Batch Reactor Research Articles

Comprehensive review of hydrothermal liquefaction data for use in machine‐learning models

AbstractHydrothermal liquefaction is a new, sustainable pathway to generate biogenic liquids from organic resources. The technology is compatible with a wide variety of resources such as lignocellulosic resources, organic waste, algae, and sewage sludge. The chemistry is complex and predictions of yields are notoriously difficult. Understanding and modeling of hydrothermal liquefaction is currently mostly based on a simplified biochemical analysis and product yield data. This paper presents a large dataset of 2439 experiments in batch reactors that were extracted from 171 publications in the scientific literature. The data include biochemical composition data such as fiber content and composition, proteins, lipids, carbohydrates, and ash. The experimental conditions are recorded for each experiment as well as the reported yields. The objective of this paper is to make a large database available to the scientific community. This database is analyzed with machine‐learning tools. The results show that there is no consensus on the analysis techniques, experimental procedures, and reported data. There are many inconsistencies across the literature that should be improved by the scientific community. Machine‐learning tools with a large dataset allow the generation of reliable yield production tools with a large application field. Given the accuracy of the data, the overall precision of prediction in an extrapolation to new results can be expected to be around 10%.

Aerobic granulation and resource production under continuous and intermittent saline stress

Three sequential batch reactors (SBR) were operated to evaluate salt addition's impact on granulation, performance, and biopolymer production in aerobic granular sludge (AGS) systems. System R1 was fed without adding salt (control); system R2 operated with saline pulses, i.e., one cycle with salt (2.5 g NaCl/L) addition followed by another without salt; and R3 received continuous supplementation of 2.5 g NaCl/L. The results indicated that the reactors supplemented with salt presented higher concentrations of mixed liquor volatile suspended solids (MLVSS) and better settleability than R1, showing that osmotic pressure contributed to biomass growth, accelerated granulation, and improved physical characteristics. The faster granulation occurred in R2, thus proving the beneficial effects of intermittent salt addition through alternating pulses. Salt addition did not impair the simultaneous removal of carbon, nitrogen, and phosphorus. In fact, R2 showed better carbon removals. In conclusion, continuous or intermittent (pulsed) supplementation of 2.5 g NaCl/L did not lead to increased production of extracellular polymeric substances (EPS) and alginate-like exopolymers (ALE). This outcome could be attributed to the low saline concentration employed, a higher food-to-microorganism (F/M) ratio observed in R1, and possibly greater endogenous consumption of biopolymers in the famine period in R2 and R3 due to the greater solids retention time (SRT). Therefore, this study brings important results that contribute to a better understanding of the effect of salt in continuous dosing or in pulses as a selection pressure strategy to accelerate granulation, as well as the behavior of the AGS systems for saline effluents.

Nitrification–Autotrophic Denitrification Using Elemental Sulfur as an Electron Donor in a Sequencing Batch Reactor (SBR): Performance and Kinetic Analysis

Simultaneous nitrification and autotrophic denitrification (SNAD) has received attention as an efficient biological nitrogen removal alternative. However, SNAD using elemental sulfur (S0) has scarcely been studied. Thus, the main objective of this research was to study the behavior of a simultaneous nitrification–autotrophic denitrification operation in a sequential batch reactor (SNAD-SBR) at a lab scale using S0 as an electron donor, including its kinetics. Two-scale reactors were operated at lab scales in cycles for 155 days with an increasing nitrogen loading rate (NLR: 0.0296 to 0.0511 kg N-NH4+/m3/d) at 31 °C. As a result, simultaneous nitrification–autotrophic denitrification using S0 as an electron donor was performed successfully, with nitrification efficiency of 98.63% and denitrification efficiency of 44.9%, with autotrophic denitrification as the limiting phase. The kinetic model adjusted for ammonium-oxidizing bacteria (AOB) was the Monod-type kinetic model (µmax = 0.791 d−1), while, for nitrite-oxidizing bacteria (NOB), the Haldane-type model was employed (µmax = 0.822 d−1). For denitrifying microorganisms, the kinetic model was adjusted by a half order (k1/2v = 0.2054 mg1/2/L1/2/h). Thus, we concluded that SNAD could be feasible using S0 as an electron donor, with kinetic behavior similar to that of other processes.

