Chord length characterization using focused beam reflectance measurement probe - methodologies and pitfalls

The impact of the solid concentration and refractive index of dispersing medium on the FBRM measurement of chord length and particle counts were investigated using the PVC (polyvinylchloride) particle systems. It was found that the chord length increased with the solid concentration in the diluted region, but decreased as the concentration became greater than 1.1%. The total particle counts were found to increase initially with the solid concentration, tapering off at high concentrations. The measured counts of small chords (1 μm-50 μm) were found to increase linearly with the solid concentration, those of the large chords increased with the concentration initially and leveled off (50 μm-200 μm) or decreased (200 μm-500 μm) with further increase of concentration. The impact of the refractive index of the dispersing medium on the FBRM measurement was also investigated, the result of which was corroborated by microscopy studies. Comparison between the FBRM and other sizing techniques revealed that when appropriate weighting factors were applied, good agreement could be achieved between the median average values of the chord length and particle size distributions.     

Effect of solvent type on preparation of ethyl cellulose microparticles by solvent evaporation method with double emulsion system using focused beam reflectance measurement

The purpose of this study was to investigate the effect of solvent type on the solidification rate of ethyl cellulose (EC) microparticles and particle size/distribution of emulsion droplets/hardened microparticles during the solvent evaporation process using focused beam reflectance measurement (FBRM). EC microparticles were prepared with a water‐in‐oil‐in‐water solvent evaporation method using various solvents, including dichloromethane, dichloromethane–methanol (1:1), ethyl acetate and chloroform. The particle size/distribution of the emulsion droplets/hardened microparticles was monitored using FBRM. The morphology of EC microparticles was characterized using scanning electron microscopy (SEM). The transformation of the emulsion droplets into solid microparticles for all solvents occurred within the first 10–90 min. The square weighted mean chord length of EC microparticles prepared using chloroform was smallest, but the chord count was not the highest. The chord length distribution (CLD) measured by FBRM showed that a larger mean particle size gave longer CLD and a lower peak of particle number. SEM data revealed that the morphology of microparticles was influenced by the type of solvent. FBRM can be employed for online monitoring of the shift in the microparticle CLD and detect transformation of emulsion droplets into solid microparticles during the solvent evaporation process. The microparticle CLD and transformation process were strongly influenced by solvent type. © 2017 Society of Chemical Industry     

Estimation of particle size distributions from focused beam reflectance measurements based on an optical model

A popular in situ particle characterization technique, which can be applied without dilution, is the focused beam reflectance measurement (FBRM^®). The FBRM probe measures a chord length distribution (CLD) which is different from a particle size distribution (PSD). In order to compare results obtained by an FBRM probe with other measurement technologies such as laser diffraction, it is necessary to reconstruct the PSD from a measured CLD. For this reconstruction a measurement model and an inversion procedure are required. Most FBRM models presented in the literature assume that an FBRM records a geometric chord which can be deduced from a two-dimensional projection of the particle silhouette. In previous work [Kail, N., Briesen, H., Marquardt, W., 2008. Analysis of FBRM measurements by means of a 3D optical model. Powder Technology 185 (3), 211-222] it has been demonstrated that FBRM data show significant deviations from this geometric model. Consequently, an estimation of a PSD using such a geometric FBRM model will fail. A novel FBRM model is developed in this work. This model imitates the chord discrimination algorithm used in a Lasentec D600L FBRM system and takes the intensity profile of the laser beam and the optical aperture of the probe into account. The model is ideally suited for the estimation of a PSD from a measured CLD using a sequential, linear inversion routine, as proposed in this work. The novel FBRM model and the inversion procedure are evaluated using small, mono-disperse polystyrene beads, large ion-exchanger beads, and α-lactose-monohydrate particles. The applicability of the FBRM for PSD measurements is discussed on the basis of these results.     

