In this work, novel dummy molecularly imprinted polymers (DMIP) with propanamide as a dummy template molecule were prepared based on a green synthesis strategy of less consumption of hazardous/organic reagents and at mild conditions for magnetic solid-phase extraction (MSPE) of acrylamide in biscuit samples, followed by high performance liquid chromatography (HPLC) determination. The resultant DMIP was well characterized by FT-IR, SEM, TEM and VSM, exhibiting uniform nanoscale coreshell structure and good magnetic property in favor of simple rapid separation. Several main variables influencing MSPE efficiency were investigated, including DMIP dosage, sample solution pH, extraction time and desorption solvent; central composite design (CCD) and response surface methodology (RSM) were employed to assist in the MSPE condition optimization with rapidity and reliability. Under optimized conditions, excellent linearity for acrylamide was obtained in the range of 5.0-5000.0 µg kg −1 , and low detection and quantification limits were 1.3 µg kg −1 and 4.4 µg kg −1 , respectively. The method recoveries at five spiked concentrations were found within 86.0-98.3% with relative standard deviations (RSDs) of 1.2-4.1%. Furthermore, endogenous acrylamide was detected in five different biscuit samples and the RSDs values were lower than 3.3%. The present study suggested promising perspectives of water-compatible eco-friendly DMIP based MSPE-HPLC method for highly effective sample pretreatment and targeted analytes determination in complicated matrices. Recently, chromatographic techniques coupled with sensitive detectors (hyphenated techniques) such as gas chromatography-mass spectrometry (GC-MS) [7], GC-electron capture spectrometry [8],
The present study the ultrasound assisted adsorption of dyes in single system onto FeO magnetite nanoparticles loaded on activated carbon (FeO-MNPs-AC) was described following characterization and identification of this adsorbent by conventional techniques likes field emission scanning electron microscopy, transmission electron microscopy, particle-size distribution, X-ray diffraction and Fourier transform infrared spectroscopy. A central composite design in conjunction with a response surface methodology according to f-test and t-test for recognition and judgment about significant term led to construction of quadratic model which represent relation among responses and effective terms. This model has unique ability to predict adsorption data behavior over a large space around central and optimum point. Accordingly Optimum conditions for well and quantitative removal of present dyes was obtained best operation and conditions: initial SY, MB and EB dyes concentration of 15, 15 and 25mgL, 4.0, 6.0 and 5.0 of pH, 360, 360 and 240s sonication time and 0.04, 0.03 and 0.032g of FeO-MNPs-AC. Replication of similar experiment (N=5) guide that average removal percentage of SY, MB and EB were found to be 96.63±2.86%, 98.12±1.67% and 99.65±1.21% respectively. Good agreement and closeness of Predicted and experimental result and high adsorption capacity of dyes in short time strongly confirm high suitability of present method for waste water treatment, while easy separation of present nanoparticle and its good regeneration all support good applicability of FeO-MNPs-AC for waste water treatment. The kinetic study can be represented by combination of pseudo second-order and intraparticle diffusion. The obtained maximum adsorption capacities correspond to Langmuir as best model for representation of experimental data correspond to dyes adsorption onto FeO-MNPs-AC were 76.37, 78.76 and 102.00mgg for SY, MB and EB, respectively. In addition, the performance comparison of ultrasound-assisted, magnetic stirrer assisted and vortex assisted adsorption methods demonstrates that ultrasound is an effective and good choice for facilitation of adsorption process via. Compromise of simple and facile diffusion.
In this study, the Sulfonated graphene oxide (SGO)/Fe 3 O 4 nanosheets were synthesized by hydrothermal method and incorporated into blend sulfonated poly(ether ether ketone) (SPEEK)/poly(vinyl alchole) (PVA) matrix with different weight percent of (SGO)/Fe 3 O 4 nanosheets. The performances of prepared membranes were investigated by water uptake, membrane swelling, mechanical and thermal stability, proton conductivity, methanol permeability and DMFC test. It was found that the water uptake and tensile strength of SPEEK membrane increased and proton conductivity and power density decreased by 2 blending with PVA. Incorporation of SGO/Fe 3 O 4 nanosheets into SPEEK/PVA matrix enhanced mechanical stability, proton conductivity and methanol barrier properties of membrane. The SPEEK/PVA/SGO/Fe 3 O 4 nanocomposite membrane with optimal nanosheets content (5 wt%) exhibits low methanol permeability (8.83 × 10 −7 cm 2 s -1 ), high tensile strength (51.2 MPa), high proton conductivity (0.084 S cm -1 at 25°C) and high power density (122.7 mW cm -2 at 80°C) and suggests its potential application in DMFCs.
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