Determination of traces of free acid in uranyl salt solutions

A method for the determination of free acid in the presence of uranium(VI) is suggested. It involves the extraction of uranium by TBP from a solution saturated with potassium nitrate or chioride in order to prevent interference from the hydrolysis of uranium. The end-point is detected potentiometrically at pH 3.4. The method is suitable for the determination of 0.1–1.5 millimoles of acid in the presence of as much as 1.0 millimole of uranium.     

Spectrophotometric method for the direct determination of uranium in carbonate solution

Summary A spectrophotometric method for direct determination of uranium in carbonate solution has been developed. No extraction or decomposition steps are necessary. The highly sensitive (4-2-pyridylazo) resorcinol, as well as 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, producing very stable uranium(VI) complexes, were used for its spectrophotometric determination.The usefulness of the proposed methods was examined by determination of uranium in real samples from a wet-process phosphoric acid estimation of uranium.     

Use of diethazine hydrochloride for the extractive spectrophotometric determination of uranium and as a redox indicator

Optimum conditions have been established for the formation and extraction of the complex formed from diethazine, thiocyanate and uranium(VI). An extractive spectrophotometric method for the determination of uranium(VI) is described. Experimental conditions have been also established for the direct titrimetric determination of uranium(IV) with potassium dichromate, using diethazine hydrochloride as redox indicator. Interferences have been considered.     

Rapid laser fluorometric method for the determination of uranium in soil, ultrabasic rock, plant ash, coal fly ash and red mud samples

A simple and rapid laser fluorometric determination of trace and ultra trace level of uranium in a wide variety of low uranium content materials like soil, basic and ultra basic rocks, plant ash, coal fly ash and red mud samples is described. Interference studies of some common major, minor and trace elements likely to be present in different, geological materials on uranium fluorescence are studied using different fluorescence enhancing reagents like sodium pyrophosphate, orthophosphoric acid, penta sodium tri-polyphosphate and sodium hexametaphosphate. The accurate determination of very low uranium content samples which are rich in iron, manganese and calcium, is possible only after the selective separation of uranium. Conditions suitable for the quantitative single step extraction of 25 ng to 20 μg uranium with tri-n-octylphosphine oxide and single step quantitative stripping with dilute neutral sodium pyrophosphate, which also acts as fluorescence enhancing reagent is studied. The aqueous strip is used for the direct laser fluorometric measurement without any further pretreatment. The procedure is applied for the determination of uranium in soil, basalt, plant ash, coal fly ash and red mud samples. The accuracy of the proposed method is checked by analyzing certain standard reference materials as well as synthetic sample with known quantity of uranium. The accuracy and reproducibility of the method are fairly good with RSD ranging from 3 to 5% depend upon the concentration of uranium.     

A titrimetric method for the sequential determination of thorium and uranium

A method for the sequential determination of thorium and uranium has been developed. In the sample solution containing thorium and uranium, thorium is first determined by complexometric titration with ethylenediaminetetraacetic acid (EDTA) and then in the same solution uranium is determined by redox titration employing potentiometry. As EDTA interferes in uranium determination giving positive bias, it is destroyed by fuming with HClO₄ prior to the determination of uranium. A precision and accuracy of better than ±0.15% is obtained for thorium at 10mg level and uranium ranging from 5 mg to 20 mg in the aliquot.     

Determination of plutonium in the presence of uranium by alpha-spectrometry

The plutonium determination by alpha-particle spectrometry with semiconductor detectors in the presence of uranium has been described. It has been found that plutonium as well as uranium can be electrodeposited quantitatively on nickel or stainless steel discs from solutions in isopropanol. The time of deposition does not exceed 35–40 min. The determination of plutonium is possible within the uranium to plutonium weight ratio of 4000 with the accuracy better than 2%.     

Determination of micro amounts of uranium by a molybdenum blue method

A new and highly sensitive spectrophotometric method has been developed for the determination of micro amounts of uranium by a molybdenum blue method. The method is based on the observation that at low acidities uranium(IV) reduces ammonium molybdate to molybdenum blue, the absorbance of which is proportional to the amount of uranium present. The variables affecting development of the colour have been investigated and the conditions optimized. Beer's law is found to hold good for uranium concentrations between 1 and 20 ppm, with a precision of 2%. The effect of diverse ions has been studied. The method is useful for the determination of uranium present as an impurity (down to 0.1%) in plutonium, neptunium or thorium.     

