RESUMEN
In this initial study, the impact of thermosonication as an alternative to the traditional fusion in Brazilian cheese spread (Requeijão Cremoso) manufacture was investigated. The effect of ultrasound (US) power was evaluated considering various aspects such as gross composition, microstructure, texture, rheology, color, fatty acid composition, and volatile compounds. A 13 mm US probe operating at 20 kHz was used. The experiment involved different US power levels (200, 400, and 600 W) at 85 °C for 1 min, and results were compared to the conventional process in the same conditions (85 °C for 1 min, control treatment). The texture became softer as ultrasound power increased from 200 to 600 W, which was attributed to structural changes within the protein and lipid matrix. The color of the cheese spread also underwent noticeable changes for all US treatments, and treatment at 600 W resulted in increased lightness but reduced color intensity. Moreover, the fatty acid composition of the cheese spread showed variations with different US power, with samples treated at 600 W showing lower concentrations of saturated and unsaturated fatty acids, as well as lower atherogenicity and thrombogenicity indexes, indicating a potentially healthier product. Volatile compounds were also influenced by US, with less compounds being identified at higher powers, especially at 600 W. This could indicate possible degradation, which should be evaluated in further studies regarding US treatment effects on consumer perception. Hence, this initial work demonstrated that thermosonication might be interesting in the manufacture of Brazilian cheese spread, since it can be used to manipulate the texture, color and aroma of the product in order to improve its quality parameters.
Asunto(s)
Queso , Queso/análisis , Sonicación/métodos , Brasil , Manipulación de Alimentos/métodos , Compuestos Orgánicos Volátiles/química , Compuestos Orgánicos Volátiles/análisis , Ácidos Grasos/química , Color , TemperaturaRESUMEN
Microwave-induced combustion (MIC) was proposed in this study for honey decomposition aiming for As, Cd, Hg, and Pb determination by inductively coupled plasma mass spectrometry (ICP-MS). Sample mass (up to 1.0 g), absorbing solution (0.5 to 14.4 mol L-1 HNO3, and H2O), heating program, and combustion aids were evaluated. The Eurachem guidelines were used for method validation. The proposed method enabled combustion of a high sample mass (0.8 g of honey, with 0.4 g of microcrystalline cellulose and 100 µL of 6 mol L-1 NH4NO3) using 6 mL of an absorbing solution consisting of 1 mol L-1 HNO3, which resulted in low residual carbon in solution (< 25 mg L-1). Honey samples from different geographical origins were analyzed. Results showed no significant difference in comparison to other two microwave decomposition methods, based on microwave-assisted wet digestion with single reaction chamber (MAWD-SRC) and microwave-assisted wet digestion (MAWD). Standard addition experiments resulted in recoveries higher than 98%. The limits of detection ranged from 1.10 (As) to 4.60 ng g-1 (Pb). In addition to using only diluted reagents and resulting in digests virtually free of interferences, the proposed method was faster (< 30 min) than most of those presented in the literature.
Asunto(s)
Miel , Microondas , Espectrometría de Masas/métodos , Plomo , Análisis EspectralRESUMEN
Honey is a food product consumed all over the world. Besides its nutritional properties, honey presents antibacterial, antioxidant, and wound-healing properties. To ensure that the final product meets qualitative and microbiological standards, honey treatment is of great importance. Conventional honey treatment is based on the heating of honey samples for decrystallization and bacteria and yeast inactivation. However, conventional heating can cause negative effects on honey quality, such as the formation of toxic compounds, reduction of enzyme activity, and loss of antioxidant and antimicrobial properties. The application of ultrasonic waves has demonstrated interesting effects on honey processing. Ultrasound (US) treatment can lead to the fragmentation of glucose crystals in crystalized honey and has little effect on its properties. In addition to inactivating microorganisms, US-assisted honey processing also preserves phenolic compounds content and antimicrobial properties. However, there is still limited information about honey sonication. The aim of the present review is to comprehensively show the possibilities of US application in honey processing and its effects on honey properties.
