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Development of Analytical Methodologies for the Assessment of Odorous and Fragrance Compounds in Wastewater Treatment Plants

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Development of Analytical Methodologies for the Assessment of Odorous and Fragrance Compounds in Wastewater Treatment Plants DEVELOPMENT OF ANALYTICAL METHODOLOGIES FOR THE ASSESSMENT OF ODOROUS AND FRAGRANCE COMPOUNDS IN WASTEWATER TREATMENT PLANTS Anna GODAYOL BOIX Dipòsit legal: Gi. 776-2014 http://hdl.handle.net/10803/133077 ADVERTIMENT. L'accés als continguts d'aquesta tesi doctoral i la seva utilització ha de respectar els drets de la persona autora. Pot ser utilitzada per a consulta o estudi personal, així com en activitats o materials d'investigació i docència en els termes establerts a l'art. 32 del Text Refós de la Llei de Propietat Intel·lectual (RDL 1/1996). Per altres utilitzacions es requereix l'autorització prèvia i expressa de la persona autora. En qualsevol cas, en la utilització dels seus continguts caldrà indicar de forma clara el nom i cognoms de la persona autora i el títol de la tesi doctoral. No s'autoritza la seva reproducció o altres formes d'explotació efectuades amb finalitats de lucre ni la seva comunicació pública des d'un lloc aliè al servei TDX. Tampoc s'autoritza la presentació del seu contingut en una finestra o marc aliè a TDX (framing). Aquesta reserva de drets afecta tant als continguts de la tesi com als seus resums i índexs. ADVERTENCIA. El acceso a los contenidos de esta tesis doctoral y su utilización debe respetar los derechos de la persona autora. Puede ser utilizada para consulta o estudio personal, así como en actividades o materiales de investigación y docencia en los términos establecidos en el art. 32 del Texto Refundido de la Ley de Propiedad Intelectual (RDL 1/1996). Para otros usos se requiere la autorización previa y expresa de la persona autora. En cualquier caso, en la utilización de sus contenidos se deberá indicar de forma clara el nombre y apellidos de la persona autora y el título de la tesis doctoral. No se autoriza su reproducción u otras formas de explotación efectuadas con fines lucrativos ni su comunicación pública desde un sitio ajeno al servicio TDR. Tampoco se autoriza la presentación de su contenido en una ventana o marco ajeno a TDR (framing). Esta reserva de derechos afecta tanto al contenido de la tesis como a sus resúmenes e índices. WARNING. Access to the contents of this doctoral thesis and its use must respect the rights of the author. It can be used for reference or private study, as well as research and learning activities or materials in the terms established by the 32nd article of the Spanish Consolidated Copyright Act (RDL 1/1996). Express and previous authorization of the author is required for any other uses. In any case, when using its content, full name of the author and title of the thesis must be clearly indicated. Reproduction or other forms of for profit use or public communication from outside TDX service is not allowed. Presentation of its content in a window or frame external to TDX (framing) is not authorized either. These rights affect both the content of the thesis and its abstracts and indexes. Doctoral Thesis DEVELOPMENT OF ANALYTICAL METHODOLOGIES FOR THE ASSESSMENT OF ODOROUS AND FRAGRANCE COMPOUNDS IN WASTEWATER TREATMENT PLANTS Anna Godayol Boix 2014 Doctoral program in Experimental Sciences and Sustainability Supervised by Dr. Enriqueta Anticó Daró and Dr. Juan Manuel Sánchez Navarro This manuscript has been presented to obtain the degree of Doctor by the Universitat de Girona Dr. Enriqueta Anticó Daró and Dr. Juan Manuel Sánchez Navarro, of Universitat de Girona, WE DECLARE: That the thesis titles Development of analytical methodologies for the assessment of odorous and fragrance compounds in wastewater treatment plants, presented by Anna Godayol Boix to obtain a doctoral degree, has been completed under our supervision. For all intentions and purposes, we hereby sign this document. Dr. Enriqueta Anticó Daró Dr. Juan Manuel Sánchez Navarro Girona, 10TH of February of 2014 The development of this thesis has been funded by the following research project from the Spanish Government: “Evaluación de la eficacia de las plantas de tratamiento de aguas residuales en la eliminación de compuestos orgánicos emergentes de las aguas para su reutilización” (CTM2008-06847- C02-02). Anna Godayol Boix gratefully acknowledges a PhD research grant from the Generalitat de Catalunya (2013FI_B2 00126) and the financial support of the DRAC program (Xarxa Vives d’Universitats) for her research stay at the University Rovira i Virgili (Tarragona). The research described in this thesis has result in the publication of three scientific papers and two more that are in preparation: . Godayol, A., Alonso, M., Besalú, E., Sanchez, J.M., Anticó, E. Odour-causing compounds in wastewater treatment plants: Evaluation of