谷物中锗的干灰化-氢化物发生-原子荧光光谱法测定

Determination of Germanium in Grain By Dry Ashing-Hydride Generation-Atomic Fluorescence Spectrometry

建立一种干灰化-氢化物发生-原子荧光光谱法测定谷物中锗的方法。采用控温程序的干灰化为前处理方式,实现谷物中锗的原子荧光光谱法测定。灰化程序:第一步,200℃保持10min;第二步,500℃保持20min的条件下,称样2g的谷物样品灰化效果良好。优化仪器参数和试剂浓度条件,考察灯电流、负高压、载气、酸浓度、还原剂浓度等对锗荧光强度的影响。结果表明,锗元素浓度0~30μg/L,线性相关r为0.999,方法检出限为0.12μg/kg,方法精密度(n=7)在3.9%~5.8%,加标回收率为94.5%~104.5%。该方法操作简单、高效、稳定性良好,适用于谷物中锗的批量检测。

Method for the determination of germanium in grain by dry ashing-hydride generation-atomic fluorescence spectrometry was established.The determination of germanium in grain by atomic fluorescence spectrometry(afs)was realized by dry ash pretreatment with temperature control program.In the ashing process:in the first step,keep it at 200℃for 10min;In the second step,under the condition of keeping at 500℃for 20min,the grain sample of 2g had good ashing effect.The influence of lamp current,negative high voltage,carrier gas,acid concentration and reducing agent concentration on the fluorescence intensity of germanium was investigated.The results showed that the concentration of germanium was 0~30μg/kg,linearly correlated was better than 0.999,the detection limit of the method was 0.12g/K,the method precision(n=7)was between3.9%~5.8%,and the standard recovery was between 94.5%~104.5%.The method is simple,efficient and stable,and is suitable for the bulk detection of germanium in grain.