A Novel Microextraction Technique for Pb(II) Ion Preconcentration Using 3-Mercapto Propyltrimethoxysilane- Modified Glass Powder

A Novel Microextraction Technique for Pb(II) Ion Preconcentration Using 3-Mercapto Propyltrimethoxysilane- Modified Glass Powder | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article A Novel Microextraction Technique for Pb(II) Ion Preconcentration Using 3-Mercapto Propyltrimethoxysilane- Modified Glass Powder Sorour karimi, Soleiman Bahar, Parisa Poormoghadam This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7232218/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Accurate measurement of lead (Pb) in water samples is critical because of its high toxicity and potential to accumulate in living organisms, leading to serious health risks such as anemia, kidney damage, and neurological disorders. This study introduces a novel microextraction technique for the preconcentration of Pb(II) ions using glass powder modified with 3-mercaptopropyltrimethoxysilane (MPTMS-GP). The MPTMS-GP adsorbent was synthesized via surface modification and characterized using Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The Pb(II) extraction efficiency was optimized using the microextraction in a packed syringe (MEPS) technique, with graphite furnace atomic absorption spectrometry (GFAAS) for quantification. The optimal conditions for Pb(II) extraction were five extraction cycles, a pH of 6, 2 mg of adsorbent, 100 µL of 1 M hydrochloric acid for elution, and a sample volume of 4 mL. The method demonstrated a limit of detection (LOD) of 0.0013 ng/mL and a linear range of 0.01–50 µg/L, showing excellent sensitivity. The MPTMS-GP adsorbent exhibited remarkable selectivity for Pb(II), achieving recovery rates between 97.9% and 103.6% in real samples, such as water, vegetables, and cosmetics. The preconcentration factor was calculated to be 35.95, indicating the method’s efficiency. This approach offers a highly effective, precise, and eco-friendly solution for the extraction and quantification of Pb(II) in environmental and biological sample. Physical sciences/Chemistry Earth and environmental sciences/Environmental sciences Pb(II) preconcentration microextraction in a packed syringe MPTMS-modified glass powder atomic absorption spectrometry lead environmental analysis Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Introduction Heavy metals can cause serious damage to vital human body functions at high concentrations because of their toxicity. Hazardous metals such as lead, copper, nickel, cadmium, and mercury can enter the body through food consumption, inhalation, or dermal absorption [ 1 – 3 ]. Although lead (Pb) is among the most hazardous heavy metals, it is widely utilized in the industry for making batteries, pigments, catalysts, and alloys [ 4 ]. Pb(II) is dispersed in the environment through various chemical pollutants and has the potential to enter the food chain. This metal has a strong tendency to accumulate in the bodies of living organisms, and its accumulation, especially in the bone marrow, can lead to life-threatening diseases such as anemia, kidney and brain damage, paralysis, miscarriage, and behavioral disorders [ 5 , 6 ]. Therefore, the accurate and sensitive determination of Pb(II)in water is necessary. To measure heavy metals such as lead, atomic absorption spectrometry is a common choice in laboratories because of its simplicity and cost-effectiveness. However, when the concentration of metals is very low (at the µg l –1 level), the use of flame atomic absorption is not practical because of its low sensitivity and interference from other elements present in the sample [ 7 – 9 ]. To address this issue, separation and preconcentration methods such as cloud point extraction [ 10 ], ion exchange [ 11 ], electrocoagulation [ 12 , 13 ], liquid-liquid extraction [ 14 , 15 ], electrodeposition [ 16 ], dispersive liquid-liquid microextraction [ 17 , 18 ], solid-phase extraction [ 19 , 20 ], and dispersive micro-solid-phase extraction [ 21 , 22 ] have been developed for the preconcentration of Pb(II). Solid-phase extraction (SPE) is popular among researchers because of its simplicity, speed, ease of compatibility with pre-concentration, and ability to integrate with flow injection analysis (FIA) techniques for measuring trace metals. This method also offers a high enrichment factor and enables the processing of large sample volumes without sample contamination. For these reasons, SPE is widely used for the preconcentration and separation of organic and inorganic species at low and ultralow concentrations, enhancing the sensitivity of analytical methods and eliminating interference from the sample matrix [ 23 , 24 ]. Investigating the efficiency of new and economically viable materials as solid-phase extractors is a key aspect of research on the solid-phase extraction of transition metals at low concentrations. Waste glass is an abundant material derived from municipal solid waste (MSW) or construction debris and can be regarded as a low-cost adsorbent compared to expensive commercial adsorbents such as activated carbon or zeolites. Collecting glass waste contributes to environmental preservation because glass is non-biodegradable and persists in the environment for long periods. Glass surfaces are well-suited for adsorption applications because they are composed of various oxides, such as SiO 2 , Al 2 O 3 , CaO, and Na 2 O. When these oxides come into contact with water, they form reactive surface hydroxyl groups, such as Si–OH, which serve as active sites that can adsorb heavy metal ions such as Pb(II), Cd(II), and Ni(II) [ 25 , 26 ]. Another benefit of glass powder is its ability to become porous, with its specific surface area being enhanced through either chemical or thermal processes. The adsorption capacity of waste glass can be significantly improved by altering its surface using methods such as acid activation, hydrothermal treatment, calcination, and the application of pore-forming agents [ 25 , 27 ]. For example, it has been shown that waste glass possesses a large specific surface area (about 557.912 m 2 /g) and very small pore diameter (2.099 nm), which contribute to its remarkable adsorption capacity [ 26 ]. In another study, the maximum adsorption capacity for metal ions such as Pb 2+ was reported to be as high as 11.68 mg/g, indicating the high efficiency of these materials in removing heavy metals [ 28 ]. The economic and environmental aspects of using glass powder as an adsorbent are also significant, as recycling and reusing waste glass not only results in economic savings but also reduces the negative impacts associated with landfilling glass at disposal sites [ 26 , 27 , 29 ]. The high stability of glass allows glass-based adsorbents to be regenerated and reused over several cycles. Adsorption on glass surfaces often involves ion exchange (for example, Na + and Ca 2+ ions present in the glass are replaced by heavy metal ions), physisorption, electrostatic interactions, and surface complexation. Ion exchange plays an important role in heavy metal removal [ 25 – 28 , 30 ]. Various adsorbents have been used for the extraction and preconcentration of Pb(II) ions in water, including natural adsorbents such as agri-waste biosorbents [ 31 ], natural bentonite [ 32 ], agricultural wastes [ 33 ], carbon-based adsorbents such as activated carbon [ 34 ] and graphene oxide [ 35 ], inorganic adsorbents such as functionalized Fe 3 O 4 [ 36 ], TiO 2 nanocomposites [ 37 ], metal-organic frameworks [ 38 ], ion-imprinted polymers [ 39 ], and others. The efficiency of adsorbents in binding metal ions is attributed to their ability to form complexes between the ligands present on the adsorbent surface and the metal ions. The selectivity of a specific ligand toward the target metal ion results from conventional acid-base interactions between the two [ 40 ]. Therefore, an ideal adsorbent should possess the highest possible specific surface area and allow easy surface chemical modification. Nanoparticles, with their elevated specific surface areas, serve as an outstanding platform for adsorbing heavy metals. Moreover, the functional groups present on the surface of the nanoparticles play a crucial role in the selectivity of the adsorbent because of the affinity between these groups and the target molecules [ 41 ]. Functionalization of the glass powder surface with thiol groups (–SH) via modification with mercapto propyltrimethoxysilane (MPTMS) is critical for the preconcentration of Pb(II) in solution for several reasons. First, thiol groups (S-H) can effectively remove these pollutants from aqueous solutions because of their high binding affinity for heavy metal ions (e.g., lead). Thiol groups create specific ionic interactions with soft Lewis acids, including mercury (Hg(II)), cadmium (Cd(II)), and lead (Pb(II)) ions [ 42 , 43 ]. Surface modification of glass powder leads to a significant increase in its surface area, which enhances the number of active binding sites and consequently boosts its adsorption capacity for heavy metals [ 44 ]. Additionally, the hydrophobicity imparted by MPTMS on the glass inhibits the adsorption of water molecules onto the active sites, thereby improving the efficiency and selectivity of heavy metal removal. Furthermore, the unique properties of MPTMS-modified glass can be leveraged to design and fine-tune it for specific applications in heavy metal removal [ 45 ]. This study assessed the effectiveness of glass powder treated with 3-mercaptopropyl trimethoxysilane (MPTMS), noted for its excellent sensitivity and selectivity, as a straightforward adsorbent for the separation and measurement of Pb(II) ions. The method employed microextraction using the packed syringe (MEPS) technique, which was paired with detection using graphite furnace atomic absorption spectrometry (GFAAS). The physical and chemical properties of raw GP and MPTMS-GP were characterized using Fourier Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDAX), X-ray Diffraction (XRD), and Thermogravimetric Analysis (TGA). The variables influencing Pb(II) extraction efficiency were investigated and optimized in this study. Finally, the MPTMS-GP adsorbent was used to extract and quantify Pb(II) in real-world samples, including vegetables, cosmetic products, and water from Lake Zriwar. Materials and Equipment Materials All chemical materials used were of analytical grade. Nitric acid (HNO 3 , 65%), hydrochloric acid (HCl, 37%), sulfuric acid (H 2 SO 4 , 98%), glacial acetic acid (CH 3 COOH), hydrogen peroxide (H 2 O 2 , 30% v/v), sodium hydroxide (NaOH, in tablet form), tetraethyl orthosilicate (TEOS, C 8 H 20 O 4 Si), and 3-mercaptopropyl trimethoxysilane (MPTMS, C 6 H 16 O 3 SSi) were all obtained from Merck (Germany). A Pb(II) standard stock solution with a concentration of 1000 mg/L was prepared by dissolving an appropriate amount of lead nitrate (Pb(NO 3 ) 2 , Merck) in dilute nitric acid. Instruments An accurate AXIS digital balance (model ALN220, Spotka, Poland) with a precision of 0.1 mg was used to weigh the sample. Quantitative Pb(II) measurement was performed using a Varian/Agilent atomic absorption spectrometer model SpectrAA 220 equipped with a GTA 110 graphite furnace (GFAAS). Material characterization analyses included recording FTIR spectra with a Bruker Vector 22 instrument (in the range of 4000 − 400 cm –1 ), surface morphology and elemental composition examination by field emission scanning electron microscopy (FESEM) model TESCAN Mira 3-LMU (with 30 kV voltage and equipped with EDX analyzer), crystal structure determination with X-ray diffraction (XRD) model Rigaku Ultima IV (Japan), and thermal analysis with TGA model PerkinElmer STA6000 (USA). Additionally, an RST16 centrifuge (made in Iran, 5000 rpm) and an ultrasonic bath (Spectron) were used in the various stages of sample preparation and processing. Glass powder (GP) preparation Glass powder (GP) was prepared by crushing clean glass capillary tubes using a porcelain mortar. The resulting powder was subsequently mixed with tetraethoxysilane (TEOS), and the mixture was agitated with a magnetic stirrer for 12 h. This process facilitated TEOS hydrolysis and increased the number of surface hydroxyl (Si-OH) groups. The solid product was separated by centrifugation and washed repeatedly with distilled water. The final activated glass powder was dried in an oven at 60–70°C after separation. Synthesis of Glass Powder Modified with 3-Mercaptopropyltrimethoxysilane (GP-MPTMS) The surface modification of the glass powder with 3-mercaptopropyltrimethoxysilane was performed according to the method shown in the diagram, adapted from a previous study [ 46 ]. First, a silane hydrolysis solution was prepared by adding 40 µL of MPTMS to 100 mL of a water/ethanol mixture (volume ratio of 9:1). The pH of the resulting solution was adjusted to the range-3-4 using acetic acid. Then, 0.5 g of the activated glass powder (prepared in the previous step) was added to the silane solution. The resulting suspension was placed in a water bath at 60–70°C for 30 min under continuous stirring. The initial