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Abstract(s)
O presente relatório traduz o trabalho que foi realizado na Symington Family Estates, S.A., inserido no âmbito da unidade curricular Dissertação/Estágio do 2º ano do Mestrado em Engenharia Química no ramo de Qualidade no Instituto Superior de Engenharia do Porto. Esta tese de mestrado tem o tema “Validação de método para determinação de 2,4,6-tricloroanisol em rolhas por HS-SPME-GC-ECD”.
Os principais objetivos desta dissertação foram implementar o método de análise interno para todos os tipos de rolhas que a empresa recebe e validar o método, garantindo que os resultados obtidos são precisos e exatos.
Para além do desenvolvimento do tema de estágio, também foi dado apoio aos técnicos do laboratório em todas as análises realizadas aos diferentes materiais utilizados no engarrafamento.
Para a validação do método, garantiu-se que a gama de trabalho era adequada, determinaram-se os limites de deteção (LOD) e de quantificação (LOQ), a precisão (repetibilidade, precisão intermédia), a exatidão (ensaios de recuperação, ensaios interlaboratoriais), traçaram-se as cartas de contolo e determinou-se a incerteza do resultado.
A gama de trabalho utilizada foi de 0,5 a 10,0 ng/L; o limite de deteção foi de 0,2 ng/L; o limite de quantificação foi de 0,6 ng/L; os coeficientes de variação da repetibilidade foram de 7,0 e 3,3% para as soluções padrão de 0,5 e 10,0 ng/L, respetivamente; o desvio-padrão da precisão intermédia foi de 0,2 ng/L e os coeficientes de variação foram de 5,8 e 6,8% para as soluções padrão de controlo de 2,0 e 4,0 ng/L, respetivamente; as taxas de recuperação obtidas foram entre 93 e 109%; os z-scores obtidos foram de 0, 0,4 e 0,8, sendo todos resultados aceitáveis. Assim, garantiu-se que todos os parâmetros deste método foram validados.
Os pontos das cartas de controlo das soluções padrão de controlo com 2,0 e 4,0 ng/L de 2,4,6-TCA e dos declives das retas de calibração encontram-se dentro dos limites inferior e superior de controlo.
A incerteza expandida foi de 0,3 ng/L, permitindo assim que a empresa tenha segurança quando rejeitar um lote de rolhas por excesso de 2,4,6-TCA.
O valor estimado para cada análise de 2,4,6-TCA em rolhas foi de 5,47 €. A implementação deste método na Symington permite uma poupança de cerca de 17,53 €/amostra para a empresa.
This report reflects the work that was carried out at Symington Family Estates S.A., inserted in the curricular unit Dissertation / Internship of the 2nd year of the Master in Chemical Engineering at the Instituto Superior de Engenharia do Porto. This thesis has the theme "Validation of method for determination of 2,4,6-trichloroanisol in corks by HS-SPME-GCECD". The main objectives of this dissertation were to implement the internal analysis method for all types of corks that the company receives and validate the method, ensuring that the results obtained are accurate and exact. In addition to the development of the thesis theme, support was also given to laboratory workers in all analyzes carried out on the different materials used in bottling of wine. For the validation of the method, it was ensured that the range of work was adequate, imits of detection (LOD) and quantification (LOQ), precision (repeatability, intermediate precision), accuracy (recovery tests, assays interlaboratory), the charts were drawn and the uncertainty of the result was determined. The working range was 0,5 to 10,0 ng/L; the detection limit was 0,2 ng/L; the limit of quantification was 0,6 ng/L; the coefficients of variation of the repeatability were of 7,0 and 3,3% for standard solutions of 0,5 and 10,0 ng/L; the standard deviation of the intermediate precision was 0,2 ng/L and the coefficients of variation were 5,8 and 6,8% for standard solutions of 2,0 and 4,0 ng/L; recovery rates were between 93 and 109%; the z-scores obtained were 0, 0,4 and 0,8, all of which were acceptable. Thus, it was ensured that all parameters of this method were validated. The control chart points of the control standard solutions with 2,0 and 4,0 ng/L of 2,4,6- TCA and the slopes of the calibration lines are within the lower and upper control limits. The uncertainty of the result was 0,3 ng/L, thus allowing the company to have safety when rejecting a batch of corks for excess of 2,4,6-TCA. The estimated value for each analysis of 2,4,6-TCA in stoppers was 5,47 €. The implementation of this method at Symington allowed a saving of around € 17.53 €/sample for the company.
This report reflects the work that was carried out at Symington Family Estates S.A., inserted in the curricular unit Dissertation / Internship of the 2nd year of the Master in Chemical Engineering at the Instituto Superior de Engenharia do Porto. This thesis has the theme "Validation of method for determination of 2,4,6-trichloroanisol in corks by HS-SPME-GCECD". The main objectives of this dissertation were to implement the internal analysis method for all types of corks that the company receives and validate the method, ensuring that the results obtained are accurate and exact. In addition to the development of the thesis theme, support was also given to laboratory workers in all analyzes carried out on the different materials used in bottling of wine. For the validation of the method, it was ensured that the range of work was adequate, imits of detection (LOD) and quantification (LOQ), precision (repeatability, intermediate precision), accuracy (recovery tests, assays interlaboratory), the charts were drawn and the uncertainty of the result was determined. The working range was 0,5 to 10,0 ng/L; the detection limit was 0,2 ng/L; the limit of quantification was 0,6 ng/L; the coefficients of variation of the repeatability were of 7,0 and 3,3% for standard solutions of 0,5 and 10,0 ng/L; the standard deviation of the intermediate precision was 0,2 ng/L and the coefficients of variation were 5,8 and 6,8% for standard solutions of 2,0 and 4,0 ng/L; recovery rates were between 93 and 109%; the z-scores obtained were 0, 0,4 and 0,8, all of which were acceptable. Thus, it was ensured that all parameters of this method were validated. The control chart points of the control standard solutions with 2,0 and 4,0 ng/L of 2,4,6- TCA and the slopes of the calibration lines are within the lower and upper control limits. The uncertainty of the result was 0,3 ng/L, thus allowing the company to have safety when rejecting a batch of corks for excess of 2,4,6-TCA. The estimated value for each analysis of 2,4,6-TCA in stoppers was 5,47 €. The implementation of this method at Symington allowed a saving of around € 17.53 €/sample for the company.
Description
Keywords
Validação de método HS-SPME-GC-ECD 2,4,6-tricloroanisol Rolhas Validation of method HS-SPME-GC-ECD 2,4,6-trichloroanisol Corks