Asunto(s)
Miel , Miel/análisis , Antioxidantes , Fenoles/análisis , Antibacterianos/farmacologíaRESUMEN
Ultrasonic waves can induce physical and chemical changes in liquid media via acoustic cavitation. Various applications have benefitted from utilizing these effects, including but not limited to the synthesis of functional materials, emulsification, cleaning, and processing. Several books and review articles in the public domain cover both fundamental and applied aspects of ultrasonics and sonochemistry. The Editors of the Ultrasonics Sonochemistry journal possess diverse expertise in this field, from theoretical and experimental aspects of acoustic cavitation to materials synthesis, environmental remediation, and sonoprocessing. This article provides Editors' perspectives on various aspects of ultrasonics and sonochemistry that may benefit students and early career researchers.
RESUMEN
A simple, fast and promising sample preparation method based on microwave-induced combustion in disposable vessels (MIC-DV) was developed for Cl and S determination in crude oil by inductively coupled plasma optical emission spectrometry (ICP-OES). The MIC-DV consists of a new approach of conventional microwave-induced combustion (MIC). For the combustion, crude oil was pipetted on a disk of filter paper and placed on a quartz holder, followed by the addition of igniter solution (40 µL of 10 mol L-1 NH4NO3). The quartz holder was inserted into a commercial 50 mL disposable polypropylene vessel containing the absorbing solution, which was then inserted in an aluminium rotor. The combustion occurs under atmospheric pressure in a domestic microwave oven not compromising the operator's safety. The following parameters of combustion were evaluated: type, concentration and volume of absorbing solution, sample mass and the possibility of performing consecutive combustion cycles. Using MIC-DV, up to 10 mg of crude oil were efficiently digested, using 2.5 mL of ultrapure H2O as absorbing solution. Moreover, up to 5 consecutive combustion cycles were possible without analyte losses, reaching a total sample mass of 50 mg. The MIC-DV method was validated according to Eurachem Guide recommendations. Results obtained for Cl and S by MIC-DV were in agreement with those obtained using conventional MIC, as well as those obtained for S in a certified reference material of crude oil (NIST 2721). Analyte spike recovery experiments were performed and recoveries at three concentration levels ranged from 99 to 101% for Cl and from 95 to 97% for S, indicating a good accuracy. The limit of quantification achieved by ICP-OES after MIC-DV were 73 and 50 µg g-1 for Cl and S respectively, applying 5 consecutive combustion cycles.
RESUMEN
This work presents the first report of the application of microwave-induced combustion in disposable vessels (MIC-DV) as a simple and fast sample preparation step for fluoride determination by ion-selective electrode (ISE) in leguminous seeds and oilseeds samples. Several experimental conditions of MIC-DV were evaluated, such as sample mass, absorbing solution, volume of combustion igniter, purging time with oxygen, and the use of successive combustion cycles. The accuracy of MIC-DV/ISE method was evaluated by comparing the results obtained by microwave-induced combustion and determination by ion chromatography, with agreements ranged from 94 to 106%. The method allowed to achieve relatively low limits of quantification (8.3 to 16 µg g-1) comparing to AOAC method (40 µg g-1), besides the use of small amounts of reagents, less handling of digests, making the method greener and with portable features comparing to other methods.
