Solid Phase Extraction Of Lead Research Articles

Micro solid phase extraction of lead and cadmium using functionalized nanodiamonds@CuAl2O4@HKUST-1 nanocomposite for FAAS analysis in food and water samples

This study focuses on the development and application of a novel nanocomposite (functionalized nanodiamonds@CuAl2O4@HKUST-1)-based µ-SPE method for the sensitive and selective extraction of Pb and Cd from food and water samples. The technique offers high sensitivity and selectivity, allowing accurate measurement of these metals at trace levels. The detection limit is 0.031 µg kg−1 for Cd and 0.052 µg kg−1 for Pb, with a relative standard deviation of 1.7 % for Cd and 4.8 % for Pb. The method was successfully applied to real samples and efficiently quantified Pb and Cd in food and natural water samples. The highest concentrations were found in red lentils (0.274 µg kg−1 Pb) and fresh mint (0.197 µg kg−1Cd), but still below recommended limits set by FAO/WHO (300 µg kg−1 for Pb and 200 µg kg−1 for Cd). It promises to ensure food safety, monitor environmental contamination, and informs regulatory decisions to protect public health.

Metal organic framework composite (Ti3AlC2 @ZIF-67) for vortex assisted solid phase extraction of lead from water and food samples

A composite of Ti3AlC2 max phase and ZIF-67 metal-organic framework (Ti3AlC2 @ ZIF- 67) was synthesized by mixing Ti3AlC2 and ZIF-67 in dimethyl formamide and used for solid phase extraction of Pb(II). Fourier transformation infrared spectroscopy, scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray were used to find functional group, surface morphology, surface area elemental composition, and crystalline structure of Ti3AlC2 @ ZIF-67. Factors like solution pH (7.0), adsorbent dose (10.0 mg), sample volume, eluent concentration and volume (0.5 M, 1.0 mL), and vortex time (1.0 min) were optimized. The effect of interfering ions has been checked to determine the method's selectivity. Analytical parameters such as limit of detection (LOD) 0.26 µg L−1, limit of quantification (LOQ) 0.86 µg L−1, preconcentration factor (PF) 21, enhancement factor (EF) 20 and relative standard deviation (RSD) 4.6% were calculated under optimized experimental condition. Certified reference materials TMDA-64.3 water samples and INCT-OBTL-5 tobacco leaves were used to validate the accuracy of the proposed method for trace metals detection. The technique was also used for lead determination in food and water samples with satisfactory recovery results.

Synthesis of Silica Gel Chelated with Alizarin and 1-Nitroso-2-Naphthol for Solid Phase Extraction of Lead in Ground Water Samples

Silica gel chemically functionalized with alizarin (Si-AZ) and 1-nitroso-2-naphthol (Si-NN) was synthesized and characterized by FT-IR, N2 adsorption-desorption, SEM, and elemental analysis. The two chelators show adequate sorption properties for Pb (II) and are hence used as SPE sorbents prior to their determination with ICP-MS. Both chelators showed high sorption efficiency for the Pb (II) ion at pH 8. Batch experiments demonstrate that the synthesized resins could remove more than 95% Pb (II) out of solutions containing 100 μg/mL of the ion. At optimum conditions, the maximum adsorption capacities for S-TDI-AZ and S-TDI-NN for Pb (II) were 9.56 and 9.43 mg/g, respectively. Method development was performed to investigate the applicability of the chelating resins as packing materials for SPE using model solutions and real groundwater samples. The method detection limits of SPE were 0.0025 and 0.0026 μg/L with high precision (R.S.D. < 3%). The recoveries of spiked Pb (II) with ground water were 104.70 and 102.62%. The proposed method was successfully applied to the determination of Pb (II) in the groundwater by ICP-MS.

