流动注射催化动力学光度法测定痕量锰
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摘要
为了克服温度及加热、冷却时间等因素对测定锰的影响，提出室温下测定痕量锰的新方法，即氨三乙酸(NTA)存在下，在pH5.4的HAc—NaAc缓冲溶液中，锰(Ⅱ)对高碘酸钠氧化季胺[4，4’—对(二甲氨基)—二苯基甲烷]反应有显著的催化作用，并利用流动注射技术分析速度快的特点测定了在602nm处有最大吸收的蓝色不稳定产物。在60样h分析速度下检出限为7.3×10~(-11)g／mL，线性范围为锰(Ⅱ)0～20μg／L，对10μg／L锰标准溶液测定11次的相对标准偏差为0.5％。应用于天然水样测定，结果令人满意。
本文包括以下主要内容：
第一章是绪论部分。简述了流动注射分析技术的基本理论，阐明了实验的催化动力学基本原理和体系的主要特点，并对催化动力学光度法测定锰的体系和应用进行了综述。
第二章是试验部分。主要介绍实验仪器、实验试剂和实验方法。
第三章是结果与讨论部分。首先论述了体系用于流动注射分析的可能性，然后介绍流动注射分析流路设计及试验参数的优化，探讨了反应的机理，最后检验了共存组分对测定的影响并进行了实际样品的测定。为验证方法的准确性和可靠性，对加拿大国家测量标准所的水质标样SLEW-2按本方法进行了测定。
第四章是结论部分。
Trace levels of Mn is determined using flow-injection catalytic kinetic spectrophotometry. Due to the catalytic effects of Mn(II), strongly enhanced by nitrilotriacetic acid, sodium periodate could oxidize tetrabase [4,4'-bis(dimethylamino)-diphenylmethane] rapidly at room temperature in an acetate buffer medium (pH=5.4). Flow injection technique is used to control the merging and reaction timing of the reagents and samples. The measurements are conducted at 602 nm
the unstable blue intermediate product of the reaction, which greatly improves the sample throughput. A detection limit (3 o ) of 0.073 ug/L is achieved at a sampling frequency of 60/h.The relative standard deviation is 0.5% for the determination of 10 ug/L Mn (n=l 1).
The thesis is divided into four chapters.
In the first chapter, a review is provided on the basic theories and advantages of flow injection analysis technique, and the basic principles of catalytic kinetic spectrophotometry and its main characteristics with the emphasis on the applications of manganese analysis by catalytic kinetic spectrophotometry.
Chapter 2 introduces the apparatus, the reagents and the methods used in the present study.
In the Results and Discussion, practical considerations on flow injection systems for the catalytic kinetic analysis of trace amounts of manganese are discussed, leading to the optimized flow injection manifold used in the present study. The possible mechanism of the kinetic reaction is given and discussed. The physical and chemical parameters are optimized and the potential effects of interferences on determination of manganese are examined. The optimized system is validated by the analysis of an estuarine water reference material, SLEW-2 (National Research Council of Canada) and applied to the analyses of several natural waters with satisfactory recoveries.
Chapter 4 summarizes the characteristics of the proposed system.
本文包括以下主要内容：
第一章是绪论部分。简述了流动注射分析技术的基本理论，阐明了实验的催化动力学基本原理和体系的主要特点，并对催化动力学光度法测定锰的体系和应用进行了综述。
第二章是试验部分。主要介绍实验仪器、实验试剂和实验方法。
第三章是结果与讨论部分。首先论述了体系用于流动注射分析的可能性，然后介绍流动注射分析流路设计及试验参数的优化，探讨了反应的机理，最后检验了共存组分对测定的影响并进行了实际样品的测定。为验证方法的准确性和可靠性，对加拿大国家测量标准所的水质标样SLEW-2按本方法进行了测定。
第四章是结论部分。
Trace levels of Mn is determined using flow-injection catalytic kinetic spectrophotometry. Due to the catalytic effects of Mn(II), strongly enhanced by nitrilotriacetic acid, sodium periodate could oxidize tetrabase [4,4'-bis(dimethylamino)-diphenylmethane] rapidly at room temperature in an acetate buffer medium (pH=5.4). Flow injection technique is used to control the merging and reaction timing of the reagents and samples. The measurements are conducted at 602 nm
the unstable blue intermediate product of the reaction, which greatly improves the sample throughput. A detection limit (3 o ) of 0.073 ug/L is achieved at a sampling frequency of 60/h.The relative standard deviation is 0.5% for the determination of 10 ug/L Mn (n=l 1).
