Search results for: falling-needle rheometer

Authors: Lalnuntluanga Hmar, Hardik Vyas

Abstract:

Hydraulic fracturing has become an essential procedure to break apart the rock and release the oil or gas which are trapped tightly in the rock by pumping fracturing fluids at high pressure down into the well. To open the fracture and to transport propping agent along the fracture, proper selection of fracturing fluids is the most crucial components in fracturing operations. Rheology properties of the fluids are usually considered the most important. Among various fracturing fluids, Borate crosslinked fluids have proved to be highly effective. Borate in the form of Boric Acid, borate ion is the most commonly use to crosslink the hydrated polymers and to produce very viscous gels that can stable at high temperature. Guar and HPG (Hydroxypropyl Guar) polymers are the most often used in these fluids. Borate gel rheology is known to be a function of polymer concentration, borate ion concentration, pH, and temperature. The crosslinking using Borate is a function of pH which means it can be formed or reversed simply by altering the pH of the fluid system. The fluid system was prepared by mixing base polymer with water at pH ranging between 8 to 11 and the optimum borate crosslinker efficiency was found to be pH of about 10. The rheology of laboratory prepared Borate crosslinked fracturing fluid was determined using Anton Paar Rheometer and Fann Viscometer. The viscosity was measured at high temperature ranging from 200ᵒF to 250ᵒF and pressures in order to partially stimulate the downhole condition. Rheological measurements reported that the crosslinking increases the viscosity, elasticity and thus fluid capability to transport propping agent.

Keywords: borate, crosslinker, Guar, Hydroxypropyl Guar (HPG), rheology

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Authors: Christopher Giehl, Anja Allabar, Daniela Ehgartner

Abstract:

Rotational rheometry is standard practice for the viscosity measurement of molten glass, neglecting the viscoelastic properties of this material, especially at temperatures approaching the glass transition. Oscillatory rheometry serves as a powerful toolbox for glass melt characterization beyond viscosity measurements. Heating and cooling rates and the time-dependent visco-elastic behavior influence the temperature where materials undergo the glass transition. This study presents quantitative thermo-mechanical visco-elasticity measurements on three samples in the Na-K-Al-Si-O system. The measurements were performed with a Furnace Rheometer System combined with an air-bearing DSR 502 measuring head (Anton Paar) and a Pt90Rh10 measuring geometry. Temperature ramps were conducted in rotation and oscillation, and the (complex) viscosity values were compared to calculated viscosity values based on sample composition. Furthermore, temperature ramps with different frequencies were conducted, also revealing the frequency-dependence of the shear loss modulus G’’ and the shear storage modulus G’. Here, lower oscillatory frequency results in lower glass transition temperature, as defined by the G’-G’’ crossover point. This contribution demonstrates that oscillatory rheometry serves as a powerful toolbox beyond viscosity measurements, as it considers the visco-elasticity of glass melts quantifying viscous and elastic moduli. Further, it offers a strong definition of Tg beyond the 10^12 Pas concept, which cannot be utilized with rotational viscometry data.

Keywords: frequency dependent glass transition, Na-K-Al-Si-O glass melts, oscillatory rheometry, visco-elasticity

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Authors: J. Samuel, S. Al-Enezi, A. Al-Banna

Abstract:

High-density polyethylene reinforced with carbon nanofibers (HDPE/CNF) have been prepared via melt processing using dialkylimidazolium tetrafluoroborate (ionic liquid) as a dispersion agent. The prepared samples were characterized by thermogravimetric (TGA) and differential scanning calorimetric (DSC) analyses. The samples blended with imidazolium ionic liquid exhibit higher thermal stability. DSC analysis showed clear miscibility of ionic liquid in the HDPE matrix and showed single endothermic peak. The melt rheological analysis of HDPE/CNF composites was performed using an oscillatory rheometer. The influence of CNF and ionic liquid concentration (ranging from 0, 0.5, and 1 wt%) on the viscoelastic parameters was investigated at 200 °C with an angular frequency range of 0.1 to 100 rad/s. The rheological analysis shows the shear-thinning behavior for the composites. An improvement in the viscoelastic properties was observed as the nanofiber concentration increases. The progress in the modulus values was attributed to the structural rigidity imparted by the high aspect ratio CNF. The modulus values and complex viscosity of the composites increased significantly at low frequencies. Composites blended with ionic liquid exhibit slightly lower values of complex viscosity and modulus over the corresponding HDPE/CNF compositions. Therefore, reduction in melt viscosity is an additional benefit for polymer composite processing as a result of wetting effect by polymer-ionic liquid combinations.

