A novel set-up and a CFD approach to study the biofilm dynamics as a function of local flow conditions encountered in fresh-cut food processing equipments

The hydrodynamic conditions as well as design and surface properties within fresh-cut food processing equipment create a complex environment for biofilms. A new experimental approach was thus proposed to identify those physical parameters impacting biofilm development in such conditions. A set-up comprising original mock-ups mimicking generic features of washing tanks (e.g. welds, folds, flat surfaces, air/liquid/wall interface) was designed. The flow pattern therein was characterized using two computational fluid dynamic calculation approaches. Full trials were run for 48 h at 10 °C with a Pseudomonas fluorescens strain to identify the preferential biofilm formation areas. As in current industrial systems, the pilot rig had recirculation areas and low wall shear stress rates (τ_w < 0.1 Pa) in corners and angles. These were identified as critical areas with Surface Microbial Loads (SML) over 5 Log₁₀/cm². However, τ_w alone failed to explain why SML in areas under unidirectional flow was higher than in the mock-ups. Lastly, air/liquid/wall interface conditions were more critical than immersed surfaces. This study validated the possibility of using CFD methods to understand the way in which flow pattern influences biofilm formation. The methodology proposed would be helpful in quantifying equipment components criticality based on biofilm growth parameters.     

CO2 laser peeling of Al2O3 ceramic and an application for the polishing of laser cut surfaces

A laser controlled fracture peeling technique is demonstrated to smooth the Al₂O₃ ceramic surface without thermal damages. It was found that a chip can be separated and curled from the ceramic surface during a focused CO₂ continuous wave (CW) laser dual-scanning. The thickness of the curled chip is ～50 μm and the formed subsurface roughness (R_a ≈ 2 μm) is close to the surface machined by mechanical breaking (R_a = 1.84 μm). The chip formation is attributed to the controlled fracture by the residual tensile stress in the recast layer, whereas the chip curling only occurs when the melting depth is shallower than the position of lateral cracks. The peeling technique can be applied to polish the cut surface of laser fusion cutting in ceramics. The polished cut surface (R_a = 2.18 μm) is free from recast, crack and heat effects. The microstructure is similar to the base material. The material removal rate during polishing is up to 0.125 mm³/s.     

In vitro Streptococcus mutans biofilm formation on surfaces of chlorhexidine-containing dentin bonding systems

This in vitro study evaluated the influence of chlorhexidine diacetate (CDA) when blended within dentin bonding systems (DBSs) on Streptococcus mutans (S. mutans) biofilm formation.One commercially available 0.2% wt CDA-containing DBS (Peak Universal Bond) and five experimental 0.2% wt CDA-containing DBS formulations (experimental Adper Scotchbond 1XT plus experimental resins, R₂, R₃, R₄, R₅) were assessed vs their no-CDA containing counterparts. Twenty-eight DBSs disks were prepared for each group (6.4 mm×1.0 mm) and cured for 80 s at 800 mW/cm² in a nitrogen atmosphere. A modified Drip-Flow Reactor was used to grow S. mutans biofilms on specimen surfaces for 24 h and adherent, viable biomass was evaluated using a tetrazolium salt assay (MTT). Two specimens from each of the tested materials were processed with LIVE/DEAD stain and observed using laser confocal microscopy (CLSM) while two disks from each group were examined by using scanning electron microscopy (SEM).MTT assay, CLSM and SEM observations showed that CDA addition decreased, increased or did not change S. mutans biofilm formation. The lowest biofilm formation was obtained with Peak Universal Bond and R₅ (with and without CDA).It may be concluded that the chemical composition of DBSs determines their ability to promote or hamper biofilm formation. Therefore, CDA addition may be helpful in modulating biofilm formation provided that DBS formulation is tuned and optimized.     

