Sustainable Chemistry

Driven by the urgent need for large-scale disposal and resource valorization of bauxite residue (red mud), this review adopts a narrative review perspective, grounded in the Earth’s Macro-Cycle concept, and employs a structured yet non-systematic literature survey across multiple databases (Web of Science, ScienceDirect, etc.) to compare the physicochemical property differences of red mud derived from different production processes and to establish a classification–evaluation system integrating calcium content gradient with reaction type. Building upon this framework, three distinct cementitious systems are elucidated: three-dimensional network formation via low-calcium geopolymerization, the symbiotic coexistence of C-(A)-S-H and N-A-S-H dual gels in medium- and high-calcium systems, and the integration of clinker hydration with alkali activation in high-calcium systems. Furthermore, by evaluating alkalization, heavy metal stabilization, and fluoride immobilization behaviors, we propose optimal, scenario-specific application pathways: Low-calcium geopolymer systems are ideal for the ecological or structural remediation of acid-contaminated sites, medium-to-high-calcium systems for backfilling large-scale mining voids, and high-calcium systems for the structural repair of expressways. This work bridges the gap between fundamental solid waste mineralogy and practical engineering applications, offering robust strategies for the high-value, environmentally safe, and large-scale recycling of industrial solid wastes. Full article

Cellulose crystallinity is frequently associated with lignocellulosic biomass digestibility, yet its development during multistep biorefinery processing and its relationship with enzymatic hydrolysis remain difficult to isolate. This study investigated the evolution of cellulose crystallinity in wheat straw (Triticum aestivum) during Hot-Water Pretreatment (HWP), Water Pretreatment (WP), Organosolv extraction, sequential washing, and drying, and related these changes to enzymatic glucose yield. Crystallinity was determined using X-ray diffraction and an ATR-FTIR-based PLS model, while enzymatic hydrolysis was evaluated by HPLC-based glucose quantification. HWP caused a temperature-dependent decrease in crystallinity from 47.5 ± 1.3% in untreated straw to 27.0 ± 2.2% at 120 °C, whereas WP at room temperature caused no significant change. However, without subsequent Organosolv extraction, both pretreatments alone resulted in low glucose yields of approximately 10%, indicating that cellulose crystallinity is only one of several factors governing enzymatic hydrolysis efficiency. During washing after Organosolv extraction, crystallinity increased from 40.6 ± 2.1% to 54.2 ± 1.3%, whereas, under the tested conditions, glucose yield was more closely associated with the estimated residual ethanol concentration than with the change in crystallinity. Drying had the strongest effect, increasing crystallinity by up to 53.6% relative to the wet state. Overall, cellulose crystallinity should be considered as one of several interacting factors governing enzymatic digestibility, and sample moisture history must be carefully controlled when comparing crystallinity data. Full article

This study developed an oleic acid (OA)-functionalized, bio-derived calcium carbonate (Bio-CaCO₃) filler recovered from Asian green mussel (Perna viridis) shell waste for incorporation into a hydroxypropyl methylcellulose (HPMC)-glycerol (Gro) matrix as a hydrophobic composite coating for reducing pesticide deposition on mandarin surfaces. Aragonite-rich Bio-CaCO₃ was extracted through a combined chemical treatment and mechanical pulverization process. The extracted Bio-CaCO₃ was characterized by scanning electron microscopy, X-ray diffraction, laser diffraction, and ATR FT-IR spectroscopy. At the optimal OA concentration, surface functionalization yielded OA-functionalized Bio-CaCO₃ (OA-Bio-CaCO₃) powder beds that exhibited apparent superhydrophobicity; successful functionalization was confirmed by X-ray photoelectron spectroscopy. The resulting HPMC-Gro-OA-Bio-CaCO₃ coating dispersion (CD-OA) formed hydrophobic composite films (f-CD-OA), as demonstrated by water contact-angle measurements and surface-morphology analysis. The CD-OA coating formulation was successfully applied to mandarin surfaces by a dip-coating process. Colorimetric screening indicated that organophosphate pesticide residues on coated mandarins did not exceed hazardous levels, even at 20 times the manufacturer-recommended application rate. Quantitative LC-MS/MS and GC-MS/MS analyses demonstrated that the optimized CD-OA coating formulation provided substantial short-term protection against acetamiprid and chlorothalonil with pesticide-deposition reductions of 89% and ≥96%, respectively, after 1 d relative to pristine mandarins. These findings advance the functional reuse of biogenic CaCO₃ and offer a simple, water-based dip-coating approach that provides temporary surface protection for citrus production and food-safety management. Full article

