Low NaOH Concentration Research Articles

Kinetic modeling of arabinoxylan extraction from Brewers’ spent grain using alkaline pretreatment at atmospheric pressure

This study evaluated the kinetic modeling of arabinoxylan (AX) extraction from Brewers’ spent grain (BSG) by alkaline pretreatment at atmospheric pressure, considering severe (low concentration of NaOH and high temperature) and moderate (high concentration of NaOH and low temperatures) process conditions. The effects of NaOH concentration and temperature on yield extraction were studied over time, as well as the concentration of weak acids and phenolic compounds at the end of the pre-treatment. The AX yield extraction varied from 41.2 % (1 M, 90 °C) to 64.8 % (4 M, 40 °C) after 1 h and 16 h, respectively. Acetic acid ranging from 420 ppm to 1020 ppm was released, while ferulic acid was the phenolic compound produced at the highest concentration ranging from 78.3 ppm to 224.1 ppm. In addition, rates of chemical reactions were correlated mathematically from the experimental data with a good fit, and a sensitivity analysis was performed to understand the kinetic behavior. The first-order kinetic model demonstrates that increasing AX extraction requires both low temperatures (between 30 and 40 °C) and low NaOH concentration, but at the same time, this effect increases the time required (16 h) to obtain the maximum AX yield (64.8 %).

Alkaline water electrolysis: Ultrasonic field and hydrogen bubble formation

In alkaline water electrolysis, gas bubble coverage of the electrode surface is directly linked with an increase in cell potential. Ultrasonic field presence in water electrolysis has been proven effective in removing gas bubbles from the electrode and enhancing mass transfer and bubble removal. Most studies regarding water electrolysis under sonification focused on low-concentration NaOH electrolyte solutions so there is a lack of information regarding operating conditions similar to commercial solutions. This work focused on an experimental evaluation of the effect of an ultrasonic field with a 40 kHz frequency on water electrolysis using a lab-scale electrolyser with three different KOH solutions varying in concentration (15, 25, 35% (w/w)) at 30, 40, 50, 60 °C. A reduction in cell potential was registered across all test conditions and it was maximum for 15 and 25% KOH solutions at 30 °C with 52 and 34 mV, respectively, and decreased with an increase in temperature. For a 35% KOH solution, the cell potential reduction stayed constant across all temperatures (16–19 mV). This difference was thought to be caused by the ultrasonic frequency and power and therefore required further testing. To further investigate the effect of gas bubble accumulation on the electrode surface, measurements of hydrogen bubbles’ critical diameter were taken. It was found that a higher electrolyte concentration results in a lower critical diameter (0.404, 0.356, and 0.293 mm with a 15, 25, and 35% KOH, respectively) assumed to be a consequence of higher viscosity and gas formation rate at higher concentrations.

A dilute sodium hydroxide technique for radiolarian extraction from cherts

Radiolarians have been used to determine geological ages and have contributed markedly to our understanding of Earth’s history. Hydrofluoric acid (HF) has traditionally been used to extract radiolarian fossils from siliceous deposits (i.e., radiolarian cherts), but this acid is strictly regulated because of environmental and human health concerns. Here we report on the successful extraction of radiolarians from cherts using a low-concentration NaOH solution (1 mol/L NaOH) as an alternative to HF. The degree of chert dissolution in NaOH is strongly temperature-dependent and is limited at < 80 °C. However, even a 1 mol/L NaOH solution is sufficient to dissolve chert at 100 °C. Our new NaOH method yields better-preserved radiolarian fossils compared with the conventional HF method. The 1 mol/L NaOH solution is less hazardous, easier to handle, and has fewer effects on the environment and human health than HF. Therefore, this method can be widely used for research and teaching purposes in studies of radiolarian fossils, even in institutions where HF cannot be used owing to chemical restrictions.

Optimizing crystal transitions in low-temperature, low-concentration NaOH solutions to prepare cellulose I and II composite materials

Optimizing crystal transitions in low-temperature, low-concentration NaOH solutions to prepare cellulose I and II composite materials

Alkali Extraction of Arsenic from Groundwater Treatment Sludge: An Essential Initial Step for Arsenic Recovery.