Extraction fluorimetric determination of uranium by conventional spectrophotometry

The determination of uranium by a fluorimetric method using a conventional spectrophotometer has been elaborated. The quenching effect of the matrix was reduced by separation with liquid-liquid extraction and emulsion liquid membrane extraction methods using D2EHPA as a selective extraction reagent. The method was employed for uranium determination in radioactive waste solutions and proved to be very fast and easy to perform. It was found that it is possible to determinate as low as 0.2 ppm of uranium in a 10 ml sample.     

Novel method for determination of uranium isotopes in environmental samples by liquid–liquid extraction with triisooctylamine in sulfuric and hydrochloric acid media

Novel and robust method for determination of uranium isotopes in various environmental materials is presented. The method is based on total decomposition of the solid materials by the use of closed vessels microwave acid digestion systems and pre concentration of uranium from the liquid samples. The separation of uranium from interfering radionuclides and stable matrix elements is attained by liquid–liquid extraction with triisooctylamine/xylene in sulfuric and consecutively in hydrochloric acid media. Purified uranium is electrodeposited on a stainless steel disks and then measured by alpha spectrometry. The critical steps in the method were examined. The analytical method has been successfully applied to the determination of uranium isotopes in mineral and tap waters, as well as in soils from Northwestern Bulgaria. The analytical quality was checked by analyzing reference materials with different matrices.     

Assay for oxygen in uranium in the 0.1–1.0 wt% range using 14-MeV neutron activation

The X-ray spectrometric method for uranium determination in sea water is discussed. Two techniques of uranium enrichment are presented: (1) precipitation with the chelating agent ammonium-1-pyrrolidine dithiocarbamate (APDC) in the presence of iron(II) as a carrier and (2) complexation with APDC followed by adsorption on activated carbon. The best pH range and the other optimized conditions for uranium determination in sea water with both methods are reported.     

Individual determination of uranium and plutonium in a single aliquot

Studies on the individual potentiometric determination of uranium and plutonium in a single aliquot have been initiated recently in our laboratory. It was required to adapt the reported procedures (for the precise determination of uranium and plutonium individually when present together in a sample) at various stages to make them suitable for the successive application of the procedures to the same aliquot. Two alternative schemes are proposed in the present work. In the first, plutonium is determined by HClO₄ oxidation followed by the determination of total uranium and plutonium by Zn(Hg) reduction. In the second, plutonium is determined by AgO oxidation following the determination of total uranium and plutonium by Zn(Hg) reduction. Amount of uranium is computed in both cases from the difference of two determinations. Precision for the assay of plutonium and uranium was found to be ±0.25% and ±0.35%, respectively, at milligram levels.     

Effect of plutonium on the potentiometric determination of uranium

Effect of the presence of plutonium on the determination of uranium by potentiometric method has been studied. The presence of large quantities of plutonium does not appear to affect the determination of uranium present at 5 mg as well as 250 mg levels.     

Simultaneous determination of lead and nickel in uranium by square-wave polarography

A sensitive method for the simultaneous determination of trace lead and nickel in uranium is described. These elements are separated from uranium by anion exchange and then determined by square-wave polarography using the alkaline cyanide solution as supporting electrolyte. The procedure is applicable to uranium metal and its compounds containing as little as 1 p.p.m. of lead and nickel.     

Indirect determination of uranium by the on-line reduction and fluorimetric detection of cerium(III).

A novel flow injection method has been developed for the indirect determination of uranium by the on-line reduction and subsequent fluorimetric detection of cerium(III). A sample solution containing uranium(VI), prepared as a sulfuric acid solution, was injected into a sulfuric acid carrier solution and passed through a column packed with metal bismuth to reduce uranium(VI) to uranium(IV). The sample solution was merged with a cerium(IV) solution to oxidize uranium(IV) to uranium(VI) and the cerium(III) generated was then monitored fluorimetricaly. The present method is free from interference from zirconium, lanthanides, and thorium, and has been successfully applied to the determination of uranium in monazite coupled with an anion-exchange separation in a sulfuric acid medium to eliminate iron(III). The sample throughput was 25 per hour and the lowest detectable concentration was 0.0042 mg l(-1).     

