TFM: Màster Universitari en Tècniques Cromatogràfiques AplicadesSIY009http://hdl.handle.net/10234/731472024-03-29T13:12:23Z2024-03-29T13:12:23ZIdentification of VOCs responsibles for odours in wastewater by HS-SPME with GC-EI-Q-OrbitrapGranell Granell, Marcoshttp://hdl.handle.net/10234/2005652022-10-27T01:22:39Z2022-06-30T00:00:00ZIdentification of VOCs responsibles for odours in wastewater by HS-SPME with GC-EI-Q-Orbitrap
Granell Granell, Marcos
This study evaluates the capabilities of identification of unknown compounds and the optimisation of the extraction technique for odour-causing volatile organic compounds (VOCs) in wastewater samples based on headspace solid-phase microextraction (HS-SPME). The water samples were analysed by gas chromatography coupled to mass spectrometry using a Q-Orbitrap mass analyser. A total of 3 wastewater samples from 3 WWTPs (Castellón: influent; Benicasim: outlet of the primary settling tank; Villarreal: outlet of the biological reactor) were mixed and used as a model for the development and optimisation of the method. Additionally, a total number of 16 samples were collected every 15 days from the three WWTP. In order to optimise the HS-SPME method, a multivariate approach using the response surface method was used obtaining optimum values of 3 mL of sample, 45ºC as extraction temperature and 0.6 g of NaCl (20% in the sample). To ensure reliable identification, the parameters of comprehensive score greater than 80, RSI>700 and ΔRI≤50 were established as reference values. As a result, 67 compounds could be identified, from which 12 were responsible for odours.
Treball Final de Màster Universitari en Tècniques Cromatogràfiques Aplicades (Pla de 2013). Codi: SIY009 Curs acadèmic: 2021-2022
2022-06-30T00:00:00ZDevelopment and validation of a QuEChERS-like method coupled to UHPLC-MS/MS for the determination of tobacco-specific toxicants in silicone personal samplersPalau Sánchez, Mireiahttp://hdl.handle.net/10234/1955982021-11-23T02:03:28Z2021-09-10T00:00:00ZDevelopment and validation of a QuEChERS-like method coupled to UHPLC-MS/MS for the determination of tobacco-specific toxicants in silicone personal samplers
Palau Sánchez, Mireia
Air pollution is currently a problem that affects all living species in the globe and a ubiquitous group of compounds is rising concern about their ubiquitous presence in the atmosphere. These are toxicants derived from tobacco consumption worldwide and humans are exposed to them constantly and involuntarily. This exposure can be studied through the thirdhand smoke (THS), which is the residual tobacco present in the air and surfaces after a cigarette has been smoked. This determination is conducted to urine samples but recently, silicone wristbands have been introduced as effective personal samplers as they can absorb a large number of compounds, which later are extracted and analysed to provide the amount of pollutants to which the person has been exposed during a period of time. This work purposes a method to determine simultaneously nicotine and five derivatives that are absorbed in a silicone wristband worn seven days as a personal passive sampler. For the optimization purposed, several optimization processes have been performed to reach to a method based on a QuEChERS extraction of the wristbands followed by a HPLC-MS/MS analysis. All compounds showed a good linearity whilst the extraction recoveries obtained ranged from 71-115% and the repeatability between 6-15%. As part of the validation process, two samples were analysed one being a non-smoker/non-exposed person and another being a smoker/exposed. Applying the method, it was able to identify all the target compounds in the smoker sample with levels of 2031ng·g-1 WB of nicotine, otherwise only nicotine and cotinine were detected in the non-smoker. With this it was proved the existence of ubiquitous tobaccospecific toxicants in the environment.