Arsenic (As)-bearing Fe(III) precipitate groundwater treatment sludge has traditionally been viewed by the water sector as a disposal issue rather than a resource opportunity, partly due to assumptions of the low value of As. However, As has now been classified as a Critical Raw Material (CRM) in many regions, providing new incentives to recover As and other useful components of the sludge, such as phosphate (P) and the reactive hydrous ferric oxide (HFO) sorbent. Here, we investigate alkali extraction to separate As from a variety of field and synthetic As-bearing HFO sludges, which is a critical first step to enable sludge upcycling. We found that As extraction was most effective using NaOH, with the As extraction efficiency increasing up to >99% with increasing NaOH concentrations (0.01, 0.1, and 1 M). Extraction with Na2CO3 and Ca(OH)2 was ineffective (<5%). Extraction time (hour, day, week) played a secondary role in As release but tended to be important at lower NaOH concentrations. Little difference in As extraction efficiency was observed for several key variables, including sludge aging time (50 days) and cosorbed oxyanions (e.g., Si, P). However, the presence of ∼10 mass% calcite decreased As release from field and synthetic sludges considerably (<70% As extracted). Concomitant with As release, alkali extraction promoted crystallization of poorly ordered HFO and decreased particle specific surface area, with structural modifications increasing with NaOH concentration and extraction time. Taken together, these results provide essential information to inform and optimize the design of resource recovery methods for As-bearing treatment sludge.

Influence of NaOH Concentration on Structural, Morphological, Optical, and Electrical Characterization of Perovskite Sodium Bismuth Titanate Prepared by Hydrothermal Method

The hydrothermal method successfully prepares a lead-free sodium bismuth titanate (NBT) perovskite film. The prepared films were studied structurally, and morphologically using X-ray diffraction, and field-emission scanning electron microscopy (FESEM), respectively. Varying the concentration of NaOH showed a noticeable effect on the properties studied. Good crystallization of NBT perovskite films without impurities was obtained at 18 and 20 M concentrations, where the crystalline size was 14 nm according to the Scherer equation. Also, when varying the concentration of NaOH, a similar film thickness was obtained through a cross-section of the FESEM images. It was observed that there was a difference in the intensity of the peaks of the photoluminescence spectra of the prepared films with a change in the concentration of NaOH, which confirms a change in the concentration of oxygen vacancies. The activation energy of the prepared films was deduced from the Arrhenius plot, as it showed small values in the films prepared with a low concentration of NaOH. The results showed that the maximum value of mobility of NBT films was at 20 M of NaOH concentration through the Hall Effect.

Low-temperature and low-concentration sodium hydroxide pretreatment for enhanced enzyme hydrolysis rate from Quercus variabilis Blume

A surface response design was employed to develop a sodium hydroxide (NaOH) pretreatment method for Quercus variabilis Blume using low NaOH concentration at low temperature. Nevertheless, the persistent issues associated with alkaline pretreatment of lignocellulose, namely high-water consumption and wastewater generation, remain prevalent in this pretreatment process. To address these challenges, this study aimed to conduct enzymatic hydrolysis of NaOH-treated Q. variabilis Blume without the intermediary washing steps. The results revealed that, following pretreatment and solid-liquid separation, NaOH-treated Q. variabilis Blume could be directly subjected to cellulase-mediated hydrolysis with pH adjustment, eliminating the need for washing steps. The maximum enzymatic hydrolysis efficiency reached 95.9% under specific conditions (1.2% NaOH, 8.9 °C, 32.1 h). This approach offers a promising avenue to enhance the enzyme hydrolysis rate of NaOH-treated lignocellulose. Notably, the low-temperature and low-concentration NaOH treatment effectively removed a substantial portion of lignin and hemicelluloses, resulting in a higher crystallinity index of the cellulose-rich residue compared to substrates treated solely with steam explosion. The integration of direct pretreatment and alkaline treatment emerges as an environmentally friendly and economically viable method for producing glucose and high-purity lignin. The obtained lignin can be further transformed into high-value products within the biorefinery framework.

Elucidating the structural changes of cellulose molecules and dynamics of Na ions during the crystal transition from cellulose I to II in low temperature and low concentration NaOH solution

Low-concentration alkali treatments at low temperatures facilitate the crystal transition of cellulose I to II. However, the transition mechanism remains unclear. Hence, in this study, we traced the transition using in situ solid-state 13C CP/MAS NMR, WAXS, and 23Na NMR relaxation measurements. In situ solid-state 13C CP/MAS NMR and WAXS measurements revealed that soaking cellulose in NaOH at low temperatures disrupts the intramolecular hydrogen bonds and lowers the crystallinity of cellulose. The dynamics of Na ions (NaOH) play a crucial role in causing these phenomena. 23Na NMR relaxation measurements indicated that the Na-ion correlation time becomes longer during the crystal transition. This transition requires the penetration of Na ions (NaOH) into the cellulose crystal and a reduction in Na-ion mobility, which occurs at low temperatures or high NaOH concentrations. The interactions between cellulose and NaOH disrupt intramolecular hydrogen bonds, inducing a conformational change in the cellulose molecules into a more stable arrangement. This weakens the hydrophobic interactions of cellulose, and facilitates the penetration of NaOH and water into the crystal, leading to the formation of alkali cellulose. Our findings suggest that a strategy to control NaOH dynamics could lead to the discovery of a novel preparation method for cellulose II.

