流动注射化学发光法测定Mn(Ⅱ)

在酸性条件下,溴酸钾氧化鲁米诺产生化学发光,Mn2 对这一体系的化学发光具有增强作用.据此,结合流动注射技术,建立了一种测定Mn2 的新方法.线性范围为1.0×10-8～6.0×10-6 mol/L;检出限为8.0×10-9 mol/L (3σ);对1.0×10-6 mol/L的Mn2 进行了平行测定(n=11),其相对标准偏差为2.4%.该方法可用于矿泉水中Mn2 的测定.     

流动注射化学发光法检测甲基嘧啶磷残留

研究发现,在碱性介质中甲基嘧啶磷能够有效增强鲁米诺-H2O2体系的化学发光。据此,结合流动注射分析法,建立了测定甲基嘧啶磷的流动注射化学发光分析方法,并对可能的反应机理进行了探讨。考察了甲基嘧啶磷-鲁米诺-H2O2体系的化学发光反应动力学以及反应体系pH、鲁米诺浓度、H2O2浓度、流速、进样体积等因素对化学发光的影响。结果表明:在最佳条件下,甲基嘧啶磷在5.0×10-8～1.0×10-5g/mL的浓度范围内与发光强度呈良好的线性关系,检出限(S/N=3)为2.5×10-8g/mL。将该体系应用于加标小麦样品测定,回收率为94.7%～113.0%,相对标准偏差为2.2%～3.6%。     

KMnO4-鲁米诺-香叶木素化学发光体系的研究

KMnO4-鲁米诺-香叶木素在碱性条件下有较好的发光特性,且香叶木素浓度在1.0×10-9～3.0×10-7g/mL范围内有很好的线性关系,该体系的检出限为3.7 ×10-10g/mL,对1.0×10-7 g/mL香叶木素进行11次平行测定,其RSD为1.9％.研究了体系的化学发光及紫外光谱特性,提出了发光反应可能的机...     

流动注射-化学发光法测定盐酸地尔硫卓

发现了盐酸地尔硫卓在过硫酸钾-鲁米诺化学发光反应体系中的后化学发光反应.据此发现建立了利用后化学发光反应测定盐酸地尔硫卓的流动注射化学发光新方法.方法的线性范围为3.0×10-6～1.0×10-4 g/mL,检出限为3×10-7 g/mL,对6.0×10-5 g/mL的盐酸地尔硫卓标准溶液进行11次平行测定的相对标准偏差为1.6%.方法已用于盐酸地尔硫卓片剂中盐酸地尔硫卓含量的测定.     

鲁米诺-过硫酸钠体系后化学发光法测定银

邻菲罗啉存在下,银对鲁米诺-Na2S2O8体系的后化学发光具有增敏作用,建立了流动注射后化学发光测定银的新方法.在优化实验条件下,该法测定银的线性范围为1.0×10-9～4.0×10-7 mol/L,线性相关系数为0.9987(n =7),检出限为3.53×10-10mol/L(n=11),对1.0×10-7 mol/...     

流动注射化学发光法测定河水中对苯二酚

在碱性介质中,高碘酸钾氧化鲁米诺产生化学发光,对苯二酚对此反应具有极强的增敏作用,据此建立了鲁米诺-高碘酸钾-对苯二酚化学发光体系测定对苯二酚的方法。对苯二酚溶液浓度在1.0×10-8~1.5×10-7mol.L-1范围内与化学发光强度呈线性关系,检出限为8.5×10-9mol.L-1,用于河水中对苯二酚的测定并测得其回收率在93.4%~104.4%之间。探讨了对苯二酚的增敏机理。     

流动注射化学发光法测定硫离子

在0.06 mol.L-1硫酸介质中,溴酸钾氧化鲁米诺产生化学发光,硫离子对这一体系的化学发光具有增强作用。据此,结合流动注射技术,提出了一种测定硫离子的方法。线性范围为1.0×10-6～1.0×10-3g.L-1(分为3个浓度区间),检出限(3s/b)为8.0×10-7g.L-1。对1.0×10-4g.L-1硫离子标准溶液进行平行测定,其相对标准偏差(n=11)为3.4%。该方法用于水样中硫离子的测定,并以此样品为基体做回收试验,测得回收率在96.5%～105.0%之间。     

铁氰化钾-鲁米诺体系后化学发光反应及其分析应用研究 ————-分子印迹-后化学发光法测定双嘧达莫

研究了双嘧达莫在铁氰化钾-鲁米诺化学发光反应体系中的后化学发光反应, 并在研究其反应的动力学性质、化学发光光谱、荧光光谱以及一些相关问题的基础上, 探讨了反应机理; 合成了双嘧达莫的分子印迹聚合物, 以此聚合物为分子识别物质, 利用铁氰化钾-鲁米诺-双嘧达莫后化学发光体系, 建立了测定双嘧达莫的高选择性分子印迹-后化学发光分析方法. 所建方法的线性范围为1.0×10-8-1.0×10-6 g/mL(r=0.999 2), 检出限为3×10-9 g/mL, 相对标准偏差为2.7%(1.0×10-7 g/mL双嘧达莫, n=11).     

