Este trabalho descreve um método para a determinação quantitativa de ácido acetilsalicílico (ASA) utilizando procedimento "spot test" e reflectância difusa. O método é baseado na formação do complexo de cor roxa intensa entre o ácido salicílico, obtido a partir da hidrólise alcalina do ASA, e íons Fe(III). O procedimento proposto permite a análise de medicamentos contendo ASA de forma fácil e simples, uma vez que não é necessário fazer separações. A reflectância da mistura final, colocada sobre um disco de papel de filtro, é medida diretamente. Foram analisados nove medicamentos comerciais contendo ASA cujos resultados apresentaram um desvio padrão relativo médio de 0,9%. O limite para a determinação quantitativa é de 0,6 mg de ASA na solução de trabalho. As análises feitas com o método proposto foram comparadas com outras análises, das mesmas amostras, segundo o procedimento recomendado pela "United States Pharmacopoeia", onde se observou um desvio padrão relativo de 0,6%. Compararam-se os dois métodos utilizando-se o teste t de Student. Para um grau de liberdade ν = 4 (ν = n 1 + n 2 -2) e um limite de confiança α = 0.05, onde t = 2,78, todos os resultados foram concordantes.This paper describes a quantitative reflectance spot test procedure for the determination of acetylsalicylic acid (ASA) in pharmaceutical preparations. The method is based on the reaction of salicylic acid, obtained from the hydrolysis of ASA, with Fe(III) forming a deep blue-violet compound. Medicines containing ASA can be easily analyzed by the proposed method as it is not necessary to do any separation. The final mixture is placed on a sheet of filter paper, and the reflectance is directly measured. Nine commercial medicines containing acetylsalicylic acid were analyzed with the proposed method. The mean RSD was 0.9%. Results were compared with those obtained with the United States Pharmacopoeia recommended procedure (RSD 0.6%). The quantitative detection limit is 0.6 mg ASA in the working solution. For a degree of freedom ν = 4 (ν = n 1 + n 2 -2) and a confidence coefficient α = 0.05 all the results agree under the tabulated t-Student test value (2.78).
A colorimetric method for the quantitative determination of CO by diffuse reflectance is described. This method is based on the reduction by CO of Mo (VI) from the indicator reagent molybdosilicic acid (H8Si[Mo2O7]6). The reduction yielded a change of color from clear yellow to dark green on white disk filter chart paper wetted with reagent indicator solution. The gaseous mixture containing CO was forced to pass through this chart paper, initiating the reaction. The intensity of the color produced, measured by diffuse reflectance, was proportional to the CO concentration present in exhaust gases in the range from 0.02 to 12% volume/volume (v/v). A 650-nm light-emitting diode was used as a light source. A two-fiber-optic system carried the light from the source to the detection system, which was composed of a photodiode, an amplification circuit, and a digital display. The method was applied with success in field measurements for automobiles in the Otto cycle. In a previous paper, this method was used for the quantitative determination of exhaust emissions from diesel-fueled vehicles.
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