The thesis is divided into four chapters.
In the first chapter, a review is provided on the basic theories and advantages of flow injection analysis technique, and the basic principles of catalytic kinetic spectrophotometry and its main characteristics with the emphasis on the applications of manganese analysis by catalytic kinetic spectrophotometry.
Chapter 2 introduces the apparatus, the reagents and the methods used in the present study.
In the Results and Discussion, practical considerations on flow injection systems for the catalytic kinetic analysis of trace amounts of manganese are discussed, leading to the optimized flow injection manifold used in the present study. The possible mechanism of the kinetic reaction is given and discussed. The physical and chemical parameters are optimized and the potential effects of interferences on determination of manganese are examined. The optimized system is validated by the analysis of an estuarine water reference material, SLEW-2 (National Research Council of Canada) and applied to the analyses of several natural waters with satisfactory recoveries.
Chapter 4 summarizes the characteristics of the proposed system.
引文
[1] 徐淑坤，孙励敬，方肇伦．痕量碘的四元碱流动注射分光光度法研究粮食中微量碘的测定．分析实验室，1992，11(4)：16
[2] Zhu, Z.H. and Fang, Z.L. Spectrophotometric determination of total cyanide in waste waters in a flow injection system with gas-diffusion separation and preconcentration. Anal. Chim. Acta, 1987, 198:25
[3] Ruzicka, J. and Hansen, E.H. Flow-injection analyses part Ⅰ: A new concept of fast continuous flow analysis. Anal. Chim. Acta, 1975, 78:145
[4] Ruzicka, J. and Hansen, E.H. Flow Injection Analysis. First edition, John Wiley & Sons, New York, 1981
[5] Ruzicka, J. and Hansen, E.H. Flow Injection Analysis. Second edition, John Wiley & Sons, New York, 1988
[6] Fang, ZL. Non-equilibrated sample manipulation the essence of flow injection analysis. Microchem. J.,1992, 45:137
[7] Ruzicka, J., Hansen, E.H. and Ramsing, A.U. Flow Injection Analyzer for students, teaching and research. Anal. Chim. Acta, 1982, 134:55
[8] Lown, J.A., Koile, R. and Johnson, D.C. Amperometric flow-through wire detector: a practical design with high sensitivity. Anal. Chim. Acta, 1980, 116:33
[9] 孙励敬，方肇伦等．土壤速效磷的流动注射分析．分析化学，1981，9：586
[10] Erickson, B.C., Ruzicka, J. and Kowalski, B. Applications of a versatile injection valve for flow injection analysis. Anal. Chem.,1987, 59:1246
[11] Fang, Z.L., Ruzicka, J. and Hansen, E.H. An efficient flow-injection system with on-line ion-exchange preconcentration for the determination of trace amounts of heavy metals by atomic absorption spectrometry. Anal. Chim. Acta, 1984, 164:23
[12] Wolf, W.R. and Stewart, K.K. Automated multiple flow injection analysis for flame atomic absorption spectrometry. Anal. Chem., 1979, 51:1201
[13] Hansen, E.H., Ruzicka, J. and Ghose, A.K. Flow injection analysis for calcium in serum,water and waste waters by spectrophotometry and by ion-selective electrode.