Keywords: high-density polyethylene, carbon nanofibers, ionic liquid, complex viscosity

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Authors: Mohammad Reza Dousti, Yaman Boluk, Vivek Bindiganavile

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During the past few decades, oil and natural gas consumption have increased significantly. The limited amount of hydrocarbon resources on earth has led to a stronger desire towards efficient drilling, well completion and extracting, with the least time, energy and money wasted. Well cementing is one of the most crucial and important steps in any well completion, to fill the annulus between the casing string and the well bore. However, since it takes place at the end of the drilling process, a satisfying and acceptable job is rarely done. Hence, a large and significant amount of time and energy is then spent in order to do the required corrections or retrofitting the well in some cases. Oil well cement paste needs to be pumped during the cementing process, therefore the rheological and flow behavior of the paste is of great importance. This study examines the use of innovative cellulose-based nanomaterials on the flow properties of the resulting cementitious system. The cementitious paste developed in this research is composed of water, class G oil well cement, bentonite and cellulose nanocrystals (CNC). Bentonite is used as a cross contamination component. Initially, the influence of CNC on the flow and rheological behavior of CNC and bentonite suspensions was assessed. Furthermore, the rheological behavior of oil well cement pastes dosed with CNC was studied using a steady shear parallel-plate rheometer and the results were compared to the rheological behavior of a neat oil well cement paste with no CNC. The parameters assessed were the yield shear stress and the viscosity. Significant changes in yield shear stress and viscosity were observed due to the addition of the CNC. Based on the findings in this study, the addition of a very small dosage of CNC to the oil well cement paste results in a more viscous cement slurry with a higher yield stress, demonstrating a shear thinning behavior.

Keywords: cellulose nanocrystal, flow behavior, oil well cement, rheology

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Authors: Andrea Vasquez, Pedro Maldonado-Alvarado

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In general, 'gluten-free' foods like breadmaking products provide functional or nutraceutical benefits for the consumer's health and increased their demand on the market. In Ecuador, there is an overproduction of superfoods, and the food by-products are undervalued. For the first time, to the author's best knowledge, gluten-free bread mixtures from quinoa and banana flour, cassava starch, lupine flour (LF), or whey protein (WP) with hydroxypropylmethylcellulose (HPMC) and transglutaminase (TG) were evaluated on their functional and sensory properties. Free amino groups and thiols, rheology, and electrophoresis SDS PAGE were performed to analyze the crosslinking of TG at different concentrations with HC or PL proteins. Dough characterization, pasting properties were evaluated, respectively, by a MIXOLAB and a rheometer with a pasting cell. The texture, porosity, and loaf volume were characterized using a texturometer, ImageJ software, and breadmaking ability, respectively. Finally, a breadmaking aptitude and sensorial bread acceptability were performed. A significant decrease in the content of free amino groups (0.16 to 0.11 and 0.46 to 0.36 mM/mg of protein) and free thiol groups (0.37 to 0.21 and 1.79 to 1.32 mM/mg protein) was observed when 1.0% and 0.5% TG were added to LF and WP, respectively. In apparent viscosity analysis, the action of TG on HC proteins changes their viscosity, while the viscosity of LF is not modified by TG. Results of electrophoresis in PL showed bands of higher molecular weight of different fragments of proteins with 1% TG. Formulation with 59.8, 39.9, 160.8, 6.0, 1.0, and 1.5% of, respectively, QF, BF, CS, LF or WP, TG, and HPMC had the best properties in dough parameters, pasting parameters (lower pasting temperature and higher peak viscosity), best crumb structure, lower crumb hardness and higher loaf volume (2.24 and 2.28 mL/g). All the loaves of bread were acceptable in baking aptitude and general acceptability.

