Porous Silica Monoliths Research Articles

Bifunctionalised acid-base hierarchically structured monolithic microreactor for continuous-flow tandem catalytic process of cyanocinnamate synthesis

The results on zirconia-amine bifunctional modification of hierarchically porous silica monoliths for continuous-flow processes ar presented. The study reports the synthesis and properties of the modified porous monoliths and their performance in the tandem process of deacetalization-Knoevenagel condensation reaction. The properties of the materials were studied by thermal analysis, FTIR spectroscopy, XRF and nitrogen adsorption. It was found that both active centres were uniformly distributed along the monolithic cores, and the antagonistic interaction of the acid and base centres was not observed. It was shown that hydrophobicity of the monolith surface has opposite effects on the efficiency of the studied reactions. The overall rate of the tandem process depends on the rate of the condensation reaction. The performance of the bifunctional microreactors was checked and compared with those of cascade-connected monofunctional microreactors and batch reactor. The yield of cyanocinnamate product obtained in both flow systems was ca. 78%; however, pressure drop in the bimodified reactor was only half of that in the cascade. An effective way of water supply to the reaction system has been proposed. The research demonstrates the benefits of using flow-through structured micro-/mesoreactors in tandem reaction processes.

Time-of-Flight Secondary Ion Mass Spectrometry Revealing the Organocatalyst Distribution in Functionalized Silica Monoliths.

Hierarchically porous monolithic silica shows promise as a carrier material for immobilized organocatalysts. Conventional analysis usually includes physisorption, infrared spectroscopy and elemental analysis, among others, to elucidate the pore space and degree of functionalization of the material. However, these methods do not yield information about the spatial distribution of the organic species inside the monolithic reactor. In this work, time-of-flight secondary ion mass spectrometry has been applied to characterize the surface of organically functionalized silica monoliths. Cross sections of a silica monolith functionalized with 4-dimethylaminopyridine were analyzed and the results were compared with physisorption and elemental analysis experiments of the same material. This way, insight into the radial distribution of the catalyst could be achieved, which might assist in interpreting the performance of such reactors in heterogeneous flow catalysis.

Powdered Hierarchically Porous Silica Monoliths for the Selective Extraction of Scandium.

Scandium (Sc) is a high value Critical Material that is most commonly used in advanced alloys. Due to current and potential supply limitations, there has been an international effort to find new and improved ways to extract Sc from existing and novel resources. Solid-phase extraction (SPE) is one promising approach for Sc recovery, particularly for use with low-grade feedstocks. Here, unfunctionalized, powdered hierarchically porous silica monoliths from DPS Inc. (DPS) are used for Sc extraction in batch and semicontinuous flow systems at model conditions. The sorbent exhibits excellent mass transfer properties, much like the whole monoliths, which should permit Sc to be rapidly recovered from large volumes of feedstock. The Sc adsorption capacity of the material is ∼142.7 mg/g at pH 6, dropping to ∼12.0 mg/g at pH 3, and adsorption is furthermore highly selective for Sc compared with the other rare earth elements (REEs). Under semicontinuous flow conditions, recovery efficiency is limited by a kinetic process. The primary mechanism responsible for the system's slow approach to equilibrium is the Sc adsorption reaction kinetics rather than inter- or intraparticle diffusion. Overall, this unmodified hierarchically porous silica powder from DPS shows great promise for the selective extraction of Sc from various feedstocks.

Diffusion of gold nanoparticles in porous silica monoliths determined by dynamic light scattering

HypothesisThe applicability of the dynamic light scattering method for the determination of particle diffusivity under confinement without applying refractive index matching was not adequately explored so far. The confinement effect on particle diffusion in a porous material which is relevant for particle chromatography has also not yet been fully characterized. ExperimentsDynamic light scattering experiments were performed for unimodal dispersions of 11-mercaptoundecanoic acid-capped gold nanoparticles. Diffusion coefficients of gold nanoparticles in porous silica monoliths were determined without limiting refractive index matching fluids. Comparative experiments were also performed with the same nanoparticles and porous silica monolith but applying refractive index matching. FindingsTwo distinct diffusivities could be determined inside the porous silica monolith, both smaller than that in free media, showing a slowing-down of the diffusion processes of nanoparticles under confinement. While the larger diffusivity can be related to the slightly slowed-down diffusion of particles in the bulk of the pores and in the necks connecting individual pores, the smaller diffusivity might be related to the diffusion of particles near the pore walls. It shows that the dynamic light scattering method with a heterodyne detection scheme can be used as a reliable and competitive tool for determining particle diffusion under confinement.

