Determination of low levels of an antioxidant in polyolefins by large volume injection temperature-programmed packed capillary liquid chromatography.
| Title |
Determination of low levels of an antioxidant in polyolefins by large volume injection temperature-programmed packed capillary liquid chromatography. |
| Publication year |
1999 |
| General note |
doi:10.1016/S0021-9673(99)01006-7 |
| Language |
English |
| Author |
Molander, Paal |
| Co-Authors |
Greibrokk, Tyge - Lundanes, Elsa - Haugland, Karine - Ommundsen, Espen (Norner) - Hegna, Dag R. (Norner) |
| Source |
Journal of Chromatography A, 864 (1), 1999, 103-109 |
| Abstract |
Sub-ambient column temperatures, promoting strong interactions between the analyte and the stationary phase material, were utilized to focus large volumes of the polyolefin antioxidant Irganox 1076 [benzenepropanoic acid, 3,5-bis(1,1-dimethylethyl)-4-hydroxy-, octadecyl ester] on the column inlet, using pure acetonitrile as sample solvent and mobile phase. Injection volumes up to 100 ml were successfully employed on a 50 cm3320 mm I.D. capillary column packed with 5 mm Kromasil 100 ODS particles. Irganox 1076 was eluted after completed injection by temperature programming, using a 21 temperature program from 7 to 908C, in 38C min . UV detection, using a low-dispersion 'U'-shaped flowcell, was performed at 280 nm. The method was applied for the determination of Irganox 1076 that was extracted from low-density polyethylene (0.6 ppm, w/ w). Both Soxhlet and microwave-aided solvent extractions were performed, using chloroform and acetonitrile as solvents, respectively. The microwave-aided extraction with cetonitrile was found to give approximately the same yield as the standard Soxhlet reference method. Consequently, small volumes of acetonitrile could be used both as extraction solvent, sample solvent and mobile phase, simplifying the analysis process. The mass limit of detection of the method was found to be 3.3 ng, corresponding to a concentration limit of detection of 33 ng ml , utilizing an injection volume of 100 ml. The within and between day precision of retention times displayed relative standard deviations below 1.2%. |