No abstract

A coulometria é considerada o método de maior qualidade metrológica para medição de quantidade de substância de padrões primários. Entretanto, a contaminação de sais de elevada pureza está presente em níveis traços sendo necessária a sua identificação e quantificação. Este trabalho apresenta os estudos desenvolvidos pelo Inmetro (Instituto Nacional de Metrologia, Normalização e Qualidade Industrial, Brasil) para determinar a pureza do cloreto de potássio (KCl) por titulação coulométrica a corrente constante, além da determinação do brometo como seu principal contaminante por cromatografia iônica (IC). Esses estudos foram necessários para desenvolver material de referência certificado (MRC) de KCl para garantir a qualidade dos resultados das medições químicas principalmente as de titulometria. A caracterização do candidato a MRC de KCl apresentou pureza de 99,9662%, a qual foi obtida após a correção do brometo, em fração mássica, obtido por IC, de 182,47 ± 3,03 mg kg -1 (incerteza expandida, k = 2, para um nível de confiança de aproximadamente de 95%).Coulometry is considered the highest metrological method for measuring the amount of substance of high-purity compounds. However, the contamination of the high purity salts is present in trace levels and its identification and quantification are necessary. This work aims to present the studies performed by Inmetro (National Institute of Metrology, Standardization and Industrial Quality, Brazil) to determine the purity of potassium chloride (KCl) by constant-current coulometric titration, as well as the determination of bromide as the main impurity in the KCl through ion chromatography (IC). These studies were needed to develop certified reference material (CRM) of KCl to guarantee the quality of the chemical measurements, mainly those performed by titrimetric analysis. The characterization of the candidate CRM of KCl by coulometric titration presented the purity of 99.9662%. This value was obtained after bromide correction of 182.47 ± 3.03 mg kg -1 (expanded uncertainty for k = 2, for a confidence level of approximately 95%) for the mass fraction bromide assayed by IC.

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No abstract

<p>The production of selenium and selenomethionine certified reference material in yeast (<em>Saccharomyces cerevisiae</em>) and certification studies for its homogeneity, stability and characterization, have been accomplished before in our laboratory. Based on such results and experience of our laboratory in Metrology and according to literature, we discuss here the advantages and limitations of the calibration by “single point” as an alternative method to the classical calibration curve. The method traceability to the SI is checked in order to secure a robust determination. As the model analyte the mass fraction of the Se species selenomethionine is measured and compared in yeast samples. Results showed that a good agreement was obtained by both methods (the reference one of the calibration curve and “single point calibration”). This simple approach can be used for routine control of selenomethionine in commercial supplements of yeast samples, but the work carried out demonstrated its potential for the general routine quantitative analysis of the possible and important selenium species in other Se-enriched supplements commercialised in Latin America (i.e. mushrooms, garlic etc).</p>