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	Author	Neven, L.; Barich, H.; Rutten, R.; De Wael, K.
	Title	Novel (photo)electrochemical analysis of aqueous industrial samples containing phenols			Type	A1 Journal article
	Year	2022	Publication	Microchemical journal	Abbreviated Journal
	Volume	181	Issue		Pages	107778-11
	Keywords	A1 Journal article; Engineering sciences. Technology; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
	Abstract	Phenols are considered as toxic pollutants and their discharge into the environment by industries is regulated by a concentration limit. As these limits are in the low mg L−1 to µg L−1-range, sensitive methods are necessary to detect these phenols. Here, aqueous industrial phenolic samples throughout a cleaning process were analyzed by two novel electrochemical sensors. Both the photoelectrochemical (PEC) sensor and the square wave voltammetric (SWV) sensor could successfully follow the decrease of the concentration of phenols along the industrial cleaning process. The discharge sample (μg L−1) could only be analyzed by the PEC sensor and not by the SWV sensor, as the phenolic concentration was close to the LOD of the latter. With HPLC-diode array detector (DAD) measurements, classical phenols such as phenol (PHOH), hydroquinone, resorcinol and o-cresol could be identified in the industrial samples, and their presence could be linked to the electrochemical responses. At last, the performance of the PEC and SWV sensors were compared with commercial colorimetric and chemical oxygen demand (COD) test kits. This comparison demonstrated the high sensitivity of the PEC sensor in the μg L−1 concentrated phenolic samples. Together with the identification of the redox peaks through HPLC-DAD analysis, the SWV sensor can be a powerful tool in the qualitative analysis of mg L−1 concentrated phenolic samples due to its speed, simplicity and absence of laborious sample pre-treatment steps.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000837838400003	Publication Date	2022-07-20
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	0026-265x; 0026-265x	ISBN		Additional Links	UA library record; WoS full record
	Impact Factor		Times cited		Open Access	OpenAccess
	Notes				Approved	no
	Call Number	UA @ admin @ c:irua:189428			Serial	8906
Permanent link to this record



	Author	Neven, L.; Barich, H.; Ching, H.Y.V.; Khan, S.U.; Colomier, C.; Patel, H.H.; Gorun, S.M.; Verbruggen, S.; Van Doorslaer, S.; De Wael, K.
	Title	Correlation between the fluorination degree of perfluorinated zinc phthalocyanines, their singlet oxygen generation ability, and their photoelectrochemical response for phenol sensing			Type	A1 Journal article
	Year	2022	Publication	Analytical chemistry	Abbreviated Journal	Anal Chem
	Volume	94	Issue	13	Pages	5221-5230
	Keywords	A1 Journal article; Organic synthesis (ORSY); Sustainable Energy, Air and Water Technology (DuEL); Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
	Abstract	Electron-withdrawing perfluoroalkyl peripheral groups grafted on phthalocyanine (Pc) macrocycles improve their single-site isolation, solubility, and resistance to self-oxidation, all beneficial features for catalytic applications. A high degree of fluorination also enhances the reducibility of Pcs and could alter their singlet oxygen (1O2) photoproduction. The ethanol/toluene 20:80 vol % solvent mixture was found to dissolve perfluorinated FnPcZn complexes, n = 16, 52, and 64, and minimize the aggregation of the sterically unencumbered F16PcZn. The 1O2 production ability of FnPcZn complexes was examined using 9,10-dimethylanthracene (DMA) and 2,2,6,6-tetramethylpiperidine (TEMP) in combination with UV–vis and electron paramagnetic resonance (EPR) spectroscopy, respectively. While the photoreduction of F52PcZn and F64PcZn in the presence of redox-active TEMP lowered 1O2 production, DMA was a suitable 1O2 trap for ranking the complexes. The solution reactivity was complemented by solid-state studies via the construction of photoelectrochemical sensors based on TiO2-supported FnPcZn, FnPcZn\|TiO2. Phenol photo-oxidation by 1O2, followed by its electrochemical reduction, defines a redox cycle, the 1O2 production having been found to depend on the value of n and structural features of the supported complexes. Consistent with solution studies, F52PcZn was found to be the most efficient 1O2 generator. The insights on reactivity testing and structural–activity relationships obtained may be useful for designing efficient and robust sensors and for other 1O2-related applications of FnPcZn.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000786254500002	Publication Date	2022-03-22
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	0003-2700; 5206-882x	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor	7.4	Times cited		Open Access	OpenAccess
	Notes				Approved	Most recent IF: 7.4
	Call Number	UA @ admin @ c:irua:187522			Serial	7141
Permanent link to this record



	Author	Neven, L.; Barich, H.; Sleegers, N.; Cánovas, R.; Debruyne, G.; De Wael, K.
