New voltammetry-based technique for the determination of tebuthiuron in crystal and brown sugar samples

Sugar is widely consumed worldwide and Brazil is the largest producer, consumer, and exporter of this product. To guarantee proper development and productivity of sugar cane crops, it is necessary to apply large quantities of agrochemicals, especially herbicides and pesticides. The herbicide tebuthiuron (TBH) prevents pre- and post-emergence of infesting weed in sugarcane cultures. Considering that it is important to ensure food safety for the population, this paper proposes a reliable method to analyse TBH in sugar matrixes (brown and crystal) using square wave voltammetry (SWV) and differential pulse voltammetry (DPV) at bare glassy carbon electrode and investigate the electrochemical behavior of this herbicide by cyclic voltammetry (CV). Our results suggest that TBH or the product of its reaction with a supporting electrolyte is oxidized through irreversible transfer of one electron between the analyte and the working electrode, at a potential close to +1.16 V vs. Ag |AgClsat in 0.10 mol L-1 KOH as supporting electrolyte solution. Both DPV and SWV are satisfactory for the quantitative analysis of the analyte. DPV is more sensitive and selective, with detection limits of 0.902, 0.815 and 0.578 mg kg-1, and quantification limits of 0.009, 0.010 and 0.008 mg kg-1 in the absence of the matrix and in the presence of crystal and brown sugar matrix, respectively. Repeatability lay between 0.53 and 13.8%, precision ranged between 4.14 and 15.0%, and recovery remained between 84.2 and 113% in the case of DPV conducted in the absence of matrix and in the presence of the crystal sugar matrix, respectively.

Modificação superficial de fibras de juta com descarga corona para melhora da aderência com matriz poliéster

Seeking alternatives for the total or partial substitution of synthetic fibers for natural fibers, with reinforcement in polymeric materials, this work was conducted with the objective of evaluating the treatment with corona discharge on the adherence of juta fibers with resin. The fibers were exposed to corona discharge for 1, 5, 10 and 15 minutes, as well as after treatment with hot water, molding composites fiber-reinforced with filaments treated for 10 and 15 minutes, and without the treatment. The chemical structures were evaluated by spectrometry in the region of Fourier transform infrared with attenuated total reflection (FTIR/ATR), observing the formation of a new band and the increase in the absorption of groupings with oxygen. The thermal analyses, such as thermogravimetry (TG) and differential scanning calorimetry (DSC) revealed the degradation of cellulose, hemicellulose and lignin. The microstructural characterization by scanning electron microscopy (SEM) showed changes in the surface of the fiber, such as roughness, superficial depressions, surface degradation and cavity formation. The adhesion of the fibers was evaluated by the pullout test, allowing us to verify the increase in adhesion strength after treatment with corona discharge. In conclusion, the treatment with corona discharge changes the surface of the juta fibers, resulting in better adherence with the resin.

Cathodic stripping voltammetric determination of arsenic in sugarcane brandy at a modified carbon nanotube paste electrode

We have developed an eletroanalytical method that employs Cu2+ solutions to determine arsenic in sugarcane brandy using an electrode consisting of carbon paste modified with carbon nanotubes (CNTPE) and polymeric resins. We used linear sweep (LSV) and differential-pulse (DPV) voltammetry with cathodic stripping for CNTPE containing mineral oil or silicone as binder. The analytical curves were linear from 30 to 110 μg L−1 and from 10 to 110 μg L−1 for LSV and DPV, respectively. The limits of detection (L.O.D.) and quantification (L.O.Q.) of CNTPE were 10.3 and 34.5 μg L−1 for mineral oil and 3.4 and 11.2 μg L−1 for silicone. We applied this method to determine arsenic in five commercial sugarcane brandy samples. The results agreed well with those obtained by hydride generation combined with atomic absorption spectrometry (HG AAS).

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.