本文選題：松香　切入點：電感耦合等離子體質(zhì)譜　出處：《光譜學與光譜分析》2017年02期

【摘要】：建立測定松香中16個雜質(zhì)元素含量的分析方法。松香經(jīng)乙醇溶解稀釋后直接采用電感耦合等離子體質(zhì)譜(ICP-MS)法測定。高濃度乙醇對等離子體所產(chǎn)生的負載以及有機碳不完全燃燒可能會在采樣錐和截取錐孔沉積導致信號逐漸降低,通過優(yōu)化等離子體的射頻功率、載氣流量以及樣品提升量等儀器的操作條件,增加了等離子體中心通道的溫度,提高等離子體的電離效率。采用在等離子體中加入低濃度氧氣使有機碳充分燃燒,消除了積碳現(xiàn)象,維持了質(zhì)譜分析信號的穩(wěn)定。通過儀器調(diào)諧和同位素的選擇有效地降低了氧化物和雙電荷質(zhì)譜干擾,避開了大量同量異位素干擾以及多原子離子干擾,利用碰撞/反應池(CRC)技術(shù),分別選用氦碰撞模式和氫反應模式,消除了其余質(zhì)譜干擾,選擇內(nèi)標元素補償了樣品與標準之間的粘度差異來匹配不同基體。結(jié)果表明,該方法的檢出限在0.002~0.035μg·g~(-1)之間,實際樣品的加標回收率為94.00%~106.00%,相對標準偏差(RSD)≤3.34%。方法采用乙醇溶解松香后直接測定,無需專用的樣品前處理設備,具有操作簡單、分析速度快、靈敏準確等優(yōu)點,為松香中雜質(zhì)元素的質(zhì)量評價提供了一種新的分析方法。
[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.
【作者單位】： 湖南工學院材料與化學工程系;長江師范學院化學化工學院;
【基金】：國家自然科學基金項目(21271187) 重慶市自然科學基金項目(cstc2015jcyjA10053,cstc2015jcyjA10038) 湖南省教育廳重點科研資助項目(14A035) 湖南省重點學科建設資助項目(湘教發(fā)[2011]76號)資助
【分類號】：O657.63;TQ351.471

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