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The fault gouge, a crushed fault rock resulting from seismic slip, exhibits variations in crystallinity and particle size contingent on the magnitude of deformation. Therefore, the fabrication of fault gouge analogues with carefully controlled properties such as crystallinity, grain size, and mineral composition is necessary to systematically study their role in a range of fault slips. While the single mineral fault gouge analogues have been reproduced using a milling method, the fabrication methods for multi-mineralic fault gouge analogues with varying particle size and crystallinity are rarely reported, yet. In this study, we propose two methodologies for fabricating multi-mineralic fault gouges controlling the degree of amorphization and the particle size using a high-energy ball mill: mixing-grinding (MG) and grinding-mixing (GM) types. The MG type was designed to simulate the fault gouge that the same grinding energy is applied to all the constituent minerals, while the GM type can be controlled the degree of deformation of each mineral according to the research objective. To investigate the effects of these methodologies on the reduction in crystallinity and particle size, we compared the characteristics of MG type_6h and GM type_6h samples, both ground for 6 h. Consequently, despite undergoing the same grinding duration, the GM type_6h sample exhibited more significant reduction in crystallinity and more heterogeneous particle size. Additionally, we fabricated the GM type_Xc50 sample, where the crystallinity of all constituent minerals was reduced to < 50%. For this, each mineral was ground for an optimized duration that reduced its crystallinity to < 50%, after which the samples were mixed. Consequently, the GM type_Xc50 sample demonstrated the greatest reduction in crystallinity and the most uniform particle size distribution. To fabricate the generation process of natural fault gouge, it is appropriate to use the MG type to apply the same energy to constituent mineral, resulting the deformation reflecting its hardness. The GM type is recommended for use in fabricating the characteristics of the fault gouge that has undergone intense deformation at the slip surface, which allows for controlling the uniform crystallinity and particle size reduction of each constituent mineral. Our results suggest that the diverse nature of naturally occurring fault gouges can be fabricated in laboratory settings by adjusting the grinding conditions. This study offers effective methods for fabricating fault gouge analogue for frictional experiments for fault slip and potential applications in simulating geochemical reactions in fault zones. [ABSTRACT FROM AUTHOR]

Aqueous suspensions containing crystalline drug in the sub-micron range is a favorable platform for long-acting injectables where particle size can be used to obtain a desired plasma-concentration profile. Stabilizers are added to the suspensions and screened extensively to define the optimal formulation composition. In the initial formulation screening the amount of drug compound can be limited, necessitating milling methods for small-volume screening predictable for scale-up. Hence, adaptive focused ultrasound was investigated as a potential milling method for rapid small-volume suspensions by identifying the critical process parameters during preparation. Suspensions containing drug compounds with different mechanical properties and thereby grindability, i.e., cinnarizine, haloperidol, and indomethacin with brittle, elastic, and plastic properties, respectively, were investigated to gain an understanding of the manufacturing with adaptive focused acoustics as well as comparison to already established milling techniques. Using a DoE-design, peak incident power was identified as the most crucial process parameter impacting the milling process for all three compounds. It was possible to decrease the sizes of drug particles to micron range after one minute of focused ultrasound exposure which was superior compared to other milling techniques (e.g., non-focused ultrasound exposure). The addition of milling beads decreased the drug particle sizes even further, thus to a lower degree than other already established milling techniques such as milling by dual centrifugation. This study thereby demonstrated that adaptive focused ultrasonication was a promising method for rapid homogenization and particle size reduction to micron range for different compounds varying in grindability without altering the crystalline structure. [ABSTRACT FROM AUTHOR]

Particle size reduction by ultrasound is more favorable than conventional grinding due to its tendency to preserve the material's crystal structure. For palygorskite clay, the optimization was carried out using response surface methodology for the variables of sonication time, power, duty cycle, and clay loading. A 2FI model was fit to the dimensionless size number to navigate the design space of the model with an r-squared value of 0.9662. We found that the most optimal conditions for the size reduction were 45 min of sonication time, 110 W of sonication power, 90% duty cycle and 0.06 g/mL of clay loading. The loading and duty cycle terms had a positive effect on the particle size reduction, while an increase in power increased the particle size of the clay. The effect of time was found to be dependent on the values of the clay loading as well as the duty cycle. The XRD analysis of palygorskite clay for the untreated and treated samples indicated that ultrasound causes minimal changes to the crystal structure of the clay. The overall outcome of the study suggests that at optimal ultrasound conditions, particle size is reduced to ~ 1/16 times the initial value and the electric power input in the ultrasound generator takes an energy requirement of ~ 0.0124 kWh/g of solids processed for size reduction. [ABSTRACT FROM AUTHOR]

