电感耦合等离子体质谱测定法中汞元素记忆效应与稳定性研究
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摘要
目的探究电感耦合等离子体质谱(ICP-MS)法测定汞元素时加金与不加金对记忆效应和稳定性的影响,以及考察加金量。方法采用ICP-MS测定溶液中汞元素的量。射频功率为1 550 W,载气(高纯氩气)流速为1.05 L·min~(-1),等离子气体流速为15.0 L·min~(-1),蠕动泵转速0.2 r·s~(-1),采样深度8 mm,积分时间为0.1 s。结果汞溶液质量浓度在0.4 ng·m L~(-1)时开始形成较明显的记忆效应;汞溶液在不加任何稳定剂的情况下常温放置超过2 h后逐渐不稳定,相对标准偏差(RSD)逐渐变大,而加入金元素后在48 h内较为稳定,RSD在5%以内;金汞比为2∶1时就能够降低记忆效应,同时很好的保证其稳定性;汞元素标准溶液单独制备与其他元素混合制备并无区别。结论本实验对汞元素检测分析具有参考作用,为相关检测标准方法的修订和提高提供了技术支持。
OBJECTIVE To investigate the effect of adding gold when determing the memory effect and stability of mercury by ICP-MS,and determine the appropriate amount of gold.METHODS ICP-MS method was used to determine the amount of mercury in the solution.The RF power was 1 550 W,flow rate of carrier gas was 1.05 L·min~(-1),plasma gas flow rate was 15.0 L·min~(-1),peristaltic pump speed was 0.2 r·s~(-1),and sampling depth was 8 mm.The integration time was 0.1 s.RESULTS Mercury solution began to demonstrate obvious memory effect at the concentration of 0.4 ng·m L~(-1).It gradually became unstable and the coefficient of variation gradually increased after being placed at room temperature for more than 2 h in the absence of stabilizer.After adding gold,the mercury soulution was stable within 48 h,and the coefficient of variation was within 5%.When the ratio of gold to mercury was2∶1,the memory effect of mercury was decreaed,and its stability was well guaranteed.There was no difference when the mercury standard solution was prepared with or without other elements.CONCLUSION This study plays a reference role in the detection and analysis of mercury and provides technical support for the revision and improvement of relevant detection methods.
OBJECTIVE To investigate the effect of adding gold when determing the memory effect and stability of mercury by ICP-MS,and determine the appropriate amount of gold.METHODS ICP-MS method was used to determine the amount of mercury in the solution.The RF power was 1 550 W,flow rate of carrier gas was 1.05 L·min~(-1),plasma gas flow rate was 15.0 L·min~(-1),peristaltic pump speed was 0.2 r·s~(-1),and sampling depth was 8 mm.The integration time was 0.1 s.RESULTS Mercury solution began to demonstrate obvious memory effect at the concentration of 0.4 ng·m L~(-1).It gradually became unstable and the coefficient of variation gradually increased after being placed at room temperature for more than 2 h in the absence of stabilizer.After adding gold,the mercury soulution was stable within 48 h,and the coefficient of variation was within 5%.When the ratio of gold to mercury was2∶1,the memory effect of mercury was decreaed,and its stability was well guaranteed.There was no difference when the mercury standard solution was prepared with or without other elements.CONCLUSION This study plays a reference role in the detection and analysis of mercury and provides technical support for the revision and improvement of relevant detection methods.
引文
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[18]LI Y F,CHEN H Y,BAI L,et al.Elimination efficiency of different reagents for the memory effect of mercury using ICP-MS[J].J Anal Atom Spectrom,2006,21(1):94-96.
[19]YUAN Y,ZHOU Y,WANG T.Determination of mercury by ICP-MS with L-cysteine and gold[J].Chin J Heal Lab Technol(中国卫生检验杂志),2016,26(14):2025-2029.
[20]DUAN J K,FANG H W,ZHAO Y Y.Study on ascorbic acid signal enhancement for Hg determined by inductively coupled plasma mass spectrometry[J].Chin J Heal Lab Technol(分析测试学报),2017,36(2):284-287.
[21]ZUO T T,LI Y L,JIN H Y,et al.Determination of residues of heavy metals and harmful elements in 18 types of animal medicines by ICP-MS and preliminary risk analysis[J].Chin J Pharm Anal(药物分析杂志),2017,37(2):237-242.
[22]Ch.P(2015)VolⅣ(中国药典2015年版.四部)[S].2015:206-207.
[2]MA S C,JIN H Y,LIU L N,et al.Control of exogenous harmful residues in traditional Chinese medicines[J].Chin Pharm J(中国药学杂志),2015,50(2):99-103.