Modelling particle disruption of an organic fine chemical compound using Lasentec focussed beam reflectance monitoring (FBRM) in agitated suspensions

The focussed beam reflectance monitoring (FBRM) instrument developed by Lasentec is a ‘powerful’ tool used as an ‘in-situ’ particle monitoring technique for in-line real-time measurement of particle size. This technique was successfully used to monitor particulate attrition and breakage of an organic fine chemical in a turbulently agitated suspension. The great advantage of using the FBRM technique is that the change in the crystal size distribution (CSD) for different particle size classes (fine, intermediate and coarse) can be monitored as a function of time. The attrition rates can be calculated to produce a model for the disruption kernel for the organic compound. The shift in the CSD that was observed with an increase in the specific power input was found to be largely due to micro-attrition effects rather than particle breakage (splitting).     

乙醇连续发酵过程中自絮凝酵母颗粒粒径分布的模拟

以酿酒酵母和粟酒裂殖酵母的融合株——自絮凝颗粒酵母SPSC01为研究对象,选择搅拌式反应器为模式系统,利用聚焦光束反射测量仪（FBRM）在线检测了絮凝酵母颗粒的弦长频率分布.研究表明,在含有絮凝缓冲液的模拟系统中,自絮凝酵母颗粒粒径分布符合对数正态分布.粒径分布的特征参数（M）与搅拌转速（r）之间的关系可用对数方程表示,从而简化了絮凝酵母颗粒粒径分布的定量表征.在真实的乙醇连续发酵过程中,细胞代谢生成的CO₂对测量体系产生了干扰,利用建立的自絮凝酵母颗粒粒径分布的在线检测和定量表征方法,在数据处理过程中排除了这种干扰,得到了自絮凝酵母SPSC01絮凝颗粒的粒径分布.     

Measuring the particle size of a known distribution using the focused beam reflectance measurement technique

The accuracy of the focused beam reflectance measurement (FBRM) probe, which measures a chord length distribution, from Mettler-Toledo Lasentec^® has been explored. A particle video microscope (PVM) probe, which provides in situ digital images, was used as a direct visual method to test the reliability of the FBRM results. These probes can provide in situ particle characterization at high pressures. The FBRM has been used to study emulsions and ice and clathrate hydrate formation. The ability of the FBRM to accurately characterize unimodal and bimodal distributions of particles and droplets and to measure agglomeration events was investigated. It was found that while the FBRM can successfully identify system changes, certain inaccuracies exist in the chord length distributions. Particularly, the FBRM was found to oversize unimodal distributions of glass beads, but undersize droplets in an emulsion and was unable to measure full agglomerate sizes. The onset of ice and hydrate nucleation and growth were successfully detected by the FBRM, but quantitative analysis of the particle and agglomerate sizes required simultaneous PVM measurements to be performed.     

L-缬氨酸对Streptomyces natalensis HW-2合成纳他霉素的影响

以Streptomyces natalensis HW-2为研究对象,考察了添加L-缬氨酸对纳他霉素生物合成途径的影响。结果表明:在纳他霉素发酵至36 h时添加0.5 g/L L-缬氨酸,纳他霉素产量达到1.83 g/L,比对照组提高了84.85%。添加L-缬氨酸后引起菌体生物量降低和pH升高,而葡萄糖利用速率加快;胞内丙酮酸激酶(PK)、磷酸烯醇式丙酮酸羧化酶(PEPC)和丙酮酸羧化酶(PC)活性增强,柠檬酸合酶(CS)活力降低了26.57%;发酵液中丙酮酸(色谱法)、草酰乙酸(色谱法)和乙酰辅酶A(分光光度法)的含量分别提高了80.50%、53.28%和47.19%,乙酸(色谱法)、丙酸(色谱法)和α-酮戊二酸(色谱法)的含量分别提高了16.98%、10.65%和15.40%,而柠檬酸(色谱法)的含量降低了27.01%。     