Fault gouge, located in highly deformed fault cores, shows substantial particle size reduction and loss of crystallinity, which could affect the physicochemical properties and thus control the slip behavior and earthquake stability of a fault. To systematically investigate the effect of deformed fault gouge on fault slip behavior in laboratory-scale experiments, a fault gouge analog with variable particle size and crystallinity is required. However, the systematic study for formation of a fault gouge analog (i.e., controlling the particle size and crystallinity) was not performed well. In this study, we investigated the effect of the rotation speed of a high-energy ball mill on particle size reduction rate and degree of amorphization. As the rotation speed increased from 500 to 2000 rpm, the comminution rate linearly increased, and reached a reduced particle size limit. The degree of amorphization and its rate also increased with increasing rotation speed. Upon grinding, the X-ray diffraction (XRD) peaks markedly decreased and reached critical amorphization points within 120 min, except for the case of grinding with a rotation speed of 500 rpm. Talc ground with a rotation speed of 500 rpm did not reach steady-state in mechanical amorphization after 360 min of grinding, thus necessitating prolonged grinding for further amorphization. A comparison of talc powders having similar specific surface areas, but ground at different rotation speeds, shows that grinding with a higher rotation speed for a shorter duration preserves the crystalline structure relatively well compared with grinding at a lower rotation speed for a longer duration. These results indicate that optimizing the grinding rotation speed facilitates the formation of talc fault gouge analogs with systematically varying particle size and crystallinity. The specific surface area of talc increased from 6.1 to 365 m2/g, and the degree of crystallinity decreased from approximately 75% to 11%. Our results indicate that an artificial talc fault gouge can be prepared by varying the particle size and crystallinity using a high-energy ball mill. [ABSTRACT FROM AUTHOR]

In pharmaceutical research and development, various new chemical entities (NCE) are found to be poorly water-soluble. Therefore, solubility enhancement, a key factor for higher bioavailability, is a major challenge in pharmaceutical industries. Particle size reduction is one such method that increases the surface area of the pharmaceutical compounds and subsequently leads to a higher dissolution rate and bioavailability. Conventional processes such as milling, high-pressure homogenization, and spray drying are well established and widely used for particle size reduction. However, a few disadvantages such as a broader particle size distribution (PSD) and thermal and chemical degradation of the product are major concerns for the product quality. Non-conventional processes such as liquid anti-solvent crystallization, supercritical anti-solvent process, rapid expansion of supercritical solutions, particles from gas saturated solutions, and pulsed laser ablation are emerging as potential alternatives to overcome the disadvantages of conventional processes. This review critically summarizes the milling, spray drying, high-pressure homogenization, liquid anti-solvent crystallization, spray freeze-drying, supercritical carbon dioxide (SC C O 2) –based micronization processes, pulsed laser ablation and combinative techniques. The success of these processes in enhancing the dissolution rate and bioavailability of many active pharmaceutical ingredients (APIs) has been critically examined. The advantages and limitations of these processes are also discussed. Finally, opportunities for future research are also proposed. [ABSTRACT FROM AUTHOR]

The conditions of size reduction of particles of an emulsion disperse phase during its movement in the holes of the rotor and stator of a high-speed rotary disperser are studied. Analytical relationships that allow determination of the magnitude of tensile forces acting on the ends of the particle located on the sharp edge of the rotor hole were obtained. It is shown that the magnitude of tensile forces depends on the particle mass, angles of the hole edges, diameter, and angular speed of the rotor. As the rotation speed increases and the rotor hole edge angles decrease, the tensile forces acting on the particle ends increase, which increases the probability of its fragmentation into two parts. [ABSTRACT FROM AUTHOR]

Temperature sweep tests and steady shear properties of five different food hydrocolloids (guar gum, xanthan gum, carboxymethylcellulose, pectin and carrageenan) in two different particle sizes groups have been determined at 25, 40, 60 and 80 °C in 1% aqueous solution. Also, the Scanning Electron Microscopy (SEM) images of gums were taken to investigate the morphological properties of the samples. The particle size and processing temperature significantly affected all rheological parameters of the hydrocolloid solutions. The flow behavior of the samples was fitted to Ostwald de Waele model (R2 = 0.959). The highest n value was recorded at 60 °C for all samples. The most drastic changes in consistency coefficient (K) values of the samples were observed in carrageenan solution and it was ranged from 0.013 to 1.774 Pa.sn before the size reduction and from 0.007 to 0.337 Pa.sn after the size reduction process. As the consistency coefficient (K) and apparent viscosity (η50) decreased with the temperature, the flow behavior index increased in both group of samples. As a result, it was concluded that the increase in processing temperature and size reduction process caused a decrease in resistance of hydrocolloid solutions subjected to the deformation, which is a very important factor affecting the quality and good mouth-feel of products. [ABSTRACT FROM AUTHOR]

