Characterization of modified polypropylene by scanning electron microscopy

Characterizing the morphology of modified multiphasic polymer systems, as are often applied for improving the impact strength, is normally a complicated and tedious task. Nevertheless, knowledge about the volume fraction and particle‐size distribution of the elastomer phase is important for the specific development of high‐impact systems. Direct production in the reactor enables only indirect control of these two quantities. Computer‐controlled scanning electron microscopy in combination with image processing allows an automated measurement of both all the necessary particle parameters (size distribution, shape, orientation, etc.) and the elastomer content of the material. Since bulk materials are used for the investigation, additionally, three‐dimensional information about the structure of the material can be gained by simply varying the electron energy, without the necessity to resort to multiple slices. This information is especially important in the case of particles with extremely irregular shapes, as obtained, for example, by strong agglomeration of the modifier particles. The mathematical routines used for calculation of the particle‐size distributions from the measured profile‐size distributions cannot be applied in such cases. The method was tested for several materials with significantly different compositions, both immediately after molding and also after a subsequent thermal relaxation. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 1152–1161, 2000     

Prediction of the porosity of multi-component mixtures of cohesive and non-cohesive particles

This paper presents an experimental and theoretical study of the packing of mixtures of cohesive (fine) and non-cohesive (coarse) particles. The experimental results, produced by means of a standard funnel packing method with glass beads as experimental materials, are first used to depict the similarity between the packings of fine and coarse particles. On this basis, the so-called linear packing model is extended to estimate the porosity of mixtures of fine and coarse particles with a wide size range. Its interaction functions and equivalent packing size are determined empirically. The applicability of the resultant model is demonstrated by the good agreement between the predicted and measured results for typical packing systems, including particles with the Gaudin–Schuhmann distribution or with a mixture size distribution. Finally, the packing of particles with a lognormal distribution, involving both cohesive and non-cohesive particles, is investigated in detail. This example also demonstrates how the proposed model can be used to solve a packing problem.     

Sedimentation Analysis of Disperse Materials

A scanning photosedimentograph with a high accuracy of determination of the granulometric composition of materials is described, which has increased measurement reliability and durability due to the absence of a mechanical drive and the presence of eight measuring channels. Original mathematical software is developed, which allows for automatic determination of integral size distribution of particles.     

Determination of Coating Thickness of DEHS on Submicron Particles by Means of Low Pressure Impaction

The increasing use of submicron and nano‐scaled particles in process engineering sets a demand for new methods for the characterization of particle properties. In the present work low pressure impaction as a very sensitive method for the characterization of the coating of nanoparticles is introduced. The determination of the coating thickness is based on the change of effective density due to the differing densities of particle and coating material. As model systems the coating of spherical silver nanoparticles and agglomerates of silver nanoparticles with DEHS (di(2‐ethylhexyl)sebacate) were used. A tandem differential modelling analyzer (DMA) setup served as a reference for the measurement results obtained with the low pressure impactor (LPI). The LPI showed a very high sensitivity for the coating of spherical particles. Changes of the particle radius below 1 nm could be detected. In contrast to spherical particles, agglomerated particles did not show a clear correlation between coating thickness and the change of effective density for coated agglomerates.     

胶体石墨中石墨细颗粒的制备

胶体石墨是一种多相胶体，其中的分散相（石墨）需求达到一细度，这是制备胶体石墨的先决条件，不同用途的胶体石墨细颗粒的纯度，粒子形态，粒度分布等的要求有所不同，因此在利用机械方法制备石墨细颗粒的过程中，需综合考虑石墨的结构，性能，粉碎过程中的晶体结构变化及所选粉碎设备，粉碎方式，粉碎环境等因素。     

Droplet Size Distribution Obtained by Atomization with Two‐Fluid Nozzles in a Spray Dryer

The possibility of predicting the droplet size distribution from the particle size distribution was investigated. For that purpose, suspensions of different types of materials were dried in a laboratory‐scale spray drier. Drying of suspensions was performed with different sizes of two‐fluid nozzles. Droplet size distribution was evaluated from the data obtained for spray drying of bismuth molybdate suspension. The method was validated experimentally with other tested materials. Investigated systems involve processes of drying, crystallization, and coating. The proposed methodology can be applied when nonagglomerated particles, spherical particles, or spherical agglomerates were obtained by spray drying.     