Anal. Chim. Acta, 1978, 100:151
[14] Nalbach, U., Schiemenz, H., Stamm, W.W. and Kula, M.R. On-line flow-injection monitoring of the enzyme inductor phenylalanine in the continuous cultivation of rhodococcus SP. M_4. Anal. Chim. Acta, 1988, 213:55
[15] Ahira, M., Arai, M. and Tomitsugu, T. Flow injection spectrofluorimetric determination of tebium (Ⅲ) based on solubilizing its tetnary complex in micellar solution. Anal. Lett., 1986, 19:1907
[16] Steig, S. and Nieman, T.A. Experimental and theoretical considerations of low cell design in analytical chemiluminescence. Anal. Chem., 1978, 50:401
[17] Burguera, J.L., Townshend, A. and Greenfield, S. Flow injection analysis for monitoring chemiluminescent reactions. Anal. Chim. Acta, 1980, 114:209
[18] Mullin, J.L. and Seitz, W.R. Two-phase flow cell for chemiluminescence and bioluminescence measurements. Anal. Chem., 1984, 56:1046
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[21] Fang, Z.L. and Xu, S.K. Petermination of molybdenum at ug.L~(-1) levels by catalytic spectrophotometric flow injection analysis. Anal. Chim. Acta, 1983, 145: 143
[22] Fan, S.H., Muller, W.H., Schweizer, B. and Bohme, W. Fourth International Symposium on Kinetics in Analytical Chemistry, Erlangen, 1992
[23] Ruzicka, J. and Marshall, GD. Sequential injection: a new concept for chemical sensors, process analysis and laboratory assays. Anal. Chim. Acta, 1990, 237:329
[24] Quintero, M.C., Silva, M. and Perez-Bendito, D. Evaluation of the analytical use of the manganese-catalysed malachite green-periodate reaction by the stopped-flow technique. Talanta, 1989, 36:1091
[25] Zolotov, Yu.A., Shpigun, L.K. and Kolotyrkina, I.Ya. The trace determination of some heavy metals in waters by flow- injection spectrophotometry and potentiometry. Anal.
Chim. Acta, 1987, 200:21
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[34] 李锦昕，刘国钧．流动注射催化光度法测定地质样品中痕量锰．岩矿测试，1997，16(1)：57
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[2] Zhu, Z.H. and Fang, Z.L. Spectrophotometric determination of total cyanide in waste waters in a flow injection system with gas-diffusion separation and preconcentration. Anal. Chim. Acta, 1987, 198:25
[3] Ruzicka, J. and Hansen, E.H. Flow-injection analyses part Ⅰ: A new concept of fast continuous flow analysis. Anal. Chim. Acta, 1975, 78:145
[4] Ruzicka, J. and Hansen, E.H. Flow Injection Analysis. First edition, John Wiley & Sons, New York, 1981
[5] Ruzicka, J. and Hansen, E.H. Flow Injection Analysis. Second edition, John Wiley & Sons, New York, 1988
[6] Fang, ZL. Non-equilibrated sample manipulation the essence of flow injection analysis. Microchem. J.,1992, 45:137
[7] Ruzicka, J., Hansen, E.H. and Ramsing, A.U. Flow Injection Analyzer for students, teaching and research. Anal. Chim. Acta, 1982, 134:55
[8] Lown, J.A., Koile, R. and Johnson, D.C. Amperometric flow-through wire detector: a practical design with high sensitivity. Anal. Chim. Acta, 1980, 116:33
[9] 孙励敬，方肇伦等．土壤速效磷的流动注射分析．分析化学，1981，9：586
[10] Erickson, B.C., Ruzicka, J. and Kowalski, B. Applications of a versatile injection valve for flow injection analysis. Anal. Chem.,1987, 59:1246
[11] Fang, Z.L., Ruzicka, J. and Hansen, E.H. An efficient flow-injection system with on-line ion-exchange preconcentration for the determination of trace amounts of heavy metals by atomic absorption spectrometry. Anal. Chim. Acta, 1984, 164:23
[12] Wolf, W.R. and Stewart, K.K. Automated multiple flow injection analysis for flame atomic absorption spectrometry. Anal. Chem., 1979, 51:1201
[13] Hansen, E.H., Ruzicka, J. and Ghose, A.K. Flow injection analysis for calcium in serum,water and waste waters by spectrophotometry and by ion-selective electrode.