Keywords: breadmaking, gluten-free, superfoods, by-products, Ecuador

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Authors: Gerardo Sanjuan Sanjuan, Ángel Enrique Chavéz Castellanos

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The knowledge of the rheological behavior of partially solidified metal alloy is an important issue when modeling and simulation of die filling in semisolid processes. Many experiments for like steady state, the step change in shear rate tests, shear stress ramps have been carried out leading that semi-solid alloys exhibit shear thinning, thixotropic behavior and yield stress. More advanced investigation gives evidence some viscoelastic features can be observed. The viscoelastic properties of materials are determinate by transient or dynamic methods; unfortunately, sparse information exists about oscillation experiments. The aim of this present work is to use small amplitude oscillatory tests for knowledge properties such as G´ and G´´. These properties allow providing information about materials structure. For this purpose, we investigated tin-lead alloy (Sn-15%Pb) which exhibits a similar microstructure to aluminum alloys and is the classic alloy for semisolid thixotropic studies. The experiments were performed with parallel plates rheometer AR-G2. Initially, the liquid alloy is cooled down to the semisolid range, a specific temperature to guarantee a constant fraction solid. Oscillation was performed within the linear viscoelastic regime with a strain sweep. So, the loss modulus G´´, the storage modulus G´ and the loss angle (δ) was monitored. In addition a frequency sweep at a strain below the critical strain for characterized its structure. This provides more information about the interactions among solid particles on a liquid matrix. After testing, the sample was removed then cooled, sectioned and examined metallographically. These experiments demonstrate that the viscoelasticity is sensitive to the solid fraction, and is strongly influenced by the shape and size of particles solid.

Keywords: rheology, semisolid alloys, thixotropic, viscoelasticity

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Authors: T. S. Soliman, A. G. Galyas, E. V. Rusinova, S. A. Vshivkov

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The liquid crystals combining properties of a liquid and an anisotropic crystal substance play an important role in a science and engineering. Molecules of cellulose and its derivatives have rigid helical conformation, stabilized by intramolecular hydrogen bonds. Therefore the macromolecules of these polymers are capable to be ordered at dissolution and form liquid crystals of cholesteric type. Phase diagrams of solutions of some cellulose derivatives are known. However, little is known about the effect of a magnetic field on the viscosity of polymer solutions. The systems hydroxypropyl cellulose (HPC) – ethanol, HPC – ethylene glycol, HPC–DМАA, HPC–DMF, ethyl cellulose (EC)–ethanol, EC–DMF, were studied in the presence and absence of magnetic field. The solution viscosity was determined on a Rheotest RN 4.1 rheometer. The effect of a magnetic field on the solution properties was studied with the use of two magnets, which induces a magnetic-field-lines directed perpendicularly and parallel to the rotational axis of a rotor. Application of the magnetic field is shown to be accompanied by an increase in the additional assembly of macromolecules, as is evident from a gain in the radii of light scattering particles. In the presence of a magnetic field, the long chains of macromolecules are oriented in parallel with field lines. Such an orientation is associated with the molecular diamagnetic anisotropy of macromolecules. As a result, supramolecular particles are formed, especially in the vicinity of the region of liquid crystalline phase transition. The magnetic field leads to the increase in viscosity of solutions. The results were used to plot the concentration dependence of η/η0, where η and η0 are the viscosities of solutions in the presence and absence of a magnetic field, respectively. In this case, the values of viscosity corresponding to low shear rates were chosen because the concentration dependence of viscosity at low shear rates is typical for anisotropic systems. In the investigated composition range, the values of η/η0 are described by a curve with a maximum.

