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1.
Environ Res ; 252(Pt 4): 119065, 2024 May 07.
Article En | MEDLINE | ID: mdl-38723990

The present research study combines chitin from shrimp waste with the oxide-rich metakaolin. Metakaolin is a blend of mixed oxides rich in silica and alumina with good adsorbent properties. The chitin@metakaolin (CHt@M.K.) composite was synthesized and characterized using FTIR, SEM, TGA, XRD and XPS techniques. Cr(VI) removal studies were compared for chitin and CHt@M.K. through adsorption. It was found that the adsorption capacity of CHt@M.K. is 278.88 mg/g, almost double that of chitin, at pH 5.0 in just 120 min of adsorption. Isotherm models like Langmuir, Freundlich, Temkin and Dubinin-Radushkevich were investigated to comprehend the adsorption process. It was revealed that Langmuir adsorption isotherm is most suitable to elucidate Cr(VI) adsorption on CHt@M.K. The adsorption kinetics indicate that pseudo first order was followed, indicating that the physisorption was the process that limited the sorption process rate. The positive enthalpy change (20.23 kJ/mol) and positive entropy change (0.083 kJ/mol K) showed that the adsorption process was endothermic and more random at the solid-liquid interface. The negative free energy change over entire temperature range was an indicator of spontaneity of the process. Apart from all these, the non-covalent interactions between Cr(VI) and composite were explained by quantum calculations based models.

2.
Environ Res ; 252(Pt 1): 118764, 2024 Mar 26.
Article En | MEDLINE | ID: mdl-38527722

The primary aim of this research is to comprehensively assess the applicability of chitosan biopolymer towards water treatment application and to enhance its adsorption capacity towards Remazol brilliant blue R-19 dye. This has been achieved through physical modification to obtain the material in hydrogel form and chemical modification by crosslinking it with barbituric acid. The characterization of the resulting Chitosan-barbituric acid hydrogel (CBH) was carried out using various analytical techniques such as SEM-EDX, FT-IR, TGA-DTA, XRD, and BET. CBH was employed as the adsorbent to eliminate R-19 dye from aqueous media. Utilizing response surface methodology (RSM), the parameters were fine-tuned, leading to the achievement of more than a 95% removal for R-19 dye. The adsorption behavior closely adhered to the Langmuir isotherm and pseudo-second-order kinetics. An interesting observation indicated that the rise in temperature leads to rise in adsorption capacity of CBH. The maximum adsorption capacities evaluated at 301.15 K, 313.15 K, 318.15 K, and 323.15 K were 566.6 mg g-1, 624.7 mg g-1, 671.3 mg g-1, and 713.5 mg g-1 respectively, in accordance with the Langmuir isotherm model. Examining the thermodynamics of the adsorption process revealed its spontaneous nature (ΔG = -21.14 to -27.09 kJ mol-1) across the entire temperature range. Furthermore, the assessment of the isosteric heat of adsorption (ΔHads) was conducted using the Clausius-Clapeyron equation, with results indicating an increase in ΔHads from 1.85 to 2.16 kJ mol-1 with temperature rise from 301.15 K to 323.15 K due to augmented surface loading. This suggested the existence of lateral interactions between the adsorbed dye molecules. The potential of adsorbent for regeneration was investigated, demonstrating the ability to reuse the material. Sustainability parameter calculated for synthesis process reflected a notably low E-factor value of 0.32 demonstrated the synthesis is environment friendly.