Magnetic solid phase extraction of lead(II) from food and water samples on magnetic MWCNTs/MgAl2O4/TiO2

A magnetic [email protected]2O4@TiO2 novel nanocomposite was synthesized using the sol-gel method. The characterization of synthesized nanocomposite was done using FTIR, XRD, and SEM techniques. The adsorbent was used for dispersive solid-phase extraction of Pb(II). The analytical parameters that affect the extraction recovery of the analyte were optimized, involving the pH, adsorbent amount, sample volume, and interfering ions. The figures of merit such as preconcentration factor (PF), the limit of detection (LOD), the limit of quantification (LOQ), correlation coefficient (R2) and relative standard deviation (RSD) of Pb(II) are 100, 0.42 μg L−1, 1.39 μg L−1, 0.996 % and 4.1 % respectively. TMDA 64.3 fortified lake water and NCS DC 73349 bush, branches and leaves certified reference materials were used to validate the presented procedure. The synthesized adsorbent was used for separation-preconcentration and determination Pb(II) from water and food samples prior to its determination by FAAS.

Magnetic Adsorbent Decorated with Poly(N-Isopropylacrylamide) (PNIPAM) Brushes for the Vortex-Assisted Solid Phase Extraction (VASPE) of Lead in Water, Cigarettes and Soil with High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) Detection

Here is reported the synthesis of a magnetic phosphorus-containing adsorbent decorated with poly(N-isopropylacrylamide) (PNIPAM) brushes via surface-initiated atom transfer radical polymerization (SI-ATRP) and its application for vortex assisted solid phase extraction of lead in water, cigarettes and soil. The adsorbent was characterized using Fourier-transform infrared spectroscopy (FT-IR) and energy dispersive x-ray (EDX) spectroscopy. A high-resolution continuum source flame atomic absorption spectrometer (HR-CS FAAS) was used for the quantification of lead. All factors affecting the extraction efficiency including the solution pH, adsorbent dose, sample volume, vortex time, and elution protocols were optimized. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.05 µg L−1 and 0.18 µg L−1, respectively. The preconcentration and enhancement factors were 20 and 18. Validation was performed using TMDA 64.3 fortified water and INCT-OBTL-5 tobacco leaves certified reference materials with satisfactory recoveries. The method was shown to be sensitive, efficient and reproducible.

Magnetic dispersive solid phase extraction of lead(II) as dithizone chelates in food and environmental samples on Fe3O4@XAD-8 prior to its flame atomic absorption spectrometric detection

ABSTRACT A magnetic dispersive solid phase extraction method has been developed using Fe3O4@XAD-8 adsorbent to separate and preconcentrate Pb (II) ions as dithizone chelates from environmental samples. Fe3O4@XAD-8 was characterised by SEM, FT-IR and BET methods. Analytical parameters such as pH, adsorbent amount, ligand volume, eluent type and volume, model solution volume and matrix effects which are effective on method recovery are optimised. Limit of detection (LOD) and limit of quantification (LOQ) values were 0.048 µg mL−1 and 0.159 µg mL−1, respectively. The accuracy of the developed method has been proven by TMDA – 64.2 certified reference material and addition-recovery studies in water samples. Lead content of some food and water samples was determined by using the developed dispersive magnetic solid-phase extraction method.

Fe3O4 nanoparticles coated with double imprinted polymers for magnetic solid phase extraction of lead(II) from biological and environmental samples.

Double imprinted polymer coated magnetic nanoparticles were fabricated with 4-nm size ZnO nanoparticles acting as the sacrifice templates, which were co-imprinted with template Pb(II) ions. After template removal, abundant transfer pores derived from ZnO nanoparticles were left around the selective adsorption sites derived from Pb(II) ions. The magnetic sorbent exhibit good selectivity, rapid adsorption kinetic and large adsorption capacity for Pb(II). They were used to extract trace Pb(II) followed by graphite furnace atomic absorption spectrometry detection. After the optimization of extraction conditions, following merits are found: (a) rapid extraction (10min), (b) high preconcentration factor (100 fold), (c) sensitive detection with the detection limit of 9.4ng·L-1, and (d) low relative standard deviation (6.9%) at a level of 50ng·L-1 of Pb(II) analyzed 7 times. The method was employed in extraction and quantification of trace Pb in biological and environmental samples with satisfactory recoveries of 87.5-104%. Graphical abstractDouble imprinted polymer coated magnetic nanoparticles (MNPs@DIP) were fabricated and used for extraction of Pb(II) followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. The method was successfully applied for the determination of Pb in environmental and biological samples.

