ABSTRACT
In this work, we report on the synthesis of four morphologies of ZnO, namely, nanoparticles, nanorods, nanosheets, and nanoflowers, from a single precursor Zn(CH3COO)2·2H2O under different reaction conditions. The synthesised nanostructured materials were characterised using powder X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Raman spectroscopy, UV-Vis, XPS analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and nitrogen sorption at 77 K. The XRD, FTIR, and Raman analyses did not reveal any significant differences among the nanostructures, but differences in the electronic properties were noted among the different morphologies. The TEM and SEM analyses confirmed the four different morphologies of the ZnO nanostructures. The textural characteristics revealed that the specific surface areas were different, being 1.3, 6.7, 12.7, and 26.8 m2/g for the nanoflowers, nanoparticles, nanorods, and nanosheets, respectively. The ZnO nanostructures were then mixed with carbon nanoparticles (CNPs) and cellulose acetate (CA) to make nanocomposites that were then used as sensing materials in solid-state sensors to detect methanol, ethanol, and isopropanol vapour at room temperature. The sensors' responses were recorded in relative resistance. When detecting methanol, 6 out of 12 sensors were responsive, and the most sensitive sensor was the composite with a mass ratio of 1:1:1 of ZnO nanorods:CNPs:CA with a sensitivity of 0.7740 Ω ppm-1. Regarding the detection of ethanol vapour, 9 of the 12 sensors were responsive, and the 3:1:1 mass ratio with ZnO nanoparticles was the most sensitive at 4.3204 Ω ppm-1. Meanwhile, with isopropanol, 5 out of the 12 sensors were active and, with a sensitivity of 3.4539 Ω ppm-1, the ZnO nanoparticles in a 3:1:1 mass ratio were the most sensitive. Overall, the response of the sensors depended on the morphology of the nanostructured ZnO materials, the mass ratio of the sensing materials in the composites, and the type of analyte. The sensing mechanism was governed by the surface reaction on the sensing materials rather than pores hindering the analyte molecules from reaching the active site, since the pore size is larger than the kinetic diameter of the analyte molecules. Generally, the sensors responded well to the ethanol analyte, rather than methanol and isopropanol. This is due to ethanol molecules displaying a more enhanced electron-donating ability.
ABSTRACT
Environmental pollutants, such as mycotoxins, pesticides, and pharmaceuticals, are a group of contaminates that occur naturally, while others are produced from anthropogenic sources. With increased research on the adverse ecological and human health effects of these pollutants, there is an increasing need to regularly monitor their levels in food and the environment in order to ensure food safety and public health. The application of magnetic nanomaterials in the analyses of these pollutants could be promising and offers numerous advantages relative to conventional techniques. Due to their ability for the selective adsorption, and ease of separation as a result of magnetic susceptibility, surface modification, stability, cost-effectiveness, availability, and biodegradability, these unique magnetic nanomaterials exhibit great achievement in the improvement of the extraction of different analytes in food. On the other hand, conventional methods involve longer extraction procedures and utilize large quantities of environmentally unfriendly organic solvents. This review centers its attention on current applications of magnetic nanomaterials and their modifications in the extraction of pollutants in food commodities.
Subject(s)
Magnets/chemistry , Mycotoxins/isolation & purification , Nanostructures/chemistry , Pesticides/isolation & purification , Pharmaceutical Preparations/isolation & purification , Solid Phase Extraction/methods , Animals , Environmental Pollutants/analysis , Environmental Pollutants/isolation & purification , Food Contamination/analysis , Food Safety , Humans , Mycotoxins/analysis , Pesticides/analysis , Pharmaceutical Preparations/analysis , Solid Phase Extraction/instrumentationABSTRACT
Considering its availability, renewable character and abundance in nature, this review assesses the opportunity of the application of biomass as a precursor for the production of carbon-based nanostructured materials (CNMs). CNMs are exceptionally shaped nanomaterials that possess distinctive properties, with far-reaching applicability in a number of areas, including the fabrication of sustainable and efficient energy harnessing, conversion and storage devices. This review describes CNM synthesis, properties and modification, focusing on reports using biomass as starting material. Since biomass comprises 60-90% cellulose, the current review takes into account the properties of cellulose. Noting that highly crystalline cellulose poses a difficulty in dissolution, ionic liquids (ILs) are proposed as the solvent system to dissolve the cellulose-containing biomass in generating precursors for the synthesis of CNMs. Preliminary results with cellulose and sugarcane bagasse indicate that ILs can not only be used to make the biomass available in a liquefied form as required for the floating catalyst CVD technique but also to control the heteroatom content and composition in situ for the heteroatom doping of the materials.
