微波消解结合ICP-MS测定内衬纸和框架纸中7种元素

目的 基于高压密封微波消解技术,构建一种新型微波消解体系,并将其与电感耦合等离子体质谱(ICP-MS)联用,用于烟用内衬纸和框架纸中铬、镍、砷、硒、镉、汞和铅元素含量的测定.方法 在新的消解体系中,用氟化铵(NH4F)代替传统方法中的氢氟酸(HF),以降低对实验操作人员的危害,并考察不同实验条件对实验结果的影响.结果 最佳消解条件为0.2 g纸质样品在6 mL硝酸和0.5 mL NH4F体系中消解,微波消解程序为温度从室温升至185°C(20 min)保持30 min后降至55°C(20 min);7种元素的标准曲线线性良好(r2>0.9990),检出限低,加样回收率和重现性良好;在检测实际样品时,与传统方法相比,该方法的测定结果无显著性差异(P>0.05).结论 该方法快速准确、安全环保,适合于烟用内衬纸和框架纸中7种元素含量的测定.

Simultaneously Determination of 7 Elements in Inner Lined and Frame Paper by Microwave Digestion Combined with ICP-MS

A new microwave digestion system was successfully constructed based on the high-pressure sealed microwave digestion technology and used in combination with inductively coupled plasma mass spectrometry (ICP-MS) for the determination of Cr, Ni, As, Se, Cd, Hg, and Pbin inner lined and frame paper of cigarettes. In the new digestion system, ammonium fluoride (NH4F) was used instead of hydrofluoric acid (HF) in the conventional method to reduce the hazards in experimental operations and to examine the effects of different experimental conditions on the experimental results.The results showed that optimal conditions were that 0.2 g paper was digested in thesystem of 6 mL HNO3 and 0.5 mL NH4F, and then reacted in the microwave digestion instrument. The temperature program was raised from room temperature to 185 °C for 20 min, kept for 30 min, and then dropt to 55 °C for 20 min. The correlation coefficient (r2) of 7 elements was more than 0.9990, and limits of detection ranged from 0.007 to 0.044 mg/kg. The recoveries and RSD were good. There was no significant difference between the experimental results of this method and the results determined by the traditional method (P>0.05). This method was shown to be fast, accurate, safe, environment friendly, and suitable for analyzing the 7 elements in inner lined and frame paper.