Basic Principles of Analytical Supercritical Fluid Extraction

  • Jerry W. King
  • John E. France


The analytical chemist in general employs several procedural steps for the characterization of complex samples. These steps can be classified into three major tasks: sample preparation, analysis, and interpretation of the resultant data. Advances in analytical chemistry have reduced the experimental burden and time required for these task areas; however, to date, sample preparation continues to consume much of the analyst’s time in the entire analysis protocol. Improved methods for sample preparation would be welcomed in the analytical laboratory as well as techniques that minimize the use of chemical reagents and their attendant disposal problems. This is particularly true in analytical protocols that require the use of toxic or carcinogenic organic solvents in the sample preparation schemes. The relatively new technique of supercritical fluid extraction (SFE) offers the analyst an alternative for preparing samples prior to analysis, that is rapid and environmentally less hazardous. This chapter will describe the basic principles involved in applying the technique for sample preparation in analytical chemistry.


Supercritical Fluid Sample Matrix Supercritical Fluid Extraction Supercritical Fluid Chromatography Extraction Pressure 
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  1. 1.
    Majors RE (1989) LC-GC 7:92Google Scholar
  2. 2.
    Steinwandter H (1989) In: Zweig G, Sherma J (eds) Analytical methods for pesticides and plant growth regulators, Vol 17. Academic, New York, pp 63–71Google Scholar
  3. 3.
    Giddings JC, Myers MN, King JW (1969) J Chromatogr Sci 7:276Google Scholar
  4. 4.
    Sie ST, Rijnders GWA (1967) Separation Sci 2:755CrossRefGoogle Scholar
  5. 5.
    Stahl E, Schilz W, Schutz W, Willing E (1978) Angew Chem Int Ed Engl 17:731CrossRefGoogle Scholar
  6. 6.
    Stahl E, Quirin KW, Gerard D (1988) Dense gases for extraction and refining. Springer-Verlag, BerlinCrossRefGoogle Scholar
  7. 7.
    Hawthorne SB, Miller DJ (1986) J Chromatog Sci 24:258Google Scholar
  8. 8.
    Schantz MM, Chesler SN (1986) J Chromatog 363:397CrossRefGoogle Scholar
  9. 9.
    Alexandrou N, Pawliszyn J (1989) Anal Chem 61:2770CrossRefGoogle Scholar
  10. 10.
    Hawthorne SB, Krieger MS, Miller DJ (1989) Anal Chem 61:736CrossRefGoogle Scholar
  11. 11.
    Onuska FI, Terry KA (1989) J High Resolut Chromatog 12:357CrossRefGoogle Scholar
  12. 12.
    Dooley KM, Kao CP, Gambreil RP, Knopf FC (1987) Ind Eng Chem Res 26:2058CrossRefGoogle Scholar
  13. 13.
    King JW (1989) J Chromatog Sci 27:355Google Scholar
  14. 14.
    Nam KS, Kapila S, Pieczonka G, Clevenger TE, Yanders AF, Viswanath DS, Mallu B (1988) In: Perrut M (ed) Proceedings of the international symposium on supercritical fluids. Tome 2 Institute National Polytechnique de Lorraine, France, p 743–750Google Scholar
  15. 15.
    Wheeler JR, McNally ME (1989) J Chromatog Sci 27:534Google Scholar
  16. 16.
    Janda V, Steenbeke G, Sandra P (1989) J Chromatog 479:200CrossRefGoogle Scholar
  17. 17.
