Page:NIOSH Manual of Analytical Methods - 2541.pdf/5

 FORMALDEHYDE: METHOD 2541, Issue 2, dated 15 August 1994 - Page 5 of 5 APPENDIX B: SORBENT PREPARATION (optional if commercially-prepared tubes are used) Extract 4 h in Soxhlet with 50/50 (v/v) acetone/methylene chloride. Replace with fresh solvent and repeat. Vacuum dry overnight. Add 1 g purified 2-(hydroxymethyl)piperidine in 50 mL toluene for each 9 g extracted XAD-2 sorbent. Allow this mixture to stand 1 h with occasional swirling. Remove the solvent by rotary evaporation at 37 °C and dry at 130 kPa (1 mm Hg) at ambient temperature for ca. 1 h. To determine the amount of background for each batch, desorb several 120-mg portions of the coated sorbent with toluene and analyze (steps 12 and 13). No blank peak is expected for any aldehydes other than formaldehyde and possibly acetaldehyde.

APPENDIX C: SYNTHESIS OF FORMALDEHYDE OXAZOLIDINE Place a solution of purified 2-(hydroxymethyl)piperidine (0.57 g, 5 mmol) in 10 mL of toluene in a 50-mL round-bottomed flask. Use several 2-mL portions of toluene to rinse residual 2-(hydroxymethyl) piperidine from the container used for weighing. Add magnesium sulfate (2.5 g) to the round-bottomed flask to dry the aldehyde solution as it is added and to remove the water which forms during the reaction. Add a solution of 1 mL 37% aqueous formaldehyde in 10 mL toluene to the 2-(hydroxymethyl)piperidine solution dropwise with stirring over 1 h. Stir the solution overnight, then filter to remove the magnesium sulfate. Remove the toluene from the solution at reduced pressure by rotary evaporation.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94