Construction of C8/threonine-functionalized mesoporous silica aerogel based on mixed-mode and its adsorption properties for both anionic and cationic dyes

High adsorption and desorption efficiencies for both anionic and cationic dyes are still a challenge for adsorbents to treat dyestuffs wastewater. In this study, the C8/threonine-functionalized mesoporous silica aerogel based on mixed-mode was constructed to overcome the challenge, with properties of hydrophobicity and switchable surface charge of n-octyl and threonine groups. With methylene blue and azophloxine as cationic and anionic dye models, batch tests were conducted. The consequences proofed the adsorption process was efficient and fast, and the highest adsorption quantities for methylene blue and azophloxine were estimated as 274.30 mg/g and 152.43 mg/g, respectively. Additionally, the adsorbent showed good removal efficiency and reusability. The desorption efficiencies exceeded 97% using low concentration HCl or NaOH as eluents. Mechanism investigation proved that adsorption process relied on hydrophobicity and electrostatic interactions. These results instructed that SG-C8/Thr was a promising adsorbent with excellent adsorption and desorption efficiencies for both anionic and cationic dyes.

Effect of GGBFS and fly ash proportions on fresh, tensile and cracking features of alkali activated concrete with low NaOH concentrations

This study mainly investigated the tensile and cracking features of ash alkali activated concrete with different slag-fly ash proportions and low NaOH concentrations cured at ambient temperature. High-molarity NaOH leads to risk and is costly, whereas, in field conditions, heat curing is difficult. Therefore, in this study three mixes (mix-A, B and C) were developed using 0/100, 20/80, 40/60, 60/40, 80/20, and 100/0 slag-fly ash proportions in this study. Sodium hydroxide (SH) and sodium silicate (SS) were used as activators and concentrations of sodium hydroxide were used as 1M, 2M and 4M in mixes A, B and C respectively, but alkaline ratio (SS/SH) was fixed as 1.5 in all the mixes. Slump, and strength aspects (compressive, split tensile, and flexural) were evaluated. The tensile (tensile strength, tension stiffening) and cracking characteristics (crack spacing, crack width) were evaluated under uniaxial tensile loading on reinforced prismatic members. From test outcomes, workability in terms of slump of the composites decreased with increased percentage of slag or granulated blast furnace slag (GGBFS) in the total binder, but the tensile (tensile stress and tension stiffening effect) and compressive strengths increased with increasing percentage of GGBFS. Better cracking properties (i.e., minimum crack widths and reduced crack spacings) were observed when the mixes contained higher percentages of GGBFS. The obtained crack spacings were correlated with CEB-FIP model code, and existing research studies. The crack spacings obtained in this study are consistent with CEB-FIP model code. Finally, this study demonstrated that when slag-fly ash alkali activated concretes were prepared with solutions containing low NaOH concentrations and cured at room temperature (ambient), there was an increase in the strength and cracking properties with higher percentages GGBFS.

Experimental study on the mass transport characteristics of dilute iodine vapor from air to caustic soda solution in a packed column using different packing materials

It is imperative to minimize radioiodine release to the environment through gaseous emissions of spent fuel reprocessing facilities, thereby mitigating its potential impact on the general public. One effective and widely adopted strategy for achieving this objective is caustic scrubbing, a method that involves the absorption of molecular iodine from gaseous streams using caustic soda ( NaOH ) solution in a packed column. In-depth laboratory-scale experiments were conducted to ascertain the overall volumetric mass transfer coefficient K G a for the absorption of dilute iodine vapor from air into a caustic soda solution in a packed column and to establish optimum performance parameters for this process. The investigation yielded noteworthy findings: K G a increased proportionately to (Gas phase Reynolds number)1.0 at constant liquid flow rates across all types of packing tested. K G a displayed relative independence from liquid velocities for high and moderate NaOH concentrations. However, this coefficient varied proportionately to (Liquid phase velocity)0.26 to 0.42 at lower NaOH concentrations under conditions of high gas flow rates NaOH . As the height of the column increased, K G a was found to decrease slightly. The presence of NOx at an inlet concentration of 9000 ppm in the gaseous stream led to a reduction in the mass transfer coefficient of iodine, particularly at low NaOH concentrations. In summary, the study underscores the importance of caustic scrubbing as an effective means to minimize the release of radioiodine. The investigation’s results provide valuable insights into optimizing performance parameters for this process, contributing to enhanced environmental protection.