    Lopez-Avila V, Becker WF, Billets S (1989) In: Proceedings of the 5th annual waste testing and quality assurance. Symposium, Vol 2. US EPA, Washington, DC, p 11 - 73Google Scholar
  18. 18.
    Schafer K, Baumann W (1989) Z Anal Chem 332:884CrossRefGoogle Scholar
  19. 19.
    Schneiderman MA, Sharma AK, Locke DC (1987) J Chromatog 409:343CrossRefGoogle Scholar
  20. 20.
    Schneiderman MA, Sharma AK, Locke DC (1988) J Chromatog Sci 26:458Google Scholar
  21. 21.
    Xie QL, Markides KE, Lee ML (1989) J Chromatog Sci 27:365Google Scholar
  22. 22.
    Hawthorne SB, Miller DJ (1987) J Chromatog 403:63CrossRefGoogle Scholar
  23. 23.
    McHugh MA, Krukonis VJ (1986) Supercritical fluid extraction: principles and practice. Butterworths, Boston, MAGoogle Scholar
  24. 24.
    Zosel K (1980) In: Extraction with supercritical gases. Verlag Chemie, Weinheim, Germany, pp 1–23Google Scholar
  25. 25.
    Eggers R, Tschiersch R (1978) Chem Ing Tech 50:842CrossRefGoogle Scholar
  26. 26.
    King JW, Johnson JH, Friedrich JP (1989) J Agric Food Chem 37:951CrossRefGoogle Scholar
  27. 27.
    Giddings JC, Myers MN, McLaren L, Keller RA (1968) Science 162:67CrossRefGoogle Scholar
  28. 28.
    King JW (1984) Preprints-Polymeric Materials Science & Engineering Division, Vol 51. American Chemical Society, Washington, DC, pp 707–712Google Scholar
  29. 29.
    Stahl E, Willing E (1980) Pharm Ind 42:1136Google Scholar
  30. 30.
    Hemmaplardh B, King Jr AD (1972) J Phys Chem 76:2170CrossRefGoogle Scholar
  31. 31.
    Brogle H (1982) Chem Ind (12):385Google Scholar
  32. 32.
    Francis AW (1954) J Phys Chem 58:1099CrossRefGoogle Scholar
  33. 33.
    Lira CT (1988) In: Charpentier BA, Sevenants MR (eds) Supercritical fluid extraction and chromatography. American Chemical Society, Washington DC, pp 1–25CrossRefGoogle Scholar
  34. 34.
    Chimowitz EH, Pennisi KJ (1986) AIChE J 32:1665CrossRefGoogle Scholar
  35. 35.
    Johnston KP, Barry SE, Read NK, Holcomb TR (1987) Ind Eng Chem Res 26:2372CrossRefGoogle Scholar
  36. 36.
    Peter S, Brunner G, Riha R (1976) Fette Seifen Anstrichmittel 76:45CrossRefGoogle Scholar
  37. 37.
    Dobbs JM, Wong JM, Lahiere RJ, Johnston KP (1987) Ind Eng Chem Res 26:56CrossRefGoogle Scholar
  38. 38.
    Wong JM, Johnston KP (1986) Biotech Progress 2:29CrossRefGoogle Scholar
  39. 39.
    Dobbs JM, Johnston KP (1987) Ind Eng Chem Res 26:1476CrossRefGoogle Scholar
  40. 40.
    Hedrick J, Taylor LT (1989) Anal Chem 61:1986CrossRefGoogle Scholar
  41. 41.
    Johnston KP (1989) In: Johnston KP, Penninger JML (eds) Supercritical fluid science and technology. American Chemical Society, Washington, DC, pp 1–12CrossRefGoogle Scholar
  42. 42.
    Rizvi SSH, Benado AL, Zollweg JA, Daniels JA (1986) Food Tech 40 (6):55Google Scholar
  43. 43.
    Friedrich JP, List GR, Spencer GF (1988) In: Baldwin AR (ed) Proceedings of the 7th international conference on jojoba and its uses. American Oil Chemists’ Society, Champaign, IL, 165–172Google Scholar
  44. 44.
    Hawthorne SB, Miller DJ, Krieger MS (1988) Fresenius Z Anal Chem 330:211CrossRefGoogle Scholar
