氟化铵-硝酸微波消解联合ICP-MS对烟用接装纸中7种元素含量的测定

Determination of 7 Elements in Cigarette Tipping Paper by ICP-MS Combined with Decomposition of Ammonium Fluoride-nitric Acid

采用电感耦合等离子体质谱法测定烟用接装纸中7种元素(铅、铬、镉、镍、汞、砷、硒)含量,为了降低传统前处理消解体系带来的安全隐患,建立了更为安全的氟化铵-硝酸微波消解体系,并考察了氟化铵用量、微波消解温度和消解时间对消解效果的影响。结果表明,最佳消解条件为:氟化铵0.75 mL,微波消解温度175℃,消解时间20 min。样品经氟化铵-硝酸消解后,进行电感耦合等离子体质谱测定,各元素检出限为0.007~0.044 mg/kg,样品加标回收率为90.1%~113.1%,相对标准偏差为0.29%~11.43%。采用氟化铵-硝酸消解体系前处理和传统硝酸/氟化氢/盐酸/过氧化氢消解体系前处理对实际样品进行测定,并对两种方法检测各元素值分别进行t检验分析,结果表明,各元素P>0.05,两种方法无显著性差异。

In this study,a method for the determination of 7 elements(Pb,Cr,Cd,Ni,Hg,As,Se)content in cigarette tipping paper of Inductively Coupled Plasma Mass Spectrometry(ICP-MS)was applied.In order to reduce the possible safety hazards caused by traditional pretreatment sample digestion system,a safer ammonium fluoride-nitric acid microwave digestion system was established,and the effects of ammonium fluoride dosage,digestion temperature and decomposition time on the digestion effect were investigated.The results showed that the optimum digestion conditions were 0.75 mL of ammonium fluoride at 175°C for 20 min.After the sample was digested by NH4F-HNO3,it was determined by ICP-MS.The detection limit of each element was in range of 0.007 to 0.044 mg/kg,and the recoveries of standard addition and relative standard deviation of the method were 90.1%to 113.1%and 0.29%to 11.43%,respectively.The actual samples were determined by pretreatment of ammonium fluoride-nitric acid digestion system and traditional HNO3/HF/HCl/H2O2 digestion system,the determined values of each element were carried out by t-test analysis,of which the results showed P>0.05,and there was no significant difference between two methods.