Desenvolvimento de métodos analíticos para a determinação de elementos-traço em tintas anti-incrustantes por ICP OES e LA-ICP-MS

• Autor(a) principal: Silva, Thaiane Nolasco da
• Data de Publicação: 2020
• Tipo de documento: Dissertação
• Idioma: por
• Título da fonte: Biblioteca Digital de Teses e Dissertações da UERJ
• Texto Completo: http://www.bdtd.uerj.br/handle/1/16455
• topic: Tinta anti-incrustante; ICP OES; LA -ICP-MS; Toxicologia ambiental; Espectometria; Transporte marítimo; Antifouling paints; ENGENHARIAS::ENGENHARIA QUIMICA::TECNOLOGIA QUIMICA

The antifouling paints containing Cu, Pb, and Sn are used on the watercraft hulls to avoid the marine organisms fouling. Thus, because this type of paint is harmful to the environment, it is extremely important the determination of the metals at trace level with the use of sufficiently sensitive techniques, such as inductively coupled plasma optical emission spectrometry (ICP OES) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), with the submission of samples to appropriate treatment for further analysis. Therefore, in this work, methods were developed to determine trace elements in antifouling paints by LA-ICP-MS and ICP OES. The factors: sample mass and solutions of HNO3, HF, and HCl were optimized using the central composite design (CCD) of two and three factors. As a comparison, was used a dry method with the support of the muffle and subsequent dissolution in a heating plate, using solutions of HF and HNO3. In the method optimization by LA-ICP-MS, firstly, plate was painted with enriched paint with the standard solutions of Cu, Pb, and Sn. This plate was used for the optimization of the factors by CCD with three factors, such as radiofrequency power (W), carrier gas flow He (mL min-1), and sampling depth (mm). For the evaluation of the concentrations between the methods, non-parametric analysis of longitudinal data was performed, with the aid of the “nparLD” package, through the estimate of the relative treatment effect (RTE), as well as the WTS (Wald Test Statistics) and Hotelling T2 tests, and analysis of variance (ANOVA). Relative of the study of RTE, the determination of Sn, did not show an effect with statistical significance (RTE < 0,5) between LA-ICP-MS and dry method. For the determination of Cu, the method microwave-assisted digestion using the acid mixture of HNO3+ HF has no significant effect compared to that of the dry method. On the other hand, for the determination of Pb, none of the methods showed an effect with statistical significance, except LA-ICP-MS. In general, the methods had a statistically significant difference (p-value < 0.05) using WTS and Hotelling T² tests as well as ANOVA. However, even with all the mixtures of acids allowing efficient extraction of the analytes, the one that stood out was that used HF + HNO3, mainly for ensure the dissolution of Silica present in paints.