Electrostatic Effects on Dispersion,Transport, and Deposition of Fine Pharmaceutical Powders: Development of an Experimental Method for Quantitative Analysis

Currently, there is no standard method for testing the electrostatic properties of pharmaceutical powders. The objective of this study was to develop a method of characterizing the dispersion, charging, and transport properties of fine powder flowing through tubes of different materials. Powders of known composition and size distribution were dispersed pneumatically and transported through a short section of tubing containing spiral baffle inserts of the same material to simulate powder flow in long sections of horizontal and vertical tubes with bends. The test powder was dispersed using ring jet suction and passed through the baffled tube to a sampling chamber, from which the powder cloud was sampled for particle size and electrostatic charge distribution measurement using an Electrical Single Particle Aerodynamic Relaxation Time (E-SPART) analyzer. Experimental data on the tribocharging and transport properties of different powders are presented along with an explanation of the charging mechanisms. Analyses of particle size and electrostatic charge distributions in real time and on a single particle basis using the E-SPART analyzer coupled with surface structure analyses with XPS and UPS showed that: (1) most powders are charged bipolarly with relatively high charge-to-mass ratio (Q/M) values that would have a strong effect on transport and deposition of powders; and (2) surface structures, particularly adsorbates, influence the work function and tribocharging of powder. Different methods, including plasma treatment, with minimal changes or contamination of the bulk properties of the powders are also suggested. pharmaceutical powders tribocharging dispersion work function charge distributions charge decay plasma treatment     

Electrostatic Effects on Dispersion, Transport, and Deposition of Fine Pharmaceutical Powders: Development of an Experimental Method for Quantitative Analysis

Currently, there is no standard method for testing the electrostatic properties of pharmaceutical powders. The objective of this study was to develop a method of characterizing the dispersion, charging, and transport properties of fine powder flowing through tubes of different materials. Powders of known composition and size distribution were dispersed pneumatically and transported through a short section of tubing containing spiral baffle inserts of the same material to simulate powder flow in long sections of horizontal and vertical tubes with bends. The test powder was dispersed using ring jet suction and passed through the baffled tube to a sampling chamber, from which the powder cloud was sampled for particle size and electrostatic charge distribution measurement using an Electrical Single Particle Aerodynamic Relaxation Time (E-SPART) analyzer. Experimental data on the tribocharging and transport properties of different powders are presented along with an explanation of the charging mechanisms. Analyses of particle size and electrostatic charge distributions in real time and on a single particle basis using the E-SPART analyzer coupled with surface structure analyses with XPS and UPS showed that: (1) most powders are charged bipolarly with relatively high charge-to-mass ratio (Q/M) values that would have a strong effect on transport and deposition of powders; and (2) surface structures, particularly adsorbates, influence the work function and tribocharging of powder. Different methods, including plasma treatment, with minimal changes or contamination of the bulk properties of the powders are also suggested.

pharmaceutical powders tribocharging dispersion work function charge distributions charge decay plasma treatment     

Near-infrared spectroscopic applications in pharmaceutical particle technology

Abstract

Near-infrared spectroscopy (NIRS) is nowadays an established analytical technique in the pharmaceutical industry. The aim of this review is to present the progress of NIRS in providing useful information for pharmaceutical particle technology. NIR methods are now developed to characterize a wide variety of materials (active pharmaceutical ingredients, excipients, co-processed powders, and physical mixtures) and pharmaceutical dosage forms (conventional, modified drug release technologies, and phytomedicines). This review also provides a number of spectra to illustrate the fundamental understanding of NIRS which has been gained. The sampling that must occur prior to the acquisition of near-infrared spectra is also discussed, as well as developments in monitoring mixing, tableting, and coating. This review will be valuable for product formulation and process engineering specialists.     