	Title	Development of a combi-electrosensor for the detection of phenol by combining photoelectrochemistry and square wave voltammetry			Type	A1 Journal article
	Year	2022	Publication	Analytica chimica acta	Abbreviated Journal
	Volume	1206	Issue		Pages	339732
	Keywords	A1 Journal article; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
	Abstract	The high toxicity, endocrine-disrupting effects and low (bio)degradability commonly attributed to phenolic compounds have promoted their recognition as priority toxic pollutants. For this reason, the monitoring of these compounds in industrial, domestic and agricultural streams is crucial to prevent and decrease their toxicity in our daily life. To confront this relevant environmental issue, we propose the use of a combi-electrosensor which combines singlet oxygen (1O2)-based photoelectrochemistry (PEC) with square wave voltammetry (SWV). The high sensitivity of the PEC sensor (being a faster alternative for traditional COD measurements) ensures the detection of nmol L−1 levels of phenolic compounds while the SWV measurements (being faster than the color test kits) allow the differentiation between phenolic compounds. Herein, we report on the development of such a combi-electrosensor for the sensitive and selective detection of phenol (PHOH) in the presence of related phenolic compounds such as hydroquinone (HQ), bisphenol A (BPA), resorcinol (RC) and catechol (CC). The PEC sensor was able to determine the concentration of PHOH in spiked river samples containing only PHOH with a recovery between 96% and 111%. The SWV measurements elucidated the presence of PHOH, HQ and CC in the spiked samples containing multiple phenol compounds. Finally, the practicality of the combi-electrosensor set-up with a dual SPE containing two working electrodes and shared reference and counter electrodes was demonstrated. As a result, the combination of the two techniques is a powerful and valuable tool in the analysis of phenolic samples, since each technique improves the general performance by overcoming the inherent drawbacks that they display independently.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000793070200016	Publication Date	2022-03-16
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	0003-2670; 1873-4324	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor		Times cited		Open Access	OpenAccess
	Notes				Approved	no
	Call Number	UA @ admin @ c:irua:187499			Serial	8848
Permanent link to this record



	Author	Neven, L.; Barich, H.; Pelmuş, M.; Gorun, S.M.; De Wael, K.
	Title	The role of singlet oxygen, superoxide, hydroxide, and hydrogen peroxide in the photoelectrochemical response of phenols at a supported highly fluorinated zinc phthalocyanine			Type	A1 Journal article
	Year	2022	Publication	ChemElectroChem	Abbreviated Journal
	Volume	9	Issue	6	Pages	e202200108-10
	Keywords	A1 Journal article; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
	Abstract	Photoelectrochemical (PEC) sensing of phenolic compounds using singlet oxygen (1O2)-generating photocatalysts has emerged as a powerful detection tool. However, it is currently not known how experimental parameters, such as pH and applied potential, influence the generation of reactive oxygen species (ROS) and their photocurrents. In this article, the PEC response was studied over the 6 to 10 pH range using a rotating (ring) disk (R(R)DE) set-up in combination with quenchers, to identify the ROS formed upon illumination of a supported photosensitizer, F64PcZn. The photocurrents magnitude depended on the applied potential and the pH of the buffer solution. The anodic responses were caused by the oxidation of O2.−, generated due to the quenching of 1O2 with −OH and the reaction of 3O2 with [F64Pc(3-)Zn]. The cathodic responses were assigned to the reduction of 1O2 and O2.−, yielding H2O2. These insights may benefit 1O2 – based PEC sensing applications.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000773947300003	Publication Date	2022-02-23
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	2196-0216	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor		Times cited		Open Access	OpenAccess
	Notes				Approved	no
	Call Number	UA @ admin @ c:irua:187524			Serial	8926
Permanent link to this record



	Author	Neven, L.
	Title	Singlet oxygen-based photoelectrochemical detection of phenolic contaminants			Type	Doctoral thesis
	Year	2022	Publication		Abbreviated Journal
	Volume		Issue		Pages	234 p.