  45. 45.
    King JW (1984) J Am Oil Chemists’ Soc 61:689Google Scholar
  46. 46.
    List GR, Friedrich JP, King JW (1989) Oil Mill Gazetteer 95 (6):28–34Google Scholar
  47. 47.
    Bowman Jr LM (1976) Dense gas chromatographic studies. Ph D Thesis, University of Utah, Salt Lake City, UTGoogle Scholar
  48. 48.
    Prausnitz JM (1969) Molecular thermodynamics of fluid-phase equilibria. Prentice-Hall, Englewood Cliffs, NJ, p 36–39Google Scholar
  49. 49.
    Kurnik RT, Reid RC (1981) AIChE J 27:861CrossRefGoogle Scholar
  50. 50.
    Allada SR (1984) Ind Eng Chem Process Des Dev 23:344CrossRefGoogle Scholar
  51. 51.
    Fedors RF (1974) Polym Eng Sci 14:147CrossRefGoogle Scholar
  52. 52.
    Jayasri A, Yaseen M (1980) J Coatings Tech 52 (667):41–45Google Scholar
  53. 53.
    Flory PJ (1953) Principles of polymer chemistry. Cornell University Press, Ithaca, NYGoogle Scholar
  54. 54.
    Sugiyama K, Saito M, Hondo T, Senda M (1985) J Chromatogr 332:107CrossRefGoogle Scholar
  55. 55.
    Jackson WP, Markides KE, Lee ML (1986) HRC & CC 9:213CrossRefGoogle Scholar
  56. 56.
    Skelton Jr RJ, Johnson CC, Taylor LT (1986) Chromatographia 21:4CrossRefGoogle Scholar
  57. 57.
    Gmuer W, Bosset JO, Plattner E (1987) J Chromatogr 388:335CrossRefGoogle Scholar
  58. 58.
    Engelhardt H, Gross A (1988) HRC & CC 11:38CrossRefGoogle Scholar
  59. 59.
    Raynor MW, Davies IL, Bartle KD, Clifford AA, Williams A, Chalmers JM, Cook BW (1988) HRC & CC 11:766CrossRefGoogle Scholar
  60. 60.
    McNally ME, Wheeler JR (1988) J Chromatog 435:63CrossRefGoogle Scholar
  61. 61.
    Saito M, Yamaguchi Y, Inomata K, Kottkamp W (1989) J Chromatog Sci 27:79Google Scholar
  62. 62.
    Ramsey ED, Perkins JR, Games DE, Startin JR (1989) J Chromatogr 464:353CrossRefGoogle Scholar
  63. 63.
    Thiebault D, Chervet JP, Vannoort RW, DeJong GJ, Brinkman UA, Frei RW (1989) J Chromatogr 477:151CrossRefGoogle Scholar
  64. 64.
    Sieber R (1988) In: Perrut M (ed) Proceedings of the international symposium on supercritical fluids, Vol 2. Institute National Polytechnique de Lorraine, France, p 619Google Scholar
  65. 65.
    van Wasen U, Swaid I, Schneider GM (1980) Angew Chem Int Ed Engl 19:575CrossRefGoogle Scholar
  66. 66.
    Smith RD, Udseth HR, Wright BW, Yonker CR (1987) Sep Sci Tech 22:1065CrossRefGoogle Scholar
  67. 67.
    Feist R, Schneider GM (1982) Sep Sci 17:261CrossRefGoogle Scholar
  68. 68.
    Sie ST, Van Beersum W, Rijnders GWA (1966) Sep Sci 1:459CrossRefGoogle Scholar
  69. 69.
    Parcher J, Strubinger JR (1989) J Chromatogr 479:251CrossRefGoogle Scholar
  70. 70.
    King JW, Eissler RL, Friedrich JP (1988) In: Charpentier BA, Sevenants MR (eds) Supercritical fluid extraction and chromatography. American Chemical Society, Washington, DC, p 63–88CrossRefGoogle Scholar
  71. 71.
    Markides KE, Lee ML (1989) SFC applications. Brigham Young University Press, Provo, UTGoogle Scholar
  72. 72.
    Smith RD, Udseth HR, Wright BW (1985) In: Penninger JML, Radosz M, McHugh MA, Krukonis VJ (eds) Supercritical fluid technology. Elsevier, Amsterdam, pp 191–223Google Scholar
