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- Institut für Chemie (13) (remove)
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.
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.
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.
In turbid biogenic liquid material, like blood or milk, quantitative optical analysis is often strongly hindered by multiple light scattering resulting from cells, particles, or droplets. Here, optical attenuation is caused by losses due to absorption as well as scattering of light. Fiber-based Photon Density Wave (PDW) spectroscopy is a very promising method for the precise measurement of the optical properties of such materials. They are expressed as absorption and reduced scattering coefficients (mu (a) and mu (s)', respectively) and are linked to the chemical composition and physical properties of the sample. As a process analytical technology, PDW spectroscopy can sense chemical and/or physical processes within such turbid biogenic liquids, providing new scientific insight and process understanding. Here, for the first time, several bioprocesses are analyzed by PDW spectroscopy and the resulting optical coefficients are discussed with respect to established mechanistic models of the chosen processes. As model systems, enzymatic casein coagulation in milk, temperature-induced starch hydrolysis in beer mash, and oxy- as well as deoxygenation of human donor blood were investigated by PDW spectroscopy. The findings indicate that also for very complex biomaterials (i.e., not well-defined model materials like monodisperse polymer dispersions), obtained optical coefficients allow for the assessment of a structure/process relationship and thus for a new analytical access to biogenic liquid material. This is of special relevance as PDW spectroscopy data are obtained without any dilution or calibration, as often found in conventional spectroscopic approaches.
Industrial applications of photon density wave spectroscopy for in-line particle sizing [Invited]
(2013)
Optical spectroscopy in highly turbid liquid material is often restricted by simultaneous occurrence of absorption and scattering of light. Photon Density Wave (PDW) spectroscopy is one of the very few, yet widely unknown, technologies for the independent quantification of these two optical processes. Here, a concise overview about modern PDW spectroscopy is given, including all necessary equations concerning the optical description of the investigated material, dependent light scattering, particle sizing, and PDW spectroscopy itself. Additionally, it is shown how the ambiguity in particle sizing, arising from Mie theory, can be correctly solved. Due to its high temporal resolution, its applicability to highest particle concentrations, and its purely fiber-optical probe, PDW spectroscopy possesses all fundamental characteristics for optical in-line process analysis. Several application examples from the chemical industry are presented. (C) 2013 Optical Society of America
Photonic sensing in highly concentrated biotechnical processes by photon density wave spectroscopy
(2017)
Photon Density Wave (PDW) spectroscopy is introduced as a new approach for photonic sensing in highly concentrated biotechnical processes. It independently quantifies the absorption and reduced scattering coefficient calibration-free and as a function of time, thus describing the optical properties in the vis/NIR range of the biomaterial during their processing. As examples of industrial relevance, enzymatic milk coagulation, beer mashing, and algae cultivation in photo bioreactors are discussed.
Most investigations on phase inversion (PI) of resins upon addition of water have been carried out by dynamic light scattering (DLS), torque, and viscosity measurements. The main problem, however, is analytic discontinuity due to sample removal and a changing matrix due to dilution during the preparation of the aqueous resin dispersions. This work presents Photon Density Wave (PDW) spectroscopy as a tool for the inline characterization of the acetone process for an acrylic copolymer with high acrylic acid (AA) content. PDW spectroscopy revealed different trends for optical properties compared to torque during water feed. Also the absence of PI due to dissolution of copolymer in the solvent/water mixture is observed by PDW spectroscopy. PI for the investigated copolymer did not occour during water feed but during removal of solvent. Different feeding rates of water gave similar trends while a change in temperature and degree of AA neutralization led to changes in optical properties and torque. Thermal processing showed that the optical properties of mixtures prior and after removal of solvent were completely different caused by changes of solubility.
A simple, convenient, and inexpensive method to fabricate optical fiber based biosensors which utilize periodic hole arrays in gold films for signal transduction is reported. The process of hole array formation mainly relies on self-assembly of hydrogel microgels in combination with chemical gold film deposition and subsequent transfer of the perforated film onto an optical fiber tip. In the fabrication process solely chemical wet lab techniques are used, avoiding cost-intensive instrumentation or clean room facilities. The presented method for preparing fiber optic plasmonic sensors provides high throughput and is perfectly suited for commercialization using batch processing. The transfer of the perforated gold film onto an optical fiber tip does not affect the sensitivity of the biosensor ((420 +/- 83) nm/refractive index unit (RIU)), which is comparable to sensitivities of sensor platforms based on periodic hole arrays in gold films prepared by significantly more complex methods. Furthermore, real-time and in-line immunoassay studies with a specially designed 3D printed flow cell are presented exploiting the presented optical fiber based biosensors.
Photon Density Wave (PDW) spectroscopy was applied for temperature dependent monitoring of melting and crystallization of milk fat within homogenized fresh milk. As an in-line process analytical technique, PDW spectroscopy quantifies continuously the optical properties of turbid material, providing an insight into its structural processes. Here, the measured absorption coefficients reflect temperature as well as fat content of milk and the reduced scattering coefficients probe physical changes of the light scattering fat droplets and casein micelles. Thermal processing reveals breakpoints within the temperature trend of the reduced scattering coefficient of fat containing milk. Found at 16 degrees C and 24 degrees C while cooling and heating, respectively, they are associated to the phase transitions of milk fat. Continuous isothermal measurement of the optical coefficients showed that the crystallization process requires several hours. The strongly changing reduced scattering coefficient implies that the thermal history of milk will have a major impact on any method based on light scattering as quantitative analytical technique.