Asunto(s)
Fabaceae , Flúor , Electrodos de Iones Selectos , Semillas , MicroondasRESUMEN
In this study, a miniaturized liquid-liquid extraction (LLE) method for pre-concentration of Na, K, Ca, and Mg in crude oil was proposed. Analytes in crude oil were quantitatively extracted to the aqueous phase, followed by flame atomic absorption spectrometry (FAAS) determination. The following parameters were evaluated: type of extraction solution, sample mass, heating temperature and time, stirring time, centrifugation time, and the use of toluene and chemical demulsifier. Accuracy was evaluated by comparing the results obtained by the proposed method (LLE-FAAS) with those obtained after high-pressure microwave-assisted wet digestion and FAAS determination (reference values). No statistical difference was observed between the reference values and those using the optimized conditions for LLE-FAAS: 2.5 g of sample; 1000 µL of 2 mol L-1 HNO3, 50 mg L-1 of chemical demulsifier in 500 µL of toluene, 10 min of heating at 80 °C, 60 s of stirring, and 10 min of centrifugation. Relative standard deviations were lower than 6%. The limits of quantification (LOQ) were 1.2, 1.5, 5.0, and 0.50 µg g-1 for Na, K, Ca, and Mg, respectively. The proposed miniaturized LLE method presents several advantages, such as ease-of-use, high throughput (up 10 samples can be processed per 1 h), uses a high sample mass reaching low LOQs. In addition, the use of a diluted solution for extraction reduces the amount of reagents (around 40 times) and consequently laboratory residue generation, becoming an environmental friendly method. Suitable LOQs were achieved for analyte determination at low concentration even using a simple and low-cost sample preparation system (miniaturized LLE method) and a relatively low-cost determination technique (FAAS), avoiding the use of microwave ovens and more sensitivity techniques, which are required for routine analyses.
RESUMEN
In this work, a continuous flow extraction system assisted by ultrasound (US) was developed for the extraction of Cr(III) from residual tanned leather shavings. US energy was delivered into the system by a tubular applicator (clamp-on tube US applicator). The effect of the US energy was investigated at 20 kHz of frequency and electrical input power of 75, 150, 300 and 600 W. Residence time and temperature profile were also evaluated. It was observed that the internal temperature profile was affected by the presence of US and inverted in comparison with the conditions without US. In this way, the temperature profile generated by the US was reproduced by using electrical resistances in order to compare the obtained results. The US intensity was measured using a hydrophone connected to a sound pressure meter. The use of the US did not alter the dynamic behavior of the system but increased the extraction efficiency when compared to the silent condition. US power above 75 W did not lead to increased extraction efficiency, when the residence time was 30 min. However, when 60 min of residence time were employed, the optimized US power was 150 W, resulting in an extraction efficiency of 71.7 ± 0.7 %, about 28 % higher when compared to the silent condition in the same temperature and other conditions. The US energy allowed a reduction in processing time and operational temperature when compared to the silent condition with the same temperature profile. The overall energy consumption with US was similar or lower than that observed without US, showing the feasibility of the proposed extraction system.
Asunto(s)
Cromo , Residuos Sólidos , Residuos Sólidos/análisis , Tecnología , TemperaturaRESUMEN
Background: Previous studies have suggested that guarana (Paullinia cupana) and açai (Euterpe oleracea) have antioxidant, anti-inflammatory, and proliferative properties, indicating their potential therapeutic action in wound healing. We produced a conjugated guarana-açai (GA) extract and tested its healing action on earthworms (Eisenia fetida) subjected to tail amputation by surgical incision. Methods: Extract from roasted guarana seeds and fresh açai seed berries was produced. The antioxidant and genoprotective capacity of GA extract was tested. The concentration with the most remarkable healing potential was used in subsequent tests. The last three posterior segments of the clitellate earthworm tail reared under standardized conditions were surgically amputated. Next, topical PBS or GA extract was applied to the surgical wound. The rate of cell migration and tissue regeneration at the local wound site was histologically evaluated after the procedure. Expression of the SOX4 gene that acts in epithelial-to-mesenchymal transition was determined by RT-qPCR. Results: Sixteen bioactive molecules, including some previously described substances, were identified. All tested concentrations exhibited antioxidant and genoprotective effects. The GA extract accelerated the healing processes as observed through macroscopic and histological analyses and increased expression of SOX4. Conclusion: The GA extract has a potential role in the healing of surgically induced wounds.
