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Pre-concentration of Ta(V) by solvent extraction before determination of trace amounts of Ta in Nb and Nb compounds

机译:在确定Nb和Nb化合物中的痕量Ta之前,通过溶剂萃取对Ta(V)进行预浓缩

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The paper presents the results of a study on the efficiency of the separation of Ta(V) and Nb(V) from fluoride solutions by solvent extraction with methyl isobutyl ketone with a view to applying the extraction process to the purification of Nb from Ta and for the pre-concentration of Ta prior to its determination in Nb and its compounds over a wide range of initial concentrations. With strict control of the hydrofluoric acid concentration and the re-extraction of Ta into an aqueous phase using an ammonium oxalate solution, the mean recovery factors [%] for Ta were 94a€“108% in the initial weight ratio mNb:mTa = (??Nb/Ta) range 10a€“1000000 with only a small scatter about the mean value (RSD a‰¤ 6%), with the exception of (??Nb/Ta) = 1000000. The effect of the composition of the re-extraction solution on the excitation conditions of Ta in ICP-OES (ICP-MS) plasma was negligible and small amounts of Nb and other contaminants co-extracted with Ta did not affect its determination.
机译:本文介绍了用甲基异丁基酮进行溶剂萃取从氟化物溶液中分离Ta(V)和Nb(V)的效率的研究结果,以期将萃取工艺应用于从Ta和Na中纯化Nb的研究。在宽范围的初始浓度范围内,先测定Ta中的Nb及其化合物中的Ta浓度。通过严格控制氢氟酸浓度和使用草酸铵溶液将Ta再萃取到水相中,在初始重量比mNb:mTa =(下)中,Ta的平均回收率[%]为94a–108%。 Nb / Ta)的范围在10a-1000000之间,只有很小的平均值散布(RSD≤6%),但(ΔNb/ Ta)= 1000000除外。 ICP-OES(ICP-MS)等离子体中Ta激发条件下的二次萃取溶液微不足道,与Ta共萃取的少量Nb和其他污染物不影响其测定。

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