Comparison and evaluation of copper complex-containing siloxane polymers as stationary phases for capillary gas chromatography

Two metallomesogenic polymers, P-C11CuC18 and P-C11CuC12 consisting of flex ible aliphatic side chains with copper carboxylate complexes have been synt hesized on the basis of addition reactions with polysiloxane. The applicabi lity of the prepared columns to the analysis of phthalate esters that are o f environmental concern was assessed. For preparation of the capillary colu mn with its wall coated with the metallomesogenic polymer, both static and dynamic methods were employed. Factors affecting the retention and the samp le selectivity on both columns were examined. A better separation of phthal ates was achieved with P-C11CuC18 than P-C11CuC12. The former phase showed a higher solute-solvent interaction than the latter. With static coating, t he wall-coated P-C11CuC18 capillary column (15 mX250 mum I.D.) showed that the baseline separation of all 14 phthalates could be achieved within 38 mi n with high reproducibility. The calibration graphs for phthalate ester det ermination were linear over the range of 10-625 mug ml(-1). The mass detect ion limits were lower than the ng range based on three times the standard d eviation of seven measurements of the lowest peak that could be detected. ( C) 2001 Elsevier Science B.V. All rights reserved.