3.
Environ Res ; 247: 118228, 2024 Apr 15.
Article En | MEDLINE | ID: mdl-38246296

The primary aim of this investigation was to synthesise novel adsorbent by incorporating greenly synthesized zinc oxide nanoparticles into chitosan matrix (G-ZnO-Cs). The production of ZnO Nanoparticles via a green approach involved the utilization of extracts derived from Nymphaeaceae fronds. This assertion was substantiated by the application of Field Emission Scanning Electron Microscopy (FESEM) and X-ray Diffraction (XRD) analytical techniques. Several Analytical methods such as Fourier Transform Infrared spectroscopy (FT-IR), Energy Dispersive X-ray Analysis (EDAX), FESEM, Thermogravimetric Analysis (TGA), XRD, Brunauer-Emmett-Teller (BET) analysis, and point-of-zero charge determination were used to characterize G-ZnO-Cs. Further study investigates the impact of five key processing parameters, namely pH, interaction duration, G-ZnO-Cs dosage, temperature, and initial concentration of dyes, on the removal of three organic dyes Reactive Blue 19 (RB 19), Reactive Orange 16 (RO 16), and Congo Red (CR) The adsorption process of Reactive Blue 19 (RB 19), Reactive Orange 16 (RO 16), and Congo Red (CR) dyes on G-ZnO-Cs were determined to comply to the pseudo-second-order (PSO) and Langmuir models, as determined through equilibrium and kinetic experiments. The highest adsorption capabilities for RB 19, RO 16 and CR dye were revealed to be 219.6 mg/g, 129.6 mg/g, and 118.8 mg/g, respectively. The elimination success rate of the fixed-bed column approach for treating huge volumes was highlighted in the conducted research. Moreover, the G-ZnO-Cs composite exhibited significant reusability due to its ability to undergo elution and simultaneous regeneration processes.


Anthraquinones , Azo Compounds , Chitosan , Nanocomposites , Water Pollutants, Chemical , Zinc Oxide , Congo Red , Coloring Agents/chemistry , Chitosan/chemistry , Zinc Oxide/chemistry , Spectroscopy, Fourier Transform Infrared , Adsorption , Kinetics , Water Pollutants, Chemical/chemistry , Hydrogen-Ion Concentration
4.
Environ Res ; 242: 117762, 2024 Feb 01.
Article En | MEDLINE | ID: mdl-38029812

The objective of this research is to conduct a comprehensive characterization of chitosan while also improving its attributes by crosslinking with malonic acid, with a focus on its efficacy in removing hexavalent chromium, arsenite and fluoride ions. Crosslinking chitosan in 1:0.5 mass ratio forming a film led to substantial enhancement in confiscation of these target pollutants. The characterization of the adsorbent involved several techniques, including FT-IR, TGA-DSC, SEM-EDX, XRD, and BET surface area analysis. In batch adsorption experiments, Chitosan-malonic acid (CMA) was employed to remove CrVI, AsIII and F- from aqueous solutions. These experiments were conducted while varying conditions such as pH, dosage, concentration, temperature, and time. Through the implementation of response surface methodology (RSM), parameters were optimized, resulting in over 95% removal of CrVI, AsIII and F- ions. The isotherm and kinetics data demonstrated a good fit with the Langmuir isotherm model and pseudo second-order kinetics, respectively. According to the Langmuir isotherm, the maximum adsorption capacities on CMA for CrVI, AsIII and F- were determined to be 687.05 mg g-1, 26.72 mg g-1 and 51.38 mg g-1 respectively under optimum pH of 4.0, 7.0 and 5.0 respectively under ambient temperature of 303 K. Thermodynamic analysis indicated that the adsorption process was spontaneous and driven by enthalpy. The regenerability of the adsorbent was validated through five adsorption-desorption cycles, signifying its reusability. An assessment of the adsorbent's sustainability indicated an eco-friendly synthesis, as reflected by the low E-factor value of 0.0028.


Chitosan , Malonates , Water Pollutants, Chemical , Water Purification , Chitosan/chemistry , Spectroscopy, Fourier Transform Infrared , Adsorption , Water Pollutants, Chemical/chemistry , Water Purification/methods , Thermodynamics , Chromium/chemistry , Kinetics , Ions , Hydrogen-Ion Concentration
5.
Environ Res ; 244: 117921, 2024 Mar 01.
Article En | MEDLINE | ID: mdl-38101721