Keywords: rheology, liquid crystals, magnetic field, cellulose ethers

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Authors: Gargi Ghoshal, Ashay Jain, Deepika Thakur, U. S. Shivhare, O. P. Katare

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The main objectives of this work were the rheological characterization of dispersions, emulsions at different pH used in the microcapsules preparation and the microcapsules obtain from gum arabic (A), guar gum (G), casein (C) and whey protein isolate (W) to keep β-carotene protected from degradation using the complex coacervation microencapsulation technique (CCM). The evaluation of rheological properties of dispersions, emulsions of different pH and so obtained microencapsules manifest the changes occur in the molecular structure of wall materials during the encapsulation process of β-carotene. These dispersions, emulsions of different pH and formulated microencapsules were subjected to go through various conducted experiments (flow curve test, amplitude sweep, and frequency sweep test) using controlled stress dynamic rheometer. Flow properties were evaluated as a function of apparent viscosity under steady shear rate ranging from 0.1 to 100 s-1. The frequency sweep test was conducted to determine the extent of viscosity and elasticity present in the samples at constant strain under changing angular frequency range from 0.1 to 100 rad/s at 25ºC. The dispersions and emulsion exhibited a shear thinning non-Newtonian behavior whereas microencapsules are considered as shear-thickening respectively. The apparent viscosity for dispersion, emulsions were decreased at low shear rates 20 s-1 and for microencapsules, it decreases up to ~50 s-1 besides these value, it has shown constant pattern. Oscillatory shear experiments showed a predominant viscous liquid behavior up to crossover frequencies of dispersions of C, W, A at 49.47 rad/s, 57.60 rad/s and 21.45 rad/s emulsion sample of AW at pH 5.0 it was 17.85 rad/s and GW microencapsules 61.40 rad/s respectively whereas no such crossover was found in G dispersion, emulsion with C and microencapsules still it showed more viscous behavior. Storage and loss modulus decreases with time also a shift of the crossover towards lower frequencies for A, W and C was observed respectively. However, their microencapsules showed more viscous behavior as compared to samples prior to blending.

Keywords: viscosity, gums, proteins, frequency sweep test, apparent viscosity

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Authors: Fengxia Li, Lufeng Zhang, Haibo Wang

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The tight sandstone gas reservoir in the Xujiahe Formation of the Sichuan Basin has huge reserves, but its utilization rate is low. Fracturing and stimulation are indispensable technologies to unlock their potential and achieve commercial exploitation. Slickwater is the most widely used fracturing fluid system in the fracturing and renovation of tight reservoirs. However, its viscosity is low, its sand-carrying performance is poor, and the risk of sand blockage is high. Increasing the sand carrying capacity by increasing the displacement will increase the frictional resistance of the pipe string, affecting the resistance reduction performance. The variable viscosity slickwater can flexibly switch between different viscosities in real-time online, effectively overcoming problems such as sand carrying and resistance reduction. Based on a self-developed indoor loop friction testing system, a visualization device for proppant transport, and a HAAKE MARS III rheometer, a comprehensive evaluation was conducted on the performance of variable viscosity slickwater, including resistance reduction, rheology, and sand carrying. The indoor experimental results show that: 1. by changing the concentration of drag-reducing agents, the viscosity of the slippery water can be changed between 2~30mPa. s; 2. the drag reduction rate of the variable viscosity slickwater is above 80%, and the shear rate will not reduce the drag reduction rate of the liquid; under indoor experimental conditions, 15mPa. s of variable viscosity and slickwater can basically achieve effective carrying and uniform placement of proppant. The layered fracturing effect of the JiangX well in the dense sandstone of the Xujiahe Formation shows that the drag reduction rate of the variable viscosity slickwater is 80.42%, and the daily production of the single layer after fracturing is over 50000 cubic meters. This study provides theoretical support and on-site experience for promoting the application of variable viscosity slickwater in tight sandstone gas reservoirs.