Mitigation Measures of Swelling Characteristics in Alkali-Contaminated Red Earth using Fly Ash and GGBS Blends

Alkali contamination induces swelling in the inherently non-swelling soils, resulting in heave severely damaging the sub and superstructures. Stabilization measures must be taken in vulnerable areas to prevent such colossal losses. Considerable research has been conducted regarding the swelling behavior of soils contaminated with alkalis and the impact of subsequent stabilization techniques utilizing different industrial byproducts and pozzolanic materials. However, there is a paucity of such studies on the Red Earth (RE) of the Visakhapatnam region. Furthermore, limited attention was given to the effects of extremely low concentrations of alkalis on the swelling behavior of soils. RE in the study area of the Visakhapatnam region predominantly consists of quartz, kaolinite, and hematite. In phase 1 of the experimental analysis, RE was contaminated with a highly dilute NaOH solution (0.05 N), and the resulting swell characteristics were investigated. A free swell of 10% was observed. One-dimensional standard oedometer tests revealed an equilibrium swelling of 5.6%, indicating significant potential for substantial heave and subsequent damage. X-ray diffraction (XRD) analysis revealed the formation of natrolite and analcime zeolites with a hollow structure, which caused the swell. Peaks of silicate minerals like paragonite and ussingite were also observed, indicating the dissolution of authigenic minerals and new precipitations even at lower concentrations of NaOH. In phase 2, swell tests were conducted on a mixture of contaminated red earth (50% w/w), fly ash (25% w/w), and ground granulated blast furnace slag (GGBS, 25% w/w), and it was observed that the swelling was completely arrested. XRD analysis unveiled that even though siliceous zeolites were formed, the development of chrysotile, attapulgite, tobermorite, and dicalcium silicate effectively inhibited the swelling with their pozzolanic behavior.

Anomalous Temperature-Induced Particle Size Reduction in Manganese Oxide Nanoparticles.

The intricate role of temperature in the structure-property relationship of manganese oxide nanoparticles (Mn3O4 NPs) remains an open question. In this study, we successfully synthesized Mn3O4 NPs using the hydrothermal method with two differing temperatures, namely, 90 and 150 °C. Interestingly, a smaller average particle size is found when Mn3O4 NPs are synthesized at 150 °C compared to 90 °C, corresponding to 46.54 and 63.37 nm, respectively. This was confirmed by the time variation of temperature setting of 150 °C where the size evolution was insignificant, indicating a competing effect of nucleation and growth particles. Under varying NaOH concentrations (2-6 M) at 150 °C, a reduction in the particle size is found at the highest NaOH concentration (6 M). The particle grows slightly, indicating that the growth state is dominant compared to the nucleation state at low concentrations of NaOH. This finding implies that the high nucleation rate originates from the excessive monomer supply in the high-temperature reaction. In terms of crystallinity order, the structural arrangement of Mn3O4 NPs (150 °C) is largely decreased; this is likely due to a facile redox shift to the higher oxidation state of manganese. In addition, the higher ratio of adsorbed oxygen and lattice oxygen in Mn3O4 NPs at 150 °C is indirectly due to the higher oxygen vacancy occupancies, which supported the crystallinity decrease. Our findings provide a new perspective on manganese oxide formation in hydrothermal systems.

Study on the deacetylation and mechanism of chitin in natural deep eutectic solvent

A large number of hydrogen bonds is the main reason for hindering the dissolution and reaction of chitin, and a mild and green deacetylation method to prepare chitosan for a wider range of applications is urgent. As a non-toxic and degradable green solvent, the deep eutectic solvent can effectively interfere with the hydrogen bond network of chitin, making chitin more susceptible to other solvents. Therefore, a NADES system consisting of betaine and glycerol was proposed for application in the deacetylation reaction of chitin to facilitate further attack of N-acetyl groups by low concentrations of NaOH. After optimizing the reaction conditions, chitosan with 83.77 % deacetylation was prepared, requiring only a concentration of 25 wt% NaOH. The analysis of the product chitosan showed that NADES could not only effectively improve the degree of deacetylation, but also reduce the degree of damage to the molecular weight by alkali. In addition, the potential mechanisms involved in the deacetylation process by NADES were explored. The nature of the reaction was verified by FT-IR, XRD and theoretical calculations as the process of opening intra/intermolecular hydrogen bonds of chitin by NADES. More importantly, experimental and in-depth theoretical studies provide a reference for the green preparation of chitosan.