Drying of Hierarchically Organized Porous Silica Monoliths-Comparison of Evaporative and Supercritical Drying.

In this study, we present a detailed comparison between a conventional supercritical drying process and an evaporative drying technique for hierarchically organized porous silica gel monoliths. These gels are based on a model system synthesized by the aqueous sol-gel processing of an ethylene-glycol-modified silane, resulting in a cellular, macroporous, strut-based network comprising anisotropic, periodically arranged mesopores formed by microporous amorphous silica. The effect of the two drying procedures on the pore properties (specific surface area, pore volume, and pore widths) and on the shrinkage of the monolith is evaluated through a comprehensive characterization by using nitrogen physisorption, electron microscopy, and small-angle X-ray scattering. It can clearly be demonstrated that for the hierarchically organized porous solids, the evaporative drying procedure can compete without the need for surface modification with the commonly applied supercritical drying in terms of the material and textural properties, such as specific surface area and pore volume. The thus obtained materials deliver a high specific surface area and exhibit overall comparable or even improved pore characteristics to monoliths prepared by supercritical drying. Additionally, the pore properties can be tailored to some extent by adjusting the drying conditions, such as temperature.

N-Phenyl acrylamide-incorporated porous silica-bound graphene oxide sheets with excellent removal capacity for Cr(iii) and Cr(vi) from wastewater.

The sophisticatedly altered Hummer's and sol-gel procedures were applied for the synthesis of graphene oxides and porous silica monolith particles respectively. The Fischer esterification protocol was used for coupling silica monoliths with graphene oxides. A N-phenyl acrylamide-incorporated porous polymer was synthesized at the surface of composites via reversible addition fragmentation chain transfer polymerization. The composition was confirmed by Fourier transform infra-red spectroscopy, FE-SEM, X-ray diffraction, zeta potential (zeta pH), Brunauer-Emmett-Teller (BET/BJH) analysis, and EDAX analysis. The resulting polymer-bound composite efficiently removed Cr(vi) and Cr(iii) from waste water. Adsorption parameters such as contact time, pH effect, temperature, and adsorbent and adsorbate concentration were optimized for the optimal output of the composite. The kinetic and equilibrium models were applied to the adsorption of Cr(vi) and Cr(iii) at the adsorbent surface. The maximum adsorption capacity (qe) of Cr(vi) and Cr(iii) was found to be 298.507 mg g-1 and 401.874 mg g-1, respectively, using the same initial concentration of Cr(vi) and Cr(iii) [10-60 ppm]. The adsorption data of both states of the Cr-metal followed the pseudo 2nd-order kinetic model with regression values of 0.996 ∼ Cr(vi) and 0.999 ∼ Cr(iii) at ambient temperature. Similarly, the adsorption data of Cr(vi) best fit into the Langmuir adsorption isotherm (R2 = 0.972) while that of Cr(iii) followed the Freundlich model (R2 = 0.983).

Construction of hierarchical porous 3D nanostructures with high specificity as SERS aptasensors for rapid and ultrasensitive detection of MC-LR

The construction of plasmonic nanostructures is a frontier research area in the field of Surface enhanced Raman scattering (SERS). Three-dimensional (3D) porous materials coupled with aptamers have attracted increasing attention for application in SERS sensing, owing to their great promise towards offering both high specific and ultrasensitive detection capacity. However, most of these SERS sensors are plane-shaped or solution-based, which makes target molecules with a reduced mass transfer, thus leading to a relatively poor capture efficiency. Herein, we demonstrate a capillary-based porous nanostructure coupled with aptamers that can serve as a type of SERS aptasensor for rapid trace detection. The aptasensor was prepared by immobilization of aptamer-modified SERS nanotags on a porous silica monolith which was obtained by an in-situ polymerization in a capillary with a facile fabrication process. The 3D porous silica monolith (3D-PSM) with a hierarchical biporous structure that could enable the rapid permeation of the aqueous phase and provide high specific surface area and active sites, endows the material with high capture efficiency of target molecules. Besides, according to the size of aptamers, stable and uniformed hotspots of 7–8 nm in size were formed, which precisely guaranteed the sensitivity, specificity, and stability of detection. The experimental verification showed that the proposed aptasensor could detect the presence of microcystin-LR at concentrations as low as 0.01 nmol/L, with fast recognition time (10 min), low sample consumption (20 μL), and simple operation. All the results suggest that this new strategy has promising potential in rapid microvolume trace analysis in various fields.

