Person:
Echeverría Morrás, Jesús

person.page.identifierURI

https://academica-e.unavarra.es/handle/2454/48930

Last Name

Echeverría Morrás

First Name

Jesús

person.page.departamento

Química Aplicada

ORCID

0000-0001-8126-1429

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110

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Now showing 1 - 10 of 13

Open Access
Strategies for fabrication of hydrogen peroxide sensors based on electrostatic self-assembly (ESA) method
(Elsevier, 2004) Del Villar, Ignacio; Matías Maestro, Ignacio; Arregui San Martín, Francisco Javier; Echeverría Morrás, Jesús; Claus, Richard O.; Ingeniería Eléctrica y Electrónica; Ingeniaritza Elektrikoa eta Elektronikoa; Gobierno de Navarra / Nafarroako Gobernua
An optical fiber sensor has been fabricated for detection of 5 M–0.1mM concentrations of hydrogen peroxide with a linear response. The deposition method used is electrostatic self-assembly (ESA) of polymer cationic and anionic layers. Prussian Blue (PB) has been included in the polycation layers. The optical fiber sensor is included in a reflection setup, where the measuring technique is based on the slope of the optical reflected power change caused by oxidation of Prussian White (PW) to Prussian Blue. The sensor recovers after immersion in a reductive agent and is immune against a variety of components. Measurement of hydrogen peroxide has been proved successfully in a wide range pHs between 3 and 9. Some techniques have been applied in order to avoid the lost of indicator.
Open Access
Phenyl siloxane hybrid xerogels: structure and porous texture
(Springer US, 2019) Moriones Jiménez, Paula; Echeverría Morrás, Jesús; Parra, Bernardo; Garrido Segovia, Julián José; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias; Gobierno de Navarra / Nafarroako Gobernua
The aim of this research is to investigate the effect of phenyltriethoxysilane (PhTEOS) and tetraethoxysilane (TEOS) molar ratios as silicon precursors on the structure and porous texture of xerogels. We have prepared phenyl-silane hybrid xerogels from mixtures of PhTEOS and TEOS at pH 10 and 333 K, using ethanol as a solvent. Characterization techniques include 29Si NMR, FTIR, XRD, FE-SEM, HRTEM, TGA-DSC, helium density, and gas adsorption (N2 at 77 K and CO2 at 273 K). In order to assess the contribution of the quadrupolar moment of N2 and CO2 in the adsorption we obtained the adsorption– desorption isotherm of Ar at 87.3 K for the xerogel synthesized from 50% PhTEOS. The morphology of xerogels changed from aggregates of spherical particles for 20% PhTEOS to lamellae for samples obtained with PhTEOS percentages equal or larger that 60%. The incorporation of phenyl groups into the xerogel matrix caused an increase in the spacing bond between silicon atoms and led to an intramolecular reaction and the formation of lamellar domains. Increasing the PhTEOS molar ratio in the mixture of silicon precursors produced hybrid xerogels with lower specific surface area, pore volume and characteristic energy. The similarity between the isotherms of N2 at 77 K and Ar at 87.3 K indicates that the main retention mechanism is physisorption and that the variation in the surface chemistry with the incorporation of phenyl groups doesn’t inhibit the retention of N2.
Open Access
Fiber optic sensors based on hybrid phenyl-silica xerogel films to detect n-hexane: determination of the isosteric enthalpy of adsorption
(Beilstein-Institut, 2017) Echeverría Morrás, Jesús; Calleja, Ignacio; Moriones Jiménez, Paula; Garrido Segovia, Julián José; Kimika Aplikatua; Institute for Advanced Materials and Mathematics - INAMAT2; Química Aplicada; Gobierno de Navarra / Nafarroako Gobernua, 269/01/08