Keywords: slickwater, hydraulic fracturing, dynamic sand laying, drag reduction rate, rheological properties

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Authors: Mehmet Doğan, Mahir Alkan, Yasemin Turhan, Zürriye Gündüz, Pinar Beyli, Serap Doğan

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Advances and new discoveries in the field of the material science on the basis of technological developments have played an important role. Today, material science is branched the lower branches such as metals, nonmetals, chemicals, polymers. The polymeric nano composites have found a wide application field as one of the most important among these groups. Many polymers used in the different fields of the industry have been desired to improve the thermal stability. One of the ways to improve this property of the polymers is to form the nano composite products of them using different fillers. There are many using area of boron compounds and is increasing day by day. In order to the further increasing of the variety of using area of boron compounds and industrial importance, it is necessary to synthesis of nano-products and to find yourself new application areas of these products. In this study, PMMA/boronoxide nano composites were synthesized using solution intercalation, polymerization and melting methods; and PAA/boronoxide nano composites using solution intercalation method. Furthermore, rheological properties of nano composites synthesed according to melting method were also studied. Nano composites were characterized by XRD, FTIR-ATR, DTA/TG, BET, SEM, and TEM instruments. The effects of filler material amount, solvent types and mediating reagent on the thermal stability of polymers were investigated. In addition, the rheological properties of PMMA/boronoxide nano composites synthesized by melting method were investigated using High Pressure Capillary Rheometer. XRD analysis showed that boronoxide was dispersed in polymer matrix; FTIR-ATR that there were interactions with boronoxide between PAA and PMMA; and TEM that boronoxide particles had spherical structure, and dispersed in nano sized dimension in polymer matrix; the thermal stability of polymers was increased with the adding of boronoxide in polymer matrix; the decomposition mechanism of PAA was changed. From rheological measurements, it was found that PMMA and PMMA/boronoxide nano composites exhibited non-Newtonian, pseudo-plastic, shear thinning behavior under all experimental conditions.

Keywords: boronoxide, polymer, nanocomposite, rheology, characterization

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Authors: Amani A. Saleh, Maram M. Saudy, Mohamed N. AbouZeid

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Asphalt cement concrete is a very commonly used material in the construction of roads. It has many advantages, such as being easy to use as well as providing high user satisfaction in terms of comfortability and safety on the road. However, there are some problems that come with asphalt cement concrete, such as its high carbon footprint, which makes it environmentally unfriendly. In addition, pavements require frequent maintenance, which could be very costly and uneconomic. The aim of this research is to study the effect of mixing waste-based geopolymers with asphalt binders. Geopolymer mixes were prepared by combining alumino-silicate sources such as fly ash, silica fumes, and metakaolin with alkali activators. The purpose of mixing geopolymers with the asphalt binder is to enhance the rheological and microstructural properties of asphalt. This was done through two phases, where the first phase was developing an optimum mix design of the geopolymer additive itself. The following phase was testing the geopolymer-modified asphalt binder after the addition of the optimum geopolymer mix design to it. The testing of the modified binder is performed according to the Superpave testing procedures, which include the dynamic shear rheometer to measure parameters such as rutting and fatigue cracking, and the rotational viscometer to measure workability. In addition, the microstructural properties of the modified binder is studied using the environmental scanning electron microscopy test (ESEM). In the testing phase, the aim is to observe whether the addition of different geopolymer percentages to the asphalt binder will enhance the properties of the binder and yield desirable results. Furthermore, the tests on the geopolymer-modified binder were carried out at fixed time intervals, therefore, the curing time was the main parameter being tested in this research. It was observed that the addition of geopolymers to asphalt binder has shown an increased performance of asphalt binder with time. It is worth mentioning that carbon emissions are expected to be reduced since geopolymers are environmentally friendly materials that minimize carbon emissions and lead to a more sustainable environment. Additionally, the use of industrial by-products such as fly ash and silica fumes is beneficial in the sense that they are recycled into producing geopolymers instead of being accumulated in landfills and therefore wasting space.

Keywords: geopolymer, rutting, superpave, fatigue cracking, sustainability, waste

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Authors: Francisco J. Cedano, Laura M. Pinzón, Camila I. Castro, Felipe Salcedo, Juan P. Casas, Juan C. Briceño

