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Determination of ethylene oxide oligomer distributions in alcohol ethoxylates by HPLC using a rotating disc-flame ionization detector

  • Technical
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Journal of the American Oil Chemists’ Society

Abstract

A high performance liquid chromatographic (HPLC) method has been developed for the quantitative determination of ethylene oxide (EO) oligomer distributions (% wt) in acetylated alcohol ethoxylates, R(OCH2CH2)nOH, from n=0, 1 to n=30 using a rotating disc-flame ionization detector. Both single carbon number and mixed carbon number alcohol-based (NEODOL® ethoxylates) samples have been analyzed by gradient elution with 2 different solvent systems on a Waters μ-Porasil column. With both solvent systems, 95% hexane is the initial solvent but with one system, 100% acetone is the final solvent and with the other, 10% methanol/90% acetone is used. The latter solvent elutes the higher ethoxylates from n=21 to n=30 quantitatively from the μ-Porasil column which the 100% acetone solvent fails to do. The 100% acetone solvent separates n=2 and n=3 from n=0,1 which the methanol-containing solvent does not do. Response factors for n=3 and n=8 have been experimentally determined and the response factors for the other EO units have been calculated from these 2 results. The corrected EO oligomer distributions for both NEODOL® 25-9 and NEODOL® 23-6.5 determined by HPLC are in good agreement with those determined earlier by circular thin layer chromatography (up to n=16 can be determined by this method). The average EO numbers determined by the HPLC method and by a wet chemical (phthalic anhydride) method are in excellent agreement for the above 2 samples and a sample of NEODOL® 23-7.5. The results are discussed in terms of Snyder’s theory for gradient elution in HPLC using the gradient steepness parameter.

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References

  1. Glidenberg, L., and J.R. Trowbridge, JAOCS 42:69 (1965).

    Google Scholar 

  2. Tornquist, J., Acta Chem. Scand. 20:572 (1966).

    Article  CAS  Google Scholar 

  3. McCoy, R.N., and A.B. Bullock, JAOCS 46:289 (1969).

    CAS  Google Scholar 

  4. Allen, M.C., and D.E. Linder, JAOCS, in press (presented at the ISF/AOCS World Congress in New York City, April 27–May 1, 1980).

  5. Nakamura, K., and I. Matsumoto, J. Chem. Soc. Japan 8:1342 (1975).

    Google Scholar 

  6. Szakasits, J.J., and R.E. Robinson, Anal. Chem. 46:1648 (1974).

    Article  CAS  Google Scholar 

  7. Shell Method Series 561.

  8. Snyder, L.R., J.W. Dolan and J.R. Gant, J. Chromatogr. 165:3 (1979).

    Article  CAS  Google Scholar 

  9. Dolan, J.W., J.R. Gant and L.R. Snyder, J. Chromatogr. 165:31 (1979).

    Article  CAS  Google Scholar 

  10. Snyder, L.R., in High Performance Liquid Chromatography, edited by C. Horwath, Academic Press, New York, NY, 1980.

    Google Scholar 

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Authors and Affiliations

  1. Shell Development Company, Westhollow Research Center, 77001, Houston, TX

    J. D. McClure

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  1. J. D. McClure
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McClure, J.D. Determination of ethylene oxide oligomer distributions in alcohol ethoxylates by HPLC using a rotating disc-flame ionization detector. J Am Oil Chem Soc 59, 364–373 (1982). https://doi.org/10.1007/BF02541021

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  • DOI: https://doi.org/10.1007/BF02541021

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