Monday 20 September 2021

Extraction and Separation of Nano-Sized Zirconia from in High Purity ZrO(NO) Using PC88A, D2EHPA and Determination of Impurities by ICP-MS | Chapter 5 | Challenges and Advances in Chemical Science Vol. 5

Many nuclear reactor components, especially the fuel cladding tubes, require high purity zirconium (Zr) elements. Separation from the Zr matrix is required to determine impurities in Zr materials due to the influence of the matrix. Solvent extraction is a typical extraction method that works well in large-scale manufacturing. The capacity of 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (PC88A) and di-(2-ethylhexyl) phosphoric acid (D2EHPA) to extract Zr(IV) was investigated in this chapter using FT-IR, UV spectra of ZrO(NO3)2 salt, PC88A-toluene solvent, and Zr-PC88A-toluen ZrO2 (from the Institute for Technology of Radioactive and Rare Elements - ITRRE) and ZrCl4 (from Merck) are combined to make ZrO2 (NO3) 2, after being isolated from the Zr matrix, was tested for impurities using a 50 percent PC88A dissolved in toluene internal standard (indium, In). In two phases, impurities were removed from the Zr matrix. The Zr matrix and impurities were removed in 3.0 M HNO3 for one cycle using 50 percent PC88A/toluene. Second, contaminants were removed using 4.0-6.0 M HNO3 in two cycles. Approximately 74% of Zr(IV) was segregated into the organic phase, whereas 26% remained in the aqueous phase, according to the data. ICP-MS recovery of impurities after separation from the Zr matrix using an internal standard revealed a 95–100% recovery of impurities. With the amount of Zr given, the influence of the Zr matrix on ICP-MS element determination is negligible. Relative standard deviations (RSDs) of less than 6.9% and recoveries (Revs) of 88.6–98.8% were found in impurity levels. As a result, contamination assessment is exceedingly precise and trustworthy. Back-extraction of Zr(IV) in organic phase with 1.0 - 1.5 M H2SO4 returned 99.5 percent of the Zr matrix to the aqueous phase.

After that, NH3 was added to the Zr-containing solution to produce Zr(OH)4, which was then dehydrated to yield ZrO2. According to X-ray Diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM) images, the new ZrO2 product has a spherical nanostructure with diameters of less than 25 nm, making it suitable for applications such as colourant treatment, metal ions in wastewater sources, and the manufacture of anti-corrosion steel. Furthermore, an energy dispersive X-ray (EDX) study of the new ZrO2 product demonstrated that it is exceptionally pure.


Author (S) Details


Nhuong Chu Manh

Faculty of Chemistry, Thai Nguyen University of Education, Thai Nguyen City 24000, Vietnam


N. T. H. Lan

Faculty of Chemistry, Thai Nguyen University of Education, Thai Nguyen City 24000, Vietnam.


M. X. Truong

Faculty of Chemistry, Thai Nguyen University of Education, Thai Nguyen City 24000, Vietnam.


D. T. Huong

Faculty of Chemistry, Thai Nguyen University of Education, Thai Nguyen City 24000, Vietnam.


N. T. T. Loan

Faculty of Chemistry, Thai Nguyen University of Education, Thai Nguyen City 24000, Vietnam.


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