RESUMEN
The potentiometric titration method was used for characterization of uranium compounds to be applied in intercomparison programs. The method is applied with traceability assured using a potassium dichromate primary standard. A semi-automatic version was developed to reduce the analysis time and the operator variation. The standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization and compatible with those obtained by manual techniques.
Asunto(s)
Potenciometría/métodos , Radiometría/métodos , Radiometría/normas , Robótica/métodos , Uranio/análisis , Uranio/química , Algoritmos , Brasil , Semivida , Internacionalidad , Potenciometría/normas , Dosis de Radiación , Estándares de Referencia , Valores de Referencia , Robótica/normasRESUMEN
A potentiometric azide-selective sensor based on the use of iron(III) hydrotris(3,5-dimethylpyrazolyl)borate acetylacetonate chloride [Tp(Me2)Fe(acac)Cl] as a neutral carrier for an azide-selective electrode is reported. Effect of various plasticizers, viz. o-nitrophenyloctyl ether (o-NPOE), dioctylphthalate (DOP), dibutylphthalate (DBP), and benzylacetate (BA), and an anion excluder, hexadecyltrimethylammonium bromide (HTAB), with [Tp(Me2)Fe(acac)Cl] complex in poly(vinyl chloride) (PVC) were studied. The best performance was obtained with a membrane composition of [Tp(Me2)Fe(acac)Cl]/HTAB/DOP/PVC in a ratio of 5:2:190:100 (w/w). The sensor exhibits significantly enhanced selectivity toward azide ions over the concentration range 6.3 x 10(-7) to 1.0 x 10(-2) M with a lower detection limit of 3.8 x 10(-7) M and a Nernstian slope of 59.4 +/- 1.1 mV decade(-1). Influences of the membrane composition, pH and possible interfering anions were investigated on the response properties of the electrode. Fast and stable response, good reproducibility, long-term stability and applicability over a wide pH range (3.5-9.0) are demonstrated. The sensor has a response time of 14 s and can be used for at least 45 days without any considerable divergence in the potential response. The proposed electrode shows fairly good discrimination of azide from several inorganic and organic anions. It was successfully applied to the direct determination of azide in orange juice, tea extracts and human urine samples.