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Complex fractures located in articular surfaces are challenging to treat and their reduction with conventional treatments could compromise the functionality of the affected limb. An adhesive material to treat those fractures is desirable for orthopedic surgeons. This adhesive must be biocompatible and have a high adhesion to bone surface in an aqueous environment. The proposed adhesive is based on chitosan, given its adhesive and biocompatibility properties. Chitosan is mixed with calcium carbonate and hydroxyapatite, which contribute to structural support and a gel like behavior, and glutaraldehyde is used as a cross-linking agent to keep the adhesive mechanical performance in aqueous environment. This work aims to evaluate the rheological, adhesion strength and biocompatibility properties of the proposed adhesive using in vitro tests. The gelification process of the adhesive was monitored by oscillatory rheometry in an ARG-2 TA Instruments rheometer, using a parallel plate geometry of 22 mm and a gap of 1 mm. Time sweep experiments were conducted at 1 Hz frequency, 1% strain and 37°C from 0 to 2400 s. Adhesion strength is measured using a butt joint test with bovine cancellous bone fragments as substrates. The test is conducted at 5 min, 20min and 24 hours after curing the adhesive under water at 37°C. Biocompatibility is evaluated by a cytotoxicity test in a fibroblast cell culture using MTT assay and SEM. Rheological results concluded that the average gelification time of the adhesive is 820±107 s, also it reaches storage modulus magnitudes up to 106 Pa; The adhesive show solid-like behavior. Butt joint test showed 28.6 ± 9.2 kPa of tensile bond strength for the adhesive cured for 24 hours. Also there was no significant difference in adhesion strength between 20 minutes and 24 hours. MTT showed 70 ± 23 % of active cells at sixth day of culture, this percentage is estimated respect to a positive control (only cells with culture medium and bovine serum). High vacuum SEM observation permitted to localize and study the morphology of fibroblasts presented in the adhesive. All captured fibroblasts presented in SEM typical flatted structure with filopodia growth attached to adhesive surface. This project reports an adhesive based on chitosan that is biocompatible due to high active cells presented in MTT test and these results were correlated using SEM. Also, it has adhesion properties in conditions that model the clinical application, and the adhesion strength do not decrease between 5 minutes and 24 hours.

Keywords: bioadhesive, bone adhesive, calcium carbonate, chitosan, hydroxyapatite, glutaraldehyde

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Authors: Muhammed Ertugrul Celoglu, Beyza Furtana, Mehmet Yilmaz, Baha Vural Kok

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Biomass, which is considered to be one of the largest renewable energy sources in the world, has a potential to be utilized as a bitumen additive after it is processed by a wide variety of thermochemical methods. Furthermore, biomasses are renewable in short amounts of time, and they possess a hydrocarbon structure. These characteristics of biomass promote their usability as additives. One of the most common ways to create materials with significant economic values from biomasses is the processes of pyrolysis. Pyrolysis is defined as the process of an organic matter’s thermochemical degradation (carbonization) at a high temperature and in an anaerobic environment. The resultant liquid substance at the end of the pyrolysis is defined as bio-oil, whereas the resultant solid substance is defined as biochar. Olive pomace is the resultant mildly oily pulp with seeds after olive is pressed and its oil is extracted. It is a significant source of biomass as the waste of olive oil factories. Because olive pomace is waste material, it could create problems just as other waste unless there are appropriate and acceptable areas of utilization. The waste material, which is generated in large amounts, is generally used as fuel and fertilizer. Generally, additive materials are used in order to improve the properties of bituminous binders, and these are usually expensive materials, which are produced chemically. The aim of this study is to investigate the usability of biochars obtained after subjecting olive pomace and smashed olive seeds, which are considered as waste materials, to pyrolysis as additives in bitumen modification. In this way, various ways of use will be provided for waste material, providing both economic and environmental benefits. In this study, olive pomace and smashed olive seeds were used as sources of biomass. Initially, both materials were ground and processed through a No.50 sieve. Both of the sieved materials were subjected to pyrolysis (carbonization) at 400 ℃. Following the process of pyrolysis, bio-oil and biochar were obtained. The obtained biochars were added to B160/220 grade pure bitumen at 10% and 15% rates and modified bitumens were obtained by mixing them in high shear mixtures at 180 ℃ for 1 hour at 2000 rpm. Pure bitumen and four different types of bitumen obtained as a result of the modifications were tested with penetration, softening point, rotational viscometer, and dynamic shear rheometer, evaluating the effects of additives and the ratios of additives. According to the test results obtained, both biochar modifications at both ratios provided improvements in the performance of pure bitumen. In the comparison of the test results of the binders modified with the biochars of olive pomace and smashed olive seed, it was revealed that there was no notable difference in their performances.

