原子荧光光度法测定固体废弃物中总锡量的研究

Determination of the content of total tin in solid waste by atomic fluorescence spectrometry

建立以氢氟酸—盐酸—硝酸为消解体系,运用原子荧光光度计测定固体废弃物中总锡质量分数的分析方法。比较不同酸介质、还原剂及掩蔽剂的试验效果,得出最佳的工作条件下,该方法锡元素校准曲线的相关系数稳定在0.9998,检出限为0.06 mg/kg。对GSS-4a平行测定8次计算得RSD=3.58%;选取从低到高4种不同锡质量分数的标准样品测得结果的相对误差为-3.85%~4.11%;在8、4和2μg/L 3种加标量下,方法的加标回收率在93.7%~107.0%之间。该方法检出限低、稳定性高、操作性强,可满足实验室检测固体废弃物中总锡的质量分数,提高检测效率,适用于日常大批量分析样品的要求。

An analytical method for the determination of the mass fraction of total tin in solid waste by atomic fluorescence spectrometry using hydrofluoric,acid-hydrochloric,and acid-nitric as the digestion system was established.Comparing the experimental effects of different acid media,reducing agents and masking agents,the correlation coefficient of the calibration curve of this method for elemental tin was stable at 0.9998 under optimal working conditions,and the limit of detection(LOD)was 0.06 mg/kg.The RSD of the GSS-4a was calculated to be 3.58%for eight parallel determinations.The relative errors of four standard samples with different mass fractions of tin from low to high are-3.85%~4.11%.The recoveries of the method ranged from 93.7%to 107.0%at three spiked levels of 8μg/L,4μg/L and 2μg/L.The method has a low detection limit,high stability and high operability,which can meet the requirements of laboratory detection of the mass fraction of total tin in solid waste,improve detection efficiency,and is suitable for the daily analysis of large quantities of samples.