2023
Authors
Vasconcelos, H; Matias, A; Mendes, J; Araujo, J; Dias, B; Jorge, PAS; Saraiva, C; de Almeida, JMMM; Coelho, LCC;
Publication
TALANTA
Abstract
Hydrogen peroxide is usually added to products to delay the development of microorganisms mainly in milk, hence increasing its stability over time, however the side effects can become devastating to human health.A technique is presented consisting of detecting hydrogen peroxide as an adulterant in milk through a sensor where pretreatment of the sample is not necessary, using a single use membrane. The detection of hydrogen peroxide in fresh-raw, whole, semi-skimmed and skimmed milk was performed using a luminol chem-iluminescence reaction.For hydrogen peroxide water solutions, a linear response was attained from 1.0 x 10-4 to 9.0 x 10-3 %w/w and an LOD (limit of detection) of 3.0 x 10-5 %w/w was determined. An R-squared value of 0.97 and a relative standard deviation lower than 10%, were achieved.Hydrogen peroxide concentration as low as 1.0 x 10-3 %w/w was measured for fresh-raw, skim and whole milk and for semi-skimmed milk, as low as 2.0 x 10-3 %w/w.The methodology presented, as long as our knowledge, is original, rapid, ecological and inexpensive. In regard of the sensitivity obtained, the methodology has great possibility to be applied in the detection of hydrogen peroxide in several areas. It is envisaged monitoring of food quality, agriculture systems and environment pollution.
2023
Authors
Lopes, T; Rodrigues, P; Cavaco, R; Capela, D; Ferreira, MFS; Guimaraes, D; Jorge, PAS; Silva, NA;
Publication
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
Abstract
Imaging the spatial distribution of chemical elements at a sample surface is a common application of laserinduced breakdown spectroscopy with vast scientific and technological applications. Yet, typical imaging solutions only explore the creation of two-dimensional maps, which can limit the interpretability of the results and further diagnostics in three-dimensional settings. Within this context, this work explores the combination of spectral imaging techniques and photogrammetry to deploy a versatile solution for the creation of threedimensional spectral imaging models. First, by making use of a numerical algorithm that is able to match features in the spectral image with those of the three-dimensional model, we show how to match the mesh from distinct sensor modalities. Then, we describe a possible visualization workflow, making use of dedicated photogrammetry and visualization software to easily deploy interactive models. Overall, the results demonstrate the versatility of our approach and pave for the development of novel spectral imaging diagnostic strategies that are able to deliver better qualitative analysis and insight in the three-dimensional space.
2023
Authors
Silva, AT; Figueiredo, R; Azenha, M; Jorge, PAS; Pereira, CM; Ribeiro, JA;
Publication
ACS SENSORS
Abstract
Over the past decade, molecular imprinting (MI) technologyhasmade tremendous progress, and the advancements in nanotechnology havebeen the major driving force behind the improvement of MI technology.The preparation of nanoscale imprinted materials, i.e., molecularlyimprinted polymer nanoparticles (MIP NPs, also commonly called nanoMIPs),opened new horizons in terms of practical applications, includingin the field of sensors. Currently, hydrogels are very promising forapplications in bioanalytical assays and sensors due to their highbiocompatibility and possibility to tune chemical composition, size(microgels, nanogels, etc.), and format (nanostructures, MIP film,fibers, etc.) to prepare optimized analyte-responsive imprinted materials.This review aims to highlight the recent progress on the use of hydrogelMIP NPs for biosensing purposes over the past decade, mainly focusingon their incorporation on sensing devices for detection of a fundamentalclass of biomolecules, the peptides and proteins. The review beginsby directing its focus on the ability of MIPs to replace biologicalantibodies in (bio)analytical assays and highlight their great potentialto face the current demands of chemical sensing in several fields,such as disease diagnosis, food safety, environmental monitoring,among others. After that, we address the general advantages of nanosizedMIPs over macro/micro-MIP materials, such as higher affinity towardtarget analytes and improved binding kinetics. Then, we provide ageneral overview on hydrogel properties and their great advantagesfor applications in the field of Sensors, followed by a brief descriptionon current popular routes for synthesis of imprinted hydrogel nanospherestargeting large biomolecules, namely precipitation polymerizationand solid-phase synthesis, along with fruitful combination with epitopeimprinting as reliable approaches for developing optimized protein-imprintedmaterials. In the second part of the review, we have provided thestate of the art on the application of MIP nanogels for screeningmacromolecules with sensors having different transduction modes (optical,electrochemical, thermal, etc.) and design formats for single use,reusable, continuous monitoring, and even multiple analyte detectionin specialized laboratories or in situ using mobiletechnology. Finally, we explore aspects about the development of thistechnology and its applications and discuss areas of future growth.
