National Institute for Occupational Safety and Health

Summary

National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

The molecular ion for a particular aldehyde is equal to the molecular weight of the original aldehyde plus 97. Fragmentation patterns are also important for the identification of the oxazolidines. NOTE 2: The absence of some C 3-C 5 aldehydes, such as propionaldehyde, isobutyraldehyde and crotonaldehyde, does not necessarily mean that these compounds are not present in the air sampled. These compounds are not efficiently trapped by the sorbent, and will readily breakthrough the sampler sorbent beds.
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National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

For the other aldehydes, add measured aliquots (ca. 12 :L) of each to toluene in 10-mL volumetric flasks and dilute to the mark. From the density of each aldehyde, determine the amount of each aldehyde present in each solution (ca. 1 :g/:L) . b. Inject 10 :L of the standard aldehyde solutions separately onto blank tubes from the same lot as the field samples. c. Analyze (steps 4 through 7 and 10 through 12) along with blanks for qualitative identification of derivative peaks by retention times.
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National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

METHOD 2539, Issue 2, dated 15 August 1994 - Page 4 of 10 chrom atogram ) . a. Analyze samples with GC retention times matching any oxazolidine by GC/MS using the same GC columns and conditions if possible. Alternate columns such as a DB-WAX (formaldehyde, acetaldehyde, propanal) or DB-1 (remaining aldehydes) may also be used for GC/MS confirmation depending on which aldehyde is suspected. b. Determine the presence of oxazolidines by monitoring for specific ions known to be present in the derivative spectra.
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