, Brazil. Sample preparation requires the use of approximately 3 g of H3BO3 as sample holder and 1.8 g of U3Si2. However, because boron is a neutron absorber, this procedure precludes U3Si2 sample’s recovery, which, in time, considering routinely analysis, may account for significant unusable uranium waste. An estimated average of 15 samples per month is expected to be analyzed by WDXRF, resulting in approx. 320 g of U₃Si₂ that wouldn’t return to the nuclear fuel cycle. This not only impacts in production losses, but generates another problem: radioactive waste management. The purpose of this paper is to present the mathematical models that may be applied for the correction of systematic errors when H3BO3 sample holder is substituted by cellulose-acetate {[C₆H₇O₂(OH)₃-m(OOCCH₃)m], m = 0~3}, thus enabling U₃Si₂ sample’s recovery. The results demonstrate that the adopted mathematical model is statistically satisfactory, allowing the optimization of the procedure.U₃Si₂, XRF, WDXRF.

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Author Biography

Marcos Antonio Scapin, Instituto de Pesquisas Energéticas e Nucleares

Possui Bacharelado e Licenciatura em Ciências com Habilitação em Química, Mestrado e Doutorado em Ciências na área de Tecnologia Nuclear pelo IPEN-USP. Atualmente desenvolve atividades de análises químicas e físicas por meio das técnicas de fluorescência de raios X e microscopia eletrônica nos Centros de Química e Meio Ambiente e Lasers e Aplicações no Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP). As atividades de pesquisas estão concentradas no desenvolvimento de metodologias para o estudo de materiais aplicados nas diferentes áreas de conhecimento, como nuclear, nanotecnologia, ambiental, saúde forense e outras, com ênfase nas técnicas de fluorescência de raios X e microscopia eletrônica.

References

M. A. SCAPIN, V. L. R. SALVADOR, M. E. B. COTRIM, M. A. F. PIRES. Uncertainty measurement evaluation of WDXRF and EDXRF techniques for the Si and Utotal determination in U3Si2 nuclear fuel. J Radioanal Nucl Chem, DOI: 10.1007/s10967-010-0897-6, 2011.

M. A. SCAPIN, M. B. E. COTRIM, C. P. SILVA, M. A. F. PIRES, Application of multivari-ate calibration for simultaneous determination of major and minor constituents in U3Si2 by WDXRF technique. J. Radioanal. Nucl. Chem., DOI 10.1007/s10967-014-3332-6, 2014.

WEST, M.; ELLIS, A. T.; . POTTS, P. J.; STRELI. C.; VANHOOF, C.; WOBRAUSCHEK, P. 2015 Atomic Spectrometry Update – a review of advances in X-ray fluorescence spectrometry and their applications. J. Anal. At. Spectrom, DOI 10.1039/C5JA90033F, 2015.

IPEN - Instituto de Pesquisas Energéticas e Nucleares. CCN se adequa para atender demanda do RMB. São Paulo, Brasil, 2015. Available at: <https://www.ipen.br/portal_por/portal/interna.php?secao_id=38&campo=1977>. (2015). Last ac-cessed: 17 Nov. 2017.

M. A. SCAPIN, M. B. E. COTRIM, C. P. SILVA, M. A. F. PIRES, Application of multivari-ate calibration for simultaneous determination of major and minor constituents in U3Si2 by WDXRF technique. In: INTERNATIONAL NUCLEAR ATLANTIC CONFERENCE, 2013, Recife, Annals… Available at: <http://www.iaea.org/inis/collection/NCLCollectionStore/_Public/46/021/46021415.pdf>. Last ac-cessed: 17 Nov. 2017.

D. W. PRESTON; E. R. DIETZ, The art of experimental physics, Nova York: John Wiley & Sons, 1991.

RIGAKU CORPORATION. Rigaku multi-element simultaneous X-ray fluorescence spec-trometer Simultix 14. Instruction Manual, Tokyo, Japan, 1999.

INMETRO – Instituto Nacional de Metrologia, Qualidade e Tecnologia. 4. Orientação sobre validação de métodos analíticos (DOQ-CGRE-008) Review 05. (2016). Available at: <http://www.inmetro.gov.br/Sidoq/Arquivos/CGCRE/DOQ/DOQ-CGCRE-8_05.pdf > Last acces-sed: 17 Nov. 2017.