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1. In-situ monitoring of calcium carbonate scale progression on reverse osmosis membranes using Raman spectroscopy

   https://doi.org/10.5004/dwt.2022.28883  

   Park, Danielle J.; Supekar, Omkar D.; Greenberg, Alan R.; Gopinath, Juliet T.; Bright, Victor M. (January 2022, DESALINATION AND WATER TREATMENT)

   Direct monitoring techniques of fouling in membrane-based filtration processes can be implemented as part of an effort to reduce the negative effects of membrane fouling. In particular, monitoring techniques with chemical characterization capability are crucial for the formulation of effective fouling prevention and mitigation strategies. In the present work, Raman spectroscopy was applied as an in-situ monitoring technique for calcium carbonate scaling on commercial reverse osmosis membranes. The bench-scale Raman monitoring system allowed for a qualitative chemical assay of the scaled membrane surface at sequential downstream and upstream axial positions. The time evolution of the downstream and upstream calcium carbonate Raman signal was evaluated with respect to computed values of local concentration at the membrane surface, revealing a statistically significant dependence (p < 0.001). The real-time Raman data were bolstered by results of post-mortem analysis (scanning electron microscopy, gravimetric measurements, and laser interferometry). The employed technique was capable of detecting crystals with characteristic lengths <50 μm. Preliminary evidence of polymorph detection was also presented with recommendations for improvements in the technique. 

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2. A comprehensive study on combined organic fouling and gypsum scaling in reverse osmosis: Decoupling surface and bulk phenomena

   https://doi.org/10.1016/j.memsci.2023.122399  

   Park, Shinyun; Saavedra, Mayca; Liu, Xitong; Li, Tianshu; Anger, Bridget; Tong, Tiezheng (February 2024, Journal of Membrane Science)

   Reverse osmosis (RO), as an energy efficient desalination technology that is critical to mitigate water scarcity, encounters feedwater containing both organic foulants and inorganic scalants. However, comparing with extensive studies on individual fouling or scaling, our knowledge of the behavior and mechanisms associated with combined organic fouling and mineral scaling is still lacking. Due to the potential occurrence of mineral formation in both bulk solution and on the membrane surface, a complete, mechanistic understanding of combined fouling and scaling requires decoupling of surface and bulk phenomena. Herein, our study employed a comprehensive investigation to delve into the intricate interplay of gypsum scaling and organic fouling in RO process. Our systematic approach is accomplished through three sets of experiments that include static experiments and two types of dynamic experiments (i.e., (1) combined fouling and scaling, and (2) gypsum scaling on foulant-conditioned membranes). A variety of model foulants including humic acid, alginate, bovine serum albumin (BSA), and lysozyme were used to investigate the effects of foulant type. Our results demonstrate that the behavior of combined organic fouling and gypsum scaling aligns more with that of gypsum scaling on foulant-conditioned membranes rather than static experiments where bulk nucleation occurs, indicating the predominance of surface nucleation in RO. BSA exhibited a remarkable hindering effect on gypsum scaling, whereas other foulants displayed an additive effect. The lack of scaling mitigation by lysozyme suggests that molecular properties of protein must play a role in regulating the behavior of combined fouling and scaling. Results from multiple characterization techniques reveal the foulant-scalant interactions by delineating the morphological and chemical features of the fouling/scaling layers. Our study not only elucidates the mechanisms of combined organic fouling and gypsum scaling but also sheds light on potential strategies for membrane scaling control in RO desalination. 

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3. A tale of two minerals: contrasting behaviors and mitigation strategies of gypsum scaling and silica scaling in membrane desalination

   https://doi.org/10.1007/s11783-025-1923-9  

   Tong, Tiezheng; Park, Shinyun; Yao, Yiqun (January 2025, Frontiers of Environmental Science & Engineering)