稀土永磁材料NdFeN三种粒度分析方法的比较

粉体粒度及粒度分布是粉体颗粒最重要的特性。以稀土永磁材料NdFeN为例,采用激光散射法（干法和湿法）和扫描电镜法对其粒度进行了分析,并比较了三种方法的测试结果。测试结果显示,粒度分析时样品的充分分散是准确测量的基础。将显微镜的直观与激光粒度仪的快速、准确和方便结合起来,对于保证粒度分析结果的可靠性非常有用。     

Effect of base roughness on size segregation in dry granular flows

This paper presents simulations of dry granular flows along a sloping channel using the discrete element method. The kinetic sieving and squeeze expulsion theories are utilized to study the effects of base roughness on size segregation and the underlying mechanisms. Basal friction has a significant influence on flowing regimes inside the granular body, and a larger base friction accelerates the size segregation process. The front zone of the granular body is more likely to be collision dominated with increasing base friction; as a result, the energy dissipated by frictional shearing decreases, and damping energy due to particles collisions is enhanced. Meanwhile, granular flows become much looser, and collisions between particles increase rapidly. It is shown that the differences in the kinetics among grains of mixed sizes and the mechanical effects of particle contacts can explain the mechanism of size segregation. The parameter representing the intensity of particles exchange also increases as base friction increases. The forces acting on particles are also affected by base friction. The dimensionless contact force describing the contribution of contact channel-normal stress increases as base friction increases, which indicates that a higher dispersive trend has developed inside the granular body.     

Pristine and cadmium-doped zinc oxide: chemical synthesis and characterizations

The chemical synthesis of pristine and cadmium-doped ZnO powders using a simple, cost-effective at 65 °C is reported and characterized for their structures, optical and morphological studies using X-ray diffraction, UV–visible–Near Infra-Red (UV–Vis–NIR) spectroscopy, scanning electron microscopy measurement techniques where XRD spectra confirm the formation of ZnO and Cd-doped ZnO with hexagonal crystal structure. The particle size of ZnO is reduced on Cd-doping from 16 to 14 nm. Plane-view surface morphology analysis supported for spherical-type crystallites and UV–Vis–NIR spectra reveal shift in the band edge of ZnO after Cd-doping. Photo-degradation study of Methylene Blue dye shows Pristine ZnO degrades dye faster than Cd-doped ZnO.     

Segregation of cohesive granular materials during discharge from a rectangular hopper

Granular materials may readily segregate due to differences in particle properties such as size, shape, and density. Segregation is common in industrial processes involving granular materials and can occur even after a material has been uniformly blended. The specific objective of this work is to investigate via simulation the effect of particle cohesion due to liquid bridging on particle segregation. Specifically, a bi-disperse granular material flowing from a 3-D hopper is simulated using the discrete element method (DEM) for cohesive particles and the extent of discharge segregation is characterized over time. The cohesion between the particles is described by a pendular liquid bridge force model and the strength of the cohesive bond is characterized by the Bond number determined with respect to the smaller particle species. As the Bond number of the system increases, the extent of discharge segregation in the system decreases. A critical value of Bo = 1 is identified as the condition where the primary mechanism of segregation in the cohesionless hopper system, i.e. gravity-induced percolation, is essentially eliminated due to the liquid bridges between particles.     

超声方式和分散时间对注射成形用铁、镍粉末粒度测量的影响

利用激光衍射法对注射成形用铁、镍原材料粉末进行粒度测量，分别从超声方式和超声时间上对测量条件进行研究。结果表明，对铁粉，宜在大功率超声装置上将样品分散15min后进行测量；对于镍粉，宜在大功率超声装置上将样品分散30min后进行测量。     

A comparison of analytical and data preprocessing methods for spectral fingerprinting

Spectral fingerprinting, as a method of discriminating between plant cultivars and growing treatments for a common set of broccoli samples, was compared for six analytical instruments. Spectra were acquired for finely powdered solid samples using Fourier transform infrared (FT-IR) and Fourier transform near-infrared (NIR) spectrometry. Spectra were also acquired for unfractionated aqueous methanol extracts of the powders using molecular absorption in the ultraviolet (UV) and visible (VIS) regions and mass spectrometry with negative (MS-) and positive (MS+) ionization. The spectra were analyzed using nested one-way analysis of variance (ANOVA) and principal component analysis (PCA) to statistically evaluate the quality of discrimination. All six methods showed statistically significant differences between the cultivars and treatments. The significance of the statistical tests was improved by the judicious selection of spectral regions (IR and NIR), masses (MS+ and MS-), and derivatives (IR, NIR, UV, and VIS).     

