索氏提取-原子荧光光谱法测定含油岩心中的汞和砷
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摘要
原油对测定含油岩心中的汞和砷有很大影响,目前去除原油等有机物的方法主要有高温烧制、强酸高温氧化等,要求反应温度较高,会造成汞和砷的损失而使测定结果偏低。本文采用索氏提取法,以氯仿作为提取剂在75℃下低温提取分离岩心中的原油,再用50%的王水溶解剩余样品,原子荧光光谱法测定汞和砷的含量。该方法对汞和砷的检出限分别为0. 003mg/kg和0. 10mg/kg,相对标准偏差分别为7. 3%和5. 1%,加标回收率均大于92. 5%。与传统方法相比较,该方法避免了由于原油的疏水性造成样品与王水接触不充分、样品分解不完全和反应温度过高导致汞元素损失的问题,测定汞的相对标准偏差由33. 0%降低至7. 3%,测定砷的相对标准偏差由25. 0%提高至5. 1%,为含油岩心中其他元素的检测提供了借鉴。
BACKGROUND: Crude oil had a great influence on the determination of mercury and arsenic in oil-bearing cores by atomic fluorescence spectrometry. At present,the main methods of removing organic matter such as crude oil are high-temperature firing and high-temperature oxidation with strong acid. In these methods,high reaction temperature will cause loss of mercury and arsenic,resulting in lower results.OBJECTIVES: To develop a separation method with low operating temperature.METHODS: Mercury and arsenic in oil-bearing cores were determined by atomic fluorescence spectrometry with Soxhlet extraction at a low temperature for this method of 75℃ and the remaining part was decomposed by 50%aqua regia.RESULTS: The detection limits were 0. 003 mg/kg and 0. 10 mg/kg for mercury and arsenic,respectively. The relative standard deviations were 7. 3% and 5. 1%,respectively. The relative standard deviation of mercury decreased from 33. 0% to 7. 3%,and the relative standard deviation of arsenic decreased from 25. 0% to 5. 1%.The recoveries of standard addition were greater than 92. 5%.CONCLUSIONS: Compared with traditional methods,this method avoided the problems of insufficient contact between samples and aqua regia due to the hydrophobicity of crude oil,incomplete decomposition of samples and mercury loss due to excessive reaction temperature. The proposed method provides a reference for the determination of other elements in oil-bearing cores.
BACKGROUND: Crude oil had a great influence on the determination of mercury and arsenic in oil-bearing cores by atomic fluorescence spectrometry. At present,the main methods of removing organic matter such as crude oil are high-temperature firing and high-temperature oxidation with strong acid. In these methods,high reaction temperature will cause loss of mercury and arsenic,resulting in lower results.OBJECTIVES: To develop a separation method with low operating temperature.METHODS: Mercury and arsenic in oil-bearing cores were determined by atomic fluorescence spectrometry with Soxhlet extraction at a low temperature for this method of 75℃ and the remaining part was decomposed by 50%aqua regia.RESULTS: The detection limits were 0. 003 mg/kg and 0. 10 mg/kg for mercury and arsenic,respectively. The relative standard deviations were 7. 3% and 5. 1%,respectively. The relative standard deviation of mercury decreased from 33. 0% to 7. 3%,and the relative standard deviation of arsenic decreased from 25. 0% to 5. 1%.The recoveries of standard addition were greater than 92. 5%.CONCLUSIONS: Compared with traditional methods,this method avoided the problems of insufficient contact between samples and aqua regia due to the hydrophobicity of crude oil,incomplete decomposition of samples and mercury loss due to excessive reaction temperature. The proposed method provides a reference for the determination of other elements in oil-bearing cores.
引文
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[2]阮东亮，盘思伟，韦正乐，等．砷对商业V2O5-WO3/Ti O2催化剂脱硝性能的影响[J]．化工进展，2014,33(4):925-929.Ruan D L,Pan S W,Wei Z L,et al. Effect of arsenic on de-NO efficiency over commercial V2O5-WO3/Ti O2catalyst[J]. Chemical Industry and Engineering Progress,2014,33(4):925-929.
