title: Increased sensitivity of OSHA method analysis of diacetyl and 2,3-pentanedione in air.
abstract: Gas chromatography/mass spectrometry (GC/MS) operated in selected ion monitoring mode was used to enhance the sensitivity of OSHA Methods 1013/1016 for measuring diacetyl and 2,3-pentanedione in air samples. The original methods use flame ionization detection which cannot achieve the required sensitivity to quantify samples at or below the NIOSH recommended exposure limits (REL: 5 ppb for diacetyl and 9.3 ppb for 2,3-pentanedione) when sampling for both diacetyl and 2,3-pentanedione. OSHA Method 1012 was developed to measure diacetyl at lower levels but requires an electron capture detector, and a sample preparation time of 36 hours. Using GC/MS allows detection of these two alpha-diketones at lower levels than OSHA Method 1012 for diacetyl and OSHA Method 1016 for 2,3-pentanedione. Acetoin and 2,3-hexanedione may also be measured using this technique. Method quantification limits were 1.1 ppb for diacetyl (22% of the REL), 1.1 ppb for 2,3-pentanedione (12% of the REL), 1.1 ppb for 2,3-hexanedione, and 2.1 ppb for acetoin. Average extraction efficiencies above the limit of quantitation were 100% for diacetyl, 92% for 2,3-pentanedione, 89% for 2,3-hexanedione, and 87% for acetoin. Mass spectrometry with OSHA Methods 1013/1016 could be used by analytical laboratories to provide more sensitive and accurate measures of exposure to diacetyl and 2,3-pentanedione.
authors: a Field Studies Branch, Respiratory Health Division, National Institute for Occupational Safety and Health , Morgantown , West Virginia.
authors: Ryan
authors: R
authors: LeBouf
authors: b Methods Development Team, Occupational Safety and Health Administration , United States Department of Labor , Sandy , Utah.
authors: Michael
authors: M
authors: Simmons
mesh_terms: D003931:Diacetyl / Q000032:analysis* / Q000737:chemistry; D004784:Environmental Monitoring / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D009314:National Institute for Occupational Safety and Health, U.S.; D016273:Occupational Exposure / Q000032:analysis*; D010422:Pentanones / Q000032:analysis* / Q000737:chemistry; D014481:United States; D014489:United States Occupational Safety and Health Administration
chemical_list: D010422:Pentanones; D003931:Diacetyl; C013186:2,3-pentanedione
keywords: 2,3-pentanedione; OSHA Methods 1013/1016; diacetyl; increased sensitivity; mass spectrometry