Synthesis of a biocompatible polymer using siloxane-based surfactants in supercritical carbon dioxide

Poly(N-vinyl-2-pyrrolidone) (PVP) particles were prepared by dispersion polymerization in the presence of 2,2′-azobisisobutyronitrile as the initiator and siloxane-based surfactant in supercritical carbon dioxide (scCO₂). The dispersants used in this study were non-ionic, non-reactive and commercially produced siloxane-based surfactants (Monasil PCA and KF-6017). We investigated the effect of kinds and concentrations of the surfactants, in addition to the reaction temperature and the concentration of the monomer on the particle size and morphology. PVP microspheres were prepared in 0.23–0.74 μm size range with Monasil PCA and 0.71–1.98 μm size range with KF-6017, respectively. The resulting polymer particle of >90% yield was obtained. Particle size slightly increased with the amount of monomer in polymerization with Monasil PCA. In the case of KF-6017 as the surfactant, there was not an obvious variation in particle size with increasing monomer. Particle size of PVP decreased as surfactant concentration increased from 5.0 to 15.0 wt.% basis on concentration of monomer. The narrow particle size distribution (D_n = 0.23 μm and PSD = 1.06) was presented at the high concentration of Monasil PCA (15 wt.% on monomer concentration). As indicated by the reaction temperature and the addition of organic solvent, which affected solubility of monomer, polymer and surfactant in scCO₂, particle size and particle size distribution of PVP varied. PVP particles with Monasil PCA strongly aggregated at 75 °C in contrast to KF-6017 which showed discrete particles at 65 and 70 °C, but particle size distribution was broad. Particle size was slightly reduced with a little amount of hexane, with an inverse relationship of adding hexane reduced the particle size. The amount of the relative residual surfactants on surface of the polymer after extracting with supercritical fluid process (SFE) was measured by using SEM/EDS and EPMA analysis to map out the distribution of silicon element qualitatively. The original polymer particle before the extraction using CO₂ had the high level of silicon element, but the average level of silicon element became low after CO₂ extraction.     

Supercritical CO2 extraction of lutein esters from marigold (Tagetes erecta L.) enhanced by ultrasound

As a novel technique, supercritical CO₂ (SC-CO₂) extraction enhanced by ultrasound was applied to the extraction of lutein esters from marigold and the extraction curves were described by Sovová model. The mass transfer coefficient in the solid phase (k_s) increased from 3.1 × 10⁻⁹ to 4.3 × 10⁻⁹ m/s due to ultrasound. The effect of extraction parameters including particle size of matrix, temperature, pressure, flow rate of CO₂, and ultrasonic conditions consisting of power, frequency and irradiation time/interval on the yield of lutein esters were investigated with single factor experiments. The results showed that the yield of lutein esters increased significantly with the presence of ultrasound (p < 0.05). The maximal yield of lutein esters (690 mg/100 g) was obtained for a particle size fraction of 0.245–0.350 mm, extraction pressure of 32.5 MPa, temperature of 55 °C and CO₂ flow rate of 10 kg/h with ultrasonic power of 400 W, ultrasonic frequency of 25 kHz and ultrasonic irradiation time/interval of 6/9 s.     

Ovicidal activities of supercritical CO2 and N2O on Ascaris suum eggs

This study examined whether supercritical CO₂ and N₂O fluids are effective in inactivating Ascaris suum eggs, which were chosen as a model for parasite eggs. The treatments were carried out in a multibatch apparatus, in which, the eggs could be placed atop a solid surface (non-immersed condition) or in aqueous solution (immersed condition). Various CO₂ and N₂O phases—including gas (6 MPa, 30 °C), liquid (8 MPa, 30 °C), subcritical (10 MPa, 30 °C), and supercritical (10 MPa, 37 °C)—were tested with exposure times ranging from 1 to 20 min. Supercritical CO₂ and N₂O both showed a similar, strong ovicidal effect, requiring only 1 min in non-immersed conditions and 5 min in water-immersed conditions to achieve a 2.4-log inactivation. Subcritical CO₂ and N₂O showed a weaker ovicidal effect. The effect was significantly reduced for the gas and liquid phases, compared with the supercritical phases. This study reports that supercritical CO₂ and N₂O can be effectively employed as a non-thermal treatment technique to control parasite egg contamination in fecal matter and food.     

