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采用微波消解和电热板消解2种方法前处理含氧化铁黄基体的油墨样品,再以萃取法去除样品中基体铁元素,最后用等离子发射光谱仪检测样品中Pb含量。该方法解决了以往该类样品中Pb元素检测时高干扰的问题。仪器检出限为0.02 mg/kg,方法检出限为0.08 mg/kg;方法的RSD为0.02;微波消解试验的加标回收率为95.2%,电热板消解试验的加标回收率为90.2%。建议该类产品Pb元素的定量检测采用微波消解法来前处理样品。
The samples containing iron oxide yellow matrix were pretreated by microwave digestion and hot plate digestion, then the matrix iron was removed by extraction method. Finally, the content of Pb in the samples was measured by plasma emission spectrometer. The method solves the problem of high interference in the detection of Pb elements in such samples in the past. The detection limit was 0.02 mg / kg and the detection limit was 0.08 mg / kg. The RSD of the method was 0.02. The spiked recoveries of microwave digestion were 95.2%. The spiked recoveries were 90.2% . It is suggested that the quantitative determination of Pb in these products should be pre-treated by microwave digestion.