ABSTRACT
Multiwalled carbon nanotube (MWCNT) was fixed onto the surface of a magnetic silica (Fe3O4@SiO2) substrate via chemical vapour deposition (CVD). Acetylene gas was used as the carbon source and cobalt oxide as the catalyst. The chemical and physical characteristics of the materials were investigated by transmission electron microscopy (TEM), Raman spectroscopy (RS), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), and nitrogen adsorption/desorption isotherm. The synthesized Fe3O4@SiO2-MWCNT nanocomposite was used as a magnetic solid phase extraction (MSPE) adsorbent for the preconcentration of organophosphorus pesticides (OPPs), specifically, azinphos methyl, chlorpyrifos, parathion, and malathion. The factors influencing the extraction efficiency such as pH, contact time, and adsorbent dosage were investigated and optimized by response surface methodology (RSM) and desirability function. Linear response was obtained in the concentration range of 10-200 µg/L for the analytes with determination coefficients ranging between 0.9955 and 0.9977. The limits of detection (LODs) and quantification (LOQs) were in the range of 0.004-0.150 µg/L and 0.013-0.499 µg/L, respectively. Fe3O4@SiO2-MWCNT was applied in the extraction and subsequent determination of OPPs in water samples from Vaal River and Vaal Dam with recoveries ranging from 84.0 to 101.4% (RSDs = 3.8-9.6%, n = 3) in Vaal River and 86.2 to 93.8% (RSDs = 2.9-10.4%, n = 3) in Vaal Dam. The obtained results showed that the newly synthesized Fe3O4@SiO2-MWCNT nanocomposite can be an efficient adsorbent with good potential for the preconcentration and extraction of selected OPPs from aqueous media.
ABSTRACT
In this study, aluminosilicate rich clay soils were prepared through mechanochemical activation. The chemical and mineralogical properties were investigated using X-Ray Fluorescence (XRF) and X-ray diffraction (XRD). The functional groups, morphology and surface area were evaluated using Fourier Transform Infra-Red (FTIR), Scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) analysis. Batch experiments were used to evaluate its defluoridation efficiency while antibacterial activities were assessed using well diffusion method. Maximum adsorption capacity was found to be 1.87 mg/g with 32% fluoride removal. Fluoride adsorption was found to reduce in the presence of Cl-, PO42- and CO32- while it increased in the presence of SO42- and NO3-. Adsorption data fitted well to Freundlich isotherms, hence, confirming heterogeneous multilayer adsorption. Kinetic studies revealed that fluoride adsorption fitted well to pseudo-second order model. The sorption of F- onto the clays' surface followed intra-particle diffusion mode. High correlation coefficient indicates that the sorption process was greatly controlled by particle diffusion while it is minimal in pore diffusion model. Antibacterial studies revealed no zone of inhibition for all the activated clays, hence indicating that they are not active against the bacterial strains of Escherichia coli used in this study. The results showed activated clays' potential for defluoridation. Its effectiveness in pathogen removal is limited. Hence further modifications of the clays' surfaces are hereby recommended.
Subject(s)
Aluminum Silicates/chemistry , Bacteria/isolation & purification , Clay/chemistry , Fluorides/analysis , Groundwater/analysis , Soil/chemistry , Water Purification/methods , Adsorption , Groundwater/chemistry , Groundwater/microbiology , Kinetics , Spectrometry, X-Ray Emission , Water Purification/instrumentation , X-Ray DiffractionABSTRACT
Porous materials such as metal organic frameworks (MOFs), zeolite templated carbons (ZTC), and some porous polymers have endeared the research community for their attractiveness for hydrogen (H2) storage applications. This is due to their remarkable properties, which among others include high surface areas, high porosity, tunability, high thermal, and chemical stability. However, despite their extraordinary properties, their lack of processability due to their inherent powdery nature presents a constraining factor for their full potential for applications in hydrogen storage systems. Additionally, the poor thermal conductivity in some of these materials also contributes to the limitations for their use in this type of application. Therefore, there is a need to develop strategies for producing functional porous composites that are easy-to-handle and with enhanced heat transfer properties while still retaining their high hydrogen adsorption capacities. Herein, we present a simple shaping approach for ZTCs and their MOFs composite using a polymer of intrinsic microporosity (PIM-1). The intrinsic characteristics of the individual porous materials are transferred to the resulting composites leading to improved processability without adversely altering their porous nature. The surface area and hydrogen uptake capacity for the obtained shaped composites were found to be within the range of 1,054-2,433 m2g-1 and 1.22-1.87 H2 wt. %, respectively at 1 bar and 77 K. In summary, the synergistic performance of the obtained materials is comparative to their powder counterparts with additional complementing properties.