On‐line monitoring of chord distributions in liquid–liquid dispersions and suspension polymerizations by using the focused beam reflectance measurement technique

The on‐line monitoring of the droplet/particle size distributions is very important to ensure the quality and applicability of various products in heterogeneous systems. For this reason, the main objective of the present work was to study the usage of the focused beam reflectance measurement (FBRM) technique for monitoring of liquid–liquid dispersions (styrene dispersion in aqueous solutions) and suspension polymerization of styrene. To do better understand the FBRM technique in these systems, the effects of surfactant concentrations, agitation speed and ambient light were evaluated during the in‐line monitoring of average chord lengths and chord‐length distributions (CLD) at different operation conditions in batch experiments. In addition, a preliminary investigation of the optimal probe position was conducted in the polymerization experiments. It is shown that the FBRM technique is sensitive to variations of particle sizes in the characteristic ranges of particle diameters of typical styrene suspension polymerizations, being useful for monitoring and also control applications that require the on‐line characterization of CLD in real time in liquid–liquid dispersions and polymerization systems. POLYM. ENG. SCI., 56:309–318, 2016. © 2015 Society of Plastics Engineers     

Comparison of dielectric constant meter with turbidity meter and focused beam reflectance measurement for metastable zone width determination

This work demonstrates a detailed process analytical technology (PAT) comparison study of dielectric constant measurement with turbidity measurement and focused beam reflectance measurement (FBRM) in detecting phase transitions during crystallization of three model solutions, namely stearic acid–ethyl acetate, paracetamol–ethanol and carbamazepine–methanol. The cloud and clear points determined by the dielectric constant measurement are found to be in close agreement with those obtained from the other two well-established PAT tools. A calibration technique can be further applied on the dielectric constant to improve the accuracy of the cloud point detection. The results have shown that the dielectric constant meter can be reliably used for metastable zone width (MZW) determination. This study opens new opportunities for the use of the dielectric constant meter as a simple and inexpensive alternative PAT tool for process monitoring of solution crystallization.     

3D reconstruction of SOFC anodes using a focused ion beam lift-out technique

Improvements to electrode performance are essential to accelerate the commercialisation of SOFC technology. A key metric of performance for SOFC electrodes is the length and distribution of three or triple phase boundaries (TPBs) which provide an indication of electrochemical performance. Techniques that can be used to characterise TPB length are highly valuable; with an increasing knowledge of electrode microstructures, electrochemical performance can be optimised. One such technique for electrode characterisation uses focused ion beams (FIB) to sequentially mill and image an electrode surface, obtaining a sequence of 2D images that may be reconstructed in a 3D space. In this paper we present a technique to maximise the quality of the raw data obtained via ex-situ characterisation of electrode micro-sections based on FIB lift-out. With improved raw data, we have been able to conduct semi-automated image analysis to extract key microstructural information, including the length and distribution of TPBs.Reconstructions have been carried out using both single and dual beam instruments; two reconstructions of Ni-YSZ anode structures are presented here.     

Image‐based spectral reflectance reconstruction using the matrix R method

The ultimate goal of spectral imaging is to achieve high spectral accuracy, so that the spectral information can be used to calculate colorimetrically accurate images for any combination of illuminant and observer. A new spectral reconstruction method, called the matrix R method, was developed to reconstruct spectral reflectance factor accurately while simultaneously achieving high colorimetric performance for a defined illuminant and observer. The method combines the benefits of both colorimetric and spectral transformations. Tristimulus values were predicted by a colorimetric transformation from multi‐channel camera signals, while spectral reflectance factor was estimated by a spectral transformation from the same signals. The method reconstructed reflectance factor by combining the fundamental stimulus from the predicted tristimulus values with the metameric black from the estimated spectral reflectance, based on the Wyszecki hypothesis. The experimental results verified the new method as a promising technique for building a spectral image database. © 2007 Wiley Periodicals, Inc. Col Res Appl, 32, 343–351, 2007     