Ibuprofen- and diclofenac-loaded organobentonites are thermally converted to carbon-decorated bentonites and probed as materials for supercapacitors and peroxide production. TGA shows a ~40% mass loss in an inert atmosphere and a ~2% further reduction in air, with the diclofenac-loaded sample showing slightly higher loss due to less stable surface groups. FTIR and Raman spectroscopies indicate similar surface groups and defect densities in the end materials, which are reflected in similar electrochemical responses. Capacitance values of around 20 F/g are measured when taking the whole mass, bentonite and carbon, into account, rising to a maximum of 805 F/g if only the carbon fraction is taken into account. Rotating ring–disk measurements reveal that the prepared materials show selectivity toward peroxide production when oxygen reduction is probed, reaching a 93% yield, making it an exceptional candidate for peroxide production. Full article

In recent years, consumers have been turning to natural products. Following this trend, the European Union has now recognized natural rosemary extract as a natural preservative (E392) in various foods. Considering this, the current study aimed to extract antioxidant compounds from rosemary leaves employing green techniques. More specifically, non-toxic solvents (water-ethanol) and green extraction techniques, such as Atmospheric Room Temperature Plasma (ARTP) for pretreatment of rosemary leaves and subsequently Pressurized Liquid Extraction (PLE) for the recovery of the antioxidant compounds, were used. Response Surface Methodology (RSM) was applied to optimize ARTP operating parameters, and the optimized ARTP + PLE extract was evaluated using spectrophotometric assays and HPLC-DAD. Under optimal conditions, the extract yielded a total polyphenol content (TPC) of ~72 mg gallic acid equivalents per g and an ascorbic-acid-associated reducing capacity (AACRC) of ~19 mg/g, while the extract exhibited relatively high antioxidant capacity as assessed by the FRAP (ferric-reducing antioxidant power) assay (~924 μmol ascorbic acid equivalents per g) and DPPH radical scavenging activity (~467 μmol ascorbic acid equivalents per g). Compared with the untreated PLE control, the ARTP-PLE extract showed increases of 3.1% in TPC, 2.03% in FRAP, 5.61% in DPPH and 25.86% in AACRC. Four commercial rosemary antioxidant preparations (E392) of different formulation types were also analyzed to contextualize the composition of the optimized extract. The commercial products, analyzed in their native form, displayed compositional patterns characteristic of oil-based formulations, whereas the ARTP + PLE extract reflected the profile of hydroethanolic rosemary extracts. These differences arise from extraction conditions and solvent systems. The comparison is descriptive and does not imply quality ranking or stability differences. Overall, the study provides insight into how plasma pretreatment can influence the composition of rosemary extracts within hydroethanolic systems. Full article

Bio-derived functional materials are key platforms for long-term sustainable environmental remediation. Pine wood fibres (WF) are an abundant and renewable material with functional properties suited to specialized applications, including high density of hydroxyl groups at its surface and mechanical toughness imparted by the lignin fraction. In the present work, monometallic and bimetallic nanoparticles (MNP) of first-series transition metals, Fe, Co, Cu and Fe/Cu were immobilized onto original WF and WF treated with NaOH (WF_N). The prepared WF-supported MNP were characterized by SEM/EDS, XPS, XRD and FTIR-ATR, and evaluated in the catalytic reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in aqueous solution, at room temperature, by NaBH₄. Copper-based materials exhibited superior catalytic efficiency, with the NaOH pre-treatment of the fibres yielding shorter induction times and enhanced stability. For the WF_NCu material, 97% of 4-NP reduction was achieved in 3 min with a rate constant of k¹ = 2.147 min⁻¹. This material was used for five successive cycles with no decrease in 4-NP reduction efficiency, being easily recovered from the reaction media. Full article