The novel glutamic acid crosslinked chitosan membrane (CsG) was fabricated and tested for its adsorption capabilities for the removal of multiple pollutants like Cr (VI), cyanide, fluoride and diclofenac sodium from wastewater. This fabricated CsG membrane was characterized by various techniques like FT-IR, SEM, EDX and XRD, BET to assess its structural, compositional and morphological properties. The working parameters studied by batch experiments were solution pH, CsG dose, contact time, pollutant concentration and solution temperature. The CsG membrane exhibited maximum adsorption capacity of 410.7 mg/g, 310.2 mg/g, 14.3 mg/g, 132.7 mg/g for Cr (VI), cyanide, fluoride and diclofenac respectively. The validation of the operational parameters was performed by Response Surface Methodology (RSM). The experimental data fitted well with Langmuir isotherm model and followed pseudo second order kinetics for all the four targeted contaminants. The spontaneity of the process was checked by thermodynamics studies. The high partition coefficients of 7669 L/kg Cr(VI), 23,309 L/kg (CN-), 649 L/kg (F-) and 2613 L/kg (DFC) are the indicators of excellent attractive interaction between CsG membrane and target toxicants. The CsG membrane showed efficient regenerative adsorption properties up to 5 adsorption-desorption cycles. Overall, the developed novel CsG membrane promised as an effective material for the removal of multiple number of pollutants from water.


Chitosan , Environmental Pollutants , Water Pollutants, Chemical , Water Purification , Chitosan/chemistry , Glutamic Acid , Spectroscopy, Fourier Transform Infrared , Fluorides , Chromium/chemistry , Water Pollutants, Chemical/chemistry , Water Purification/methods , Hydrogen-Ion Concentration , Thermodynamics , Adsorption , Kinetics , Cyanides
6.
ACS Omega ; 8(11): 10051-10061, 2023 Mar 21.
Article En | MEDLINE | ID: mdl-36969446

This work synthesized a novel chitosan-loaded MgAl-LDH (LDH = layered double hyroxide) nanocomposite, which was physicochemically characterized, and its performance in As(V) removal and antimicrobial activity was evaluated. Chitosan-loaded MgAl-LDH nanocomposite (CsC@MgAl-LDH) was prepared using cross-linked natural chitosan from shrimp waste and modified by Mg-Al. The main mechanisms predominating the separation of As(V) were elucidated. The characteristic changes confirming MgAl-LDH modification with chitosan were analyzed through Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetric analysis-differential thermal analysis, and Brunauer-Emmett-Teller measurements. Porosity and the increased surface area play an important role in arsenic adsorption and microbial activity. Adsorption kinetics follows the general order statistically confirmed by Bayesian Information Criterion differences. To understand the adsorption process, Langmuir, Freundlich, and Liu isotherms were studied at three different temperatures. It was found that Liu's isotherm model was the best-fitted model. CsC@MgAl-LDH showed the maximum adsorption capacity of 69.29 mg g-1 toward arsenic at 60 °C. It was observed that the adsorption capacity of the material rose with the increase in temperature. The spontaneous behavior and endothermic nature of adsorption was confirmed by the thermodynamic parameters study. Minimal change in percentage removal was observed with coexisting ions. The regeneration of material and adsorption-desorption cycles revealed that the adsorbent is economically efficient. The nanocomposite was very effective against Staphylococcus aureus and Bacillus subtilus.

7.
Int J Biol Macromol ; 223(Pt A): 636-651, 2022 Dec 31.
Article En | MEDLINE | ID: mdl-36370863

The aim of the study is to characterize and hierarchically modify chitosan using partially lateritized khondalite (PLK) rock. PLK is a metamorphic rock rich in mineral oxides and is not commercialized thus, treated as a mining reject. Chitosan was sequentially altered to Chitosan-PLK (Ch-PLK) and Chitosan-PLK-Epichlorohydrin (Ch-PLK-ECH) and both the materials were characterized by FT-IR, SEM, EDX, XRD, XRF and BET surface area analysis. The adsorbents were used for removal of cyanide ions from aqueous solution using batch adsorption experiments. The experiments were performed varying operational parameters and were optimized using RSM. The conditions optimized by RSM were carried out, more than 90 % of CN- adsorption was observed. The isotherm and kinetics studies have shown that the adsorption process fitted well with Langmuir isotherm model and pseudo second order kinetics. Using Langmuir isotherm, the maximum adsorption capacities of Ch-PLK and Ch-PLK-ECH towards cyanide ions at 30 °C were found to be 23.98 mg g-1 and 65.27 mg g-1 respectively. Thermodynamic studies described that adsorption process was spontaneous, enthalpy-driven over entire temperature range. Column studies established that the adsorbents may be applicable to large volume of samples. The adsorbents were tested for regeneration for 5 adsorption-desorption cycles suggesting reusability of the materials.