Asunto(s)
Oligoquetos , Paullinia , Amputación Quirúrgica , Animales , Antioxidantes/farmacología , Fibroblastos , Estrés Oxidativo , Extractos Vegetales/farmacología , Extractos Vegetales/uso terapéutico , Cicatrización de HeridasRESUMEN
The effects of thermosonication processing (TS, 90 °C, ultrasound powers of 200, 400, and 600 W) on the quality parameters of Jamun fruit dairy dessert compared to conventional heating processing (high-temperature short time, (HTST), 90 °C/20 s) were evaluated. Microbiological inactivation and stability, rheological parameters, physical properties, volatile and fatty acid profiles, and bioactive compounds were assessed. TS provided more significant microbial inactivation (1 log CFU mL-1) and higher microbial stability during storage (21 days) than HTST, with 3, 2, and 2.8 log CFU mL-1 lower counts for yeasts and molds, aerobic mesophilic bacteria, and lactic acid bacteria, respectively. In addition, TS-treated samples showed higher anti-hypertensive (>39%), antioxidant (>33%), and anti-diabetic (>27%) activities, a higher concentration of phenolic compounds (>22%), preservation of anthocyanins, and better digestibility due to the smaller fat droplet size (observed by confocal laser scanning microscopy). Furthermore, lower TS powers (200 W) improved the fatty acid (higher monounsaturated and polyunsaturated fatty acid contents, 52.78 and 132.24%) and volatile (higher number of terpenes, n = 5) profiles and decreased the atherogenic index. On the other hand, higher TS powers (600 W) maintained the rheological parameters of the control product and contributed more significantly to the functional properties of the products (antioxidant, anti-hypertensive, and anti-diabetic). In conclusion, TS proved to be efficient in treating Jamun fruit dairy dessert, opening space for new studies to define process parameters and expand TS application in other food matrices.
Asunto(s)
Antocianinas , Antioxidantes , Antihipertensivos , Antioxidantes/farmacología , Ácidos Grasos , Frutas , SonicaciónRESUMEN
Ultrasound induced cavitation (acoustic cavitation) process is found useful in various applications. Scientists from various disciplines have been exploring the fundamental aspects of acoustic cavitation processes over several decades. It is well documented that extreme localised temperature and pressure conditions are generated when a cavitation bubble collapses. Several experimental techniques have also been developed to estimate cavitation bubble temperatures. Depending upon specific experimental conditions, light emission from cavitation bubbles is observed, referred to as sonoluminescence. Sonoluminescence studies have been used to develop a fundamental understanding of cavitation processes in single and multibubble systems. This minireview aims to provide some highlights on the development of basic understandings of acoustic cavitation processes using cavitation bubble temperature, sonoluminescence and interfacial chemistry over the past 2-3 decades.
Asunto(s)
Acústica , TemperaturaRESUMEN
In this work, high purity graphite, a high chemically stable material, was effectively digested using a single method allowing compatible solutions for the further multitechnique determination of halogens by: ion chromatography (F and Cl), inductively coupled plasma mass spectrometry (Cl, Br and I) and by ion selective electrode (only for F). The recent system using microwave-induced self-ignition (MISI) is based on the strong interaction between microwave radiation and graphite in a closed system pressurized with oxygen (Maxwell-Wagner effect). Carbon-based materials present intense and specific interfacial polarization when exposed to microwave electromagnetic field resulting in a fast heating rate. This effect associated to a pressurized oxygen system, provides a quick self-ignition of carbon-based materials and consequent combustion/digestion of organic matrices. Under optimized conditions, sample masses up to 600 mg were fully digested in a quartz vessel under 20 bar of oxygen pressure and using just a diluted solution (100 mmol L-1 NH4OH) for the quantitative absorption of all the analytes. MISI method was validated, and the accuracy (better than 94%) was evaluated by comparison of results obtained by pyrohydrolysis for two coal certified reference materials as well as with subsequent analytes determination by the three techniques: IC, ICP-MS and ISE. It is important to point out that no filter paper disks, electrical connections or other ignition aids are required as in the case of previous or classical combustion methods. Moreover, just a diluted absorbing solution was used resulting in negligible blanks and relatively low limits of detection. The digestion efficiency was higher than 99%, making the proposed method a suitable and powerful alternative for the quasi complete digestion of graphite and determination of halogens virtually free of interferences.