solid product was separated by centrifugation and dried for 4 h at 110°C in an oven. To remove unreacted materials and weakly bonded silanes, the dried powder was immersed in deionized water for 24 h. The solid was then purified through successive cycles of centrifugation and washing with distilled water. Finally, the MPTMS-modified glass powder (GP-MPTMS) was completely dried for 24 h in an oven at 110°C after separation (See Scheme 1 for details of the synthesis steps). Calibration Curve For the calibration curve (Fig. 1 ), a standard lead nitrate solution with an initial concentration of 1000 ppm was employed. A sequence of standard solutions at varying concentrations was prepared by diluting the stock solutions. The optical absorption of each standard was measured using a spectrophotometer. A standard calibration curve for Pb(II) was established over a concentration range of 0.000001–2 ppm, facilitating the determination of unknown sample concentrations. Preparation of Real Samples Water Water samples collected from Lake Zarivar were filtered using 0.48 micrometer membrane filters. After pH adjustment, the filtered samples were directly subjected to extraction and analysis, without further preparation. Vegetables Samples of commonly consumed vegetables, including parsley (Petroselinum crispum), lettuce (Lactuca sativa), leek (Allium ampeloprasum), basil (Ocimum basilicum), and coriander (Coriandrum sativum), were selected for the analysis [150, 151]. Initially, fresh vegetable samples were meticulously rinsed with tap and distilled water. Subsequently, the samples were placed in an oven set to 120°C until they reached a stable weight. Each dried vegetable sample (10 g) was accurately weighed and transferred to a beaker for further analysis. For wet digestion, 100 mL of concentrated nitric acid (HNO 3 ), 20 mL of hydrogen peroxide (H 2 O 2 , 30% v/v), and 30 mL of deionized water were added to each beaker. The mixture obtained was heated at 80°C for a duration–20–30 minutes. Once cooled to room temperature, the mixture was filtered using a Whatman No. 42 filter paper. The filtered solution was slowly transferred to a 250 mL volumetric flask and diluted with deionized water. Next, 20 mL of this stock solution was placed in a 100 mL volumetric flask and brought up to the mark with distilled water. The pH of the resulting solutions was adjusted prior to extraction and analysis [ 47 , 48 ]. Lipstick The sample preparation process for lipstick analysis was performed according to a reference method [ 49 ] with minor modifications. For this purpose, 0.5 g of the lipstick sample was carefully weighed and transferred to a digestion beaker. Subsequently, 30 mL of concentrated nitric acid (HNO3) and 10 mL of concentrated hydrochloric acid (HCl) were introduced into the sample. The mixture was subjected to a controlled heating program: initially, the temperature was held at 130°C for 15 min, after which it was elevated to 200°C and maintained for 35 min. Once this stage was finished and the contents had cooled to approximately 50°C, 100 mL of a 4% (w/v) boric acid solution (H3BO3) was introduced. The mixture was subsequently maintained at 180°C for 15 min. Once it was fully cooled to ambient temperature, the solution was transferred to a 250 mL volumetric flask and diluted using deionized water. Subsequently, 20 mL of this solution was transferred to a 100 mL volumetric flask and diluted to the mark using deionized water. The pH of the resulting solution was adjusted before extraction and analysis. Rice A rice sample from Iran was used in this study. Initially, the rice grains were washed with distilled water, followed by drying in an oven set at 105°C for 48 h. The desiccated samples were finely pulverized using a laboratory mill. A precise amount of rice powder (0.5 g) was measured and placed in a digestion flask. The wet digestion process was initiated according to a method by adding 4 mL of concentrated sulfuric acid (H 2 SO 4 ) [ 50 ]; the mixture was gently heated for 3–5 min until it reached the boiling point. After this initial stage, 16.5 mL of hydrogen peroxide (H 2 O 2 ) (30% v/v) was gradually and carefully added to the flask until the solution became completely clear. Heating was continued for 1 min after the solution became clear. Once the solution was cooled to ambient temperature, it was passed through a Whatman No. 42 filter paper into a 100 mL volumetric flask. The solution was then topped up with distilled water for further analysis. Measurement in Real Samples Extraction was performed using a standard 1 mL MEPS syringe. Approximately 2 mg of MPTMS-GP adsorbent was manually placed between two porous polymer frits at the terminal section of the syringe barrel (near the needle) to form a packed bed. The compaction was adjusted to prevent adsorbent leakage and channeling while allowing easy solution passage. Prior to the first extraction, the adsorbent bed was conditioned by passing 4 mL of deionized water through it. A total of 4 mL of the sample solution was processed through the adsorbent bed for analyte extraction by conducting five consecutive draw and eject cycles with a syringe. Following sample loading, the adsorbent bed was washed with 2 mL of deionized water to eliminate any possible matrix interferences. The elution stage of the adsorbed Pb(II) was performed using a 1 M hydrochloric acid (1M HCl) solution as the eluent. This operation was carried out by passing 100 µL of 1 M HCl solution through the adsorbent bed over ten draw/eject cycles. The final solution obtained from the elution, which contained a concentrated analyte, was collected. To prevent Pb(II) memory effects on the adsorbent and prepare the syringe for reuse, the adsorbent bed was regenerated after each extraction step. This stage involved sequential washing with 1 M HCl solution, followed by deionized water, until a baseline signal was obtained. Pb(II) determination was performed by monitoring the analytical signal at 193.7 nm, using a spectral slit width of 0.5 nm. Results and discussion Characterization of GP-MPTMS Fourier Transform Infrared Spectroscopy (FT-IR) Analysis The FT-IR spectrum shown in Fig. 2 A reveals two absorption bands around 3450 cm –1 corresponding to the hydroxyl group (O–H) stretching vibrations, while the bands within the range of 2950–2850 cm –1 are associated with the stretching vibrations of aliphatic C–H bonds, which are more intense in the glass powder sample [ 51 ]. Moreover, the absorption bands located near 1020 cm –1 and 780 cm –1 are associated with the asymmetric stretching vibrations of Si–O–Si bonds and symmetric stretching vibrations of Si–O bonds, respectively [ 52 – 54 ]. In the MPTMS-GP sample, these peaks appeared with lower intensity. In this spectrum, the vibrations related to the functional groups of the MPTMS coupling agent overlapped with those of other groups, and no distinct peak for the S–H group was observed. X-ray Diffraction (XRD) Analysis The XRD patterns of GP and MPTMS-GP were also investigated (Fig. 2 B). Comparative analysis of the diffraction patterns showed that both samples exhibited a characteristic broad peak in the 2θ range of 10–40° with a center at approximately 24° [ 55 ]. This diffraction pattern confirms the amorphous nature of the synthesized adsorbent, consistent with the XRD results. The lack of significant change in the diffraction pattern after surface modification with MPTMS indicates that the functionalization process preserved the fundamental structure and amorphous properties of the glass powder, and the changes were limited to the surface of the material, confirming the maintenance of the mechanical and structural stability of the adsorbent for surface adsorption. FE-SEM Analysis The field-emission scanning electron microscopy (FE-SEM) images in Fig. 3 show the surface morphologies of GP, MPTMS-GP in the absence of Pb, and MPTMS-GP in the presence of Pb at identical magnifications. As expected, the modified adsorbent demonstrated a suitable capability for analyte adsorption. Significant changes in the surface morphology, particularly in the sample exposed to the analyte, including the appearance of aggregated structures, indicated the success of the adsorption process and the presence of Pb(II) on the adsorbent surface after the adsorption process. EDX analysis was performed to determine the elemental composition, distribution, and dispersion of elements (in weight or atomic percentages) in the MPTMS-GP sample. The results are presented in Fig. 4 and Fig. 5 . The EDX spectrum of MPTMS-GP confirmed the presence of silicon, sulfur, carbon, and oxygen, where the carbon and sulfur signals originated specifically from the thiol functional group in MPTMS. Other elements belonging to the glass structure, including Ca, Al, and Na, were also observed in the sample. Notably, after contact of the MPTMS-GP with Pb(II) cations, a weak but distinct Pb(II) peak was observed in the EDX spectrum (Fig. 5 ), providing direct evidence of successful heavy metal adsorption on the MPTMS-GP. Thermogravimetric Analysis (TGA) A comparison of the TGA profiles presented in Fig. 6 demonstrates significant differences in the thermal behavior of the studied samples. The unmodified GP exhibited high thermal stability, with no significant mass loss observed within the tested temperature range. In contrast, the MPTMS-GP sample exhibited a distinct thermal decomposition stage in the 200–400°C range. The observed mass reduction was attributed to the thermal degradation of the alkoxy and mercapto groups, which constitute the silane structure affixed to the glass surface. This finding confirms the successful attachment of the silane coupling agent to the glass powder surface [ 56 ]. Optimization of MEPS Extraction Conditions The optimization of the operational parameters of the MEPS method to achieve maximum extraction efficiency and reduce memory effects is considered a critical stage in the development of this method. In this regard, the variables affecting the extraction process were systematically evaluated, and the results are reported. Sample Extraction Cycles One of the main advantages of the MEPS technique is the possibility of multiple passages of the sample through the sorbent bed and the gradual concentration of analytes. In this study, the effect of the number of extraction cycles in the range of 3–10 cycles was investigated, and the results are shown in Fig. 7 A. Data analysis showed that increasing the number of extraction cycles up to five cycles led to a significant improvement in the analytical signal, whereas a further increase in the number of cycles had no significant effect on the extraction efficiency and reached a plateau. Based on this, five extraction cycles were selected as the optimal value for the operational parameter. Number of Elution Cycles The effectiveness of the adsorption/desorption process was assessed by examining the number of elution cycles as a significant factor. In this study, 5–12 consecutive desorption cycles were investigated systematically. The results of this optimization, shown in Fig. 7 B, indicate that increasing the number of desorption cycles up to 10 cycles significantly improves the desorption amount. However, further increasing the number of cycles (beyond 10 cycles) had no significant effect on the process efficiency. Therefore, 10 desorption cycles were determined to be the optimal conditions for achieving maximum efficiency in this system. Solution pH To optimize the adsorption conditions and understand the influencing mechanisms, the effect of solution pH on the adsorption capacity of MPTMS-GP for Pb (II) ions was evaluated systematically. The results of this investigation, shown in Fig. 7 C, demonstrate that the adsorption capacity exhibited a significant upward trend with increasing pH from the acidic range to pH = 6. However, at values higher than this optimal point, a significant decrease in the adsorption efficiency was observed. This pH-dependent adsorption behavior can be attributed to two competing processes: in alkaline environments (pH > 6), the increased concentration of hydroxide ions leads to the formation of Pb(OH) 2 precipitate, which limits the accessibility of metal ions to the adsorption sites and subsequently causes a reduction in the adsorption capacity. However, under acidic conditions (pH < 6), the high concentration of protons (H + ) creates significant competition with Pb(II) for binding to the mercapto (thiol) functional groups present on the adsorbent surface [ 57 , 58 ]. This ionic competition results in the occupation of some active adsorption sites by protons, consequently reducing the adsorbent's capability for Pb(II) removal. Eluent Type and Concentration The selection of an appropriate solvent for analyte desorption from the adsorbent surface is considered a determining parameter for extraction process efficiency. The effectiveness of this process depends on the interaction strength between the analyte and eluent solvent; thus, the optimal solvent should be capable of separating the maximum amount of analyte from the adsorbent surface with a minimum solvent