De A K, Sen A K
Department of Chemistry, Jadavpur University, Calcutta-32, India.
Talanta. 1966 Jun;13(6):853-6. doi: 10.1016/0039-9140(66)80290-4.
A method is proposed for the rapid extraction and separation of microgram amounts of niobium(V). The niobium is extracted quantitatively by 100 % TBP from 7.7-9.4 M (initial) hydrochloric acid and determined spectrophotometrically as the thiocyanate in TBP-acetophenone solution. Beer's Law is obeyed at 430 mmu over the range 0.8-9.0 mug ml . The system is stable for 72 hr. Caesium, calcium, strontium, barium, aluminium, titanium(IV), zirconium(IV), cerium(TV), fluoride, thiocyanate and oxalate do not interfere (1 mg). Niobium(V) can be determined in a niobium(V)-tantalum(V) mixture. The method is accurate and reproducible to within +/-2%.
提出了一种快速提取和分离微克量铌（V）的方法。铌通过100%磷酸三丁酯从7.7 - 9.4 M（初始）盐酸中定量萃取，并在磷酸三丁酯 - 苯乙酮溶液中以硫氰酸盐形式进行分光光度法测定。在430毫微米处，0.8 - 9.0微克/毫升范围内符合比尔定律。该体系72小时内稳定。铯、钙、锶、钡、铝、钛（IV）、锆（IV）、铈（IV）、氟化物、硫氰酸盐和草酸盐不产生干扰（1毫克）。铌（V）可在铌（V） - 钽（V）混合物中测定。该方法准确且重现性在±2%以内。