Facile Synthesis of WS2/WO3 Materials in a Batch Reactor for the Hydrogen Evolution Reaction

In this study, a new and facile process was developed for the preparation of composite catalysts based on tungsten oxide (WO3) by batch reactor routes. The structures, morphologies, compositions, and characteristics of synthesized materials were investigated and confirmed. Using batch reactor processes, WO3 nanorods (WO3 NR), heterostructures of WS2/WO3 nanobricks (WS2/WO3 NB), and WS2/WO3 nanorods (WS2/WO3 NR) were successfully prepared. The prepared materials were then employed for hydrogen evolution reaction (HER) to investigate their catalytic performance. The results indicated that the electrocatalytic activities of WS2/WO3 NR are significantly improved compared to those of WO3 NR and WS2/WO3 NB. This improvement could be attributed to the formation of heterostructure between WS2 and WO3 elements in highly uniform materials, which could create the synergistic effect and further improve the catalytic activities of the catalyst. The data shows that the Tafel slope of WS2/WO3 NR (82.7 mV dec−1) is significantly lower than that of WO3 NR (112.5 mV dec−1) and WS2/WO3 NB (195.5 mV dec−1). Furthermore, the resistance of WS2/WO3 NR (397.7 Ω) is markedly decreased compared to those of WO3 NR (1816 Ω) and WS2/WO3 NB (3597 Ω). The results indicate that WS2/WO3 NR could be a great catalyst for electrochemical applications.

Raney Nickel‐Catalyzed Deuterium Labeling of Nitrogen‐Containing Heterocycles and Pharmaceuticals under Continuous Flow Conditions

Deuterium‐labeled compounds play a pivotal role in physical organic chemistry, life sciences, and materials science. This has resulted in a surge of interest in deuterium‐labeled active pharmaceutical ingredients in recent years. In this study, we present a continuous flow Raney nickel‐catalyzed hydrogen isotope exchange process that boasts compatibility with a wide spectrum of nitrogen‐containing heterocycles and pharmaceutical compounds. The broad applicability of the developed method was demonstrated through successful labeling of various purine bases, imidazoles, pyridines, and active pharmaceutical ingredients, including complex structures like abacavir and remdesivir. Control experiments revealed Raney nickel's crucial role in the exchange process, showcasing the superiority of the continuous flow approach over batch reactions. Furthermore, a scaled‐up experiment demonstrated the robustness of the catalyst.

Integrated partial nitrification and Tribonema minus cultivation for cost-effective ammonia recovery and lipid production from slaughterhouse wastewater

High ammonium content in untreated anaerobic digestion (AD) wastewater can inhibit microalgal growth, hindering both bioremediation and biomass/lipid productivity. This study investigated the potential of partial nitrification (PN) as a pretreatment step for AD effluent before cultivating the oleaginous microalga Tribonema minus for bioremediation and lipid production. The PN process transforms inhibitory ammonium into nitrate, a nitrogen form that microalgae can effectively utilize, thereby reducing ammonia toxicity. The results showed remarkable resilience in T. minus, with the species being able to tolerate high ammonium levels (≤120 mg/L) when combined with nitrate in synthetic wastewater. However, when ammonium was the sole nitrogen source (>30 mg/L), its inhibitory effect on T. minus growth became evident. Nevertheless, successful cultivation of T. minus was achieved in PN effluent from slaughterhouse AD using a Sequencing Batch Reactor (SBR) (25 °C and hydraulic retention time (HRT) of 1.5 h) containing 190 mg/L ammonium, achieving 51.25 % lipid accumulation. Additionally, cultivation with 125 mg/L NH4+-N in the PN effluent resulted in removal rates exceeding 95 % for NH4+-N. This approach, therefore, delivered the dual advantage of not only mitigating the environmental risks associated with wastewater but also fostering renewable biomass production for cleaner energy.

Simultaneous nitrification and denitrification pattern in aerated moving-bed sequencing batch reactor: Choosing appropriate SRT for different COD/N ratios