volume. Furthermore, the selected solvent should not cause structural degradation of the adsorbent to enable its reuse while maintaining high efficiency during successive extraction cycles. In this study, two strong acids (nitric acid and hydrochloric acid) and one weak acid (acetic acid) were evaluated as candidate eluent solvents, and their spectral responses were compared. The results showed that hydrochloric acid (HCl) demonstrated favorable performance in the desorption of Pb(II) from the MPTMS-GP surface. To optimize the concentration of this acid, HCl solutions with concentrations of 0.1, 0.5, 1, and 1.5 M were prepared, and their effectiveness in the desorption process was assessed. As shown in Fig. 7 D, the extraction efficiency increased with increasing acid concentration up to 1 M; however, at higher concentrations, no significant improvement in the process efficiency was observed. Complementary investigations revealed that the use of HCl at optimal concentration had no destructive effect on the adsorbent structure, and the adsorption efficiency remained at a desirable level after several cycles of use and desorption. The rationale for this is the effective breaking of the bond between Pb(II) ions and the thiol groups (-SH) on the MPTMS-GP surface without causing significant structural damage to the adsorbent and maintaining the structural integrity of the adsorbent during repeated cycles [ 45 , 59 ]. This is in agreement with another finding where 0.5 M HCl achieved 97% Pb(II) desorption, and both the structural integrity of the adsorbent and maximum efficiency were achieved [ 60 ]. Based on these results, 1 M hydrochloric acid was selected as the optimal eluent for the desorption of Pb(II) from the surface of the synthesized adsorbent. Effect of Elution Solvent Volume Because of the limited amount of adsorbent phase used in the MEPS technique, optimizing the elution solvent volume is particularly important for achieving a high concentration factor (CF). This study assessed the influence of varying the volume of the elution solvent on the efficiency of analyte extraction. The results from systematic experiments (Fig. 7 E) showed that increasing the elution solvent volume to 100 µL resulted in an upward trend in analyte recovery, with the extraction efficiency increasing significantly. However, using volumes higher than this amount led to a decrease in the final analyte concentration in the elution solution, owing to the dilution effect caused by increasing the solvent volume. Based on these findings, 100 µL of hydrochloric acid was selected as the optimal elution solvent volume for subsequent experiments. Adsorbent Amount Recognizing the critical role of sorbent quantity in extraction efficiency, we conducted a systematic study using various sorbent amounts from 1 to 4 mg, and the outcomes are presented in Fig. 7 F. The data showed that increasing the sorbent amount did not correlate with improved extraction efficiency and analyte adsorption; conversely, amounts exceeding 2 mg resulted in decreased analyte adsorption. This phenomenon can be attributed to the powdery nature of the sorbent and the compression effects in the confined loading space of the syringe tip, which impede the optimal flow of the solvent or sample through the sorbent bed [ 58 ]. Consequently, 2 mg of sorbent was considered the optimal amount for the experiment. Adsorption Cure and Adsorbent Capacity Aqueous solutions of Pb(II) with various concentrations ranging from 0.01 to 50.0 µg/L were prepared in this section, with all solutions adjusted to a pH of 6. To investigate the adsorption capacity, 4 mL of each solution was tested under the optimized MEPS conditions using 2 mg of MPTMS-GP adsorbent. The adsorption curve of the desorbed solutions after extraction was plotted against the concentration of the aqueous Pb(II) samples (Fig. 8 A). The results from this curve showed that at a Pb(II) concentration of 50 µg/L, the adsorption amount reached a constant value, indicating the maximum extraction capacity of the 2 mg of adsorbent used in the MEPS. Based on these data, the amount of Pb (II) extracted per milligram of adsorbent (adsorption capacity) was determined. Figure 8 B (curve of extracted analyte amount per milligram of adsorbent) shows an adsorption capacity equivalent to 3595.66 ng/mg. Adsorbent Selectivity To evaluate the adsorbent performance in real environments, the potential interference effects of competitive ionic species on the preconcentration and extraction processes of Pb(II) were investigated (Fig. 9 ). In this regard, a standard Pb(II) solution with a concentration of 50 µg/L was analyzed after adding different concentrations of potential interfering species. The results obtained from these experiments, summarized in Table 1 , show that within the investigated concentration ranges, no significant interference effect (higher than 5% relative error) was observed on the Pb(II) extraction and measurement process. This finding confirms that the MPTMS-GP adsorbent possesses high selectivity for Pb(II) cations, even in the presence of other competing ionic species. This characteristic ensures the efficiency of this adsorbent for the analysis of complex samples with real matrices. Table 1 Selectivity of the method for Pb(II) adsorption compared with other ions. Co-existing substance Tolerance limit (C ion /C pb ) As(v), Hg 2+ 2000 Cl – 1000 Fe 2+ , Mn 2+ ,Cu 2+ , CO 3 2– 500 Cd 2+ , NO 3 – 100 Cr 2+ 80 Zn 2+ 50 Method Validation The optimized approach determined the best operational parameters to include five extraction cycles, maintaining a pH of 6, and employing 100 µL of 1 M hydrochloric acid as the desorption solvent. To assess the analytical effectiveness of the proposed method, key parameters such as measurement precision (RSD%), limit of detection (LOD), and linear dynamic range (LDR) were examined using aqueous standard solutions of Pb (II). The linear range of the method was identified by constructing a calibration curve for aqueous Pb(II) samples extracted using MEPS, as shown in Fig. 1 . Linear regression analysis revealed a correlation coefficient of 0.9981, demonstrating a strong and satisfactory correlation between the analytical signal and analyte concentration. The LOD was determined using the obtained linear equation and statistical calculations using the following equations: $$\:{\text{S}}_{\text{b}}=\sqrt{\frac{\sum\:{\left[{x}_{i}-\:\stackrel{-}{x}\right]}^{2}}{\text{n}-1}}\:,\:\text{L}\text{O}\text{D}=\frac{3{s}_{b}}{m}$$ 1 where n is the number of blank solution measurements, x i is the calculated concentration of the blank solution from the absorption signal obtained in the linear calibration equation for Pb(II) standard solutions to determine the extraction concentration by MEPS, and x̅ is the average of the calculated concentrations of the blank solution. Parameter m represents the slope of the linear calibration equation obtained for Pb(II) standard solutions. The linear range obtained was 0.01-50 ng/mL (R 2 = 0.9981), and the LOD in this range was 0.0013 ng/mL with an RSD (n = 3) of 1.71%. The repeatability of the method was assessed by performing three consecutive extractions of an aqueous Pb(II) solution at a specified concentration, resulting in an RSD of 0.97%. The efficiency of analyte extraction and concentration factor were determined using the absorption signal from an aqueous solution with an initial analyte concentration of 50 ppb (C0). This absorption signal was then interpolated into the calibration equation to calculate the extracted concentration (C ext ) as follows: $$\:\text{R}\left(\text{\%}\right)=\left({\text{Q}}_{\text{e}\text{x}\text{t}}∕{\text{Q}}_{0}\right)\times\:100=\left({\text{C}}_{\text{e}\text{x}\text{t}}{\text{V}}_{\text{e}\text{x}\text{t}}∕{\text{C}}_{0}{\text{V}}_{0}\right)\times\:10$$ 2 $$\:\text{F}={\text{C}}_{\text{e}\text{x}\text{t}}/{\text{C}}_{0}$$ 3 In these relationships, V₀ and Vₑₓₜ represent the volumes of the aqueous solution of the Pb(II) sample under extraction (4000 µL) and the extractant solvent (100 µL), respectively. Qₑₓₜ and Q₀ represent the extracted and initial amounts of Pb(II), respectively. According to the calculations performed, the extraction efficiency was 89% and the concentration factor was 35.95. Extraction and Measurement of Pb(II) in Real Samples The results obtained from the quantitative analysis for determining the Pb(II) content in Lake Zarivar water samples, cosmetic materials (lipstick), and five different vegetable species are shown in Table 2 . The accuracy of the proposed analytical method was assessed by incorporating specific quantities of standard Pb(II) solution into the real sample matrix. The recovery percentage, which ranged from 97.9–103.6%, demonstrated that the precision and accuracy of the method were acceptable. These results confirm that the synthesized adsorbent can effectively extract Pb(II) from real samples with complex matrices. Based on the obtained results and calculations, the Pb(II) concentrations in basil, lettuce, parsley, coriander, leek, and lipstick samples were determined to be 0.1065, 0.1185, 0.0825, 0.0945, 0.0885, and 9.9400 µg/g, respectively. These data demonstrate the importance of the developed extraction method for analytical applications in environmental and biological sample analyses. Table 2 Results of Pb(II) measurements in real samples using MPTMS-GP sorbent by MEPS method with GF-AAS Sample Added (µg/L) Found (µg/L) Recovery (%) Basil 0 5 10 8.50 13.70 ± 0.08 18.45 ± 0.11 –– 103.60 99.30 Lettuce 0 5 10 9.48 14.60 ± 0.13 19.41 ± 0.09 –– 102.40 99.30 Chervil 0 5 10 6.60 11.61 ± 0.07 16.43 ± 0.12 –– 100.20 98.30 Coriander 0 5 10 7.56 12.50 ± 0.11 17.40 ± 0.09 –– 98.80 98.40 Leek 0 5 10 7.08 12.07 ± 0.07 16.94 ± 0.10 –– 99.80 98.60 Lip stick 0 5 10 39.77 44.80 ± 0.17 50.10 ± 0.15 –– 100.60 103.30 Water (Zerivar lake) 0 5 10 6.45 11.58 ± 0.10 16.24 ± 0.12 –– 102.60 97.90 Comparison of the Proposed Method with literature A comparison of the analytical performance of the Pb(II) extraction and measurement method using the MPTMS-GP adsorbent with other adsorbents and analytical methods reported in previous studies is presented in Table 3. The analytical parameters demonstrate that the proposed method exhibits significant performance in terms of the linear calibration range and extraction accuracy compared to other similar adsorbents and analytical methods. Furthermore, the LOD obtained from this method showed satisfactory results compared to the values reported in reliable sources, indicating the efficiency of the synthesized adsorbent in extracting and measuring low concentrations of Pb(II) in the samples. Table 3. Comparison of the proposed method for Pb (II) extraction and determination using the synthesized MPTMS-GP sorbent by MEPS with graphite furnace atomic absorption spectrometry with other reported methods Methods Linear range (ng/mL) LOD (ng/mL) RSD (n = 3) %Recovery Reference 2,2′-dipyridyl ketone SPE AAS 0.6–10.5 0.2 2.6 98–98.6 [ 61 ] PHBvbNCl a SPME FAAS 0.1–250 0.03 1.8 97.7–98.2 [ 62 ] NCp b VS-SPE c FAAS 20–120 6.5 4.2 94–100 [ 63 ] ox-MWCNTd DMSPE FAAS 2–25 0.25 2.3 98.5–106.7 [ 64 ] MWCNT e DMSPE GF-AAS f 0.2–10 0.003 3 [ 65 ] Ag/Ni@g-C3N4 DSPME g FAAS - 270 4.06–5.2% -98.5–104.1% [ 66 ] SPE MNPs-BP FAAS 0.523–0.876 0.519 4.02% 97 ± 5% [ 67 ] Glass powder (TEOS) /MPTMS MEPS GF-AAS 0.01-50 0.0013 1.71 97.9–103.6 This work a Poly-3-hydroxy butyrate-polyvinyl triethyl ammonium chloride comb-type amphiphilic cationic block copolymer, b Nano clinoptilolite modified with 5(p-dimethyl aminobenzylidene), c Vortex-assisted solid phase extraction d Oxidized multiwalled carbon nano tubes, e Multiwalled carbon nano tubes, f Graphite furnace atomic absorption spectrometry, g Dispersive Solid Phase Microextraction Conclusion In this study, an innovative microextraction method was developed, employing glass powder modified with 3-mercaptopropyltrimethoxysilane (MPTMS) to concentrate Pb(II) ions in water-based solutions. The MPTMS-GP glass powder exhibited outstanding adsorption capacity, a strong preference for Pb(II) ions, and good reusability over several extraction cycles. The process was optimized using the following parameters: five extraction cycles, ten elution cycles, a pH of 6, 1 M hydrochloric acid as the elution solvent, 100 µL of elution solvent volume, and 2 mg of adsorbent. The method demonstrated a low limit of detection (LOD) of 0.0013 ng/mL, achieved a recovery rate ranging from 97.9–103.6%, and had a concentration factor of 35.95, making it an exceptionally effective tool for identifying Pb(II) in practical samples. The robustness of the method was established by testing it on various environmental and food samples, including water, vegetables, and cosmetic products. These findings validate the practical utility of the proposed method for analyzing real-world samples. The MPTMS-GP adsorbent stands out from current methods because of its enhanced sensitivity, selectivity, and cost efficiency, making it a promising option for monitoring environmental conditions and conducting health-related research on heavy metals. Authorship contribution statement Sorour karimi: Investigation, Writing – original draft, Soleiman Bahar: Methodology, Supervision, Writing – review & editing, Parisa Poormoghadam: Writing – original draft. Declarations Declaration of competing interest The authors declare that they have no conflicts of interest. Funding There was no Funding for this work. Author Contribution Sorour karimi: Investigation, Writing – original draft, Soleiman Bahar: Methodology, Supervision, Writing – review & editing, Parisa Poormoghadam: Writing – original draft. