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A particularly rapid HPTLC method has been established for chromatographic separation and quantification of p -aminobenzoic acid (PABA) in complex dietary supplement tablets. After chromatography, PABA was determined by spectrodensitometry at 270 nm. PABA spots were then visualized by a novel staining procedure involving the Bratton-Marshall coupling reaction after spraying with 8-hydroxyquinoline in situ on the chromatographic plates. After visualization, spectrodensitometric analysis was repeated at 500 nm. Linearity, intermediate precision, sensitivity, accuracy, and precision were compared for both methods. Results from tablet analysis were verified with the modified Bratton-Marshall spectrophotometric procedure.

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Abstract  

8-Hydroxyquinoline (8-HOQ) is known as an important chelating agent for several metal ions. This compound is practically insoluble in water. For this reason, in this study its water soluble sulfate salt has been used for complexing uranyl ions and the stability constants of the complex have been determined. The Irving-Rosotti method computing the Calvin-Bjerrum pH-titration data, was applied. Finally, the stability constants of the complex formed between (8-HOQN-H)2SO4 and uranyl ions were found to be lgK1=8.25 and lgK2=4.15, the overall stability constant being {ie55-1}.

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Solubility and pH precipitation studies were carried out to obtain the binuclear complex {[TiO(C9H6NO)2][Sn(C9H6NO)2]} involving 8-hydroxyquinoline as chelating agent. The compound, the individual mononuclear complexes and their physical mixture were evaluated by means of techniques such as TG, DTA, elemental analysis, X-ray diffraction, IR spectroscopy. The properties of the original compounds and also the thermoanalytical conditions exerted a great influence on the degree of crystallinity and on the crystalline phase of the mixed oxide obtained as final product of the thermal decomposition.

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We studied the preparation of some specific adsorbers capable of isolating and concentrating actinides. Bases of the 8-hydroxyquinoline family, diphosphineamine and tribenzylamine, salted by benzohydroxamic, benzylic or phthalic acid, are able to complex actinides in different oxidation states. As a result of the presence of the benzene rings, all the compounds are easily incorporated into active charcoal to obtain adsorbers with a highly specific surface. The adsorption behaviors of uranyl U(VI) ion, thorium(IV) and Eu(III) were studied by evaluating their distribution coefficients, K d. Results show that all the prepared salts can adsorb the ions in the III and IV oxidation state from weak acid solutions, whereas uranyl ion is adsorbed mainly from weak basic solutions. The prepared compounds can be used successfully to absorb and concentrate actinides from nearly neutral solutions, such as natural waters. The 8-hydroxyquinoline salt of the benzylic anion showed the highest adsorption values and thus seems to be the most appropriate salt to use in the analysis of actinides in water.

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Solvent extractions of thorium(IV) and uranium(VI) by a commercially available chelating extractant LIX-26 (an alkylated 8-hydroxyquinoline) or 8-hydroxyquinoline, benzoic or salicylic acid, dipentyl sulphoxide (DPSO) and their mixtures with butanol as modifier in benzene/methylisobutyl ketone (MIBK) as the diluent have been studied. Extraction of uranium(VI) by 10% LIX-26 and 10% butanol in benzene becomes quantitative at pH 5.0. The pH 0.5 values for the extraction of thorium(IV) and uranium(VI) are 4.95 and 3.35, respectively. Quantitative extraction of thorium(IV) by the mixture of 0.1 M oxine and 0.1 M salicylic acid in methylisobutyl ketone was observed at pH 5.0. The influence of concentration of various anions on the extraction of Th4+ by mixtures of LIX-26 and benzoic acid has been studied. Studies on extraction of thorium(IV) and uranium(VI) by mixtures of LIX-26 (HQ) and DPSO show that the extracted species are possibly of the type [ThQ2/DPSO/2/SCN/2] and [UO2Q2/DPSO/], respectively.