Asunto(s)
Grafito , Halógenos , Digestión , Halógenos/análisis , Espectrometría de Masas/métodos , MicroondasRESUMEN
This study proposes the use of an ultrasound-assisted adsorption system coupled to porous ceramic fragments to improve the removal of iron from FeSO4 aqueous solution. Ultrasound was applied using an ultrasound bath at a low frequency (37 kHz, 330 W). The optimized conditions for Fe removal were achieved by 7â g of adsorbent, 40â min of sonication, 20â mg L-1 of initial Fe concentration, and 30 °C of reaction temperature. After optimizing the conditions, the method was applied for the removal of iron in groundwater. A central composite design and response surface methodology were used to evaluate the degree to which different variables had a significant effect on iron removal. The efficiency of iron removal using the selected conditions for FeSO4 solution was near to 100%. However, for groundwater samples, the maximum iron removal efficiencies of the system with and without ultrasound were 80.7% and 51.1%, respectively, indicating that the adsorption with ultrasound was significantly higher than that without ultrasound. It was shown that the proposed ultrasound-assisted adsorption system can be used to enhance the removal of inorganic iron from groundwater.
Asunto(s)
Contaminantes Químicos del Agua , Purificación del Agua , Adsorción , Cerámica , Concentración de Iones de Hidrógeno , Hierro , Cinética , Porosidad , Agua , Contaminantes Químicos del Agua/análisis , Purificación del Agua/métodosRESUMEN
Many efforts have been recently made to improve the digestion efficiency by using powerful equipment or by using an auxiliary reagent. In this work, an alternative method is reported, which explores a digestion system based on a single reaction chamber (SRC) technology pressurized with O2 for reducing the amount of acid, without impairing the digestion efficiency. Before digestion, the system was pressurized with compressed air (20 bar, 20% O2) while the temperature was evaluated from 180 up to 270 °C. The procedure was also carried out under O2 pressure (20 bar). For each temperature several acid concentrations were evaluated (0.1 to 3 mol L-1 HNO3), being possible to correlate the effectiveness of each acid concentration with temperature. The proposed method was applied to the simultaneous digestion of several organic matrices with variable content of fat, protein, and carbohydrate (whole milk powder, bovine liver, parsley, and linseed). The residual carbon content was lower than 4% (C lower than 200 mg L-1 in digests), showing the high digestion efficiency of the proposed approach. Up to 250 mg of all food matrices were digested using a sub-stoichiometric amount of HNO3 (1 mol L-1 solution), which was only achieved due to the use of O2 as an auxiliary reagent. Barium, Ca, Cu, Fe, K, Mg, Mn, Na, Sr, and Zn were determined by ICP-OES, and the accuracy was better than 95% for standard reference materials of corn bran, whole milk powder, and bovine liver. It is an important feature, being in agreement with green chemistry recommendations because very low amounts of reagents are required for sample digestion, as well as low amounts of residues are generated.
Asunto(s)
Ácido Nítrico , Oxígeno , Animales , Bovinos , Metales , Microondas , Leche/química , Ácido Nítrico/análisis , Ácido Nítrico/química , Oxígeno/análisis , Oxígeno/químicaRESUMEN
This paper proposes a greener approach to the intensification of base oil recovery for truck engines (32,500 km of use) using ethanol, propan-2-ol, 2-methylpropan-1-ol, and butan-1-ol as solvents for the extraction of base oil, combining mechanical stirring (220 rpm) and ultrasound (25 °C, 24 kHz, and 400 W). The results indicated that the recovery yields of the base oil, using the mechanical stirring and ultrasound (MS-US) system, for ethanol, propan-2-ol, 2-methylpropan-1-ol, and butan-1-ol were approximately 3.1, 25.6, 71.6, and 85.5%, respectively. By contrast, the recovery yields using only mechanical stirring were 8.8, 28.9, 58.9, and 76.1%, respectively. The system with pre-extraction could effectively remove Ca (85.3-93.0%), Mg (67.2-82.9%), Na (31.7-62.5%), and Zn (0.0-71.7%). Finally, the results showed a reduction of almost 100% for the concentrations of Al, Cr, Fe, and Mo in the pre-extraction system. The mechanical stirring (5 min) and ultrasound (5 min) system were able to intensify the extraction process using environmentally friendly solvents.