Comparison of the rate of CO2 absorption into aqueous ammonia and monoethanolamine

Aqueous ammonia has been proposed as an absorbent for use in CO₂ post combustion capture applications. It has a number of advantages over MEA such as high absorption capacity, low energy requirements for CO₂ regeneration and resistance to oxidative and thermal degradation. However, due to its small molecular weight and large vapour pressure absorption must be carried at low temperature to minimise ammonia loss. In this work the rate of CO₂ absorption into a falling thin film has been measured using a wetted-wall column for aqueous ammonia between 0.6 and 6 mol L^?1, 278–293 K and 0–0.8 liquid CO₂ loading. The results were compared to 5 mol L^?1 MEA at 303 and 313 K. It was found that the overall mass transfer coefficient for aqueous ammonia was at least 1.5–2 times smaller than MEA at the measured temperatures. From determination of the second-order reaction rate constant k₂ (915 L mol^?1 s^?1 at 283 K) and activation energy E_a (61 kJ mol^?1) it was shown that the difference in mass transfer rate is likely due to both the reduced temperature and differences in reactivity between ammonia and MEA with CO₂.     

Fructooligosacharides production in aqueous medium with inulinase from Aspergillus niger and Kluyveromyces marxianus NRRL Y-7571 immobilized and treated in pressurized CO2

This work investigated the influence of compressed CO₂ treatment on the enzymatic activity of immobilized inulinases, and the production of fructooligosacharides in aqueous medium using these enzymes. The effects of system pressure, exposure time and depressurization rate on the enzymatic activity were evaluated through central composite designs (CCD) 2³. Inulinase from Kluyveromyces marxianus NRRL Y-7571 presented an increase of 104% in the residual activity using CO₂ at 275 bar submitted to 6 h treatment, at a depressurization rate of 10 kg m^?3 min^?1. For Aspergillus niger commercial inulinase, a decrease in enzyme activity was observed (residual activity of 39%) using CO₂ treatment at 75 bar for 6 h exposure at the highest depressurization rate (200 kg m^?3 min^?1). Enzymatic activities changed significantly depending on the enzyme source and the experimental treatment conditions investigated. The values of FOS obtained using inulinases from A. niger were 30.64% of GF2; 13.90% of GF3 and 2.88% of GF4 in the medium containing inulin as substrate. Results demonstrate that the use of compressed CO₂ might be of technological importance as a preceding, preparation step, to improve enzyme activity, hence helping the development of new biotransformation processes.     

Enrichment of docosahexaenoic acid from tuna oil via lipase-mediated esterification under pressurized carbon dioxide

This study focused on the use of pressurized CO₂ as a reaction medium for the enrichment of docosahexaenoic acid (DHA) from tuna oil fatty acids via lipase-mediated esterification. Of the three lipases tested, Lipozyme RM IM from Rhizomucor miehei was selected for further study. Enzyme loading, water addition, and reaction time were also explored. Near-supercritical CO₂, prepared at 25 °C and 8.3 MPa, was the most effective reagent tested for enriching DHA from the residual fatty acid fraction. In addition to near-supercritical CO₂, optimal conditions included addition of 0.2 wt% (based on total substrates) water, enzyme loading of 5 wt% (based on total substrates), and a reaction time of 18 h. The DHA concentration and recovery yield for the residual fatty acid fraction under these optimal conditions were 75.8 wt% and 81 wt%, respectively.     

Effect of calcination and reaction conditions on the catalytic performance of Co–Ni/Al2O3 catalyst for CO hydrogenation

The Co–Ni/Al₂O₃ catalysts prepared using impregnation procedure, were used for the Fischer–Tropsch synthesis. The effect of calcination conditions of the catalyst as well as reactor situation was studied. It was found that the catalyst calcined at 550 °C for 6 h in air atmosphere has shown the best catalytic performance for CO hydrogenation. The best operational conditions were obtained as following: T = 350 °C, P = 1 atm and H₂/CO = 2/1.     