Fluidity and Flow Properties of Fine Powders

ABSTRACT

Fluidization and/or flow properties of many fine powders (d₅₀ < 50 μm), including pharmaceutical powders, toners, powder paints, and ceramic powders, are of critical importance. Particles in this range behave as cohesive powder because of the relatively large inter-particle forces (electrostatic, van der Waals', and liquid bridge forces), compared to the hydrodynamic force exerted on the particles by the fluid flowing around the particles. Flow additives, mechanical agitation, and other forces such as acoustic and electromagnetic, are often applied for good fluidization and uniform dilute phase flow. In this paper, we present a brief discussion and experimental data on fluidization properties, fluidity, and flow behavior of several fine powders as functions of particle size distribution, relative humidity, relative concentration of flow additives, and the frequency and amplitude of mechanical agitation. Electrostatic charging, dependent upon the chemical composition and electrical conductivity of the particles, and its influence upon the flow properties are also presented.     

Overcoming Particle Segregation in the Pharmaceutical and Cosmetics Industries

Abstract

Segregation (separation) of particles in mixtures is a common problem in many industries. In the pharmaceutical industry such segregation is often of major concern when handling direct compression formulations prior to pressing tablets or capsules. The result can be unacceptable variations in tablet or capsule weights and/or assays. Similarly in the cosmetics industry, particle segregation can cause severe quality control problems.

Particle segregation can occur by one of five primary mechanisms, three of which are common in the pharmaceutical and cosmetics industries. Which mechanism is predominant in a given application depends on the physical properties of the material being handled as well as the type of equipment being used.

Each of the three common mechanisms will be described in detail. Then typical solutions will be presented for both retrofitting existing facilities as well as designing new plants. While it is not always possible to eliminate segregation, it can usually be minimized to the point that significant gains in product quality can be realized.     

PARTICLE SIZE DISTRIBUTION STUDY OF LANTHANUM-DOPED YTTRIA POWDERS BY SEM-IMAGE ANALYSIS AND LASER LIGHT-SCATTERING METHODS

Particle size analysis of lanthana-doped yttria powders by automatic image analysis (IA) has been used to improve the quality of sizing data obtained using classical laser light scattering methods. A calibration test using monomodal, standard polystyrene spheres confirmed that the IA method provides a narrower distribution and improved size resolution compared to that obtained by light scattering. To ensure that the light-scattering distributions obtained in a study of lanthana-doped yttria powders were accurate, image analysis methods were used to obtain particle size distribution data from which corrected parameters for data reduction of the light-scattering data were obtained. In one case, a bimodal distribution obtained by light-scattering data was found to be artifactural when compared to the distribution obtained from IA measurements. It is concluded that direct particle size distribution analysis by image analysis can be successfully applied in light-scattering studies of yttria powders and can be extended to sizing studies of other powder types.     

Particle size determination in aluminum hydroxide suspensions using near-infrared transmittance spectroscopy

A new method for particle size determination in polystyrene and aluminum hydroxide suspensions using near-infrared transmittance spectroscopy is described. Mono-dispersed polystyrene particle size standards were used to establish the calibration model. The particle sizes used in the study are similar to the wavelength range of 700-1300 nm, where light scattering is wavelength dependent. The wavelength dependency of near-infrared (NIR) absorbance is found to be linear with the particle size when the analysis is based on the same spectrum starting point (the same absorbance at 700 nm). Partial least squares regression (PLSR) is applied to model this linear relationship. Compared to laser diffraction (LD) the NIR method has similar accuracy and precision in the measurement of particles with a uniform size. For a sample containing multiple sizes of particles, the mean size measured by the NIR method is shown to be weighted by the particle mass. The application of the model to aluminum hydroxide suspension shows that the NIR method is suitable for the detection of particle size changes during the production process and storage. The advantages of the NIR method are that no knowledge of the refractive index and the concentration of a sample are necessary and that the method is fast and easy to operate.     