Chitosan , Water Pollutants, Chemical , Water Purification , Cyanides , Spectroscopy, Fourier Transform Infrared , Hydrogen-Ion Concentration , Temperature , Adsorption , Kinetics , Thermodynamics
8.
Chemosphere ; 306: 135524, 2022 Nov.
Article En | MEDLINE | ID: mdl-35779687

The primary goal of this study is to prepare and characterize a ghatti gum/poly(acrylic acid)/TiO2 (GG/poly(AA)/TiO2) hydrogel nanocomposite for adsorption of the dye malachite green (MG) from the aqueous phase in a discontinuous system. A variety of approaches were used to investigate the structure, morphology, and thermomechanical characteristics of the synthesized hydrogel nanocomposite. Response surface methodology (RSM) was performed to analyze the impact of three processing parameters, namely adsorbent dosage, dye concentration, contact duration, and their interactions on MG dye adsorption capacity. Analysis of variance was used to assess the experimental findings, which revealed that the quadratic regression model was statistically acceptable. The integration of TiO2 nanoparticles into the hydrogel matrix improved its thermal stability, mechanical strength, and performance in adsorbing MG dye from water. The kinetics and isotherm were evaluated, and the adsorption process was well fitted with pseudo-second order and Temkin isotherm models, respectively. Using the Langmuir equation, the maximum adsorption capacity at 45 °C within 50 min was calculated to be 2145 mg/g. Thermodynamic analysis at 25-45 °C revealed that the MG dye was spontaneously absorbed by the hydrogel nanocomposite. The prepared hydrogel nanocomposite demonstrated excellent reusability without a noticeable loss in MG dye adsorption capability for 6 cycles.


Nanocomposites , Water Pollutants, Chemical , Water Purification , Acrylates , Acrylic Resins , Adsorption , Hydrogels/chemistry , Hydrogen-Ion Concentration , Kinetics , Nanocomposites/chemistry , Plant Gums , Rosaniline Dyes , Thermodynamics , Titanium , Water , Water Pollutants, Chemical/chemistry , Water Purification/methods
9.
Int J Biol Macromol ; 190: 862-875, 2021 Nov 01.
Article En | MEDLINE | ID: mdl-34517029

We present an approach for synthesis of a micro-porous composite of two well-known biopolymers, namely chitosan and alginate, using glutaraldehyde as the cross-linking agent. Alginate and chitosan were pre-treated before being mixed, and the two biopolymers' proportions were also monitored. Chitosan was modified using aniline with the help of formaldehyde crosslinker and then the twizer was further crosslinked with alginate using glutaraldehyde. The synthesized composite, glutaraldehyde cross-linked chitosan-alginate composite [(Cs-F-An)-G-Al] was characterized using spectral techniques and employed as a potential adsorbent for three dyes namely Brilliant green, Methyl orange and Patent Blue V. The pHPZC of the material was 7.5 and the maximum monolayer adsorption capacity (Qmax) was found to be 235.82, 198.09 and 117.34 mg g-1 for BG (at pH 8.0), MO (at pH 6.0) and PBV (at pH 3.0) respectively. It was found that the adsorption process follows a Freundlich adsorption isotherm and pseudo second order kinetics. A thermodynamic study revealed that the process of adsorption was enthalpy-driven and spontaneous in nature. Interestingly, the values of the adsorption capacity obtained in column adsorption method are in close agreement with those obtained in batch adsorption experiments, which shows the potential of the synthesized composite for uptake of dyes.