  73. 73.
    McMahon D, Cohen KA, Taylor LT (eds) (1988) Chromatography illustrated. Preston Publications, Niles, IL, pp 73–90Google Scholar
  74. 74.
    Fields SM, Grolimund K (1988) HRC & CC 11:727CrossRefGoogle Scholar
  75. 75.
    McNally ME, Wheeler JR (1988) J Chromatogr 447:53CrossRefGoogle Scholar
  76. 76.
    Klesper E, Leyendecker D, Schmitz FP (1986) J Chromatogr 366:235CrossRefGoogle Scholar
  77. 77.
    Levy JM, Ritchey WM (1986) J Chromatogr Sci 24:242Google Scholar
  78. 78.
    Hawthorne SB, Miller DJ (1987) Anal Chem 59:1705CrossRefGoogle Scholar
  79. 79.
    Engelhart WG, Gargus AG (1988) 20 (2):30Google Scholar
  80. 80.
    Swanson JT, Andersen MR, Richter BE (1990) Theory of mass transfer applied to micro-SFE. Paper presented at the symposium/workshop on supercritical fluid chromatography, Part City, UTGoogle Scholar
  81. 81.
    Hawthorne SB (1990) Anal Chem 62:633ACrossRefGoogle Scholar
  82. 82.
    Andersen MR, Swanson JT, Porter NL, Richter BE (1989) J Chromatogr Sci 27:371CrossRefGoogle Scholar
  83. 83.
    Levy JM, Cavalier RA, Bosch TN, Rynaski AF, Huhak WE (1989) J Chromatogr Sci 27:341Google Scholar
  84. 84.
    King JW, France JE, Taylor SL (1990) In: Sandra P, Redant G (eds) Proceedings - 11th international symposium on capillary chromatography. Hüthig, Heidelberg, pp 595–601Google Scholar
  85. 85.
    Synder JM, Friedrich JP, Christianson DD (1984) J Am Oil Chemists’ Soc 61:5475Google Scholar
  86. 86.
    Roselius W, Vitzhum OG, Hubert P (1976) DBP 2142205Google Scholar
  87. 87.
    Yamaguchi K, Murakami M, Nakano H, Konosu S, Kokura T, Yamamoto H, Kosaka M, Hata K (1986) J Agric Food Chem 34:904CrossRefGoogle Scholar
  88. 88.
    King JW (1989) Abstracts of the Pittsburgh conference, Atlanta, GA, #397Google Scholar
  89. 89.
    Chiou JS, Barlow JW, Paul DR (1985) J Apply Polym Sci 30:3911CrossRefGoogle Scholar
  90. 90.
    Nicholas J, Bartle KD, Clifford AA (1990) In: Sandra P, Redant G (eds) Proceedings - 11th international symposium on capillary chromatography. Hüthig, Heidelberg, pp 665–672Google Scholar
  91. 91.
    Modell M, deFilippi RP, Krukonis V (1980) In: Suffet IH, McGuire MJ (eds) Activated carbon adsorption of organics from the aqueous phase, Vol 1. Ann Arbor Science Publishers Inc, Ann Arbor, MI, pp 447–462Google Scholar
  92. 92.
    Picht RD, Dillman TR, Burke DJ, deFilippi RP (1982) In: Ma YH (ed) Recent advances in adsorption and ion exchange, Vol 78. AIChE, New York, NY, pp 136–149Google Scholar
  93. 93.
    King JW (1987) In: Squires TG, Paulaitis ME (eds) Supercritical fluids: Chemical and engineering principles and applications. American Chemical Society, Washington, DC, pp 150–171CrossRefGoogle Scholar
  94. 94.
    Randolph TW (1990) Trends in Biotech 8:78CrossRefGoogle Scholar
  95. 95.
    Fisher RJ (1989) Food Tech 43(3):90Google Scholar

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© Springer-Verlag Berlin Heidelberg 1992

Authors and Affiliations

  • Jerry W. King
  • John E. France

There are no affiliations available

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