Turkowska Magdalena, Karoń Krzysztof, Milewski Andrzej, Jakóbik-Kolon Agata
InorChem Centre for Research and Development, Łukasiewicz Research Network New Chemical Syntheses Institute, Sowińskiego 11, 44-101 Gliwice, Poland.
Faculty of Chemistry, Silesian University of Technology, Krzywoustego 6, 44-100 Gliwice, Poland.
Materials (Basel). 2022 Feb 17;15(4):1513. doi: 10.3390/ma15041513.
Reactor-grade niobium steel is used as a construction material for nuclear reactors. In this case, the presence of tantalum, which is characterized by a 20 times higher active cross section for capturing thermal neutrons than the cross section of niobium (Ta: 21.3 barn), cannot exceed 100 ppm. Analytical methods for quality and new separation method development control need very pure niobium matrices-niobium compounds with a low tantalum content, which are crucial for preparing matrix reference solutions or certified reference materials (CRMs). Therefore, in this paper, a new, efficient method for separating trace amounts of Ta(V) from Nb(V) using extraction chromatography with the use of sorbents impregnated with methyl isobutyl ketone MIBK solvent is proposed. Various types of MIBK-impregnated sorbents were used (AG 1-X8 Anion Exchange Resin, AMBERLITE™ IRC120 Na Ion Exchange Resin, SERVACEL Cellulose Anion Exchangers DEAE 52, active carbons of various grain size, carbonized blackcurrant pomace, carbonized chokeberry pomace, bentonite, and polyurethane foam in lumps). The highest tantalum removal efficiency was determined using active coal-based materials (>97%). The separation effectivity of tantalum from niobium was also determined in dynamic studies using a fixed-bed column with MIBK-impregnated active carbon. Solutions of various Nb:Ta weight ratios (1:1, 100:1, 1000:1) were used. The most impressive result was obtaining 70 mL of high purity niobium solution of tantalum content 0.027 ppm (in relation to Nb) with 88.4% yield of niobium from a solution of Nb:Ta, weight ratio 1000:1 (purge factor equaled 35,000). It proves the presented system to be applicable for preparation of pure niobium compounds with very low contents of tantalum.
反应堆级铌钢用作核反应堆的建筑材料。在这种情况下，钽的存在量不能超过100 ppm，钽对热中子的俘获活性截面比铌的截面高20倍（钽：21.3靶恩）。质量分析方法和新分离方法开发控制需要非常纯的铌基体——钽含量低的铌化合物，这对于制备基体参考溶液或有证标准物质（CRM）至关重要。因此，本文提出了一种新的、高效的方法，即使用浸渍有甲基异丁基酮（MIBK）溶剂的吸附剂通过萃取色谱法从铌（V）中分离痕量钽（V）。使用了各种类型的浸渍MIBK的吸附剂（AG 1-X8阴离子交换树脂、AMBERLITE™ IRC120 Na离子交换树脂、SERVACEL纤维素阴离子交换剂DEAE 52、各种粒度的活性炭、碳化黑加仑果渣、碳化苦樱桃果渣、膨润土和块状聚氨酯泡沫）。使用基于活性炭的材料确定了最高的钽去除效率（>97%）。还使用装有浸渍MIBK的活性炭的固定床柱在动态研究中确定了钽与铌的分离效果。使用了各种Nb:Ta重量比（1:1、100:1、1000:1）的溶液。最令人印象深刻的结果是从Nb:Ta重量比为1000:1的溶液中获得了70 mL钽含量为0.027 ppm（相对于Nb）的高纯度铌溶液，铌的产率为88.4%（净化因子等于35,000）。这证明了所提出的系统适用于制备钽含量极低的纯铌化合物。