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-7232218","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":496340771,"identity":"e2c15a39-25ce-44b1-978d-7259f7ce0169","order_by":0,"name":"Sorour karimi","email":"","orcid":"","institution":"University of Kurdistan","correspondingAuthor":false,"prefix":"","firstName":"Sorour","middleName":"","lastName":"karimi","suffix":""},{"id":496340772,"identity":"3f3d837e-21cd-4933-90fa-67a75192009b","order_by":1,"name":"Soleiman Bahar","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAwklEQVRIiWNgGAWjYFACHgZmICnHwMAG5RKrxZh0LYkNUC2EgXwD78HPBTX30jccb0tg+FHDIGPeQECLwQG+ZOkZx4pzN5w5doCx5xgDj8wBQloYeAykedgScjfcSG9g4G1g4JEg7DAe4988/xLSDYBaGP8So4XhAI+ZNG9bQoLBjbQDzETZYnCYL82aty/BcOaZYwmHZY5JEOGw9t7Dt3m+JcjzHW8zfPimxsaesMOYkR3JwEBYwygYBaNgFIwCIgAAT6s1mMVBj2EAAAAASUVORK5CYII=","orcid":"","institution":"University of Kurdistan","correspondingAuthor":true,"prefix":"","firstName":"Soleiman","middleName":"","lastName":"Bahar","suffix":""},{"id":496340773,"identity":"10197d32-42c3-4bf2-bc36-22797ea081a7","order_by":2,"name":"Parisa Poormoghadam","email":"","orcid":"","institution":"University of Kurdistan","correspondingAuthor":false,"prefix":"","firstName":"Parisa","middleName":"","lastName":"Poormoghadam","suffix":""}],"badges":[],"createdAt":"2025-07-28 09:38:21","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-7232218/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-7232218/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":88553203,"identity":"2d097771-d8bb-4c05-96d0-dd0267f66b59","added_by":"auto","created_at":"2025-08-07 15:57:15","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":31817,"visible":true,"origin":"","legend":"\u003cp\u003eCalibration curve of standard lead solutions with known concentrations.\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/065527e330f5ef3a15489f6d.png"},{"id":88553205,"identity":"742d1a8a-b1e7-4dc1-be67-6605f520d169","added_by":"auto","created_at":"2025-08-07 15:57:15","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":124635,"visible":true,"origin":"","legend":"\u003cp\u003eA)\u003cstrong\u003e \u003c/strong\u003eFT-IR spectra of GP and MPTMS-GP/Pb and B) XRD patterns of GP and MPTMS-GP\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/b8aea63631f9255c01f8c87a.png"},{"id":88553657,"identity":"77bc4517-0d5d-4a14-b47c-1caf2942470b","added_by":"auto","created_at":"2025-08-07 16:05:15","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":452197,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of GP (A), MPTMS-GP in the absence of analyte (B), and MPTMS-GP in the presence of analyte (C)\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/40089aaec884f71a4f614c26.png"},{"id":88553658,"identity":"ee4c4cf9-93af-4cb2-9c27-8af5e93a5aa6","added_by":"auto","created_at":"2025-08-07 16:05:15","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":339693,"visible":true,"origin":"","legend":"\u003cp\u003eEDX spectrum and elemental mapping of MPTMS-GP\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/371645ea00acfff2f888c55b.png"},{"id":88553659,"identity":"dc9a571b-45ec-4d5e-b9d7-1c168d14d571","added_by":"auto","created_at":"2025-08-07 16:05:15","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":321665,"visible":true,"origin":"","legend":"\u003cp\u003eEDAX spectrum and elemental mapping of MPTMS-GP/Pb nanoplates.\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/c07e1818d1779bfa7f1dc901.png"},{"id":88555119,"identity":"5c73ab44-5b15-4b45-9bee-acf7d4d52aeb","added_by":"auto","created_at":"2025-08-07 16:21:15","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":27106,"visible":true,"origin":"","legend":"\u003cp\u003eTGA profiles of (A) GP and (B) MPTMS-GP samples.\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/988476dbbe61f2bbd6ab2b84.png"},{"id":88553208,"identity":"574b7997-190b-4f0a-b94b-4c2d497d9509","added_by":"auto","created_at":"2025-08-07 15:57:15","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":147510,"visible":true,"origin":"","legend":"\u003cp\u003eThe effects of A) Number of adsorption cycles, B) Number of elution cycles, C) pH, D) Elution solvent concentration, E) Elution solvent volume, F) Adsorbent amount\u003c/p\u003e","description":"","filename":"7.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/cd7eca74aa805a92fe89ce12.png"},{"id":88553662,"identity":"a988670f-3160-4739-9fe3-87a3d744266a","added_by":"auto","created_at":"2025-08-07 16:05:15","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":42965,"visible":true,"origin":"","legend":"\u003cp\u003e(A) Adsorption curve diagram (B) Extraction valve curve of pb(II) using MPTMS-GP in the concentration range of 0.01-50 ppb\u003c/p\u003e","description":"","filename":"8.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/9f6f703ad7d983460258c437.png"},{"id":88553214,"identity":"a277d9c2-6753-4fb4-ab5d-f2837624a537","added_by":"auto","created_at":"2025-08-07 15:57:15","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":26202,"visible":true,"origin":"","legend":"\u003cp\u003eSelectivity of the method for Pb(II) absorption compared to other ions\u003c/p\u003e","description":"","filename":"9.png","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/0c8554949e40bccd556a35af.png"},{"id":90197004,"identity":"61602134-ec0a-4035-8817-15c279041bc7","added_by":"auto","created_at":"2025-08-29 17:31:49","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2770089,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7232218/v1/6b418d45-e0ca-40d3-84c4-f77828b06f51.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"A Novel Microextraction Technique for Pb(II) Ion Preconcentration Using 3-Mercapto Propyltrimethoxysilane- Modified Glass Powder","fulltext":[{"header":"Introduction","content":"\u003cp\u003eHeavy metals can cause serious damage to vital human body functions at high concentrations because of their toxicity. Hazardous metals such as lead, copper, nickel, cadmium, and mercury can enter the body through food consumption, inhalation, or dermal absorption [\u003cspan additionalcitationids=\"CR2\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e–\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. Although lead (Pb) is among the most hazardous heavy metals, it is widely utilized in the industry for making batteries, pigments, catalysts, and alloys [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. Pb(II) is dispersed in the environment through various chemical pollutants and has the potential to enter the food chain. This metal has a strong tendency to accumulate in the bodies of living organisms, and its accumulation, especially in the bone marrow, can lead to life-threatening diseases such as anemia, kidney and brain damage, paralysis, miscarriage, and behavioral disorders [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. Therefore, the accurate and sensitive determination of Pb(II)in water is necessary. To measure heavy metals such as lead, atomic absorption spectrometry is a common choice in laboratories because of its simplicity and cost-effectiveness. However, when the concentration of metals is very low (at the µg l\u003csup\u003e–1\u003c/sup\u003e level), the use of flame atomic absorption is not practical because of its low sensitivity and interference from other elements present in the sample [\u003cspan additionalcitationids=\"CR8\" citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e–\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. To address this issue, separation and preconcentration methods such as cloud point extraction [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e], ion exchange [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e], electrocoagulation [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e], liquid-liquid extraction [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e], electrodeposition [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], dispersive liquid-liquid microextraction [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e, \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], solid-phase extraction [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e, \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e], and dispersive micro-solid-phase extraction [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e] have been developed for the preconcentration of Pb(II).\u003c/p\u003e\u003cp\u003eSolid-phase extraction (SPE) is popular among researchers because of its simplicity, speed, ease of compatibility with pre-concentration, and ability to integrate with flow injection analysis (FIA) techniques for measuring trace metals. This method also offers a high enrichment factor and enables the processing of large sample volumes without sample contamination. For these reasons, SPE is widely used for the preconcentration and separation of organic and inorganic species at low and ultralow concentrations, enhancing the sensitivity of analytical methods and eliminating interference from the sample matrix [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eInvestigating the efficiency of new and economically viable materials as solid-phase extractors is a key aspect of research on the solid-phase extraction of transition metals at low concentrations. Waste glass is an abundant material derived from municipal solid waste (MSW) or construction debris and can be regarded as a low-cost adsorbent compared to expensive commercial adsorbents such as activated carbon or zeolites. Collecting glass waste contributes to environmental preservation because glass is non-biodegradable and persists in the environment for long periods. Glass surfaces are well-suited for adsorption applications because they are composed of various oxides, such as SiO\u003csub\u003e2\u003c/sub\u003e, Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, CaO, and Na\u003csub\u003e2\u003c/sub\u003eO. When these oxides come into contact with water, they form reactive surface hydroxyl groups, such as Si–OH, which serve as active sites that can adsorb heavy metal ions such as Pb(II), Cd(II), and Ni(II) [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. Another benefit of glass powder is its ability to become porous, with its specific surface area being enhanced through either chemical or thermal processes. The adsorption capacity of waste glass can be significantly improved by altering its surface using methods such as acid activation, hydrothermal treatment, calcination, and the application of pore-forming agents [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eFor example, it has been shown that waste glass possesses a large specific surface area (about 557.912 m\u003csup\u003e2\u003c/sup\u003e/g) and very small pore diameter (2.099 nm), which contribute to its remarkable adsorption capacity [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. In another study, the maximum adsorption capacity for metal ions such as Pb\u003csup\u003e2+\u003c/sup\u003e was reported to be as high as 11.68 mg/g, indicating the high efficiency of these materials in removing heavy metals [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. The economic and environmental aspects of using glass powder as an adsorbent are also significant, as recycling and reusing waste glass not only results in economic savings but also reduces the negative impacts associated with landfilling glass at disposal sites [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThe high stability of glass allows glass-based adsorbents to be regenerated and reused over several cycles. Adsorption on glass surfaces often involves ion exchange (for example, Na\u003csup\u003e+\u003c/sup\u003e and Ca\u003csup\u003e2+\u003c/sup\u003e ions present in the glass are replaced by heavy metal ions), physisorption, electrostatic interactions, and surface complexation. Ion exchange plays an important role in heavy metal removal [\u003cspan additionalcitationids=\"CR26 CR27\" citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e–\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e, \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. Various adsorbents have been used for the extraction and preconcentration of Pb(II) ions in water, including natural adsorbents such as agri-waste biosorbents [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e], natural bentonite [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e], agricultural wastes [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e], carbon-based adsorbents such as activated carbon [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e] and graphene oxide [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e], inorganic adsorbents such as functionalized Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e], TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites [\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e], metal-organic frameworks [\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e], ion-imprinted polymers [\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e], and others. The efficiency of adsorbents in binding metal ions is attributed to their ability to form complexes between the ligands present on the adsorbent surface and the metal ions. The selectivity of a specific ligand toward the target metal ion results from conventional acid-base interactions between the two [\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. Therefore, an ideal adsorbent should possess the highest possible specific surface area and allow easy surface chemical modification. Nanoparticles, with their elevated specific surface areas, serve as an outstanding platform for adsorbing heavy metals. Moreover, the functional groups present on the surface of the nanoparticles play a crucial role in the selectivity of the adsorbent because of the affinity between these groups and the target molecules [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e]. Functionalization of the glass powder surface with thiol groups (–SH) via modification with mercapto propyltrimethoxysilane (MPTMS) is critical for the preconcentration of Pb(II) in solution for several reasons. First, thiol groups (S-H) can effectively remove these pollutants from aqueous solutions because of their high binding affinity for heavy metal ions (e.g., lead). Thiol groups create specific ionic interactions with soft Lewis acids, including mercury (Hg(II)), cadmium (Cd(II)), and lead (Pb(II)) ions [\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e, \u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. Surface modification of glass powder leads to a significant increase in its surface area, which enhances the number of active binding sites and consequently boosts its adsorption capacity for heavy metals [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]. Additionally, the hydrophobicity imparted by MPTMS on the glass inhibits the adsorption of water molecules onto the active sites, thereby improving the efficiency and selectivity of heavy metal removal. Furthermore, the unique properties of MPTMS-modified glass can be leveraged to design and fine-tune it for specific applications in heavy metal removal [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThis study assessed the effectiveness of glass powder treated with 3-mercaptopropyl trimethoxysilane (MPTMS), noted for its excellent sensitivity and selectivity, as a straightforward adsorbent for the separation and measurement of Pb(II) ions. The method employed microextraction using the packed syringe (MEPS) technique, which was paired with detection using graphite furnace atomic absorption spectrometry (GFAAS). The physical and chemical properties of raw GP and MPTMS-GP were characterized using Fourier Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDAX), X-ray Diffraction (XRD), and Thermogravimetric Analysis (TGA). The variables influencing Pb(II) extraction efficiency were investigated and optimized in this study. Finally, the MPTMS-GP adsorbent was used to extract and quantify Pb(II) in real-world samples, including vegetables, cosmetic products, and water from Lake Zriwar.\u003c/p\u003e"},{"header":"Materials and Equipment","content":"\u003cp\u003e\u003cb\u003eMaterials\u003c/b\u003e\u003c/p\u003e\u003cp\u003eAll chemical materials used were of analytical grade. Nitric acid (HNO\u003csub\u003e3\u003c/sub\u003e, 65%), hydrochloric acid (HCl, 37%), sulfuric acid (H\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e, 98%), glacial acetic acid (CH\u003csub\u003e3\u003c/sub\u003eCOOH), hydrogen peroxide (H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e, 30% v/v), sodium hydroxide (NaOH, in tablet form), tetraethyl orthosilicate (TEOS, C\u003csub\u003e8\u003c/sub\u003eH\u003csub\u003e20\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003eSi), and 3-mercaptopropyl trimethoxysilane (MPTMS, C\u003csub\u003e6\u003c/sub\u003eH\u003csub\u003e16\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003eSSi) were all obtained from Merck (Germany). A Pb(II) standard stock solution with a concentration of 1000 mg/L was prepared by dissolving an appropriate amount of lead nitrate (Pb(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e, Merck) in dilute nitric acid.\u003c/p\u003e\u003cp\u003e\u003cb\u003eInstruments\u003c/b\u003e\u003c/p\u003e\u003cp\u003eAn accurate AXIS digital balance (model ALN220, Spotka, Poland) with a precision of 0.1 mg was used to weigh the sample. Quantitative Pb(II) measurement was performed using a Varian/Agilent atomic absorption spectrometer model SpectrAA 220 equipped with a GTA 110 graphite furnace (GFAAS). Material characterization analyses included recording FTIR spectra with a Bruker Vector 22 instrument (in the range of 4000 − 400 cm\u003csup\u003e–1\u003c/sup\u003e), surface morphology and elemental composition examination by field emission scanning electron microscopy (FESEM) model TESCAN Mira 3-LMU (with 30 kV voltage and equipped with EDX analyzer), crystal structure determination with X-ray diffraction (XRD) model Rigaku Ultima IV (Japan), and thermal analysis with TGA model PerkinElmer STA6000 (USA). Additionally, an RST16 centrifuge (made in Iran, 5000 rpm) and an ultrasonic bath (Spectron) were used in the various stages of sample preparation and processing.\u003c/p\u003e\u003cp\u003e\u003cb\u003eGlass powder (GP) preparation\u003c/b\u003e\u003c/p\u003e\u003cp\u003eGlass powder (GP) was prepared by crushing clean glass capillary tubes using a porcelain mortar. The resulting powder was subsequently mixed with tetraethoxysilane (TEOS), and the mixture was agitated with a magnetic stirrer for 12 h. This process facilitated TEOS hydrolysis and increased the number of surface hydroxyl (Si-OH) groups. The solid product was separated by centrifugation and washed repeatedly with distilled water. The final activated glass powder was dried in an oven at 60–70°C after separation.\u003c/p\u003e\u003cp\u003e\u003cb\u003eSynthesis of Glass Powder Modified with 3-Mercaptopropyltrimethoxysilane (GP-MPTMS)\u003c/b\u003e\u003c/p\u003e\u003cp\u003eThe surface modification of the glass powder with 3-mercaptopropyltrimethoxysilane was performed according to the method shown in the diagram, adapted from a previous study [\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e]. First, a silane hydrolysis solution was prepared by adding 40 µL of MPTMS to 100 mL of a water/ethanol mixture (volume ratio of 9:1). The pH of the resulting solution was adjusted to the range-3-4 using acetic acid. Then, 0.5 g of the activated glass powder (prepared in the previous step) was added to the silane solution. The resulting suspension was placed in a water bath at 60–70°C for 30 min under continuous stirring. The initial solid product was separated by centrifugation and dried for 4 h at 110°C in an oven. To remove unreacted materials and weakly bonded silanes, the dried powder was immersed in deionized water for 24 h. The solid was then purified through successive cycles of centrifugation and washing with distilled water. Finally, the MPTMS-modified glass powder (GP-MPTMS) was completely dried for 24 h in an oven at 110°C after separation (See Scheme \u003cspan refid=\"Sch1\" class=\"InternalRef\"\u003e1\u003c/span\u003e for details of the synthesis steps).\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003cb\u003eCalibration Curve\u003c/b\u003e\u003c/p\u003e\u003cp\u003eFor the calibration curve (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), a standard lead nitrate solution with an initial concentration of 1000 ppm was employed. A sequence of standard solutions at varying concentrations was prepared by diluting the stock solutions. The optical absorption of each standard was measured using a spectrophotometer. A standard calibration curve for Pb(II) was established over a concentration range of 0.000001–2 ppm, facilitating the determination of unknown sample concentrations.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003cb\u003ePreparation of Real Samples\u003c/b\u003e\u003c/p\u003e\u003cp\u003e\u003cb\u003eWater\u003c/b\u003e\u003c/p\u003e\u003cp\u003eWater samples collected from Lake Zarivar were filtered using 0.48 micrometer membrane filters. After pH adjustment, the filtered samples were directly subjected to extraction and analysis, without further preparation.\u003c/p\u003e\u003cp\u003e\u003cb\u003eVegetables\u003c/b\u003e\u003c/p\u003e\u003cp\u003eSamples of commonly consumed vegetables, including parsley (Petroselinum crispum), lettuce (Lactuca sativa), leek (Allium ampeloprasum), basil (Ocimum basilicum), and coriander (Coriandrum sativum), were selected for the analysis [150, 151]. Initially, fresh vegetable samples were meticulously rinsed with tap and distilled water. Subsequently, the samples were placed in an oven set to 120°C until they reached a stable weight. Each dried vegetable sample (10 g) was accurately weighed and transferred to a beaker for further analysis. For wet digestion, 100 mL of concentrated nitric acid (HNO\u003csub\u003e3\u003c/sub\u003e), 20 mL of hydrogen peroxide (H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e, 30% v/v), and 30 mL of deionized water were added to each beaker. The mixture obtained was heated at 80°C for a duration–20–30 minutes. Once cooled to room temperature, the mixture was filtered using a Whatman No. 42 filter paper. The filtered solution was slowly transferred to a 250 mL volumetric flask and diluted with deionized water. Next, 20 mL of this stock solution was placed in a 100 mL volumetric flask and brought up to the mark with distilled water. The pH of the resulting solutions was adjusted prior to extraction and analysis [\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e, \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003cb\u003eLipstick\u003c/b\u003e\u003c/p\u003e\u003cp\u003eThe sample preparation process for lipstick analysis was performed according to a reference method [\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e] with minor modifications. For this purpose, 0.5 g of the lipstick sample was carefully weighed and transferred to a digestion beaker. Subsequently, 30 mL of concentrated nitric acid (HNO3) and 10 mL of concentrated hydrochloric acid (HCl) were introduced into the sample. The mixture was subjected to a controlled heating program: initially, the temperature was held at 130°C for 15 min, after which it was elevated to 200°C and maintained for 35 min. Once this stage was finished and the contents had cooled to approximately 50°C, 100 mL of a 4% (w/v) boric acid solution (H3BO3) was introduced. The mixture was subsequently maintained at 180°C for 15 min. Once it was fully cooled to ambient temperature, the solution was transferred to a 250 mL volumetric flask and diluted using deionized water. Subsequently, 20 mL of this solution was transferred to a 100 mL volumetric flask and diluted to the mark using deionized water. The pH of the resulting solution was adjusted before extraction and analysis.\u003c/p\u003e\u003cp\u003e\u003cb\u003eRice\u003c/b\u003e\u003c/p\u003e\u003cp\u003eA rice sample from Iran was used in this study. Initially, the rice grains were washed with distilled water, followed by drying in an oven set at 105°C for 48 h. The desiccated samples were finely pulverized using a laboratory mill. A precise amount of rice powder (0.5 g) was measured and placed in a digestion flask. The wet digestion process was initiated according to a method by adding 4 mL of concentrated sulfuric acid (H\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e) [\u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e]; the mixture was gently heated for 3–5 min until it reached the boiling point. After this initial stage, 16.5 mL of hydrogen peroxide (H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e) (30% v/v) was gradually and carefully added to the flask until the solution became completely clear. Heating was continued for 1 min after the solution became clear. Once the solution was cooled to ambient temperature, it was passed through a Whatman No. 42 filter paper into a 100 mL volumetric flask. The solution was then topped up with distilled water for further analysis.