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The determination in air of selected low-molecular weight aldehydes as their oxazolidines by capillary gas chromatography.
Kennedy-ER; Gagnon-YT; Okenfuss-JR; Teass-AW
Appl Ind Hyg 1988 Oct; 3(10):274-279
A method was presented for sampling and analysis of low molecular weight aldehyde compounds in air as their oxazolidine derivatives. Tested chemicals included 2-furaldehyde (98011), pentanedial (111308), and pentanal (110623). Sample vapors were generated and trapped in sorbent tubes. Sorbent tubes contained XAD-2 resin coated with 2-(hydroxymethyl)piperidine, which reacted with the compounds to form their oxazolidine derivatives. These were then eluted with toluene and analyzed by capillary gas chromatography and mass spectroscopy. The derivatives were resolved from each other and from the derivatizing agent on fused silica DB-5 columns of 10 and 30 meter lengths. Not all isomers were completely resolved. Calibration curves constructed from combined isomer peak areas were linear over the range of 1 to 100 nanograms per microliter. Detection limits were 0.6 to 9.2 micrograms (microg) per sample for 2-furaldehyde, 0.2 to 6.8microg per sample for pentanedial, and 0.4 to 4.6microg per sample for pentanal. Recovery of each aldehyde from sorbent was essentially quantitative. Maximum sampling parameters based on breakthrough studies were determined for each compound. The method was tested on five other chemicals: 2- methylpropanal (78842), propanal (107028), 2-butenal (4170303), formaldehyde (50000), and acrolein (107028). The acrolein derivative was not resolved from the propanal derivative, and sorbent capacity limitations for 2-methylpropanal, propanal, and 2- butenal were too severe to warrant method development. Pooled relative standard deviations were 7.6 percent for 2-furaldehyde, 8.7 percent for pentanedial, and 7.3 percent for pentanal. The latter two compounds could be stored at room temperature for 5 and 4 weeks, respectively, without loss of integrity, while 2-furaldehyde could only be stored for 2 weeks. The authors conclude that this sampling and analysis method exhibits precision and accuracy within established criteria.
NIOSH-Author; Analytical-methods; Air-samples; Aldehydes; Gas-chromatography; Sampling-methods; Sample-preparation; Chromatographic-analysis
98-01-1; 111-30-8; 110-62-3; 78-84-2; 107-02-8; 4170-30-3; 50-00-0; 107-02-8
Issue of Publication
Applied Industrial Hygiene
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Content source: National Institute for Occupational Safety and Health Education and Information Division