Preparation of polar embedded C18 stationary phase for efficient separation of peptides and proteins in high performance liquid chromatography

Peptides and proteins have great therapeutic potential, and owing to their unique biological properties, their separation is very challenging. A polar embedded C18 stationary phase was prepared by functionalization of porous silica monolith particles with N-3-(trimethoxysilyl) propyl stearamide. The stationary phase was packed in narrow bore column (100 × 2.1 mm) and evaluated for the separation of peptides and proteins in HPLC. Number of theoretical plates (N) as high as 520,000 and 340,000 plates/meter were obtained for peptides and proteins respectively. The separation performance of C18-amide column was compared with four commercial amide columns i.e. Ascentis Express RP-Amide, Accucore 150 Amide, TSKgel Amide-80, and XBridge Amide column. The performance of C18-amide column was much better than these commercial amide columns in terms of efficiency and resolution. Owing to high efficiency and good resolution for peptides and proteins separation, C18-amide column could be used as alternative to expansive commercial columns.

Monolithic Silica Microbands Enable Thin-Layer Chromatography Analysis of Single Cells.

A picoliter thin-layer chromatography (pTLC) platform was developed for analyzing extremely miniature specimens, such as assay of the contents of a single cell of 1 picoliter volume. The pTLC chip consisted of an array of microscale bands made from highly porous monolithic silica designed to accept picoliter-scale volume samples. pTLC bands were fabricated by combining sol-gel chemistry and microfabrication technology. The width (60-80 μm) and depth (13 μm) of each band is comparable to the size of single cells and acted to reduce the lateral diffusion and confine the movement of compounds along the microbands. Ultrasmall volumes (tens of pL) of model fluorescent compounds were spotted onto the microband by a piezoelectric microdispenser and successfully separated by pTLC. The separation resolution and analyte migration were dependent on the macropore size (ranging from 0.3 to 2.3 μm), which was adjustable by changing the porogen concentration during the sol-gel process. For a 0.3 μm macropore size, attomoles of analyte were detectable by fluorescence using standard microscopy methods. The separation resolution, theoretical plate number, and separation times ranged from 1.3 to 2.1, 4 to 357, and 2 to 8 min, respectively, for the chosen model biological lipids. To demonstrate the capability of pTLC for separating analytes from single mammalian cells, cells loaded with fluorescent lipophilic dyes or sphingosine kinase reporter were spotted on microbands, and the single-cell contents separated by pTLC were detected from their fluorescence. These results demonstrate the potential of pTLC for applications in many areas where miniature specimens and high-throughput parallel analyses are needed.

Experimental and modeling of tetracycline degradation in water in a flow-through enzymatic monolithic reactor.

In this work, the laccase from Trametes versicolor was immobilized in highly porous silica monoliths (0.6-cm diameter, 0.5-cm length). These monoliths feature a unique homogeneous network of interconnected macropores (20 μm) with mesopores (20 nm) in the skeleton and a high specific surface area (330 m2/g). The enzymatic monoliths were applied to degrade tetracycline (TC) in model aqueous solutions (20 ppm). For this purpose, a tubular flow-through reactor (FTR) configuration with recycling was built. The TC degradation was improved with oxygen saturation, presence of degradation products, and recirculation rate. The TC depletion reaches 50% in the FTR and 90% in a stirred tank reactor (CSTR) using crushed monoliths. These results indicate the importance of maintaining a high co-substrate concentration near active sites. A model coupling mass transfers with a Michaelis-Menten kinetics was applied to simulate the TC degradation in real wastewaters at actual TC concentration (2.8 10-4 ppm). Simulation results show that industrial scale FTR reactor should be suitable to degrade 90% of TC in 5 h at a flow rate of 1 mL/min in a single passage flow configuration. Nevertheless, the process could certainly be further optimized in terms of laccase activity, oxygen supply near active sites, and contact time.

