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Publications

Publications by CAP

2016

On the enhancement of Er3+ diffusion in LiNbO3 crystals by Er3+/Ti4+ co-diffusion

Authors
Marques Martins de Almeida, JMMM; Sadac, C;

Publication
MATERIALS RESEARCH BULLETIN

Abstract
After carrying out a revision of the literature on the enhancement of Er3+ diffusion in LiNbO3 crystals by Er3+/Ti4+ co-diffusion and analyzing our own experimental results, we conclude that no reproducible results were reported, meaning that further research on this subject is necessary.

2016

Quantitative determinations and imaging in different structures of buried human bones from the XVIII-XIXth centuries by energy dispersive X-ray fluorescence - Postmortem evaluation

Authors
Guimaraes, D; Dias, AA; Carvalho, M; Carvalho, ML; Santos, JP; Henriques, FR; Curate, F; Pessanha, S;

Publication
TALANTA

Abstract
In this work, a non-commercial triaxial geometry energy dispersive X-ray Fluorescence (EDXRF) setup and a benchtop mu-XRF system were used to identify postmortem contamination in buried bones. For two of the individuals, unusually high concentrations of Cu and Pb, but also Zn (in one individual) were observed. The pigments of the burial shroud coverings have been identified as the source of contamination. Accurate and precise quantitative results were obtained by nondestructive process using fundamental parameters method taking into account the matrix absorption effects. A total of 30 bones from 13 individuals, buried between the mid-XVlllth to early XIXth centuries, were analyzed to study the elemental composition and elemental distribution. The bones were collected from a church in Almada (Portugal), called Ermida do Espirito Santo, located near the Tagus River and at the sea neighbourhood. The triaxial geometry setup was used to quantify Ca, Fe, Cu, Zn, Br, Sr and Pb of powder pressed bone pellets (n=9 for each bone). Cluster analysis was performed considering the elemental concentrations for the different bones. There was a clear association between some bones regarding Fe, Cu, Zn, Br and Pb content but not a categorization between cortical and trabecular bones. The elemental distribution of Cu, Zn and Pb were assessed by the benchtop p.-analysis, the M4 Tornado, based on a polycapillary system which provides multi-elemental 2D maps. The results showed that contamination was mostly on the surface of the bone confirming that it was related to the burial shroud covering the individuals.

2016

Evaluation of portable XRF instrumentation for assessing potential environmental exposure to toxic elements

Authors
McIntosh, KG; Guimarães, D; Cusack, MJ; Vershinin, A; Chen, ZW; Yang, K; Parsons, PJ;

Publication
International Journal of Environmental Analytical Chemistry

Abstract
Portable instruments based on X-Ray Fluorescence Spectrometry (XRF) have the potential to assist in field-based studies, provided that the data produced are reliable. In this study, we evaluate the performance of two different types of XRF instrument (XOS prototype and Thermo Niton XL3t). These two XRF analysers were evaluated in a laboratory setting, and data were reported for 17 elements (As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Se, Sn, Sr, Ti, V, and Zn). Samples analysed (n = 38) included ethnic herbal medicine products (HMPs), ethnic spices (ES), and cosmetic products (CPs). Comparison analyses were carried out using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). In general, results reported for Cd, Cu, and Pb by the XOS prototype analyser, using the non-metal mode, were negatively biased (5–95%) as compared to ICP-OES. In contrast, results reported for Pb, As, Cd, Cu and Zn by the Niton, using the soil mode, were positively biased, in some instances (Cd) by up to four orders of magnitude. While the sensitivity of both instruments was insufficient for reliably ‘quantifying’ toxic elements below 15 mg/kg, XRF was still capable of positively ‘detecting’ many elements at the low single-digit mg/kg levels. For semi-quantification estimates of contaminants at higher levels, and with limited sample preparation, both XRF instruments were deemed fit for the purpose. This study demonstrates that modern XRF instrumentation is valuable for characterising the elemental content of food, cosmetic, and medicinal products. The technology is particularly useful for rapidly screening large numbers of products (100’s per day) in the field, and quickly identifying those that may contain potentially hazardous levels of toxic elements. Toxic elements can be confirmed by examining the raw spectrum, and the limitations of factory-based calibration are generally manageable for field-based studies. © 2015 Wadsworth Center, New York State Department of Health.

2016

Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

Authors
Guimarães, D; Praamsma, ML; Parsons, PJ;

Publication
Spectrochimica Acta - Part B Atomic Spectroscopy

Abstract
X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the µg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD Mobile® XRF units were shown to be suitable for rapid screening of samples likely to be encountered in field based studies. © 2016 Elsevier B.V.

2016

Internal and External Temperature Monitoring of a Li-Ion Battery with Fiber Bragg Grating Sensors

Authors
Novais, S; Nascimento, M; Grande, L; Domingues, MF; Antunes, P; Alberto, N; Leitao, C; Oliveira, R; Koch, S; Kim, GT; Passerini, S; Pinto, J;

Publication
SENSORS

Abstract
The integration of fiber Bragg grating (FBG) sensors in lithium-ion cells for in-situ and in-operando temperature monitoring is presented herein. The measuring of internal and external temperature variations was performed through four FBG sensors during galvanostatic cycling at C-rates ranging from 1C to 8C. The FBG sensors were placed both outside and inside the cell, located in the center of the electrochemically active area and at the tab-electrode connection. The internal sensors recorded temperature variations of 4.0 +/- 0.1 degrees C at 5C and 4.7 +/- 0.1 degrees C at 8C at the center of the active area, and 3.9 +/- 0.1 degrees C at 5C and 4.0 +/- 0.1 degrees C at 8C at the tab-electrode connection, respectively. This study is intended to contribute to detection of a temperature gradient in real time inside a cell, which can determine possible damage in the battery performance when it operates under normal and abnormal operating conditions, as well as to demonstrate the technical feasibility of the integration of in-operando microsensors inside Li-ion cells.

2015

Ammonia Sensing System Based on Wavelength Modulation Spectroscopy

Authors
Viveiros, D; Ferreira, J; Silva, SO; Ribeiro, J; Flores, D; Santos, JL; Frazao, O; Baptista, JM;

Publication
PHOTONIC SENSORS

Abstract
A sensing system in the near infrared region has been developed for ammonia sensing based on the wavelength modulation spectroscopy (WMS) principle. The WMS is a rather sensitive technique for detecting atomic/molecular species, presenting the advantage that it can be used in the near-infrared region by using the optical telecommunications technology. In this technique, the laser wavelength and intensity were modulated by applying a sine wave signal through the injection current, which allowed the shift of the detection bandwidth to higher frequencies where laser intensity noise was typically lower. Two multi-pass cells based on free space light propagation with 160 cm and 16 cm of optical path length were used, allowing the redundancy operation and technology validation. This system used a diode laser with an emission wavelength at 1512.21 nm, where NH3 has a strong absorption line. The control of the NH3 gas sensing system, as well as acquisition, processing and data presentation was performed.

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