We investigated the response of three fiber optic sensing elements prepared at pH 10 from phenyltriethoxysilane (PhTEOS) and tetraethylsilane (TEOS) mixtures with 30, 40, and 50% PhTEOS in the silicon precursor mixture. The sensing elements are referred to as Ph30, Ph40 and Ph50, respectively. The films were synthesized by the sol–gel method and affixed to the end of optical fibers by the dip-coating technique. Fourier transform infrared spectroscopy, N2 adsorption–desorption at 77 K and X-ray diffraction analysis were used to characterize the xerogels. At a given pressure of n-hexane, the response of each sensing element decreased with temperature, indicating an exothermic process that confirmed the role of adsorption in the overall performance of the sensing elements. The isosteric adsorption enthalpies were obtained from the calibration curves at different temperatures. The magnitude of the isosteric enthalpy of n-hexane increased with the relative response and reached a plateau that stabilized at approximately −31 kJ mol−1 for Ph40 and Ph50 and at approximately −37 kJ mol−1 for Ph30. This indicates that the adsorbate–adsorbent interaction was dominant at lower relative pressure and condensation of the adsorbate on the mesopores was dominant at higher relative pressure.
Open Access
Effect of Cu substitution on the magnetic and magnetic induction heating response of CdFe₂O₄ spinel ferrite
(Elsevier, 2020) Ghasemi, R.; Echeverría Morrás, Jesús; Pérez de Landazábal Berganzo, José Ignacio; Beato López, Juan Jesús; Naseri, M.; Gómez Polo, Cristina; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Ciencias
In this work, a comparative study of the effect of Cu on the structural, magnetic and magnetic induction heating response in CdFe2O4 spinel is presented. The ceramic nanoparticles (Cu1−xCdxFe2O4; 0 ≤ x ≤ 1) were synthesized by co-precipitation from Cu(II), Cd(II) and Fe(III) salts. The samples, characterized by X-ray diffractometry, display the characteristic spinel cubic structure (space group Fm3m) where CdO is detected as main secondary phase (≈ 16% weight for x = 1). A high degree of nanoparticle agglomeration is inferred from the Transmission Electron Microscopy (TEM) images, as a consequence of the employed synthesis procedure. Regarding the magnetic properties, superparamagnetic behavior at room temperature can be disregarded according to the low field magnetization response (ZFC-FC curves). For 0.4 ≤ x ≤ 0.8 ratios, the samples display maximum values in the magnetic moment that should be correlated to the cation distribution between the octahedral and tetrahedral sites. Maximum magnetization values lead to an enhancement in the magnetic induction heating response characterized by highest heating temperatures under the action of an ac magnetic field. In particular, maximum SAR values are estimated for x = 0.8 as a combined effect of high magnetic moment, low dc coercive field (high susceptibility). Although these Cu-Cd ferrite nanoparticles display moderate SAR values (around 0.7 W/g), the control of the maximum heating temperatures through the cation distribution (composition) provides promising properties to be used as nanosized heating elements (i.e. hyperthermia agents).
Open Access
Kinetics of the acid-catalyzed hydrolysis of tetraethoxysilane (TEOS) by 29Si NMR spectroscopy and mathematical modeling
(Springer, 2018) Echeverría Morrás, Jesús; Moriones Jiménez, Paula; Arzamendi Manterola, María Cruz; Garrido Segovia, Julián José; Gil Idoate, María José; Cornejo Ibergallartu, Alfonso; Martínez Merino, Víctor; Química Aplicada; Kimika Aplikatua; Institute for Advanced Materials and Mathematics - INAMAT2
Tetraethoxysilane (TEOS) is widely used to synthesize siliceous material by the sol–gel process. However, there is still some disagreement about the nature of the limiting step in the hydrolysis and condensation reactions. The goal of this research was to measure the variation in the concentration of intermediates formed in the acid-catalyzed hydrolysis by 29Si NMR spectroscopy, to model the reactions, and to obtain the rate constants and the activation energy for the hydrolysis and early condensation steps. We studied the kinetics of TEOS between pH 3.8 and 4.4, and four temperature values in the range of 277.2–313.2 K, with a TEOS:ethanol:water molar ratio of 1:30:20. Both hydrolysis and the condensation rate speeded up with the temperature and the concentration of oxonium ions. The kinetic constants for hydrolysis reactions increased in each step kh1 < kh2 < kh3 < kh4, but the condensation rate was lower for dimer formation than for the formation of the fully hydrolyzed Si(OH)4. The system was described according to 13 parameters: six of them for the kinetic constants estimated at 298.2 K, six to the activation energies, and one to the equilibrium constant for the fourth hydrolysis. The mathematical model shows a steady increase in the activation energy from 34.5 kJ mol−1 for the first hydrolysis to 39.2 kJ mol−1 in the last step. The activation energy for the condensation reaction from Si(OH)4 was ca. 10 kJ mol−1 higher than the largest activation energy in the hydrolytic reactions. The decrease in the net positive charge on the Si atom contributes to the protonation of the ethoxy group and makes it a better leaving group.