DMAP Immobilized on Porous Silica Particles and Monoliths for the Esterification of Phenylethanol in Continuous Flow

AbstractWe report the immobilization of 4‐dimethylaminopyridine (DMAP), a versatile organocatalyst for sterically demanding esterifications, on mesoporous silica particles and macro‐mesoporous silica monoliths, both possessing optimized properties for continuous flow synthesis. An alkyne‐functionalized DMAP derivative was immobilized via click chemistry; the materials were characterized by physisorption analysis, diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) and elemental analysis. While silica particles were functionalized in batch and packed into a packed‐bed reactor, monoliths were cladded with a polyether ether ketone (PEEK) tube after sol‐gel synthesis and functionalized in a circulating flow process. Samples with three different catalyst loadings were prepared, in order to study the impact of the catalyst amount on the mesopore space as well as the catalytic performance. In continuous flow experiments, complete conversion of 1‐phenylethanol to phenylethylacetate was achieved with both materials and short contact times. Monoliths exhibited far lower pressures than packed bed reactors (7 bar at a flow rate of 1 mL min−1) and reached turnover rates up to 9.3x10−2 s−1, which is almost twice as high as a comparable batch experiment. The absence of diffusion limitations in monoliths made investigations on reaction kinetics with microkinetics‐dominated experiments possible. This study demonstrates that all properties needed for a successful transfer of immobilized organocatalysts to sophisticated flow syntheses with complex organocatalysts can be met with functionalized meso‐macroporous monoliths.

Sequestering of Radioactive Thorium from Wastewater Using Highly Porous Silica Monoliths

Sequestering of Radioactive Thorium from Wastewater Using Highly Porous Silica Monoliths

Efficient Removal of Pb(II) from Aqueous Medium Using Chemically Modified Silica Monolith.

The adsorptive removal of lead (II) from aqueous medium was carried out by chemically modified silica monolith particles. Porous silica monolith particles were prepared by the sol-gel method and their surface modification was carried out using trimethoxy silyl propyl urea (TSPU) to prepare inorganic–organic hybrid adsorbent. The resultant adsorbent was evaluated for the removal of lead (Pb) from aqueous medium. The effect of pH, adsorbent dose, metal ion concentration and adsorption time was determined. It was found that the optimum conditions for adsorption of lead (Pb) were pH 5, adsorbent dose of 0.4 g/L, Pb(II) ions concentration of 500 mg/L and adsorption time of 1 h. The adsorbent chemically modified SM was characterized by scanning electron microscopy (SEM), BET/BJH and thermo gravimetric analysis (TGA). The percent adsorption of Pb(II) onto chemically modified silica monolith particles was 98%. An isotherm study showed that the adsorption data of Pb(II) onto chemically modified SM was fully fitted with the Freundlich and Langmuir isotherm models. It was found from kinetic study that the adsorption of Pb(II) followed a pseudo second-order model. Moreover, thermodynamic study suggests that the adsorption of Pb(II) is spontaneous and exothermic. The adsorption capacity of chemically modified SM for Pb(II) ions was 792 mg/g which is quite high as compared to the traditional adsorbents. The adsorbent chemically modified SM was regenerated, used again three times for the adsorption of Pb(II) ions and it was found that the adsorption capacity of the regenerated adsorbent was only dropped by 7%. Due to high adsorption capacity chemically modified silica monolith particles could be used as an effective adsorbent for the removal of heavy metals from wastewater.

Probe tethered monolithic architectures as facile solid-state chemosensors for the on-site colorimetric recognition of Co(II) in aqueous and industrial samples

In this work, we report two novel solid-state opto-chemosensors that proffer exclusive selectivity and excellent sensitivity for the naked-eye detection of ultra-trace Co2+ ions. The opto-chemosensors are concocted using structurally engineered porous silica and polymer monolith templates that are uniformly arranged with a chromoionophoric probe i.e., (Z)-2-mercapto-5-(quinolin-8-yldiazenyl)pyrimidine-4,6-diol (AQTBA). The probe anchored monolithic opto-chemosensors induces sequential color transitions, from yellowish-orange to dark brown, with incremental addition of Co2+ ions. The optimized ground state structure of the AQTBA probe and its AQTBA-Co2+ complex are analyzed using a gaussian 16 program at B3LYP level, with a 6–311+ G (d, p) basis set. The structural and surface morphology of the opto-sensors are characterized using various microscopic, spectroscopic, and diffraction techniques, which discloses a uniform pattern of pore network that proffers rapid ion diffusion kinetics to the probe chelating sites. The proposed monolithic sensors exhibit a high degree of tolerance towards various foreign cations and anions, thus revealing its exclusive selectivity in targeting ultra-trace concentrations of Co2+. The silica and polymer monolithic sensors exhibit a broad linear response range of 0–200 ppb, with a detection limit of 0.35 and 0.07 ppb for Co2+ ions, respectively. The unique features of the proposed sensors are their faster response kinetics (120 s), greater reusability (nine cycles), excellent chemical and thermal durability (pH ≤ 12.0; T ≤ 200 °C), with reliable data reproducibility (recovery ≥99.3 %; RSD ≤2.3 %). The proposed solid-state opto-chemosensors paves way for maximum waste reduction strategy, along with the feasibility for real-time monitoring of environmental and industrial water samples.