	Keywords	Doctoral thesis; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
	Abstract	Phenolic compounds can be found everywhere in our daily lives but exhibit high toxicity, low (bio)degradability and hormone-disrupting effects when they are released in the environment. It is for this reason imperative to develop detection strategies for these pollutants. A promising approach involves the use of a photoelectrochemical (PEC) sensor. In this sensor, a photosensitiser (PS) type II, which generates 1O2 under illumination, is used to oxidise phenolic compounds present in the sample. The oxidised phenols are reduced at the electrode surface leading to the generation of an electrocatalytic redox cycle. In this thesis, an in-depth understanding, through the identification of the reactive oxygen species (ROS) in the PEC sensing mechanism, is obtained. The detection strategy is optimised by choosing the PS with the highest 1O2 production and by optimising the detection parameters so that the PEC sensor can be successfully applied for the detection of phenols in industrial samples. First, it was determined that the use of highly fluorinated zinc phthalocyanine derivatives, F52PcZn and F64PcZn, as photocatalysts was optimal for the sensing of phenol due to their high 1O2 production and improved single-site isolation. However, next to 1O2, it was shown that the ROS O2•- and H2O2 were also generated in the PEC sensor. Their contribution to the photocurrent response was studied by rotating disk electrode measurements in function of the pH and applied potential. After this, the PEC detection strategy was optimised in terms of pH and applied potential for the detection of doxycycline, cefadroxil, and phenol. It was found that the use of alkaline pH-levels led to nmol L-1-level detection limits. The combination with square wave voltammetry (SWV) was, also, proposed to allow the quantification and identification of phenolic compounds in a specific sample. At last, the developed PEC and SWV sensors were applied for the measurement of phenolic compounds in industrial water samples. The PEC sensor could follow the decrease of the phenolic concentration throughout the wastewater treatment process while the SWV sensor provided the electrochemical fingerprints of these samples. The thesis concluded that the use of the PEC sensor was advantageous in the measurement of lower concentrated phenolic samples due to its high sensitivity and fast measurement time in comparison to commercial test kits.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos		Publication Date
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN		ISBN		Additional Links	UA library record
	Impact Factor		Times cited		Open Access
	Notes				Approved	no
	Call Number	UA @ admin @ c:irua:187029			Serial	8932
Permanent link to this record



	Author	Moro, G.; Barich, H.; Driesen, K.; Montiel, N.F.; Neven, L.; Mendonca, C.D.; Thiruvottriyur Shanmugam, S.; Daems, E.; De Wael, K.
	Title	Unlocking the full power of electrochemical fingerprinting for on-site sensing applications			Type	A1 Journal article
	Year	2020	Publication	Analytical And Bioanalytical Chemistry	Abbreviated Journal	Anal Bioanal Chem
	Volume		Issue		Pages	1-14
	Keywords	A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
	Abstract	Electrochemical sensing for the semi-quantitative detection of biomarkers, drugs, environmental contaminants, food additives, etc. shows promising results in point-of-care diagnostics and on-site monitoring. More specifically, electrochemical fingerprint (EF)-based sensing strategies are considered an inviting approach for the on-site detection of low molecular weight molecules. The fast growth of electrochemical sensors requires defining the concept of direct electrochemical fingerprinting in sensing. The EF can be defined as the unique electrochemical signal or pattern, mostly recorded by voltammetric techniques, specific for a certain molecule that can be used for its quantitative or semi-quantitative identification in a given analytical context with specified circumstances. The performance of EF-based sensors can be enhanced by considering multiple features of the signal (i.e., oxidation or reduction patterns), in combination with statistical data analysis or sample pretreatments or by including electrode surface modifiers to enrich the EF. In this manuscript, some examples of EF-based sensors, strategies to improve their performances, and open challenges are discussed to unlock the full power of electrochemical fingerprinting for on-site sensing applications.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000523396300002	Publication Date	2020-04-04
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	1618-2642	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor	4.3	Times cited	3	Open Access
	Notes	; The presented review is the result of a concerted effort and fruitful discussions among enthusiastic, young, and (for the occasion) female researchers of the AXES research group, each of them with specific expertise and background, under the guidance of the corresponding author. The authors acknowledge FWO-Flanders, BOF-UA, IOF-UA, FAPESP and EU for funding. ;			Approved	Most recent IF: 4.3; 2020 IF: 3.431
	Call Number	UA @ admin @ c:irua:168563			Serial	6647
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	Author	Neven, L.; Thiruvottriyur Shanmugam, S.; Rahemi, V.; Trashin, S.; Sleegers, N.; Carrion, E.N.; Gorun, S.M.; De Wael, K.