Open Access
Comprehensive kinetics of hydrolysis of organotriethoxysilanes by 29Si NMR
(American Chemical Society, 2019) Moriones Jiménez, Paula; Arzamendi Manterola, María Cruz; Cornejo Ibergallartu, Alfonso; Garrido Segovia, Julián José; Echeverría Morrás, Jesús; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2
The kinetics of several representative hybrid precursors were studied via 29Si NMR: three alkyl precursors, methyltriethoxysilane, ethyltriethoxysilane, and propyltriethoxysilane; as well as two unsaturated radicals, vinyltriethoxysilane and phenyltriethoxysilane. The reaction rate is related to the chemical shift of 29Si in the NMR spectra, which gives information about the electronic density of the Si atoms and the inductive effects of substituents. The concentration of the precursors decreased exponentially with time, and the intermediate products of hydrolysis and the beginning of the condensation reactions showed curves characteristic of sequential reactions, with a similar distribution of the species as a function of the fractional conversion. For all of the precursors, condensation started when the most hydrolyzed species reached a maximum concentration of 0.30 M, when the precursor had run out. A prediction following the developed mathematical model fits the experimental results in line with a common pathway described by eight parameters.
Open Access
Steering the synthesis of Fe3O4 nanoparticles under sonication by using a fractional factorial design
(Elsevier, 2021) Echeverría Morrás, Jesús; Moriones Jiménez, Paula; Garrido Segovia, Julián José; Ugarte Martínez, María Dolores; Cervera Gabalda, Laura María; Garayo Urabayen, Eneko; Gómez Polo, Cristina; Pérez de Landazábal Berganzo, José Ignacio; Ciencias; Zientziak; Estadística, Informática y Matemáticas; Estatistika, Informatika eta Matematika; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate Publikoa; Gobierno de Navarra / Nafarroako Gobernua
Superparamagnetic iron oxide nanoparticles (MNPs) have the potential to act as heat sources in magnetic hyperthermia. The key parameter for this application is the specific absorption rate (SAR), which must be as large as possible in order to optimize the hyperthermia treatment. We applied a Plackett-Burman fractional factorial design to investigate the effect of total iron concentration, ammonia concentration, reaction temperature, sonication time and percentage of ethanol in the aqueous media on the properties of iron oxide MNPs. Characterization techniques included total iron content, Fourier Transform Infrared Spectroscopy, X-Ray Diffraction, High Resolution Transmission Electron Microscopy, and Dynamic Magnetization. The reaction pathway in the coprecipitation reaction depended on the initial Fe concentration. Samples synthesized from 0.220 mol L−1 Fe yielded magnetite and metastable precipitates of iron oxyhydroxides. An initial solution made up of 0.110 mol L−1 total Fe and either 0.90 or 1.20 mol L−1 NH3(aq) led to the formation of magnetite nanoparticles. Sonication of the reaction media promoted a phase transformation of metastable oxyhydroxides to crystalline magnetite, the development of crystallinity, and the increase of specific absorption rate under dynamic magnetization.
Open Access
Mid-infrared spectroscopy (MIR) for simultaneous determination of fat and protein content in meat of several animal species
(Springer, 2017) Lozano Saiz, María; Rodríguez Ulibarri, Pablo; Echeverría Morrás, Jesús; Beruete Díaz, Miguel; Sorolla Ayza, Mario; Beriain Apesteguía, María José; Institute of Smart Cities - ISC; Institute on Innovation and Sustainable Development in Food Chain - ISFOOD; Institute for Advanced Materials and Mathematics - INAMAT2
