电感耦合等离子体原子发射光谱法测定再生锌原料中锗

Determination of germanium in regenerated zinc materials by inductively coupled plasma atomic emission spectrometry

再生锌原料中含锌烟尘、含锌渣常常伴有锗的存在,锗具有很高的回收价值,是贸易结算和金属平衡考察的重要指标。常见锗测定方法测定范围为0.000 1%~0.10%(质量分数,下同)和1%~99%,不满足再生锌原料中0.1%~1%锗的测定。实验提出采用硝酸、磷酸、高锰酸钾和氢氟酸分解样品,样品溶液中加入15mL盐酸进行蒸馏,蒸馏至体积为15~30mL,用7.5%~15%(体积分数)盐酸吸收以四氯化锗形态逸出的锗,使锗与干扰元素分离。仪器工作条件设定为射频(RF)功率1 150W、辅助气流量0.50L/min、雾化气流量0.50L/min、蠕动泵速50r/min,选择Ge 209.426nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锗,从而建立了再生锌原料中锗的测定方法。锗的质量浓度在0.050~5.0μg/mL范围内与发射强度呈线性,相关系数大于0.999 9;方法检出限为0.000 58%。蒸馏过程中带入吸收液中的少量共存元素对测定结果没有影响。按照实验方法测定7种再生锌原料中锗,结果的相对标准偏差(RSD,n=11)为0.41%~2.7%,加标回收率为95%~104%。

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 were0.000 1%-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.15 mL of hydrochloric acid was added into sample solution.The solution was then distilled until the volume was in range of 15-30 mL.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 1 150 W,auxiliary gas flow rate of 0.50 L/min,atomization gas flow rate of 0.50 L/min,and peristaltic pump speed of 50 r/min.Ge 209.426 nm 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 0.999 9.The detection limit of method was 0.000 58%.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%.