Chitin was successfully grafted with polystyrene by free radical mechanism using ammonium persulfate (APS) initiator. The reaction was carried out in aqueous medium. The effect of pH, chitin:monomer weight ratio, APS, reaction time and reaction temperature were investigated. The results showed that the optimum conditions for grafting of polystyrene were found as follows: pH 7, chitin:monomer weight ratio of 1:3, 0.4 g of APS, reaction temperature of 60 °C and reaction time 2 h. The graft copolymer was characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA) and differential scanning electron microscopy (DSC). Gel permeation chromatography (GPC) analysis carried out on the hydrolyzed graft copolymer showed that the Mn and Mw were 6.3395×10(4) g/mol and 1.69283×10(5) g/mol, respectively, with polydispersity index of 2.7.
LOD and LOQ are two important performance characteristics in method validation. This work compares three methods based on the International Conference on Harmonization and EURACHEM guidelines, namely, signal-to-noise, blank determination, and linear regression, to estimate the LOD and LOQ for volatile organic compounds (VOCs) by experimental methodology using GC. Five VOCs, toluene, ethylbenzene, isopropylbenzene, n-propylbenzene, and styrene, were chosen for the experimental study. The results indicated that the estimated LODs and LOQs were not equivalent and could vary by a factor of 5 to 6 for the different methods. It is, therefore, essential to have a clearly described procedure for estimating the LOD and LOQ during method validation to allow interlaboratory comparisons.
Grafting of crosslinked chitosan with monomer, N-vinyl-2-pyrrolidone, has been carried out to investigate its adsorption capacity toward Orange G (OG) from aqueous solutions. The adsorption performance of modified chitosan (cts(x)-g-PNVP) was examined and compared with that of the unmodified chitosan. The effects of initial pH, contact time and initial dye concentration were investigated in a batch system. The experimental data were correlated with the Langmuir and Freundlich isotherm models. The maximum adsorption capacity of cts(x)-g-PNVP (63.7mgg-1) based on Langmuir equation was relatively higher than that of the unmodified chitosan (1.7mgg-1). The kinetic studies showed that the adsorption process was consistent with the pseudo-second order kinetic model. Interaction mechanisms between OG and cts(x)-g-PNVP were also proposed. The overall results suggested that the prepared cts(x)-g-PNVP stands a good candidate as adsorbent for removal of anionic dye from aqueous solutions.
Crosslinked chitosan beads were grafted with N-vinyl-2-pyrrolidone (NVP) using ammonium persulfate (APS) as free radical initiator. Important variables on graft copolymerization such as temperature, reaction time, concentration of initiator and concentration of monomer were optimized. The results revealed optimum conditions for maximum grafting of NVP on 1g crosslinked chitosan as follows: reaction temperature, 60°C; reaction time, 2h and concentrations of APS and NVP of 2.63×10-1M and 26.99×10-1M, respectively. The modified chitosan beads were characterized by FTIR spectroscopy, 13C NMR, SEM and BET to provide evidence of successful crosslinking and grafting reactions. The resulting material (cts(x)-g-PNVP) was evaluated as adsorbent for the removal of Cu(II) ions from aqueous solutions in a batch experiment. The Langmuir and Freundlich adsorption models were also applied to describe the equilibrium isotherms. The results showed that the adsorption of the copper ions onto the beads agreed well with Langmuir model with the maximum capacity (qmax) of 122mgg-1.