The aim of this research was to study the application of MIR spectroscopy as an alternative to conventional methods to determine fat and protein content. Samples of the main species used to produce meat products were analyzed, showing all of them absorption bands at similar wavenumbers though with different intensity. Correlation analysis of absorption intensities showed that bands around 2925, 2854, and 1746 cm−1 are associated with fat content, whereas bands around 3288, 1657, and 1542 cm−1 are associated with proteins. During the validation process, prediction models of fat and protein content were successfully obtained withR2 0.9173 and 0.7534, respectively. Finally, a good result (R2 =0.8829) was obtained on the estimation of the lipid content when the information at only one wavenumber was used.
Open Access
Tenderness of PGI "Ternera de Navarra" beef samples determined by FTIR-MIR spectroscopy
(MDPI, 2022) Beriain Apesteguía, María José; Lozano Saiz, María; Echeverría Morrás, Jesús; Murillo Arbizu, María Teresa; Insausti Barrenetxea, Kizkitza; Beruete Díaz, Miguel; Institute on Innovation and Sustainable Development in Food Chain - ISFOOD; Institute for Advanced Materials and Mathematics - INAMAT2; Ingeniería Eléctrica, Electrónica y de Comunicación; Ingeniaritza Elektrikoa, Elektronikoaren eta Telekomunikazio Ingeniaritzaren
Understanding meat quality attribute changes during ageing by using non-destructive techniques is an emergent pursuit in the agroindustry research field. Using beef certified samples from the protected geographical indication (PGI) “Ternera de Navarra”, the primary goal of this study was to use Fourier transform infrared spectroscopy on the middle infrared region (FTIR-MIR) as a tool for the examination of meat tenderness evolution throughout ageing. Samples of the longissimus dorsi muscle of twenty young bulls were aged for 4, 6, 11, or 18 days at 4 °C. Animal carcass classification and sample proximate analysis were performed to check sample homogeneity. Raw aged steaks were analyzed by FTIR-MIR spectroscopy (4000–400 cm−1) to record the vibrational spectrum. Texture profile analysis was performed using a multiple compression test (compression rates of 20%, 80%, and 100%). Compression values were found to decrease notably between the fourth and sixth day of ageing for the three compression rates studied. This tendency continued until the 18th day for C20. For C80 and C100, there was not a clear change in the 11th and 18th days of the study. Regarding FTIR-MIR as a prediction method, it achieved an R2 lower than 40%. Using principal component analysis (PCA) of the results, the whole spectrum fingerprint was used in the discrimination of the starting and final ageing days with correct maturing time classifications. Combining the PCA treatment together with the discriminant analysis of spectral data allowed us to differentiate the samples between the initial and the final ageing points, but it did not single out the intermediate points.
Open Access
Bioavailability of heavy metals in soils amended with sewage sludge
(Agricultural Institute of Canada, 2002) Morera Luzán, María Teresa; Echeverría Morrás, Jesús; Garrido Segovia, Julián José; Química Aplicada; Kimika Aplikatua
The recycling of sewage sludge to agricultural land results in the slow accumulation of potentially toxic heavy metals in soils. A greenhouse experiment was conducted to determine the bioavailability of Cu, Ni, Pb and Zn applied to soils in urban anaerobically stabilized sewage sludge. The soils were Lithic Haplumbrept (Lh), Calcixerollic Xerochrept (Cx1 and Cx2) and Paralithic Xerorthent (Px). Sunflower plants (Helianthus annuus L) were grown in. the soils following amendment with the sludge. The addition of sewage sludge markedly increased the average dry weight of the plants in the soils that had lower yields without sludge addition (Lh, Cx2, and Px). The acid pH of the Lh soil favoured the bioavailability of Zn from sewage sludge. The bioavailability of Cu was greater in the alkaline soils than in the acidic soil (Lh), which can be attributed to the high organic matter content of the Lh soil which complexes Cu and impairs its uptake by the plants. The concentration of metals in the plants increased with the sewage sludge dose. The effect of the soil type on the metal concentration in plants was greater that the effect of the dose.