Determination of trace mercury in liquefied petroleum gas by inductively coupled plasma mass spectrometry after enrichment with resin
ZHONG Sheng-hui1,2, YAN Wei-shan1, WANG Hong-ying3, CHENG Nan-nan1
1. Oriental Energy (Ningbo) New Material Co., Ltd., Ningbo 315812, China; 2. School of Petrochemical Engineering,Changzhou University, Changzhou 213164, China; 3. Oriental Energy Co., Ltd., Nanjing 210042, China
Abstract：The propane dehydrogenation technology receives more and more attention. The control of mercury content in raw material liquefied petroleum gas (LPG) is the key step for the production. Therefore, it is imperative to develop a high-efficiency and stable method for the detection of mercury. Mercury in LPG was on-line enriched using cation exchange resin. After wet digestion with 20% (volume fraction, similarly hereinafter) aqua regia, the determination method of mercury in LPG by inductively coupled plasma mass spectrometry (ICP-MS) was established. The enrichment conditions and digestion methods were optimized. The on-line enrichment conditions for mercury were obtained as follows: pressure of 1.3MPa and flow rate of 500mL/h. The digestion procedures of sample were found as below: 50mL of 20% aqua regia was added into 12g of sample followed by digestion at 60℃ for 1h. The matrix effect was corrected using the matrix matching standard solution. The MS interference was eliminated using 202Hg as the isotope for determination. The results showed that the linear range of method was 0.08-50μg/L, the linear correlation coefficient was 0.999795, and the detection limit was 0.02μg/L. The proposed method was applied for the analysis of mercury in actual LPG sample. The relative standard deviations (RSD, n=5) of measured results were between 1.3% and 6.6%. The recoveries were between 95% and 101%.
钟升辉, 严维山, 王红英, 程南南. 树脂富集-电感耦合等离子体质谱法测定液化石油气中痕量汞[J]. 冶金分析, 2018, 38(5): 30-34.
ZHONG Sheng-hui, YAN Wei-shan, WANG Hong-ying, CHENG Nan-nan. Determination of trace mercury in liquefied petroleum gas by inductively coupled plasma mass spectrometry after enrichment with resin. , 2018, 38(5): 30-34.
韩香莲.丙烯生产工艺研究进展[J].山东化工,2013,42(5):60-62.HAN Xiang-lian.Development of propylene production technology[J].Shangdong Chemical Industry,2013,42(5):60-62.
[2]
陈硕,王定博,吉媛媛,等.丙烯为目的产物的技术进展[J].石油化工,2011,40(2):217-224.CHEN Shuo,WANG Ding-bo,JI Yuan-yuan,et al.Development in on-purpose propylene technology[J].Petrochenical Technology,2011,40(2):217-224.
[3]
付磊.烷烃脱氢制烯烃技术及工艺比较[J].辽宁化工,2016,45(9):1210-1212.FU Lei.Preparation technology of olefin from alkane by dehydrogenation and comparison of different processes[J].Liaoning Chemical Industry,2016,45(9):1210-1212.
[4]
舒凤,张远志,王宏磊,等. ICP-MS测定汞的记忆效应的研究[J].中国卫生检验杂志,2016,26(2):189-191.SHU Feng,ZHANG Yuan-zhi,WANG Hong-lei,et al.Research on the memory effect of determining mercury by ICP-MS[J].Chinese Journal of Health Laboratory Technology,2016,26(2):189-191.
[5]
靳兰兰,王秀季,李会来,等.电感耦合等离子体质谱技术进展及其在冶金分析中的应用[J].冶金分析,2016,36(7):1-14.JIN Lan-lan,WANG Xiu-ji,LI Hui-lai,et al.Progress in inductively coupled plasma mass spectrometry technology and its application in metallurgical analysis[J].Metallurgical Analysis,2016,36(7):1-14.
[6]
庄美华,朱辉忠,蔡伟星,等.应用ICP-MS分析汽油中微量的砷、汞、铅[J].分析测试技术与仪器,2005(4):300-302.ZHUANG Mei-hua,ZHU Hui-zhong,CAI Wei-xing,et al.Determination of trace arsenic,mercury and lead in gasoline by ICP-MS[J]. Analysis and Testing Technology and Instruments,2005(4):300-302.
[7]
张秀武,李永华,杨林生,等.温控湿法消解ICP-MS测定全血中铅镉硒砷汞5种微量元素[J].光谱学与光谱分析,2010,30(7):1972-1974.ZHANG Xiu-wu,LI Yong-hua,YANG Lin-sheng,et al.Determination of five trace elements (Pb,Cd,Se,As and Hg) in human whole blood by temperature-controllable wet digestion and ICP-MS technique[J].Spectroscopy and Spectral Analysis,2010,30(7):1972-1974.
[8]
王文青,张丽媛,魏宇锋,等. 微波消解/ICP-MS法测定食品级润滑油(脂)中的锑、砷、镉、铅、汞、硒[J].分析试验室,2014,33(12):1430-1433.WANG Wen-qing,ZHANG Li-yuan,WEI Yu-feng,et al.ICP-MS determiatin of hatmful elements of As,Se,Cd,Sb,Hg,Pb in food-grade lubricating oils and greases with microwave digestion[J].Chinese Journal of Analysis Laboratory,2014,33(12):1430-1433.
[9]
王枚博,王柯. ICP-MS法测定化妆品中汞的干扰现象分析及消除[J].香料香精化妆品,2014(6):36-38.WANG Mei-bo,WANG Ke.Analysis and elimination of interference in determination of mercury in cosmetics by ICP-MS[J].Flavour Fragrance Cosmetics,2014(6):36-38.
[10]
胡圣虹,林守麟,刘勇胜,等.等离子体质谱法测定地质样品中痕量稀土元素的基体效应及多原子离子干扰的校正研究[J].高等学校化学学报,2000(3):368-372.HU Sheng-hong,LIN Sou-lin,LIU Yong-sheng,et al.Studies on the calibration of matrix effects and polyatomic ion for rare earth elements in geochemical samples by ICP-MS[J].Chemical Journal of Chinese Universities,2000(3):368-372.
[11]
田衎,孙自杰,周裕敏,等.电感耦合等离子体质谱法分析高纯金属银中痕量杂质元素[J].冶金分析,2016,36(7):51-55.TIAN Kan,SUN Zi-jie,ZHOU Yu-min,et al.Determination of trace impurity elements in high purity metal silver by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(7):51-55.
[12]
Berglund M,Wieser M E.Isotopic compositions of the elements 2009(IUPAC Technical Report)[J].Pure and Applied Chemistry,2011,83(2):397-410.