Ultrasound-assisted magnetic solid phase extraction of lead and thallium in complex environmental samples using magnetic multi-walled carbon nanotubes/zeolite nanocomposite

Magnetic multi-walled carbon nanotubes@zeolite (MWCNT-Fe3O4@Zeo) nanocomposite was facilely synthesized using a one-pot solvothermal method. The MWCNT-Fe3O4@Zeo was characterized by VSM, BET, XRD, TEM and SEM/EDS. The Zeolite-coated multi-walled carbon nanotubes–magnetite was used as an adsorbent in ultrasonic-assisted magnetic solid phase extraction (UA-MSPE) for preconcentration of trace Pb and Tl. The analytes were detected and quantified using inductively coupled plasma optical emission spectrometry (ICP-OES). The optimization of experimental parameters affecting the preconcentration method was achieved using a multivariate approach. Under optimal experimental conditions, the linearity ranged from 0.1 to 500 μg L−1 for lead and 0.1–600 μg L−1 for thallium. Preconcentration factors, limits of detection and quantification for Pb and Tl ranged from 90 to 100, 0.28–0.23 μg L−1, 0.93–0.77 μg L−1. The intraday precisions (repeatability, n = 20) expressed as the relative standard deviation, were found to be 1.6% and 1.4% for Pb and Tl, respectively. In addition, the interday precisions (reproducibility, n = 5) were 2.6% and 3.1% for Pb and Tl, respectively. The accuracy of the method was investigated using standard reference material as well as spiked recovery test and satisfactory recoveries (97–99.3%) were obtained. The maximum adsorption capacities were 37.8 mg g−1 and 44.5 mg g−1, for Pb and Tl, respectively. The developed UA-MSPE/ICP-OES method was effectively applied for simultaneous preconcentration and determination of Pb and Tl in environmental samples.

Dispersive solid phase extraction of lead in water samples using embedded 1,5-diphenylcarbazone grafted graphene oxide in microporous magnetic chitosan coupled with flame atomic absorption spectrometry

In the current study, an embedded 1,5-diphenylcarbazone (DPC) grafted graphene oxide (GO) in porous magnetic chitosan (MC) nanocomposite was synthesized and used for preconcentration of trace amount of Pb(II). For this purpose, a magnetic dispersive solid phase extraction (MDSPE) was utilized prior to determination by flame atomic absorption spectrometry (FAAS). The adsorbent was characterized using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The parameters influencing the extraction efficiency such as pH, extraction and desorption time, adsorbent amount and type, concentration and volume of eluent were optimized by design of experiment. Under the optimum conditions, calibration curve was linear within the range of 3.0–300 ng mL−1 with regression coefficient of 0.9957. The enhancement factor was obtained as 13.5 corresponding to the absolute recovery of 81%. The limits of detection (LOD, 3Sb/m) and quantification (LOQ) were found to be 0.13 ng mL−1 and 0.43 ng mL−1, respectively. Intra- and inter-day precisions (n = 5) were estimated using the relative standard deviation (RSD%) at three concentrations of 25, 100 and 250 ng mL−1 and were less than 3.2% and 5.6%, respectively. The maximum adsorption capacity (qm), calculated by the Langmuir equation, was found to be 57.47 mg g−1. The method was validated by analysis of an SRM-1643f standard reference material for trace elements in water. Finally, the method was successfully applied for the determination of trace amount of Pb(II) in various water samples with good relative recoveries ranged from 92.3 to 105%.

Synthesis of a magnetic WO3 nanocomposite for use in highly selective preconcentration of Pb(II) prior to its quantification by FAAS.

