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Trace Detection and Photothermal Spectral Characterization by a Tuneable Thermal Lens Spectrometer with White-Light Excitation
Mladen Franko, Dorota Korte, Humberto Cabrera, 2018, original scientific article

Abstract: In the thermal lens experimental set-up we replaced the commonly employed pump laser by a halogen lamp, combined with an interference lter, providing a tuneable, nearly monochromatic pump source over the range of wavelengths 430–710 nm. Counter-propagating pump and probe beams are used and a 1 mm path-length sam- ple cell together with the interference lter makes an optical cavity, providing ampli cation of the thermal lens signal, which leads to enhancement of the measurement sensitivity, and enables detection of absorbances on the order of 5×10− 6. Ampli ed thermal lens signal allows us to replace the typical lock-in ampli er and digital os- cilloscope with a silicon photodetector, Arduino board, and a personal computer, offering the possibility for a compact, robust and portable device, useful for in- eld absorption measurements in low concentration or weakly absorbing species. The use of a white light source for optical pumping, an interference lter for wavelength selection and direct diagnostic of the thermal lens signal increase the versatility of the instrument and simpli- es substantially the experimental setup. Determination of Fe(II) concentrations at parts per billion levels was performed by the described white-light thermal lens spectrophotometer and the absorption spectrum for 50μg/ L Fe(II)-1,10-phenanthroline was well reproduced with an average measurement precision of 4%. The obtained limits of detection and quantitation of Fe(II) determination at 510nm are 3μgL− 1 and 11μgL− 1, respectively. The calibration curve was linear in the concentration range of LOQ-500μgL− 1 with reproducibility between 2% and 6%, con rming that this instrument provides good spectrometric capabilities such as high sensitivity, tune- ability and good reproducibility. In addition, the versatility of the instrument was demonstrated by recording the photothermal spectrum of gold nanostructured material and determination of excitation wavelength with most ef cient optical to thermal energy conversion, which differs considerably (cca 100 nm) from the absorption maximum of the investigated sample.
Found in: ključnih besedah
Summary of found: ...thermal lens spectrometry, Fe(II) determination, photothermal technique, multi-wavelength excitation...
Keywords: thermal lens spectrometry, Fe(II) determination, photothermal technique, multi-wavelength excitation
Published: 21.02.2018; Views: 1542; Downloads: 0
.pdf Fulltext (889,82 KB)

The detection and study of biologically active compounds in environmental processes and samples
Mojca Žorž Furlan, doctoral dissertation

Abstract: Environmental pollution in the 21th century still represents a global problem for human and animal health. Despite general awareness about released substances and their degradation products their fate and possibilities of removal are not well investigated. Even though the chemicals released are dispersed and diluted in water cycles, their poor biodegradability and/or strong accumulation can result in the intoxication of exposed organisms. Similarly, as a part of the environment, food can get contaminated by bioactive substances during different steps of preparation. Not only artificial compounds such as pesticides or pharmaceuticals, but also natural toxins enter the food chain and impact negatively on humans' and animals' health. In addition, the activity of some bacteria can influence the production of amines from amino acids after fermentation, to which the human body responds with several symptoms of intoxication. Several analytical methods for the determination of trace levels of broad range contaminants have been developed. Due to the largely robust, selective and sensitive features of the conventional (rearguard) techniques, they represent the first choice for analysing multiple organic compounds in frequently very complex matrices. However, screening (vanguard) methods are paving the way in the chemical analytics as a solution that provides simplicity and rapid analytical responses with binary (yes/no) answers. They require little or no sample treatment as well as more economically-efficient instrumentation. The combination of vanguard-rearguard analytical strategies hence offers a compromise between classical analytical figures of merit and productivity-related characteristics. In the first part of our research feasibility studies for the application of TLS and/or TLM in novel analytical methods for the determination of lipid-lowering drug atorvastatin and a mycotoxin ochratoxin A . The survey on atorvastatin performed spectrophotometrically has shown a decrease of ATV-sulpho-vanillin product at the wavelength of its maximum absorbance after dilution by organic solvent, which was investigated due to the possible increasing of the method sensitivity. As the predicted LODs that could be obtained by TLM (0.3 mg/L) could not reach the concentration of ATV usually present in the environment (ng/L-g/L) further experiments on this subject were therefore not justified. On the other hand, the ELISA assay for the determination of ochratoxin A was performed. In case of μFIA-TLM, the measurements were influenced by high background signal resulting in high LODs of TLM (470 pg/mL), which is known as a background limited technique. It was estimated that the LODs of standard ELISA assay could not be significantly improved, therefore no further research was conducted in this direction. In the second part of the dissertation, a sensitive rearguard system by coupling HPLC and TLS for the determination of biogenic amines in wine samples was developed. Putrescine, cadaverine, histamine and tyramine were separated and detected on a HPLC-TLS system after derivatization by dabsyl chloride. The method was optimized in terms of chromatographic conditions and in terms of TLS parameters. Also, the sensitivity of the newly developed method was evaluated by comparing the TLS detection with DAD detection in terms of LOD values, where TLS showed 3.6-fold improvement compared to DAD. Afterwards, the standard addition calibration was performed and evaluated for its recoveries (86−117%) in the determination of the four BAs. The applicability of the novel method was tested by the analysis of real white and red wine samples and by comparing the results to the standard HPLC-FL method and concentrations of BAs in wine samples were in good accordance. In addition, the dabsylated BAs showed better stability compared to the OPA derivatives as they have not lost the peak intensity after 17h of storage. In the third part, a vanguard system for detection of the overall biogenic amines concentration was developed by employing μFIA-TLM. Initially, NH4Cl standard solutions were applied in the indophenol reaction for batch mode, off-line μFIA-TLM and in an on-line indophenol formation for μFIA-TLM detection. By adding 50 % of EtOH to indophenol we obtained 9-fold improvement. In addition, indophenol showed good stability under TLM conditions. We optimized the microfluidic and TLM parameters in the off-line and on-line indophenol reaction. The addition of 5% ethanol to the reagent in the on-line reaction resulted in the 3-fold improvement of the signal-to-noise ratio. Further on, the overall reaction, including the enzymatic and the following indophenol reaction, was optimized by choosing the optimal buffer (pH=7, 0.5 M) and alkaline conditions (2M NaOH). The influence of interferences from amino compounds was also evaluated and discussed. The off-line and on-line μFIA-TLM were evaluated by their performance characteristics. The LOD for ammonia detection reached 2.3 μM and the applicability in ammonia detection in water samples was discussed. Similar LOD of 3.2 μM was obtained for the overall concentration of BAs and LOD of 3.8 μM for histamine, which is more than 4-folds lower value as the lowest suggested limits of intake for histamine in wine samples (2 mg/L; 18 μM). Finally, an immobilization procedure on magnetic nanoparticles was developed for the possible implementation of the selected enzyme in a miniaturized biosensor.
Found in: ključnih besedah
Summary of found: ...thermal lens spectrometry, thermal lens microscopy, high performance liquid chromatography,...
Keywords: thermal lens spectrometry, thermal lens microscopy, high performance liquid chromatography, microfluidics, biogenic amines, microbial transglutaminase, indophenol (Berthelot) reaction
Published: 04.06.2018; Views: 1724; Downloads: 152
.pdf Fulltext (2,90 MB)

