Comparison of pressurised fluid extraction and microwave assisted extraction with atmospheric pressure methods for extraction of additives from polypropylene

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Harold J. Vandenburg, Anthony A. Clifford, Keith D. Bartle, John Carroll and Ian D. Newton

Extraction of Irganox 1010 from freeze-ground polypropylene using several methods has been compared. Pressurised fluid extraction (PFE) (of which accelerated solvent extraction is an example) using a modified supercritical fluid extractor (SFE) and microwave assisted extraction (MAE) both gave faster extraction than any conventional method, and recoveries were not significantly different. The times taken to reach 90% extraction for PFE using propan-2-ol at 150 °C and acetone at 140 °C were 5 and 6 min, respectively. Reflux with chloroform was found to be the fastest atmospheric pressure method with 90% extraction in 24 min. Reflux with cyclohexane–propan-2-ol (1 + 1) required 38 min; ultrasonic, shake-flask and Soxhlet extraction required about 80 min (90% extraction). For effectively complete extraction, from loaded extraction vessel to extract ready for analysis, PFE required 15 min, MAE 28 min and reflux with chloroform 45 min.


  1. H. J. Vandenburg, A. A. Clifford, K. D. Bartle, J. Carroll, I. D. Newton, L. M. Garden, J. R. Dean and C. T. Costley, Analyst, 1997, 122, R101 Search PubMed.
  2. C. T. Costley, J. R. Dean, I. D. Newton and J. Carroll, Anal. Commun., 1997, 34, 89 RSC.
  3. W. Freitag and O. John, Angew. Makromol. Chem., 1990, 175, 181 CrossRef CAS.
  4. R. C. Nielson, J. Liq. Chromatogr., 1991, 14, 503 CAS.
  5. X. Lou, H. Janssen and C. A. Cramers, Anal. Chem., 1997, 69, 1598 CrossRef CAS.
  6. H. J. Vandenburg, A. A. Clifford, K. D. Bartle, S. A. Zhu, J. Carroll, I. D. Newton and L. M. Garden, Anal. Chem., 1998, 70, 1943 CrossRef CAS.
  7. K. D. Bartle, A. A. Clifford, S. B. Hawthorne, J. J. Lagenfield, D. J. Miller and R. Robinson, J. Supercrit. Fluids, 1990, 3, 143 CrossRef CAS.
  8. H. J. Vandenburg, R. Carlson, A. A. Clifford, K. D. Bartle, J. Carroll and I. D. Newton, Anal. Chem., submitted for publication Search PubMed.
  9. A. F. M. Barton, Handbook of Polymer-Liquid Interaction Parameters and Solubility Parameters, CRC Press, Boca Raton, FL, 1990 Search PubMed.
  10. A. F. M. Barton, Handbook of Solubility Parameters and Other Cohesion Parameters, CRC Press, Boca Raton, FL, 1983 Search PubMed.