ABSTRACT The effect of chemical oxygen demand (COD)/N ratio and sludge retention time (SRT) on the simultaneous nitrification and denitrification (SND) process in an aerated moving-bed sequencing batch reactor (A-MBSBR), for treating synthetic municipal wastewater, was studied. Three lab-scale reactors with SRTs of 5, 10, and 15 days were operated under COD/N ratios of 10 (phase 1) and 20 (phase 2). The high correlation coefficients between nitrification and denitrification efficiencies in both phases demonstrated that the denitrification efficiency in A-MBSBRs was strongly affected by nitrification efficiency (nitrate concentration). A high COD/N ratio of 20 in phase 2 provided suitable conditions for the increase and dominance of the population of heterotrophic bacteria over autotrophic nitrifiers, which led to weak nitrification (29.6–39.1%) and consequently weak denitrification (15.8–27.9%) in all reactors. In phase 2, increasing SRT from 5 to 15 days was beneficial for both nitrification and denitrification reactions. Therefore, the optimal SND efficiency in phase 2 was expected to be achieved under SRTs higher than 15 days. Under the COD/N ratio of 10 in phase 1, a better balance between the population of heterotrophs and autotrophs resulted in higher nitrification and denitrification efficiencies (44.4–62.7% and 26.3–42.8%, respectively). In phase 1, the highest and the lowest nitrification and denitrification efficiencies were obtained at SRTs of 10 and 5 days, respectively.

On the synthesis of diphenhydramine: Steady state kinetics, solvation effects, and in-situ Raman and benchtop NMR as PAT

Diphenhydramine is a first-generation antihistamine that is available over-the-counter to treat maladies such as allergic reactions and insomnia. Despite its ubiquity in society and high demand, the kinetics for either step of diphenhydramine synthesis have not been explored in detail. In this work, for the first step, a methodology has been devised to obtain kinetics from the heterogeneous halogenation of benzhydrol with hydrochloric acid in a batch reactor equipped with in-situ Raman probe and further verified with ex-situ low-field NMR spectroscopy. For the second step, the kinetics of etherification have been explored using a microfluidic flow reactor and at-line NMR spectroscopy in a variety of solvents. Arrhenius and Eyring parameters are determined for Step 2. We find that the reaction performance is well correlated with the acceptor number of the solvent indicating that the Lewis acidity of the solvent plays a significant role in the overall performance.

A comparison of batch and semi-batch reactors for leaching battery cathodes (LiCoO2) under controlled addition of HCl and H2O2

Recovery of cobalt and lithium from end-of-life Li-ion battery wastes have been evaluated in batch and semi-batch leaching systems. In this preliminary study, HCl and H2O2 were used as leaching and reducing agents, respectively. The comparison of batch and semi-batch processes was carried out, obtaining an improvement from 40% to 70% in the metal mass extracted (i.e. Co and Li) for semi-batch experiments under the same experimental conditions. Effects of the initial concentration of reducing and leaching agents were evaluated for a semi-batch system in which the acid was continuously fed to maintain a constant pH value. From experimental results, it was found that the concentration of H2O2 plays an important role in the leaching process in terms of selectivity. For the experiments carried out using 0.1 M of HCl and 1 M of H2O2, the percentage of Li and Co extracted was 90% for a leaching time of 30 min. The double-controlled addition of HCl and H2O2 to the semi-batch system allows the reduction of the H2O2 concentration to 0.5 M. The optimization of reactants entails not only the decrease of their consumption but also maximize the selectivity of the reactions desired, which represents promising results for the environmental sustainability of the process. Further work will examine the fate of chloride ions in the process.

Effluent quality improvement in sequencing batch reactor-based wastewater treatment processes using advanced control strategies.

The treatment of wastewater is highly challenging due to large fluctuations in flowrates, pollutants, and variable influent water compositions. A sequencing batch reactor (SBR) and modified SBR cycle-step-feed process (SSBR) configuration are studied in this work to effectively treat municipal wastewater while simultaneously removing nitrogen and phosphorus. To control the amount of dissolved oxygen in an SBR, three axiomatic control strategies (proportional integral (PI), fractional proportional integral (FPI), and fuzzy logic controllers) are presented. Relevant control algorithms have been designed using plant data with the models of SBR and SSBR based on ASM2d framework. On comparison, FPI showed a significant reduction in nutrient levels and added an improvement in effluent quality. The overall effluent quality is improved by 0.86% in FPI in comparison with PI controller. The SSBR, which was improved by precisely optimizing nutrient supply and aeration, establishes a delicate equilibrium. This refined method reduces oxygen requirements while reliably sustaining important biological functions. Focusing solely on the FPI controller's performance in terms of total air volume consumption, the step-feed SBR mechanism achieves an excellent 11.04% reduction in consumption.

