On‐line Determination of Particle Size Distributions in Flowing Dispersions

Emulsions are of great importance to industry. They are involved in many engineering operations, including chemical reactions, extraction, emulsification and suspension polymerization, etc. However, an important problem for these processes is how to control the size distribution of the dispersed phase. Indeed, off‐line analysis of the emulsion may generate uncertainties due to sampling and dilution of the product, which are likely to change the dispersion state and physico‐chemical properties. In this work, an on‐line optical method is proposed to characterize dispersed media in real flowing conditions. This method is based on the time‐analysis of back‐scattered light fluctuations. The present paper deals with the development of this method and its application to dispersions of alumina in water. The results obtained with the on‐line optical method are compared with those acquired by classical laser light scattering and microscopy.     

Development of a Method for the Measurement of Particle Size and Velocity based on Projection onto a Variable Frequency Grating

Irregular particles down to approximately 3.8 μm have been sized by imaging them onto a variable frequency grating using laser illumination. Velocity can also be determined. The method was successful for certain particle types that were rough or irregular, partly absorbing or translucent. It was not successful for transparent spheres that display glare spots in the image, or other particles that produce localised regions of high brightness.     

Estimating Average Particle Size by Focused Beam Reflectance Measurement (FBRM)

The Lasentec focused beam reflectance measurement (FBRM) probe provides in situ particle characterisation over a wide range of suspension concentrations. This is a significant advantage over conventional instruments that require sampling and dilution. However, FBRM gives a chord distribution, rather than a conventional diameter distribution. Both theoretical and empirical methods for converting from chord to diameter data are available, but the empirical method was found to be more successful.     

Size and Shape Analysis of Sedimentary Grains by Automated Dynamic Image Analysis

The application of Automated Dynamic Image Analysis (ADIA) for measuring the size and shape of sedimentary grains is presented. This technique determines the size and shape of a large number of particles (typically 5,000 to 50,000 or greater) in the size range between 10 to 1,500 μm. ADIA measurements are carried out using a RapidVue particle analyzer. The size and shape of particles are obtained by analyzing digital images. Each image is composed of shapes representing two‐dimensional projections of particles. The analysis yields the area and perimeter of each particle cross‐section, which are transformed into size‐independent shape values. The analysis of such a large number of particles results in a very small statistical variation of the results, ca. 0.3% for 50,000 particles. Since operator selection of images does not enter the measurement procedure, the risk of bias caused by subjective sample selection is eliminated. The combination of ADIA with a two‐dimensional Kolmogorov‐Smirnov test, allows the identification of similarities and differences between sedimentary grains.     

On‐line Determination of Aggregate Size and Morphology in Suspensions

Information concerning the aggregation state of fine solid particles is an important element for process control and monitoring of product quality in many applications of industrial slurries. This work deals with the application of different in‐line methods to the characterization of silica aggregate size and morphology. All of these methods exploit turbidity signals, obtained by various means including: from analysis of turbidity fluctuations in homogeneous suspension and from overall turbidity decrease during particle settling. This work also presents the opportunity to report progress in morphological and optical models of small aggregates. As a result of these models, the morphological characteristics of the aggregates along with the number of their constituting particles are derived from experimental results. Similarities between the different methods are examined and discussed.     

A Comparative Study of Various Size Distribution

One of the major product specifications of a crystalline material is the crystal size distribution (CSD). In order to monitor and control the CSD in an industrial crystallization process, on‐line sensors are required. Over the years, a number of techniques to measure the CSD have been established. In this paper, three instruments operated in an on‐line fashion and an off‐line method are compared. The instruments were the OPUS, a HELOS/VARIO (both manufactured by Sympatec) and a Malvern 2600c (manufactured by Malvern). They were implemented on an 1100‐l evaporative draft tube baffle (DTB) crystallizer producing ammonium sulfate crystals from aqueous solution. Samples from this crystallizer were also analyzed offline by wet sieving. The results show reasonably good agreement between the different on‐line techniques and the wet sieving technique concerning the shape of the distribution. However, there is a discrepancy regarding the absolute values, which can be explained by the fact that the techniques used are based on different measuring principles.     

