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以分光光度法为检测手段,采用苯基荧光酮测定铌钽矿中Ta,对反应条件进行了实验及优化:铌钽矿石经碱熔融预处理后,甲基异丁基酮分离Ta,以酒石酸作为辅助络合剂,在表面活性剂氯化十六烷基吡啶存在下,控制温度在20℃,苯基荧光酮与Ta发生灵敏的显色反应。络合物的摩尔吸光系数为2.42×105L·mol-1·cm-1,其最大吸收波长为526 nm,与试剂空白溶液相比,发生了65 nm红移,且Ta质量浓度在0.16~0.80μg/mL范围内符合比尔定律,线性回归方程为A=1.3938ρ-0.030,相关系数为0.9992。常量的Mg2+,Sr2+,Ba2+,Fe3+,Pb2+等对Ta的测定几乎不干扰,方法已应用于铌钽矿中Ta的测定。
By means of spectrophotometry, the determination of Ta in niobium-tantalum ore by phenylfluorone was carried out. The reaction conditions were optimized and experimentally studied. After pretreatment of niobium-tantalum ore by alkali fusion, Ta was separated by methyl isobutyl ketone, As an auxiliary complexing agent, phenylfluorone reacted with Ta sensitively in the presence of the surfactant cetylpyridinium chloride at a controlled temperature of 20 ℃. The molar absorption coefficient of the complex was 2.42 × 105 L · mol-1 · cm-1 and its maximum absorption wavelength was 526 nm. Compared with the reagent blank solution, the complex had a 65 nm red shift and the mass concentration of Ta was 0.16 ~ 0.80 Beer’s law was obeyed in the range of μg / mL, the linear regression equation was A = 1.3938ρ-0.030, and the correlation coefficient was 0.9992. The determination of Ta with Mg2 +, Sr2 +, Ba2 +, Fe3 +, Pb2 + and so on has almost no interference. The method has been applied to the determination of Ta in niobium and tantalum ore.