Semi‐continuous non‐sterile production of medium chain‐length polyhydroxyalkanoates from fatty acids

AbstractMedium chain‐length polyhydroxyalkanoates (mcl‐PHAs) are efficiently synthesized from fatty acids. It was hypothesized that under non‐axenic conditions, the anti‐microbial properties of fatty acids would reduce growth of microbial competitors and allow Pseudomonas putida LS46 to dominate the population resulting in non‐sterile mcl‐PHA production. Non‐sterile batch and fed‐batch cultures produced similar final mcl‐PHA content, monomer composition, and productivity during 24–27 h cultivations when compared to sterile control cultures for initial octanoic acid concentrations ranging from 5 to 40 mM at an initial pH of 6.5. In the absence of a P. putida inoculum, growth was eventually observed in non‐sterile medium after a lag period of up to 120 h, the length of which was dependent on the octanoic acid concentration. The efficacy of prolonged non‐sterile cultivation was tested using a sequential batch reactor (SBR). After 28 days (672 h), 1.62 g L−1 of total biomass was observed, of which the mcl‐PHA content was 47%. This resulted in a PHA titer of 0.77 g L−1, and a volumetric PHA productivity of 32 mg L−1 h−1. The polymer composition remained stable throughout at 87.0 ± 2.7% C8 monomers, and short‐chain length (scl‐) monomers were not detected. This study is the first of its kind to report that purely mcl‐PHAs were produced after prolonged periods in a non‐sterile environment and demonstrate that medium chain‐length fatty acids exert a strong selective pressure toward organisms that synthesize mcl‐PHA. This suggests an opportunity for mcl‐PHA production in open continuous cultivation, which could reduce both fixed and operating costs.

Design space identification of a coupled two-stage batch reactor system

The design space (DS) is defined as the combination of materials and process conditions that guarantees the assurance of quality. This principle ensures that as long as a process operates within DS, it consistently produces a product that meets specifications. It was originally developed for a single unit system. Many industrial processes frequently involve multiple unit operations. Assessing the interaction of Critical Process Parameters (CPPs) with Critical Quality Attributes (CQAs) across stages enables informed decision-making and the capacity to balance different requirements. Analysis and visualization of the complex, multi-dimensional DS is a challenging task. This paper presents a framework for identification such DSs, considering both joint and decoupled strategies using a detailed analysis of a two-stage batch reactor case study. We assess and discuss the practicality and relevance of these methods.

Upscaling the reaction rates in porous media from pore- to Darcy-scale

Modeling and prediction of reactive transport in porous media are challenging due to the complexity of the characterization of reactions across spatial and time scales. The application of reaction rates obtained from batch experiments to porous media is not valid because it disregards the influences of flow pathways, distribution of residence time, transport limitations within the porous media, as well as neglecting the impact of surface mineralogy heterogeneity. In this study, we presented how the pore-scale modeling can help to improve the Darcy-scale simulations. First, the reactive transport was simulated in a pore-network model and was validated against the experiments. Then, the pore-network results were averaged to obtain the effective reaction rates as a function of pore velocity, the inlet concentration, and the resident concentration. The upscaled function was incorporated into the Darcy-scale model and showed a significant improvement in predicting the concentration profiles. Notably, the use of batch reaction rates in the Darcy model (ADRE-batch) led to significant underestimation, up to 93%, of the required pore volume injection for complete contaminant removal from the simulation domain.

Process Intensification of the Continuous Synthesis of Bio-Derived Monomers for Sustainable Coatings Using a Taylor Vortex Flow Reactor.

We describe the optimization and scale-up of two consecutive reaction steps in the synthesis of bio-derived alkoxybutenolide monomers that have been reported as potential replacements for acrylate-based coatings (Sci. Adv.2020, 6, eabe0026). These monomers are synthesized by (i) oxidation of furfural with photogenerated singlet oxygen followed by (ii) thermal condensation of the desired 5-hydroxyfuranone intermediate product with an alcohol, a step which until now has involved a lengthy batch reaction. The two steps have been successfully telescoped into a single kilogram-scale process without any need to isolate the 5-hydroxyfuranone between the steps. Our process development involved FTIR reaction monitoring, FTIR data analysis via 2D visualization, and two different photoreactors: (i) a semicontinuous photoreactor based on a modified rotary evaporator, where FTIR and 2D correlation spectroscopy (2D-COS) revealed the loss of the methyl formate coproduct, and (ii) our fully continuous Taylor Vortex photoreactor, which enhanced the mass transfer and permitted the use of near-stoichiometric equivalents of O2. The use of in-line FTIR monitoring and modeling greatly accelerated process optimization in the Vortex reactor. This led to scale-up of the photo-oxidation in 85% yield with a projected productivity of 1.3 kg day-1 and a space-time yield of 0.06 mol day-1 mL-1. Higher productivities could be achieved while sacrificing yield (e.g., 4 kg day-1 at 40% yield). The use of superheated methanol at 200 °C in a pressurized thermal flow reactor accelerated the second step, the thermal condensation of 5-hydroxyfuranone, from a 20 h batch reflux reaction (0.5 L, 85 g) to a space time of <1 min in a reactor only 3 mL in volume operating with projected productivities of >700 g day-1. Proof of concept for telescoping the two steps was established with an overall two-step yield of 67%, producing a process with a projected productivity of 1.1 kg day-1 for the methoxybutenolide monomer without any purification of the 5-hydroxyfuranone intermediate.