   Abstract Mineral scaling represents a major constraint that limits the efficiency of membrane desalination, which is becoming increasingly important for achieving sustainable water supplies in the context of a changing climate. Different mineral scales can be formed via distinct mechanisms that lead to a significant variation of scaling behaviors and mitigation strategies. In this article, we present a comprehensive review that thoroughly compares gypsum scaling and silica scaling, which are two common scaling types formed via crystallization and polymerization respectively, in membrane desalination. We show that the differences between scale formation mechanisms greatly affect the thermodynamics, kinetics, and mineral morphology of gypsum scaling and silica scaling. Then we review the literatures on the distinct behaviors of gypsum scaling and silica scaling during various membrane desalination processes, examining their varied damaging effects on desalination efficiency. We further scrutinize the different interactions of gypsum and silica with organic foulants, which result in contrasting consequences of combined scaling and fouling. In addition, the distinctive mitigation strategies tailored to controlling gypsum scaling and silica scaling, including scaling-resistant membrane materials, antiscalants, and pretreatment, are discussed. We conclude this article with the research needs of attaining a better understanding of different mineral scaling types, aiming to inspire researchers to take scale formation mechanism into consideration when developing more effective approaches of scaling control in membrane desalination. 

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4. Antiscalants for mitigating silica scaling in membrane desalination: Effects of molecular structure and membrane process

   https://doi.org/10.1016/j.watres.2023.120701  

   Yao, Yiqun; Ge, Xijia; Yin, Yiming; Minjarez, Ronny; Tong, Tiezheng (November 2023, Water Research)

   Silica scaling is a major type of mineral scaling that significantly constrains the performance and efficiency of membrane desalination. While antiscalants have been commonly used to control mineral scaling formed via crystallization, there is a lack of antiscalants for silica scaling due to its unique formation mechanism of polymerization. In this study, we performed a systematic study that investigated and compared antiscalants with different functional groups and molecular weights for mitigating silica scaling in membrane distillation (MD) and reverse osmosis (RO). The efficiencies of these antiscalants were tested in both static experiments (for hindering silicic acid polymerization) as well as crossflow, dynamic MD and RO experiments (for reducing water flux decline). Our results show that antiscalants enriched with strong H-accepters and H-donors were both able to hinder silicic acid polymerization efficiently in static experiments, with their antiscaling performance being a function of both molecular functionality and weight. Although poly(ethylene glycol) (PEG) with abundant H-accepters exhibited high antiscaling efficiencies during static experiments, it displayed limited performance of mitigating silica scaling during MD and RO. Poly (ethylene glycol) diamine (PEGD), which has a PEG backbone but is terminated by two amino groups, was efficient to both hinder silicic acid polymerization and reduce water flux decline in MD and RO. Antiscalants enriched with H-donors, such as poly(ethylenimine) (PEI) and poly(amidoamine) (PAMAM), were effective of extending the water recovery of MD but conversely facilitated water flux decline of RO in the presence of supersaturated silica. Further analyses of silica scales formed on the membrane surfaces confirmed that the antiscalants interacted with silica via hydrogen bonding and showed that the presence of antiscalants governed the silica morphology. Our work indicates that discrepancy in antiscalant efficiency exists between static experiments and dynamic membrane filtration as well as between different membrane processes associated with silica scaling, providing valuable insights on the design principle and mechanisms of antiscalants tailored to silica scaling. 

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5. Raman imaging of membrane fouling

   https://doi.org/https://doi.org/10.1016/j.seppur.2020.116763  

   Azizighannad, S.; Intrchomb, W.; Mitra, S. (February 2020, Separation and purification technology)

   Membrane processes are widely used in industrial applications such water purification, food processing and pharmaceutical manufacturing. During their operation, the accumulation of foulants in membrane pores and on membrane surfaces lead to the reduction in flux, membrane lifetime and increase in operational cost, and the understanding of the fouling phenomenon is important for mitigating these problems. In this paper we report the application of Raman chemical imaging as a means of identify and map foulants on a membrane surface. The surface of a Polytetrafluoroethylene (PTFE) membrane was studied by Raman chemical imaging before and after fouling during desalination via membrane distillation. Information about location and concentration of three different salts namely CaSO4, BaSO4 and CaCO3 was studied. The three salts showed different distribution patterns, and their distribution was analyzed by correlation mapping and multivariate curve resolution. It was observed that CaSO4 agglomerated in specific places while the BaSO4 and CaCO3 were more distributed. Raman imaging appears to be a powerful tool for studying membrane foulants and can be effective in identifying the distribution of different species on a membrane surface. 

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