Machine vision based particle size and size distribution determination of airborne dust particles of wood and bark pellets

Dust management strategies in industrial environment, especially of airborne dust, require quantification and measurement of size and size distribution of the particles. Advanced specialized instruments that measure airborne particle size and size distribution apply indirect methods that involve light scattering, acoustic spectroscopy, and laser diffraction. In this research, we propose a simple and direct method of airborne dust particle dimensional measurement and size distribution analysis using machine vision. The method involves development of a user-coded ImageJ plugin that measures particle length and width and analyzes size distribution of particles based on particle length from high resolution scan images. Test materials were airborne dust from soft pine wood sawdust pellets and ground pine tree bark pellets. Subsamples prepared by dividing the original dust using 230 mesh (63 μm) sieve were analyzed as well. A flatbed document scanner acquired the digital images of the dust particles. Proper sampling, layout of dust particles in singulated arrangement, good contrast smooth background, high resolution images, and accurate algorithm are essential for reliable analysis. A “halo effect” around grey-scale images ensured correct threshold limits. The measurement algorithm used Feret's diameter for particle length and “pixel-march” technique for particle width. Particle size distribution was analyzed in a sieveless manner after grouping particles according to their distinct lengths, and several significant dimensions and parameters of particle size distribution were evaluated. Results of the measurement and analysis were presented in textual and graphical formats. The developed plugin was evaluated to have a dimension measurement accuracy in excess of 98.9% and a computer speed of analysis of < 8 s/image. Arithmetic mean length of original wood and bark pellets airborne dust particles were 0.1138 ± 0.0123 and 0.1181 ± 0.0149 mm, respectively. The airborne dust particles of wood and bark pellets can be described as non-uniform, finer particles dominated, very finely skewed with positive skewness, leptokurtic, and very well sorted category. Experimental mechanical sieving and machine vision methods produced comparable particle size distribution. The limitations and merits of using the machine vision technique for the measurement of size and size distribution of fine particles such as airborne dust were discussed.     

On mixing indices

The current efforts at the National Bureau of Standards to produce a standard reference material (SRM)_for accurate size and concentration measurements in fine particle technology are discussed. Two batches of latex spheres are being characterized as calibration materials for “flow-through” particle counters. The criteria for selecting these materials, and the choice of the packaging techniques are described. The methods of measuring the size of the particles, which will be furnished in aqueous suspension, are discussed along with the measurement data.     

长石粒度对平板玻璃熔制的影响

长石是平板玻璃生产中的一种难熔原料,其粒度大小对配合料的质量存在明显的影响。应用光学显微镜、Ｘ－射线衍射分析等手段研究具有不同长石粒度配合料的熔制、澄清过程,从而确定符合生产需要的长石粒度的优化范围,同时从理论上加以探讨,过粗的长石颗粒不利于玻璃的熔制,其上限应控制在４０￣６０目;而长石颗粒过细也会加剧配合料结团,其下限应控制在１８０目左右。     

A language to simplify computation of differential mobility analyzer response functions

A language for computation of differential mobility analyzer (DMA) response functions is introduced. The language consists of short programming language expressions that evaluate to the size distribution of particles exiting a DMA. The language permits application of the same framework to single and tandem DMA setups. Expressions are derived for calculation of the convolution matrix used in inversion of size distribution data, calculation of the convolution matrix for transit through tandem DMA systems, and calculation of the size and mobility distribution through DMA systems that involve one or multiple DMAs. The contribution of multiply charged particles to the total response distributions can be explicitly resolved. The derived convolution matrix is suitable for inverting scanning mobility particle sizer response functions using standard regularization techniques. Users can modify and substitute any of the convolution terms—comprising the DMA transfer function, detector efficiency, loss rate, and charging efficiencies—to express response functions of nonstandard DMA configurations. Example applications are presented, including classification of particle size, measurement of size-resolved cloud condensation nuclei activity, characterization of hygroscopicity and volatility tandem DMA response functions, and characterization of the dual tandem DMA system for dimer preparation. The source code and examples are shared as free software and are hosted on an online collaborative software development platform that allows for version tracking and crediting contributors. Adoption of the language may facilitate the design and optimization of custom-built systems that involve unique arrangements of DMAs and detectors.

Copyright © 2018 The Author(s). Published with license by Taylor & Francis Group, LLC.     