Asunto(s)
Etanol , Lubricantes , SolventesRESUMEN
In this work, two microwave-assisted sample preparation methods based on combustion and ultraviolet digestion for futher determination of Br, Cl, and I in blood by inductively coupled plasma mass spectrometry were proposed. For microwave-induced combustion (MIC), blood was spotted on square pieces of Munktell TFN paper, and water and diluted NH4OH were evaluated as absorbing solutions. The stability of the analytes in the spotted blood was also evaluated. During 90 days, no changes of halogen content were observed for samples (with and without anticoagulant) on paper stored in a desiccator at 20 ± 5 °C. Whole blood was also digested by microwave-assisted ultraviolet digestion (MAD-UV). Some parameters as the volume of HNO3 solution, the influence of H2O2, and the effect of UV radiation were investigated. The interferences caused by C and K on halogen determination were carefully investigated. The results for MIC and MAD-UV and Br, Cl and I determination by ICP-MS presented no difference. The accuracy of MIC and MAD-UV was also evaluated by analyte spike with reference solutions of Br, Cl and I using inorganic species and also organic I standard (T4-levothyroxine). For both methods, recoveries were 94 and 108% for Br, 96 and 103% for Cl, and 104 and 97% for I. In case of organic I, recoveries were 99 and 111% for MIC and MAD-UV, respectively. The limits of quantification for MIC and MAD-UV after ICP-MS determination were 0.06 and 0.04 µg g-1 for Br, 14 and 30 µg g-1 for Cl and 12 and 8 ng g-1 for I, respectively. The proposed methods provide a suitable digestion approach, assuring safety and high digestion efficiency for further halogen determination in blood, with the possibility to use in clinical analysis.
Asunto(s)
Halógenos , Microondas , Peróxido de Hidrógeno , Espectrometría de Masas , Análisis EspectralRESUMEN
Nowadays, the application of ultrasound (US) energy for assisting the lignocellulosic biomass and waste materials conversion into value-added products has dramatically increased. In this sense, this review covers theoretical aspects, promising applications, challenges and perspectives about US and its use for biomass treatment. The combination of US energy with a suitable reaction time, temperature and solvent contributes to the destruction of recalcitrant lignin structure, allowing the products to be used in thermochemical and biological process. The main mechanisms related to US propagation and impact on the fragmentation of lignocellulosic materials, selectivity, and yield of conversion treatments are discussed. Moreover, the synergistic effects between US and alternative green solvents with the perspective of industrial applications are investigated. The present survey analysed the last ten years of literature, studying challenges and perspectives of US application in biorefinery. We were aiming to highlight value-added products and some new areas of research.