ABSTRACT
The occurrence of eight pharmaceuticals was monitored during four seasons (spring, summer, autumn, and winter) along a 250-km stretch of the Msunduzi and Mgeni rivers in KwaZulu-Natal, South Africa. This paper describes an optimized method for the determination of nonsteroidal anti-inflammatory drugs (NSAIDs) in sediments. The method combines ultrasonic, centrifuge, and gas chromatography-mass spectrometry for the detection of these drugs in solid samples. Most of the parameters that affect the extraction step were optimized. Solid samples were placed in a centrifuge tube and extracted with ethyl acetate:acetone (1:1, two cycles), followed by clean-up with Oasis HLB cartridge and derivatization with N, O-bis(trimethylsilyl) trifluoroacetamide (BSTFA). Satisfactory recoveries were obtained ranging from 66 to 130%, depending on the analyte. Precision expressed as RSD (%) (n = 3) was less than 20% for all analytes. The LODs and LOQs were in the range of 0.024 to 1.90 ng g-1 which allowed to be applied in the analysis solid samples in Msunduzi and Mgeni rivers. In the solid samples analyzed, NSAID concentration ranged from not detected to 221 ng g-1.
Subject(s)
Anti-Inflammatory Agents, Non-Steroidal/analysis , Environmental Monitoring/instrumentation , Environmental Monitoring/methods , Geologic Sediments/chemistry , Rivers/chemistry , Water Pollutants, Chemical/analysis , Gas Chromatography-Mass Spectrometry/methods , Solid Phase Extraction/methods , South Africa , UltrasonicsABSTRACT
A method was optimized for derivatization, separation, detection and quantification of salicylic acid, acetylsalicylic acid, nalidixic acid, ibuprofen, phenacetin, naproxen, ketoprofen, meclofenamic acid and diclofenac in surface water using gas chromatography-mass spectrometry. For most of the acidic drugs, recovery was in the range 60-110% and the percent standard deviation was below 15% for the entire method, with limits of detection ranging from 0.041 to 1.614 µg L-1. The developed method was applied in the analysis of acidic drugs in Umgeni River system, KwaZulu-Natal South Africa. All of the selected acidic drugs were detected and quantified, their concentration in Umgeni River system ranged from 0.0200 to 68.14 µg L-1.
Subject(s)
Water Pollutants, Chemical/analysis , Acids, Carbocyclic/analysis , Aspirin/analysis , Environmental Monitoring , Gas Chromatography-Mass Spectrometry/methods , Hydrogen-Ion Concentration , Nalidixic Acid/analysis , Naproxen/analysis , Phenacetin/analysis , Rivers/chemistry , South Africa , Water/chemistryABSTRACT
Mesoporous silica, specifically SBA-15, acid-treated multi-walled carbon nanotubes and a hybrid nanocomposite of SBA-15 coated onto the sidewalls acid-treated multi-walled carbon nanotubes (CNTs) were prepared and used as supports for anatase TiO2. Sol-gel methods were adapted for the synthesis of selected supports and for coating the materials with selected wt% loading of titania. Physical and chemical properties of the supports and catalyst composite materials were investigated by powder X-ray diffraction (XRD), Raman spectroscopy, thermogravimetric analysis, scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), UV-vis diffuse reflectance spectroscopy and fluorescence spectroscopy. The photo-activity of the catalyst composites were evaluated on the decolorisation of methylene blue as a model pollutant. Coating CNTs with SBA-15 improved the thermal stability and textural properties of the nanotubes. All supported titania composites had high surface areas (207-301 m(2)/g), altered band gap energies and reduced TiO2 crystallite sizes. The TiO2/SBA-CNT composite showed enhanced photo-catalytic properties and activity than the TiO2/SBA-15 and TiO2/CNT composites. In addition, an interesting observation was noted with the TiO2/SBA-15 nanocomposites, which had a significantly greater photo-catalytic activity than the TiO2/CNT nanocomposites in spite of the high electron-hole recombination phenomena observed with the photoluminescence results. Discussions in terms of morphological, textural and physical-chemical aspects to account for the result are presented.