[3]周曙光，周克法，王金林，等．基于晕状特征提取的化探异常信息识别及其在成矿预测中的应用[J]．干旱区地理，2015,38(7):763-769.Zhou S G,Zhou K F,Wang J L,et al. Identifying of geochemical anomalies according to the Halo pattern of trace elements for mineral exploration[J]. Arid Land Geography,2015,38(7):763-769.
[4]尚玉俊，王秀莉，宋丹丹，等．萃取分离-碘量自动电位滴定法测定三氧化二锑中砷[J]．冶金分析，2016,36(3):31-34.Shang Y J,Wang X L,Song D D,et al. Determination of arsenic in antimony trioxide by automatic potentiometric-iodometry with extraction separation[J]. Metallurgical Analysis,2016,36(3):31-34.
[5]孙蕾，郭金喜．LC-AFS法测定新疆阿勒泰狗鱼中的无机汞、甲基汞、乙基汞[J]．食品工业，2018,39(3):325-327.Sun L,Guo J X. Determination of inorganic mercury,methylmercury,ethylmercury in Xinjiang Aletai Pike by LC-AFS[J]. The Food Industry,2018,39(3):325-327.
[6]陕红，袁志华，刘丹丹，等．HPLC-ICP-MS法测定农业废水中有机砷与无机砷的方法研究[J]．农业资源与环境学报，2014,31(2):197-201.Shan H,Yuan Z H,Liu D D,et al. Analysis of organic and inorganic arsenic in waste water of agricultural environment by high performance liquid chromatography and inductively coupled plasma mass spectrometry[J].Journal of Agricultural Resources and Environment,2014,31(2):197-201.
[7]黄会秋，黄莉来，夏坪，等．水相衍生-气相色谱-质谱法同时测定水产品中甲基汞和无机砷[J]．色谱，2016,34(9):918-924.Huang H Q,Huang L L,Xia P,et al. Simultaneous determination of methylmercury and inorganic arsenics in aquatic products by gas chromatography-mass spectrometry with aqueous derivatization[J]. Chinese Journal of Chromatography,2016,34(9):918-924.
[8]杜米芳，聂富强，杜丽丽，等．电感耦合等离子体原子发射光谱法测定船用钢中砷锡锑[J]．冶金分析，2017,37(2):70-75.Du M F,Nie F Q,Du L L,et al. Determination of arsenic,tin and antimony in steel for ship by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2017,37(2):70-75.
[9]杨理勤，陈占生，谢璐，等．卡林型金矿金砷成分分析标准物质研制[J]．岩矿测试，2018,37(2):209-216.Yang L Q,Chen Z S,Xie L,et al. Preparation of gold and arsenic certified reference materials for chemical composition analysis in Carlin-type gold deposits[J].Rock and Mineral Analysis,2018,37(2):209-216.
[10]苟体忠，张文华，王艳，等．微波消解-氢化物发生-冷原子荧光光谱法快速测定水系沉积物中的总汞[J]．分析试验室，2015,34(12):1457-1459.Gou T Z,Zhang W H,Wang Y,et al. Rapid determination of total mercury contents in aquo-system sediment by microwave digestion and hydride generation-cold atomic fluorescence spectrometry[J]. Chinese Journal of Analysis Laboratory,2015,34(12):1457-1459.
[11] Kumar K R,Madhavi K,Shyamala P,et al. A novel synergetic salt-and acid-induced ligandless mixed micelle cloud point extraction of ultratrace levels of Cd,Hg,Bi,and Tl from petrochemical effluents followed by ETAAS determination[J]. Atomic Spectroscopy,2018,39(3):118-125.
[12] Suvarapu L N,Baek S O. Recent studies on the speciation and determination of mercury in different environmental matrices using various analytical techniques[J]. International Journal of Analytical Chemistry,2017,2017:3624015.
