Effect of nano-metakaolin addition on the hydration characteristics of fly ash blended cement mortar

The effect of nano-metakaolin (NMK) addition on hydration characteristics of fly ash (FA) blended cement mortar was experimentally investigated. The amorphous or glassy silica, which is the major component of a pozzolan, reacts with the calcium hydroxide liberated during calcium silicate hydration. It is believable to add FA and NMK particles in order to make high performance concrete. The physico-mechanical properties of FA blended cement mortars made with different percentages of NMK were investigated. The experimental results showed that the compressive and flexural strengths of mortars containing NMK are higher than those of FA blended cement mortar at 60 days of hydration age. It is demonstrated that the nanoparticles enhances strength than FA. In addition, the hydration process was monitored using scanning electron microscopy and thermal gravimetric analysis (TG). The results of these examinations indicate that NMK behaves not only as a filler to improve microstructure, but also as an activator to promote the pozzolanic reaction.     

Influence of Submicron Fibrillated Cellulose Fibers from Cotton on Hydration and Microstructure of Portland Cement Paste

This paper reports the influence of submicron hydrophilic fibers on the hydration and microstructure of Portland cement paste. Submicron fibrillated cellulose (SMC) fibers was prepared by the acid hydrolysis of cotton fibers in H₂SO₄ solution (55% v/v) for 1.5 h at a temperature of 50 °C. The SMC fibers were added into cement with a dosage of 0.03 wt.%, and the effect of SMC on the hydration and microstructure of cement paste was investigated by calorimeter analysis, XRD, FT-IR, DSC-TG, and SEM. Microcrystalline cellulose (MCC) fibers were used as the contrast admixture with the same dosage in this study. The results show that the addition of SMC fibers can accelerate the cement hydration rate during the first 20 h of the hydration process and improve the hydration process of cement paste in later stages. These results are because the scale of SMC fibers more closely matches the size of the C-S-H gel compared to MCC fibers, given that the primary role of the SMC is to provide potential heterogeneous nucleation sites for the hydration products, which is conducive to an accelerated and continuous hydration reaction. Furthermore, the induction and bridging effects of the SMC fibers make the cement paste microstructure more homogeneous and compact.     

Physicochemical Properties and Antioxidant Activity of Spray-Dry Broccoli (Brassica oleracea var Italica) Stalk and Floret Juice Powders

This research presents the microencapsulation and conservation of antioxidants of broccoli juice processed by spray drying, and proposes the use of a by-product as a technological application. Broccoli juice (BJ) extracted from two sources, stalks and florets, was spray-dried employing maltodextrin (MX) as a carrier agent at concentrations of 5, 7.5, and 10%, and inlet temperatures of 150 and 220 °C. The total phenolic content (TPC), and antioxidant activity (AA) of the BJ-MX powders were determined together with the physicochemical characteristics, including particle morphology, microstructure, and thermal properties. Based on the TPC and AA, the optimal processing conditions found were 5% of MX and a drying temperature of 220 °C. However, the florets showed higher TPC, while stalks presented higher AA under those processing conditions. The particles exhibited micrometric sizes and a mixture of spherical-shape particles and pseudo-spherical particles. The diffractograms indicated an amorphous microstructure in all samples. The glass transition temperature (Tg) was determined in the range of 50 °C for the samples dried at 150 °C and 55 °C for those dried at 220 °C. This suggested that powders might be stored at temperatures below the Tg without presenting any loss of antioxidants.     

The Influence of Nd and Sm on the Structure and Properties of Sol-Gel-Derived TiO2 Powders

TiO₂ nanopowders modified by Nd and Sm were prepared using the sol-gel technique. It was found by XRD analysis that the samples containing Sm are amorphous up to 300 °C, while those with Nd preserve a mixed organic-inorganic amorphous structure at higher temperatures (400 °C). The TiO₂ (rutile) was not detected up to 700 °C in the presence of both modified oxides. TiO₂ (anatase) crystals found at about 400 °C in the Sm-modified sample exhibited an average crystallite size of about 25–30 nm, while doping with Nd resulted in particles of a lower size—5–10 nm. It was established by DTA that organic decomposition is accompanied by significant weight loss occurring in the temperature range 240–350 °C. Photocatalytic tests showed that the samples heated at 500 °C possess photocatalytic activity under UV irradiation toward Malachite green organic dye. Selected compositions exhibited good antimicrobial activity against E. coli K12 and B. subtilis.     