\u003c/p\u003e\u003cp\u003e\u003cb\u003eMeasurement in Real Samples\u003c/b\u003e\u003c/p\u003e\u003cp\u003eExtraction was performed using a standard 1 mL MEPS syringe. Approximately 2 mg of MPTMS-GP adsorbent was manually placed between two porous polymer frits at the terminal section of the syringe barrel (near the needle) to form a packed bed. The compaction was adjusted to prevent adsorbent leakage and channeling while allowing easy solution passage. Prior to the first extraction, the adsorbent bed was conditioned by passing 4 mL of deionized water through it. A total of 4 mL of the sample solution was processed through the adsorbent bed for analyte extraction by conducting five consecutive draw and eject cycles with a syringe. Following sample loading, the adsorbent bed was washed with 2 mL of deionized water to eliminate any possible matrix interferences. The elution stage of the adsorbed Pb(II) was performed using a 1 M hydrochloric acid (1M HCl) solution as the eluent. This operation was carried out by passing 100 µL of 1 M HCl solution through the adsorbent bed over ten draw/eject cycles. The final solution obtained from the elution, which contained a concentrated analyte, was collected. To prevent Pb(II) memory effects on the adsorbent and prepare the syringe for reuse, the adsorbent bed was regenerated after each extraction step. This stage involved sequential washing with 1 M HCl solution, followed by deionized water, until a baseline signal was obtained. Pb(II) determination was performed by monitoring the analytical signal at 193.7 nm, using a spectral slit width of 0.5 nm.\u003c/p\u003e"},{"header":"Results and discussion","content":"\u003cp\u003e\u003cstrong\u003eCharacterization of GP-MPTMS\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFourier Transform Infrared Spectroscopy (FT-IR) Analysis\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe FT-IR spectrum shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003eA reveals two absorption bands around 3450 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e corresponding to the hydroxyl group (O\u0026ndash;H) stretching vibrations, while the bands within the range of 2950\u0026ndash;2850 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e are associated with the stretching vibrations of aliphatic C\u0026ndash;H bonds, which are more intense in the glass powder sample [\u003cspan class=\"CitationRef\"\u003e51\u003c/span\u003e]. Moreover, the absorption bands located near 1020 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e and 780 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e are associated with the asymmetric stretching vibrations of Si\u0026ndash;O\u0026ndash;Si bonds and symmetric stretching vibrations of Si\u0026ndash;O bonds, respectively [\u003cspan class=\"CitationRef\"\u003e52\u003c/span\u003e\u0026ndash;\u003cspan class=\"CitationRef\"\u003e54\u003c/span\u003e]. In the MPTMS-GP sample, these peaks appeared with lower intensity. In this spectrum, the vibrations related to the functional groups of the MPTMS coupling agent overlapped with those of other groups, and no distinct peak for the S\u0026ndash;H group was observed.\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003cp\u003e\u003cstrong\u003e\u0026nbsp;X-ray Diffraction (XRD) Analysis\u003c/strong\u003e\u003c/p\u003e\n\u003c/div\u003e\n\u003cp\u003eThe XRD patterns of GP and MPTMS-GP were also investigated (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003eB). Comparative analysis of the diffraction patterns showed that both samples exhibited a characteristic broad peak in the 2\u0026theta; range of 10\u0026ndash;40\u0026deg; with a center at approximately 24\u0026deg; [\u003cspan class=\"CitationRef\"\u003e55\u003c/span\u003e]. This diffraction pattern confirms the amorphous nature of the synthesized adsorbent, consistent with the XRD results. The lack of significant change in the diffraction pattern after surface modification with MPTMS indicates that the functionalization process preserved the fundamental structure and amorphous properties of the glass powder, and the changes were limited to the surface of the material, confirming the maintenance of the mechanical and structural stability of the adsorbent for surface adsorption.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFE-SEM Analysis\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe field-emission scanning electron microscopy (FE-SEM) images in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e show the surface morphologies of GP, MPTMS-GP in the absence of Pb, and MPTMS-GP in the presence of Pb at identical magnifications. As expected, the modified adsorbent demonstrated a suitable capability for analyte adsorption. Significant changes in the surface morphology, particularly in the sample exposed to the analyte, including the appearance of aggregated structures, indicated the success of the adsorption process and the presence of Pb(II) on the adsorbent surface after the adsorption process.\u003c/p\u003e\n\u003cp\u003eEDX analysis was performed to determine the elemental composition, distribution, and dispersion of elements (in weight or atomic percentages) in the MPTMS-GP sample. The results are presented in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e and Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e. The EDX spectrum of MPTMS-GP confirmed the presence of silicon, sulfur, carbon, and oxygen, where the carbon and sulfur signals originated specifically from the thiol functional group in MPTMS. Other elements belonging to the glass structure, including Ca, Al, and Na, were also observed in the sample. Notably, after contact of the MPTMS-GP with Pb(II) cations, a weak but distinct Pb(II) peak was observed in the EDX spectrum (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e), providing direct evidence of successful heavy metal adsorption on the MPTMS-GP.\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003cp\u003e\u003cstrong\u003eThermogravimetric Analysis (TGA)\u003c/strong\u003e\u003c/p\u003e\n\u003c/div\u003e\n\u003cp\u003eA comparison of the TGA profiles presented in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e6\u003c/span\u003e demonstrates significant differences in the thermal behavior of the studied samples. The unmodified GP exhibited high thermal stability, with no significant mass loss observed within the tested temperature range. In contrast, the MPTMS-GP sample exhibited a distinct thermal decomposition stage in the 200\u0026ndash;400\u0026deg;C range. The observed mass reduction was attributed to the thermal degradation of the alkoxy and mercapto groups, which constitute the silane structure affixed to the glass surface. This finding confirms the successful attachment of the silane coupling agent to the glass powder surface [\u003cspan class=\"CitationRef\"\u003e56\u003c/span\u003e].\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eOptimization of MEPS Extraction Conditions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe optimization of the operational parameters of the MEPS method to achieve maximum extraction efficiency and reduce memory effects is considered a critical stage in the development of this method. In this regard, the variables affecting the extraction process were systematically evaluated, and the results are reported.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eSample Extraction Cycles\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eOne of the main advantages of the MEPS technique is the possibility of multiple passages of the sample through the sorbent bed and the gradual concentration of analytes. In this study, the effect of the number of extraction cycles in the range of 3\u0026ndash;10 cycles was investigated, and the results are shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eA. Data analysis showed that increasing the number of extraction cycles up to five cycles led to a significant improvement in the analytical signal, whereas a further increase in the number of cycles had no significant effect on the extraction efficiency and reached a plateau. Based on this, five extraction cycles were selected as the optimal value for the operational parameter.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eNumber of Elution Cycles\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe effectiveness of the adsorption/desorption process was assessed by examining the number of elution cycles as a significant factor. In this study, 5\u0026ndash;12 consecutive desorption cycles were investigated systematically. The results of this optimization, shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eB, indicate that increasing the number of desorption cycles up to 10 cycles significantly improves the desorption amount. However, further increasing the number of cycles (beyond 10 cycles) had no significant effect on the process efficiency. Therefore, 10 desorption cycles were determined to be the optimal conditions for achieving maximum efficiency in this system.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eSolution pH\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eTo optimize the adsorption conditions and understand the influencing mechanisms, the effect of solution pH on the adsorption capacity of MPTMS-GP for Pb (II) ions was evaluated systematically. The results of this investigation, shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eC, demonstrate that the adsorption capacity exhibited a significant upward trend with increasing pH from the acidic range to pH\u0026thinsp;=\u0026thinsp;6. However, at values higher than this optimal point, a significant decrease in the adsorption efficiency was observed. This pH-dependent adsorption behavior can be attributed to two competing processes: in alkaline environments (pH\u0026thinsp;\u0026gt;\u0026thinsp;6), the increased concentration of hydroxide ions leads to the formation of Pb(OH)\u003csub\u003e2\u003c/sub\u003e precipitate, which limits the accessibility of metal ions to the adsorption sites and subsequently causes a reduction in the adsorption capacity. However, under acidic conditions (pH\u0026thinsp;\u0026lt;\u0026thinsp;6), the high concentration of protons (H\u003csup\u003e+\u003c/sup\u003e) creates significant competition with Pb(II) for binding to the mercapto (thiol) functional groups present on the adsorbent surface [\u003cspan class=\"CitationRef\"\u003e57\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e58\u003c/span\u003e]. This ionic competition results in the occupation of some active adsorption sites by protons, consequently reducing the adsorbent's capability for Pb(II) removal.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEluent Type and Concentration\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe selection of an appropriate solvent for analyte desorption from the adsorbent surface is considered a determining parameter for extraction process efficiency. The effectiveness of this process depends on the interaction strength between the analyte and eluent solvent; thus, the optimal solvent should be capable of separating the maximum amount of analyte from the adsorbent surface with a minimum solvent volume. Furthermore, the selected solvent should not cause structural degradation of the adsorbent to enable its reuse while maintaining high efficiency during successive extraction cycles. In this study, two strong acids (nitric acid and hydrochloric acid) and one weak acid (acetic acid) were evaluated as candidate eluent solvents, and their spectral responses were compared. The results showed that hydrochloric acid (HCl) demonstrated favorable performance in the desorption of Pb(II) from the MPTMS-GP surface. To optimize the concentration of this acid, HCl solutions with concentrations of 0.1, 0.5, 1, and 1.5 M were prepared, and their effectiveness in the desorption process was assessed. As shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eD, the extraction efficiency increased with increasing acid concentration up to 1 M; however, at higher concentrations, no significant improvement in the process efficiency was observed. Complementary investigations revealed that the use of HCl at optimal concentration had no destructive effect on the adsorbent structure, and the adsorption efficiency remained at a desirable level after several cycles of use and desorption. The rationale for this is the effective breaking of the bond between Pb(II) ions and the thiol groups (-SH) on the MPTMS-GP surface without causing significant structural damage to the adsorbent and maintaining the structural integrity of the adsorbent during repeated cycles [\u003cspan class=\"CitationRef\"\u003e45\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e59\u003c/span\u003e]. This is in agreement with another finding where 0.5 M HCl achieved 97% Pb(II) desorption, and both the structural integrity of the adsorbent and maximum efficiency were achieved [\u003cspan class=\"CitationRef\"\u003e60\u003c/span\u003e]. Based on these results, 1 M hydrochloric acid was selected as the optimal eluent for the desorption of Pb(II) from the surface of the synthesized adsorbent.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEffect of Elution Solvent Volume\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eBecause of the limited amount of adsorbent phase used in the MEPS technique, optimizing the elution solvent volume is particularly important for achieving a high concentration factor (CF). This study assessed the influence of varying the volume of the elution solvent on the efficiency of analyte extraction. The results from systematic experiments (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eE) showed that increasing the elution solvent volume to 100 \u0026micro;L resulted in an upward trend in analyte recovery, with the extraction efficiency increasing significantly. However, using volumes higher than this amount led to a decrease in the final analyte concentration in the elution solution, owing to the dilution effect caused by increasing the solvent volume. Based on these findings, 100 \u0026micro;L of hydrochloric acid was selected as the optimal elution solvent volume for subsequent experiments.