@article{HaeneBruehwilerEckeretal.2019, author = {Haene, Janick and Bruehwiler, Dominik and Ecker, Achim and Hass, Roland}, title = {Real-time inline monitoring of zeolite synthesis by Photon Density Wave spectroscopy}, series = {Microporous and mesoporous materials : zeolites, clays, carbons and related materials}, volume = {288}, journal = {Microporous and mesoporous materials : zeolites, clays, carbons and related materials}, publisher = {Elsevier}, address = {Amsterdam}, issn = {1387-1811}, doi = {10.1016/j.micromeso.2019.109580}, pages = {6}, year = {2019}, abstract = {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).}, language = {en} } @article{HartwigHass2018, author = {Hartwig, Anne and Hass, Roland}, title = {Monitoring lactose crystallization at industrially relevant concentrations by photon density wave spectroscopy}, series = {Chemical engineering \& technology}, volume = {41}, journal = {Chemical engineering \& technology}, number = {6}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0930-7516}, doi = {10.1002/ceat.201700685}, pages = {1139 -- 1146}, year = {2018}, abstract = {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.}, language = {en} } @article{HassMunzkeRuizetal.2015, author = {Hass, Roland and Munzke, Dorit and Ruiz, Salome Vargas and Tippmann, Johannes and Reich, Oliver}, title = {Optical monitoring of chemical processes in turbid biogenic liquid dispersions by Photon Density Wave spectroscopy}, series = {Analytical \& bioanalytical chemistry}, volume = {407}, journal = {Analytical \& bioanalytical chemistry}, number = {10}, publisher = {Springer}, address = {Heidelberg}, issn = {1618-2642}, doi = {10.1007/s00216-015-8513-9}, pages = {2791 -- 2802}, year = {2015}, abstract = {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.}, language = {en} }