Biomass-derived nanoengineered carbon materials have emerged as key platforms in environmental technologies due to their high surface area, electrical conductivity, chemical stability, and sustainable synthetic route starting from renewable feedstock. This broad family comprises dimensionally nanoscale materials, such as carbon dots, carbon nanofibers, and graphene-based structures, as well as biochars, hydrochars, activated carbons, and related porous carbonaceous materials whose pore architecture, surface chemistry, or defects are deliberately engineered at the nanometer scale. Beyond their traditional role as passive supports, these materials can actively regulate adsorption phenomena, charge transport, and catalytic microenvironments through precise control of heteroatom doping, graphitic domains, and hierarchical porosity. Among current environmental priorities, carbon dioxide (CO₂) management represents one of the most pressing challenges. Biomass-derived nanocarbons offer tunable adsorption sites for selective CO₂ capture while simultaneously serving as active matrices for catalytic conversion. Tailored doped-carbon frameworks can stabilize key reaction intermediates, suppress competing pathways such as hydrogen evolution, and promote selective transformation into fuels and high-value chemicals. In addition, these materials are excellent hosts for atomically dispersed metals, dual-site catalysts, and semiconductor hybrids used in electrochemical and photocatalytic CO₂ reduction. By combining renewable sourcing with nanoscale control of reactivity, carbon materials create a bridge between environmental remediation and carbon valorization. This review critically examines recent progress in biomass-derived nanoengineered carbon materials for integrated CO₂ capture and conversion, with emphasis on structure-property-performance relationships, mechanistic roles, scalability, and sustainability. Particular attention is also devoted to catalytic conversion and electrochemical CO₂ sensing, where carbon-based and hybrid interfaces enable the transduction of CO₂ recognition into measurable electrical responses. These materials represent a promising yet underexplored pathway toward circular carbon management and the development of next-generation low-carbon chemical technologies. Full article

The contribution of the cathode to system-level efficiency in electrochemical oxidation (EO) is rarely isolated from anodic selectivity limitations, even though its influence on cell voltage, hydrogen evolution kinetics, and energy consumption is well recognized. This study presents a multicriteria methodology that deconvolutes cathode performance from these anodic constraints. A stable lead dioxide anode was paired with three cathodes, carbon felt (CF), stainless steel (SS), and titanium dioxide (TiO₂), for Rhodamine B degradation. The methodology combines conventional electrochemical diagnostics, a ten-parameter multicriteria assessment spanning activity, efficiency, and economics, and a sensitivity analysis prioritizing operational metrics. Application revealed that cathode material governs system-level performance through trade-offs between degradation rate and energy consumption: SS minimized cathodic voltage contribution, while CF maximized degradation rate, with sensitivity analysis confirming CF as the optimal practical choice. However, all systems were constrained by a universal limitation: Faradaic efficiencies remained below 0.3% at an applied current of 30 mA, with anode potential well above the oxygen evolution reaction (OER) threshold and more than 99.7% of charge diverted to unwanted water oxidation. Thus, cathode selection modulates cost and yield but cannot resolve the underlying anodic OER limitation. This methodology offers a transferable diagnostic protocol, indicating that future efforts should prioritize integrated system design over single-electrode optimization to overcome EO selectivity limitations. Full article

Wine pomace is the residue of pressed grapes from wine production. This research focuses on expanding the use of winery by-products by evaluating the bioactivity and safety of Portugieser wine pomace. Moreover, the study discussed that the valorisation of winery by-products can support circular economy principles and improve resource efficiency in agro-industrial management systems. Here, the phenolic profile and bioactivity of Portugieser wine pomace extract (WPE) were investigated. The (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide) (MTT) assay was carried out on malignant human neuroblastoma (SH-SY5Y) and normal human fibroblast cells (MRC-5). The MIC assay and growth dynamics were evaluated in probiotic and pathogenic Escherichia coli strains. WPE antioxidant activity and in vivo toxicity in Artemia salina were evaluated. Predominant WPE compounds included trans-cinnamic acid, gallic acid, catechin, and naringenin. Moderate cytotoxicity to SH-SY5Y cells has been detected (up to 41.7%). The growth capacity of probiotic E. coli has been enhanced. WPE showed notable antioxidant activity and good safety, as indicated by the Artemia survival rate (LD₅₀: 2.27 mg/mL, 24 h). The results justify further rigorous testing of WPE to unambiguously confirm its potential as a functional ingredient and its application in the development of value-added products. Moreover, the study highlights the need for organisational strategies to foster the sustainable valorisation of by-products, such as wine pomace. Full article

