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Analytical problems encountered with NIOSH method 5521 for total isocyanates

R J Key-Schwartz1

  • 1Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, Cincinnati, Ohio 45226, USA.

American Industrial Hygiene Association Journal
|May 1, 1995
PubMed
Summary

National Institute for Occupational Safety and Health Method 5521 faced challenges identifying isocyanate oligomers in air samples. Supplementing with UV spectra from a photodiode array detector improved identification, questioning the original method's sufficiency.

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Area of Science:

  • Occupational Health and Safety
  • Analytical Chemistry
  • Environmental Monitoring

Background:

  • National Institute for Occupational Safety and Health (NIOSH) Method 5521 is used for analyzing total isocyanates in air.
  • Challenges exist in identifying specific oligomeric isocyanate species using this method.
  • Common issues include false negative and false positive results in chromatographic analysis.

Purpose of the Study:

  • To address difficulties in identifying oligomeric isocyanate species using NIOSH Method 5521.
  • To evaluate the effectiveness of supplementing the method's ratio criterion with additional spectral data.
  • To determine if the existing ratio criterion is adequate for qualitative identification of isocyanate oligomers.

Main Methods:

  • Analysis of total isocyanates in air samples using NIOSH Method 5521.

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  • High-performance liquid chromatography (HPLC) with UV detection.
  • Supplementation of the method's ratio criterion with complete UV absorption spectra from a photodiode array (PDA) detector.
  • Main Results:

    • A false negative response was observed in most field samples during HPLC analysis.
    • An anomalous peak caused false positive results in some field blanks and samples.
    • Supplementing with PDA UV spectral data successfully identified the problematic peaks, including an oligomeric isocyanate species.

    Conclusions:

    • The ratio criterion of NIOSH Method 5521 alone may be insufficient for the qualitative identification of isocyanate oligomers.
    • Utilizing complete UV absorption spectra from a PDA detector enhances the accuracy of isocyanate analysis.
    • Further validation is needed to confirm the reliability of NIOSH Method 5521 for oligomeric isocyanate identification.