Absorption Spectra of Ethanol and Water Using a Photothermal Lens Spectrophotometer
Humberto Cabrera, Jehan Akbar, Dorota Korte, Imrana Ashraf, Evelio E. Ramírez- Miquet, Ernesto Marin, Joseph Niemela, 2018, original scientific article

Found in: ključnih besedah
Summary of found: ...Thermal lens spectrometry, TLS, absorption of water, absorption of ethanol,...
Keywords: Thermal lens spectrometry, TLS, absorption of water, absorption of ethanol, vibration overtones
Published: 08.06.2018; Views: 1545; Downloads: 0
.pdf Fulltext (390,44 KB)

X-ray spectrometry in plant biology
Primož Pelicon, Peter Kump, Anja Kavčič, Alojz Kodre, Iztok Arčon, Katarina Vogel-Mikuš, 2018, published scientific conference contribution abstract (invited lecture)

Abstract: Trace elements are essential components of living systems, but at the same time they can be toxic at concentrations beyond those necessary for their biological functions. In addition, the toxicity can be extended to other non-essential elements of very similar atomic characteristics that can mimic the properties of a trace element. Trace element malnutrition affects more than half of the world’s population, while on the other hand industrialization, traffic and extensive use of fertilizers have resulted in exceedingly high concentrations of non-essential elements in food crops, posing risks to human health. In order to be able to develop and improve phyto-technologies that enable production of safe and quality food, knowledge on the basic mechanisms involved in trace and non-essential element uptake, transport, accumulation and ligand environment in plants is needed. Such studies are nowadays supported by highly sophisticated X-ray based techniques, such as synchrotron based X-ray fluorescence spectrometry, proton induced X-ray emission and X-ray absorption spectroscopy, enabling imaging of element distribution and determination of speciation and ligand environment of trace elements in biological tissues and cells with high spatial resolution and sensitivity. Selected case studies of metal distribution and speciation in selected model and crop plants, achieved by interdisciplinary work, will be presented.
Found in: ključnih besedah
Keywords: X-ray spectrometry, plants, XANES, EXAFS
Published: 12.09.2018; Views: 1086; Downloads: 0
.pdf Fulltext (62,44 KB)

Photocatalytic properties of metal modified TiO2 by photothermal techniques
Mladen Franko, Dorota Korte, Urška Lavrenčič Štangar, Olena Pliekhova, Humberto Cabrera, Zeinab Ebrahimpour, 2018, published scientific conference contribution abstract