The ordered copper-based intermetallic compound Cu_0.83Si_0.17 is capable of enhancing the catalytic efficiency of the in-demand green process of the electrochemical reaction of ammonia synthesis from nitrite in comparison with a pure copper metal catalyst, which is well known and studied. The Faradaic efficiency reaches 99% with its maximum at a potential of −0.525 V (RHE), and even at low potentials (−0.1 V) it does not fall below 90%, with an NH₃ yield rate of 132.3 µmol h⁻¹ cm⁻². In addition, the catalyst demonstrated high selectivity and stability. Full article

Plastic waste presents a persistent environmental burden, yet its constituent polymers represent structurally valuable chemical feedstocks. Mechanical recycling remains limited due to polymer degradation, additive contamination, and material downcycling, underscoring the need for alternative strategies. Chemical upcycling offers pathways to convert post-consumer plastics into higher-value monomers, functional chemicals, and bioactive or pharmaceutical precursors by exploiting inherent structural motifs such as aromatic rings, ester linkages, and heteroatom-containing backbones. Approaches such as catalytic depolymerization, molecular functionalization, microbial and enzymatic transformation, and scaffold repurposing enable the recovery of polymer-derived building blocks with improved functional value. Case studies illustrating the conversion of discarded plastics into advanced materials and biologically relevant small molecules demonstrate the potential of these approaches to stimulate innovation and expand sustainable chemical practices. Collectively, such developments align with green chemistry principles, support emerging circular chemical economies, and contribute to global sustainability priorities reflected in the United Nations Sustainable Development Goals. This review aims to outline the guiding principles of chemical upcycling and highlight the challenges in chemical design, encouraging the modern chemistry community to tap into the hidden potential of waste plastics. Full article

Libidibia coriaria (Cascalote), an underutilized leguminous species native to the tropical Americas, is a promising source of bioactive phenolic compounds with pharmaceutical and nutraceutical potential. This study compared microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), and their hybrid combination (UMAE) for the recovery of hydrolyzable and condensed phenolics from cascalote pods and evaluated the antioxidant capacity of the resulting extracts. UMAE achieved the highest total phenolic content (223.49 mg GAE/g dry matter), while antioxidant capacity varied by assay: MAE showed the highest DPPH radical scavenging activity and FRAP reducing power, whereas UAE exhibited the highest ABTS radical-scavenging activity. Nevertheless, UMAE showed the lowest IC₅₀ values for DPPH and ABTS (228.91 and 155.65 mg/L, respectively), indicating greater concentration-dependent radical-scavenging efficiency. Qualitative HPLC–MS tentatively identified gallotannins, ellagitannins, and hydroxybenzoic acid derivatives. UAE yielded the broadest phenolic profile, whereas MAE and UMAE shared several major tannin-related compounds. FTIR analysis supported the presence of characteristic functional groups associated with gallotannins and ellagitannins. Overall, under the evaluated conditions, UMAE was the most effective extraction method for improving phenolic recovery. These findings highlight the potential of this hybrid extraction approach for the valorization of L. coriaria pods as a source of high-value bioactive phenolic compounds. Full article

Cellulose nanofibers (CNFs) are typically supplied as a 3 wt.% suspension and this leads to higher costs because of the economics associated with shipping a product that is 97% water. Filter pressing is the common approach to reduce shipping cost as water removal leads to approximately 20 wt.% CNF suspensions. In this manuscript, we describe a method to achieve an approximately 35 wt.% CNF suspension by contact dewatering with a dissolvable particle. In this work, contact dewatering was performed using slightly anionic precipitated calcium carbonate (PCC), anionic ground calcium carbonate (GCC), and cationic GCC. After dewatering, calcium carbonate is removed from the CNF suspension by washing with acidic water, and thus a pure CNF suspension is regenerated. Fiber size analysis and scanning electron microscopy imaging showed that the regenerated CNF suspensions had the same properties as the original supplied suspensions. Full article