Crystal Shape Characterisation of Dry Samples using Microscopic and Dynamic Image Analysis

A standard method to determine particle shape and size is by image analysis. This paper addresses microscopic image analysis (semi‐automated) investigations of two different organic crystalline chemicals generated by batch cooling crystallisation. The results generated from microscopic image analysis were compared with data obtained by dynamic image analysis (automated) because very few contributions are available in the open literature. The chemical systems were polymorphic L‐glutamic acid which crystallises into α (prismatic) or β (needle) form and the non‐polymorphic mono sodium glutamate which crystallises into needles. The images from these techniques were processed to generate information on crystal shape and size. It has been observed that shape effects can distort the size obtained in size characterization studies. In this study, comparisons were made of processing time, number of crystals and accuracy between microscopic and dynamic image analysis. For representative microscopic image analysis, 5000 crystals were analysed in an average of eight hours while several hundred thousand crystals were processed using dynamic image analysis within 15 minutes. Using the parameters D₁₀, D₅₀, D₉₀, span and aspect ratio for statistical comparison, it was found that the results obtained for D₅₀ by the two techniques were comparable and in accordance with other measurements (laser diffraction spectroscopy and ultrasonic attenuation spectroscopy) even though these non‐spherical particles had different orientations during measurement by the two methods. However, substantial differences in span of the distribution and aspect ratio were returned by the two techniques.     

On‐line surface enhanced Raman spectroscopic detection in a recyclable Au@SiO2 modified glass capillary

A facile method was developed to fabricate a high sensitive, reproducible and recyclable surface enhanced Raman spectroscopy (SERS) active glass capillary. The Au nanoparticles were synthesized through a seed‐mediated growth approach and then self‐assembled onto the inner wall of glass capillaries. The attached Au nanoparticles were homogeneously coated with thin silica shell by using the silane coupling agent to functionalize the Au surface. By using thiophenol (TP) as SERS probe molecules, the substrate exhibited robust SERS effects. The adsorbed SERS probe molecules could be rapidly and completely removed away by flowing sodium borohydride solution and thus to obtain a refresh Au@SiO₂ film‐coated substrate for the cyclic detection on different species. The on‐line detection of TP and malachite green (MG) with different concentrations was performed in the flowing system. The intensities of SERS signals were dependent on concentrations of the detected molecules. The results indicated that the SERS‐active substrate has potential applications on the on‐line qualitative and quasi‐quantitative analysis. Copyright © 2014 John Wiley & Sons, Ltd.     

Method of Measuring the Spectral Shape of the Radiation Line of a Three-Micron Long-Path Laser Gas Analyzer

A new method to experimentally determine the spectral shape of the radiation line of a tunable long-path absorption laser gas analyzer operating in a three-micron range ( = 2.5–4.5 m) on the basis of a difference-frequency generator is suggested. The method is based on measurement of the transmission function of a gas medium upon modulation of its optical thickness or pressure. Specific vibrational–rotational transitions and also optimal pressures of CO₂, N₂O, and CH₄ are recommended for carrying out experiments.     

A Novel Device for Single Particle Light Scattering Size Analysis and Concentration Measurement at High Pressures and Temperatures

Based on the findings of previous work, a novel instrument was developed for the size analysis and concentration measurement of particles dispersed in gases at high temperatures (600 °C) and pressures (16 bar). The main motivation for the construction of this device was a measurement requirement at the conditions of a pressurized pulverized coal combustion (PPCC) test installation in Dorsten, Germany. The development of a high efficiency (> 50 %), coal based, combined cycle process, and specifically, the development of efficient gas cleaning technology for gas combustion under demanding conditions (1400 °C and 16 bar) was the main target. A suitable measurement technique was required for the determination of particle size and concentration downstream of the gas cleaning equipment, which is able to operate close to the given conditions. The performance of the novel device was tested in several measurement series with various monodisperse aerosols at ambient conditions as well as in high pressure, high temperature situations with very satisfactory results, i.e., the lower detection limit (50 % counting efficiency at ca. 0.3 μm) and resolution of the novel device are comparable to state of the art instruments (of the same principle) intended for room temperature operation.     

光外差-塞曼调制磁旋转光谱技术的线型研究

光外差－塞曼调制磁旋光谱技术是一种高灵敏的吸收光谱技术。它同时对激光频率和样品的塞曼效应进行调制,然后通过双解调来提取微弱的光谱信号。文内导出了该信号的数学表达式,并对影响线型和灵敏度的多种物理参数进行了分析,获得了与实验相符合的结果。     

Characterization of Particle Size Standard NIST 1019b with Synchrotron X‐ray Microtomography and Digital Data Extraction

We show that synchrotron x‐ray microtomography (μCT) followed by digital data extraction can be used to examine the size distribution and particle morphologies of the polydisperse (750 to 2450 μm diameter) particle size standard NIST 1019b. Our size distribution results are within errors of certified values with data collected at 19.5 μm/voxel. One of the advantages of using μCT to investigate the particles examined here is that the morphology of the glass beads can be directly examined. We use the shape metrics aspect ratio and sphericity to examine of individual standard beads morphologies as a function of spherical equivalent diameters. We find that the majority of standard beads possess near‐spherical aspect ratios and sphericities, but deviations are present at the lower end of the size range. The majority (> 98 %) of particles also possess an equant form when examined using a common measure of equidimensionality. Although the NIST 1019b standard consists of loose particles, we point out that an advantage of μCT is that coherent materials comprised of particles can be examined without disaggregation.     

A Multi‐Thresholding Algorithm for Sizing out of Focus Particles

A methodology is presented that enables efficient acquisition of sufficient droplet information (e.g. diameter and aspect ratio) from images of in and out of focus droplets. The newly developed multi‐threshold algorithm is successfully implemented in the automatic particle/droplet image analysis (PDIA) system. Under the same optical hardware set‐up, and compared to the dual threshold methods [1], the multi‐threshold method increases the measurable/acceptable depth of field (DoF) of particles, especially for the small particles of diameters less than 50 μm (1098 pixels in this optical set‐up). When testing the 70 μm~110 μm and 100 μm~200 μm moving glass spheres, the dual threshold method can only detect 11%~29 % of the particles found by the multi‐threshold method. The multi‐threshold method is also capable of generating the aspect ratios of particles more accurately than dual threshold methods.     

Two‐Dimensional Au Nanocrystals: Shape/Size Controlling Synthesis,Morphologies, and Applications

The fascinating roles of two‐dimensional (2D) nanomaterials in natural super‐strong bio‐composites (i.e. aragonite platelets in nacre and apatite platelets in bone) have aroused great interest in scientific communities to synthesize their artificial counterparts with controllable geometric and physical properties. The quantum 2D confinement of electrons recently revealed in graphene nanosheets further inspires to explore 2D metal nanocrystals with intrinsic anisotropic properties and quantum size effect. Among them, 2D Au nanocrystals stand out not only due to their unique structure‐ and environmental‐dependent properties, but also due to their rapid development in synthesis approaches and emerging applications in electronics, optics, sensing and biomedicines. In this Review the aim is to rationalize numerous newly published studies on 2D Au nanocrystals and to gain insight into their shape/size controlling synthesis, diverse morphologies, properties, and applications, potentially serving a handy guide to achieve on‐demand 2D Au nanocrystals.     

On‐chip stimulated Brillouin Scattering for microwave signal processing and generation

Demonstration of continuously tunable delay, low‐noise lasers, dynamically controlled gratings, and optical phase shifting using the stimulated Brillouin scattering (SBS) process has lead to the emergence of SBS as a promising technology for microwave photonics. On‐chip realization of SBS enables photonic integration of microwave photonic signal processing and offers significantly enhanced performance and improved efficiency. On‐chip stimulated Brillouin scattering is reviewed in the context of slow‐light based tunable delay, low‐noise narrow linewidth lasers and filtering for integrated microwave photonics. A discussion on key material and device properties, necessary to enable on‐chip Brillouin scattering using both the single‐pass and resonator geometry, is presented along with an outlook for photonic integration of microwave signal processing and generation in other platforms.     

On‐chip THz spectrometer for bunch compression fingerprinting at fourth‐generation light sources

The layout of an integrated millimetre‐scale on‐chip THz spectrometer is presented and its peformance demonstrated. The device is based on eight Schottky‐diode detectors which are combined with narrowband THz antennas, thereby enabling the simultaneous detection of eight frequencies in the THz range on one chip. The size of the active detector area matches the focal spot size of superradiant THz radiation utilized in bunch compression monitors of modern linear electron accelerators. The 3 dB bandwidth of the on‐chip Schottky‐diode detectors is less than 10% of the center frequency and allows pulse‐resolved detection at up to 5 GHz repetition rates. The performance of a first prototype device is demonstrated at a repetition rate of 100 kHz at the quasi‐cw SRF linear accelerator ELBE operated with electron bunch charges between a few pC and 100 pC.     

Tunable On‐Chip Sources with Aperiodic Metasurface

Surface plasmons show tremendous capability in integrated communication, quantum computing and sensing. Excitations and manipulations of surface plasmons are essential in developing integrated photonic devices. Here, a systematic study of tunable emission of surface plasmons with an eightfold quasicrystal metasurface, which acts as an on‐chip source, is presented. It is shown that the quasicrystal structure can switch on or off the surface plasmons propagation channels in the desired direction. Meanwhile, such a quasicrystal structure can be polarization‐dependent or polarization‐independent based on different constituent slit pairs. The proposed quasicrystal design provides more freedom for steering surface plasmons in the launching process. Thus, it may significantly simplify the design and fabrication of integrated plasmonic devices.     

On Modeling of the Spectral Line Shape of Heavy Neutral Nonhydrogen-Like Emitters

A method of simulating the contour of the asymmetric spectral lines of neutral nonhydrogen-like atoms in a plasma is suggested. The methods of nonlinear regression are used to approximate the experimental data by a model function. The method has been checked on the spectral lines emitted by the electric arc stabilized by the walls. The method makes it possible to evaluate the Stark parameters directly from the experimentally obtained shapes of isolated or overlapping spectral lines.     

Characterization of Nano‐Particles Using Laser‐Induced Incandescence

Laser‐induced incandescence (LII) is introduced as a valuable tool for the characterization of nanoparticles. This optical measurement technique is based on the heating of the particles by a short laser pulse and the subsequent detection of the thermal radiation. It has been applied successfully for the investigation of soot in different fields of application, which is described here in the form of an overview with a focus on work done at the LTT‐Erlangen during the last 10 years. In laboratory flames the soot primary particle size, volume concentration, and relative aggregate size have been determined in combination with the number density of primary particles. Furthermore, the primary particle sizes of carbon blacks have been measured in situ and online under laboratory conditions and also in production reactors. Measurements with different types of commercially available carbon black powders, which were dispersed in a measurement chamber yielded a good correlation between LII results and the specified product properties. Particle diameters determined by LII in a furnace black reactor correlate very well with the CTAB‐absorption number, which is a measure for the specific surface area. It turned out that the LII method is not affected by variations of the aggregate structure of the investigated carbon blacks. The LII signal also contains information on the primary particle size distribution, which can be reconstructed by the evaluation of the signal decay time at, at least, two different time intervals. Additionally, soot mass concentrations have been determined inside diesel engines and online measurements were performed in the exhaust gas of such engines for various engine conditions simultaneously providing information about primary particle size, soot volume, and number concentration. The LII results exhibit good correlation with traditional measurement techniques, e.g., filter smoke number measurements. In addition to the soot measurements, primarily tests with other nanoparticles like TiO₂ or metal particles are encouraging regarding the applicability of the technique for the characterization of such different types of nanoparticles.