[3]FAN X,PANG F,ZHANG J D,et al.The study on rapid method for determinationof mercury seafoods[J].J Inspec Quaran(检验检疫学刊),2011,21(1):24-32.
[4]ZHAO P,WU J,SHI L G,et al.Application of measurement standard of mercury in food testing[J].Grain Pro(粮食加工),2011,36(4):85-88.
[5]TANG X P,SUN X G,LIU Y,et al.Research advances in analysis of mercury in textiles[J].China Textile Leader(纺织导报),2013,840(11):80-82.
[6]ZHANG W N,LI C L,LI Y H,et al.Determination of mercury and arsenic in traditional Chinese medicine by hydride generation-atomic fluorescence spectrometry with bomb digestion[J].Chem Anal Met(化学分析计量),2017,26(5):28-31.
[7]ZUO T T,LI Y L,CHEN P,et al.Determination and preliminary risk assessment of heavy metals and harmful elements in American ginseng,the fruit of Chinese wolfberry and hawthorn[J].Chin J Pharm Anal(药物分析杂志),2016,36(11):2016-2021.
[8]CHEN J,QIAO F,JIN H Y,et al.Evaluation of the uncertainty for the determination of heavy metals in Strychni Semen by ICP-MS[J].Chin J Pharm Anal(药物分析杂志),2013,33(12):2176-2179.
[9]ZHANG S X,WEI S Q,YU Y H.Determination of arsenic and mercury in vegetables by double channel atomic fluorescence spectrometer[J].Chin J Inorg Anal Chem(中国无机分析化学),2015,5(1):4-6.
[10]LIU L P,LV C,WANG Y.Investigation of mercury speciation analysis in aquatic products by liquid chromatography-inductively coupled plasma-mass spectrometry[J].J Instr Anal(分析测试学报),2010,29(8):767-771.
[11]MAO H,QIN D Y,GONG L T.Determination of methylmercury,ethylmercury and inorganic mercury in fish by liquid chromatography-atomic fluorescence spectrometry[J].Chin JHeal Lab Technol(中国卫生检验杂志),2010,20(10):2439-2442.
[12]ZONG W L.Determination of methylmercury in grilled fish fillets by gas chromatography-mass spectrometry[J].Life Sci Instrum(生命科学仪器),2014,12(4):45-48.
[13]PENG L,ZHANG M.Mercury detection in plant sample by lowtemperature exposure dissolution-ICP-MS[J].J Anhui Ag Ti Sci(安徽农业科学),2016,44(12):96-138.
[14]SHU F,ZHANG Y Z,WANG H L,et al.Research on the memory effect of determination mercury by ICP-MS[J].Chin J Heal Lab Technol(中国卫生检验杂志),2016,26(2):189-191.
[15]YANG J,WANG Z T,YANG D J.Progress in method of determination of total mercury in foods[J].Chin J Food Hygiene(中国食品卫生杂志),2008,20(4):346-351.
[16]XU P,CHEN M X,MOU R X,et al.Determination of nine trace elements in plant samples by inductively coupled plasma mass spectrometry in mixed mode[J].J Instr Anal(分析测试学报),2011,30(10):1138-1142.
[17]TANG J,ZHANG Z Y,CHEN S J,et al.Accuracy in detecting trace mercury,cadmium,lead and arsenic in various kinds of food using ICP-MS assisted by microwave digestion[J].Chin JPublic Health Eng(中国卫生工程学),2014,13(5):407-413.
[18]LI Y F,CHEN H Y,BAI L,et al.Elimination efficiency of different reagents for the memory effect of mercury using ICP-MS[J].J Anal Atom Spectrom,2006,21(1):94-96.
[19]YUAN Y,ZHOU Y,WANG T.Determination of mercury by ICP-MS with L-cysteine and gold[J].Chin J Heal Lab Technol(中国卫生检验杂志),2016,26(14):2025-2029.
[20]DUAN J K,FANG H W,ZHAO Y Y.Study on ascorbic acid signal enhancement for Hg determined by inductively coupled plasma mass spectrometry[J].Chin J Heal Lab Technol(分析测试学报),2017,36(2):284-287.
[21]ZUO T T,LI Y L,JIN H Y,et al.Determination of residues of heavy metals and harmful elements in 18 types of animal medicines by ICP-MS and preliminary risk analysis[J].Chin J Pharm Anal(药物分析杂志),2017,37(2):237-242.
[22]Ch.P(2015)VolⅣ(中国药典2015年版.四部)[S].2015:206-207.