Electrochemical conversion of carbon dioxide (CO₂) to ethanol offers a potential route for integrating carbon utilization with low-carbon electricity; however, its environmental performance is governed by the complete process system rather than by catalytic selectivity alone. This study presents a detailed attributional cradle-to-gate life cycle assessment of anion-exchange-membrane (AEM) and bipolar-membrane (BPM) electrolyzer systems using a functional unit of 1 kg of ethanol at the plant gate. The foreground inventory combines stoichiometric balances, peer-reviewed electrochemical evidence, process-energy estimates, and transparent engineering assumptions, while background processes are represented using ecoinvent 3.7.1. Climate-change impacts are evaluated with the IPCC 2021 100-year global warming potential method. The modeled AEM and BPM systems require 23.32 and 27.92 kWh of electricity per kilogram of ethanol, respectively. Wind-powered operation yields the lowest reported impacts, at 0.318 kg CO₂-eq kg⁻¹ ethanol for AEM and 0.442 kg CO₂-eq kg⁻¹ for BPM. Photovoltaic scenarios yield 1.812 and 2.231 kg CO₂-eq kg⁻¹, whereas the Austrian-grid scenarios yield 1.349 and 4.686 kg CO₂-eq kg⁻¹, respectively. Electricity supply is the dominant environmental driver, while separation heat, carbon utilization, component lifetime, and oxygen co-product treatment remain important secondary parameters. The BPM Austrian-grid result is disproportionately high relative to the 19.7% increase in modeled electricity demand and therefore requires exchange-level verification before it can be interpreted as a physical membrane effect. Overall, environmentally credible CO₂-to-ethanol deployment requires low-carbon electricity, reduced cell voltage, efficient carbon management, concentrated product streams, durable components, and transparent co-product accounting. Full article

The isoxazole-5-one ring system is a central structure in many synthetic bioactive molecules, showing a wide range of biological activities, including antibacterial, antitumor, anticorrosion, antifungal, antituberculosis, and antioxidant. They are also applied as agrochemicals with potential fungicidal effects. Given various applications, these pharmaceutically and biologically significant heterocyclic compounds have attracted the attention of chemistry researchers. This study aimed to investigate the application of glycerol as a reaction medium for the three-component synthesis of arylidenisoxazol-5(4H)-one derivatives. The results of the optimized investigations revealed that 3.0 mL of glycerol is the best reaction medium. Evaluation of the effect of reaction temperature showed that the best temperature for this strategy is 60 °C. In the present environmentally friendly study, the desired heterocyclic compounds were quickly synthesized via a one-pot three-component reaction of two keto-esters with hydroxylamine hydrochloride and a number of aryl/heteroaryl aldehydes. This synthetic approach has significant merits, such as cost-effectiveness of the reaction medium, rapid green synthesis, operational simplicity, easy workup, avoiding chromatographic purification, sustainability, acceptable yields, and relatively inexpensive as well as commercially available starting materials. Full article

Black seed (Nigella sativa L., Ranunculaceae) possesses antimicrobial activity due to its bioactive compound, thymoquinone. This study aimed to extract thymoquinone from black seed using an alternative natural deep eutectic solvent (NADES) through an optimization approach. A NADES based on malic acid and choline chloride was employed in this work. The Box–Behnken design was used to investigate the effects of the molar ratio of malic acid to choline chloride, water addition, and ultrasonication time. These variables were varied as follows: the malic acid to choline chloride molar ratio ranged from 2:1 to 4:1, the mass ratio of water to NADES from 0.5:2 to 1.5:2, and the ultrasonication time from 60 to 120 min. The results showed that the malic acid to choline chloride molar ratio, the quadratic term of the malic acid to choline chloride molar ratio, and the quadratic term of ultrasonication time significantly affected thymoquinone extraction. The optimal condition, which yielded the highest thymoquinone concentration, was determined to be a malic acid to choline chloride molar ratio of 4:1, a mass ratio of water to NADES of 1:2, and an ultrasonication time of 60 min. Under these conditions, the thymoquinone concentration was 70.57 ± 5.78 µg/mL, closely aligning with the predicted value. The thymoquinone-rich extract obtained using NADES exhibited antimicrobial activity against Staphylococcus aureus, Staphylococcus epidermidis, and Candida albicans. In conclusion, NADES serves as an effective alternative solvent for extracting thymoquinone from black seed. Full article