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAdsorbent Amount\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eRecognizing the critical role of sorbent quantity in extraction efficiency, we conducted a systematic study using various sorbent amounts from 1 to 4 mg, and the outcomes are presented in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003eF. The data showed that increasing the sorbent amount did not correlate with improved extraction efficiency and analyte adsorption; conversely, amounts exceeding 2 mg resulted in decreased analyte adsorption. This phenomenon can be attributed to the powdery nature of the sorbent and the compression effects in the confined loading space of the syringe tip, which impede the optimal flow of the solvent or sample through the sorbent bed [\u003cspan class=\"CitationRef\"\u003e58\u003c/span\u003e]. Consequently, 2 mg of sorbent was considered the optimal amount for the experiment.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAdsorption Cure and Adsorbent Capacity\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAqueous solutions of Pb(II) with various concentrations ranging from 0.01 to 50.0 \u0026micro;g/L were prepared in this section, with all solutions adjusted to a pH of 6. To investigate the adsorption capacity, 4 mL of each solution was tested under the optimized MEPS conditions using 2 mg of MPTMS-GP adsorbent. The adsorption curve of the desorbed solutions after extraction was plotted against the concentration of the aqueous Pb(II) samples (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e8\u003c/span\u003eA). The results from this curve showed that at a Pb(II) concentration of 50 \u0026micro;g/L, the adsorption amount reached a constant value, indicating the maximum extraction capacity of the 2 mg of adsorbent used in the MEPS. Based on these data, the amount of Pb (II) extracted per milligram of adsorbent (adsorption capacity) was determined. Figure\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e8\u003c/span\u003eB (curve of extracted analyte amount per milligram of adsorbent) shows an adsorption capacity equivalent to 3595.66 ng/mg.\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\n\u003cp\u003e\u003cstrong\u003eAdsorbent Selectivity\u003c/strong\u003e\u003c/p\u003e\n\u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003eTo evaluate the adsorbent performance in real environments, the potential interference effects of competitive ionic species on the preconcentration and extraction processes of Pb(II) were investigated (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e9\u003c/span\u003e). In this regard, a standard Pb(II) solution with a concentration of 50 \u0026micro;g/L was analyzed after adding different concentrations of potential interfering species. The results obtained from these experiments, summarized in Table\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e, show that within the investigated concentration ranges, no significant interference effect (higher than 5% relative error) was observed on the Pb(II) extraction and measurement process. This finding confirms that the MPTMS-GP adsorbent possesses high selectivity for Pb(II) cations, even in the presence of other competing ionic species. This characteristic ensures the efficiency of this adsorbent for the analysis of complex samples with real matrices.\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003ctable id=\"Tab1\" border=\"1\"\u003e\u003ccaption\u003e\n\u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e\n\u003cdiv class=\"CaptionContent\"\u003e\n\u003cp\u003eSelectivity of the method for Pb(II) adsorption compared with other ions.\u003c/p\u003e\n\u003c/div\u003e\n\u003c/caption\u003e\n\u003cthead\u003e\n\u003ctr\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eCo-existing substance\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eTolerance limit (C\u003csub\u003eion\u003c/sub\u003e/C\u003csub\u003epb\u003c/sub\u003e)\u003c/p\u003e\n\u003c/th\u003e\n\u003c/tr\u003e\n\u003c/thead\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eAs(v), Hg\u003csup\u003e2+\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e2000\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eCl\u003csup\u003e\u0026ndash;\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e1000\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eFe\u003csup\u003e2+\u003c/sup\u003e, Mn\u003csup\u003e2+\u003c/sup\u003e,Cu\u003csup\u003e2+\u003c/sup\u003e, CO\u003csub\u003e3\u003c/sub\u003e\u003csup\u003e2\u0026ndash;\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e500\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eCd\u003csup\u003e2+\u003c/sup\u003e, NO\u003csub\u003e3\u003c/sub\u003e\u003csup\u003e\u0026ndash;\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e100\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eCr\u003csup\u003e2+\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e80\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eZn\u003csup\u003e2+\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e50\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eMethod Validation\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe optimized approach determined the best operational parameters to include five extraction cycles, maintaining a pH of 6, and employing 100 \u0026micro;L of 1 M hydrochloric acid as the desorption solvent. To assess the analytical effectiveness of the proposed method, key parameters such as measurement precision (RSD%), limit of detection (LOD), and linear dynamic range (LDR) were examined using aqueous standard solutions of Pb (II). The linear range of the method was identified by constructing a calibration curve for aqueous Pb(II) samples extracted using MEPS, as shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e. Linear regression analysis revealed a correlation coefficient of 0.9981, demonstrating a strong and satisfactory correlation between the analytical signal and analyte concentration.\u003c/p\u003e\n\u003cp\u003eThe LOD was determined using the obtained linear equation and statistical calculations using the following equations:\u003c/p\u003e\n\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\n\u003cdiv id=\"FileID_Equ1\" class=\"mathdisplay\"\u003e$$\\:{\\text{S}}_{\\text{b}}=\\sqrt{\\frac{\\sum\\:{\\left[{x}_{i}-\\:\\stackrel{-}{x}\\right]}^{2}}{\\text{n}-1}}\\:,\\:\\text{L}\\text{O}\\text{D}=\\frac{3{s}_{b}}{m}$$\u003c/div\u003e\n\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003ewhere n is the number of blank solution measurements, x\u003csub\u003ei\u003c/sub\u003e is the calculated concentration of the blank solution from the absorption signal obtained in the linear calibration equation for Pb(II) standard solutions to determine the extraction concentration by MEPS, and x̅ is the average of the calculated concentrations of the blank solution. Parameter m represents the slope of the linear calibration equation obtained for Pb(II) standard solutions. The linear range obtained was 0.01-50 ng/mL (R\u003csup\u003e2\u003c/sup\u003e\u0026thinsp;=\u0026thinsp;0.9981), and the LOD in this range was 0.0013 ng/mL with an RSD (n\u0026thinsp;=\u0026thinsp;3) of 1.71%.\u003c/p\u003e\n\u003cp\u003eThe repeatability of the method was assessed by performing three consecutive extractions of an aqueous Pb(II) solution at a specified concentration, resulting in an RSD of 0.97%. The efficiency of analyte extraction and concentration factor were determined using the absorption signal from an aqueous solution with an initial analyte concentration of 50 ppb (C0). This absorption signal was then interpolated into the calibration equation to calculate the extracted concentration (C\u003csub\u003eext\u003c/sub\u003e) as follows:\u003c/p\u003e\n\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\n\u003cdiv id=\"FileID_Equ2\" class=\"mathdisplay\"\u003e$$\\:\\text{R}\\left(\\text{\\%}\\right)=\\left({\\text{Q}}_{\\text{e}\\text{x}\\text{t}}∕{\\text{Q}}_{0}\\right)\\times\\:100=\\left({\\text{C}}_{\\text{e}\\text{x}\\text{t}}{\\text{V}}_{\\text{e}\\text{x}\\text{t}}∕{\\text{C}}_{0}{\\text{V}}_{0}\\right)\\times\\:10$$\u003c/div\u003e\n\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Equ3\" class=\"Equation\"\u003e\n\u003cdiv id=\"FileID_Equ3\" class=\"mathdisplay\"\u003e$$\\:\\text{F}={\\text{C}}_{\\text{e}\\text{x}\\text{t}}/{\\text{C}}_{0}$$\u003c/div\u003e\n\u003cdiv class=\"EquationNumber\"\u003e3\u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003eIn these relationships, V₀ and Vₑₓₜ represent the volumes of the aqueous solution of the Pb(II) sample under extraction (4000 \u0026micro;L) and the extractant solvent (100 \u0026micro;L), respectively. Qₑₓₜ and Q₀ represent the extracted and initial amounts of Pb(II), respectively. According to the calculations performed, the extraction efficiency was 89% and the concentration factor was 35.95.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eExtraction and Measurement of Pb(II) in Real Samples\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe results obtained from the quantitative analysis for determining the Pb(II) content in Lake Zarivar water samples, cosmetic materials (lipstick), and five different vegetable species are shown in Table\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e. The accuracy of the proposed analytical method was assessed by incorporating specific quantities of standard Pb(II) solution into the real sample matrix. The recovery percentage, which ranged from 97.9\u0026ndash;103.6%, demonstrated that the precision and accuracy of the method were acceptable. These results confirm that the synthesized adsorbent can effectively extract Pb(II) from real samples with complex matrices.\u003c/p\u003e\n\u003cp\u003eBased on the obtained results and calculations, the Pb(II) concentrations in basil, lettuce, parsley, coriander, leek, and lipstick samples were determined to be 0.1065, 0.1185, 0.0825, 0.0945, 0.0885, and 9.9400 \u0026micro;g/g, respectively. These data demonstrate the importance of the developed extraction method for analytical applications in environmental and biological sample analyses.\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003ctable id=\"Tab2\" border=\"1\"\u003e\u003ccaption\u003e\n\u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e\n\u003cdiv class=\"CaptionContent\"\u003e\n\u003cp\u003eResults of Pb(II) measurements in real samples using MPTMS-GP sorbent by MEPS method with GF-AAS\u003c/p\u003e\n\u003c/div\u003e\n\u003c/caption\u003e\n\u003cthead\u003e\n\u003ctr\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eSample\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eAdded (\u0026micro;g/L)\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eFound (\u0026micro;g/L)\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eRecovery (%)\u003c/p\u003e\n\u003c/th\u003e\n\u003c/tr\u003e\n\u003c/thead\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eBasil\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e8.50\u003c/p\u003e\n\u003cp\u003e13.70\u0026thinsp;\u0026plusmn;\u0026thinsp;0.08\u003c/p\u003e\n\u003cp\u003e18.45\u0026thinsp;\u0026plusmn;\u0026thinsp;0.11\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e103.60\u003c/p\u003e\n\u003cp\u003e99.30\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eLettuce\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e9.48\u003c/p\u003e\n\u003cp\u003e14.60\u0026thinsp;\u0026plusmn;\u0026thinsp;0.13\u003c/p\u003e\n\u003cp\u003e19.41\u0026thinsp;\u0026plusmn;\u0026thinsp;0.09\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e102.40\u003c/p\u003e\n\u003cp\u003e99.30\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eChervil\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e6.60\u003c/p\u003e\n\u003cp\u003e11.61\u0026thinsp;\u0026plusmn;\u0026thinsp;0.07\u003c/p\u003e\n\u003cp\u003e16.43\u0026thinsp;\u0026plusmn;\u0026thinsp;0.12\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e100.20\u003c/p\u003e\n\u003cp\u003e98.30\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eCoriander\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e7.56\u003c/p\u003e\n\u003cp\u003e12.50\u0026thinsp;\u0026plusmn;\u0026thinsp;0.11\u003c/p\u003e\n\u003cp\u003e17.40\u0026thinsp;\u0026plusmn;\u0026thinsp;0.09\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e98.80\u003c/p\u003e\n\u003cp\u003e98.40\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eLeek\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e7.08\u003c/p\u003e\n\u003cp\u003e12.07\u0026thinsp;\u0026plusmn;\u0026thinsp;0.07\u003c/p\u003e\n\u003cp\u003e16.94\u0026thinsp;\u0026plusmn;\u0026thinsp;0.10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e99.80\u003c/p\u003e\n\u003cp\u003e98.60\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eLip stick\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e39.77\u003c/p\u003e\n\u003cp\u003e44.80\u0026thinsp;\u0026plusmn;\u0026thinsp;0.17\u003c/p\u003e\n\u003cp\u003e50.10\u0026thinsp;\u0026plusmn;\u0026thinsp;0.15\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e100.60\u003c/p\u003e\n\u003cp\u003e103.30\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eWater (Zerivar lake)\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0\u003c/p\u003e\n\u003cp\u003e5\u003c/p\u003e\n\u003cp\u003e10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e6.45\u003c/p\u003e\n\u003cp\u003e11.58\u0026thinsp;\u0026plusmn;\u0026thinsp;0.10\u003c/p\u003e\n\u003cp\u003e16.24\u0026thinsp;\u0026plusmn;\u0026thinsp;0.12\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e\u0026ndash;\u0026ndash;\u003c/p\u003e\n\u003cp\u003e102.60\u003c/p\u003e\n\u003cp\u003e97.90\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003e\u003cstrong\u003eComparison of the Proposed Method with literature\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eA comparison of the analytical performance of the Pb(II) extraction and measurement method using the MPTMS-GP adsorbent with other adsorbents and analytical methods reported in previous studies is presented in Table\u0026nbsp;3. The analytical parameters demonstrate that the proposed method exhibits significant performance in terms of the linear calibration range and extraction accuracy compared to other similar adsorbents and analytical methods. Furthermore, the LOD obtained from this method showed satisfactory results compared to the values reported in reliable sources, indicating the efficiency of the synthesized adsorbent in extracting and measuring low concentrations of Pb(II) in the samples.