电感耦合等离子体-串联质谱(ICP-MS/MS)法测定道路尘土中的铂族元素(PGEs)含量
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摘要
建立了道路尘土中的铂族元素(platinum group elements,PGEs)含量测定的分析方法。道路尘土以王水(2mL HNO_3+6mL HCl)为混合消解试剂经微波消解后直接测定。在MS/MS模式下向碰撞反应池中通入氧气或氨气,分别利用氧气质量转移、氧气原位质量和氨气原位质量法消除多原子离子质谱干扰。在MS/MS模式下,分别向碰撞/反应池(CRC)中加入O_2和NH_3-He(1∶9,V/V),消除质谱干扰,采用O_2质量转移法对铑进行测定,O_2原位质量法和高氦(HeHe)法对钯进行测定,NH_3原位质量法对铑和铂进行测定。通过分析国际标准参考物质(BCR-723)验证方法的准确性和精密度,所测定结果与参考值基本一致,RSD≤7.8%,表明本方法具有良好的准确性和精密度。本方法具有前处理简单、高灵敏度、无干扰、稳定性好等优势,可用于道路尘土样品中超痕量铂、铑,钯含量的测定。
A method for determination of platinum group elements(PGEs)in road dust was established.The road dust sample was determined directly after microwave digestion by aqua regia(2 mL HNO_3+6 mL HCl).In the MS/MS mode,oxygen or ammonia was injected into the collision reaction pool,and the oxygen in mass-shift,oxygen in on-mass mode and ammonia in onmass mode were used to eliminate the interference of multi-atomic ion mass spectra.Based on the results,under the mode of MS/MS,the collision/reaction pool(CRC)with O_2 and NH_3-He(1∶9,V/V)were used respectively to remove the mass spectrum interference.The method of O_2 mass-shift mode were applied in the determination of rhodium,O_2 in on-mass mode and high helium(HeHe)method were applied for determination of palladium,NH_3 in on-mass method was for determination of rhodium and platinum.The ICP-MS/MS procedure was validated using BCR-723(road dust)as a reference material.The results were in a good agreement with the range of the reference value and RSD≤7.8%,showing that this method has a good accuracy and precision.This method has the advantages of simple pretreatment,high sensitivity,no interference and good stability.It can be used for determination of the content of super trace platinum,rhodium and palladium in road dust samples.
A method for determination of platinum group elements(PGEs)in road dust was established.The road dust sample was determined directly after microwave digestion by aqua regia(2 mL HNO_3+6 mL HCl).In the MS/MS mode,oxygen or ammonia was injected into the collision reaction pool,and the oxygen in mass-shift,oxygen in on-mass mode and ammonia in onmass mode were used to eliminate the interference of multi-atomic ion mass spectra.Based on the results,under the mode of MS/MS,the collision/reaction pool(CRC)with O_2 and NH_3-He(1∶9,V/V)were used respectively to remove the mass spectrum interference.The method of O_2 mass-shift mode were applied in the determination of rhodium,O_2 in on-mass mode and high helium(HeHe)method were applied for determination of palladium,NH_3 in on-mass method was for determination of rhodium and platinum.The ICP-MS/MS procedure was validated using BCR-723(road dust)as a reference material.The results were in a good agreement with the range of the reference value and RSD≤7.8%,showing that this method has a good accuracy and precision.This method has the advantages of simple pretreatment,high sensitivity,no interference and good stability.It can be used for determination of the content of super trace platinum,rhodium and palladium in road dust samples.
引文
[1]邹晓雯,高博,周怀东,等.光谱学与光谱分析,2016,36(4):1202.
[2] M.Moldovan et al.Science of the Total Environment,2002,296:199.
[3] Machado R,Amaral C,Schiavo D,et al.Micro Chemical Journal,2017,130:271.
[2] M.Moldovan et al.Science of the Total Environment,2002,296:199.
[3] Machado R,Amaral C,Schiavo D,et al.Micro Chemical Journal,2017,130:271.