Deep eutectic solvents (DESs) have undergone a remarkable transformation over the past two decades, evolving from a laboratory curiosity into one of the most actively investigated solvent platforms in green chemistry. Yet, despite this rapid expansion, and although the field is well served by numerous topical reviews, it still lacks a corpus-wide, cross-disciplinary synthesis capable of guiding strategic research priorities, identifying critical knowledge gaps, and informing policy and industrial investment decisions. The present work addresses this need through a thorough analysis of global DES research from 2003 to 2025, based on a deduplicated corpus of 17,757 publications retrieved from the Web of Science Core Collection and Scopus following PRISMA-adapted screening guidelines. The analysis maps temporal publication dynamics, geographic and institutional contributions, thematic evolution, journal landscape, component usage patterns, international collaboration networks, market projections, and alignment with the United Nations Sustainable Development Goals. The results document an exponential growth trajectory—from a single publication in 2004 to 3954 in 2025 (CAGR > 30%)—and reveal a clear thematic transition from early electrochemistry-dominated research toward extraction, pharmaceutical, and environmental applications, with machine-learning-assisted design and hydrophobic DES formulations emerging as the most dynamic current frontiers. China leads global output with 6819 publications (38.4%), while the United States and Malaysia achieve the highest citation-per-publication ratios among the leading nations (≈46.7 and ≈38.9, respectively, versus ≈27.6 for China), and Spain pairs a comparatively modest output with a high h-index, indicating that impact is large relative to volume. Type III DESs and NADESs collectively account for approximately 69% of the literature, with choline chloride present in 72% of reported formulations. The global DES market, valued at approximately USD 166 million in 2024, is projected to reach USD 370 million by 2030. Despite this progress, critical translational barriers persist: fewer than 0.3% of publications include techno-economic or life cycle assessment analysis, standardized characterization protocols remain absent, and toxicological datasets are systematically incomplete. This panoramic analysis is intended to serve as an evidence-based reference for researchers prioritizing future directions, for funding agencies assessing the maturity and needs of the field, and for industrial stakeholders evaluating the readiness of DES technologies for scale-up. Full article

This work reports the design and validation of a reusable platinum (Pt) electrode platform (ST-E) for green electrochemical analysis. The device integrates Pt working and counter electrodes with an external Ag/AgCl reference and is engineered for repeated regeneration and refunctionalization. Surface renewal by alumina polishing followed by electrochemical activation in 0.5 M H₂SO₄ restores a clean, reproducible Pt surface, as confirmed by diffusion-controlled, reversible ferricyanide voltammetry over 5–150 mV s⁻¹ with near-Nernstian peak separation and i_pa/ipc ≈ 1. Platform versatility is demonstrated in two applications. First, ST-E is functionalized with PFOA-selective molecularly imprinted nanoparticles on an APTES layer, enabling trace determination of perfluorooctanoic acid (1–5 pg mL⁻¹), with a detection limit of 0.50 pg mL⁻¹ and sensitivity of 3.16 μA (pg mL⁻¹)⁻¹. Responses correlate with an equivalently modified commercial screen-printed electrode (r = 0.990, p < 0.005), with Bland–Altman analysis confirming concordance. Second, after regeneration, electropolymerization of o-phenylenediamine yields an insulating poly(o-phenylenediamine) film that attenuates redox currents and increases ΔE_p, illustrating compatibility with diverse surface chemistries. Green metrics (AGREE, AGREEprep ≈ 0.80; BAGI = 75.0) highlight reduced waste and solvent use versus single-use transducers and compatibility with portable potentiostats, supporting circular electrochemical sensing. Full article

This study investigates the synthesis of La_0.6Ca_0.4FeO₃ (LCF) perovskite via a ball milling method for application in reverse water–gas shift chemical looping (RWGS-CL) for CO₂-to-CO conversion. Unlike conventional wet-chemical routes such as the Pechini method, the ball milling approach offers a solvent-free, scalable synthesis using low-cost metal oxide precursors (e.g., La₂O₃, CaO, Fe₂O₃). Structural analysis by XRD confirmed the successful formation of single-phase cubic perovskite, with no secondary phases when using oxide precursors. Crystallite size increased with calcination temperature, from 118.9 Å (no calcination) to 404.3 Å (1050 °C). BET analysis revealed a decrease in surface area from 2.5 m²/g (no calcination) to 0.51 m²/g (1050 °C), consistent with sintering at higher temperatures. TPR-H₂ and TPO-CO₂ studies revealed that non-calcined LCF possesses slightly enhanced redox properties, with oxygen vacancy formation and CO₂ reoxidation activity both at 500 °C. RWGS-CL experiments demonstrate that all LCF samples exhibit stable CO production (910–970 µmol/g_LCF) over multiple cycles at 500 °C, with comparable performance across calcination conditions. A cost and sensitivity analysis reveals that the ball milling method had lower synthesis costs by approximately 92% at the laboratory-scale and 88% at the industrial-scale compared to the Pechini method, highlighting its strong potential for large-scale perovskite production. Full article