solid-phase microextraction as a concentration technique. Journal of Chromatography A, 1218 (2011) 4863-4868. Impact factor: 4.612 (2012) Field, rank: Chemistry, Analytical; position 6 of 75 (1st quartile) Times cited: 6 (17/12/2013) . Godayol, A., Alonso, M., Sanchez, J.M., Anticó, E. Odour-causing compounds in air samples: Gas-liquid partition coefficients and determination using solid-phase microextraction and GC with mass spectrometric detection. Journal of Separation Science, 36 (2013) 1045-1053. Impact factor: 2.591 (2012) Field, rank: Chemistry, Analytical; position 25 of 75 (2nd quartile) Times cited: 2 (17/12/2013) . Godayol, A., Marcé, R.M., Borrull, F., Anticó, E., Sanchez, J.M. Development of a method for the monitoring of odor-causing compounds in atmospheres surrounding wastewater treatment plants. Journal of Separation Science, 36 (2013) 1621-1628. Impact factor: 2.591 (2012) Field, rank: Chemistry, Analytical; position 25 of 75 (2nd quartile) Times cited: 0 (17/12/2013) . Godayol, A., Besalú, E., Anticó, E., Sanchez, J.M. Monitoring of sixteen fragrance allergens and two polycyclic musks in wastewaters by solid phase microextraction coupled to gas chromatography. In preparation. Godayol, A., Gonzalez-Olmos, R., Sanchez, J.M., Anticó, E. UV and chlorination for the degradation of fragrances in water samples. In preparation. INDEX OF TABLES Table 1.1. Compounds associated with the odorous emissions from WWTPs ......................... 13 Table 1.2. Characteristics of the commercially available SPME fibre coatings. PDMS: poly(dimethylsiloxane), PA: polyacrylate, DVB: divinylbenzene, CAR: carboxen, CW: carbowax, TR: templed resin ....................................................................................................................... 20 Table 1.3. Fragrances included in the SCCS list, with their chemical structures and main properties ................................................................................................................................... 26 Table 1.4. Chemical structure and main properties of musk fragrances ................................... 29 Table 3.1. Factor levels considered in the experimental design optimisation ......................... 52 Table 3.2. OTCs, retention times and m/z ratios of the target compounds. Values in bold are the quantifier ions. n.a.: not available ............................................................................................. 53 Table 3.3. Statistical results for the experimental design. Significance p-values are given for main effects, double and triple interactions and for curvature evidence. Most relevant single and double variable terms effects are also shown in decreasing order of importance ................... 56 Table 3.4. Quality parameters obtained in standard solutions analysis. Standard deviations are showed in parenthesis. a: intercept, Sa :standard deviation of the intercept, b: slope, Sb: standard deviation of the slope ................................................................................................................ 59 Table 3.5. Concentrations, recoveries and intra-day precision values (n=5) obtained in spiked milli-Q water solution and real sample analysis. Standard deviations are shown in parenthesis .................................................................................................................................................... 60 Table 3.6. Results obtained in WWTP samples analysis. Concentrations in μg·L-1. Standard deviations are showed in parenthesis. n.d.: not detected. (n=3) .............................................. 63 Table 4.1. Volatile compounds evaluated in the present study, with their OTCs, retention times and m/z ratios. n.a.: not available .............................................................................................. 73 Table 4.2. Quality parameters obtained in the analysis of gaseous standards. (-): not determined .................................................................................................................................................... 79 Table 4.3. Concentrations (µg·L-1) for the studied compounds found in wastewater samples at different WWTPs. Standard deviations are showed in parenthesis. n.d.: not detected. Last column shows the selected values for the spiked water sample used in the determination of partition coefficients .................................................................................................................. 81 Table 4.4. Partition coefficient (pc) values obtained for the target compounds applying the proposed method. Three independent samples were analysed by SPME (n=2) ....................... 82 Table 4.5. Results obtained in the analysis of WWTP gas samples. Concentrations in µg·m-3. n.d.: not detected ..............................................................................................................................
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