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1.
Environ Sci Process Impacts ; 24(2): 265-276, 2022 Feb 23.
Artigo em Inglês | MEDLINE | ID: mdl-35037685

RESUMO

Ecotoxicity caused by neonicotinoid pesticides is largely due to oxidative stress on non-target species. Due to the fact that reactive radical species reach the environment, materials intended for pesticide removal should be applicable for the simultaneous removal of reactive radicals, as well. This work uses the spectroscopic, adsorptive and antioxidant responses from MFI, FAU and BEA zeolites as descriptors of their potential environmental importance. Different network structures and Si/Al ratios were correlated with excellent zeolite adsorption properties, as over 200 mg g-1 of investigated neonicotinoids, acetamiprid and imidacloprid, was achieved in one cycle. Additionally, after two regeneration steps, over 450 mg g-1 adsorbed pesticides were retained, in three adsorption cycles. Overall the best results were detected for the FAU zeotype in both tested applications, insecticide adsorption and radical-scavenging performance, with and without insecticides present. The proposed mechanism for adsorption relies on kinetic investigation, isotherm modelling and spectroscopic post-adsorption analysis and targets zeolite hydroxyl/siloxane groups as active sites for insecticide adsorption via hydrogen bonding. Neat, well-defined zeolite structures enable their prospective application in ecotoxic species removal.


Assuntos
Praguicidas , Zeolitas , Adsorção , Cinética , Neonicotinoides , Zeolitas/química
2.
Spectrochim Acta A Mol Biomol Spectrosc ; 191: 469-477, 2018 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-29080501

RESUMO

The Church of the Holy Mother of God Hodegetria in Pec is decorated with wall paintings that date from the beginning of the 14th century. In terms of style they correspond to Byzantine wall paintings from the epoch of Paleologos. The painting technique and pigment pallete has been examined on micro fragments in thin cross-sections by means of optical microscopy (OM), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) and micro- Raman spectroscopy. Use of the fresco technique and two supporting plaster layers was noted on the majority of samples, while in large blue painted areas, a combination of fresco and secco techniques was used. The SEM-EDS results showed the presence of Ca as the main component of plaster besides the traces of Si and Mg. In some samples egg white as a binder was identified. The paint film is often multilayered. Twelve pigments were identified, mainly natural earth pigments such as red ochre, yellow ochre and green earth. A mixture of pigments was used for attaining desirable optical and aesthetical impressions. As decay product only weddelite was detected in many preparatory and painted samples.

3.
Artigo em Inglês | MEDLINE | ID: mdl-26301540

RESUMO

Micro Raman spectroscopy was applied to investigate the speciation of heteropoly and isopoly molybdates in 0.05 and 0.005 M aqueous solutions of 12-molybdophosphoric acid at pH values between 1 and 6. For comparative purposes, (31)P NMR spectroscopy was applied too. It is shown that stability of Keggin anion is influenced both by pH and concentration of solution. The Keggin structure is stable in acidic solutions (pH<1.6) while defective Keggin structures are formed with further alkalization (up to pH5.6). Monolacunary anion PMo11O(39)(7-) is the main component in the pH region from 1.6 to 3.4. Further removal of molybdenyl species causes the appearance of other vacant Keggin structures such as PMo9O31(OH)(3)(6-) and PMo6O(25)(9-) at about pH4. At pH5.0, anion PMo6O(25)(9-) is the main species. In solutions with pH greater than 5.0, heteropolymolybdates disappear completely and isopolymolybdates Mo7O(24)(6-) and MoO(4)(2-) are formed in higher amounts. In more diluted solution of 0.005 M, the decomposition scheme of 12-molybdophosphoric acid solution with increasing of pH takes place without observation of significant amounts of Mo7O(24)(6-) species. If alkalinization is performed with 0.5 M instead of 5 M NaOH, there are no significant changes in the Raman spectra of solutions. It is shown that the spectra of evaporated samples may be used for the identification of molecular species in corresponding concentrated solutions. However, Raman spectra of dry residues of more diluted solutions differ from spectra of corresponding solutions due to the reactions performed during the process of drying and cannot be used for unambiguous identification of species in solution. Acidification of 0.05 M solution of Na2MoO4 shows that at pH>5.6, molybdate anion MoO(4)(2-) dominates, while in the pH range between 5.6 and 1, heptamolybdate anion Mo7O(24)(6-) is preferentially formed.

4.
Artigo em Inglês | MEDLINE | ID: mdl-24608014

RESUMO

We report the low-temperature Raman scattering study of racemic ibuprofen. Detailed analysis of the racemic ibuprofen crystal symmetry, related to the vibrational properties of the system, has been presented. The first principle calculations of a single ibuprofen molecule dynamical properties are compered with experimental data. Nineteen, out of 26 modes expected for the spectral region below 200cm(-1), have been observed.


Assuntos
Analgésicos não Narcóticos/química , Ibuprofeno/química , Temperatura Baixa , Modelos Moleculares , Análise Espectral Raman/métodos
5.
Talanta ; 70(2): 301-6, 2006 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-18970767

RESUMO

In this study, we have developed a sensitive, rapid and simple procedure for the energy dispersive X-ray fluorescence (EDXRF) spectrometry measurement of tungsten in tobacco plant parts. Only 0.1g of dried plant material is needed instead of the usual 1g. EDXRF spectrometry is used for quantitative measurement, after the foliar application of solutions of tungstophosphoric acid (WPA), its magnesium salt and compounds with glycine (Gly) and alanine (Ala), in exact quantities. After that, the leaves, trunks and summits were collected and prepared separately. Tungsten is determined directly in raw dried material, and the overlap of the tungsten peak with zinc's that is present is avoided by the spectral deconvolution to obtain quantitative results. The prepared dry tablets weighed 100mg, and measurement time was 2000s. The radioisotope excitation source used was (109)Cd and tungsten was identified and quantified at the L(alpha1) and L(alpha2) lines at the energies of 8397.6eV and 8335.2eV, respectively. EDXRF spectrometry was applied in a wide range of concentrations (up to 2000mg/kg), with an estimated detection concentration limit of 15mg/kg, calculated on dried material. Quantitative analysis of different parts of the treated plant plus the washings gave 94.47% recovery of the applied tungsten in different compound forms. After the foliar application of investigated WPA compounds, there were noticed both vertical and horizontal distributions of tungsten through out the tobacco plants, according to the EDXRF spectrometry results. This conclusion is also in agreement with the positive effects of WPA on Tobacco mosaic tobamovirus (TMV) infection of Nicotiana tabacum (Solanaceae).

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