Potentiometric determination of uranium in phosphate-perchlorate medium and its applicability in the natural uranium fuel cycle

A potentiometric method has been developed for the determination of uranium in phosphate-perchlorate medium. A significant feature of this method is its applicability for the determination of uranium in uranium-bearing CaF₂ slags and fused salt cakes generated at the natural uranium conversion and fabrication plants, respectively. These uraniumbearing slags and cakes contain large amounts of calcium and barium, respectively, where the conventional Davies-Gray and the related methods cannot be applied. A distinct advantage of the present method over coulometric determination of uranium in perchloric acid medium is that it can easily be adopted for routine analysis.     

用新显色剂1,1′-[2,2′-(4,4′-双噻唑基)-双偶氮]-2,2′-双萘酚与TritonX-100体系析相光度法测定微量铀

将新显色剂1,1′-[2,2′-(4,4′-双噻唑基)-双偶氮]-2,2′-双萘酚(简称4,4′-bi-TAN),用作为测定铀的高选择性的试剂。析相体系为UO_2~(2+)-4,4′-bi-TAN-TritonX-100,在580nm波长下测定UO_2~(2+),许多共存离子不干扰测定,用此法测定了铀矿废水中UO_2~(2+)的含量,结果令人满意。     

Application of Adsorptive Stripping Voltammetry for Determination of Uranium in the Presence of 3-Hydroxy-2-Naphthoic Hydrazide

Abstract

A new method is presented for determination of uranium based on a cathodic adsorptive stripping of the complex of uranium with a 3-hydroxy-2-naphthoic hydrazide at a hanging mercury drop electrode (HMDE). The most suitable operating conditions and parameters, such as pH, deposition potential, deposition time, ligand concentration, and others, were selected and the determination of uranium from aqueous solutions using the standard addition method was possible. Under optimum conditions, the measured peak current is proportional to the concentration of uranium over the range of 1–500 nA with a detection limit of 0.75 nM.     

Simultaneous Spectrophotometric Determination of Uranium and Thorium Using Arsenazo III by H‐Point Standard Addition Method and Partial Least Squares Regression

Simultaneous determination of uranium and thorium using arsenazo III as a chromogenic reagent at pH 1.70 by H‐point standard addition method (HPSAM) and partial least squares (PLS) calibration is described. Under optimum conditions, the simultaneous determinations of uranium and thorium by HPSAM were performed. The absorbencies at one pair of wavelengths, 649 and 669 nm, were monitored with the addition of standard solutions of uranium. The results of applying the HPSAM showed that uranium and thorium can be determined simultaneously with weight concentration ratios of uranium to thorium varying from 20:1 to 1:15 in the mixed sample. By multivariate calibration methods such as PLS, it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. In this study, the calibration model is based on absorption spectra in the 600–750 nm range for 25 different mixtures of uranium and thorium. Calibration matrices contained 0.10–21.00 and 0.25–18.5 μg mL^?1 of uranium and thorium, respectively. The RMSEP for uranium and thorium were 0.7400 and 0.7276, respectively. Both proposed methods (HPSAM and PLS) were also successfully applied to the determination of uranium and thorium in several synthetic and real matrix samples.     

Simultaneous determination of uranium and thorium in high grade thorium ores

A routine procedure has been developed for the simultaneous determination of uranium and thorium in high concentration thorium ores. INAA is used to determine the uranium and thorium concentration. However, for very low concentrations of uranium a radiochemical procedure based on the use of NPy/benzene as an extractant has to be employed. The precision and accuracy of the method has been determined by analyzing IAEA and NBL standard thorium/uranium ores.     

Determination of uranium by fluorescence method

The paper describes a procedure for the determination of uranium in dilute solutions by fluorescence method. Factors influencing the determination in a phosphoric acid medium were studied. The detection limit of uranium determination is 0.04–0.05 ppm.