A chemometric approach using I-optimal design for optimising Pb(II) removal using bentonite-chitosan composites and beads.

ABSTRACT

This paper reports adsorption studies of Pb(II) ions onto Bentonite-Chitosan (Bt-Ch) composites or beads when using an I-optimal design experiment approach. Three adsorption factors (pH, adsorbent dosage, and initial concentration) were optimised whilst simultaneously investigating multiple adsorbents. The Bt-Ch composites and beads (type A and B) adsorbents were made using weight ratios 90%/10% and differed characteristically due to their preparation methods of solution blending and precipitation, respectively. A batch procedure was used for adsorption experiments, and the amounts of Pb(II) ions (adsorbed onto Bt-Ch composites/beads) were analysed using inductively coupled plasma optical emission spectrometry (ICP-OES). Adsorption experimental parameters were analysed and optimised by using a response surface method (I-optimal design) generated from Design-Expert® 13.0 software. The main achievements of this study were to intensify the understanding and application of I-optimal experimental designs, which allow simultaneous determination of adsorption capacities and efficiencies across multiple adsorbents in an economical manner. A reduced quadratic model provided the best fit for the experimental data and exhibited minimal deviation between predicted and experimental values. This was evidenced by the very small covariance (CV) values of 1.81% and 1.33% observed for adsorption capacity and adsorption efficiency, respectively, also suggesting high reproducibility. It was observed that the adsorption factors studied (pH, adsorbent dose, and initial concentration) have a more pronounced effect on the adsorption capacity (F-value = 714.37) compared to adsorption efficiency (F-value = 140.62). Adsorbent dosage was found to have the greatest effect on adsorption capacity, while the initial pH of Pb(II) solution had the greatest effect on adsorption efficiency. Under optimal conditions, the adsorption capacities of beads-A (73.2 mg/g) and beads-B (77.6 mg/g) were found to be higher than that of the corresponding composite (51.7 mg/g). Whilst the optimum adsorption efficiency values for all three adsorbents were ∼100% (with ranges of pH 2-5, initial concentrations 50-200 mg/L, and adsorbent dosage 0.05-0.5 mg). The desirability indexes for the optimised conditions for these respective responses (and each adsorbent) were found to be within the ranges of 0.892-0.974 and 0.945-0.967 for adsorption capacity and adsorption efficiency, respectively. These high desirability index values for both responses indicate that the optimised conditions lead to very good performance for both measures. The information obtained in this study provides detailed understanding of the adsorption phenomena of the adsorbents studied. It gives confidence in the use of I-optimal designs to be applied as a chemometric tool for the specific adsorbents studied herein and others.