Platinum catalyzed reduction of uranium(VI) with hydrazine in sulfuric acid media

The process of platinum-catalyzed uranium(VI) reduction with hydrazine in sulfuric acid media has been studied. The influence of sulfuric acid and hydrazine concentrations, and temperature on the reaction rate were investigated. A new reaction mechanism is proposed. The process allows to obtain pure U(IV) sulfate solutions with concentrations of up to 0.3 mol·l^–1. Further increase of initial U(VI) concentrations is limited by the reductant solubility in sulfuric acid media.     

Determination of folic acid by adsorptive stripping voltammetry at the static mercury drop electrode

Folic acid can be determined at nanomolar concentrations by controlled adsorptive accumulation of folic acid on a static mercury drop electrode held at ?0.3 V vs. Ag/AgCl followed by reduction of the surface species. In 0.1 M sulfuric acid, a cathodic scan gives peaks at ?0.47 v and ?0.75 V vs. Ag/Agcl; the latter peak provides greater sensitivity. Differential-pulse stripping is shown to be superior to normal-pulse and d.c. stripping. After a 5-min preconcentration, the detection limit is about 1 × 10^?10 M folic acid. The adsorptive stripping response is evaluated with respect to concentration dependence, preconcentration time and potential, solution acidity and the presence of gelatin and bromide. The relative standard deviation at the 5 × 10^?8 M level is 1.2%. This method is applied to the determination of folic acid in pharmaceutical tablets.     

Drop-scale chronopotentiometry

Chronopotentiometry has been successfully carried out on one drop of solution. A simple arrangement enabled determinations to be performed in one to two minutes. A potential holdup was clearly indicated for the oxidation of iodide ions on electrolyzing 0.07 ml of a 5·10^-6M potassium iodide solution 1M in sulfuric acid, a total of 3.5·10^-10 equivalents of iodide ions.     

Automatic sample preparation of35S labelled organic compounds for liquid scintillation counting

An automatic sample preparation method for the determination of³⁵S in organic compounds by liquid scintillation counting is described. The sample is burned in a stream of oxygen and the combustion products are led onto a quartz wool column wetted with dilute hydrogen peroxide. Sulfur oxides are retained on the quartz wool as sulfuric acid, while the other acid producing combustion products are eliminated by evaporation. The residual sulfuric acid in rinsed with distilled water, the sulfuric acid solution obtained is added to a liquid scintillation cocktail and the radioactivity is measured with a liquid scintillation counter. The combustion-evaporation process runs automatically according to the operational program carried out by an electronic programmer.     

A New Polarographic Adsorptive Catalytic Wave for the Determination of Trace Tellurium in Smog Dust and Wheat Flour

Linear-sweep polarography of tellurium in sulfuric acid solution containing methylene blue produces a wave at −0.82 V (vs SCE). In a cathodic sweep, the derivative peak current is directly proportional to the concentration of tellurium over the range 4 × 10⁻⁹to 1 × 10⁻⁷g/ml, and the detection limit is 2 × 10⁻⁹g/ml. The polarographic wave is an adsorptive catalytic hydrogen wave. This method has been applied to the determination of trace amounts of tellurium in smog dust and wheat flour, with satisfactory results.     

Chemiluminescence behavior based on oxidation reaction of rhodamine B with cerium(IV) in sulfuric acid medium

The chemiluminescence (CL) of the rhodamine B (RhB)-cerium(IV) system was investigated by flow-injection. Rhodamine B was suggested to be a suitable chemiluminescent reagent in acidic conditions. When the concentration of rhodamine B was 100 mg l⁻¹ and cerium sulfate was 1.6 mmol l⁻¹ in sulfuric acid, the chemiluminescent intensity was found to be highest by using 0.3 mol l⁻¹ sulfuric acid as a carrier solution. The particular chemiluminescent system could tolerate such distinct acidic environments that it was utilized for detecting many compounds that are stable in acidic solutions. Furthermore, by virtue of IR, UV-Vis and luminescence spectroscopic measurements, the chemiluminescent behavior of rhodamine B was studied and a possible mechanism for this chemiluminescent reaction was proposed. The emitter was affirmed to be a radical species due to one of the oxidation products of RhB; the chemiluminescent emissive wavelength was about 425 nm.     

Sine-wave polarographic determination of zirconium or niobium in aqueous media

The sine-wave polarographic determination of zirconium in aqueous media was investigated using solutions which were 0.55 – 5.5·10^-3M in zirconyl chloride and 1 M in potassium chloride and had been adjusted to pH 2.0 with hydrochloric acid. It was possible to determine zirconium in the concentration range of 0.05 to 0.4 mg per ml. The sine-wave polarographic behavior of zirconium in aqueous solutions in the pH range 2–3 is discussed. The sine-wave polarographic determination of niobium in aqueous media was investigated using concentrated sulfuric acid containing 5 to 0.1 mg of niobium per ml in a supporting electrolyte of citric acid; the determination of niobium was possible down to 0.1 mg of niobium per ml of concentrated sulfuric acid although the D.C. polarographic method was impractical for the determination of less than 0.5 mg of niobium per ml.     

