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Nano ZrO2 Synthesis by Extraction of Zr(IV) from ZrO(NO3)2 by PC88A, and Determination of Extraction Impurities by ICP-MS

Chu, Manh Nhuong and Nguyen, T. H. Lan and Mai, Xuan Truong and Doan, Van Thuan and Bach, Long Giang and Nguyen, Duy Chinh and Nguyen, Duc Cuong (2018) Nano ZrO2 Synthesis by Extraction of Zr(IV) from ZrO(NO3)2 by PC88A, and Determination of Extraction Impurities by ICP-MS. Metals, 8 (851). pp. 1-15. ISSN 2075-4701

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High purity Zirconium (Zr) materials are essential in many components of nuclear reactors, especially fuel cladding tubes. Due to the matrix influence, determination of impurities in the Zr materials requires separation from the Zr matrix. Among extraction methods, solvent extraction is common and suitable for large-scale production. In this study, extraction capability of Zr(IV) by 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (PC88A) was examined by FT-IR and UV of ZrO(NO3)2 salt, PC88A-toluene solvent, and Zr-PC88A-toluene complex. ZrO2 (obtained from Institute for Technology of Radioactive and Rare Elements—ITRRE), after being separated from the Zr matrix, was determined for impurities using internal standard (indium, In) by 50% of PC88A dissolved in toluene. Separation of impurities from the Zr matrix underwent two stages. First, one cycle of extraction of the Zr matrix and impurities in 3 M HNO3 using 50% PC88A/toluene was conducted. Second, impurities were scrubbed by 4 M HNO3 in two cycles. Results revealed that approximately 74% of Zr(IV) was separated to the organic phase and 26% remained in the aqueous phase. Determination of impurities after separation from the Zr matrix by ICP-MS using internal standard in revealed that the recovery of impurities achieved 95–100%. With the mentioned amount of Zr, the effect of the Zr matrix on the determination of elements by ICP-MS is negligible. Levels of impurities have relative standard deviations (RSD) of less than 6.9% and recovery of 88.6–98.8%. Therefore, the determination of impurities has high reliability and accuracy. The back-extraction of Zr(IV) in organic phase by 1 M H2SO4 has stripped about 99.5% of the Zr matrix back to the aqueous phase. Following this, NH3 was added to the solution containing Zr after back-extraction to form Zr(OH)4 which was then desiccated to produce ZrO2. X-ray Diffraction (XRD), Scanning and Transmission Electron Microscopy (SEM and TEM) images showed that the new ZrO2 product has spherical nanostructure with diameters of less than 25 nm, which is suitable for applications for the treatment of colorants, metal ions in wastewater sources and manufacture of anti-corrosion steel. In addition, the energy dispersive X-ray (EDX) of the new ZrO2 product showed that it has high purity.

Item Type: Article
Subjects: Scopus-indexed journals
ISI-indexed journals
Divisions: Faculty of Engineering Physics and Nanotechnology (FEPN)
Depositing User: Dr. Duc Cuong Nguyen
Date Deposited: 15 Nov 2018 09:20
Last Modified: 15 Nov 2018 09:20

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