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The adsorption conditions of uranium, neptunium, thorium, europium on the adsorbers containing the benzylate salts of the 8-hydroxyquinoline (adsorber B), and of 2-methyl- 8-hydroxyquinoline (adsorber R), were prepared, supported onto charcoal and compared with an adsorber, containing the benzylic acid, (G), stabilized with d-glucoseamine, and adsorbed onto charcoal as well. Thorium, protoactinium, and europium are adsorbed nearly completely from aqueous solutions at a large pH range, even in low acid medium, whereas uranium and neptunium are completely adsorbed only from basic solutions of pH 9. The actinides are preferentially adsorbed with respect to other ions, which are present in natural waters, such as calcium or magnesium. This feature make the analysis of most actinides in natural waters easily to be performed without changing the pH of the original system. The uranium (neptunium) analysis indeed may be accomplished after adjusting the original pH to a fairly basic value (about to 9). The adsorption experiments from real samples showed that the analysis of the actinides dispersed in natural water systems may be successfully performed after previous concentration on the adsorbers prepare.

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Extraction of copper(II) and zinc(II) from acidic chloride solutions with mixtures of two extractants: a basic or solvating one and a chelating extractant was discussed. Processes for recovery and separation of Cu(II) from Zn(II) were proposed, which consist of the following steps: extraction from chloride media with the formation of metal chlorocomplex ion pair or solvate, scrubbing of chloride ions with an aqueous solution of appropriate pH with simultaneous transfer of the metal ion to the chelate, traditional stripping with sulphuric acid and conditioning of the basic extractant. Both effective recovery and separation of metal ions with simultaneous change of the system from the chloride to the sulphate state can be achieved. A bifunctional reagent, such as alkyl derivative of 8-hydroxyquinoline, can be also used instead of the extractant mixture.

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The ultrafiltration preconcentration of Cd2+ using micellar extraction with 8-hydroxyquinoline (8-HQ), solubilized in anionic micelles of sodium dodecylsulphate (SDS)) were studied. The n-butanol was used as a co-surfactant. Ultrafiltration yields (R, %) on cellulose acetate membranes (wet, 20000 MW-CO) under 400 kPa pressure were determined. Distribution ratios (D) of cadmium between bulk liquid phase and micellar pseudophase were estimated. The constants (app.) for the cadmium-sodium exchange on SDS micelles surface at pH values of 4.8 and 5.3 (3.36 and 3.86, respectively) were determined. It was found, that the values of ultrafiltration yields of the cadmium (at constant concentration of 8-HQ) are influenced not only by the pH and by the concentration values, but also by the ratio of the concentrations of the metal and the anionic surfactant.

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The extraction of bismuth has been investigated in dependence of dilution and stoichiometry, using the reagents 8-hydroxyquinoline, N-benzyl-N-phenylhydroxylamine, diphenylthiocarbazone and substituted carbamates. Stripping of bismuth from organic solutions of the respective chelates using ligands such as EGTA, thioglycollic acid and 2,3-dimercaptopropane-1-sulfonate was also studied. It has been demonstrated that the equations proposed for determining the range of quantitative substoichiometric extraction are valid in the case of bismuth only at concentrations above 10−5 M Bi. At further dilutions (10−6–10−8 M), which would be of major interest in devising analytical methods based on the substoichiometric radioisotope dilution technique for determining bismuth at the trace level, the equilibria are shifted in favour of the competing hydrolytic reactions, so that the extraction is quantitative only with ammonium tetramethylenedithiocarbamate present in excess.

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Recently, a new type of resinous adsorbent has been developed as an effective adsorbent for a number of organic materials. The adsorbent has macro-reticular structure and no ion-exchange capacity. This paper deals with the adsorption of typical fission products and induced radionuclides on Amberlite XAD-2, with 8-hydroxyquinoline (oxine) as the organic reagent. It was found that60Co,59Fe,144Ce,95Zr, and106Ru were transferred to the adsorbent phase from various solutions, when oxinates of the nuclides were formed in the solutions. Without oxine, most of the nuclides were not adsorbed on the adsorbent.137Cs and85Sr were not adsorbed on XAD-2 with or without oxine.

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