Fluorimetric reaction-rate method for determination of mercury with 2,2′-dipyridylketone hydrazone

A simple and sensitive fluorimetric reaction-rate method for determination of mercury(II) (0.03-0.3 ppm), based on its catalytic effect on the autoxidation of 2,2′-dipyridylketone hydrazone, has been developed. The reaction is followed by the measurement of the rate of appearance of blue fluorescence (λ_ex = 359 nm, λ_em = 430 nm). The experimental variables and interferences in the determination are also reported.     

A spectrophotometric method for the determination of thorium with acid alizarin black Sn

Acid alizarin black SN reacts with thorium at pH 4.2 to give a highly sensitive colour reaction with thorium, ε₆₀₀ mμ = 28,000. There is no interference from Ba, Ca, Cd, Ce(III), Gd, Hg, La, Mg, Mn, Pb, Pr. Sm, Sr, Zn, Zr, Cl(su-), CN(-), I(su-), NO(3-), SO₄^2-. The interferences of Al, Bi, Co, Cu, Fe, Ni, Mo, Sb, Sn, Ti and W may be overcome by addition of masking agents. Only U(VI) and V(V) still interfere and these can be determined sequentially with the thorium. The nature of the complex is studied and the mode of its formation.     

Fluorimetric kinetic method for the determination of total ascorbic acid with o-phenylenediamine

A fluorimetric reaction-rate method for the determination of L-ascorbic acid (AA) in aqueous solution is presented. The technique is based on the rapid oxidation of AA by mercury(II) chloride to dehydro-L-ascorbic acid, which then reacts with o-phenylenediamine to form a fluorescent quinoxaline. The formation of the product is monitored fluorimetrically with a data acquisition system based on a microcomputer, a voltage-to-frequency converter and a timer-counter board. The initial rate is estimated with a fixed-time computational method. With a 20-s measurement time (after a 5-s delay from initiation of the reaction), the detection limit for AA is 0.02 μg ml^?1 with a linear dynamic range extending to 10 μg ml^?. The procedure is applied to the determination of the AA in vitamin pills and juice. The relative standard deviation is 1.9% or better.     

Fluorimetric determination of ascorbic acid with o-phenylenediamine

A simple and sensitive fluorimetric method for the determination of ascorbic acid (AA) is described. The method is based on the condensation reaction between AA and o-phenylenediamine (OPDA) in the absence of the oxidant. The fluorescence intensity is measured at excitation and emission wavelengths of 360 and 430 nm, respectively. Under optimum condition, a linear relationship is obtained between the fluorescence intensity and the concentration of AA in the range of 0.05-40 μg ml⁻¹. The detection limit is 0.006 μg ml⁻¹, which is obviously lower than that of other fluorimetric methods reported.     

Fluorimetric reaction-rate methods of inorganic analysis: a review

A review is given of the utilization in analytical chemistry of the rate of fluorescence reactions of inorganic species. These methods are of recent development and suggest the possibility of further analytical procedures. Two main types of methods, enzymatic and non-enzymatic, are distinguished, and their applications to inorganic analysis are discussed.     

Fluorimetric method for the determination of uranium in natural waters

A method is described for the fluorimetric determination of uranium in natural waters. The limit of detection is 0.3 ppM. Ion-exchange is used to preconcentrate the uranium by a factor of 22 and separate it from quenching ions in the sample. The fluorescence is measured in a medium that is 1.35M in both sulphuric and phosphoric acids. The uranyl ions are excited by radiation of wavelength 280 nm and bandwidth 40 nm. The emitted signal is scanned from 470 to 510 nm. After spiking of the sample solution with a small volume of standard uranium solution, the fluorescence signal is scanned again and the uranium content of the sample calculated from the two readings. The coefficient of variation is 8.5% for determinations of U in a synthetic water sample having a uranium content of 1.9 ppM. Destruction of organic matter in the eluates gives 0.1 ppM detection limit.     

Spectrophotometric reaction-rate method for the determination of nitrite in waters with pyridine-2-aldehyde 2-pyridylhydrazone

A method for the kinetic determination of submicrogram amounts of nitrite has been developed, based on its acceleration of the rate of bromate oxidation of pyridine-2-aldehyde 2-pyridylhydrazone in acidic medium. The reaction is monitored spectrophotometrically at 372 nm. A comparative study with hydrochloric acid and perchloric acid media shows that the analytical parameters are affected by the type of acid used. Within-day precision, based on ten replicate determinations, was better than 0.011 μ/ml, which corresponds to 2.2-1.5% relative standard deviation at the concentrations examined. Application of this method in the determination of nitrite in water has been discussed. The recovery of nitrite from drinking waters ranges from 90 to 117% and the average relative standard deviation for nitrite determinations in polluted river water is 3.2%. Large amounts of nitrate and ammonium ions do not interfere. However, there is interference by Cu²⁺, Pd²⁺ and electroactive substances. Major advantages for the method are simplicity, absence of a reagent blank, and the wide determination range.     

Fluorimetric method for the determination of long-chain amines in water

A method is presented for the determination of long-chain quaternary ammonium salts, tertiary amines and secondary amines in water or aqueous raffinates, based on their extraction and fluorimetric determination as amine salts with Eosine Yellowish in toluene-hexanol (4:1) as solvent. No interferences were obtained from metal ions, or chloride, nitrate or phosphate ions when a back-washing method was applied to the sample extract. The method allows the determination of long-chain tertiary amines down to 4 ppM.     