[13] Yuksel B,Arica E. Assessment of toxic,essential,and other metal levels by ICP-MS in Lake Eymir and Mogan in Ankara,Turkey:An environmental application[J].Atomic Spectroscopy,2018,39(5):179-184.
[14]吕天峰，袁懋，吕怡兵．测汞仪直接测定空气颗粒物中的总汞[J]．中国测试，2016,42(12):42-44.LüT F,Yuan M,LüY B. Direct determination of total mercury in air particulates by mercury analyzer[J].China Measurement&Test,2016,42(12):42-44.
[15]聂黎行，张烨，朱俐，等．便携式X射线荧光光谱快速无损分析牛黄清心丸(局方)中汞、砷含量及均匀度[J]．光谱学与光谱分析，2017,37(10):3225-3228.Nie L X,Zhang Y,Zhu L,et al. Fast nondestructive analysis of content of mercury and aesenic and homogeneity of Niuhuang Qinxin pills by portable X-ray florescence spectrometry[J]. Spectrometry and Spectral Analysis,2017,37(10):3225-3228.
[16]苏明跃，臧世阳，冯爽，等．顺序注射-氢化物发生-原子荧光光谱法测定矿石中砷和汞含量[J]．理化检验(化学分册)，2013,49(8):943-945.Su M Y,Zang S Y,Feng S,et al. Sequential injectionHG-AFS determination of arsenic and mercury in ores[J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2013,49(8):943-945.
[17]倪润祥，雒昆利．湿消解-原子荧光法测定煤中硒和砷[J]．光谱学与光谱分析，2015,35(5):1404-1408.Ni R X,Luo K L. Deterniation of total selenium and arsenic in coal by wet digestion hydride generation atomic fluorescence spectrometry(HG-AFS)[J].Spectroscopy and Spectral Analysis,2015,35(5):1404-1408.
[18]于跃，高亚丽，赵雪，等．悬浮颗粒物浓度对溢油沉潜过程影响的试验研究[J]．海洋环境科学，2017,36(6):858-863.Yu Y,Gao Y L,Zhao X,et al. A laboratory study on the effect of suspended particulate matter concentration on the submerging and sinking process of oil spill[J].Marine Environment Science,2017,36(6):858-863.
[19]罗荣根．应用固体测汞仪直接测定载金炭中的总汞[J]．岩矿测试，2016,35(4):420-424.Luo R G. Detrermination of total mercury in gold-loaded carbon by solid mercury analyzer[J]. Rock and Mineral Analysis,2016,35(4):420-424.
[20]杨常青，张双双，吴楠，等．微波消解-氢化物发生原子荧光光谱法和质谱法测定高有机质无烟煤中汞砷的可行性研究[J]．岩矿测试，2016,35(5):481-487.Yang C Q,Zhang S S,Wu N,et al. Feasibility study on content determination of mercury and arsenic in high organic anthracite by microwave digestion-hydride generation-atomic fluorescence spectrometry and mass spectrometry[J]. Rock and Mineral Analysis,2016,35(5):481-487.
[21]刘景龙，罗守娟．原子荧光光谱法测定汞标准系列溶液稳定性的探讨[J]．中国无机分析化学，2018,8(4):61-64.Liu J L,Luo S J. Determination of the mercury standard solution serious stability by atomic fluorescence spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry,2018,8(4):61-64.
[22]江朝华，陈旭明．茶叶及大米中有机氯农药残留量前处理方法的研究[J]．包装与食品机械，2018,36(3):59-61.Jiang C H,Chen X M. Research on the pretreatment methods for determination of residual organochlorine pesticides in tea and rice[J]. Packaging and Food Machinery,2018,36(3):59-61.
[23]袁永海，尹昌慧，元志红，等．氢化物发生-原子荧光光谱法同时测定锡矿石中砷和锑[J]．冶金分析，2016,36(3):39-43.Yuan Y H,Yin C H,Yuan Z H,et al. Determination of arsenic and antimony in tin ore by hydride generationatomic fluorescence spectrometry[J]. Metallurgical Analysis,2016,36(3):39-43.
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