The Quenching and Sonication Effect on the Mechanical Strength of Silver Nanowires Synthesized Using the Polyol Method

This study aims to determine the effect of fast cooling (quenching) on thermal properties, mechanical strength, morphology and size of the AgNWs. The synthesis of AgNWs was carried out at three different quenching-medium temperatures as follows: at 27 °C (ambient temperature), 0 °C (on ice), and −80 °C (in dry ice) using the polyol method at 130 °C. Furthermore, the AgNWs were sonified for 45 min to determine their mechanical strength. Scanning electron microscopy analysis showed that the quenched AgNWs had decreased significantly; at 27 °C, the AgNWs experienced a change in length from (40 ± 10) to (21 ± 6) µm, at 0 °C from (37 ± 8) to (24 ± 8) µm, and at −80 °C from (34 ± 9) to (29 ± 1) µm. The opposite occurred for their diameter with an increased quenching temperature: at 27 °C from (200 ± 10) to (210 ± 10) nm, at 0 °C from (224 ± 4) to (239 ± 8) nm, and at −80 °C from (253 ± 6) to (270 ± 10) nm. The lower the temperature of the quenching medium, the shorter the length and the higher the mechanical strength of AgNWs. The UV-Vis spectra of the AgNWs showed peak absorbances at 350 and 411 to 425 nm. Thermogravimetric analysis showed that AgNWs quenched at −80 °C have better thermal stability as their mass loss was only 2.88%, while at the quenching temperatures of 27 °C and 0 °C the mass loss was of 8.73% and 4.17%, respectively. The resulting AgNWs will then be applied to manufacture transparent conductive electrodes (TCEs) for optoelectronic applications.     

Effect of Heat Exposure on Activity Degradation of Enzymes in Mango Varieties Sindri,SB Chaunsa,and Tommy Atkins during Drying

Mango has been described as a valuable source of nutrients and enzymes that are beneficial to human health. Drying at different temperatures not only affects the nutritional properties but can also contribute to the degradation of valuable enzymes in dried fruit. The novelty of this paper is to investigate the quality of hot air dried mango in terms of activity retention of the heat-sensitive enzymes (HSE). For this, HSE was first screened in fresh mango flesh of the variety Samar Bahisht (SB) Chaunsa. Later, the combined effect of different drying temperatures (40 °C, 50 °C, 60 °C, 70 °C, and 80 °C) and air velocities (1.0 ms⁻¹ and 1.4 ms⁻¹) on the activity retention of HSE in dried mango slices of the varieties Sindri, SB Chaunsa, and Tommy Atkins were investigated. The results showed that the drying temperature had a significant impact on the degradation of HSE, while at the same time some influence of the air velocity was also observed. Drying at 40 °C and an air velocity of 1.4 ms⁻¹ retained more HSE compared to those samples dried at higher temperatures. The least retention of HSE was found in samples dried at 80 °C.     

The Effects of Prolonged Storage on ARPE-19 Cells Stored at Three Different Storage Temperatures

This study aimed to investigate how prolonged storage of adult retinal pigment epithelial (ARPE-19) cell sheets affects cell metabolism, morphology, viability, and phenotype. ARPE-19 cell sheets were stored at three temperatures (4 °C, 16 °C, and 37 °C) for three weeks. Metabolic status and morphology of the cells were monitored by sampling medium and examining cells by phase-contrast microscopy, respectively, throughout the storage period. Cell viability was analyzed by flow cytometry, and phenotype was determined by epifluorescence microscopy after the storage. Lactate production and glucose consumption increased heavily, while pH dropped considerably, through storage at 37 °C compared to 4 °C and 16 °C. During storage, morphology started to deteriorate first at 4 °C, then at 37 °C, and was maintained the longest at 16 °C. Viability of the cells after three weeks of storage was best preserved at 16 °C, while cells stored at 4 °C and 37 °C had reduced viability. Dedifferentiation indicated by reduced expression of retinal pigment epithelium-specific protein 65 (RPE65), zonula occludens protein 1 (ZO-1), and occludin after three weeks of storage was noticed in all experimental groups compared to control. We conclude that storage temperature affects the metabolic status of ARPE-19 cells and that 16 °C reduces metabolic activity while protecting viability and morphology.     