Keywords: bituminous binders, biochar, biomass, olive pomace, pomace, pyrolysis

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Authors: Jéssica Bernegossi, Lívia Nordi Dovigo, Marlus Chorilli

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Mucoadhesive liquid crystalline systems are emerging how delivery systems for oral cavity. These systems are interesting since they facilitate the targeting of medicines and change the release enabling a reduction in the number of applications made by the patient. The buccal mucosa is permeable besides present a great blood supply and absence of first pass metabolism, it is a good route of administration. It was developed two systems liquid crystals utilizing as surfactant the ethyl alcohol ethoxylated and propoxylated (30%) as oil phase the oleic acid (60%), and the aqueous phase (10%) dispersion of polymer polyethylenimine (0.5%) or dispersion of polymer poloxamer 407 (16%), with the intention of applying the buccal mucosa. Initially, was performed for characterization of systems the conference by polarized light microscopy and rheological analysis. For the preparation of the systems the components described was added above in glass vials and shaken. Then, 30 and 100% artificial saliva were added to each prepared formulation so as to simulate the environment of the oral cavity. For the verification of the system structure, aliquots of the formulations were observed in glass slide and covered with a coverslip, examined in polarized light microscope (PLM) Axioskop - Zeizz® in 40x magnifier. The formulations were also evaluated for their rheological profile Rheometer TA Instruments®, which were obtained rheograms the selected systems employing fluency mode (flow) in temperature of 37ºC (98.6ºF). In PLM, it was observed that in formulations containing polyethylenimine and poloxamer 407 without the addition of artificial saliva was observed dark-field being indicative of microemulsion, this was also observed with the formulation that was increased with 30% of the artificial saliva. In the formulation that was increased with 100% simulated saliva was shown to be a system structure since it presented anisotropy with the presence of striae being indicative of hexagonal liquid crystalline mesophase system. Upon observation of rheograms, both systems without the addition of artificial saliva showed a Newtonian profile, after addition of 30% artificial saliva have been given a non-Newtonian behavior of the pseudoplastic-thixotropic type and after adding 100% of the saliva artificial proved plastic-thixotropic. Furthermore, it is clearly seen that the formulations containing poloxamer 407 have significantly larger (15-800 Pa) shear stress compared to those containing polyethyleneimine (5-50 Pa), indicating a greater plasticity of these. Thus, it is possible to observe that the addition of saliva was of interest to the system structure, starting from a microemulsion for a liquid crystal system, thereby also changing thereby its rheological behavior. The systems have promising characteristics as controlled release systems to the oral cavity, as it features good fluidity during its possible application and greater structuring of the system when it comes into contact with environmental saliva.

Keywords: liquid crystal system, poloxamer 407, polyethylenimine, rheology

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Authors: Adeline Meriaux, Claire Gaiani, Jennifer Burgain, Frantz Fournier, Lionel Muniglia, Jérémy Petit

Abstract:

