Dynamic Sampling Method for Diacetyl and Acetoin Using Tenax TA Solid Sorbent and (2,3, 4,5, 6-Pentafluorobenzyl) Hydroxylamine Hydrochloride (PFBHA)

Details

• Personal Author:
  Que Hee S ; Takaku S
• Description:
  The research was performed to develop a dynamic sampling method for diacetyl and acetoin based on 10% (w/w) (2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) coated on Tenax TA (80/100 mesh). Diacetyl (buttery taste and smell) and acetoin are the dominant flavoring-additive ketones used for microwave popcorn, and both are associated with incidents of Bronchiolitis obliterans. Because diacetyl has two carbonyl groups, the monosubstituted and the disubstituted, O-oxime derivatives had to be synthesized to assess the chemisorption of diacetyl onto the coated solid sorbent. The O-oxime of acetoin and mono- and disubstituted O-oximes of diacetyl with PFBHA were synthesized to make standard curves. The yields of the derivatives were 93.9 +/- 1.8%, 93.8 +/- 4.2%, and 73.8 +/- 2.8%, and their purities were 98.9 +/- 0.6%, 99.1 +/- 0.2%, and 88.8 +/- 8.3%, respectively, using temperature-programmed capillary gas chromatography-mass spectrometry by m/z 181 selective ion monitoring. The linear range was 17-32 ng for the acetoin derivative and 2.4-42 ng for the mono- and disubstituted diacetyl derivatives. Five different concentrations (0, 0.1, 0.5, 1.0, 1.5, and 2.0 mg/m3) of acetoin and diacetyl were generated in Tedlar gas bags by injection of the appropriate mass of ketone in water solvent and using the appropriate air volume. Each gas bag, in triplicate at each concentration, was sampled using a personal sampling pump set at calibrated flow rates of 10 and 50 mL/min. Preliminary results showed that the 50 mL/min flow rate caused breakthrough through a 200-mg front section onto a 50-mg back section at 2.0 mg/m3. The 2.0 mg/m3 concentration of acetoin and diacetyl was detected on the front section, with 82 +/- 20% and 79 +/- 16% recovery, respectively, at 10 mL/min. Similar recoveries were obtained at 1.0 and 1.5 mg/m3. Both diacetyl and acetoin can be separated and determined by this method from the same air sample. [Description provided by NIOSH]
• Subjects:
  Diacetyl Environmental Monitoring Flavoring Agents Occupational Health Safety
• Keywords:
  Acetoin Air Sampling Flavorings Gas Chromatography Mass Spectrometry Sampling Methods
• Publisher:
  American Industrial Hygiene Association
• Document Type:
  Text
• Funding:
  Grant
• Genre:
  Abstract or Summary
• Place as Subject:
  California ; OSHA Region 9
• CIO:
  National Institute for Occupational Safety and Health (NIOSH)
• Topic:
  Workplace Safety & Health
• Location:
  North America
• Pages in Document:
  13
• NIOSHTIC Number:
  nn:20058546
• Citation:
  AIHce 2009: American Industrial Hygiene Conference and Exposition, May 30 - June 4, 2009, Toronto, Canada. Fairfax, VA: American Industrial Hygiene Association, 2009 May; :13
• CAS Registry Number:
  Acetoin (CAS RN 513-86-0) ; Butanedione (CAS RN 431-03-8)
• Federal Fiscal Year:
  2009
• Performing Organization:
  University of California Los Angeles
• Peer Reviewed:
  False
• Start Date:
  20050701
• Source Full Name:
  AIHce 2009: American Industrial Hygiene Conference and Exposition, May 30 - June 4, 2009, Toronto, Canada
• End Date:
  20270630
• Collection(s):
  National Institute for Occupational Safety and Health
• Main Document Checksum:
  urn:sha-512:826bf206e40ac552f7ba0ee278307680c352d64b1c38bf9e285498939a6b501c95f0a0f3373fba748592a2687359d042ce6817566e059dc1fb51753043af930e
• Download URL:
  https://stacks.cdc.gov/view/cdc/221611/cdc_221611_DS1.pdf
• File Type:
  [PDF - 179.81 KB ]