Improvement of Naturally Derived Food Colorant Performance with Efficient Pyranoanthocyanin Formation from Sambucus nigra Anthocyanins Using Caffeic Acid and Heat

Consumers and regulations encourage the use of naturally derived food colorants. Anthocyanins (ACN), plant pigments, are unstable in foods. In aged red wines, ACN with a free hydroxyl group at C-5 condenses to form pyranoanthocyanins (PACN), which are more stable but form inefficiently. This study attempted to produce PACN efficiently using high cofactor concentration and heat. Elderberry anthocyanins were semi-purified and caffeic acid (CA) was dissolved in 15% ethanol and diluted with a buffer to achieve ACN:CA molar ratios of 1:50, 1:100, 1:150, and 1:200, then incubated at 65 °C for 5 days. The effect of temperature was tested using ACN samples incubated with or without CA at 25 °C, 50 °C, and 75 °C for 7 days. Compositional changes were monitored using uHPLC-PDA-MS/MS. Higher CA levels seemed to protect pigment integrity, with ACN:CA 1:150 ratio showing the highest tinctorial strength after 48 h. PACN content growth was fastest between 24 and 48 h for all ACN:CA ratios and after 120 h, all ACN had degraded or converted to PACN. PACN formed faster at higher temperatures, reaching ~90% PACN in 24 h and ~100% PACN in 48 h at 75 °C. These results suggest that PACN can form efficiently from elderberry ACN and CA if heated to produce more stable pigments.     

Migration Testing of GPPS and HIPS Polymers: Swelling Effect Caused by Food Simulants Compared to Real Foods

Migration kinetic data from general purpose polystyrene (GPPS) and high impact polystyrene (HIPS) were generated for a set of model substances as well as styrene monomer and oligomers at different temperatures (20 °C, 40 °C, 60 °C) using food simulants stipulated in the European Regulation (EU) 10/2011 and real foods like milk, cream and olive oil (20 °C, 40 °C). The extent of polymer swelling was characterized gravimetrically and visual changes of the test specimens after migration contact were recorded. Isooctane and 95% ethanol caused strong swelling and visual changes of HIPS, overestimating real migration into foods especially at high temperatures; GPPS was affected by isooctane only at 60 °C. With 50% ethanol, after 10 days contact at 60 °C or 40 °C both polymers were slightly swollen. Contrary, most of the real foods analyzed caused no detectable swelling or visual changes of the investigated polymers. This study demonstrates that the recommendations provided by EU regulations are not always in agreement with the physicochemical properties of styrenic polymers. The critical point remains the selection of adequate food simulants/testing conditions, since the high overestimation of aggressive media can lead to non-compliance of polystyrene materials even if the migration into real food would be of no concern.     

The effect of H2O on the sulfation of Havelock limestone under oxy-fuel conditions in a thermogravimetric analyser

A gas mixture representing oxy-fuel combustion conditions was employed in a thermogravimetric analyser to determine the effect of water vapor and SO₂ concentration on limestone sulfation kinetics over the temperature range of 800 to 920 °C. Here, experiments used small samples of particles (4 mg), with small particle sizes (d_p < 38 µm) and large gas flow rates (120 mL/min@NTP) in order to minimize mass transfer interferences. The gas mixture contained 5000 ppm_v SO₂, 2% O₂, and the H₂O content was changed from 0% to 25% with the balance CO₂. When water vapor was added to the gas mixture at lower temperatures (800–870 °C), the limestone SO₂ capture efficiency increased. However, as the temperature became higher, the enhancement in total conversion values decreased. As expected, Havelock limestone at higher temperatures (890 °C, 920 °C, and 950 °C) experienced indirect sulfation and reacted at a faster rate than for lower temperatures (800–870 °C) for direct sulfation over the first five minutes of reaction time. However, the total conversion of Havelock limestone for direct sulfation was generally greater than for indirect sulfation.     

Preparation of High-Performance Activated Carbon from Coffee Grounds after Extraction of Bio-Oil

In this study, a new method for economical utilization of coffee grounds was developed and tested. The resulting materials were characterized by proximate and elemental analyses, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and N₂ adsorption–desorption at 77 K. The experimental data show bio-oil yields reaching 42.3%. The optimal activated carbon was obtained under vacuum pyrolysis self-activation at an operating temperature of 450 °C, an activation temperature of 600 °C, an activation time of 30 min, and an impregnation ratio with phosphoric acid of 150 wt.%. Under these conditions, the yield of activated carbon reached 27.4% with a BET surface area of 1420 m²·g⁻¹, an average pore size of 2.1 nm, a total pore volume of 0.747 cm³·g⁻¹, and a t-Plot micropore volume of 0.428 cm³·g⁻¹. In addition, the surface of activated carbon looked relatively rough, containing mesopores and micropores with large amounts of corrosion pits.     