Spray-drying process is widely used for the production of dairy powders for food and pharmaceuticals industries. It involves the atomization of a liquid feed into fine droplets, which are subsequently dried through contact with a hot air flow. The resulting powders permit transportation cost reduction and shelf life increase but can also exhibit various interesting functionalities (flowability, solubility, protein modification or acid gelation), depending on operating conditions and milk composition. Indeed, particles porosity, surface composition, lactose crystallization, protein denaturation, protein association or crust formation may change. Links between spray-drying conditions and physicochemical and functional properties of powders were investigated by a design of experiment methodology and analyzed by principal component analysis. Quadratic models were developed, and multicriteria optimization was carried out by the use of genetic algorithm. At the time of abstract submission, verification spray-drying trials are ongoing. To perform experiments, milk from dairy farm was collected, skimmed, froze and spray-dried at different air pressure (between 1 and 3 bars) and outlet temperature (between 75 and 95 °C). Dry matter, minerals content and proteins content were determined by standard method. Solubility index, absorption index and hygroscopicity were determined by method found in literature. Particle size distribution were obtained by laser diffraction granulometry. Location of the powder color in the Cielab color space and water activity were characterized by a colorimeter and an aw-value meter, respectively. Flow properties were characterized with FT4 powder rheometer; in particular compressibility and shearing test were performed. Air pressure and outlet temperature are key factors that directly impact the drying kinetics and powder characteristics during spray-drying process. It was shown that the air pressure affects the particle size distribution by impacting the size of droplet exiting the nozzle. Moreover, small particles lead to more cohesive powder and less saturated color of powders. Higher outlet temperature results in lower moisture level particles which are less sticky and can explain a spray-drying yield increase and the higher cohesiveness; it also leads to particle with low water activity because of the intense evaporation rate. However, it induces a high hygroscopicity, thus, powders tend to get wet rapidly if they are not well stored. On the other hand, high temperature provokes a decrease of native serum proteins which is positively correlated to gelation properties (gel point and firmness). Partial denaturation of serum proteins can improve functional properties of powder. The control of air pressure and outlet temperature during the spray-drying process significantly affects the physicochemical and functional properties of powder. This study permitted to better understand the links between physicochemical and functional properties of powder, to identify correlations between air pressure and outlet temperature. Therefore, mathematical models have been developed and the use of genetic algorithm will allow the optimization of powder functionalities.

Keywords: dairy powders, spray-drying, powders functionalities, design of experiment

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Authors: Adeline Meriaux, Claire Gaiani, Jennifer Burgain, Frantz Fournier, Lionel Muniglia, Jérémy Petit

Abstract:

Spray-drying process is widely used for the production of dairy powders for food and pharmaceuticals industries. It involves the atomization of a liquid feed into fine droplets, which are subsequently dried through contact with a hot air flow. The resulting powders permit transportation cost reduction and shelf life increase but can also exhibit various interesting functionalities (flowability, solubility, protein modification or acid gelation), depending on operating conditions and milk composition. Indeed, particles porosity, surface composition, lactose crystallization, protein denaturation, protein association or crust formation may change. Links between spray-drying conditions and physicochemical and functional properties of powders were investigated by a design of experiment methodology and analyzed by principal component analysis. Quadratic models were developed, and multicriteria optimization was carried out by the use of genetic algorithm. At the time of abstract submission, verification spray-drying trials are ongoing. To perform experiments, milk from dairy farm was collected, skimmed, froze and spray-dried at different air pressure (between 1 and 3 bars) and outlet temperature (between 75 and 95 °C). Dry matter, minerals content and proteins content were determined by standard method. Solubility index, absorption index and hygroscopicity were determined by method found in literature. Particle size distribution were obtained by laser diffraction granulometry. Location of the powder color in the Cielab color space and water activity were characterized by a colorimeter and an aw-value meter, respectively. Flow properties were characterized with FT4 powder rheometer; in particular, compressibility and shearing test were performed. Air pressure and outlet temperature are key factors that directly impact the drying kinetics and powder characteristics during spray-drying process. It was shown that the air pressure affects the particle size distribution by impacting the size of droplet exiting the nozzle. Moreover, small particles lead to more cohesive powder and less saturated color of powders. Higher outlet temperature results in lower moisture level particles which are less sticky and can explain a spray-drying yield increase and the higher cohesiveness; it also leads to particle with low water activity because of the intense evaporation rate. However, it induces a high hygroscopicity, thus, powders tend to get wet rapidly if they are not well stored. On the other hand, high temperature provokes a decrease of native serum proteins, which is positively correlated to gelation properties (gel point and firmness). Partial denaturation of serum proteins can improve functional properties of powder. The control of air pressure and outlet temperature during the spray-drying process significantly affects the physicochemical and functional properties of powder. This study permitted to better understand the links between physicochemical and functional properties of powder to identify correlations between air pressure and outlet temperature. Therefore, mathematical models have been developed, and the use of genetic algorithm will allow the optimization of powder functionalities.

Keywords: dairy powders, spray-drying, powders functionalities, design of experiment

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