微波消解—常压消解—电感耦合等离子体质谱法测定植物样中的锗

Determination of Germanium in Plant Samples by Microwave Digestion-Atmospheric Pressure Digestion-Inductively Coupled Plasma Mass Spectrometry

准确测定植物样中锗的含量对于探究其在环境体系中的迁移转化规律具有重要意义。采用微波消解—常压消解前处理方式,建立电感耦合等离子体质谱法测定植物样中锗含量的方法。采用微波消解—常压消解方式提高锗的溶出率;对硫酸、氢氟酸用量及常压消解时间进行优化,进一步改善方法的分析性能;通过数学校正模型扣除仪器测定过程中存在的干扰,保证测试结果准确可靠。研究结果表明,方法检出限为0.59 ng/g,测定下限为2.36 ng/g,方法精密度(RSD,n=8)为4.51%~11.6%。采用该方法对6种不同类型的生物国家一级标准物质进行分析,测定结果的相对误差|RE|≤13.7%,满足植物样中痕量锗的测定要求。

Accurate determination of germanium content in plant samples has great significance for exploring its migration and transformation in environmental system.Microwave digestion-atmospheric pressure digestion was used as pretreatment,and the method for the determination of germanium in plant samples by ICP-MS was established.Microwave digestion and atmospheric pressure digestion was used to improve the dissolution rate of germanium.The amount of sulfuric acid,hydrofluoric acid and the atmospheric digestion time were optimized to further improve the analytical performance of the method;the interference existing in the measurement process of the instrument was deducted through the mathematical correction model to ensure the accuracy and reliability of the test results.Research results showed that the limit of detection of the method was 0.59 ng/g,the lower limit of determination was 2.36 ng/g,and the relative standard deviation(RSD,n=8)was 4.51%-11.6%.The method was used to analyze six different types of national first-class biological reference materials.The relative error of the determination results was|RE|≤13.7%,which met the requirements for the determination of trace germanium in plant samples.