丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析  

Analysis of Ultra-Trace Metal Impurity Elements in Proprylene Glycol Monomethyl Ether Using Inductively Coupled Plasma Tandem Mass Spectrometry

作　　者：李坦平[1] 李爱阳[1] LI Tan-ping;LI Ai-yang(New Building Materials Academy,Hunan Institute of Technology,Hengyang421002,China)

机构地区：[1]湖南工学院新型建筑材料研究院,湖南衡阳421002

出　　处：《光谱学与光谱分析》2021年第2期618-623,共6页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(81603400);湖南省自然科学基金项目(2019JJ60026);湖南省应用特色学科材料科学与工程学科(湘教通[2018]469号)资助。

摘　　要：基于电感耦合等离子体串联质谱(ICP-MS/MS)建立了准确测定丙二醇甲醚中超痕量金属杂质元素的分析方法,提出了利用混合反应气消除质谱干扰的新策略。丙二醇甲醚经超纯水稀释后直接采用ICP-MS/MS测定其中具有挑战性的超痕量金属元素Mg,Al,K,Ti,V,Cr,Fe,Ni,Cu和Zn,在MS/MS模式下,选择混合气NH 3/He/H 2为反应气,Ti^+,Cr^+,Fe^+,Ni^+,Cu^+,Zn^+与NH3发生质量转移反应,在形成的团簇离子中,Ti(NH3)+6,Cr(NH3)+2,Fe(NH3)+2,Ni(NH3)+3,Cu(NH3)+2和Zn(NH3)+丰度高且无干扰,利用NH 3质量转移法将Ti^+,Cr^+,Fe^+,Ni^+,Cu^+和Zn^+转移为相应的团簇离子进行测定;H2能与加合物—NH和—NH2反应生成—NH3,增大碰撞/反应池(CRC)内—NH3的浓度,有利于提高Ti,Cr,Fe,Ni,Cu和Zn的分析灵敏度。Mg^+,Al^+,K^+和V^+几乎不能与NH 3反应,而干扰离子能与NH 3反应形成团簇离子,可以利用NH 3原位质量法进行Mg,Al,K,V的测定;H 2能快速与Ar基干扰离子发生反应,而与其他离子的反应速度很慢,反应气中加入H 2能迅速彻底消除Ar基干扰离子所形成的质谱干扰,有利于Mg,Al,K和V的测定。优选Sc+与NH 3反应生成的团簇离子Sc(NH3)+5为Ti(NH3)+6,Cr(NH3)+2,Fe(NH3)+2,Ni(NH3)+3,Cu(NH3)+2和Zn(NH3)+的内标离子,Be+与NH3反应生成的团簇离子Be(NH3)+4为Mg^+,Al^+,K^+和V^+内标离子,校正了样品溶液,标准溶液和空白溶液之间由于物理化学性质差异产生的基体效应,确保了分析信号的稳定。将所建立的方法应用实际样品的加标回收实验,并采用双聚焦扇形磁场电感耦合等离子体质谱(SF-ICP-MS)进行对比分析,评价分析方法的准确性。结果表明,各元素的检出限为0.52~61.5 ng·L^-1,加标回收率为95.6%~104.2%,相对标准偏差(RSD)≤4.5%;在95%的置信度水平,所有元素的分析结果与SF-ICP-MS的测定结果无显著性差异,验证了分析方法的准确性好,精密度高。将方法应用于丙二醇甲醚中超痕量金属杂质元素的测定,具�Based on inductively coupled plasma tandem mass spectrometry(ICP-MS/MS),an analytical method for the accurate determination of ultra-trace metal impurity elements in propylene glycol methyl ether(PGME)was established,and mixed reaction gas was used to eliminate the spectral interference.The challenging ultra-trace metal elements including Na,Mg,Al,Ti,V,Cr,Fe,Ni,Cu,and Zn in diluted PGME were determined directly by ICP-MS/MS.In the MS/MS mode,the mixed gas NH3/He/H2 was selected as the reaction gas.Ti^+,Cr^+,Fe^+,Ni^+,Cu^+,Zn^+and NH3 undergo mass shift reactions.Among the large number of cluster ions formed,Ti(NH 3)+6,Cr(NH3)+2,Fe(NH3)+2,Co(NH3)+2,Ni(NH3)+3,Cu(NH3)+2,Zn(NH 3)+have high abundances and interference-free,Ti^+,Cr^+,Fe^+,Ni^+,Cu^+,Zn^+can be transferred to the corresponding cluster ions for determination by NH3 mass shift method.H2 can react with the adducts-NH and-NH2 to form-NH3.Increasing the concentration of-NH3 in the collision/reaction cell(CRC)will help to improve the analytical sensitivity of Ti,Cr,Fe,Ni,Cu,Zn.Mg^+,Al^+,K^+,V+can hardly react with NH 3,and the interference ions can react with NH3 to form cluster ions.The NH3 on-mass method can be used to determine the contents of Mg,Al,K,and V.Argide ions react with H2 at a relatively fast rate,while nearly all elemental ions exhibit low reactivity with H2.Therefore,the addition of H2 to the reaction gas can quickly and completely eliminate the spectral interference caused by Argide ions,which is beneficial to the determination of Mg,Al,K,and V.The cluster ions Sc(NH3)+5 generated by the reaction between Sc+and NH3 were selected as the standard internal ions of Ti(NH3)+6,Cr(NH3)+2,Fe(NH3)+2,Ni(NH3)+3,Cu(NH3)+2,and Zn(NH3)+.The cluster ions Be(NH3)+4 generated by the reaction between Be+and NH3 were selected as the standard internal ions of Mg^+,Al^+,K^+,and V^+.The matrix effect caused by the difference of physical and chemical properties between sample solution,standard solution and the blank solution was corrected to ensure the stability of

关 键 词：电感耦合等离子串联质谱 丙二醇甲醚 金属杂质元素 碰撞反应池技术 NH3/He/H2 

分 类 号：O657.63[理学—分析化学]