Spectrophotometric determination of bismuth in copper and cartridge brass by the iodide method

An improved spectrophotometric method is proposed for the determination with iodide of trace amounts of bismuth in copper and cartridge brass. The sample is dissolved in nitric acid and the bismuth is separated from the copper by an ammoniacal precipitation in the presence of iron(III) hydroxide as a gathering agent. The hydroxide precipitate is dissolved in hydrochloric acid, sulfuric acid is added, the solution is evaporated to a few ml, hydrobromic acid is added to volatilize the antimony and tin, and the solution is evaporated to fumes of sulfuric acid. The bismuth iodide color is then developed with a composite potassium iodide—sodium hypophosphite reagent. Factors affecting the bismuth iodide color are investigated.     

Desolvation of acid solutions in inductively coupled plasma atomic emission spectrometry by infrared radiation. Comparison with a system based on microwave radiation

The behaviour of an infrared desolvation system with acid solutions in inductively coupled plasma atomic emission spectrometry (ICP-AES) is evaluated, and the influence of the liquid uptake rate and of the nature and concentration of the acid on the solvent and analyte transport rates and on the analytical figures of merit is studied. The results are compared with those obtained with a desolvation system based on the absorption of microwave radiation. The infrared desolvation system performs best at low sample uptake rates (0.4 ml min⁻¹) and its behaviour strongly depends on the nature and concentration of the solution used. With nitric and hydrochloric solutions, there is almost no effect of the acid concentration on the emission intensity, while for sulfuric and perchloric acids the signal decreases as the acid concentration is increased. These effects seem to be related with the different capability of the acid aerosols to be heated in an IR field. The microwave desolvation system seems to be more prone to matrix (acid) effects, specially when using sulfuric and perchloric acids, resulting in emission intensities which are usually lower than those obtained with the infrared desolvation system, though their limits of detection are quite similar.     

Oxidations with potassium permanganate in the presence of fluoride

Summary Quadrivalent selenium can be determined with fair accuracy by mixing with an excess of KMnO₄ in the presence of 25–75 ml of 2% NaF solution and 4–7 ml of 9 N sulfuric acid. After leaving the reaction mixture for 10–30 minutes the excess KMnO₄ is estimated by one of the following procedures: A) Titration of the excess KMnO₄ with monovalent mercury, B) Adding an excess of Hg₂ ²⁺ solution to react with the excess KMnO₄ followed by titrating the excess mercurous with KMnO₄ solution.Part I: Issa, I. M., and M. Hamdy, Z. analyt. Chem. 172, 94 (1980).     

Transport of sulfuric acid through anion-exchange membrane NEOSEPTA-AFN

This paper deals with the determination of the membrane mass transfer coefficient for sulfuric acid in an anion-exchange membrane NEOSEPTA-AFN. This quantity has been determined on the basis of experiments carried out in a batch dialysis cell using the method of numerical integration of the basic differential equation describing the time dependence of sulfuric acid concentration and subsequent optimization procedure. The experiments carried out made it possible to calculate the membrane mass transfer coefficient for sulfuric acid over the concentration range from 0.1 to 1.9 kmol m⁻³ in the external solution.     

钒液流电池用碳纸电极改性的研究

采用红外光谱和扫描电镜等手段研究了浓硫酸处理前、后碳纸的表面结构和形貌的变化。并将这类碳纸用作全钒液流氧化还原电池电极材料,对其电化学性能进行了详细研究。结果表明通过酸处理,碳纸表面有-COOH官能团生成,其电化学活性增强。酸处理后的碳纸电极组装成的电池在电流密度20 mA·cm^-2时有良好充放电性能,平均电流和电压效率达到95%和82%。     

Quantitation of trace aqueous halides by volatilization into a microwave-induced helium plasma

Chloride and bromide in aqueous solutions are determined using chemical vaporization occupied with a 500-W helium microwave-induced plasma emission system. The halide is converted to the corresponding hydrogen halide by mixing with concentrated sulfuric acid in a continuously flow cell. The observed linear ranges cover 2–3 orders of magnitude. Detection limits for chloride and bromide are 0.2 and 0.3 mg l^?1, respectively. The sample throughput is 6–10 h^?1. Matrix matching is needed for real samples.     

Simultaneous determination of35S and14C in double-labelled organic compounds by liquid scintillation counting

An isotope analytical method for the simultaneous determination of³⁵S and¹⁴C in double-labelled organic compounds by liquid scintillation counting is described. The sample is burned in a stream of oxygen. Sulfur oxides are converted to sulfuric acid and separated from other combustion products, including carbon-14 dioxide, on a heated quartz wool column previously wetted with hydrogen peroxide. Carbon dioxide is collected from the gas stream by an absorbent suitable for liquid scintillation counting. The residual sulfuric acid is rinsed off the column with water and the aqueous solution obtained is mixed with a liquid scintillation cocktail for radioactivity measurement. The final solutions ready for counting are obtained in less than fifteen minutes, quantitative collection recovery is achieved and no cross contamination occurs.     