Probe decorated porous silica and polymer monoliths as solid-state optical sensors and preconcentrators for the selective and fast recognition of ultra-trace arsenic ions

In this work, we manifested a new approach in designing solid-state colorimetric sensors for the selective optical sensing of As3+. The sensor fabrication is modulated using, (i) a cubic mesopores of ordered silica monolith, and (ii) a bimodal macro-/meso-porous polymer monolith, as hosting templates that are immobilized with a tailor-made chromoionophoric probe (DFBEP). The surface morphology and structural dimensions of the monolith templates and the sensor materials are characterized using p-XRD, XPS, FE-SEM-EDAX, HR-TEM-SAED, FT-IR, TGA, and BET/BJH analysis. The sensing components such as pH, probe content, sensor dosage, kinetics, temperature, analyte concentration, linear response range, selectivity, and sensitivity are optimized to arrive at the best sensing conditions. The silica and polymer-based monolithic sensors show a linear spectral response in the concentration range of 2–300 and 2–200 ppb, with a detection limit of 0.87 and 0.75 ppb for As3+, respectively. The real-time ion-monitoring propensity of the sensors is tested with spiked synthetic and real water samples, with a recovery efficiency of ≥99.1% (RSD ≤1.57%). The sensors act as both naked-eye optical sensors and preconcentrators, with a response time of ≤2.5 min. The molecular and photophysical properties of the DFBEP-As3+ complex are studied by TD-DFT calculations, using the B3LYP/6–31G (d,p) method.

Fabrication of target specific solid-state optical sensors using chromoionophoric probe-integrated porous monolithic polymer and silica templates for cobalt ions.

The article demonstrates the design of two solid-state sensors for the capturing of industrially relevant ultra-trace Co(II) ions using porous monolithic silica and polymer templates. The mesoporous silica reveals high surface area and voluminous pore dimensions that ensures homogeneous anchoring of 4-((5-(allylthio)-1,3,4-thiadiazol-2-yl)diazenyl)benzene-1,3-diol, as the chromoionophore. We report a first of its kind solid-state macro-/meso-porous polymer monolithic optical sensor from a monomeric chromoionophore, i.e., 2-(4-butylphenyl)diazenyl)-2-hydroxybenzylidene)hydrazine-1-carbothioamide. The monolithic solid-state sensors are characterized using HR-TEM-SAED, FE-SEM-EDAX, p-XRD, XPS, 29Si/13C CPMAS NMR, FT-IR, TGA, and BET/BJH analysis. The electron microscopic images reveal a highly ordered hexagonal mesoporous network of honeycomb pattern for silica monolith, and a long-range macroporous framework with mesoporous channels for polymer monolith. The sensors offer exclusive ion-selectivity and sensitivity for trace cobalt ions, through a concentration proportionate visual color transition, with a response kinetics of ≤ 5min. The optimization of ion-sensing performance reveals an excellent detection limit of 0.29 and 0.15ppb for Co(II), using silica- and polymer-based monolithic sensors, respectively. The proposed sensors are tested with industrial wastewater and spent Li-ion batteries, which reveals a superior cobalt ion capturing efficiency of ≥ 99.2% (RSD: ≤ 2.07%).