2023
Authors
Baptista, MC; Gomes, BM; Capela, D; Ferreira, MFS; Guimaraes, D; Silva, NA; Jorge, PAS; Silva, JJ; Braga, MH;
Publication
BATTERIES-BASEL
Abstract
Anode-less batteries are a promising innovation in energy storage technology, eliminating the need for traditional anodes and offering potential improvements in efficiency and capacity. Here, we have fabricated and tested two types of anode-less pouch cells, the first using solely a copper negative current collector and the other the same current collector but coated with a nucleation seed ZnO layer. Both types of cells used the same all-solid-state electrolyte, Li2.99Ba0.005ClO composite, in a cellulose matrix and a LiFePO4 cathode. Direct and indirect methods confirmed Li metal anode plating after charging the cells. The direct methods are X-ray photoelectron spectroscopy (XPS) and laser-induced breakdown spectroscopy (LIBS), a technique not divulged in the battery world but friendly to study the surface of the negative current collector, as it detects lithium. The indirect methods used were electrochemical cycling and impedance and scanning electron microscopy (SEM). It became evident the presence of plated Li on the surface of the current collector in contact with the electrolyte upon charging, both directly and indirectly. A maximum average lithium plating thickness of 2.9 mu m was charged, and 0.13 mu m was discharged. The discharge initiates from a maximum potential of 3.2 V, solely possible if an anode-like high chemical potential phase, such as Li, would form while plating. Although the ratings and energy densities are minor in this study, it was concluded that a layer of ZnO, even at 25 degrees C, allows for higher discharge power for more hours than plain Cu. It was observed that where Li plates on ZnO, Zn is not detected or barely detected by XPS. The present anode-less cells discharge quickly initially at higher potentials but may hold a discharge potential for many hours, likely due to the ferroelectric character of the electrolyte.
2023
Authors
Capela D.; Ferreira M.F.S.; Lima A.; Dias F.; Lopes T.; Guimarães D.; Jorge P.A.S.; Silva N.A.;
Publication
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
Abstract
Fast and precise identification of minerals in geological samples is of paramount importance for the study of rock constituents and for technological applications in the context of mining. However, analyzing samples based only on the extrinsic properties of the minerals such as color can often be insufficient, making additional analysis crucial to improve the accuracy of the methods. In this context, Laser-induced breakdown spectroscopy mapping is an interesting technique to perform the study of the distribution of the chemical elements in sample surfaces, thus allowing deeper insights to help the process of mineral identification. In this work, we present the development and deployment of a processing pipeline and algorithm to identify spatial regions of the same mineralogical composition through chemical information in a fast and automatic way. Furthermore, by providing the necessary labels to the results on a training sample, we can turn this unsupervised methodology into a classifier that can be used to generalize and classify minerals in similar but unseen samples. The results obtained show good accuracy in reproducing the expected mineral regions and extend the interpretability of previous unsupervised methods with a visualization tool for cluster assignment, thus paving for future applications in contexts requiring high-throughput mineral identification systems, such as mining.
2023
Authors
Ferreira, MFS; Guimaraes, D; Oliveira, R; Lopes, T; Capela, D; Marrafa, J; Meneses, P; Oliveira, A; Baptista, C; Gomes, T; Moutinho, S; Coelho, J; da Silva, RN; Silva, NA; Jorge, PAS;
Publication
SENSORS
Abstract
Evaluating the efficiency of surface treatments is a problem of paramount importance for the cork stopper industry. Generically, these treatments create coatings that aim to enhance the impermeability and lubrification of cork stoppers. Yet, current methods of surface analysis are typically time-consuming, destructive, have poor representativity or rely on indirect approaches. In this work, the use of a laser-induced breakdown spectroscopy (LIBS) imaging solution is explored for evaluating the presence of coating along the cylindrical surface and in depth. To test it, several cork stoppers with different shaped areas of untreated surface were analyzed by LIBS, making a rectangular grid of spots with multiple shots per spot, to try to identify the correspondent shape. Results show that this technique can detect the untreated area along with other features, such as leakage and holes, allowing for a high success rate of identification and for its performance at different depths, paving the way for future industry-grade quality control solutions with more complex surface analysis.
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