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采用微波消解-电感耦合等离子体-原子发射光谱法(ICP-AES),通过分析回收率,着重研究消解用无机酸(盐酸、硝酸和过氧化氢)对油墨中铅含量测定的影响。盐酸的加入对ICP-AES分析影响较小,但会与铅形成二氯化铅,造成微量损失,回收率下降。硝酸对ICP—AES分析有酸效应,过量硝酸会影响仪器精准性。当过氧化氢用量为1.0-2.0mL时,对回收率基本没有影响。结果表明,6mL硝酸和1mL过氧化氢就可使1.5g油墨消解完全,此时铅的加标回收率为100.7%。实验优化了前处理方法,使结果更加准确可靠。
The effects of digestion inorganic acids (hydrochloric acid, nitric acid and hydrogen peroxide) on the determination of lead in ink were studied by using microwave digestion-inductively coupled plasma atomic emission spectrometry (ICP-AES). The addition of hydrochloric acid has little effect on the ICP-AES analysis, but leads to the formation of lead dichloride with lead, causing slight loss and decreasing the recovery rate. Nitric acid has an acid effect on ICP-AES analysis, with excess nitric acid affecting instrument accuracy. When the amount of hydrogen peroxide is 1.0-2.0mL, the recovery rate of almost no effect. The results showed that 6mL of nitric acid and 1mL of hydrogen peroxide can 1.5g ink digestion completely, this time the recovery of lead was 100.7%. Experiments optimize the pretreatment method to make the result more accurate and reliable.