Fluid‐rock interaction experiments with andesite at 100°C for potential carbon storage in geothermal reservoirs

AbstractGeothermal energy extraction often results in the release of naturally occurring carbon dioxide (CO2) as a byproduct. Research on carbon storage using volcanic rock types other than basalt under both acidic and elevated temperature conditions has been limited so far. Our study uses batch reactor experiments at 100°C to investigate the dissolution of andesite rock samples obtained from an active geothermal reservoir in Sumatra (Indonesia). The samples are subjected to reactions with neutral‐pH fluids and acidic fluids, mimicking the geochemical responses upon reinjection of geothermal fluids, either without or with dissolved acidic gases, respectively. Chemical elemental analysis reveals the release of Ca2+ ions into the fluids through the dissolution of feldspar. The overall dissolution rate of the rock samples is 2.4 × 10–11 mol/(m2 · s) to 4.2 × 10–11 mol/(m2 · s), based on the Si release during the initial 7 h of the experiment. The dissolution rates are about two orders of magnitude lower than those reported for basaltic rocks under similar reaction conditions. This study offers valuable insights into the potential utilization of andesite reservoirs for effective CO2 storage via mineralization.

Polymeric surfactants with high acid values for emulsion type pressure-sensitive adhesives

Low molecular weight polymers with hydrophobic-carboxyl groups have been usually used as anionic surfactants in emulsion polymerization for coatings. However, such polymeric surfactants usually have low acid values below 200, because it is difficult to make high acid-value polymeric surfactants using a normal batch reactor. In this work, we polymerized high acid value polymeric surfactant having high acid values successfully up to 380 using CSTR (continuous stirring tank reactor). The synthesized polymeric surfactant was a random copolymer of P(BA-AA) and we applied them as anionic surfactants in making emulsion-type acrylic PSAs (Pressure-Sensitive Adhesives) to investigate the effects of high acid values on the adhesive properties. This CSTR can effectively control the composition and molecular weight of polymeric surfactants through varying monomer ratios, retention time, and initiator concentrations. The surface tension analysis and emulsion stability test indicated that the synthesized polymeric surfactants exhibited a similar levels of critical micelle concentration (CMC) and emulsion stability with other conventional anionic surfactants. Also, the adhesion property analysis showed that the PSA used high acid value polymeric surfactant resulting in superior adhesive properties and heat resistance than the PSAs used low acid value polymeric surfactant or conventional low molecular weight surfactant. It was very notable that polymeric surfactants having unusually high acid values above 300 because of their high contents of carboxylic acid groups could result in superior adhesive properties and heat resistance.

Effect of Feed Mass, Reactor Temperature, and Time on the Yield of Waste Polypropylene Pyrolysis Oil Produced via a Fixed-Bed Reactor.

This paper presents the results of investigations into the pyrolysis of waste polypropylene in a laboratory fixed-bed batch reactor. The experiments were designed and verified in such a way as to allow the application of the response surface methodology (RSM) in the development of an empirical mathematical model that quantifies the impacts mentioned above. The influence of the mass of the raw material (50, 100, and 150 g) together with the reactor temperature (450, 475, and 500 °C) and the reaction time (45, 50 and 75 min) was examined. It has been shown that the mass of the raw material, i.e., the filling volume of the reactor, has a significant influence on the pyrolysis oil yield. This influence exceeds the influence of reactor temperature and reaction time. This was explained by observing the temperature change inside the reactor at three different spots at the bottom, middle, and top of the reactor. The recorded temperature diagrams show that, with greater masses of feedstock, local overheating occurs in the middle part of the reactor, which leads to the overcracking of volatile products and, from there, to an increased formation of non-condensable gases, i.e., a reduced yield of pyrolytic oil.