响应面法优化从丝状真菌中制取壳聚糖的研究

以黑根霉、黑曲霉作为原料,研究了制备壳聚糖的方法。通过液体发酵获得黑根霉、黑曲霉的菌丝体,经干燥研磨后,比较稀酸稀碱热处理及微波法处理制备壳聚糖的提取效果及产率,并对微波法进行响应面的优化实验。结果表明：微波法较稀酸稀碱法提取效果好,产率高。优化结果：微波火力为480 W,消解时间为15 min,碱浓度为20％。     

Direct observation of CD4 T cell morphologies and their cross-sectional traction force derivation on quartz nanopillar substrates using focused ion beam technique

Direct observations of the primary mouse CD4 T cell morphologies, e.g., cell adhesion and cell spreading by culturing CD4 T cells in a short period of incubation (e.g., 20 min) on streptavidin-functionalized quartz nanopillar arrays (QNPA) using a high-content scanning electron microscopy method were reported. Furthermore, we first demonstrated cross-sectional cell traction force distribution of surface-bound CD4 T cells on QNPA substrates by culturing the cells on top of the QNPA and further analysis in deflection of underlying QNPA via focused ion beam-assisted technique.     

Preparation of bismuth nanowire encased in quartz template for Hall measurements using focused ion beam processing

ABSTRACT: Forming electrodes on opposite sides of an individual bismuth nanowire was attempted to prepare for Hall measurements. Although a 1-mm-long bismuth nanowire which is completely covered with a quartz template has been successfully fabricated to prevent oxidation, it is very difficult to attach Hall electrodes on the opposite sides of the nanowire due to the quartz covering. One side of the cylindrical quartz template was removed by polishing without exposure of the nanowire to the atmosphere; the thickness between the polished template surface and the nanowire was estimated to be several micrometers. Focused ion beam processing was successfully employed to expose both surfaces of the nanowire under high vacuum by removing part of the quartz template. A carbon thin film was then deposited in situ on the wire surface to fabricate an electrical contact on the bismuth nanowire sample. Furthermore, the energy dispersive X-ray analysis was performed to the area processed by focused ion beam, and the bismuth component of the nanowire was successfully detected. It was confirmed that the focused ion beam processing was applicable to attach electrodes to bismuth nanowire for Hall measurement.     

Experimental simulation of large-scale bioreaetor environments using a Monte Carlo method

Cells grown in production-scale stirred bioreactors experience fluctuating concentrations due to local variations in supply and consumption of oxygen and nutrients. A new method for studying the effects of fluctuations in local conditions on growth and productivity of cells was developed using a Monte Carlo approach to simulate circulation within a fermenter. A small fermenter was driven through cycles of aeration and feeding, with the time of each cycle controlled by a Monte Carlo method to give a log-normal distribution. Experiments with Monte Carlo supply of air to batch and fed-batch cultures of Saccharomyces cerevisiae showed that the method gave reproducible results which were different from both periodic cycling and continuous supply. When substrate was provided to a fed-batch culture of S. cerevisiae according to the Monte Carlo method, the yields of biomass were higher than experiments with continuous feeding or periodic feeding.     

Comparison of external bulk video imaging with focused beam reflectance measurement and ultra-violet visible spectroscopy for metastable zone identification in food and pharmaceutical crystallization processes

The purpose of the paper is twofold: it describes the proof of concept of the newly introduced bulk video imaging (BVI) method and it presents the comparison with existing process analytical technologies (PAT) such as focused beam reflectance measurement (FBRM) and ultra-violet visible (UV/vis) spectroscopy. While the latter two sample the system in small volumes closely to the probe, the BVI approach monitors the entire or large parts of the crystallizer volume. The BVI method is proposed as a complementary noninvasive PAT tool and it is shown that it is able to detect the boundaries of the metastable zone with comparable or better performance than the FBRM and UV/vis probes.