Asunto(s)
Biomasa , Biotecnología/métodos , Industrias , Ondas UltrasónicasRESUMEN
Urban dust is a mixture of deposited particles from different sources usually linked to potentially toxic elements (PTEs). Despite the industrialization of many South American countries, little is known about the impact of particulate matter in large cities; these data are necessary to promote environmental policies aiming to protect human health. The main objective of this work was to evaluate the particle size distribution, composition, and environmental and human health risks of settled dust particles from Barranquilla, a Colombian Caribbean industrialized area. Trace elements were analyzed by inductively coupled plasma-mass spectrometry from 35 different sites, covering all city areas. Dust was mostly composed of 10-to-70-µm particles. The average concentrations of V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Mo, Ag, Cd, Sn, Sb, Pb, and Bi were above background. High spatial heterogeneity was observed for Cu, Zn, As, Se, Mo, Ag, Sn, Sb, and Bi. Concentration factors suggest that urban dusts are extremely contaminated by Zn and Cu. The ecological risk associated with specific elements decreased in the order Cd > Cu > As > Hg > Pb > Ni > Co ≈ Zn ≈ Cr, and the contamination load index showed that 91% of the samples are polluted by PTEs. Although the carcinogenic risks of Cr, Ni, As, Co, and Cd were low, chronic exposure to several PTEs may affect quality of life. Educational programs, as well as monitoring and greater control on traffic, industry, and construction activities are needed to protect environmental and human health.
Asunto(s)
Polvo , Metales Pesados , Región del Caribe , China , Ciudades , Colombia , Polvo/análisis , Exposición a Riesgos Ambientales/análisis , Monitoreo del Ambiente , Humanos , Metales Pesados/análisis , Calidad de Vida , Medición de RiesgoRESUMEN
Nitrocellulose is a nitrated cellulose polymer with a broad application in industry. Depending on the nitrogen content, this polymer can be used for manufacturing explosives, varnishes, clothes, and films, being considered a product of high value-added. In this work, the use of ultrasound was investigated for the intensification of nitrocellulose synthesis from microcrystalline cellulose. The ultrasound-assisted nitrocellulose synthesis (UANS) was carried out using several ultrasound systems, such as baths and cup horns, allowing the evaluation of the frequency (from 20 to 130 kHz) and delivered power (from 23 to 134 W dm-3) to the reaction medium. The following parameters were evaluated: acid mixture (H2SO4, H3PO4, CH2O2 or CH3COOH with HNO3, 2 to 14.4 mol L-1), ultrasound amplitude (10 to 70%) and reaction time (5 to 50 min). Better nitrocellulose yield (nitrogen content of 12.5% was obtained from 1 g of microcrystalline cellulose employing a cup horn system operating at 20 kHz, 750 W of nominal power with 60% of amplitude, 25 mL of acid solution (13.6 mL of 18.4 mol L-1 H2SO4 + 9.2 mL of 14.4 mol L-1 HNO3 + 2.2 mL H2O), at 30 °C for 30 min. At silent conditions (mechanical stirring ranging from 100 to 500 rpm), the nitrogen content was lower than 11.8% which demonstrate the ultrasound effects for nitrocellulose synthesis.
RESUMEN
In this work, ultrasound was applied for the conversion of tannic acid into gallic acid using only diluted H2O2 as reagent. Experiments were carried out using several types of ultrasonic horns operating at 20 kHz (VC750W processor). The following experimental conditions were evaluated: H2O2 concentration (0.2 to 8.5 mol L-1), horn type (10 to 25 mm of diameter), ultrasound amplitude (20 to 70%), sonication time (10 to 45 min), tannic acid concentration (170 to 1360 mg L-1), and reaction temperature (50 to 90 °C). Gallic acid production was monitored with ultra-performance liquid chromatography with high-resolution time-of-flight mass spectrometry (UPLC-ToF-MS). The isolated gallic acid was confirmed with nuclear magnetic resonance (1H and 13C NMR). It is important to emphasize that this study was developed as a proof of concept to demonstrate the potential of ultrasound for tannic acid conversion into gallic acid using just diluted H2O2. Under selected conditions gallic acid production yield was 128 ± 4 mg g-1 of initial tannic acid (using 170 mg L-1 of tannic acid as starting material). Reaction time was set as 30 min, which was carried out using 1 mol L-1 H2O2 and ultrasound amplitude of 50% at 90 °C. At silent conditions (mechanical stirring, from 100 to 1000 rpm), gallic acid production was halved (less than 78 ± 4 mg g-1 of initial tannic acid).