A novel sorbent consisting of WO3 and Fe3O4 is described for preconcentration of Pb(II). It was prepared without consumption of organic solvents. The nano composite was characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, alternating gradient force magnetometer and Brunauer-Emmett-Teller. Having high surface area and being formed oxygen sheets propose the nanocomposite as a sorbent. Adsorption and desorption conditions were optimized and Pb(II) is quantified by flame atomic absorption spectroscopy. The sorbent can highly selectively preconcentrate Pb(II) at pH values between 3 and 7. The preconcentration time is short and sorbent is re-usable. Under the optimized conditions, the method has the following figures of merit: (a) limit of detection of 0.60ngmL-1, (b) relative standard deviation (n= 5) of 0.87%, (c) preconcentration factor of 33.33 and (d) linearity of dynamic range (10-200ng.mL-1). Isotherm adsorption, kinetic adsorption and thermodynamic adsorption were stablished. The material was applied to the preconcentration of Pb(II) from herbal medicines. Graphical abstract Schematic presentation of a nanocomposite (Fe3O4 - WO3) that was prepared from sodium tungstate (Na2WO4), oxalic acid, HCl and magnetic Fe3O4 nanoparticles for the magnetic solid phase extraction of lead at trace levels.

Preconcentration of Pb(II) by using Mg(II)-doped NiFe2O4 nanoparticles as a magnetic solid phase extraction agent.

Magnesium(II)-doped nickel ferrite (Mg-NiFe2O4) nanoparticles are introduced as a new adsorbent for magnetic solid phase extraction of lead(II) ions from aqueous solutions. The structure and morphology of the adsorbent was characterized by FTIR, X-ray diffraction and scanning electron microscopy. The effects of pH value, amount of adsorbent, type, concentration and volume of the eluent and adsorption/desorption time on the extraction efficiency were studied. Following elution with hydrochloric acid, Pb(II) ions were quantified by flame atomic absorption spectrometry. Under optimized conditions, the calibration graph is linear in the 0.5-125ngmL-1 Pb(II) ion concentration range. Other figures of merit include (a) a 0.2ngmL-1 limit of detection, (b) an enrichment factor of 200, (c) an intra-day relative standard deviation (for n= 6 at 50ngmL-1) of 1.6%, and (d) an inter-day precision of 3.8%. The method was validated by the analysis of the certified reference material, NIST SRM 1566b. It was successfully applied to the determination of Pb(II) ion in spiked water samples, industrial wastewater and acidic lead battery waters. Graphical abstract Schematic of the synthesis of Mg(II)-doped NiFeO4 nanoparticles and their application as a magnetic sorbent for solid-phase extraction of a Pb(II) ions prior to determination by flame atomic absorption spectrometry (FAAS).

Magnetic Solid Phase Extraction of Lead, Cadmium, and Cobalt on Magnetic Carboxyl-Modified Nanodiamonds (MCNDs) from Natural Water Samples and Their Determination by Flame Atomic Absorption Spectrometry

Magnetic Solid Phase Extraction of Lead, Cadmium, and Cobalt on Magnetic Carboxyl-Modified Nanodiamonds (MCNDs) from Natural Water Samples and Their Determination by Flame Atomic Absorption Spectrometry

Vortex assisted solid-phase extraction of lead(II) using orthorhombic nanosized Bi2WO6 as a sorbent.

Nanosized single crystal orthorhombic Bi2WO6 was synthesized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The crystal and molecular structure of the sorbent was examined using XRD, Raman, SEM and SEM-EDX analysis. Various parameters affecting extraction efficiency were optimized by using multivariate design. The effect of diverse ions on the extraction also was studied. Lead was quantified by flame atomic absorption spectrometry (FAAS). The recoveries of lead(II) from spiked samples (at a typical spiking level of 200-400ng·mL-1) are >95%. Other figures of merit includes (a) a detection limit of 6ng·mL-1, (b) a preconcentration factor of 50, (c) a relative standard deviation of 1.6%, and (d) and adsorption capacity of 6.6mg·g-1. The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples. Graphical abstract Nanosized single crystal orthorhombic Bi2WO6 was synthesized and characterized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples.

