松香中杂质元素的质谱分析

发布时间：2018-03-27 12:15

本文选题：松香　切入点：电感耦合等离子体质谱　出处：《光谱学与光谱分析》2017年02期

【摘要】：建立测定松香中16个杂质元素含量的分析方法。松香经乙醇溶解稀释后直接采用电感耦合等离子体质谱(ICP-MS)法测定。高浓度乙醇对等离子体所产生的负载以及有机碳不完全燃烧可能会在采样锥和截取锥孔沉积导致信号逐渐降低,通过优化等离子体的射频功率、载气流量以及样品提升量等仪器的操作条件,增加了等离子体中心通道的温度,提高等离子体的电离效率。采用在等离子体中加入低浓度氧气使有机碳充分燃烧,消除了积碳现象,维持了质谱分析信号的稳定。通过仪器调谐和同位素的选择有效地降低了氧化物和双电荷质谱干扰,避开了大量同量异位素干扰以及多原子离子干扰,利用碰撞/反应池(CRC)技术,分别选用氦碰撞模式和氢反应模式,消除了其余质谱干扰,选择内标元素补偿了样品与标准之间的粘度差异来匹配不同基体。结果表明,该方法的检出限在0.002~0.035μg·g~(-1)之间,实际样品的加标回收率为94.00%~106.00%,相对标准偏差(RSD)≤3.34%。方法采用乙醇溶解松香后直接测定,无需专用的样品前处理设备,具有操作简单、分析速度快、灵敏准确等优点,为松香中杂质元素的质量评价提供了一种新的分析方法。
[Abstract]:A method for the determination of 16 impurity elements in rosin was established. The determination of rosin was directly determined by inductively coupled plasma-mass spectrometry (ICP-MS) after ethanol dissolved and diluted. The loading of high concentration ethanol on plasma and the organic content of rosin were determined by inductively coupled plasma mass spectrometry (ICP-MS). Incomplete combustion of carbon may result in a gradual decrease of the signal due to deposition in the sampling cone and the truncated cone hole. By optimizing the operating conditions of the plasma RF power, carrier gas flow rate and sample lift, the temperature of the plasma central channel is increased. Increasing the ionization efficiency of plasma. By adding low concentration of oxygen to plasma, the organic carbon can be fully burned, thus eliminating the phenomenon of carbon accumulation. By means of instrument tuning and isotope selection, the interference of oxide and double charge mass spectrometry is effectively reduced, and a large number of isotopic interference and polyatomic ion interference are avoided. In this paper, the helium collision mode and hydrogen reaction mode are selected by using collision / reaction cell (CRC) technique. The remaining mass interference is eliminated, and the internal standard elements are selected to compensate the viscosity difference between the sample and the standard to match the different matrix. The detection limit of this method is 0.002n 0.035 渭 g / g ~ (-1), the recovery rate of the actual sample is 94.00 ~ 106.00, the relative standard deviation (RSD) is less than 3.34. The method uses ethanol to dissolve rosin and determine rosin directly, without the need of special sample pretreatment equipment, which has the advantages of simple operation and fast analysis. The advantages of sensitivity and accuracy provide a new analytical method for the quality evaluation of impurity elements in rosin.
【作者单位】：湖南工学院材料与化学工程系;长江师范学院化学化工学院;
【基金】：国家自然科学基金项目(21271187) 重庆市自然科学基金项目(cstc2015jcyjA10053,cstc2015jcyjA10038) 湖南省教育厅重点科研资助项目(14A035) 湖南省重点学科建设资助项目(湘教发[2011]76号)资助
【分类号】：O657.63;TQ351.471

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