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Experimental design approach for the optimisation of pressurised fluid extraction of additives from polyethylene films

2005; Elsevier BV; Volume: 1099; Issue: 1-2 Linguagem: Inglês

10.1016/j.chroma.2005.09.005

1873-3778

Álvaro Garrido‐López, Marı́a Teresa Tena,

Recycling and Waste Management Techniques

A pressurised fluid extraction (PFE) and normal-phase-high performance liquid chromatography (NP-HPLC) method is proposed for the determination of additives in polyethylene films. The study of PFE variables was performed using a Plackett-Burman (PB) experimental design for screening and a central composite design (CCD) for optimising the main variables obtained from the Pareto charts. The studied variables were: temperature, time, cyclohexane (CHx) and tetrahydrofuran (THF) as modifiers, flush volume and extraction cycles, and an isopropanol:CHx (92.5:7.5) mixture twice at 105 degrees C for 15 min were the final conditions selected. The additives in the PFE extracts were separated by NP-HPLC using a silica column and a gradient n-hexane:dichloromethane:acetonitrile mobile phase. Additive solubility is higher in normal-phase solvents; thus, their separation can be carried out at room temperature. Finally, the method was applied to determine additives in several polyethylene films.