Abstract：The content of niobium in aluminum-niobium alloy has significant influence on the performance and application of aluminum-niobium alloy. During the determination of niobium by paper chromatography separation-gravimetric method, the separation effect of niobium from other elements is greatly affected by the chromatographic agent composition and environment. The effects of sample mass, chromatographic agent composition, chromatographic time and coexisting element were investigated in experiments. The optimal experimental conditions were finally obtained. The accurate determination of niobium content in aluminum-niobium alloy was realized. The sample was dissolved with hydrofluoric acid and nitric acid. The concentrated solution was coated on the colored paper. The separation of niobium from other coexisting elements was realized based on the different migration rates of niobium, aluminum and other coexisting elements in the specific chromatographic agent. The colored paper containing niobium was fired to constant mass in a muffle furnace at 900℃. For the aluminum-niobium alloy containing 50%-80% niobium (mass fraction), the separation effect was best under the following experimental conditions: the sample mass was 0.10g; the volume ratio of 4-methyl-2-pentanone, butanone, hydrofluoric acid and nitric acid in chromatographic agent was 125∶42∶32∶7; the chromatographic time was 6h. The coexisting microelements such as iron, molybdenum, silicon, nickel and chromium had no influence on the determination of niobium. If the mass fraction of tantalum in sample was higher than 0.01%, the mass of tantalum oxide should be subtracted from the crude niobium oxide precipitate. The proposed method was applied for the determination of niobium in three aluminum-niobium alloy samples. The relative standard deviations (RSD, n=11) of determination results were between 0.18%-0.29%. The spiked recoveries were between 98% and 102%. Four laboratories were selected for collaborative verification, and there was no significant difference in measurement results by the Cochran test.
殷学峰,崔军,董玉兰.纸上色层重量法测定铌矿和铌渣中五氧化二铌[J].冶金分析,2003,23(5):74-75,48.YIN Xue-feng,CUI Jun,DONG Yu-lan.Gravimetric determination of niobium pentoxide in niobium ore and niobium slag with colored layer on paper[J].Metallurgical Analysis,2003,23(5):74-75,48.
陈先安,张玲云.用N2O-乙炔火焰原子吸收法测定包头铌、锰炉渣及其中间产品中微量钙[J].稀有金属(Chinese Journal of Rare Metals),1983(1):76-77.
[6]
马清文,王际祥,薛明浩,等.光度法快速测定铌铁中铌[J].山东冶金,2008,30(6):55-56.MA Qing-wen,WANG Ji-xiang,XUE Ming-hao,et al.Spectrophotometric determination of niobium in iron niobium[J].Shandong Metallurgy,2008,30(6):55-56.
[7]
周礼仙,汪雪梅.氯代磺酚C分光光度法测定钒钛磁铁矿中铌[J].冶金分析,2019,39(6):70-75.ZHOU Li-xian,WANG Xue-mei.Determination of niobium in vanadium-titanium magnetite by chlorosulfophenol C spectrophotometry[J].Metallurgical Analysis,2019,39(6):70-75.
姜玉领,郭进京,赵慧.电感耦合等离子体原子发射光谱法测定铌铁中的铌、钽、钛[J].铁合金,2019,50(3):45-48.JIANG Yu-ling,GUO Jin-jing,ZHAO Hui.Determination of niobium, tantalum and titanium in ferroniobium by inductively coupled plasma atomic emission spectrometry[J].Ferro-alloys,2019,50(3):45-48.
[10]
刘宇,魏双.高压消解-电感耦合等离子体质谱法测定铌钽矿石中铌钽含量[J].地质调查与研究,2018,41(3):232-234.LIU Yu,WEI Shuang.Determination of niobium and tantalum in niobium and tantalum ore by high pressure digestion-inductively coupled plasma mass spectrometry[J].Geological Survey and Research,2018,41(3):232-234.
安宝兰.铌铝合金中铌的测定[J].稀有金属材料与工程,2002,31(增刊2):133-136.AN Bao-lan.The determination of niobium in niobium-aluminum alloy[J].Rare Metal Materials and Engineering,2002,31(Z2):133-136.
