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Aumento da produtividade da extração sólido-líquido de hidrocarbonetos aromáticos policíclicos em amostras de materiais rodoviários
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| 4.36 MB | Adobe PDF |
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Abstract(s)
O presente trabalho teve como objetivo otimizar e automatizar o processo de extração sólido líquido de hidrocarbonetos aromáticos policíclicos (PAH) em amostras de material de revestimento/pavimento rodoviário, do tipo asfalto ou mistura betuminosa, visando aumentar a produtividade da metodologia analítica na empresa Eurofins Lab Environment Testting Portugal. O processo atualmente realizado na Eurofins consiste numa extração sólido-líquido, recorrendo a uma mistura de acetona-hexano (1:1), com agitação mecânica durante 60 min. Posteriormente, o extrato obtido é sujeito a duas etapas de lavagem com água desionizada, sendo a quantificação de PAH realizada por cromatografia gasosa acoplada à espetrometria de massa (GC-MS). Assim, com este estudo pretendeu-se otimizar a metodologia, com foco na diminuição do tempo de extração, na redução das etapas de lavagem e na automatização do processo. No âmbito da otimização do tempo de extração, foram realizados ensaios com o intuito de reduzir o tempo de extração atual de 60 min. Em amostras com concentrações superiores a 615 μg/mL de PAH, verificou-se uma redução acentuada na eficiência de extração para tempos de 15 a 45 min, comprometendo significativamente a capacidade de extração. Estudou-se ainda, a possibilidade da eliminação da segunda etapa de lavagem. Os resultados demonstraram que
uma única lavagem é suficiente para garantir taxas de recuperação comparáveis às do procedimento atual, sem perdas estatisticamente significativas de eficiência (cerca de 85 %). No que diz respeito à automatização do processo, foi avaliada a implementação do equipamento automatizado de extração EDGE. Apesar de uma boa concordância (variações inferiores a 18 %) entre os resultados obtidos pelos métodos manual e automatizado em
amostras com baixa concentração de PAH, são necessários estudos complementares com amostras que apresentem teores de PAH significativamente superiores, para uma validação definitiva quanto à eficácia da extração usando o equipamento EDGE. Desta forma, embora o tempo de extração seja um parâmetro crucial no rendimento do processo, foi possível reduzi-lo entre 25 e 75 %, para concentrações de PAH inferiores a 615 μg/mL. A eliminação da segunda lavagem mostrou-se viável, permitindo uma redução tanto no tempo do processo como no consumo de reagentes e materiais, e assim, promover um processo mais sustentável e eficiente. A implementação do sistema EDGE demonstrou potencial para automatização do processo, embora ainda careça de estudos adicionais. Este estudo permitiu viabilizar a implementação do sistema EDGE para a extração de PAH em amostras de revestimento rodoviário, contribuindo para a sustentabilidade, aumento da produtividade e modernização da metodologia analítica na Eurofins.
The aim of this study was to optimise and automate the solid-liquid extraction process of polycyclic aromatic hydrocarbons (PAH) in road surfacing material samples, such as asphalt or bituminous mixtures, in order to increase the productivity of the analytical methodology used at Eurofins Lab Environment Testing Portugal. The process currently employed at Eurofins involves a solid–liquid extraction using a 1:1 acetone–hexane mixture, with mechanical agitation for 60 min. Subsequently, the extract obtained is subjected to two washing steps with deionised water, and the quantification of PAH is performed by gas chromatography coupled with mass spectrometry (GC-MS). Thus, this study aimed to optimise the methodology, focusing on reducing extraction time, reducing washing steps and automating the process As part of the extraction time optimisation, tests were conducted to reduce the current extraction time of 60 min. In samples with concentrations above 615 μg/mL of PAH, a marked reduction in extraction efficiency was observed for times of 15 to 45 minutes, significantly compromising extraction capacity. The potential elimination of the second washing step was also studied. The results showed that a single wash is sufficient to ensure recovery rates comparable to those of the current procedure, without statistically significant losses in efficiency (approximately 85%). Regarding automating the process, the implementation of EDGE automated extraction equipment was evaluated. Despite good concordance (variations below 18 %) between the results obtained by the manual and automated methods in samples with low PAH concentrations, further studies involving samples with higher PAH concentrations are required to definitively validate the effectiveness of extraction using EDGE. In summary, although extraction time is a critical parameter in process performance, it was possible to reduce it by between 25 % and 75 % for PAH concentrations below 615 μg/mL. The elimination of the second washing step proved viable, leading to a reduction in both processing time and the consumption of reagents and materials, thereby promoting a more sustainable and efficient process. The implementation of the EDGE system showed potential for automation, although further studies are still needed. This study enabled the implementation of the EDGE system for PAH extraction in road surface samples, contributing to sustainability, increased productivity and modernisation of the analytical methodology at Eurofins.
The aim of this study was to optimise and automate the solid-liquid extraction process of polycyclic aromatic hydrocarbons (PAH) in road surfacing material samples, such as asphalt or bituminous mixtures, in order to increase the productivity of the analytical methodology used at Eurofins Lab Environment Testing Portugal. The process currently employed at Eurofins involves a solid–liquid extraction using a 1:1 acetone–hexane mixture, with mechanical agitation for 60 min. Subsequently, the extract obtained is subjected to two washing steps with deionised water, and the quantification of PAH is performed by gas chromatography coupled with mass spectrometry (GC-MS). Thus, this study aimed to optimise the methodology, focusing on reducing extraction time, reducing washing steps and automating the process As part of the extraction time optimisation, tests were conducted to reduce the current extraction time of 60 min. In samples with concentrations above 615 μg/mL of PAH, a marked reduction in extraction efficiency was observed for times of 15 to 45 minutes, significantly compromising extraction capacity. The potential elimination of the second washing step was also studied. The results showed that a single wash is sufficient to ensure recovery rates comparable to those of the current procedure, without statistically significant losses in efficiency (approximately 85%). Regarding automating the process, the implementation of EDGE automated extraction equipment was evaluated. Despite good concordance (variations below 18 %) between the results obtained by the manual and automated methods in samples with low PAH concentrations, further studies involving samples with higher PAH concentrations are required to definitively validate the effectiveness of extraction using EDGE. In summary, although extraction time is a critical parameter in process performance, it was possible to reduce it by between 25 % and 75 % for PAH concentrations below 615 μg/mL. The elimination of the second washing step proved viable, leading to a reduction in both processing time and the consumption of reagents and materials, thereby promoting a more sustainable and efficient process. The implementation of the EDGE system showed potential for automation, although further studies are still needed. This study enabled the implementation of the EDGE system for PAH extraction in road surface samples, contributing to sustainability, increased productivity and modernisation of the analytical methodology at Eurofins.
Description
Keywords
Automation Gas Chromatography EDGE Mass Spectrometry PAH Extraction Optimisation Automatização Cromatografia gasosa Espetrometria de massa Extração de PAH Otimização