催化荧光动力学分析法的研究
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摘要
催化荧光动力学分析法结合了动力学分析法和荧光分析法的特点，具有高灵敏度和更高的专属性，是用于检测痕量组分的有力手段。本文主要研究了催化荧光动力学分析法在测定痕量无机离子钒(Ⅴ)、硒(Ⅳ)和有机物对苯二酚方面的应用；对荧光猝灭法测定痕量硒(Ⅳ)进行了研究。全文分如下部分：
1．对催化荧光动力学分析法的发展和应用进行了综合评述，并对其应用前景加以展望。
2．建立了催化荧光动力学分析法测定痕量无机离子(V~(5+)和Se~(4+))的新方法。选择了最佳试验条件(温度、时间和试剂用量等)，并对催化反应机理进行了初步探讨。
3．利用有机物(对苯二酚)对钒(Ⅴ)催化溴酸钾氧化吖啶橙反应体系的活化作用，测定了实际样品中对苯二酚的含量，研究了最佳试验条件，方法迅速、简便、选择性好。初步探讨了活化作用机理。
4．利用Se~(4+)氧化碘化钾的反应产物使吖啶橙荧光猝灭，建立了荧光猝灭法测定痕量硒的新方法。方法简便灵敏，用于水、蒜样中硒(Ⅳ)的测定，结果满意。并探讨了反应机理。
The kinetic analysis of catalytic fluorimetic is a effective method in solving trace amounts analysis with high sensitivity and higher selectivity because it synthesizes the characteristics of kinetic and fluorescence analysis. This paper focuses on the application of catalytic fluorimetry in determination of trace amount inorganic ion vanadium and organic compound. The determination of selenium(IV) by fluorescence quenching reaction is also studied.
The paper consists of four parts. In part 1, the progress and application of catalytic fluorimetic analysis are reviewed. Application of the analysis and future study are prospected.
In part 2, the new method is described for the determination of trace vanadium(V) and selenium(IV). The optimized conditions(temperature, time and the quantity of reagents etal.) are selected and the mechanism of the catalytic reaction has also been discussed.
In part 3, a new method is developed for the determination of the concentration of activist in real samples. It is based on the activation effect of hydroquinone on the catalytic oxidation reaction of acridine orange by potassium bromate in the presence of vanadium( V ).The optimized conditions are studied. The method is quick, convenient and has high selectivity. The mechanism of the active reaction has been discussed.
In part 4, a new fluorescence quenching method has been proposed for the determination of trace selenium. The method is based on the fluorescence quenching of acridine orange by the oxidation reaction product of selenium(IV) with potassium iodide. The method is simple and sensitive. It has been applied to the determination of water and garlic samples with satisfactory results. The mechanism of the reaction has also been discussed.
1．对催化荧光动力学分析法的发展和应用进行了综合评述，并对其应用前景加以展望。
2．建立了催化荧光动力学分析法测定痕量无机离子(V~(5+)和Se~(4+))的新方法。选择了最佳试验条件(温度、时间和试剂用量等)，并对催化反应机理进行了初步探讨。
3．利用有机物(对苯二酚)对钒(Ⅴ)催化溴酸钾氧化吖啶橙反应体系的活化作用，测定了实际样品中对苯二酚的含量，研究了最佳试验条件，方法迅速、简便、选择性好。初步探讨了活化作用机理。
4．利用Se~(4+)氧化碘化钾的反应产物使吖啶橙荧光猝灭，建立了荧光猝灭法测定痕量硒的新方法。方法简便灵敏，用于水、蒜样中硒(Ⅳ)的测定，结果满意。并探讨了反应机理。
The kinetic analysis of catalytic fluorimetic is a effective method in solving trace amounts analysis with high sensitivity and higher selectivity because it synthesizes the characteristics of kinetic and fluorescence analysis. This paper focuses on the application of catalytic fluorimetry in determination of trace amount inorganic ion vanadium and organic compound. The determination of selenium(IV) by fluorescence quenching reaction is also studied.
The paper consists of four parts. In part 1, the progress and application of catalytic fluorimetic analysis are reviewed. Application of the analysis and future study are prospected.
In part 2, the new method is described for the determination of trace vanadium(V) and selenium(IV). The optimized conditions(temperature, time and the quantity of reagents etal.) are selected and the mechanism of the catalytic reaction has also been discussed.
In part 3, a new method is developed for the determination of the concentration of activist in real samples. It is based on the activation effect of hydroquinone on the catalytic oxidation reaction of acridine orange by potassium bromate in the presence of vanadium( V ).The optimized conditions are studied. The method is quick, convenient and has high selectivity. The mechanism of the active reaction has been discussed.
In part 4, a new fluorescence quenching method has been proposed for the determination of trace selenium. The method is based on the fluorescence quenching of acridine orange by the oxidation reaction product of selenium(IV) with potassium iodide. The method is simple and sensitive. It has been applied to the determination of water and garlic samples with satisfactory results. The mechanism of the reaction has also been discussed.