Aerodynamic Characteristics of Popcorn Ash Particles

Popcorn ash particles are fragments of sintered coal fly ash masses that resemble popcorn in low apparent density. They can travel with the flow in the furnace and settle on key places such as catalyst surfaces. Computational fluid dynamics (CFD) models are often used in the design process to prevent the carryover and settling of these particles on catalysts. Particle size, density, and drag coefficient are the most important aerodynamic parameters needed in CFD modeling of particle flow. The objective of this study was to experimentally determine particle size, shape, apparent density, and drag characteristics for popcorn ash particles from a coal-fired power plant. Particle size and shape were characterized by digital photography in three orthogonal directions and by computer image analysis. Particle apparent density was determined by volume and mass measurements. Particle terminal velocities in three directions were measured in water and each particle was also weighed in air and in water. The experimental data were analyzed and models were developed for equivalent sphere and equivalent ellipsoid with apparent density and drag coefficient distributions. The method developed in this study can be used to characterize the aerodynamic properties of popcorn-like particles.     

Mixing of solids in different mixing devices

Mixing of powders is a common operation in any industry. Most powders are known to be cohesive, many agglomerate spontaneously when exposed to humid atmosphere or elevated storage temperature. Agitation of the powder (especially powders with different bulk densities) may result in migration of smaller particles downwards and of larger ones upwards. Another problem is segregation whose main cause is the difference in particle size, density shape and resilience. There are standard mixing devices, such as drum tumblers or Turbula mixers. Alternate device type used is the static mixer of Kenics type. Static mixers save energy, disable segregation and effect particle migration. In this paper, static mixers, as devices for powder mixing, are tested as well as Turbula and V-shaped drum mixer, since those devices are commonly used for powder blending in industry. Mixtures that were blended by means of those three devices were made out of the model material, quartz sand, in different component ratios (20:80 and 30:70). The results were statistically calculated and graphically presented. Cohesion indexes were measured with Powder Flow Analyser to see the effect of material flow on the mixture quality. The results obtained by those three devices, the particle size effect and cohesion indexes, bring us to the conclusion that static mixers could be used for mixing of powders, but their shape, number of mixing elements and the mixer length should be adapted for each mixture separately, experimentally and mathematically, through modelling of the system.     

Segregation due to particle shape of a granular mixture in a slowly rotating tumbler

Using DEM particle simulations we consider segregation of a binary granular particle mixture in a slowly rotating cylindrical tumbler where the particles differ only in their shape—spherical versus more cubical particles. We find that the more cubical particles segregate to the inner core of the particle bed while the spherical particles segregate to the curved walls of the tumbler. The main mechanism for this segregation is different energy dissipation rates for the different particle shape types when avalanching down along the free surface. The cubical particles, due to their sharper corners, dissipate energy much faster than the spherical particles. This results in spherical particles reaching the bottom end of the sloped, free surface which are then transported around the cylinder adjacent to the cylinder wall, as rigid body motion. In contrast to size or density segregation, the segregation due to shape is much weaker and takes longer to reach its equilibrium or steady state. In addition, the segregation occurs along the top surface rather than through the top surface (as occurs for size and density segregation). In general, in situations where two particles differ in their ease of flow (viz flowability) the more rapidly flowing particle will segregate to the base of the free surface (which in the case of the tumbler results in spherical particles near the periphery) and the more slowly flowing particle will segregate underneath.     

