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A low-cost signal processing circuit developed to measure and drive a heat dissipation soil matric potential sensor based on a single thermosensitive resistor is demonstrated. The SnSe2 has a high thermal coefficient, from -2.4Ω/°C in the 20 to 25 °C to -1.07Ω/°C in the 20 to 25 °C. The SnSe2 thermosensitive resistor is encapsulated with a porous gypsum block and is used as both the heating and temperature sensing element. To control the power dissipated on the thermosensitive resistor and keep it constant during the heat pulse, a mixed analogue/digital circuit is used. The developed control circuit is able to maintain the dissipated power at 327.98±0.3% mW when the resistor changes from 94.96Ω to 86.23Ω. When the gravimetric water content of the porous block changes from dry to saturated (θw=36.7%), we measured a variation of 4.77Ω in the thermosensitive resistor, which results in an end-point sensitivity of 130 mΩ/%. The developed system can easily meet the standard requirement of measuring the gravimetric soil water content with a resolution of approximately Δθw=1%, since the resistance is measured with a resolution of approximately µ31µΩ, three orders of magnitude smaller than the sensitivity.
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In this work, we investigated the role of solid-state dealumination by (NH4)2SiF6 (25% Al removal and 13% Si insertion), the impregnation of niobium (10, 18, and 25 wt. %) on dealuminated *BEA (DB) zeolite and their catalytic properties in ethanol and xylose transformations. Among all the studied catalysts, 18%Nb-DB showed increased mesoporosity and external areas. A leveling effect in the number and strength of the proposed two sites (Brønsted and Lewis) present in the catalyst (n1 = 0.24 mmol g-1, -ΔH1 = 49 kJ mol-1, and n2 = 0.20 mmol g-1, -ΔH2 = 42 kJ mol-1) in the catalyst 18%Nb-DB, might be responsible for its good activity. This catalyst presented the highest selectivity for diethyl ether, DEE (97%) with 61% conversion after 50 ethanol pulses at 230 °C (turnover number, TON DEE = 1.15). These features allowed catalytically fruitful bonding of the ethanol molecules to the neighboring sites on the channels, facilitating bimolecular ether formation through a possible SN2 mechanism. The same catalyst was active and selective for transformation of xylose at 180 °C, showing 64% conversion and 51% selectivity for furfural (TON Furfural = 24.7) using water as a green solvent.
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Poly(lactic acid) (PLA) is a significant polymer that is based on renewable biomass resources. The production of PLA by polycondensation using heterogeneous catalysis is a focus for sustainable and economical processes. A series of samples comprising 12-tungstophosphoric acid (H3PW) supported on activated carbon, silica, and alumina induced the catalytic polymerization of D,L-lactic acid to form blends of PLA. The catalysts were characterized by multiple techniques to confirm the integrity of the Keggin anion as well as the acidity, which is the key property for relating structure to activity. The best reaction conditions were established for H3PW/C and tested for the other supported catalysts. The obtained polymer was a blend that was characterized as an enantiomeric excess (ee) of as much as 95% L-PLA (PLLA) with a mass average molar mass (M w ) of approximately 14,900 daltons. The role of H3PW in these polymerizations was demonstrated, i.e., without the Keggin acid, only oligomeric units (M w < 10,000 daltons) could be obtained. Additionally, inverse relationships between the M w of PLA and the enthalpy (-ΔH) of the strongest sites of the catalysts were distinguished, i.e., PLAMw-H3PW/C > PLAMw-H3PW/Al2O3 > PLAMw-H3PW/SiO2, whereas the acidity (-ΔH) order was as follows: H3PW/SiO2 > H3PW/Al2O3 > H3PW/C. These findings could be attributed to the correct tuning of strength and the accessibility of the sites to produce longer polymeric chains.
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Herein, a combination of heteropolyacids and ionic liquids as a catalytic system was studied for the Biginelli multicomponent reaction; the positive ionic liquid effect associated with the acidic strength of zeolite-supported heteropolyacids made this combination an efficient catalytic system for the multicomponent synthesis of 3,4-dihydropyrimidin-2(1H)-one/thione derivatives. The acidic strength effect was evaluated, and a range was determined in which the reaction provided better results. The mechanism of the reaction was also investigated in the presence and absence of ionic liquids, and two features of paramount importance were revealed: the mechanism could be tuned to proceed through only one reaction path among three possibilities and the kinetics of the reaction was significantly faster in the presence of an ionic liquid.
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[This corrects the article DOI: 10.1016/j.heliyon.2019.e01810.].
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The interaction of hydrophobic chitin and chitosan with sodium dodecyl sulfate (SDS) has been studied by titration calorimetry at 298.15K. The nature of interaction of the surfactant and biopolymers was followed by enthalpy interaction profiles. The mixing enthalpy curves were determined by mixing SDS solutions above their critical micelle concentration with chitin and chitosan suspensions in different concentrations. The Gibbs free energy of aggregation values were -23.21, -22.71 and -21.53 kJ mol(-1) for chitin in 0.02, 0.05 and 0.1% concentration, respectively, and 28.30, 24.38 and 24.20 kJ mol(-1) for chitosan in 0.02, 0.05 and 0.1% concentration, respectively. The critical aggregation concentration (cac) obtained by calorimetric data gave 6.32, 7.07 and 9.14 mmol kg(-1) in 0.02, 0.05 and 0.1% concentration, respectively, for chitin and 2.09, 4.91 and 5.11 mmol kg(-1) for chitosan in 0.02, 0.05 and 0.1% concentration, respectively.
Assuntos
Quitina/química , Quitosana/química , Dodecilsulfato de Sódio/química , Calorimetria/métodos , Sequência de Carboidratos , Dados de Sequência Molecular , TermodinâmicaRESUMO
The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 µL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated.