Sedimentation Image Analysis (SIA) for the Simultaneous Determination of Particle Mass Density and Particle Size

A new method for the simultaneous determination of the distribution of particle mass density and the distribution of particle size with a technique with only a single measurement is presented. The basic idea of the new optical method is the analysis of gravitational particle settling by a digital image acquisition system. Individual particles illuminated by a laser light sheet are tracked by a continuously operating CCD camera. The projected area, shape factors and the centre of gravity are detected during the sedimentation process from a series of images with a constant time spread. As the algorithm is based on single particle tracking, the heterogeneity of the sample can be taken into account. From these measured particle characteristics, particle size and settling rate are calculated. Thus particle mass density is obtained taking into account also the influence of particle shape on the settling process. This method, which we name sedimentation image analysis (SIA), is particularly suitable for the characterization of heterogeneous material, e.g. soil, in the micrometer range.     

On-line Determination of Particle Size Distribution during the manufacture of compound feed

Experimental investigations were carried out with mainly a Mogensen-Sizer, compared with test screening and additionally laser diffraction and light extinction, in order to check the qualification for on-line determination of particle size distribution under the specific conditions of feed milling. The different components of compound feed, the degree of milling, the difference in measured particle characteristics and the possibility of sample dispersion affect the comparability of the results. The results show that laser diffraction is a manysided method with accurate recording of the distribution. The modified Mogensen-Sizer can be a robust low-price alternative if the control of selected distribution parameters is sufficient.     

Determination of the Refractive Index of Water‐dispersible Granules for Use in Laser Diffraction Experiments

Modern laser light scattering equipment can cover a very broad particle size range by using complex algorithms, such as the Mie theory. A disadvantage of this theory, however, is that it requires the knowledge of the refractive index of the particles, which is not straightforward for powdered organic substances. In this study, thiram, a common dithiocarbamate fungicide, was used as a model compound. In a first part, a method was elaborated to determine the refractive index, based on refractive index measurements of solutions of the compound of interest in a range of solvents. Two different extrapolation techniques were compared. Both techniques were validated by applying them to the determination of the refractive indices of poly(vinyl acetate) and poly(methyl methacrylate). Secondly, the influence of the refractive index value on the generated particle size distribution in the laser diffraction software was investigated. It was observed that widely different particle size distributions can be generated by the laser diffraction software for a single experimental data‐set. Therefore, accurate refractive index information is required to obtain reliable particle size distribution results.     

Particle Shape Investigations with a light-scattering optical instrument

A light-scattering instrument that is normally used for particle size analysis was applied to obtain information about particle shape. Micro-cuboids of dimensions a × b × c in the range between 10 and 1000 μm, which can be accurately manufactured employing special technology, were used as labelled samples for the determination of 3-D features. Particle projections at different orientations due to turbulent motion were measured sequentially. The laser diffraction of cuboids rotating in a turbulent flow is described theoretically using a simplified model, i.e. rotation of a rectangle. The change in the projection areas of rotating cuboids is connected with their rotational velocity. The power spectrum density of rotational velocity of cuboids and spheres was determined and the influence of particle shape on the power spectrum density established. The frequency distribution of projection sizes was found to be suitable for particle shape estimation.     

Calculation of Particle Size Distributions from Ultrasonic Measurements: A Mineral Slurry Case Study

Ultrasonic transmission measurements have been used extensively to determine the particle size of solids in slurries. This case study examines the application of mathematical inversion techniques to the determination of the particle size distribution of a mineral slurry from data collected at a minerals processing plant. A new mathematical inversion technique, based on an extension of modified Chahine iteration combined with the principle of maximum entropy has been developed. Four algorithms were constructed and used to calculate particle size distributions from synthetic and raw plant data. These incorporated modified Chahine iteration and its extension, together with two different approaches to applying a density measurement constraint on the particle size distribution. In general the algorithms performed well with regression errors below 3 %. The correlation coefficients and slopes for this technique were 0.86 and 1.35 for the weight fraction of particles less than 75 microns when compared with the laser diffraction analysis. A better match was obtained for the plant data by using the new inversion technique, into which the principle of maximum entropy has been incorporated whereas this was not the case with the synthetic data, illustrating the need to match the inversion technique to the problem.     

On-Line Particle Size Analysis Using Ultrasonic Velocity Spectrometry

A new method is described for the determination of particle size distribution of slurries based on ultrasonic velocity spectrometry combined with gamma-ray transmission. This method shares the advantages of ultrasonic attenuation spectroscopy of being capable of analyzing highly concentrated samples without dilution. However the ultrasonic velocity method is better suited to fine particles of diameter from about 0.1 to 30 μm, a greater volume of slurry is analysed and therefore sampling errors are reduced, and precise theoretical models are readily available to permit the accurate determination of size distribution by inversion of ultrasonic velocity measurements. The method can also be used to accurately determine particle size cut points by linear correlation. Using either inversion or correlation methods, the accuracy of particle size information from ultrasonic velocity spectroscopy is significantly enhanced by the independent measurement of solids loading by gamma-ray transmission. In addition, larger sizes can be measured by combining the ultrasonic velocity method with ultrasonic attenuation measurements. The method has been tested in the laboratory on a wide variety of mineral and paint slurries. The method determined the size distribution of single component silica and alumina samples in water in agreement with laser diffraction measurements and the method successfully distinguished well and poorly dispersed TiO₂ suspensions. For composite samples the method discriminated separate TiO₂ and CaCO₃, components and determined their proportions to within 0.25% volume. In addition the method, in combination with ultrasonic attenuation measurements, determined the size fractions of iron ore slurries below 10 and 30 μm to within 1.3% and 1.0% relative respectively, when compared with laser diffraction measurement of particle size. The CSIRO is presently designing an industrial gauge which will be manufactured and installed in an industrial slurry stream in 1997.     

Modeling of Multiple Scattering Effects in Fraunhofer Diffraction Particle Size Analysis

A model for the direct problem of calculating the forward scattering signature of a multiple scattering medium is presented. The new formulation is optimized for integration into schemes for reconstructing the particle size distribution from laser diffraction (forward scattering) signatures obtained from optically thick media. The analysis is valid for media where the particle sizes and interparticle spacings are large (relative to the wavelength and the particle size, respectively) such that Fraunhofer diffraction theory adequately describes the properties of the forward scattered light from individual scattering events. The simulated performance of laser diffraction particle sizing instruments was then studied using predictions of the scattered light signatures which would be measured by laser diffraction instrument under multiple scattering conditions. The results were compared with experimental data and theoretical calculations based on other models.     

Determining aerosol particle size distributions using time-resolved laser-induced incandescence

The particle size distribution within an aerosol containing refractory nanoparticles can be inferred using time-resolved laser-induced incandescence (TR-LII). In this procedure, a small volume of aerosol is heated to incandescent temperatures by a short laser pulse, and the incandescence of the aerosol particles is then measured as they return to the ambient gas temperature by conduction heat transfer. Although the cooling rate of an individual particle depends on its volume-to-area ratio, recovering the particle size distribution from the observed temporal decay of the LII signal is complicated by the fact that the LII signal is due to the incandescence of all particle size classes within the sample volume, and because of this, the particle size distribution is related to the time-resolved LII signal through a mathematically ill-posed equation. This paper reviews techniques proposed in the literature for recovering particle size distributions from TR-LII data. The characteristics of this problem are then discussed in detail, with a focus on the effect of ill-posedness on the stability and uniqueness of the recovered particle size distributions. Finally, the performance of each method is evaluated and compared based on the results of a perturbation analysis. PACS  44.05.+e; 47.70.Pq; 78.70.-g; 65.80.+n; 78.20.Ci     

Shape Estimation of Anisometric Particles Using Size Measurement Techniques

This study was conducted to establish a simple method for evaluating the morphology of fine anisometric particles using size measurement techniques. The size distributions of mica particles and carbon fibers classified into narrower size ranges were measured by gravitational sedimentation and laser diffraction techniques. The ratio of mean diameters determined for flaky particles strongly depended on the aspect ratio, i.e. flatness. The relationship between particle shape and diameter is discussed theoretically. The experimental results were similar to those predicted. The flatness of fine particles can be evaluated by the ratio of the median diameter determined by laser diffraction to that determined by sedimentation.     

Aqueous Droplet Sizing by Inertial Classification

The particle size distribution of an aerosol generated from an aqueous system is difficult to analyse because of the shrinkage of the droplets due to solvent evaporation. These problems are very important for the characterization of medical nebulizers, since most of the drugs delivered via inhalation are water soluble. In situ methods for droplet size analysis, such as laser diffraction, phase Doppler anemometry and light scattering, do not determine either the initial or the equilibrium size distribution. With the residual technique, which means evaporating the droplets and measuring the size and concentration of the residuals, the instability of the aqueous droplets plays no role and the necessary radioactive labelling of the sprayed material allows a direct determination of the mass flow rate at the mouthpiece of the nebulizer. In this way it is possible to discriminate between the delivered drug solution and the water necessary to humidify the incoming air. The output of nebulizers of different designs is given for various operating conditions, filling volumes and solution concentrations. The measured droplet size distribution of a nebulizer is found to be fixed mainly by its internal impaction system.     

Particle size analysis: A comparison of various methods ii

In previous work, the relative performance of various methods used to characterize the particle size distribution of powders composed of fine irregularly shaped particles was assessed. It was found that methods employing Fraunhofer diffraction theory were inferior with respect to particle counting methods. Furthermore, calculated particle size distributions varied considerably between manufactures of Fraunhofer devices. It is well known that the Mie optical model can also be used to analyze the data collected by laser diffraction instruments. Here, we have compared particle size distributions collected using two Laser diffraction instruments to those determined by the Aerosizer. In our earlier work the Aerosizer was shown to produce results nearly identical to those determined by image analysis. The results of this study indicate that the use of the Mie optical model does not correct for deficiencies previously noted for laser diffraction methods. Considerable variation exists between the results obtained on laser diffraction instruments manufactured by different companies. Our earlier recommendation to use extreme caution when employing laser diffraction instruments to characterize fine powders continues to be supported in the present work.     

Multi-lognormal soot particle size distribution for time-resolved laser induced incandescence in diesel engines

In-cylinder and exhaust soot particle size measurements were carried out using time-resolved laser induced incandescence and electrical mobility spectrometer techniques in a single cylinder optical diesel engine and multi-cylinder high-speed diesel engine. The temporal decay of the laser induced incandescence signal from a polydisperse nanoparticle ensemble of soot during transient diesel combustion is shown to be described by both a single-lognormal distribution as well as multi-lognormal size distribution. However, a multi-lognormal particle size distribution is introduced in the existing model for a comprehensive characterisation and realistic reconstruction of the size distribution. Detailed theoretical analysis of multi-lognormal size distribution along with its application to the experimentally measured soot particle size is validated in this work. These results were also qualitatively compared and independently verified by the experimental results obtained by the electrical mobility spectrometer and published transmission electron microscopy data. These findings reveal that the in-cylinder and the exhaust soot particle size distributions in engines are better represented by a multi-lognormal size distribution.     

Quick Optical Measurement of Particle Distribution in a Sedimentation Apparatus

The determination of the particle size distribution of a powder may last up to 14 hours with standard sedimentation techniques such as an Andreasen pipette. If, in a photosedimentometer, not only the one sensor close to the bottom is incorporated but a number of sensors positioned at different heights, the time required for determining the particle size distribution of a powder may be reduced to 15 minutes. For each sensor there is an optimum location, which is determined both by the distance from the surface to the lowest and the highest sensor and by the number of sensors. The instrument, equipped with three measuring sensors and a reference sensor is connected to a personal computer. The measured particle size distributions are reproducable with a standard deviation of less than 2%. Agreement with a Sedigraph or a sedimentation balance is about the same as the agreement of these two instruments with each other. The time required for the determination of a particle size distribution of a quartz powder suspended in water with particle diameters from 1.5 to 60 μ is 15 minutes.     

激光诱导煤粉等离子体的特性研究

本文研究了煤粉形态对于激光诱导煤粉等离子体特性的影响,以指导应用激光感生击穿光谱进行煤质测量时最佳样品形态的选择.建立了一套激光诱导击穿光谱的实验台架,对同一煤种的4个不同粒径范围的粉状样品进行激光激发与光谱分析,利用钙原子不同跃迁能级发射谱线的强度分布计算了0.3～0.5μs区间内的等离子体温度,并依据谱线Stark展宽与电子密度的关系得到了等离子体的电子密度.再对激发不同粒径煤粉样品产生的等离子体温度与电子密度进行了对比.实验证明,煤粉粒径越小,等离子体温度越高且电子密度越大,也即样品的等离子化程度越高,越有利于煤中元素的定量分析.     

Constraints of two-colour TiRe-LII at elevated pressures

The main objective of this work is to investigate the influence of high-pressure conditions on the determination of primary particle size distributions of laser-heated soot particles using pyrometrically determined temperature decays. The method is based on time-resolved laser-induced incandescence measurements carried out at two different wavelengths (two-colour TiRe-LII). The LII signals are transferred into a particle ensemble averaged (effective) temperature using Planck’s thermal radiation formula. Assuming that all particles within the size distribution possess a unique temperature at the end of the laser pulse, the size distribution can be determined by numerically simulating the measured temperature decay. From our investigations, for pressures up to a few bars it is obvious that this strategy can be successfully applied if standard laser pulses of nano-second duration are used as an LII-excitation source. At higher pressures the time scales of heat conduction are decreased to such an extent that a unique temperature for all particles within the ensemble cannot be assumed at the end of the nano-second laser pulse. However, further investigations show that the presented two-colour TiRe-LII technique can be successfully adopted under technical high-pressure conditions as well, if the pulse duration of the TiRe-LII-excitation source is reduced into the pico-second range.     

Laser Diffraction – Unlimited?

Within the past 20 years, particle size analysis with laser diffraction (LD) has been subject to rapid development, extending the size range stepwise from 1–200 μm to about 0.1–3500 μm. The limits of LD are discussed in terms of light sources, the influence of the beam diameter, special Fourier optics and a new detector design. It is shown that the size range is not only restricted by the wavelength of the laser and the transmission limits of the medium. Its extension is mainly related to improvements in the measurement of the angular intensity distribution. Influences from stability and flow dominate on the coarse side of the measuring range. On the fine side, the spatial extension of aerosols and the resulting demand for extended working distances can be covered only in a parallel laser beam. Extended Fourier optics in combination with an adapatable beam expansion technique and a detector with virtual borders between semicircular elements overcome the existing limits and extend the size range to a lower limit of about 0.05 μm and an upper limit above 10 mm. The sensititivity limit of LD is approaching that of single particle counting techniques. For medical spray and inhaler applications, a 0.1% optical concentration can be converted to particle size distributions even for time-resolved analyses with sample intervals of a few milliseconds. The reproducibility of the sensor, with a standard deviation typically much less than 0.5%, is no longer the limiting factor. The reproducibility of the results is mainly dominated by the reproducibility of sampling, sample splitting, dispersion and the contamination of the optical path. The latter can be improved by the control of flow, especially for in-line and inhaler applications.     

Development of Agglomerate Size and Structure during spherical agglomeration in suspension

During the spherical agglomeration process, a suspended solid is agglomerated by adding a binding liquid. First, mircoagglomerates or flocs are produced, which are compacted in the course of the process. Agglomerate size was evaluated by laser diffraction spectrometry, image analysis was used to determine the size and some adequately defined shape parameters calculated by Fourier analysis of the particle contour. The shape analysis confirms the visual observations; the compaction of the flocs is expressed by the corresponding change of the shape parameters. The influence of several process parameters on changes in agglomerate shape can be described quantitatively and help to gain an insight into agglomeration mechanisms. The particle size distributions determined by image analysis and laser diffraction spectrometry hardly differ for fairly spherical flocs or agglomerates. Concerning the size distribution of the irregular flocs, laser diffraction spectrometry measures larger particles than image analysis.     

Characterisation of the acoustic cavitation cloud by two laser techniques

An experimental investigation of the size and volumetric concentration of acoustic cavitation bubbles is presented. The cavitation bubble cloud is generated at 20 kHz by an immersed horn in a rectangular glass vessel containing bi-distilled water. Two laser techniques, laser diffraction and phase Doppler interferometry, are implemented and compared. These two techniques are based on different measuring principles. The laser diffraction technique analyses the light pattern scattered by the bubbles along a line-of-sight of the experimental vessel (spatial average). The phase Doppler technique is based on the analysis of the light scattered from single bubbles passing through a set of interference fringes formed by the intersection of two laser beams: bubble size and velocity distributions are extracted from a great number of single-bubble events (local and temporal average) but only size distributions are discussed here. Difficulties arising in the application of the laser diffraction technique are discussed: in particular, the fact that the acoustic wave disturbs the light scattering patterns even when there are no cavitation bubbles along the measurement volume. As a consequence, a procedure has been developed to correct the raw data in order to get a significant bubble size distribution. After this data treatment has been applied the results from the two measurement techniques show good agreement. Under the emitter surface, the Sauter mean diameter D(3, 2) is approximately 10 microm by phase Doppler measurement and 7.5 microm by laser diffraction measurement at 179 W. Note that the mean measured diameter is much smaller than the resonance diameter predicted by the linear theory (about 280 microm). The influence of the acoustic power is investigated. Axial and radial profiles of mean bubble diameters and void fraction are also presented.     

等离子体光谱/质谱中悬浮液进样研究进展

等离子体光谱/质谱法是无机元素分析主要的分析方法之一,但其通常要求以溶液形式进样。文章在介绍目前几种固体试样直接进样方法的基础上,着重对悬浮液进样等离子体光谱/质谱研究进展进行综述。叙述悬浮液的制备方法及表征,包括球磨法、混合研磨、振动球磨、超声研磨等降低颗粒的方法。通过分散剂、pH调节等方法分散和稳定悬浮液,并就其关系进行阐述。叙述粒度大小分布测量的几种方法：沉降法、光学显微镜法、光透沉降式粒度仪法、激光散射法、扫描或透射电镜法等。讨论悬浮液浓度影响以及校准方法技术：简单水溶液标准校准法、内标法、经验校正系数法、标准加入法、本征内标法、标准悬浮液法。综述了悬浮液进样的有关基础研究和近年悬浮液进样等离子体光谱/质谱分析应用。