Impactor designed to increase mass output rate of nanoparticles from a pneumatic nebulizer

A modular impactor was designed to remove large droplets from aerosols generated by a pneumatic nebulizer, the Six-Jet Atomizer from TSI Inc. (Shoreview, MN), with the aim of generating dry nanoparticles. Three interchangeable nozzle heads were designed to provide droplet cutoff diameters of 0.5, 1, and 2 μm at an air flow rate of 8.3×10^?4 m³ s^?1 (50 L min^?1), which corresponds to all six jets of the nebulizer operated at 25 °C and an air pressure of 241 kPa (35 psi). The collection and output characteristics of the 0.5 μm impactor were evaluated from dry particle size distributions produced by nebulizing an aqueous solution with a NaCl mass fraction of 1% both with and without the impactor present. The impactor characteristic cutoff curve was sharp (impactor geometric standard deviation, GSD_imp=1.15–1.19) with a 50% cutoff diameter d₅₀ that ranged from 0.48 μm at 3.0×10^?4 m³ s^?1 to 0.74 μm at 11.7×10^?4 m³ s^?1. The rate of dry NaCl particle generation ranged from 0.5 to 5 g s^?1 (0.04 to 0.4 g day^?1) with mass median diameters MMD_p=80–123 nm and geometric standard deviations GSD_p=1.6–1.8 (depending on flow rate). Anomalous negative impactor efficiencies were observed at flow rates >8.3×10^?4 m³ s^?1 for 100 to 400 nm droplets and at all flow rates for droplets smaller than 100 nm. This phenomenon will be investigated further as a way to increase the generation rate of nanoparticles. A step-by-step procedure is presented for the selection of an appropriate impactor design and operating flow rate for a desired maximum aerosol particle size.     

Maximum hole concentration for Hydrogen-terminated diamond surfaces with various surface orientations obtained by exposure to highly concentrated NO2

NO₂ exposure drastically increases the hole concentration on the surface of hydrogen (H)-terminated diamond. When the NO₂ gas concentration is higher than 300 ppm, the saturated hole sheet concentration p_s stays the same. Therefore, the p_s value is regarded as the high limit of the concentration of holes on H-terminated diamond surface, p_s,max. In this work, we compared p_s,max, mobility μ, and sheet resistance R_s for (100), (110), and (111) H-terminated surfaces of chemical-vapor-deposited single-crystal diamond. On (110), (111), (100) surfaces, the p_s,max values are 1.717 × 10¹⁴ and 1.512 × 10¹⁴ cm^− 2, and 0.981 × 10¹⁴, respectively. This result supports the first-principle calculations: the hole concentration depends on the energy difference between the valence band maximum and the unoccupied orbitals of adsorbent NO₂ molecules. We have achieved R_s of 719.3 Ω/sq (p_s = 1.456 × 10¹⁴ cm^− 2 and μ = 59.6 cm² V^− 1 s^− 1), the lowest reported so far, on (111) surfaces under 20,000-ppm NO₂ atmosphere.     

Plasma catalysis over lanthanum substituted perovskites

The removal of CH₄ (3600 ppm) with O₂ (3 × 10⁴ ppm) in mixtures with Ar or N₂ as carrier gas has been studied in a plasma-catalyst system. The plasma yields CO plus H₂O as majority products. A small extra oxidation to CO₂ is found at 338 K when a catalyst (SiO₂ or La_1−xSr_xCoO_3−d (x = 0.5) perovskite) is placed in the glow zone of the plasma. With the perovskite, the oxidation efficiency to CO₂ increased with temperature up to 90% at 453 K. This result supports that this lanthanum substituted cobaltite further activates the plasma species producing a synergetic effect where the specific surface area is not a critical factor as previously reported in the literature.     