Polarographic determination of aluminium with alizarin

The polarographic determination of aluminium as its complex with alizarin in the pH range 9.2-10.1, with the cathode ray polarograph, is described. A solvent extraction procedure is used to eliminate interferences from many other metals.     

Fluorimetric determination of magnesium and aluminum via complexation with oxine in high-performance liquid chromatography

Aluminum and magnesium were determined by fluorimetric detection via pre-column and/or in-column derivatization with 8-hydroxyquinoline (oxine) in high-performance liquid chromatography. The oxine complex of aluminum was selectively detected when the eluent contained no oxine, whereas the aluminum and magnesium complexes could be simultaneously detected when the eluent contained oxine. The sensitivity was improved by using eluents containing oxine by a factor of 7.1 for aluminum, and the detection limits at S/N=3 were 18 and 16 ng/ml for magnesium and aluminum, respectively. The present system was applied to the determination of magnesium and aluminum in various water samples.     

阻抑动力学荧光分析法测定痕量苯肼

基于苯肼对吡咯红Y与亚硝酸根反应的抑制作用,建立了一种新的测定痕量苯肼的阻抑动力学荧光分析法。该方法的检出限为7.2ng mL,线性范围为8.0～60ng mL。直接用于环境水样中苯肼的测定。     

Fluorimetric determination of zinc with dibenzothiazolyl-methane

Dibenzothiazolylmethane produces a specific fluorescence with zinc in ethanolwater solutions. Zinc is determined quantitatively in solutions containing 0.05 to 50 mg of zinc/l. One part of zinc can be detected in the presence of 20,000 parts of cadmium and quantitative determinations of zinc in cadmium salts are readily done. The method can be applied to the analysis of non-ferrous alloys such as Dowmetals.     

环境水样中痕量肼的荧光分析

基于在硫酸介质中，肼与罗丹明6G反应，使其荧光增强，建立了一种荧光测定痕量肼的新方法。该方法线性范围2．0－14．0μg/L，检出限为0．62μg/L。可用于环境水样中肼含量的测定，并进行了回收实验，回收率为97％－107％。     

荧光光谱法测定中成药中微量铅

基于二价铅离子在浓盐酸体系中所形成的PbCl42-配合物在紫外光的照射下发出蓝色荧光的原理,提出了一种测定中成药品中的微量铅的灵敏的荧光分析法。体系的荧光强度与Pb(Ⅱ)的质量浓度在0.02～2.00μg/mL范围内有良好的线性关系,检测下限为8.7×10-3μg/mL。用本法测定了中成药丸及原料药粉中的铅含量,回收率分别介于92 0%～107%和94%～101%之间。     

茜素绿-蛋白质体系的共振瑞利散射光谱及其分析应用

基于蛋白质对茜素绿共振瑞利散射的增强作用,建立了一种测定水溶性蛋白质的新方法.在酸性BR缓冲溶液中,茜素绿在365 nm处的共振光散射增强与蛋白质浓度呈线性关系.对人血清白蛋白、牛血清白蛋白、γ-人球蛋白、卵白蛋白测定的检出限均低于14 ng/mL.该方法灵敏、稳定、选择性好,适用于人血清、尿液中总蛋白质的测定.     

Fluorimetric determination of zirconium with morin

Zirconium can be determination fluorimctrically with morin in 2M hydrochloric acid in the presence of such elements as Al, Be, Ga, Sb, Sn, Th and U, which fluorcsce much less strongly under the conditions, by measuring the fluorescence intensity before and after adding ethylenediaminetetraacetic acid. This substance destroys the fluorescence of zirconium only and the difference in fluorescence intensities corresponds to the concentration of zirconium in solution. The determination of zirconium in the presence of aluminum has especially been studied. Satisfactory accuracy can be obtained even when Al/Zr = 10,000, if the proper morin concentration is used. Iron docs not interfere if reduced to the ferrous state with mercap oacetic acid, Zirconium can be determined in silicate rocks without any separations except those made automatically in tlie sodium carbonate decomposition. Niobium and tantalum should not exceed 0.05%.     

酪氨酸作试剂荧光光度法测定亚硝酸根

亚硝酸盐广泛存在于土壤、食品及天然水中 ,是水体中氮循环的重要中间物。亚硝酸盐可引起急性中毒 ,还可以与仲胺和酰胺等结合成致癌的亚硝胺化合物 ,是造成环境污染的主要原因之一。因此 ,亚硝酸盐的含量是环境监测和食品分析的重要指标。荧光法测定亚硝酸根常用的试剂是 2 ,3 二氨基萘[1] ,但需用有机溶剂萃取 ,操作繁琐 ,而且由于试剂本身有毒 ,易造成二次污染。近年来有人报道了荧光猝灭法测定亚硝酸根[2 ,3] 。本文以亚硝酸根与酪氨酸反应产物在碱性介质中呈现强的荧光 ,其激发波长和发射波长分别为 31 8.0ｎｍ和 398.4ｎｍ ,建立了水…