A determinação de fluoreto por eletrodo íon seletivo (ISE) em nanotubos de carbono (CNTs) é proposta após a decomposição por piroidrólise. Até 1 g de amostra pode ser decomposta, obtendo-se assim baixos limites de detecção (1,5 mg g -1 ), boa precisão (RSD < 5%) e exatidão (concordância maior do que 95% com os valores dos materiais de referencia certificados (CRMs) e combustão iniciada por microondas (MIC)). O fluoreto é absorvido em água e a solução resultante pode ser analisada diretamente por ISE. A pirohidrólise é simples de ser executada e não requer instrumentação sofisticada, sendo bastante atrativa para controle de fluoreto em NTCs em análises de rotina.Fluoride determination by ion selective electrode (ISE) in carbon nanotubes (CNTs) is proposed after pyrohydrolysis decomposition. Up to 1 g of CNTs could be decomposed improving the limit of detection (1.5 mg g -1 ), precision (RSD < 5%) and accuracy (agreement higher than 95% with values of certified reference materials (CRMs) and microwave-induced combustion (MIC)). Fluoride could be absorbed in water and the resulting solution can be analyzed by ISE. Pyrohydrolysis is easy to be performed and does not require any sophisticated instrumentation, which is attractive for routine fluoride control in CNTs.Keywords: carbon nanotubes, fluoride, ion selective electrode, pyrohydrolysis sample preparation
IntroductionNowadays, carbon nanotubes (CNTs) are considered a promising material for several nanotechnological applications (mainly in science and medicine) due to their extraordinary electronic, mechanical and structural properties. [1][2][3][4][5] The properties of CNTs could be chemically modified by addition of halogens, as fluorine. [6][7][8][9] Some authors have reported that the functionalization of CNTs with fluorine significantly changes their electrical, mechanical and optical properties. 8 In this sense, the determination of F in CNT is an important task in order to evaluate the performance of this material for many applications. However, there is a lack of analytical procedures suitable for CNT analysis, especially related to F determination. Some works have been published concerning CNT analysis, but they are generally devoted to structural characterization, purity evaluation, metals determination, among others. 10-14 Current procedures recommended for CNT analysis are related to microwaveassisted acid digestion or dry ashing. 10,11 However, these procedures used for sample digestion are not suitable for further halogens due to the low sample mass that could be digested or the low decomposition efficiency. 10,13 Additionally, some drawbacks are related to analyte losses during sample treatment, even using closed vessels. 15 Recently, a method was proposed for halogen determination in CNTs using microwave-induced combustion (MIC) for sample decomposition and inductively coupled plasma mass spectrometry (ICP-MS), ion chromatography (IC) and also ion selective electrode (ISE) for analyte measurement. 16 It was possible to digest up to 500 mg of CNT s...