Mass transport and effective diffusion coefficient in the reduction of hydrogen ions from aqueous sulfuric acid solutions: Numerical modeling

This work presents results of the numerical solution to a system of equations of material balance and the movement of particles in solution under the influence of the forces of diffusion, migration, and convection, which describe the process of mass transport during the reduction of hydrogen ions at a rotating disk electrode from aqueous sulfuric acid solutions with and without excess supporting electrolyte. Results of the calculations show that the diffusion kinetics of hydrogen ion reduction can be observed only with measurements in dilute (≤10^?3 M) sulfuric acid solutions with an excess of indifferent supporting electrolyte. For more acidic solutions it is necessary to take into account the simultaneous diffusion of hydrogen and bisulfate ions. In the study of the regularities of hydrogen ion reduction in sulfuric acid solutions with a sulfate supporting electrolyte, it is necessary to take into account that with excess supporting electrolyte, the limiting current of hydrogen reduction is caused solely by the diffusion of bisulfate ions, but for small concentration ratios of the supporting electrolyte to acid, the influence of migration effects is significant.     

Na2EDTA滴定法测定粗二氧化碲中铅含量

建立了用氢溴酸消除锑、砷、锡干扰,用硫酸将铅形成硫酸铅沉淀,再用EDTA络合滴定法测定粗二氧化碲中铅量的方法。试样用硝酸、盐酸溶解,用硫酸沉淀铅,氢溴酸消除锑、砷、锡的干扰后,过滤分离其他共存元素,以乙酸-乙酸钠缓冲溶液溶解硫酸铅沉淀,在pH=5.0～6.0时,以二甲酚橙作指示剂,用Na_2EDTA溶液滴定溶液中铅含量。实验结果表明,氢溴酸加入量为15mL,酒石酸加入量为10mL,沉淀体积为50～60mL,沉淀时间1h以上时,方法相对标准偏差(RSD)在0.10%～1.1%,加标回收率为97.1%～102%,满足粗二氧化碲中铅量的生产控制检测要求。     

Spectrophotometric determination of aluminum in river water with bromopyrogallol red and n-tetradecyltrimethylammonium bromide by flow injection analysis

In the proposed flow injection system, the reagent solution contains bromopyrogallol red, n-tetradecyltrimethylammonium bromide and hexamine in 60% ethanolic solution, and the carrier solution contains acetate buffer, 1,10-phenanthroline and hydroxylammonium chloride. Sample solutions (160 μl) acidified by sulfuric acid are injected and the peak absorbance at 623 nm is recorded. The detection limit is about 0.001 ppm and calibration plots are linear for the ranges 0–0.3 and 0–0.1 ppm aluminum.     

Accurate all-purpose method for the assay of alkali and alkaline earth carbonates with perchloric acid

An accurate all-purpose method is proposed for the determination of carbonate in alkali and alkali earth carbonates. A large sample size (4–9 g depending on the carbonate) is dissolved in 100.00 ml of 1.2 M perchloric acid, the solution is boiled, and the excess of acid is titrated with standard 1.0 M sodium hydroxide solution to a methyl orange end-point. Perchloric acid is preferable to hydrochloric acid because there is no danger of loss of acid during the boiling; it is preferable to sulfuric acid since insoluble sulfates of barium, strontium, and calcium are not precipitated in analyzing alkali earth carbonates. Normal alkali and alkali earth carbonates (anhydrous and hydrated) are assayed on samples previously dried by heating in an oven at 250°C for 3 h. This treatment drives off all the water but it also converts any hydrogencarbonate present into carbonate. Hydrogencarbonates are assayed on samples dried in a desiccator containing sulfuric acid for 16 h. Twelve different carbonates were analyzed. The average standard deviation of the method was 0.050%.     

A Fluorescence Quenching Method for the Determination of Bromate Ion with 4,5-Dibromophenylfluorone and Cetyltrimethylammonium Bromide

Abstract

A highly sensitive and selective fluorescence quenching method was developed to determine the bromate ion (BrO₃ ^?) with 4,5-dibromophenylfluorone (DB-PF) as fluorogenic reagent. BrO₃ ^? reacts with potassium bromide in sulfuric acid solution (0.6M) giving bromine (Br₂) which is estimated with fluorescence quenching method using DB-PF as fluorogenic reagent. Bromine reacts with DB-PF to produce a compound, whose maximum excitation wavelength and emission wavelength are 543nm, 560nm respectively. The linear calibration range is 0.05–0.5 μg/25ml. The detection limit is 0.05μg/25ml. The method may be used to determine microamounts of BrO₃ ^? in potassium chlorate with satisfactory results. The method offers the advantages of simplicity, rapidity and sensitivity.     

Synthesis and characterization of phenylated pyrazino-benzimidazophenanthroline polymers

Novel phenylated quinoxaline tetraamines have been prepared and polymerized with 1,4,5,8-naphthalenetetracarboxylic acid in polyphosphoric acid solution. The resulting BBB-type polymers with pendant phenyl groups along the polymer backbone are soluble in m-cresol. The polymers, with inherent viscosities ranging from 0.3 to 0.6 dl/g in sulfuric acid, exhibited thermal stabilities near 500°C under nitrogen and near 400°C in air.