Anal. Chim. Acta, 1978, 100:151
[14] Nalbach, U., Schiemenz, H., Stamm, W.W. and Kula, M.R. On-line flow-injection monitoring of the enzyme inductor phenylalanine in the continuous cultivation of rhodococcus SP. M_4. Anal. Chim. Acta, 1988, 213:55
[15] Ahira, M., Arai, M. and Tomitsugu, T. Flow injection spectrofluorimetric determination of tebium (Ⅲ) based on solubilizing its tetnary complex in micellar solution. Anal. Lett., 1986, 19:1907
[16] Steig, S. and Nieman, T.A. Experimental and theoretical considerations of low cell design in analytical chemiluminescence. Anal. Chem., 1978, 50:401
[17] Burguera, J.L., Townshend, A. and Greenfield, S. Flow injection analysis for monitoring chemiluminescent reactions. Anal. Chim. Acta, 1980, 114:209
[18] Mullin, J.L. and Seitz, W.R. Two-phase flow cell for chemiluminescence and bioluminescence measurements. Anal. Chem., 1984, 56:1046
[19] Ruzicka, J. and Hansen, E.H. Flow Injection Analysis. 2nd edition, John Wiley & Sons, New York, 1988; FIA，徐淑坤等译，北京大学出版社，1991
[20] Ruzicka, J., Stewart, J.W.B. and Zagatto, E.A.G. Flow injection analyses part Ⅳ. Stream sample splitting and its application to the continuous spectrophotometric determination of chloride in brackish waters. Anal. Chim. Acta, 1976, 81:387
[21] Fang, Z.L. and Xu, S.K. Petermination of molybdenum at ug.L~(-1) levels by catalytic spectrophotometric flow injection analysis. Anal. Chim. Acta, 1983, 145: 143
[22] Fan, S.H., Muller, W.H., Schweizer, B. and Bohme, W. Fourth International Symposium on Kinetics in Analytical Chemistry, Erlangen, 1992
[23] Ruzicka, J. and Marshall, GD. Sequential injection: a new concept for chemical sensors, process analysis and laboratory assays. Anal. Chim. Acta, 1990, 237:329
[24] Quintero, M.C., Silva, M. and Perez-Bendito, D. Evaluation of the analytical use of the manganese-catalysed malachite green-periodate reaction by the stopped-flow technique. Talanta, 1989, 36:1091
[25] Zolotov, Yu.A., Shpigun, L.K. and Kolotyrkina, I.Ya. The trace determination of some heavy metals in waters by flow- injection spectrophotometry and potentiometry. Anal.
Chim. Acta, 1987, 200:21
[26] 罗庆尧，邓延倬，蔡汝秀，曾云鹗，分光光度分析，科学出版社，1992．
[27] 吴越，催化化学．科学出版社，1990．
[28] 杨武，高锦章，康敬万等编著．光度分析的灵敏反应及方法．科学出版社，北京，2000．
[29] Yatsimirskii, K.B. and Tikhonova, L.P. Catalytic kinetic methods for the determination of platinum metals. Talanta, 1987, 34(1): 69
[30] 周名成，晋勇，白华．水杨基萤光酮—溴化十六烷基三甲铵高灵敏分光光度法测定微量锰．分析化学，1986，14(3)：213
[31] 陈秀华，汤福隆，王小龙．5，10，15，20-四(2-羟基-5-磺酸苯基)卟啉与锰反应的吸光光度法的研究．理化检验(化)，1990，26(2)：70
[32] 周华方，张明珠，王镇浦．催化动力学光度法测定痕量锰的研究，化学通报，1994，4：42
[33] 贾欣欣，秦永惠．桑色素—过氧化氢体系催化光度法测定痕量锰的研究．光谱法与光谱分析，1999，19(3)：499
[34] 李锦昕，刘国钧．流动注射催化光度法测定地质样品中痕量锰．岩矿测试，1997，16(1)：57
[35] Nakano, S., Nozawa, M. and Yanagawa, M. Flow-injection determination of subnanogram amounts of manganese by catalysis of the oxidative coupling of N,N-dimethyl-p-pheny lenediamine with m-phenylene-diamine. Anal. Chim. Acta, 1992, 261:183
[36] 王春，秦永惠．催化光度法测定茶叶中痕量锰．分析化学，2000，28(3)：393
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