Porous silicon prepared from monolithic porous silica glass using a two‐step magnesiothermic reduction

AbstractMagnesiothermic reduction to convert silicon dioxide into silicon is difficult to control because the reduction often proceeds through the formation of magnesium silicide. To improve the yield of silicon, we have applied a two‐step magnesiothermic reduction to produce porous silicon from a monolithic porous silica glass substrate. At the first step, the porous silica glass substrate with pore size of approximately 40 nm was reacted with magnesium at 525°C for 6 hours, in which magnesium silicide was formed in the several tens of micrometers‐deep surface layer, while the inside of the substrate remained unreacted. Subsequently, in the second step, the product was heat‐treated at 650°C for 72 hours to produce silicon. In this step, the obtained magnesium silicide reacted with the unreacted silica glass and the intermediate products, which consist of silicon in the intermediate oxidation states generated in the first step of the reaction. The obtained silicon retained the characteristic porous structure of the initial porous silica glass. The sample also retained the monolithic shape of the initial substrate, even after being divided into several pieces. In addition, we found that periodical layered structures were generated in the course of the reduction procedure. We successfully obtained a monolithic porous silica glass sample, the surface region of which consists of porous silicon.

Porous silica and polymer monolith architectures as solid-state optical chemosensors for Hg2+ ions

We demonstrate a simple strategy to concoct a competent solid-state opto-chemosensor for the selective and sensitive visual detection of Hg2+ ions. The sensor fabrication involves the utilization of indigenously prepared mesoporous silica and polymer monoliths as probe anchoring templates and 8-hydroxy-7-(4-n-butylphenylazo) quinoline (HBPQ) as the chromo-ionophoric probe for Hg2+ sensing. Both the monoliths are designed with discrete structural and morphological features to serve as efficient host templates. The structural and surface features of the monoliths are characterized using p-XRD, TEM, SEM, SAED, EDAX, XPS, and N2 isotherm analysis. The synergetic features of monolith structural hierarchy along with the probe's selective chelating ability enable rapid signal response and remarkable ion selectivity for Hg2+. The solid-state sensors evince a linear signal response from 0.6 to 150μg/L for Hg2+ recognition, with superior data authenticity and replication that is preceded by an RSD value of ≤ 2.25% when tested with real water samples.Graphical abstract Mesoporous silica and polymer monolith architects hosting HBPQ probe molecules demonstrate an excellent visual sensing of ultra-trace (μg/L) Hg2+ in various water samples with a striking color transition from light orange to dark red upon complexation of probe with Hg2+. The solid-state sensors are Hg2+ ion selective, super-responsive, real-time applicable, and also reusable.

3D Printing of Ordered Mesoporous Silica Complex Structures.

Ordered mesoporous silica materials gain high interest because of their potential applications in catalysis, selective adsorption, separation, and controlled drug release. Due to their morphological characteristics, mainly the tunable, ordered nanometric pores, they can be utilized as supporting hosts for confined chemical reactions. Applications of these materials, however, are limited by structural design. Here, we present a new approach for the 3D printing of complex geometry silica objects with an ordered mesoporous structure by stereolithography. The process uses photocurable liquid compositions that contain a structure-directing agent, silica precursors, and elastomer-forming monomers that, after printing and calcination, form porous silica monoliths. The objects have extremely high surface area, 1900 m2/g, and very low density and are thermally and chemically stable. This work enables the formation of ordered porous objects having complex geometries that can be utilized in applications in both the industry and academia, overcoming the structural limitations associated with traditional processing methods.

Solid-state optical sensing of ultra-trace Hg2+ ions using chromoionophoric probe anchored silica monolithic architectures

In this work, we manifest the fabrication of a simple, portable, and benign solid-state sensor for the quantification of toxic Hg2+ ions through ocular colorimetric sensing. The sensor fabrication is modulated through sol-gel process using two different block-polymer surfactants (PEO and F108) for the formation of mesoporous silica monolithic designs that are immobilized with tailor-made probe molecules. The crack-free porous silica monoliths are structurally engineered to form, (i) highly ordered honey-combed 3D cubic, and (ii) disoriented worm-like mesopore structures that facilitates homogeneous probe anchoring through constrained spatial orientations for the selective detection of ultra-trace Hg2+ ions. The monolithic sensor materials are characterized by FE-SEM, HR-TEM, p-XRD, SAED, EDAX, XPS, FT-IR, TGA, and N2 isotherm analysis. For ensuring unambiguous ion-sensing, analytical parameters such as solution pH, temperature, kinetics, probe concentration, sensor quantity, linear signal response, matrix tolerance, the limit of detection (LD), and quantification (LQ) are optimized. The LD and LQ values for probe anchored PEO-MSM based sensor are 0.61 & 2.05 ppb and for probe anchored F108-MSM based sensor are 0.22 & 0.72 ppb, respectively, in the corresponding linear response range of 0−100 ppb and 0−50 ppb of Hg2+, which has been validated by real-time analysis of natural water samples.