National Institute for Occupational Safety and Health

“ No blank peak is expected for furfural. SYNTHESIS OF FURFURAL OXAZOLIDINE [1] : Place a solution of 0.58 g (0.5 mL; 6 mmol) freshly distilled furfural in 10 mL toluene in a 50-mL round-bottomed flask. Add 2.5 g magnesium sulfate to the flask to remove water which forms during the reaction. Add a solution of 0.61 g (5.3 mmol) purified 2-hydroxymethylpiperidine in 10 mL toluene dropwise with stirring over 1 hr. Stir the solution overnight, then filter to remove the magnesium sulfate. Remove the toluene from the solution at reduced pressure by rotary evaporation. ”

“ Prepare and analyze a set of oxazolidine standard solutions (step 9.a) and a set of working standards (step 10) including media blanks. b. Treating the working standards as unknowns, read the mass (mg) of oxazolidine found in each working standard (W) , and in the average media blank (B) . c. Using the mass of furfural, mg, spiked onto the working standard (W o) and the stoichiometric conversion factor between furfural and furfural oxazolidine (2.01) , calculate the desorption efficiency:
d. Prepare a graph of DE vs. μg furfural recovered per sample [ (W - B) /2.01] . ”

“ Break the ends of the sampler immediately before sampling. Attach sampler to personal sampling pump with flexible tubing. Sample at an accurately known flow rate between 0.01 and 0.05 L/min for a total sample size of 1 to 12 L. NOTE: Furfural reacts with 2- (hydroxymethyl) piperidine to form a derivative during sampling. Sampling rate is limited by the speed of this reaction; rates above 0.05 L/min may cause breakthrough owing to incomplete reaction.
SAMPLE PREPARATION: 4. 5.
Score each sampler with a file in back of the rear sorbent section. Break sampler at score line. ”