Purpose: To develop a small-scale set-up to rapidly and accurately determine the intrinsic dissolution rate (IDR) and apparent solubility of poorly water-soluble compounds. Methods: The IDR and apparent solubility (S) were measured in fasted state simulated intestinal fluid (FaSSIF) for six model compounds using wet-milled controlled suspensions (1.0% ( w/w) PVP and 0.2% ( w/w) SDS) and the μDISS Profiler. Particle size distribution was measured using a Zetasizer and the total surface area was calculated making use of the density of the compound. Powder and disc dissolution were performed and compared to the IDR of the controlled suspensions. Results: The IDR values obtained from the controlled suspensions were in excellent agreement with IDR from disc measurements. The method used low amount of compound (μg-scale) and the experiments were completed within a few minutes. The IDR values ranged from 0.2-70.6 μg/min/cm and the IDR/S ratio ranged from 0.015 to 0.23. This ratio was used to indicate particle size sensitivity on intestinal concentrations reached for poorly water-soluble compounds. Conclusions: The established method is a new, desirable tool that provides the means for rapid and highly accurate measurements of the IDR and apparent solubility in biorelevant dissolution media. The IDR/S is proposed as a measure of particle size sensitivity when significant solubilization may occur. [ABSTRACT FROM AUTHOR]

To improve the poor water solubility and dissolution rate of the oral hypoglycemic drug glibenclamide, it was molecularly dispersed in Neusilin UFL2, an amorphous synthetic form of magnesium aluminometasilicate, at different proportions; the physicochemical and biopharmaceutical properties, as well as the stability of the four different batches recovered were characterised, and it was determined that complete dispersion of glibenclamide in the amorphous polymer was obtained at the drug to Neusilin ratio of 1 to 2.5. Completely amorphous dispersion was proven by Thermal Analysis and X-Ray Powder Diffractometry. Very small particles were obtained, ranging from approximately 200 to 400 nm. The amorphous batches were physically and chemically stable for the entire duration of experiments. The physicochemical properties of the four batches were compared to those of the starting materials and physical mixtures of Neusilin UFL2 and glibenclamide, the latter showing the typical behaviour of simple mixes, i.e., the additivity of properties of single components. The dissolution studies of the four solid dispersions revealed a very high dissolution rate of the completely amorphous batches (Batches 3 and 4), behaviour that was ascribed to their high Intrinsic dissolution rate due to the amorphous characteristics of the solid dispersions, to their very small particle size, and to the presence of polysorbate 80 that improved solid wettability. The technique under investigation thus proved effective for recovering stable amorphous dispersions of very small particle sizes. [ABSTRACT FROM AUTHOR]

With the aim of reducing phytic acid content of wheat bran, particle size reduction (from 1,200 to 90 μm), hydrothermal (wet steeping in acetate buffer at pH 4.8 at 55 °C for 60 min) and fermentation (using bakery yeast for 8 h at 30 °C) and combination of these treatments with particle size reduction were applied and their effects on some properties of the bran were studied. Phytic acid content decreased from 50.1 to 21.6, 32.8 and 43.9 mg/g after particle size reduction, hydrothermal and fermentation, respectively. Particle size reduction along with these treatments further reduced phytic acid content up to 76.4 % and 57.3 %, respectively. Hydrothermal and fermentation decreased, while particle size reduction alone or in combination increased bran lightness. With reducing particle size, total, soluble and insoluble fiber content decreased from 69.7 to 32.1 %, 12.2 to 7.9 % and 57.4 to 24.3 %, respectively. The highest total (74.4 %) and soluble (21.4 %) and the lowest insoluble fiber (52.1 %) content were determined for the hydrothermaled bran. Particle size reduction decreased swelling power, water solubility and water holding capacity. Swelling power and water holding capacity of the hydrothermaled and fermented brans were lower, while water solubility was higher than the control. The amount of Fe, Zn and Ca decreased with reducing particle size. Fermentation had no effect on Feand Zn but slightly reduced Ca. The hydrothermal treatment slightly decreased these elements. Amongst all, hydrothermal treatment along with particle size reduction resulted in the lowest phytic acid and highest fiber content. [ABSTRACT FROM AUTHOR]