Effects of Li2CO3 addition on the microstructure and magnetic properties of low-temperature-fired NiCuZn ferrites

NiCuZn ferrites doped with 0.5 wt% Bi₂O₃ and different Li₂CO₃ contents (0–0.25 wt%) were sintered at 900 °C. The microstructure and magnetic properties of these materials were investigated. The addition of low-melting-point Li₂CO₃ led to large and uniform grains. However, excess Li₂CO₃ addition produced abnormal grains and many closed pores, thereby reducing density. Permeability initially increased and then decreased at the Li₂CO₃ content of >0.2 wt%. Maximum magnetic flux density (431.1 mT at room temperature, 339.6 mT at 100 °C) and minimum power loss were achieved at 0.2 wt% Li₂CO₃. These findings suggested the suitability of 0.2 wt% Li₂CO₃ for applications in low-temperature co-fired ceramic magnetic power components and modules.     

Extraction of jojoba oil with liquid CO2 + propane solvent mixtures

In this work liquid CO₂/propane mixtures were used to extract jojoba oil from oilseeds. First, experiments at 313 K and pressures of 70 bar and 200 bars were carried out on jojoba oil deposited on glass spheres, using different solvent concentrations (30 wt%, 50 wt% and 70 wt% CO₂), to assess the influence of the solvent composition and phase behavior on the extraction rate. Then, jojoba oil was extracted from the milled seeds under homogeneous liquid conditions, using solvent mixtures containing 30 wt% and 50 wt% CO₂ at 70 bar and 313 K. A solvent mixture with 30 wt% CO₂ exhibited good solvent power. Oil extraction yields of 98% were obtained using a minimum solvent to oilseed mass ratio of 5 g solvent/g oilseed and operating the extractor at 313 K and 70 bar.     

Highly selective CO2 capture by S-doped microporous carbon materials

S-doped microporous carbon materials were synthesized by the chemical activation of a reduced-graphene-oxide/poly-thiophene material. The material displayed a large CO₂ adsorption capacity of 4.5 mmol g⁻¹ at 298 K and 1 atm, as well as an impressive CO₂ adsorption selectivity over N₂, CH₄ and H₂. The material was shown to exhibit a stable recycling adsorption capacity of 4.0 mmol g⁻¹. The synthesized material showed a maximum specific surface area of 1567 m² g⁻¹ and an optimal CO₂ adsorption pore size of 0.6 nm. The microporosity, surface area and oxidized S content of the material were found to be the determining factors for CO₂ adsorption. These properties show that the as synthesized S-doped microporous carbon material can be more effective than similarly prepared N-doped microporous carbons in CO₂ capture.     

Supercritical CO2 oilseed extraction in multi-vessel plants. 2. Effect of number and geometry of extractors on production cost

The objective of this work was to study production costs for the supercritical CO₂ extraction of a pre-pressed oilseed (packed bed with 2-mm particles) in a 2-m³ industrial multi-vessel plant operating at 40 °C and 30 MPa, using a fully predictive mass transfer model to simulate the process. We modified the inner diameter (47.3 ≤ D ≤ 65.6 cm) and number (n = 2, 3, or 4) of extraction vessels, and the mass flow rate of CO₂ (Q = 3000 or 6000 kg/h), thus changing the aspect ratio of the extraction vessels (3 ≤ L/D ≤ 8), and superficial velocity (2.71 ≤ U ≤ 10.8 mm/s) and specific mass flow rate (6 ≤ q ≤ 24 kg/h per kg substrate) of CO₂. Production cost decreased when increasing the mass flow rate of CO₂ or the number of extraction vessels (or when increasing q). Production cost did not depend on the geometry of extraction vessel for a constant specific mass flow rate of CO₂, but it decreased with a decreasing of the L/D ratio of the vessel for a constant superficial velocity of CO₂. For any given plant, the contribution of fixed cost items (capital, labor) to the production cost increased with extraction time, unlike that of variable cost items (substrate, CO₂, energy), which decreased. Thus, there was an optimal extraction time that minimized production cost for each plant. This work proposes an expression for capital cost of an industrial multi-vessel plant as a function of the mass flow rate of CO₂ (which defines the cost of the solvent cycle of the plant), and the volume of the extraction vessels (which together with number of extraction vessels define the cost of extraction section of the plant), with a scaling factor of 0.48 for both items. Under optimal conditions, capital cost represented 30–40% of the production cost, but uncertainties in capital cost estimates (about ±50% using the proposed expression) may largely affect these estimates. The lowest production cost estimated in this work was USD 7.8/kg oil for the extraction of prepressed oilseed in a four-vessel plant using 6000 kg/h of CO₂. The mass flow rate of CO₂ and number of extraction vessels also affected annual productivity that was about 360 ton oil for the same plant operating 7200 h per year. Oil yields were above 90% for both three- and four-vessel plants.     