Found in: ključnih besedah
Summary of found: ...Thermal lens spectrometry, Photothermal beam deflection spectroscopy, Dye remediation, Photothermal...
Keywords: Thermal lens spectrometry, Photothermal beam deflection spectroscopy, Dye remediation, Photothermal technique, Photocatalytic degradation, Reactive Blue 19, TiO2 modification
Published: 09.11.2018; Views: 1029; Downloads: 0
.pdf Fulltext (208,76 KB)

Determination of bioavailable Fe redox fractions of sediment pore waters by DGT passive sampling and BDS detection
Mladen Franko, Arne Bratkič, Dorota Korte, Hanna Budasheva, 2019, published scientific conference contribution abstract

Abstract: The bioavailability and toxicity of contaminants in sediments to benthic organisms depend on the speciation of the contaminant [1]. The level of iron supply to sediments creates contrasting chemical pathways, each producing distinctive mineral assemblag- es. Reliable measurement of Fe redox species (Fe2+ and Fe3+) in sediments is essential for studies of pollutants or trace-element cycling. This is, however, a difficult task, because the distribution of chemical species often changes during sampling and storage. In this work the Diffusive Gradients in Thin-films technique (DGT) is investigated as a passive sampling approach used in combination with photothermal beam deflection spectroscopy (BDS) as a detection method for determination of labile Fe-redox species in sediments and natural waters. DGT offers the advantage of pre-concentration of labile (i.e. bioavailable) Fe species from the total dissolved Fe pool in sediment pore waters [2]. The advantage of using BDS [3-4] is also in avoiding contamination by using additional steps as extraction or pre-concentration. Furthermore, combined DGT-BDS provides 2D information about distribution of Fe2+ and the total Fe content in the resin hydrogels [5]. The goal of this research is to show the repeatability of this technique for determining trace amounts of Fe redox species in environmental samples.
Found in: ključnih besedah
Summary of found: ...beam deflection spectrometry, diffusive gradients in thin-films, iron species...
Keywords: beam deflection spectrometry, diffusive gradients in thin-films, iron species
Published: 16.07.2019; Views: 781; Downloads: 0
.pdf Fulltext (29,60 MB)

Stable carbon isotope analysis of selected halocarbons at parts per trillion concentration in an urban location
M Iqbal Mead, M Anwar H Khan, Ian D Bull, Iain R White, Graham Nickless, Dudley E Shallcross, 2008, original scientific article

Abstract: ∂13C values of a suite of halocarbons have been determined in an urban background site in Bristol, UK. A novel mobile preconcentration system, based on the use of multi-adsorbent sample tubes, has been developed for trapping relatively large-volume air samples in potentially remote areas. An Adsorption Desorption System-Gas Chromatography-Electron Capture Detector was used to measure the mixing ratios of the selected halocarbon species, while a Gas ChromatographyCombustionIsotope Ratio Mass Spectrometer was used to determine ∂13C values. For the species with strong local sources, the variation of isotope ratios has been observed over the experimental period. Some of the results reported in the present study differ from previously reported values and reasons for this are discussed. The reporting of different ∂13C values for selected halocarbons from different areas in the present study suggests that ∂13C values may be used to determine the relative magnitudes of anthropogenic and biogenic sources.
Found in: ključnih besedah
Summary of found: ...(ECD), Gas Chromatography (GC), Isotope Ratio Mass Spectrometry (IRMS)...
Keywords: Adsorption Desorption System (ADS), Automated Thermal Desorber (ATD), Electron Capture Detector (ECD), Gas Chromatography (GC), Isotope Ratio Mass Spectrometry (IRMS)
Published: 18.07.2019; Views: 759; Downloads: 0
.pdf Fulltext (227,35 KB)

Increased sensitivity in proton transfer reaction mass spectrometry by incorporation of a radio frequency ion funnel
Andrew M Ellis, Stephen Mullock, Fraser Reich, Paul S Monks, Iain R White, Robert S Blake, Shane Barber, 2012, original scientific article

Abstract: A drift tube capable of simultaneously functioning as an ion funnel is demonstrated in proton transfer reaction mass spectrometry (PTR-MS) for the first time. The ion funnel enables a much higher proportion of ions to exit the drift tube and enter the mass spectrometer than would otherwise be the case. An increase in the detection sensitivity for volatile organic compounds of between 1 and 2 orders of magnitude is delivered, as demonstrated using several compounds. Other aspects of analytical performance explored in this study include the effective E/N (ratio of electric field to number density of the gas) and dynamic range over which the drift tube is operated. The dual-purpose drift tube/ion funnel can be coupled to various types of mass spectrometers to increase the detection sensitivity and may therefore offer considerable benefits in PTR-MS work.
Found in: ključnih besedah
Keywords: Analytical performance, Detection sensitivity, Drift tube, Dynamic range, Ion funnels, Proton-transfer reaction mass spectrometry, Volatile organic compounds
Published: 18.07.2019; Views: 699; Downloads: 0
.pdf Fulltext (799,47 KB)

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