【作者】 高芝；

【导师】 高楼军；

【作者基本信息】 延安大学 ， 分析化学， 2010， 硕士

【摘要】 催化光度法具有仪器设备简单,操作简便且灵敏度高等特点,在分析测试中得到了极大地应用。随着科学技术的发展,分析工作者将FIA技术应用到催化动力学分析领域,使许多传统溶液处理方法的基本操作得以快速、自动地完成,从而弥补了采用传统的动力学分析时,反应条件不易控制、试剂消耗大,分析速度慢等缺点,极大地推动了催化动力学分析法的进展。本文包括综述和研究报告两部分:第一部分:流动注射催化光度分析综述介绍了催化光度法近七年来的研究现状;概述了近几年来流动注射催化光度法的研究现状。第二部分:包括五个研究报告,具体如下:一、以过氧化氢-橙黄G为指示反应,建立了催化褪色光度法测定痕量Co2+的新方法。在pH = 9.53的NH3-NH4Cl缓冲溶液中,沸水浴中加热6min,测定痕量Co2+的线性范围为0.006～2.0μg/25mL,检出限为3.41×10-3μg/25mL,用于维生素B12针剂中微量Co2+的测定,并与火焰原子吸收法比较,方法可靠。二、基于在pH = 11.05的NH3-NH4Cl缓冲溶液介质中,痕量c(Ⅲ)对H2O2氧化橙黄G的褪色反应具有阻抑作用,据此建立了阻抑褪色光度法测定微量Sb(Ⅲ)的新方法,该方法的线性范围为0.10～5.50μg/25mL,检出限为6.36×10-4μg/mL,成功用于水样中微量Sb(Ⅲ)的测定。三、利用在B-R缓冲溶液介质中,Sb(Ⅲ)对H2O2氧化孔雀石绿褪色反应具有催化作用,建立了一种流动注射催化动力学光度法测定微量元素Sb(Ⅲ)的新分析方法,该方法的线性范围为0.010～2.0μg/mL,检出限为7.8×10-3μg/mL,对0.1μg/mL Sb(Ⅲ)平行测定11次的标准偏差为0.97%,进样频率为22.8样/h。用于环境水样中微量Sb(Ⅲ)的测定,回收率为97.3～97.7%。四、研究了在B-R缓冲溶液介质中,Bi(Ⅲ)对H2O2氧化孔雀石绿褪色反应的显著阻抑作用,结合停留技术,建立了一种停留-反相流动注射阻抑光度法测定超痕量Bi(Ⅲ)的新分析方法,该方法的线性范围为0.001～0.54ng/L,检出限为9.9×10-4ng/L,相关系数r = 0.9992。对0.001ng/L Bi(Ⅲ)平行测定11次的标准偏差为1.3%,进样频率为20.9样/h。该方法具有极高的灵敏度和选择性,可直接用于人发和水中的超痕量Bi(Ⅲ)的测定,回收率为96.0%~102.0%。五、在H3BO3-KCl-NaOH缓冲溶液介质中,Bi(Ⅲ)对H2O2氧化结晶紫褪色反应的阻抑作用,建立了一种停留-反相流动注射阻抑光度法测定Bi (Ⅲ)的新分析方法,该方法的线性范围为0.005～0.05μg/mL,检出限为7.28×10-4μg/mL,对0.01μg/mL Bi(Ⅲ)平行测定11次的标准偏差为0.45%,进样频率为21.8样/h。用于胃药中的Bi(Ⅲ)的测定,回收率为101.5%。更多还原

【Abstract】 Catalytic spectrophotometry method is a useful technique in the determination of trace substances. It enjoys great generality in most laboratory for its high sensitivity and inexpensive instruments. Analysts combined the technique of flow injection with catalytic method, which compensated many drawbacks when traditional catalytic spectrophotometric is adopted such as high regeant cost, inconvenient control of analysis condition and low analysis speed, and which greatly promoted the development of catalytic speetrophotometric method.There are two parts in this thesis:Part one: reviewThe new development of traditional catalytic speetrophotometric method during last senve years, among which new approches, new system, performance enhancement and so on are exploited.The new development of flow-injection catalytic speetrophotometric method.Part two: study reportsA new catalytic spectrophotometic method is proposed for the determination of cobalt(Ⅱ), based on the fact that cobalt(Ⅱ) can catalyze the discolouring reaction of Orange G oxidized by hydrogen peroxide in NH3-NH4Cl buffer solution medium. Under the optimum experimental conditions, the linear range of the determination is 0.006～2.0μg/25mL and the detection limit of 3.41×10-3μg/25mL. The proposed method is applied to the determination of trace amounts of cobalt(Ⅱ) in Vitamin B12 with satisfactory results.A new inhibition discoloring spectrophotometric method for determination of antimony(Ⅲ) is described. This method is based on the innibitic effect of antimony(Ⅲ) on the reaction of Orange G and hydrogen peroxide in the NH3-NH4Cl buffer solution medium. The linear range of the determination is 0.10～5.50μg/25mL for antimony(Ⅲ) and the detection limit is 6.36×10-4μg/mL. The method has been applied for the determination of antimony(Ⅲ) in water sample with satisfactory result.A new flow-injection-inhibition discolouring spectrophotometric method using stopped-flow technique for determination of trace antimony(Ⅲ) is described. This method is based on the catalytic effect of antimony(Ⅲ) on the reaction of Malachite Green and hydrogen peroxide in the Britton-Robinson buffer solution medium. The linear range of the determination is 0.01～2.0μg/mL for antimony(Ⅲ) with a correlation coeffient of 0.9996, and the detection limit is 7.8×10-3μg/mL with the sampling rate of 22.8 times per hour. The relative standard deviation of eleven replicate measurements is 0.97% for 0.1μg/mL. The method has been applied for the determination of trace antimony(Ⅲ) in water sample with satisfactory result. The recovery is 97.3～97.7%.A new reverse flow-injection inhibition discoloring spectrophotometric method using stopped-flow technique for determination of ultra trace bismuth(Ⅲ) is described. This method is based on the innibitic effect of bismuth(Ⅲ) on the reaction of Malachite Green and hydrogen peroxide in the Britton-Robinson buffer solution medium. The linear range of the determination is 0.001～0.54ng/L for bismuth(Ⅲ) with a correlation coeffient of 0.9992, and the detection limit is 9.9×10-4ng/L with the sampling rate of 20.9 times per hour. The standard deviation of eleven replicate measurements is 1.3% for 0.001ng/L bismuth(Ⅲ). The method has been applied for the determination of ultra trace bismuth(Ⅲ) in human hair and water sample. The recovery is 96.0～102.0%.A new reverse flow-injection inhibition discoloring spectrophotometric method using stopped-flow technique for determination of bismuth(Ⅲ) is described. This method is based on the innibitic effect of bismuth(Ⅲ) on the reaction of Crystal Violet and hydrogen peroxide in the H2BO3-KCI-NaOH buffer solution medium. The linear range of the determination is 0.005～0.05μg/mL for bismuth(Ⅲ) with a correlation coeffient of 0.9998, and the detection limit is 7.28×10-4μg/mL with the sampling rate of 21.8 times per hour. The standard deviation of eleven replicate measurements is 0.45% for 0.01μg/mL bismuth(Ⅲ). The method has been applied to the determination of bismuth(Ⅲ) in bismuth aluminate compound table. The recovery is 101.5%.更多还原