Quantificação de contaminantes em aguardentes de cana/cachaças de alambique e de coluna

In the present study aimed to characterize and quantify four contaminants (ethyl carbamate, 2,3-butanedione, furfural and 5-hydroxymethylfurfural) present in alembic cachaça and industrial. Were collected forty-four samples of cachaça in the southern regions, the Midwest, southeast of Minas Gerais and São Paulo state, and subsequently subjected to physical, chemical and chromatographic analyzes. The physicochemical analyzes were performed according to the methodology described by the Ministry of Agriculture, Livestock and Supply (MAPA). The ethyl carbamate, 2,3-butanedione, furfuaral and 5 hydroxymethylfurfural were characterized and quantified by high-performance liquid chromatography (HPLC). The results of the ethyl carbamate analysis, it was found that both samples showed column cachaças outside the standards required by law, with the values 245.31 235.53 L-1 ug and none of the liquor samples alembic showed concentration greater than 210.0 ug L-1 , and the method is very sensitive to low limits of detection and quantification. In determining 2,3-butanedione, it was revealed that the column cachaças showed higher levels of contaminants when compared to cachaça alembic. In the quantification of furfural and 5-hydroxymethylfurfural was developed and validated analytical methods employed to high-performance liquid chromatography (HPLC) with DAD detector. Samples column cachaças showed higher values than the limit established by Brazilian legislation and ranged from 7.00 to 5.63 mg / 100 ml of anhydrous alcohol over the alembic cachaça.

Recuperação e aplicação do dicromato de potássio proveniente do resíduo de sulfocrômica

A simple procedure for recovering potassium dichromate (K2Cr2O7 ) from treatment of residual sulphochromic solution was proposed in the present work by means of cooling crystallization. The decrease of temperature favored the crystallization of K2Cr2O7 due to the decrease of solubility. 5.0 L of sulphochromic wastes containing 48.08 g L-1 of Cr(VI) were treated and the process of crystallization was performed in three steps until crystals were not formed anymore. On each step the content of Crtotal was determined by flame atomic absorption spectrometry and Cr(VI) by colorimetric method with 1,5- diphenylcarbazide, resulting in the removal of 91% and 92% of Crtotal and Cr(VI), respectively. After the last step, the remaining Cr(VI) in the solution was reduced to Cr(III) from the addition of NaHSO3 , recovering via precipitation in pH 8 approximately 36.13 g of Cr(OH)3 . The final supernatant was discarded since chromium content was below the maximum limit established by the Brazilian legislation for effluents discharge, which corresponds to 0.10 and 1.0 mg L-1 of Cr(VI) and Cr(III), respectively. 628.4 g of K2Cr2O7 were recovered and the salt was characterized by X-ray diffraction and differential thermal analysis. Its applicability was compared to the standard K2Cr2O7 when determining the soil organic matter, in which there was no significant difference, thus inferring that the recovered compound may be incorporated on routine analyses. This recovering process allowed the reuse of K2Cr2O7 , thus reducing costs with the acquisition of new reagents and environmental impacts caused by the inadequate discard of sulphochromic solutions.