\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u003cstrong\u003eTable\u0026nbsp;3.\u003c/strong\u003e Comparison of the proposed method for Pb (II) extraction and determination using the synthesized MPTMS-GP sorbent by MEPS with graphite furnace atomic absorption spectrometry with other reported methods\u0026nbsp;\u003c/div\u003e\n\u003cdiv class=\"colspec\" align=\"left\"\u003e\u0026nbsp;\u003c/div\u003e\n\u003ctable id=\"Tabg\" border=\"1\"\u003e\n\u003cthead\u003e\n\u003ctr\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eMethods\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eLinear range (ng/mL)\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eLOD (ng/mL)\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eRSD\u003c/p\u003e\n\u003cp\u003e(n\u0026thinsp;=\u0026thinsp;3)\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003e%Recovery\u003c/p\u003e\n\u003c/th\u003e\n\u003cth align=\"left\"\u003e\n\u003cp\u003eReference\u003c/p\u003e\n\u003c/th\u003e\n\u003c/tr\u003e\n\u003c/thead\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e2,2\u0026prime;-dipyridyl ketone\u003c/p\u003e\n\u003cp\u003eSPE\u003c/p\u003e\n\u003cp\u003eAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.6\u0026ndash;10.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e2.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e98\u0026ndash;98.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e61\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003ePHBvbNCl\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eSPME\u003c/p\u003e\n\u003cp\u003eFAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.1\u0026ndash;250\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.03\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e1.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e97.7\u0026ndash;98.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e62\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eNCp\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eVS-SPE\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eFAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e20\u0026ndash;120\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e6.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e4.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e94\u0026ndash;100\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e63\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eox-MWCNTd\u003c/p\u003e\n\u003cp\u003eDMSPE\u003c/p\u003e\n\u003cp\u003eFAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e2\u0026ndash;25\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.25\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e2.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e98.5\u0026ndash;106.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e64\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eMWCNT\u003csup\u003ee\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eDMSPE\u003c/p\u003e\n\u003cp\u003eGF-AAS\u003csup\u003ef\u003c/sup\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.2\u0026ndash;10\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.003\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e65\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eAg/Ni@g-C3N4\u003c/p\u003e\n\u003cp\u003eDSPME\u003csup\u003eg\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eFAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e270\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e4.06\u0026ndash;5.2%\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e-98.5\u0026ndash;104.1%\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e66\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eSPE\u003c/p\u003e\n\u003cp\u003eMNPs-BP\u003c/p\u003e\n\u003cp\u003eFAAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.523\u0026ndash;0.876\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.519\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e4.02%\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e97\u0026thinsp;\u0026plusmn;\u0026thinsp;5%\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e[\u003cspan class=\"CitationRef\"\u003e67\u003c/span\u003e]\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eGlass powder (TEOS) /MPTMS\u003c/p\u003e\n\u003cp\u003eMEPS\u003c/p\u003e\n\u003cp\u003eGF-AAS\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.01-50\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e0.0013\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e1.71\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003e97.9\u0026ndash;103.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd align=\"left\"\u003e\n\u003cp\u003eThis work\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003ctfoot\u003e\n\u003ctr\u003e\n\u003ctd colspan=\"6\"\u003e\u003csup\u003ea\u003c/sup\u003ePoly-3-hydroxy butyrate-polyvinyl triethyl ammonium chloride comb-type amphiphilic cationic block copolymer, \u003csup\u003eb\u003c/sup\u003eNano clinoptilolite modified with 5(p-dimethyl aminobenzylidene), \u003csup\u003ec\u003c/sup\u003e Vortex-assisted solid phase extraction\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd colspan=\"6\"\u003e\u003csup\u003ed\u003c/sup\u003e Oxidized multiwalled carbon nano tubes, e Multiwalled carbon nano tubes, \u003csup\u003ef\u003c/sup\u003e Graphite furnace atomic absorption spectrometry, \u003csup\u003eg\u003c/sup\u003e Dispersive Solid Phase Microextraction\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tfoot\u003e\n\u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e"},{"header":"Conclusion","content":"\u003cp\u003eIn this study, an innovative microextraction method was developed, employing glass powder modified with 3-mercaptopropyltrimethoxysilane (MPTMS) to concentrate Pb(II) ions in water-based solutions. The MPTMS-GP glass powder exhibited outstanding adsorption capacity, a strong preference for Pb(II) ions, and good reusability over several extraction cycles. The process was optimized using the following parameters: five extraction cycles, ten elution cycles, a pH of 6, 1 M hydrochloric acid as the elution solvent, 100 \u0026micro;L of elution solvent volume, and 2 mg of adsorbent. The method demonstrated a low limit of detection (LOD) of 0.0013 ng/mL, achieved a recovery rate ranging from 97.9\u0026ndash;103.6%, and had a concentration factor of 35.95, making it an exceptionally effective tool for identifying Pb(II) in practical samples. The robustness of the method was established by testing it on various environmental and food samples, including water, vegetables, and cosmetic products. These findings validate the practical utility of the proposed method for analyzing real-world samples. The MPTMS-GP adsorbent stands out from current methods because of its enhanced sensitivity, selectivity, and cost efficiency, making it a promising option for monitoring environmental conditions and conducting health-related research on heavy metals.\u003c/p\u003e\u003cp\u003e\u003cb\u003eAuthorship contribution statement\u003c/b\u003e\u003c/p\u003e\u003cp\u003eSorour karimi: Investigation, Writing \u0026ndash; original draft, Soleiman Bahar: Methodology, Supervision, Writing \u0026ndash; review \u0026amp; editing, Parisa Poormoghadam: Writing \u0026ndash; original draft.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003ch2\u003eDeclaration of competing interest\u003c/h2\u003e\u003cp\u003eThe authors declare that they have no conflicts of interest.\u003c/p\u003e\u003c/p\u003e\u003ch2\u003eFunding\u003c/h2\u003e\u003cp\u003eThere was no Funding for this work.\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eSorour karimi: Investigation, Writing \u0026ndash; original draft, Soleiman Bahar: Methodology, Supervision, Writing \u0026ndash; review \u0026amp; editing, Parisa Poormoghadam: Writing \u0026ndash; original draft.\u003c/p\u003e\u003ch2\u003eAcknowledgement\u003c/h2\u003e\u003cp\u003eWe thank the University of Kurdistan for its support in all aspects of the above project\u003c/p\u003e\u003ch2\u003eData Availability\u003c/h2\u003e\u003cp\u003eThe datasets used and/or analysed during the current study are available from the corresponding author on reasonable request.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eMashhadizadeh, M. 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Water Treat.\u003c/em\u003e \u003cb\u003e92\u003c/b\u003e, 245\u0026ndash;254. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.5004/dwt.2017.21497\u003c/span\u003e\u003cspan address=\"10.5004/dwt.2017.21497\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e (2017).\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Pb(II) preconcentration, microextraction in a packed syringe, MPTMS-modified glass powder, atomic absorption spectrometry, lead, environmental analysis","lastPublishedDoi":"10.21203/rs.3.rs-7232218/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7232218/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eAccurate measurement of lead (Pb) in water samples is critical because of its high toxicity and potential to accumulate in living organisms, leading to serious health risks such as anemia, kidney damage, and neurological disorders. This study introduces a novel microextraction technique for the preconcentration of Pb(II) ions using glass powder modified with 3-mercaptopropyltrimethoxysilane (MPTMS-GP). The MPTMS-GP adsorbent was synthesized via surface modification and characterized using Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The Pb(II) extraction efficiency was optimized using the microextraction in a packed syringe (MEPS) technique, with graphite furnace atomic absorption spectrometry (GFAAS) for quantification. The optimal conditions for Pb(II) extraction were five extraction cycles, a pH of 6, 2 mg of adsorbent, 100 \u0026micro;L of 1 M hydrochloric acid for elution, and a sample volume of 4 mL. The method demonstrated a limit of detection (LOD) of 0.0013 ng/mL and a linear range of 0.01\u0026ndash;50 \u0026micro;g/L, showing excellent sensitivity. The MPTMS-GP adsorbent exhibited remarkable selectivity for Pb(II), achieving recovery rates between 97.9% and 103.6% in real samples, such as water, vegetables, and cosmetics. The preconcentration factor was calculated to be 35.95, indicating the method\u0026rsquo;s efficiency. This approach offers a highly effective, precise, and eco-friendly solution for the extraction and quantification of Pb(II) in environmental and biological sample.\u003c/p\u003e","manuscriptTitle":"A Novel Microextraction Technique for Pb(II) Ion Preconcentration Using 3-Mercapto Propyltrimethoxysilane- Modified Glass Powder","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-08-07 15:57:10","doi":"10.21203/rs.3.rs-7232218/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"6fb68d68-594c-4e79-bf73-b9c01913091b","owner":[],"postedDate":"August 7th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[{"id":52716405,"name":"Physical sciences/Chemistry"},{"id":52716406,"name":"Earth and environmental sciences/Environmental sciences"}],"tags":[],"updatedAt":"2025-08-29T17:23:34+00:00","versionOfRecord":[],"versionCreatedAt":"2025-08-07 15:57:10","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-7232218","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7232218","identity":"rs-7232218","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}