Nanodiamond/MoS2 nanorod composite as a novel sorbent for fast and effective vortex-assisted micro solid phase extraction of lead(II) and copper(II) for their flame atomic absorption spectrometric detection

This study is a report on the synthesizing nanodiamond/MoS2 nanorod composite using the hydrothermal method and its application as adsorbent in micro solid phase extraction of lead(II) and copper(II) prior their determination through flame atomic absorption spectroscopy. The nanodiamond/MoS2 nanorod composite was characterized using Raman spectroscopy, BET surface analysis and scanning electronic microscopy (SEM). The optimal conditions including amount of used adsorbent, pH, vortex time, elution condition and volume investigated. Quantitative recoveries for both analytes were obtained at pH3.0. The preconcentration factor is 35, and the sorption capacity of synthesized adsorbent for lead(II) and copper(II) is 19.87 and 49.33mgg−1. The relative standard deviation is 0.9 and 1.5% for lead(II) and copper(II) at a level of 200μgL−1 (n=6), and the detection limit is 42 and 22μgL−1 for lead(II) and copper(II), respectively. The procedure accuracy was proved via analyzing the standard reference materials (SPS-WW2 Waste water Level 2 and TMDA-53.3). The presented procedure was applied for the determination of copper and lead contents of the water samples from Turkey.

Vortexing/shaking-free solid phase extraction of lead(II) by using an urchin-like NiCo2O4 hollow microsphere adsorbent

Urchin-like NiCo2O4 hollow microspheres were synthesized by a solvothermal method and characterized by using X-ray diffraction, scanning electron microscopy, Brunauer–Emmett–Teller surface area, and zeta potential measurements. It was used as an adsorbent for the solid phase extraction of Pb(II) from water, food and street dust samples prior to its extraction with dilute HCl and its determination by FAAS. Figures of merit include a preconcentration factor of 30, a detection limit of 5.9 μg L−1 and a relative standard deviation of 2.4%. The major advantage of the method is the fast equilibration during extraction without the need for vortexing or shaking. The method was successfully accurated by analyzing certified reference materials (BCR-482 Lichen, TMDA-70 Lake water and RM 8704 Buffalo River Sediment) and by analyzing spiked sea water, wastewater, well water, apple, eggplant, broccoli, ginger, lentil and street dust samples.

Vortex assisted magnetic solid phase extraction of lead(II) and cobalt(II) on silica coated magnetic multiwalled carbon nanotubes impregnated with 1-(2-pyridylazo)-2-naphthol

In the present study, silica coated magnetic multiwalled carbon nanotubes impregnated with 1-(2-pyridylazo)-2-naphthol was synthesized and characterized by using instrumental techniques such as, Fourier transform infrared spectroscopy (FT-IR), BET surface area analysis, scanning electron microscopy (SEM) and X-ray diffraction (XRD). The novel adsorbent has been used for magnetic solid phase extraction of Pb(II) and Co(II) at trace levels. The parameters including pH of solution, adsorbent dose, sample volume, temperature and matrix effect were optimized. Quantitative recoveries for analytes were obtained at pH6.5 with 100mg of adsorbent. Limit of detection values for lead and cobalt were 1.76μgL−1 and 0.55μgL−1. Preconcentration factor and standard deviation of both metals were 15 and lower than 3.3%. Kinetic data shows that the adsorption process follows pseudo second order kinetic. Positive values of ΔH° and ΔS° show that adsorption of Pb(II) and Co(II) is feasible and endothermic in nature. The validation of the method was carried out to waste water certified water reference materials. The presented separation-preconcentration method was applied to determination of lead and cobalt contents of water samples from Kayseri-Turkey.