Alginates/chemistry , Chitosan/chemistry , Coloring Agents/isolation & purification , Cross-Linking Reagents/chemistry , Glutaral/chemistry , Organic Chemicals/isolation & purification , Water Pollutants, Chemical/isolation & purification , Adsorption , Azo Compounds/isolation & purification , Hydrogen-Ion Concentration , Kinetics , Solutions , Spectrometry, X-Ray Emission , Spectroscopy, Fourier Transform Infrared , Temperature , Thermogravimetry , Time Factors , X-Ray Diffraction
10.
Carbohydr Polym ; 172: 205-212, 2017 Sep 15.
Article En | MEDLINE | ID: mdl-28606527

Chitosan, a potent amino polysaccharide, has been cross-linked with Sn(IV) chloride. The material was thoroughly characterized using FT-IR, XRD, SEM, EDX, TGA-DTA and BET studies. This Sn(IV) chloride cross-linked chitosan (Sn-Ch) has been exploited for As(III) adsorption. Various parameters like pH, amount of adsorbent, adsorption time etc have been optimized to achieve maximum adsorption efficiency. Under optimum conditions of pH 7.0±0.2, adsorption time of 45min and adsorbent dose 200mg, Sn-Ch was found to have adsorption capacity of 17.10mg/g at 298K. Adsorption of As(III) by Sn-Ch follow non-linear Freundlich isotherm model. The equilibrium studies showed that the experimental data fits well with non-linear pseudo-second-order kinetic model. Adsorption process was found to be exothermic and spontaneous. Column study proves the applicability of Sn-Ch to the larger sample volumes. It was found to be recyclable material and could be regenerated and reused multiple times adding a greener dimension.

11.
Int J Biol Macromol ; 104(Pt B): 1528-1538, 2017 Nov.
Article En | MEDLINE | ID: mdl-28259624

Chitosan, a potent amino polysaccharide, has been impregnated with Sn(IV) chloride for effective adsorption of fluoride from water. The Sn(IV) chloride impregnated chitosan was synthesized using microwave assisted technique. The material was thoroughly characterized using FTIR, SEM, EDX and XRD. The decrease in surface area and pore volume has been revealed from BET studies. Enhanced thermal stability of this material was ascertained by TGA-DTA studies. This Sn(IV) chloride impregnated chitosan(Sn-Ch) has been exploited for its defluoridation property. Various parameters like pH, amount of adsorbent, adsorption time etc have been optimized to achieve maximum defluoridation efficiency. Under optimum conditions, Sn-Ch was found to have adsorption capacity of 17. 63mg/g. The equilibrium studies showed that the data fits well with Freundlich isotherm model. Thermodynamics and kinetics parameters have been evaluated. The material has been applied for the defluoridation of real water sample. It was found to be recyclable material and can be regenerated and reused multiple times adding a greener dimension.


Chitosan/chemistry , Fluorides/chemistry , Tin Compounds/chemistry , Water Purification/methods , Water/chemistry , Adsorption , Fluorides/isolation & purification , Kinetics
12.
Int J Biol Macromol ; 104(Pt B): 1556-1568, 2017 Nov.
Article En | MEDLINE | ID: mdl-28214584

Ethylhexadecyldimethyl ammonium bromide impregnated chitosan (EHDAIC) was prepared to remove cadmium and mercury from synthetic effluent. The adsorbent was characterized by FTIR, XRD, SEM, EDX and TGA-DTA. Adsorption studies were carried out under different conditions of pH, adsorbent dose, temperature, and contact time. The results showed that the adsorption capacity of EHDAIC is a function of the solution pH and the optimum pH for these metal ions was found to be 3.0. The equilibrium data has been described using Langmuir and Freundlich isotherm models. The maximum adsorption capacity of 341.30mg/g was observed for Cd(II) and 43.43mg/g for Hg(II) in accordance with Langmuir adsorption isotherm in the form of their chloro complexes. The kinetic data fitted well with pseudo-second-order model, and equilibrium data was found to follow Freundlich isotherm model. The calculated thermodynamic parameters showed that the adsorption process was feasible, exothermic and spontaneous. Effect of common excipient ions was studied. Also the material was tested for large sample volumes using column extraction process. The adsorbent material could be regenerated for repetitive applications.


