分光光度法测定钼精矿焙烧样中铼

Spectrophotometric Determination of Rhenium in Roasted Sample of Molybdenum Concentrate

采用分光光度法测定钼精矿焙烧样中铼的含量。优化的试验条件如下:(1)测定波长为426nm;(2)在盐酸(1+1)溶液中显色;(3)350g·L^(-1)硫氰酸钾溶液的用量为1.0mL;(4)20g·L^(-1)氯化亚锡溶液的用量为1.0mL;(5)硫酸的用量为3mL;(6)加热温度为85℃;(7)加热时间为1.5h;(8)铼试剂的用量为1.0 mL;(9)样品溶液的pH为9左右。铼的质量浓度在3.0~30.0mg·L^(-1)内与其对应的吸光度呈线性关系,方法的检出限(3s/k)为1.0mg·L^(-1)。方法应用于钼精矿焙烧样的分析,测定值与电感耦合等离子体原子发射光谱法测定结果相符,测定值的相对标准偏差(n=7)为1.1%~2.2%。用标准加入法进行回收试验,测得回收率为94.0%~106%。

Spectrophotometry was applied to the determination of rhenium in roasted sample of molybdenum concentrate. The optimized conditions found were as follows： （1） wavelength of determination was 426 nm; （2） coloration in HCl （1＋1） solution; （3） amount of 350 g · L -1 potassium rhodanate solution was 1.0 mL; （4） amount of 20 g · L -1 stannous chloride solution was 1.0 mL; （5） amount of H2SO4 was 3 mL; （6） heating temperature was 85 ℃ ; （7） heating time was 1.5 h; （8） amount of rhenium reagent was 1.0 mL; （9） pH of the sample solution was about 9. Linear relationship between values of absorbanee and mass concentration of rhenium was obtained in the range of 3. 0--30. 0 mg· L -1, with detection limit （3s/k） of 1.0 mg · L-1. The proposed method was applied to the analysis of roasted sample of molybdenum concentrate, giving results in consistency with the values obtained by ICP-AES with RSD＇s （n=7） in the range of 1.1%--2. 2%. Test for recovery was performed by standard addition method, giving values of recovery in the range of 94. 0%--106%.