The Effect of the Modification of Carbon Spheres with ZnCl2 on the Adsorption Properties towards CO2

Zinc chloride and potassium oxalate are often applied as activating agents for carbon materials. In this work, we present the preparation of ZnO/carbon spheres composites using resorcinol-formaldehyde resin as a carbon source in a solvothermal reactor heated with microwaves. Zinc chloride as a zinc oxide source and potassium oxalate as an activating agent were applied. The effect of their addition and preparation conditions on the adsorption properties towards carbon dioxide at 0 °C and 25 °C were investigated. Additionally, for all tested sorbents, the CO₂ sorption tests at 40 °C, carried out utilizing a thermobalance, confirmed the trend of sorption capacity measured at 0 and 25 °C. Furthermore, the sample activated using potassium oxalate and modified using zinc chloride (a carbon-to-zinc ratio equal to 10:1) displayed not only a high CO₂ adsorption capacity (2.69 mmol CO₂/g at 40 °C) but also exhibited a stable performance during the consecutive multicycle adsorption–desorption process.     

Microstructural Evolution and High-Performance Giant Dielectric Properties of Lu3+/Nb5+ Co-Doped TiO2 Ceramics

Giant dielectric (GD) oxides exhibiting extremely large dielectric permittivities (ε’ > 10⁴) have been extensively studied because of their potential for use in passive electronic devices. However, the unacceptable loss tangents (tanδ) and temperature instability with respect to ε’ continue to be a significant hindrance to their development. In this study, a novel GD oxide, exhibiting an extremely large ε’ value of approximately 7.55 × 10⁴ and an extremely low tanδ value of approximately 0.007 at 10³ Hz, has been reported. These remarkable properties were attributed to the synthesis of a Lu³⁺/Nb⁵⁺ co-doped TiO₂ (LuNTO) ceramic containing an appropriate co-dopant concentration. Furthermore, the variation in the ε’ values between the temperatures of −60 °C and 210 °C did not exceed ±15% of the reference value obtained at 25 °C. The effects of the grains, grain boundaries, and second phase particles on the dielectric properties were evaluated to determine the dielectric properties exhibited by LuNTO ceramics. A highly dense microstructure was obtained in the as-sintered ceramics. The existence of a LuNbTiO₆ microwave-dielectric phase was confirmed when the co-dopant concentration was increased to 1%, thereby affecting the dielectric behavior of the LuNTO ceramics. The excellent dielectric properties exhibited by the LuNTO ceramics were attributed to their inhomogeneous microstructure. The microstructure was composed of semiconducting grains, consisting of Ti³⁺ ions formed by Nb⁵⁺ dopant ions, alongside ultra-high-resistance grain boundaries. The effects of the semiconducting grains, insulating grain boundaries (GBs), and secondary microwave phase particles on the dielectric relaxations are explained based on their interfacial polarizations. The results suggest that a significant enhancement of the GB properties is the key toward improvement of the GD properties, while the presence of second phase particles may not always be effective.     

Psychrotolerant Mesorhizobium sp. Isolated from Temperate and Cold Desert Regions Solubilizes Potassium and Produces Multiple Plant Growth Promoting Metabolites

Soil potassium (K) supplement depends intensively on the application of chemical fertilizers, which have substantial harmful environmental effects. However, some bacteria can act as inoculants by converting unavailable and insoluble K forms into plant-accessible forms. Such bacteria are an eco-friendly approach for enhancing plant K absorption and consequently reducing utilization of chemical fertilization. Therefore, the present research was undertaken to isolate, screen, and characterize the K solubilizing bacteria (KSB) from the rhizosphere soils of northern India. Overall, 110 strains were isolated, but only 13 isolates showed significant K solubilizing ability by forming a halo zone on solid media. They were further screened for K solubilizing activity at 0 °C, 1 °C, 3 °C, 5 °C, 7 °C, 15 °C, and 20 °C for 5, 10, and 20 days. All the bacterial isolates showed mineral K solubilization activity at these different temperatures. However, the content of K solubilization increased with the upsurge in temperature and period of incubation. The isolate KSB (Grz) showed the highest K solubilization index of 462.28% after 48 h of incubation at 20 °C. The maximum of 23.38 µg K/mL broth was solubilized by the isolate KSB (Grz) at 20 °C after 20 days of incubation. Based on morphological, biochemical, and molecular characterization (through the 16S rDNA approach), the isolate KSB (Grz) was identified as Mesorhizobium sp. The majority of the strains produced HCN and ammonia. The maximum indole acetic acid (IAA) (31.54 µM/mL) and cellulase (390 µM/mL) were produced by the isolate KSB (Grz). In contrast, the highest protease (525.12 µM/mL) and chitinase (5.20 µM/mL) activities were shown by standard strain Bacillus mucilaginosus and KSB (Gmr) isolate, respectively.     

