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Lactose is of great industrial importance and its production includes the cooling crystallization from highly concentrated solutions. Monitoring the crystallization process is essential to ensure reproducible product quality. Photon density wave (PDW) spectroscopy enables in-line monitoring of highly concentrated processes in liquid dispersions. It was applied to the determination of the solubility and nucleation points of lactose monohydrate in water, sizing of lactose crystals, and to dissolution as well as crystallization monitoring. Other process analytical technologies (focused-beam reflectance measurement, particle vision and measurement) were used as reference, and the comparison indicates that PDW spectroscopy is very robust against probe fouling and is, thus, a useful tool for monitoring crystallization processes in concentrated suspensions.
The formation process of zeolite A (Linde Type A) was monitored inline at 1.5 L scale by Photon Density Wave (PDW) spectroscopy as novel process analytical technology for highly turbid liquid suspensions. As a result, the reduced scattering coefficient, being a measure for particle number, size, and morphology, provides distinct process information, including the formation of amorphous particles and their transfer into crystalline zeolite structures. The onset and end of the crystallization process can be detected inline and in real-time. Analyses by powder X-ray diffraction and electron microscopy, based on a sampling approach, support the interpretation of the results obtained by PDW spectroscopy. In addition, the influence of the molar water content was investigated, indicating a linear increase of the time needed to reach the end of the zeolite A crystallization with increasing molar water content. Further experiments indicate a strong influence of the silica source on the course of the crystallization. The applicability of PDW spectroscopy under even more demanding chemical and physical conditions was investigated by monitoring the synthesis of zeolite L (Linde Type L).
Photon Density Wave (PDW) spectroscopy is presented as a fascinating technology for the independent determination of scattering (mu(s)’ and absorption (ita) properties of highly turbid liquid dispersions. The theory is reviewed introducing new expressions for the PDW coefficients k(I) and k(Phi). Furthermore, two models for dependent scattering, namely the hard sphere model in the Percus-Yevick Approximation (HSPYA) and the Yukawa model in the Mean Spherical Approximation (YMSA), are experimentally examined. On the basis of the HSPYA particle sizing is feasible in dispersions of high ionic strength. It is furthermore shown that in dialyzed dispersions or in technical copolymers with high particle charge only the YMSA allows for correct dilution-free particle sizing. (C) 2013 Elsevier Ltd. All rights reserved.
Depletion-induced flocculation of concentrated emulsions probed by photon density wave spectroscopy
(2020)
Stable, creaming-free oil in water emulsions with high volume fractions of oil (phi = 0.05-0.40, density matched to water) and polysorbate 80 as an emulsifier were characterized without dilution by Photon Density Wave spectroscopy measuring light absorption and scattering behavior, the latter serving as the basis for droplet size distribution analysis. The emulsion with phi = 0.10 was used to investigate flocculation processes induced by xanthan as a semi-flexible linear nonabsorbing polymer. Different time regimes in the development of the reduced scattering coefficient mu(s)' could be identified. First, a rapid, temperature-dependent change in mu(s)' during the depletion process was observed. Second, the further decrease of mu(s)' follows a power law in analogy to a spinodal demixing behavior, as described by the Cahn-Hilliard theory.
Quality attributes of fruit determine its acceptability by the retailer and consumer. The objective of this work was to investigate the potential of absorption (μa) and reduced scattering (μs’) coefficients of European pear to analyze its fruit flesh firmness and soluble solids content (SSC). The absolute reference values, μa* (cm−1) and μs’* (cm−1), of pear were invasively measured, employing multi-spectral photon density wave (PDW) spectroscopy at preselected wavelengths of 515, 690, and 940 nm considering two batches of unripe and overripe fruit. On eight measuring dates during fruit development, μa and μs’ were analyzed non-destructively by means of laser light backscattering imaging (LLBI) at similar wavelengths of 532, 660, and 830 nm by means of fitting according to Farrell’s diffusion theory, using fix reference values of either μa* or μs’*. Both, the μa* and the μa as well as μs’* and μs’ showed similar trends. Considering the non-destructively measured data during fruit development, μa at 660 nm decreased 91 till 141 days after full bloom (dafb) from 1.49 cm−1 to 0.74 cm−1 due to chlorophyll degradation. At 830 nm, μa only slightly decreased from 0.41 cm−1 to 0.35 cm−1. The μs’ at all wavelengths revealed a decreasing trend as the fruit developed. The difference measured at 532 nm was most pronounced decreasing from 24 cm−1 to 10 cm−1, while at 660 nm and 830 nm values decreased from 15 cm−1 to 13 cm−1 and from 10 cm−1 to 8 cm−1, respectively. When building calibration models with partial least-squares regression analysis on the optical properties for non-destructive analysis of the fruit SSC, μa at 532 nm and 830 nm resulted in a correlation coefficient of R = 0.66, however, showing high measuring uncertainty. The combination of all three wavelengths gave an enhanced, encouraging R = 0.89 for firmness analysis using μs’ in the freshly picked fruit.