Dissolução eletrolítica de ligas de alumínio em cavacos e determinação dos elementos constituintes por espectrometria de emissão atômica com fonte de pasma (ICP-OES) / Electrolytic dissolution of aluminum alloys (Chip form) and multi-element determination by inductively coupled plasma optical emission spectrometry (ICP-OES)

AUTOR(ES)
DATA DE PUBLICAÇÃO

2001

RESUMO

Several aluminum alloys with different chips size were dissolved using aqua regia (HCl:HNO3,3:1). The residues of the dissolution procedure were either rejected or used in silicon volatilization with hydrofluoric acid before determination of Fe, Cu, Mn, Mg, Cr, Ni, Zn, Pb, Sn, Ti and Zr by ICP-OES. The influence caused by crescent amounts of aluminum in the determination of other elements and the probable spectral interference by Cu in determination of Zn (with or without electrolytic separation of Cu) was evaluated. The electrolytic dissolution of aluminum alloys was performed by pressing chips against a platinum electrode for the electrolysis to occur, so that way the chips behaved as the anode. A tube (body of syringe of 2.5mL) with perforations around the open base was used to contain the sample and Pt electrode. The alloy was placed on synthetic wool (perlon) in this tube. An acrylic dowel with a platinum wire across its interior was fixed in the superior part a tube with Teflon film, with an orifice through which the electrolytic solution flowed (HNO3 1 mol L-1; 4.5mL min-1). A platinum dish was fixed at the inferior extremity of the platinum wire to press the sample. The solution came out through the inferior orifices of the tube to a flask, from where it was again captured (with a peristaltic pump) to go into the superior part of the tube. In this flask, a Pt wire cathode was also placed. A current of 0,6A and ten minutes of electrolysis provided good results. Due to the partial dissolution, the knowledge of percentages of previous elements analyzed after total dissolution, or using certified reference material are necessary. The results were normalized by known percentages. The calculations were made by: 1-) the ratio between the concentration of the element determind, with the determined concentration of aluminum; 2-) the ratio between concentration of the element and the sum of the concentrations of the elements determined, including Al; 3-) the ratio between the concentration of element and the sum of the concentrations of the elements determined, without the aluminum. The relative standard deviations and accuracy were <10% for the elements Fe, Cu, Mg, Ni and Cr when the concentrations were >0.1%; for the Zn were 15%, when the concentration >0.2%, and <10% for concentration <0.2%. For Ti with concentration of about 0.1%, were 15%. Relative standards deviations for the Zr, with concentration of 0.002%, were always <10%. The element Pb, Sn and Mn didnt provide good results. For these determinations, the chemical dissolution of the elements with different nitric acid concentrations and temperature was evaluated. Two other cells for the electrolytic dissolution of Al alloys followed by online ICP-OES determination were examined.

ASSUNTO(S)

icp oes química analítica instrumental spectroscopy electrolytic dissolution instrumental analytical chemistry ligas de alumínio aluminum alloys qualitative analytical chemistry dissolução eletrolítica química analítica qualitativa espectrometria de emissão atômica com plasma de argônio induzido (icp oes) química analítica analytical chemistry

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