Treball Final de Màster Universitari en Tècniques Cromatogràfiques Aplicades (Pla de 2013). Codi: SIY009
Curs acadèmic: 2020-2021
2021-09-10T00:00:00ZDesign of a method for polycyclic aromatic hydrocarbons routine determination by liquid-liquid microextraction and GC-MS/MS: Optimisation and validationGracia-Marín, Elisahttp://hdl.handle.net/10234/1955952024-03-27T11:40:20Z2021-09-10T00:00:00ZDesign of a method for polycyclic aromatic hydrocarbons routine determination by liquid-liquid microextraction and GC-MS/MS: Optimisation and validation
Gracia-Marín, Elisa
This study focuses on the optimisation and validation of a method for the determination of Polycyclic Aromatic Hydrocarbons (PAHs) to be applied in real supply waters of the Zaragoza area. The supply water samples were analysed by gas chromatography coupled to tandem mass spectrometry using ion trap (GC-MS/MS IT) due to its great selectivity and sensitivity. Injections in GC were performed by programmable temperature vaporization (PTV) in solvent venting mode of the samples. A liquid-liquid microextraction (LLME) treatment was necessary to concentrate the sample for analysis. Moreover, in order to correct matrix effects, Isotopically-Labelled Internal Standard (ILIS) was added to the samples. Several experiments were carried out to optimise the PAHs extraction method, chromatography and MS/MS conditions. The study focused mainly on Acenaphthylene and Acenaphthene as these compounds were not included in the method in use at Valero Analítica. In addition, the research also focused on Benzo(𝛽)fluoranthene, Benzo(g,h,i)perylene, Benzo(𝜅)fluoranthene and Indeno(1,2,3-c,d)pyrene, compounds regulated by RD 140/2003. The results of this work indicate that a comprehensive study of the PAHs of interest can be performed on the optimised method. The validation provides positive data for all compounds except for Acenaphthylene and Acenaphthene, which have an (limit of quantification) LOQ more than three times higher than the rest of PAHs. The results of this study contribute to report more complete PAHs data and therefore to understand which compounds are found in drinking water.
Treball Final de Màster en Tècniques Cromatogràfiques Aplicades (Pla de 2013). Codi: SIY009 Curs acadèmic: 2020-2021
2021-09-10T00:00:00ZDeterminación de compuestos orgánicos volátiles y semivolátiles en aguas mediante el uso de HS-SPME-GC-MS y SBSE-GC-MS/MSMateu Boix, José Vicentehttp://hdl.handle.net/10234/1914472021-01-26T02:06:15Z2020-11-20T00:00:00ZDeterminación de compuestos orgánicos volátiles y semivolátiles en aguas mediante el uso de HS-SPME-GC-MS y SBSE-GC-MS/MS
Mateu Boix, José Vicente
Este trabajo de final del Máster en Técnicas Cromatográficas Aplicadas se basa en la
estancia de prácticas realizada en la empresa Eurofins Iproma S.L., situada en Castellón de la Plana. Dicha empresa es referencia en la realización de estudios, tomas de muestra y análisis en los campos ambiental y alimentario entre otros. Cuenta con diferentes sedes y laboratorios a lo largo de la península: Castellón, Valencia, Madrid, Barcelona, Sevilla, Zaragoza y Pontevedra. Además tiene un equipo formado por mas de 220 profesionales de diferentes especialidades, donde más del 60% son titulados superiores como: químicos, biólogos, ingenieros.
Eurofins Iproma Castellón es la sede central de la empresa. en su parte analítica se
pueden distinguir 5 secciones: Cromatografía (donde se han llevado a cabo las prácticas), Físico-Químico, Microbiología, Ecología Acuática y Registro. Cada sección tiene su función en la generación de la información requerida por los clientes que solicitan su análisis. La sección de cromatografía cuenta con diferentes subsecciones:
Volátiles, Semivolátiles y Líquidos. Durante estas prácticas se ha trabajado bajo el
sistema de calidad de la norma UNE-EN ISO/IEC 17025:2017.
Treball de Fi de Màster Universitari en Tècniques Cromatogràfiques Aplicades (Pla de 2013). Codi: SIY009. Curs 2019/2020
2020-11-20T00:00:00Z