Extraction of phenolic compounds and anthocyanins from blueberry (Vaccinium myrtillus L.) residues using supercritical CO2 and pressurized liquids

This work explored the potential of subcritical liquids and supercritical carbon dioxide (CO₂) in the recovery of extracts containing phenolic compounds, antioxidants and anthocyanins from residues of blueberry (Vaccinium myrtillus L.) processing. Supercritical CO₂ and pressurized liquids are alternatives to the use of toxic organic solvents or extraction methods that apply high temperatures. Blueberry is the fruit with the highest antioxidant and polyphenol content, which is present in both peel and pulp. In the extraction with pressurized liquids (PLE), water, ethanol and acetone were used at different proportions, with temperature, pressure and solvent flow rate kept constant at 40 °C, 20 MPa and 10 ml/min, respectively. The extracts were analyzed and the highest antioxidant activities and phenolic contents were found in the extracts obtained with pure ethanol and ethanol + water. The highest concentrations of anthocyanins were recovered with acidified water as solvent. In supercritical fluid extraction (SFE) with CO₂, water, acidified water, and ethanol were used as modifiers, and the best condition for all functional components evaluated was SFE with 90% CO₂, 5% water, and 5% ethanol. Sixteen anthocyanins were identified and quantified by ultra performance liquid chromatography (UPLC).     

Preparation of silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction and liquid phase sintering

Dense silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction method and liquid phase sintering was reported. Ammonium peroxydisulfate ((NH₄)₂S₂O₈) and ammonium carbonate ((NH₄)₂CO₃) were used as acid and base solutions to treat the silicon carbide powder, respectively. Influence of silicon carbide powder with chemical treatment on the preparation of silicon carbide suspension was studied. It was indicated that 50 vol% and 52 vol% silicon carbide suspensions with viscosities of 0.71 Pa s and 0.80 Pa s could be prepared using acid and base treated powders. Influence of silicon carbide powder with chemical treatment on the coagulation process and properties of green bodies and sintered ceramics were studied. It was indicated that silicon carbide green bodies with compressive strength of 1.13 MPa could be prepared using base treated powder. Dense silicon carbide ceramics with relative density above 99.3% and flexural strength of 697 ± 30 MPa had been prepared by DCC via dispersant reaction and liquid phase sintering using Al₂O₃ and Y₂O₃ as additives at 1950 °C for 2 h.     

Palladium-catalyzed Mizoroki–Heck coupling reactions using sterically bulky phosphite ligand

A new catalytic system based on palladium-phosphite for Mizoroki–Heck coupling reactions of aryl iodide and bromide is described. An air-stable phosphite ligand afforded the desired products with high yields in the palladium-catalyzed Mizoroki–Heck reactions. The coupling of aryl iodides was optimized with 0.5 mol% Pd(OAc)₂, 1 mol% phosphite 2, and K₂CO₃ in DMF solvent. For the coupling of aryl bromides, 1 mol% Pd(OAc)₂ and 5 mol% phosphite 2 were required with Na₂CO₃ as base. As a coupling partner alkene, n-butyl acrylate, t-butyl acrylate, styrene and N-t-butyl acrylamide all showed good yields.