Mineral phase evolution and heavy metals migration during the hydrothermal treatment of municipal solid waste incineration fly ash

The solidification of heavy metals in the municipal solid waste incineration fly ash was realized by the hydrothermal treatment with mineral additives added. The experimental results showed that the addition of SiO2 at 200 °C with the NaOH concentration was 0.5 mol/L attributed to the formation of fibrous tobermorite and effectively reduced the heavy metals toxicity of hydrothermal products, especially Pb and Cu. When SiO2 and Al2O3 were both introduced, the generated katoite and sodalite showed a better curing effect on Zn at lower NaOH concentrations. Further, the dynamic correlation between the tobermorite formation and heavy metals solidification was explored. It was found that the heavy metals in fly ash were first dissolved into the alkaline liquid phase and then transferred into the solid phase as the treatment proceed. The solidification of Pb which finished before 8 h was mainly due to the encapsulation of the tobermorite precursor before crystallization, while that of Cu which lasted over 48 h mainly relied on the adsorption and cation exchange effect caused by the formed tobermorite. Therefore, selecting the appropriate mineral addition scheme and hydrothermal time according to the fly ash components and heavy metals categories can effectively improve the curing cost performance.

Effect of electric field on the wetting behavior of GaInSnBiZn high-entropy alloy in NaOH aqueous solution

The GaInSnBiZn low-melting-point high-entropy alloy exhibits promising prospects for utilization in the realm of flexible electronic devices, offering a promising alternative to common binary or ternary room-temperature liquid metals. By utilizing the sessile drop method, the wetting behavior of GaInSnBiZn/SiO2 was investigated, focusing on the effects of applied voltage and NaOH solution concentration. It was revealed that the alloy's electro-wetting is primarily influenced by the generation and dissolution of the surface oxide layer, as well as the interaction of the electric double-layer effect. The optimal response voltages for achieving the fastest wetting rate were found to be 16 V, 10 V, 18 V, and 8 V in 0.5 mol/L, 1.0 mol/L, 1.5 mol/L, and 2.0 mol/L concentrations, respectively, with 18 V at 1.5 mol/L concentration identified as the optimal process selection. The spreading behavior of the alloy in low-concentration NaOH solutions followed Tanner's Law, while in the 2.0 mol/L concentration, significant repellence and wetting angle saturation were observed. The wetting process of the alloy at various stages was described using the power-law equation R = atc, while the wetting mechanism of the alloy was elucidated through the application of the Lippmann equation and the electric double-layer effect equation.

Structural and emulsion-stabilizing properties of the alkali-extracted arabinoxylans from corn and wheat brans

This study investigated the structural and emulsion-stabilizing capacities of alkali-extracted arabinoxylans from corn and wheat bran (CAXs and WAXs). The results demonstrated that all AXs were mainly composed of arabinose and xylose. WAXs had a higher weight-average molecular weight (Mw, 375–473 KDa) and protein content (3.09–8.68 %) but lower total phenolic acid content (TPC, 1.18–1.91 mg gallic acid equivalents/g) than CAXs; however, CAX stabilized emulsions exhibited smaller and more regular oil droplet size (524–589 nm) and higher absolute value of ζ potential (48–52 mV) compared with WAX stabilized emulsions during storage. Moreover, the increment of NaOH concentration caused a decrease in Mw, protein content, and TPC of CAXs or WAXs and the corresponding CAXs or WAXs emulsions showed bigger and more unstable oil droplets during 14 d storage. The Mw, protein, and TPC were well correlated with their emulsion stability. Furthermore, emulsions stabilized by AXs with low-concentration NaOH could resist better various temperatures, pH, and NaCl. In conclusion, the structural properties of AXs derived from different cereal sources and treated with different concentrations of NaOH varied, leading to differences in their ability to stabilize emulsions. CAXs or WAXs obtained from low-concentration NaOH treatment demonstrated significant potential as highly effective natural emulsifiers.