Sorption properties of an amorphous hydroxo titanate towards Pb2+, Ni2+, and Cu2+ ions in aqueous solution

ABSTRACTTitanates may be selectively used as inorganic adsorbents for heavy metal ions owing to their stability and fast adsorption kinetics. Nevertheless, the synthesis of such materials usually requires extreme reaction conditions. In this work, a new titanium-based material was rapidly synthesized under mild laboratory conditions. The obtained amorphous hydroxo titanate was tested for heavy metal sorption through kinetic and equilibrium batch tests, which indicated that the new material had high adsorption rates and adsorption capacities towards Cu2+, Ni2+ and Pb2 ions. Adsorption kinetics were pseudo-second order, and equilibrium data fitted the Langmuir isotherm model. The calculated maximum adsorption capacities of Cu2+, Ni2+ and Pb2+ in deionized water were around 1 mmol g−1, and they decreased for Cu2+ and Ni2+ in the presence of Na+, Ca2+ and Mg2+ ions, whereas the alkali metal ions did not influence Pb2+ uptake. The efficiency of adsorption and recovery of lead ions were evaluated through column dynamic tests, by feeding the column with groundwater and tap water spiked with Pb2+. The high performance of the hydroxo titanate over several cycles of retention and elution suggested that the product is potentially useful for the solid phase extraction of lead at trace levels in natural water samples, with potential use in metal pre-concentration for analytical applications.

Solid phase extraction of lead, cadmium and zinc on biodegradable polyhydroxybutyrate diethanol amine (PHB-DEA) polymer and their determination in water and food samples

A new biodegradable polyhydroxybutyrate diethanol amine (PHB-DEA) polymer was used as adsorbent for the sensitive and selective separation, preconcentration and determination of Pb(II), Cd(II) and Zn(II) by using atomic absorption spectrometry. Diethyl dithiocarbamate was used as chelating reagent. Analytical parameters such as pH, eluent type and its volume, flow rates of sample solution, ligand amount, sample volume were optimized. Effects of some cations, anions and transition metal ions were also investigated. Enrichment factor and relative standard deviation were found to be 100 and 3%, respectively. The limits of detection based on three times standard deviation of blanks (N=21) were found 1.05μgL−1 for Pb(II), 0.42μgL−1 for Cd(II) and 0.13μgL−1 for Zn(II). Limits of quantification (10s, N=21) were found 3.47μgL−1 for Pb(II), 1.39μgL−1 for Cd(II) and 0.43μgL−1 for Zn(II). Accuracy evaluation of the method was confirmed with analyses of certified reference materials (NIST SRM 1515 Apple leaves, IAEA 336 Lichen, GBW 07605 Tea). Optimized method was applied to tap water and food samples after microwave digestion method. Cadmium and lead values in some samples were found higher than legal limits.

Synthesis and application of novel ion-imprinted polymer coated magnetic multi-walled carbon nanotubes for selective solid phase extraction of lead(II) ions

In this study, novel magnetic ion-imprinted polymer (MIIP) nanoparticles were utilized for the sensitive and selective detection of Pb(II) ions by graphite furnace atomic absorption spectrometry (GFAAS). The Pb(II)-imprinted polymer was synthesized by using 4-vinylpyridine (4VP) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) as the chelating agent and magnetic multi-walled carbon nanotubes (MMWCNTs) as the carrier. The synthesized MIIP materials were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Various analytical parameters such as extraction and desorption time, eluent type and concentration, pH and sample volume were systematically examined. The selectivity of MIIP sorbent for Pb(II) ions in the presence of some cations was also evaluated. The limit of detection (LOD, 3Sb) and the relative standard deviation (RSD, n=8, c=25ngL−1) were found to be 2.4ngL−1 and 5.6%, respectively. The maximum sorption capacity of the MIIP for Pb(II) was found to be 48.1mgg−1. Finally, the proposed analytical procedure was successfully applied to monitoring lead in human hair and water samples with satisfactory results for the spiked samples.

Magnetic solid phase extraction of lead(ii) and cadmium(ii) on a magnetic phosphorus-containing polymer (M-PhCP) for their microsampling flame atomic absorption spectrometric determinations

A new magnetic phosphorus-containing polymeric sorbent was successfully used in solid phase extraction for the simple, fast and efficient preconcentration of trace Pb and Cd from environmental water samples.