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作 者:钟郑飞 ZHONG Zheng-fei(Sichuan Metallurgical Geological Prospecting Bureau 605 brigade analysis and Testing Center.,MeiShan 620866,China)
机构地区:[1]四川省冶金地质勘查局六〇五大队分析测试中心,四川眉山620866
出 处:《世界有色金属》2018年第16期164-165,共2页World Nonferrous Metals
摘 要:本文研究了微波溶样-硫氰酸盐差示光度法测定钼精矿中高含量钼。在H2SO4浓度为0.72mol/L的酸度下,用9.6g/L抗坏血酸将Mo(Ⅵ)还原为Mo(Ⅴ),以0.09g/LCuSO4为催化剂,Mo(Ⅴ)再与60.72g/L硫氰酸盐显色为橙红色络合物,以钼浓度8μg/mL的显色液为参比制作标准工作曲线,得到的线性方程为y=0.051x-0.3928,R2=0.999,线性范围为8-24μg/mL,检出限为0.1271μg/mL。不同样品测定的RSD分别为:含钼39.206%:0.8%,含钼51.852%:0.5%,含钼59.16%,0.4%。不同样品的测定值与标准值绝对误差均小于0.5%,结果令人满意。The high levels of molybdenum was determined in molybdenum concentrate through microwave digestion and thiocyanate differential spectrophotometry. The optimum conditions were that: the concentration of H2SO4 was 0.72mol / L, 9.6g / L ascorbic acid was used to reduce Mo ( Ⅵ ) to Mo ( Ⅴ ), 0.09g/LCuSO4 was used as catalyst, the concentration of thiocyanate was 60.72g / L. The chromogenic complex with 8μg/mL molybdenum was used as the reference standard. The linear equation was y = 0.051x-0.3928( R2 = 0.999) with the linear range of 8- 4μg/mL. The detection limit was 0.1271μg/mL. The RSD for the different samples were: molybdenum content 39.206%, 0.8%, molybdenum content 51.852%, 0.4%,molybdenum content 59.16%, 0.5%, respectively. The absolute error of different samples were less than 0.5%, the results were satisfactory.
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