Preparation and characterization of biomedical collagen–chitosan scaffolds with entrapped ibuprofen and silver nanoparticles

In this work, the preparation and characterization of a novel multifunctional collagen–chitosan material containing silver nanoparticles and nonsteroid anti‐inflammatory drug ibuprofen is described. As a starting material, the commercially available collagen–chitosan scaffold was used. Drug‐loading procedure was performed via supercritical CO₂‐assisted impregnation technique. Silver nanoparticles were prepared via metal vapor synthesis and introduced into the composite biopolymer matrix. An analysis of the small‐angle X‐ray scattering profiles revealed that silver nanoparticles are characterized by having a logarithmic normal size distribution with the maximum at 25 nm. The average size of particles determined from the broadening of diffraction peaks is in a good agreement with this result. The surface of the materials was characterized by X‐ray photoelectron spectroscopy. The in vitro release kinetics of ibuprofen in phosphate buffer solution with pH = 7.4 from prepared materials was studied. The drug release to solution is governed by Fickian diffusion and can be described within the Ritger–Peppas model. Introduction of silver nanoparticles has no effect on the diffusion mechanism. The as‐prepared materials are promising for the medical applications such as dressings for treatments of infected wounds and infection preventing. These materials can act as a matrix for transdermal drug administration. POLYM. ENG. SCI., 59:2479–2487, 2019. © 2019 Society of Plastics Engineers     

On the effective density of non-spherical particles as derived from combined measurements of aerodynamic and mobility equivalent size

Effective densities derived from combined mobility and aerodynamic sizing provide a valuable tool for the characterization of non-spherical particles. Different effective densities have been introduced depending on the primary measurement parameters (mass, mobility and/or aerodynamic size) and the flow regime (transition, free-molecular). Here we explore the relationship between these effective densities, their physical interpretation and their dependence on particle shape, density and various equivalent diameters. We also provide an overview over the wide range of practical implications of the effective density concept with a particular focus on the characterization of particles with irregular or even unknown shape using commercially available instruments such as DMA, SMPS, FMPS, ELPI, APS, TEOM and multi-stage impactors. Finally, we identify new perspectives for particle characterization by extending the effective density concept into the free-molecular regime and by suggesting a triple-instrument approach for on-line determination of both particle density and shape as well as the dynamic shape factor for different flow regimes.     

Manufacture of Powder Coatings by Spraying of Gas‐Enriched Melts

An alternative process for the manufacture of powder coatings was developed. The continuously operated process is applicable to new (low‐melting and fast‐reacting) and conventional powder coating systems and allows to produce coatings with improved properties. The process uses the solubility of compressed gases in melts of coating polymers at pressures up to 220 bar. The single components of a powder coating mixture are melted in separated tanks and are dosed to a static mixer by means of high‐pressure pumps. In the mixer the melts are homogenized and simultaneously compressed carbon dioxide is dissolved. The so‐formed solution is depressurized directly afterwards over a nozzle into a spray tower. Thereby, the melt is atomized into fine droplets and cooled by the expanding gas. The droplets reach the solidification point of the melt and fine solid particles are formed. The particle size, particle size distribution and the morphology of the powders could be adjusted by the operating parameters of the plant.     

Probing pore blocking effects on multiphase reactions within porous catalyst particles using a discrete model

A discrete model coupling mass transfer, reaction, and phase change in porous catalyst particles is proposed to probe pore blocking effects on multiphase reactions. This discrete model is validated by comparing the results with experiments and those obtained using a continuum model, for the hydrogenation of benzene to cyclohexane in Pd/γ‐alumina catalyst particles. The results show that pore blocking has a significant effect on the effectiveness factor and can contribute to up to 50% of the hysteresis loop area for multiphase reactions in porous catalysts, indicating that pore blocking must be accounted for. Moreover, the pore blocking effects are significantly enhanced when the pore network is poorly connected and the pore‐size distribution is wide, while the pore blocking effects are insensitive to the volume‐averaged pore size. Multiphase catalyst material characterization and design should account for this effect. © 2015 American Institute of Chemical Engineers AIChE J, 62: 451–460, 2016     

