Microwave-assisted dissolution of highly refractory dysprosium-titanate (Dy2TiO5) followed by chemical characterization for major and trace elements using ICP-MS, UV-visible spectroscopy and conventional methods

被引:2
|
作者
Nagar, Brijlesh Kumar [1 ,2 ]
Kumari, Khushboo [2 ]
Deb, Sadhan Bijoy [2 ]
Saxena, Manoj Kumar [2 ]
Tomar, Bhupendra Singh [1 ,2 ]
机构
[1] Homi Bhabha Natl Inst, Bombay 400094, Maharashtra, India
[2] Bhabha Atom Res Ctr, Radioanalyt Chem Div, Dept Atom Energy, Bombay 400085, Maharashtra, India
关键词
Microwave; ICP-MS; UV-visible spectrophotometer; gravimetry; new control rod material; GRAVIMETRIC-DETERMINATION; SOLVENT-EXTRACTION; SPECTROMETRIC TECHNIQUES; ACID; OXALATE; URANIUM; COMPLEXES; TITANIUM; SAMPLE; IMPURITIES;
D O I
10.1515/ract-2018-2934
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Dysprosium-titanate (Dy2TiO5), being highly refractory in nature, its dissolution using conventional (hot-plate and fusion) methods is very difficult. Hence, for quantitative dissolution, a microwave method has been developed. The instrumental parameters and amount of acids has been optimized. Studies have been carried out for precise and accurate estimation of major elements such as Dy, Ti, and Mo. An anion exchange column has been used to separate Mo, Dy and Ti. Analysis of these elements has been carried out using ICP-MS, UV-visible spectroscopy, and gravimetric methods. In the developed method, precipitation of molybdenum and dysprosium has been done using a-benzoine oxime, and oxalic acid respectively. These precipitates have been converted into their respective oxide form. The purities of these oxides (Dy2O3 and MoO3) have been determined using ICP-MS. The method has been validated using synthetic samples where it is found that accuracy of Dy and Mo is >99 % and precision is <1 (%RSD). The titanium has been determined using UV-visible spectroscopy with accuracy >98 % and precision <2 (%RSD).
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页码:917 / 926
页数:10
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