Spectrophotometric analysis of stability of gold nanoparticles during catalytic reduction of 4-nitrophenol

Spectrophotometric monitoring of 4-nitrophenol (4-NP) reduction by sodium borohydride (NaBH₄) using gold nanoparticles (GNPs) as a catalyst has been extensively studied, but the stability of GNPs in terms of change in the surface plasmon resonance (SPR) at different temperatures has not been explored. In the present investigation, our aim was to evaluate the SPR stability of GNPs as a catalyst during the reduction of 4-NP at different elevated temperatures (i.e. 30–60 °C) and sodium borohydride concentrations. Sensitivity of this degradation process toward concentration of GNPs at a range of temperatures is also evaluated. The spectrophotometric results reveal that up to 45 °C, 12 ± 1.5 nm catalyst has a consistent optical density (OD) during the entire 4-NP reduction process, which is related to the surface integrity of catalyst atoms. As the temperature approached 50 °C, the OD gradually decreased and showed a blue shift as the reaction proceeded, which could be related to a decrease in particle size or surface dissolution of gold atoms. The present study may find application in the design of catalysts for the reduction of organic pollutants in industrial wastewater at a range of temperatures.     

Changes in Particle Size,Sedimentation, and Protein Microstructure of Ultra-High-Temperature Skim Milk Considering Plasmin Concentration and Storage Temperature

Age gelation is a major quality defect in ultra-high-temperature (UHT) pasteurized milk during extended storage. Changes in plasmin (PL)-induced sedimentation were investigated during storage (23 °C and 37 °C, four weeks) of UHT skim milk treated with PL (2.5, 10, and 15 U/L). The increase in particle size and broadening of the particle size distribution of samples during storage were dependent on the PL concentration, storage period, and storage temperature. Sediment analysis indicated that elevated storage temperature accelerated protein sedimentation. The initial PL concentration was positively correlated with the amount of protein sediment in samples stored at 23 °C for four weeks (r = 0.615; p < 0.01), whereas this correlation was negative in samples stored at 37 °C for the same time (r = −0.358; p < 0.01) due to extensive proteolysis. SDS-PAGE revealed that whey proteins remained soluble over storage at 23 °C for four weeks, but they mostly disappeared from the soluble phase of PL-added samples after two weeks’ storage at 37 °C. Transmission electron micrographs of PL-containing UHT skim milk during storage at different temperatures supported the trend of sediment analysis well. Based on the Fourier transform infrared spectra of UHT skim milk stored at 23 °C for three weeks, PL-induced particle size enlargement was due to protein aggregation and the formation of intermolecular β-sheet structures, which contributed to casein destabilization, leading to sediment formation.     

Temperature and Inoculum Origin Influence the Performance of Ex-Situ Biological Hydrogen Methanation

The conversion of H₂ into methane can be carried out by microorganisms in a process so-called biomethanation. In ex-situ biomethanation H₂ and CO₂ gas are exogenous to the system. One of the main limitations of the biomethanation process is the low gas-liquid transfer rate and solubility of H₂ which are strongly influenced by the temperature. Hydrogenotrophic methanogens that are responsible for the biomethanation reaction are also very sensitive to temperature variations. The aim of this work was to evaluate the impact of temperature on batch biomethanation process in mixed culture. The performances of mesophilic and thermophilic inocula were assessed at 4 temperatures (24, 35, 55 and 65 °C). A negative impact of the low temperature (24 °C) was observed on microbial kinetics. Although methane production rate was higher at 55 and 65 °C (respectively 290 ± 55 and 309 ± 109 mL CH₄/L.day for the mesophilic inoculum) than at 24 and 35 °C (respectively 156 ± 41 and 253 ± 51 mL CH₄/L.day), the instability of the system substantially increased, likely because of a strong dominance of only Methanothermobacter species. Considering the maximal methane production rates and their stability all along the experiments, an optimal temperature range of 35 °C or 55 °C is recommended to operate ex-situ biomethanation process.     