Flow properties of spray dried alumina granules using powder flow analysis technique

Commercially available alumina powders having an average particle size of <1 μm were spray dried to granules from aqueous slurries of different solid loadings. Spray drying is a one step granulation technique for obtaining the free flowing granules with desired sizes and morphologies from slurries. These free flowing spray dried granules on subsequent compaction processing results in the powder compacts with high densities and strength. The spray dried granules were evaluated for their flow properties in terms of cohesion index, compaction coefficient, powder flow speed dependency and caking properties using a powder flow analyzer attached to a texture analyzer. Spray-dried granules exhibited the cohesive index value of ～6.5 compared to a value of 16 for the commercially available powder. It is observed that a good correlation can be elucidated with respect to the powder particle size, surface area and morphology. The cake height ratio and compaction coefficient also complimented the above results. Powder flow analysis is an effective method to correlate the flow properties of the ceramic powders with the morphology, granule size and their distribution.     

Application of frequency domain photon migration to particle size analysis and monitoring of pharmaceutical powders

The frequency domain photon migration (FDPM) technique was employed to determine mean particle size of pharmaceutical powders. Results show that the FDPM-measured scattering coefficient increases linearly with reciprocal mean particle size of powdered samples. In contrast to near-infrared spectroscopy techniques, FDPM technique enables determination of scattering and absorption separately so that it does not require data pretreatment and chemometric calibration models. In addition, this unique advantage provides more detailed information about powder samples, which can be used as a potential tool for on-line monitoring of not only variation of active pharmaceutical ingredient concentrations from changes in the absorption coefficient but also variation of particle sizes from changes in the scattering coefficient.     

Comparison of the determination of a low-concentration active ingredient in pharmaceutical tablets by backscatter and transmission Raman spectrometry

A total of 383 tablets of a pharmaceutical product were analyzed by backscatter and transmission Raman spectrometry to determine the concentration of an active pharmaceutical ingredient (API), chlorpheniramine maleate, at the 2% m/m (4 mg) level. As the exact composition of the tablets was unknown, external calibration samples were prepared from chlorpheniramine maleate and microcrystalline cellulose (Avicel) of different particle size. The API peak at 1594 cm(-1) in the second derivative Raman spectra was used to generate linear calibration models. The API concentration predicted using backscatter Raman measurements was relatively insensitive to the particle size of Avicel. With transmission, however, particle size effects were greater and accurate prediction of the API content was only possible when the photon propagation properties of the calibration and sample tablets were matched. Good agreement was obtained with HPLC analysis when matched calibration tablets were used for both modes. When the calibration and sample tablets are not chemically matched, spectral normalization based on calculation of relative intensities cannot be used to reduce the effects of differences in physical properties. The main conclusion is that although better for whole tablet analysis, transmission Raman is more sensitive to differences in the photon propagation properties of the calibration and sample tablets.     

Synthesis and Ag Recovery of Nanosized ZnO Powder by Solution Combustion Process for Photocatalytic Applications

Nanometer-sized ZnO powders for photocatalytic applications were prepared by a solution combustion method with various starting materials and fuels. It was easy to obtain single-phase ZnO powders using the solution combustion method regardless of the starting materials and fuels. However, the particle size and shape of the synthesized ZnO powders were different than the used fuel. Using glycine as a fuel, the particle shape of ZnO powders was spherical with uniform nanosize. On the other hand, using carbohydrazide as a fuel, the particle shape was platelike. The ZnO powder synthesized using Zn(OH)₂ and glycine as starting material and fuel, respectively, showed good powder characteristics, such as average grain size of 75 nm and the specific surface area of 94 m²/g. The average particle size and specific surface area were greatly dependent on the types of oxidants and fuels. Removal of silver ions from a used photo-film developing solution was attempted to examine the photocatalytic activity of the prepared ZnO powders. It also showed excellent photocatalytic properties in that the silver ions were completely removed from the solution within 3 min.