Effect of desilication process on natural zeolite as Ni catalyst support on hydrodeoxygenation of palm fatty acid distillate (PFAD) into green diesel

Natural zeolite (NZ) from desilication and activation was prepared to support the Ni catalyst. The catalyst was utilized for the hydrodeoxygenation (HDO) of the palm fatty acid distillate (PFAD) into green diesel. Desilication using sodium hydroxide (NaOH) solution increases the porosity, surface area, and acidity of the natural zeolite, thus increasing the catalytic activity. This study aims to determine the effect of the NaOH concentration utilized in the desilication process on the characteristics of support and catalytic activity of the Ni/NZ catalyst. Additionally, pure Ni and Ni/NZ without desilication were also investigated for comparison. NZ underwent desilication by varying the concentration of NaOH (0.5, 1, and 2 N). Desilicated zeolite was then activated using a 1 M ammonium acetate solution and impregnated with Ni metals. The desilication NZ increases the acidity and surface area at a low NaOH concentration, while the zeolite structure (clinoptilolite) is still intact. Therefore, the catalytic activity of the catalyst was also increased compared to Ni and Ni/NZ catalysts without desilication. Conversely, a higher concentration of NaOH decreases the Si/Al ratio, acidity, and surface area of support. As a result, the catalytic activity of the catalyst decreases, as evidenced by the reduced liquid product in the hydrodeoxygenation of PFAD. The Ni/NZ0.5 catalyst revealed optimal catalytic activity with a liquid fraction and green diesel selectivity of 83.64% and 92.74%, respectively.

The sponge effect of phosphogypsum-based cemented paste backfill in the atmospheric carbon capture: Roles of fluorides, phosphates, and alkalinity

The use of cement for solid waste solidification/stabilization is one of the most practised methods but is under scrutiny due to its substantial emission of greenhouse gases. However, the dual role of cement-immobilized solid waste may serve as a CO2sink and promisingly reabsorb a great content of atmospheric CO2, which is hitherto unexplored. In this study, we detail the inherent potential sponge effect of phosphogypsum (PG) based cemented paste backfill (PCPB), finding that, at a high PG utilization rate, the PCPB application may produce 16.7 Mt/year of CO2 in China, whereas a reduction of 5.76 Mt/year could promisingly reach up when considering the future reabsorption. However, industrial applications are limited by the remained impurities and the maintenance of alkalinity. The results suggest that the phosphate impurities within PG have an adverse effect on CO2 uptake, which inhibits the precipitation of hydration products and inversely favors the formation of calcium-phosphate species that retard the dissolution of cement particles. By contrast, the fluorides imply an acceleration of the hydration reactions and accordingly hasten the carbonation process. Furthermore, geochemical modeling suggests that maintaining a basic pH condition of the system is another significant factor in promoting the CO2 capture capacity, of which a 35% increase in CO2 uptake can be acquired with a continuous low concentration NaOH supply, but this enhancement will require the widespread deployment of future validation. From the perspectives of CO2 balance, environmental requirements, and technological feasibility, PCPB is an effective way for in situ immobilizing PG with scalable potential. These new observations are expected to provide a deeper understanding and reliable guidance for the sustainable management of dumped PG and the zero emissions of the phosphorus fertilizer industry.

FORMACIÓN DE NANOPARTÍCULAS DE PALADIO POR EL MÉTODO DE LOSPOLIOLES: INFLUENCIA DE LAS CONDICIONES ALCALINAS

The effect of sodium hydroxide (NaOH) on the size of palladium (Pd) nanoparticles obtained by the simple polyol route was studied. Nanoparticles were synthesized at room temperature using palladium(II) chloride (PdCl2) and NaOH dissolved in ethylene glycol (EG) as reduction reaction promoters. No protective agents or stabilizers were used. We monitored the reaction kinetics and the growth of the nanoparticles by UV-vis spectroscopy and their crystallinity by powder X-ray diffraction (XRD) as a function of NaOH concentration. Crystallite size was evaluated from the diffraction pattern. We found that nanoparticle growth is strongly influenced by the NaOH: Pd molar ratio. Crystallite sizes from 2 to 24 nm were obtained for molar ratios ranging from 1 to 33. At lower concentrations of NaOH, the nucleation and growth process of the nanoparticles were found to be controlled by the reduction of the Pd ion precursors.At higher concentrations, the intermediate reduction of Pd-Cl-OH species determines the nanoparticle growth rate resulting in the formation of the smallest final-size nanoparticles.