引文
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2. Stanley R. Crouch, and Thomas F.Cullen, Kinetic determinations and some kinetics aspects of analytical chemistry, Anal.Chem, 1998,70:53～106R
3. M.Sikorski, E.Krystkowiak, R.P.Steer, The kinetics of fast fluorescence quenching processes, Journal of Photochemistry and Photobiology A: Chemistry, 1998, 117:1～16
4. D.Perez-Bendito, A.Gomez-Hens, M.Silva, Advances in drug analysis by kinetic methods, Journal of Pharmaceutical and Biomedical Analysis, 1996, 14:917～930
5. Bo Tang, Fang Han, Guo Ying Zhang, Kinetic-spectrofluorimetric determination of trace amounts of iridium, Talanta, 2002, 56:603～611
6. Zheng X Y, Lu J Z, Zhu Q Z, etal. Analyst, 1997, 122:455～458
7．俞英，洪朝辉，黄坚锋，2-(8-羟基喹啉-5-磺酸-7-偶氮)-变色酸催化荧光法测定痕量锰(Ⅱ)，分析化学，1994，22(6)：542～547
8．俞英，洪朝辉，王瑞琼等，以糠醛缩7-氨基-8-羟基喹啉-5-磺酸为试剂催化荧光法测定痕量锰(Ⅱ)，分析化学，1998，26(4)：414～417
9．张贵珠，张海清，何锡文等，荧光动力学光度法同时测定硝酸根和亚硝酸根的研究，分析化学，1994，22(10)：1006～1009
10．谢增鸿，郑肇生，陈霞，以Triton X—100为增敏剂荧光速率法测定银，分析化学，1998，26(2)：215～217
11．李彬，冯素玲，樊静，催化荧光法测定超痕量银的研究，分析试验室，1998，17(2)：68～71
12．程定玺，张红武，催化荧光光度法测定砷的研究，分析试验室，2002，21(2)：67～69
13．张贵珠，张海清，郭薇等，荧光动力学法测定痕量溴离子的研究，化学试剂，1994，16(6)：335～336
14．郑肇生，吴和舟，陈锋等，动力学法测定卤素研究，分析化学，1993，21(9)：1092～1094
15．邵建章，痕量溴的阻抑动力学荧光法测定，分析测试学报，2002，21(1)：87～88
16．邵建章，冯素玲，程定玺，速差催化荧光法同时测定痕量钴和铜，理化检验-化学分册，2002，38(7)：350～354
17．冯素玲，王瑞勇，樊静，催化荧光法测定痕量铬(Ⅵ)，分析化学，2000，28(1)：61～63
18. Chen L. H. Wang D. S. Catalytic fluorimetric determination of trace chromium(Ⅵ) based on the oxidation safranine T by hydrogen peroxide, Fenxihuaxue, 1997, 25(1):120～122
19．冯素玲，程定玺，张贵恩，动力学荧光法测定痕量铜，分析化学，1995，23(10)：1230～1232
20．陈兰化，赵新雁，吖啶黄催化荧光法测定超痕量铜的研究，理化检验(化学分册)，1997，22(6)：264～266
21. Kawakabo. S, Kato. H, Iwatsuki. M, Catalytic spectrofluorimetric determination of copper using aerial oxidation of ascorbic acid in the presence of o-phenylendiamine. Analyst, 1994, 119(9):2119～2125
22．樊静，王瑞勇，冯素玲，抑制动力学荧光法测定痕量氟，分析试验室，2001，20(2)：44～46
23．俞英，聂瑞华，黄坚锋等，KIO_4氧化茜素红催化荧光法测定痕量Fe~(3+)，高等学校化学学报，1996，17(9)：1381～1383
24．俞英，洪朝辉，催化动力学荧光分析新体系Fe~(3+)—H_2O_2-糠醛缩-7-氨基-8-羟基喹啉-5-磺酸的研究，光谱学与光谱分析，2000，20(1)：110～112
25. Zhihong Liu, Ruxiu Cai, Highly sensitive spectrofluorimetric determination of hydrogen peroxide with β-cyclodextrin-hemin as catalyst, The Analyst, 1999,124:173～178
26．邵建章，动力学荧光法测定痕量碘的研究，分析试验室，2002，21(4)：26～28
27．蒋治良，李芳，超痕量铱的催化荧光分析新方法的研究，分析测试技术与仪器，1998，4(3)：19～25
28．陈亚华，韩秀丽，催化荧光法测定痕量锰的研究，分析试验室，1994，13(1)：40～42
29．张勇，张兰芳，周漱萍，催化荧光法测定痕量锰的研究，理化检验-化学分册，1995，31(4)：227～229
30．张贵恩，陈红，冯素玲，催化荧光法测定痕量钼，分析化学，1996，24(5)：539～542
31. Kawakubo. S, Suzuki. H, Zwatsuk. M, Catalytic spectrofluorimetric determination of ultratrace molybdenum in natural fresh water, Anal. Sci. 1996, 12(5):767～772
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