	Title	Optimized photoelectrochemical detection of essential drugs bearing phenolic groups			Type	A1 Journal article
	Year	2019	Publication	Analytical chemistry	Abbreviated Journal	Anal Chem
	Volume	91	Issue	15	Pages	9962-9969
	Keywords	A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
	Abstract	The World Health Organization (WHO) model “List of Essential Medicines” includes among indispensable medicines antibacterials and pain and migraine relievers. Monitoring their concentration in the environment, while challenging, is important in the context of antibiotic resistance as well as their production of highly toxic compounds via hydrolysis. Traditional detection methods such as high-performance liquid chromatography (HPLC) or LC combined with tandem mass spectrometry or UV-vis spectroscopy are time-consuming, have a high cost, require skilled operators and are difficult to adapt for field operations. In contrast, (electrochemical) sensors have elicited interest because of their rapid response, high selectivity, and sensitivity as well as potential for on-site detection. Previously, we reported a novel sensor system based on a type II photosensitizer, which combines the advantages of enzymatic sensors (high sensitivity) and photoelectrochemical sensors (easy baseline subtraction). Under red-light illumination, the photosensitizer produces singlet oxygen which oxidizes phenolic compounds present in the sample. The subsequent reduction of the oxidized phenolic compounds at the electrode surface gives rise to a quantifiable photocurrent and leads to the generation of a redox cycle. Herein we report the optimization in terms of pH and applied potential of the photoelectrochemical detection of the hydrolysis product of paracetamol, i.e., 4-aminophenol (4-AP), and two antibacterials, namely, cefadroxil (CFD, beta-lactam antibiotic) and doxycycline (DXC, tetracycline antibiotic). The optimized conditions resulted in a detection limit of 0.2 mu mol L-1 for DXC, but in a 10 times higher sensitivity, 20 nmol L-1, for CFD. An even higher sensitivity, 7 nmol L-1, was noted for 4-AP.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000480499200086	Publication Date	2019-06-25
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	0003-2700; 5206-882x	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor	6.32	Times cited	2	Open Access
	Notes	; FWO and UA-BOF are acknowledged for financial support. The Center for Functional Materials of Seton Hall University is thanked for support (S.M.G. and E.N.C.). Joren Van Loon is thanked for the graphical abstract. This research was supported by the medium scale research infrastructure funding Hercules funding (SEM). ;			Approved	Most recent IF: 6.32
	Call Number	UA @ admin @ c:irua:161831			Serial	5763
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	Author	Trashin, S.; Rahemi, V.; Ramji, K.; Neven, L.; Gorun, S.M.; De Wael, K.
	Title	Singlet oxygen-based electrosensing by molecular photosensitizers			Type	A1 Journal article
	Year	2017	Publication	Nature communications	Abbreviated Journal	Nat Commun
	Volume	8	Issue		Pages	16108
	Keywords	A1 Journal article; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
	Abstract	Enzyme-based electrochemical biosensors are an inspiration for the development of (bio)analytical techniques. However, the instability and reproducibility of the reactivity of enzymes, combined with the need for chemical reagents for sensing remain challenges for the construction of useful devices. Here we present a sensing strategy inspired by the advantages of enzymes and photoelectrochemical sensing, namely the integration of aerobic photocatalysis and electrochemical analysis. The photosensitizer, a bioinspired perfluorinated Zn phthalocyanine, generates singlet-oxygen from air under visible light illumination and oxidizes analytes, yielding electrochemically-detectable products while resisting the oxidizing species it produces. Compared with enzymatic detection methods, the proposed strategy uses air instead of internally added reactive reagents, features intrinsic baseline correction via on/off light switching and shows C-F bonds-type enhanced stability. It also affords selectivity imparted by the catalytic process and nano-level detection, such as 20 nM amoxicillin in μl sample volumes.
	Address
	Corporate Author				Thesis
	Publisher		Place of Publication		Editor
	Language		Wos	000405466200002	Publication Date	2017-07-14
	Series Editor		Series Title		Abbreviated Series Title
	Series Volume		Series Issue		Edition
	ISSN	2041-1723	ISBN		Additional Links	UA library record; WoS full record; WoS citing articles
	Impact Factor	12.124	Times cited	26	Open Access
	Notes	; Evonik is thanked for providing samples of silicon and titanium oxides. Support from the National Science Foundation (SMG) for a portion of this work is gratefully acknowledged. FWO and UAntwerpen (BOF) are acknowledged for financial support. ;			Approved	Most recent IF: 12.124
	Call Number	UA @ admin @ c:irua:144538			Serial	5833
Permanent link to this record