流动注射化学发光法测定溶菌酶含量

基于溶菌酶催化水解壳聚糖的产物氨基葡萄糖,与金溶胶-鲁米诺可产生很强的化学发光,建立了流动注射化学发光测定溶菌酶含量的方法.对水解和化学发光反应条件进行了考察.结果表明,pH 4.0、50 ℃水解5h为最佳水解条件.在金胶、鲁米诺及NaOH的浓度分别为0.05,0.05和10 mmol/L条件下,化学发光检测效果最好....     

高碘酸钾-鲁米诺体系中一些后化学发光反应的研究

研究了葡醛内酯、盐酸美司坦和重酒石酸去甲肾上腺素等10种物质在高碘酸钾-鲁米诺体系中的后化学发光现象、后化学发光反应的动力学、化学发光光谱、荧光光谱以及其它相关性质, 提出了其可能的发光机理; 在优化的分析条件下建立了这10种物质的后化学发光分析方法, 初步构建了高碘酸钾-鲁米诺后化学发光分析体系.     

流动注射后化学发光法测定盐酸阿比朵尔

研究了盐酸阿比朵尔在鲁米诺-K3Fe(CN)6化学发光反应体系中的后化学发光反应. 据此建立了测定盐酸阿比朵尔的流动注射后化学发光分析法. 方法的线性范围为6.0×10-9～1.0×10-7 g/mL, 检出限(3σ)为2×10-9 g/mL. 对4.0×10-8 g/mL的盐酸阿比朵尔溶液连续11次平行测定, RSD=1.3%. 方法已用于盐酸阿比朵尔胶囊及尿样中盐酸阿比朵尔含量的测定. 在对这一后化学发光反应的动力学性质、化学发光光谱、紫外可见吸收光谱以及一些相关问题研究的基础上, 提出了可能的反应机理.     

Investigating the post-chemiluminescence behavior of phenothiazine medications in the luminol–potassium ferricyanide system: molecular imprinting–post-chemiluminescence method for the determination of chlorpromazine hydrochloride

A new post-chemiluminescence (PCL) phenomenon was observed when phenothiazine medications were injected into the reaction mixture after the chemiluminescence (CL) reaction of luminol and potassium ferricyanide had finished. A possible reaction mechanism was proposed based on studies of the kinetic characteristics of the CL, CL spectra, fluorescence spectra, and on other experiments. The feasibility of determining various phenothiazine medications by utilizing these PCL reactions was examined. A molecular imprinting–post-chemiluminescence (MI-PCL) method was established for the determination of chlorpromazine hydrochloride using a chlorpromazine hydrochloride-imprinted polymer (MIP) as the recognition material. The method displayed high selectivity and high sensitivity. The linear range of the method was 1.0×10⁻⁸∼1.0×10⁻⁶, with a linear correlation coefficient of 0.9985. The detection limit was 3×10⁻⁹ g/ml chlorpromazine hydrochloride, and the relative standard deviation for a 1.0×10⁻⁷ g/ml chlorpromazine hydrochloride solution was 4.0% (n=11). The method has been applied to the determination of chlorpromazine hydrochloride in urine and animal drinking water with satisfactory results.      

Effect of metal ions on the determination of semicarbazide hydrochloride with potassium bromate

Semicarbazide can be titrated quantitatively with potassium bromate in the presence of nickel(II), cobalt(III) and manganese(II) but copper(II) causes serious interference. The effects of copper ions on the reaction between potassium bromate and semicarbazide are investigated and the optimum conditions under which the reaction is quantitative are indicated.     

