A novel strategy for direct elemental determination using laser-induced breakdown spectroscopy: fluence calibration

Autor(es)

Machado, Raquel C. ^[1] ; Babos, Diego Victor ^[1] ; Andrade, Daniel F. ^[1] ; Pereira-Filho, Edenir Rodrigues ^[1]

Afiliação do(s) autor(es)

^[1] Univ Fed Sao Carlos, Grp Appl Instrumental Anal, Dept Chem, POB 676, BR-13565905 Sao Carlos, Sao Carlos Stat - Brazil

• Tipo de documento: Artigo Científico
• Fonte: Journal of Analytical Atomic Spectrometry; v. 36, n. 10 JUL 2021.
• Citações Web of Science: 0

Resumo

Quantitative analysis requires a lot of effort to obtain an adequate calibration method to overcome matrix effects employing direct solid analysis by laser-induced breakdown spectroscopy (LIBS). To this end, in this study, a new calibration strategy using different laser fluence values, named Fluence Calibration (FC), was developed and evaluated for LIBS quantitative analysis. In FC-LIBS, only one single calibration standard (a pellet with a known concentration of the analyte) and pellets of the sample are used to build a linear model from the emission signals acquired at different laser fluence values, optimized for each matrix sample used in the method development (printed circuit board - waste PCB and fertilizer samples). Satisfactory trueness was obtained for the determination of Al (94 to 115%) and Pb (98 to 100%) in PCB samples and Al, K, Mg, Na and P (ranging from 81 to 120%) in fertilizer samples, in which one sample of each matrix was used as a standard for calibration. For some fertilizer samples, the plasma normalization process did not occur and the matrix effects were not efficiently overcome using FC-LIBS. Standards for calibration were also prepared from salts and adequate figures of merit (i.e. accuracy and precision) were achieved using FC-LIBS for Al (trueness ranged from 82 to 114% and relative standard deviation - RSD 14%) in PCB samples and for Al and P (trueness ranged from 82 to 114% and RSD from 11 to 31%) in fertilizer samples. The FC-LIBS method is an alternative among the nontraditional methods of calibration that allows faster and simpler pellet preparation compared to traditional univariate calibration strategies, acquisition and data treatment for the direct analysis of complex solid samples. (AU)

• Processo FAPESP: 16/17304-0 - Proposição de métodos para a análise direta de amostras de lixo eletrônico: determinação de elementos preciosos, estratégicos e tóxicos em circuitos eletrônicos e telas touch screen
• Beneficiário: Daniel Fernandes de Andrade
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 19/24223-5 - Calibração empregando Laser-Induced Breakdown Spectroscopy (LIBS): alternativas, desafios, comparação das propostas existentes e proposição de um procedimento universal
• Beneficiário: Edenir Rodrigues Pereira Filho
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 16/01513-0 - Combinação de LIBS (Laser-Induced Breakdown Spectroscopy) e ICP OES (Inductively Coupled Plasma Optical Emission Spectrometry) na análise de amostras de resíduo eletrônico (circuito eletrônico e polímeros), alimentos e líquidas de difícil preparação
• Beneficiário: Edenir Rodrigues Pereira Filho
• Modalidade de apoio: Auxílio à Pesquisa - Regular