低阶煤煤泥和浮选精煤制备水煤浆的影响机制研究

以低阶煤煤泥(LS)和浮选精煤煤泥(LF)为原料,通过成浆性实验并结合两种煤泥煤样的粒度分布、表面特性、灰分特征、润湿特性及对分散剂吸附性的测试结果,对LS和LF制备水煤浆的影响机制进行研究。结果表明:分别使用LS和LF作为原料制备水煤浆,当分散剂添加量(干基分散剂与干基原料的质量比)从0%增加至0.7%时,LS的最高成浆浓度(干基煤粉与煤浆的质量比)从58%提高至59%;LF的最高成浆浓度从51%提高至57%;LF与LS相比,灰分质量分数从37.05%降低至13.62%,有机组成无变化,无机矿物中石英含量降低显著,粒度分布范围较窄,对分散剂的饱和吸附量降低;LS和LF煤样中颗粒的径距分别为2.22和1.51,LF中颗粒的堆积效率较低,粒度分布是造成LS和LF成浆性差异显著的主要因素,LF的颗粒较细且尺寸较为接近,煤样颗粒表面的静电力使LF颗粒容易团聚在一起,分散剂作用于粒度较细且粒径相近的LF时,主要用于抵抗分子间的作用力,从而造成LF分散剂消耗量大,采用LF制备水煤浆,需充分考虑粒度分布的影响,选用分散性能较优的水煤浆分散剂。     

Determination of the Nanoparticle Size Distribution in Media by Turbidimetric Measurements

For incorporation of nanoparticles into matrices, it is necessary to control the particle size distribution during processing. In this paper, a turbidimetric method was applied that uses spectroscopic data to determine the nanoparticle size distribution and, consequently, to control the material properties with a non‐contact measurement method. This method is based on the scattering and absorption of light by the particles. Unlike conventional turbidimetric methods, this method uses not only a few wavelengths but a whole spectral range for evaluation. To determine the distribution parameters, a nonlinear numerical least squares fit routine was established. It was validated by comparing data of water‐silica nanosuspensions with the results from the sedimentation method. The results show that this method is an accurate and easy‐to‐use analysis instrument for the characterization of nanosuspensions, emulsions, and aerosols.     

水相和特殊介质中有序聚集体的结构、性质和应用(VI)——反相胶束/微乳液、反相溶致液晶和囊泡

主要介绍了表面活性剂在非水溶剂中形成的各种反相结构体系,其中包括反相胶束/微乳液、溶致液晶以及传统和一些有特殊结构的囊泡体系。同时介绍了用近代测试手段对相应有序聚集体的性能和结构的表征。最后对它们的重要应用也做了介绍,如应用于合成纳米材料的模板,药物载体以及在萃取提纯等方面。     

Modeling of Gravitational Wet Scrubbers with Electrostatic Enhancement

Conventional gravitational wet scrubbers, which generally perform removal of fine particles with low efficiency, cannot meet new standards for pollution emissions. One way of improving the collection efficiency of fine particles is to impose additional electrostatic forces upon particles by means of particle‐charging, or droplet‐charging, or even opposite‐charging of particles and droplets. A Monte Carlo method for population balance modeling is presented to describe the particle removal processes of gravitational wet scrubbers with electrostatic enhancement, in such a way that the grade collection efficiency and particle size distribution are calculated quantitatively. Numerical results show that, the grade collection efficiency of submicron particles is only ca. 5 % in conventional wet scrubbers. However, it reaches ca. 25 % in particle‐charging wet scrubbers, ca. 70 % in droplet‐charging wet scrubbers, and even above 99 % in opposite‐charging wet scrubbers. Furthermore, population balance modeling is used to optimize the operational parameters of the droplet‐charging wet scrubbers by means of the quantitative comparison of the grade collection efficiency. It is found that the operational parameters that are beneficial to the high‐efficiency removal of fine particles are faster gas velocity, slower droplet velocity, larger liquid‐to‐gas flow ratio, larger charge‐to‐mass ratio of droplets, smaller geometric mean diameter and smaller geometric standard deviation of droplets.     

Design principles for spray-roasted iron oxides for the manufacturing of ferrites

A range of high purity iron oxides are prepared by varying basic operation parameters of an industrial spray roasting process. These iron oxides are investigated in relation to their morphology and subsequently evaluated as raw materials for MnZn-ferrite preparation. It appears that the most important morphological parameters for determining the reactivity (defined as firing shrinkage at equal compaction density) of the high purity iron oxide, and consequently the final density and magnetic properties of the ferrite specimens, are the primary particle size and the number of primary particles per aggregate. As found, the specific surface area of the iron oxide is of no predictive value for the behavior of the iron oxide in a MnZn-ferrite manufacturing process. A small primary particle size is important for a high reactivity; however, when particles are packed together in large aggregates, they are not available for the prefiring reactions. As a result, reactive sintering takes place leading to high porosity and bad microstructure. As found by the characterization methods employed in this article, the optimum iron oxides for MnZn-ferrite preparation should have a primary particle size between 0.45 and 0.55 μm with an aggregate size below 1.60 μm.