Abstract:The zinc-containing dust and zinc-containing slag in regenerated zinc materials usually contain germanium. Germanium had very high recoverable value and it was an important index for trade settlement and metal balance investigation. The determination ranges of germanium in common analysis methods were 0.0001%-0.10% (mass fraction, similarly hereinafter) and 1%-99%, which could not meet the requirements for determination of germanium (0.1%-1%) in regenerated zinc materials. The sample was decomposed with nitric acid, phosphoric acid, potassium permanganate and hydrofluoric acid. 15mL of hydrochloric acid was added into sample solution. The solution was then distilled until the volume was in range of 15-30mL. Germanium was absorbed in form of germanium tetrachloride with 7.5%-15% (volume fraction) hydrochloric acid, realizing the separation of germanium from interference elements. The working conditions of instrument were listed as below: radio frequency (RF) power of 1150W, auxiliary gas flow rate of 0.50L/min, atomization gas flow rate of 0.50L/min, and peristaltic pump speed of 50r/min. Ge 209.426nm was selected as the analytical line. The content of germanium was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently, a determination method of germanium in regenerated zinc materials was established. The mass concentration of germanium in range of 0.050-5.0μg/mL was linear to the corresponding emission intensity. The correlation coefficient was more that 0.9999. The detection limit of method was 0.00058%. Few coexisting elements introduced into absorption solution in distillation process had no influence on the determination results. The content of germanium in seven kinds of regenerated zinc materials was determined according to the experimental method. The relative standard deviations (RSD, n=11) were between 0.41% and 2.7%, and the recoveries were between 95% and 104%.
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