负载苯基荧光酮纤维富集-GFAAS法测定痕量锗

Filter Coated with Phenyl Fluorone for Enrichment and Determination of Trace Germanium by GFAAS

将负载苯基荧光酮（PF）滤纸纤维用于石墨炉原子吸收光谱法（GFAAS）测定痕量锗的预富集。对锗的富集条件、解吸条件和测定条件进行了研究，在pH=2的含Ge待富集液中，放入负载PF滤纸纤维，在60℃下搅拌60min，过滤洗涤后，加入5．0mL浓HNO3微波消解富集锗的负载PF滤纸纤维，得到含Ge清液，以镧作为基体改进剂，涂钨热解石墨管测定。检出限为0.20μg／L，回收率为95．2％-104％，RSD为2．3％-11.8％，结果满意。测定锌精矿和国家标准物质（GSS．6和GSR-5）中的Ge与推荐值吻合。

Filter fiber coated with phenyl fluorone was utilized to pre-concentrate trace amount of Germanium for determination by GFAAS. The conditions of measurement, enrichment and desorption were explored. The fibers was soaked in the pregnant solution containing trace amount of Germanium （pH = 2 ） and stirred for 60 min at 60 ℃, and then the fibers were filtered and washed. A clear solution was attained after the fibers were treated with 5.0 mL of HNO3 （98%） in a microwave digester. With pyrolytic graphite tube coated with tungsten and lanthanum as a matrix modifier, Germanium in the solution was measured by GFAAS, resulting in satisfactory results. The detection limit was 0. 20 μg/L, the recovery was in the range of 95.2% - 104% , and the RSD was between 2. 3% - 11.8%. Germanium contents in zinc headings and national standard reference samples GSS-6 and GSR-5 were measured with the established method, with good agreements with the recommended values.