Cellulosic feedstocks for bioenergy differ in composition and processing requirements for efficient conversion to chemicals and fuels. This study discusses and compares the processing requirements for three lignocellulosic feedstocks-soybean hulls, wheat straw, and de-starched wheat bran. They were ground with a hammer mill to investigate how differences in composition and particle size affect the hydrolysis process. Enzyme hydrolysis was conducted using cellulase from Trichoderma reesei at 50°C and pH 5. Ground fractions were also subjected to dilute sulfuric acid treatment at 125°C, 15 psi for 30 min prior to cellulase treatment. Reducing particle size of biomass resulted in segregated components of feedstock. Grinding wheat straw to particle size <132 μm resulted in measured lignin content from 20% to ≈5% and reduced hemicellulose content. Reducing lignin content increased the effectiveness of enzyme hydrolysis of wheat straw. Particles sized <132 μm exhibited the highest soluble sugar release upon hydrolysis for all three feedstocks studied. Hemicellulose digestion improved with dilute sulfuric acid treatment with residual hemicellulose content <5% in all three feedstocks after acid treatment. This enhanced the cellulase action and resulted in approximately 1.6-fold increase in sugar availability in de-starched wheat bran and ≈1.5-fold for wheat straw and soybean hulls. Higher sugar availability in wheat bran after acid-mediated enzyme treatment correlated to higher ethanol yields during yeast fermentation compared with soybean hulls and wheat straw. [ABSTRACT FROM AUTHOR]

The synthesis of LiFePO from a melt cast of LiCO, FePO, and carbon precursors at 1,000 °C was recently reported. The results indicate that it could be a competitive technique for the large-scale production of LiFePO. This paper focuses on particle size reduction and non-stoichiometric synthesis of LiFePO. The particles size was reduced using a planetary mill that is available in most research laboratories where the milling time and milling media were varied to obtain the best electrochemical results. In addition, the electrochemical performance of LiFePO products synthesized from $$ {\hbox{FeP}}{{\hbox{O}}_4} + x{/2}\,{\hbox{L}}{{\hbox{i}}_2}{\hbox{C}}{{\hbox{O}}_3} + {\hbox{C}} $$ (sequentially varying the amount of x) at 1,000 °C has also been measured. The stoichiometric LiFePO product shows the best capacity, while the off-stoichiometric material demonstrates different levels of impurities that have an effect on the performance of the material. The results indicate that adequate capacity at low discharge rates can be obtained using standard milling techniques, but, in order to obtain material from a melt cast synthesis that provides higher performance at faster discharge rates, a further particle size reduction will be required. [ABSTRACT FROM AUTHOR]

The purpose of this study was to design and build a supercritical CO2 anti-solvent (SAS) unit and use it to produce microparticles of the class II drug carbamazepine. The operation conditions of the constructed unit affected the carbamazepine yield. Optimal conditions were: organic solution flow rate of 0.15 mL/min, CO2 flow rate of 7.5 mL/min, pressure of 4,200 psi, over 3,000 s and at 33°C. The drug solid-state characteristics, morphology and size distribution were examined before and after processing using X-ray powder diffraction and differential scanning calorimetry, scanning electron microscopy and laser diffraction particle size analysis, respectively. The in vitro dissolution of the treated particles was investigated and compared to that of untreated particles. Results revealed a change in the crystalline structure of carbamazepine with different polymorphs co-existing under various operation conditions. Scanning electron micrographs showed a change in the crystalline habit from the prismatic into bundled whiskers, fibers and filaments. The volume weighted diameter was reduced from 209 to 29 μm. Furthermore, the SAS CO2 process yielded particles with significantly improved in vitro dissolution. Further research is needed to optimize the operation conditions of the self-built unit to maximize the production yield and produce a uniform polymorphic form of carbamazepine. [ABSTRACT FROM AUTHOR]

The aim of this study was to examine the effect of mechanical milling time on physicochemical properties and stability of Cefotaxime sodium (CS). CS was micronized by ball milling in five period of time: 30, 60, 120, 240, and 360 min. The powder properties of the samples were examined by HPLC assay, laser diffraction, helium densitometery, IR spectrophotometery, X-ray diffraction (XRD), scaning electron microscopy (SEM), differential scanning calorimetery (DSC), thermogravimetric analysis (TGA) and Karl-Fisher titrimetery. The results showed that ball milling was not an appropriate method for particle size reduction to make solid dosage form such as dry powder inhaler formulation (DPI) of CS and by increase in milling time, degradation of CS increased. [ABSTRACT FROM AUTHOR]

Lignocellulosic materials pretreated using liquid hot water (LHW) (220°C, 5 MPa, 120 s) were fermented to ethanol by batch simultaneous saccharification and fermentation (SSF) using Saccharomyces cerevisiae in the presence of Trichoderma reesei cellulase. SSF of sugarcane bagasse (as received), aspen chips (smallest dimension 3 mm), and mixed hardwood flour (−60 +70 mesh) resulted in 90% conversion to ethanol in 2-5 d at enzyme loadings of 15-30 FPU/g. In most cases, 90% of the final conversion was achieved within 75 h of inoculation. Comminution of the pretreated substrates did not affect the conversion to ethanol. The hydrolysate produced from the LHW pretreatment showed slight inhibition of batch growth of S. cerevisiae. Solids pretreated at a concentration of 100 g/L were as reactive as those pretreated at a lower concentration, provided that the temperature was maintained at 220°C. [ABSTRACT FROM AUTHOR]