柱后衍生离子色谱法同时测定瓶装水中的碘酸根、亚氯酸根和溴酸根

水中的碘酸根、亚氯酸根和溴酸根是重要的消毒副产物,主要通过大体积浓缩后直接电导检测,或通过柱前或柱后化学反应将目标物转化成容易检测的物质后检测。本方法采用大体积进样柱后衍生紫外检测的分析方法,通过条件优化获得了较高的灵敏度和信噪比。利用一套自动分析系统,可以满足饮用水中痕量碘酸根、亚氯酸根、溴酸根的同时监测。碘酸根、亚氯酸根和溴酸根的检出限分别为0.5,0.4,0.1 μg/L。对于不同的加标样品,碘酸根、亚氯酸根和溴酸根的回收率分别为70.8%~98.0%,92.4%~100%和93.2%~104.1%。该方法应用于北京市场上的瓶装饮用水分析,结果显示瓶装纯净水中的碘酸根、亚氯酸根、溴酸根浓度均低于检出限,而瓶装矿泉水中碘酸根、溴酸根的最高含量分别达到9.4 μg/L和78.4 μg/L。     

以Co2＋掺杂纳米TiO2为光催化氧化剂的原位光致化学发光分析方法 研究及其应用

研究了Co2＋掺杂TiO2纳米粒子在光信号诱导下产生的超氧阴离子自由基在纳米粒子表面的吸附和解吸特性. 当以该纳米粒子为光催化氧化剂进行原位光致化学发光反应时, 光诱导产生的超氧阴离子自由基通过扩散穿过纳米粒子表面的双电层到达本体溶液, 与溶液中的化学发光试剂进行化学发光反应. 由于超氧阴离子自由基在纳米粒子表面的吸附、解吸和双电层效应, 使得光化学反应和其后的光生氧化剂的化学发光反应具有时间和空间的分辨特性. 将 Co2＋掺杂TiO2纳米粒子光致化学发光反应的特点与鲁米诺化学发光体系结合, 建立了一种原位光致化学发光反应的新方法, 并提出了一种基于纳米技术调控化学发光反应的新思路. 在最佳反应条件下, 该方法对格列本脲响应的线性范围为2.0×10－8～1.0×10－6 g•mL－1, 检出限为6×10－9 g•mL－1.     

Volumetric studies in oxidation-reduction reactions: Reduction with ferrous ethylenediamine sulphate indirect determinations

Ferrous ethylenediamine sulphate has been. used as a reducing agent in acid medium for the indirect volumetric estimations of potassium chlorate, potassium bromate, potassium metaperiodate, potassium, dichromate, potassium ferricyanide, potassium permanganate, potassium persulphate, hydrogen peroxide and ceric sulphate. The excess of ferrous ethylenediamine sulphate added to each of the substances was titrated with standard potassium permanganate and also with. standard potassium dichromate solution. In case of potassium bromate or potassium metaperiodate the end-point was not sharp in potassium dichromate titrations; while accurate volumetric observations were made with standard potassium permanganate solution.     

Investigations of the Enhancer Effect of a High-Salt Concentration Medium on the Luminol Chemiluminescent Reaction

The enhancer effect of a high-salt concentration medium on the luminol chemiluminescence reaction catalyzed by either soluble or immobilized peroxidase has been investigated. Some widely used salts were tested at high concentration (up to 3 mol L): potassium chloride, sodium chloride, ammonium sulfate and calcium chloride. The magnitude of the light intensity enhancement depends on the nature of the salt and on the form of the peroxidase, i.e. free in solution or immobilized. The enhancement is observed whether the catalyst of the chemiluminescence reaction is peroxidase or ferricyanide. Both the enhanced or nonenhanced luminol chemiluminescence spectra have a maximum wavelength emission at around 425 nm. The results reported in this study are in favor of an action of the salts on the nonenzymatic steps of the luminol chemiluminescence reaction rather than a modification of the enzymatic process.     

Flow-injection chemiluminescence determinations for human blood lead using controlled reagent release technology

A flow-through CL method for the determination of lead combined with controlled-reagent-release technology has been developed. Chemiluminescence (CL) reagents luminol and potassium permanganate were immobilized on anion exchange resin by electrostatic interaction. Lead ion was determined by its enhancing effect on the CL reaction between luminol and potassium permanganate. Both luminol and potassium permanganate were eluted from the anion exchange resin column by sodium phosphate solution. The linear range of the system was 10 μg mL^?1, and the detection limit was 5?×?10^–9 g mL^?1 lead (3σ). A complete analysis could be performed in 1 min with a relative SD 3.2% (1.0?×?10^–7 g mL^?1, n?=?9). The column shows remarkable stability and can be reused over 350 times and 21 days. The method has been applied to determine lead in human blood samples.     

Interaction between gaseous ozone and crystalline potassium bromide

The formation of nonvolatile products of the oxidation of a bromide ion during the interaction between gaseous ozone and powdered crystalline KBr is studied. It is found that potassium bromate KBrO₃ is the main product of the reaction. The influence of major experimental factors (the duration of ozonation, the concentration of ozone, the humidity of the initial gas, and the temperature) on the rate of formation of bromate is studied. The effective constants of the formation of bromate during the interaction between O₃ and Br^– in a heterogeneous gas–solid body system and in a homogeneous aqueous solution are compared.