Comprehensive Thermal Characteristics of Different Cultivars of Flaxseed Oil (Linum usittatissimum L.)

The aim of this study was to describe the thermal properties of selected cultivars of flaxseed oil by the use of the differential scanning calorimetry (DSC) technique. The crystallization and melting profiles were analyzed depending on different scanning rates (1, 2, 5 °C/min) as well as oxidative induction time (OIT) isothermally at 120 °C and 140 °C, and oxidation onset temperatures (Ton) at 2 and 5 °C/min were measured. The crystallization was manifested as a single peak, differing for a cooling rate of 1 and 2 °C/min. The melting curves were more complex with differences among the cultivars for a heating rate of 1 and 2 °C/min, while for 5 °C/min, the profiles did not differ, which could be utilized in analytics for profiling in order to assess the authenticity of the flaxseed oil. Moreover, it was observed that flaxseed oil was highly susceptible to thermal oxidation, and its stability decreased with increasing temperature and decreasing heating rate. Significant negative linear correlations were found between unsaturated fatty acid content (C18:2, C18:3 n-3) and DSC parameters (OIT, Ton). Principal component analysis (PCA) also established a strong correlation between total oxidation value (TOTOX), peroxide value (PV) and all DSC parameters of thermo-oxidative stability.     

Investigation of early hydration of high aluminate cement-based binder at different ambient temperatures

The effect of spent FCC catalyst on early hydration (up to 48?h) of high aluminate cement (Al₂O₃ >70%) at different ambient temperatures (10, 20, and 30?°C) was investigated. Cement pastes with constant ratio of water/binder?=?0.35 (binder?=?cement?+?addition) and containing 0, 5, 10, and 15% mass of addition as replacement of cement were studied. The hydration kinetics was determined by calorimetric measurements and the structure of hardened binders after 2?days of curing at an appropriate temperature was also investigated using X-ray, SEM, and thermal analysis methods. Due to the fact that hydration of aluminate cements is highly sensitive to temperature conditions as well as certain changes of temperature are inevitable in practice, the evaluation of the impact of the waste catalyst addition in such conditions is justified. On the basis of obtained results, it was stated that the temperature determines the early hydration of high aluminate cement and decides about the influence of waste aluminosilicate. The introduction of the discussed addition has a big impact on the kinetics of cement hydration closely related to the curing temperature. The presence of spent catalyst accelerates the hydration at the temperatures of 20 and 30?°C, but at the temperature of 10?°C this waste aluminosilicate acts as a retarding agent. The effect of the addition on the microstructure of hardened binders after 48?h of hydration is rather insignificant, especially at 20?°C, compared to the influence of the temperature on hydration. At the temperature of 10?°C, a formation of low amount of C₂AH₈ can be observed because of the presence of spent catalyst, while at the temperature of 30?°C the introduction of the mineral addition prevents the hydrogarnet formation.     

Pressurized Solvent Extraction of Paulownia Bark Phenolics

Paulownia bark is mostly utilized jointly with wood, but the possibility of a separate valorization through the pressurized extraction of bark bioactives has been assessed. Subcritical water extraction and supercritical CO₂ extraction are green technologies allowing shorter times than conventional solvent extraction under atmospheric shaken conditions. Subcritical water extraction was carried out at temperatures ranging from 140 to 240 °C and supercritical CO₂ extraction was performed at different pressures (10, 20 and 30 MPa), temperatures (35, 45 and 55 °C) and ethanol concentrations (0, 10 and 15% (w/w)). Subcritical water extraction under a non-isothermal operation during heating up to 160 °C (19 min) provided extraction yields up to 30%, and the extracts contained up to 7% total phenolics with an ABTS (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)) radical scavenging capacity equivalent to 35% the activity of Trolox, whereas at 240 °C, the yield decreased to 20%, but the phenolic content reached 21%, and the antiradical activity was equivalent to 85% of Trolox. Supercritical CO₂ extraction at 30 MPa, 45 °C and 30 min reached a global yield of 2% after 180 min of extraction, but the product showed very low antiradical capacity. Gallic acid, vanillic acid, vanillin and apigenin were the major phenolic compounds found in the extracts.