Preparation of functionalizable poly(propylene–styrene)/polyacrylonitrile millimeter‐scale particles with core‐shell morphology

AbstractCore‐Shell (CS) polymeric particles have attracted great interest due to their high mechanical, thermal, and chemical stability and their surface properties. In this study, functionalizable CS poly(propylene/styrene)/poly(acrylonitrile) (PP/PS/PAN) particles were prepared through heterogeneous polymerizations in a batch reactor. Commercial PP particles and PP/PS particles (prepared by seeded suspension polymerization of styrene (Sty) on PP spheres) were applied as core components of the final structure, while the shell was prepared through acrylonitrile dispersion polymerization. The degree of swelling of the core particles by Sty played an important role for the adhesion of the PAN shell, which for PP particles was 24 wt%, whereas for PP/PS hybrid particles it was 57 wt%. The particles (PP/PS and CS) were characterized through image analysis, revealing a uniform and smooth surface for PP/PS spheres and a uniform porous shell for CS particles. Particle size distributions, thermal degradation, chemical structures, degrees of crystallinity, and textural properties were also evaluated. The PAN shell adhered to the PP/PS particles without forming a copolymer, and the CS particles formed by a PP/PS core and PAN shell had sizes of 4.54 ± 1.24 mm, specific area of 2.70 m2g−1 and PAN content of 15.98 ± 0.82% (m/m) of total particles.

A comparative study on the production of Ni1/3Co1/3Mn1/3C2O4 cathode precursor material for lithium-ion batteries using batch and slug-flow reactors

The intermittent nature of the renewable energy sources drifts research interest towards various electrochemical energy storage devices, such as the lithium ion battery, which offers consistent power supply. The manufacturing cost and electrochemical performance of a battery pack largely depends on the quality of the cathode material, which further depends on the production method and its parameters. However, the traditional stirred tank-based co-precipitation manufacturing process for precursors of lithium nickel manganese cobalt oxide (NCM111) cathode suffers from inhomogeneity in the reaction environment, which leads to non-uniform morphology and particle size distribution (PSD). In this work, slug-flow-based manufacturing platform, which offers a homogeneous reaction environment, is used for the continuous production of NCM111 oxalate precursors. One of the novel features of this work is the comparative study between the quality of batch and slug-flow-derived products. The slug-flow-derived product is found to be better in terms of having bigger particle size, narrower PSD and higher tap density. The study on the single and dual-element precipitation in similar conditions to understand the co-precipitation behavior in the slug-flow manufacturing platform is also a unique feature of this work. Furthermore, the effect of NH4OH concentration and residence time (RT) on the electrochemical performance of cathode were also studied and it is found that the cathode precursors synthesized at a NH4OH concentration of 0.08 M and a RT of 2 minutes followed by lithiation shows a better electrochemical performance of 128 mAh g−1 at 0.1 C with cycling stability of more than 80% both at 0.5 C and 1 C.

Quantitative image analysis for assessing extracellular polymeric substances in activated sludge under atrazine exposure

Extracellular polymeric substances (EPS) play a vital role in biological wastewater treatment systems. This study investigates the impact of herbicide atrazine (ATZ) on the overall performance, EPS yield, composition, and sludge morphology in an activated sludge (AS) system operated in a sequencing batch reactor (SBR). Since conventional methods for analyzing EPS are time-consuming and releases residues, a new approach was developed in this work to evaluate the EPS fractions and components, based on the morphological characterization of the biomass using quantitative image analysis (QIA) technique coupled with multivariate statistics.Results showed that exposure to ATZ inhibit biomass activity in terms of organic matter (COD) and nitrogen removal. Moreover, both tightly bound EPS (TB-EPS) and loosely bound EPS (LB-EPS) increased under ATZ, indicating that microorganisms release EPS as a defense mechanism against environmental changes. The PN/PS ratio also increases, indicating likely increased hydrophobicity in ATZ phases. Furthermore, ATZ phases exhibit a predominance of large aggregates compared to intermediate and small ones, indicating a change in aggregate morphological structure associated with EPS production. The new approach using QIA coupled with partial least squares (PLS) modeling provides accurate predictions of EPS content. The increase in TB-EPS is closely related to the rise of large aggregates in phases exposed to higher ATZ concentrations. The PLS models demonstrate high accuracy for EPS prediction (coefficients of determination, R2 above 0.86), showcasing the feasibility of using QIA for EPS assessment in AS systems. This approach offers significant potential for regular process monitoring and management, providing a more environmentally friendly methodology by eliminating the need for chemical usage.