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Abstract(s)
O presente trabalho insere-se no âmbito da unidade curricular de “Dissertação/Estágio” do Mestrado em Engenharia Química, na área de especialização de Qualidade, a realizar em contexto industrial na empresa Colep, sediada em Vale de Cambra. Tratando-se a Colep de uma empresa líder em contract manufacturing e com fábricas em todo o Mundo, é necessário assegurar que os métodos utilizados para a determinação de qualquer componente solicitado pelo cliente, sejam métodos devidamente validados e com resultados de confiança. O estágio em questão teve como objetivo a avaliação da precisão, nomeadamente a repetibilidade e precisão intermédia, na determinação de Trietil Citrato (TEC), Etilhexilglicerina (Sensiva) e Farnesol em desodorizantes e antitranspirantes. Estes compostos são adicionados ao produto na sua formulação procurando proporcionar ao mesmo propriedades emolientes, surfactantes, antimicrobianas, entre outras. A determinação de TEC, Sensiva e Farnesol foi efetuada por Cromatografia Gasosa com Detetor por Ionização de Chama (GC-FID). Foram executados dois métodos, Método A, fornecido por um cliente e o Método B, desenvolvido pela empresa, por dois operadores, 1 e 2. A precisão foi avaliada através da repetibilidade e precisão intermédia. Foi ainda efetuada a comparação entre os dois métodos. Verificou-se uma melhor repetibilidade para o operador 1 que para o operador 2 nos dois métodos. O coeficiente de variação associado ao operador 2 foi superior a 10% em algumas determinações. Para a precisão intermédia, de cada princípio ativo e para cada método considerou-se a variação da variável operador. Todos os resultados obtidos foram inferiores a 10%, exceto para as áreas da amostra relativamente ao TEC e Sensiva no Método B. Pretendeu-se verificar se existiam diferenças significativas entre os métodos A e B, relativamente às suas precisões, efetuando-se o teste Fisher-Snedecor. Verificou-se que na determinação de TEC e Farnesol não se observaram diferenças significativas ao contrário do que se constatou na determinação de TEC e Sensiva. Por fim, concluiu-se que o produto estava conforme uma vez que que as percentagens de TEC, Sensiva e Farnesol obtidas se apresentaram dentro do intervalo de valores especificados para ambos os métodos.
This thesis falls within the context of the curricular unit of “Dissertation/Internship” of Master in Chemical Engineering, branch in Quality, carried out in an industrial context at Colep, located in Vale de Cambra. Since Colep is a leading contract manufacturing company with factories all over the world, it is needed to ensure that the methods used to determine any component requested by the client, that can be effectively performed and with reliable results. The main goal was assessment of precision of Triethyl Citrate (TEC), Ethylhexylglycerine (Sensiva) and Farnesol in deodorants and antiperspirants. These compounds are added in the product formulation to provide emollient, surfactant and antimicrobial proprieties, among others. The determination of TEC, Sensiva and Farnesol was carried out by Gas Chromatography with Flame Ionization Detetor (GC-FID). Two methods were performed by two operators, 1 and 2, Method A, provided by a customer and the Method B, developed by the company. The precision was evaluated through repeatability and intermediate precision. A better repeatability was found for operator 1 than for operator 2 in both methods. The coefficient of variation of more than 10% was observed for operator 2 in some determinations. Concerning the intermediate precision of each active principle and for each method, the operator was the variable changed. All the coefficient of variation obtained were less than 10%, except for the sample areas relative to TEC and Sensiva in Method B. The Snedecor F test was applied to see if there were significant differences between method A and method B. For TEC and Farnesol determination no significant differences were observed between methods, contrary to what was found in the determination of TEC and Sensiva. Finally, it was possible to conclude that the product was compliant since the percentages of TEC, Sensiva and Farnesol obtained were within the range of specified values.
This thesis falls within the context of the curricular unit of “Dissertation/Internship” of Master in Chemical Engineering, branch in Quality, carried out in an industrial context at Colep, located in Vale de Cambra. Since Colep is a leading contract manufacturing company with factories all over the world, it is needed to ensure that the methods used to determine any component requested by the client, that can be effectively performed and with reliable results. The main goal was assessment of precision of Triethyl Citrate (TEC), Ethylhexylglycerine (Sensiva) and Farnesol in deodorants and antiperspirants. These compounds are added in the product formulation to provide emollient, surfactant and antimicrobial proprieties, among others. The determination of TEC, Sensiva and Farnesol was carried out by Gas Chromatography with Flame Ionization Detetor (GC-FID). Two methods were performed by two operators, 1 and 2, Method A, provided by a customer and the Method B, developed by the company. The precision was evaluated through repeatability and intermediate precision. A better repeatability was found for operator 1 than for operator 2 in both methods. The coefficient of variation of more than 10% was observed for operator 2 in some determinations. Concerning the intermediate precision of each active principle and for each method, the operator was the variable changed. All the coefficient of variation obtained were less than 10%, except for the sample areas relative to TEC and Sensiva in Method B. The Snedecor F test was applied to see if there were significant differences between method A and method B. For TEC and Farnesol determination no significant differences were observed between methods, contrary to what was found in the determination of TEC and Sensiva. Finally, it was possible to conclude that the product was compliant since the percentages of TEC, Sensiva and Farnesol obtained were within the range of specified values.
Description
Keywords
Cromatografia Gasosa Trietil Citrato Etilhexilglicerina Farnesol Repetibilidade Precisão Intermédia Comparação de métodos Gas Chromatography Triethyl Citrate Ethylhexylglycerine Repeatability Intermediate Precision Methods comparison