Cadmium/chemistry , Cadmium/isolation & purification , Chitosan/chemistry , Environmental Pollutants/chemistry , Environmental Pollutants/isolation & purification , Mercury/chemistry , Mercury/isolation & purification , Adsorption , Hydrogen-Ion Concentration , Kinetics , Quaternary Ammonium Compounds/chemistry
13.
Anal Chem Insights ; 10: 29-37, 2015.
Article En | MEDLINE | ID: mdl-26609215

Macrolides, one of the most commonly used class of antibiotics, are a group of drugs produced by Streptomyces species. They belong to the polyketide class of natural products. Their activity is due to the presence of a large macrolide lactone ring with deoxy sugar moieties. They are protein synthesis inhibitors and broad-spectrum antibiotics, active against both gram-positive and gram-negative bacteria. Different analytical techniques have been reported for the determination of macrolides such as chromatographic methods, flow injection methods, spectrofluorometric methods, spectrophotometric methods, and capillary electrophoresis methods. Among these methods, spectrophotometric methods are sensitive and cost effective for the analysis of various antibiotics in pharmaceutical formulations as well as biological samples. This article reviews different spectrophotometric methods for the determination of macrolide antibiotics.

14.
Anal Chem Insights ; 10: 11-6, 2015.
Article En | MEDLINE | ID: mdl-26279621

Cefixime trihydrate is a broad spectrum cephalosporin antibiotic, effective against gram-positive and gram-negative bacterial infections. Simple and rapid method has been developed for the determination of cefixime trihydrate in bulk and pharmaceutical formulations. This method was based on the formation of bluish-green ion-pair complex of cefixime trihydrate with bromophenol blue in dimethyl sulfoxide (DMSO)-acetonitrile medium. Different parameters were studied and optimized. A 2:1 complex was formed between the drug and reagent almost instantaneously at room temperature which has λmax of 610 nm. Under optimum conditions, calibration curve was found to be linear over the range of 10-130 µg mL(-1). The method was subjected to analytical quality control. The limit of detection was found to be 1.08 µg mL(-1). Recovery studies and interference studies were carried out. The proposed method was successfully applied to the determination of cefixime trihydrate in bulk and pharmaceutical formulations with high precision and accuracy.

15.
Water Sci Technol ; 70(12): 2047-55, 2014.
Article En | MEDLINE | ID: mdl-25521142

A sulfate-crosslinked chitosan (SCC) was prepared for effective detoxification of hexavalent chromium (Cr(VI)) from effluents. SCC was characterized using Fourier transform infrared, X-ray diffraction, scanning electron microscopy and energy dispersive X-ray studies. The maximum adsorption of Cr(VI) was observed at pH 6.0 with adsorption capacity of 157 mg/g in accordance with the Langmuir adsorption isotherm model. The adsorption process was found to follow the pseudo-second-order rate kinetics. From the study of various thermodynamic parameters (Gibbs energy, entropy and enthalpy changes), the adsorption capacity was found to decrease with increase in temperature. Column studies were carried out to obtain a breakthrough point of the adsorbent. The adsorbent was regenerated using sodium hydroxide with no change in the adsorption efficiency for up to 10 cycles. Effect of diverse ions on adsorption efficiency was studied and SCC was applied for Cr(VI) removal in synthetic effluents.


Chitosan/chemical synthesis , Chromium/isolation & purification , Adsorption , Environmental Pollution/prevention & control , Hydrogen-Ion Concentration , Ions , Kinetics , Microscopy, Electron, Scanning , Sulfates , Temperature , Thermodynamics , Waste Disposal, Fluid , X-Ray Diffraction
16.
Anal Sci ; 22(4): 571-4, 2006 Apr.
Article En | MEDLINE | ID: mdl-16760600

A rapid differential pulse adsorptive stripping voltammetric method has been developed for the ultra-trace determination of chromium using 2,2'-bipyridine. The base electrolyte used is 0.1 M NH4Cl (pH 6.0). The peak current was found to increase substantially with the addition of nitrite ions. A well-defined peak was observed at -1.3 V. Parameters, like concentration of the ligand, concentration of nitrite ion, accumulation potential, accumulation time, rest period, drop size, scan rate, pulse amplitude etc. have been optimized. Under the optimum conditions, the 3 sigma detection limit was found to be 0.02 ppb (3.8 x 10(-10) M). The method is highly selective and sensitive, and has been applied to the determination of Cr(VI) in spiked water, effluents and ore samples.

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