GLUTARALDEHYDE: METHOD 2531, Issue 2, dated 15 August 1993 - Page 2 of 5 EQUIPMENT:
REAGENTS: 1. Toluene, chromatographic quality. 2. 2-(Hydroxymethyl)piperidine. Recrystallize several times from isooctane until there is one major peak (>95% of area) by GC analysis. Store in desiccator. 3. Amberlite XAD-2 (Rohm and Haas) or equivalent. 4. Glutaraldehyde,* 25% (w/v) solution in water. 5. Glutaraldehyde stock solution, 10 µg/µL (see APPENDIX A). 6. Glutaraldehyde oxazolindine (see APPENDIX B) stock solution, 2 mg/mL. Add 20 mg to toluene and dilute to 10 mL. 7. Sulfuric acid, 0.02 N. 8. Sodium hydroxide, 0.01 N. 9. Sodium sulfite, 1.13 M. Prepare fresh immediately before use. 10. Water, deionized, then distilled. 11. Hydrogen, prepurified. 12. Air, filtered. 13. Helium, purified. 14. Magnesium sulfate.
See SPECIAL PRECAUTIONS.
1. Sampler: glass tube, 10 cm long, 6-mm OD, 4-mm ID, flame-sealed ends and plastic caps, containing two sections of 40/60 mesh 2(hydroxymethyl) piperidine-coated XAD-2 (see APPENDIX C). Sorbent sections are retained and separated by small plugs of silanized glass wool. Pressure drop across the tube at 0.10 L/min airflow must be less than 760 kPa (5.7 mm Hg). Tubes are commercially available (Supelco ORBO 23 or equivalent). 2. Personal sampling pump, 0.01 to 0.08 L/min, with flexible connecting tubing. 3. Gas chromatograph, flame ionization detector, integrator and column (page 2531-1). 4. Ultrasonic bath. 5. Vials, glass, 4-mL, with septum and plastic screw caps. 6. Flasks, volumetric, 10-, 25-, and 50-mL. 7. Pipets, TD, 1-, 2-, and 10-mL with pipet bulb. 8. Pipets, disposable, 2-mL. 9. Syringes, 10-µL (readable to 0.1 µL), 25-, and 50-µL. 10. File. 11. Beakers, 50-mL. 12. pH meter. 13. Magnetic stirrer. 14. Burets, 50-mL. 15. Flasks, round-bottomed, 100-mL. 16. Soxhlet extraction apparatus. 17. Vacuum oven. 18. Distillation apparatus.
SPECIAL PRECAUTIONS: Glutaraldehyde can irritate the mucous membranes and act on the central nervous system [3]. Work with this compound only in a well-ventilated hood.
SAMPLING: 1. 2. 3.
Calibrate each personal sampling pump with a representative sampler in line. Break ends of the sampler immediately before sampling. Attach sampler to personal sampling pump with flexible tubing. Sample at an accurately know flow rate between 0.01 and 0.08 L/min for a total sample size of 4 to 39 L. For ceiling determination, sample at 0.2 L/min for 20 min. NOTE: The aldehyde reacts with the 2-(hydroxymethyl)piperidine to form an oxazolidine derivative in the sorbent bed during sampling (see equation below). Sampling rate is limited by the speed of this reaction. Sampling rates above 0.1 L/min for extended periods may cause breakthrough owing to incomplete reaction, possibly invalidating the sample. O=CH(CH 2)3CH=O + 2 C 5H9NHCH 2OH glutaraldehyde 2-(hydroxymethyl)piperidine
= (C 7H12NO) 2(CH 2)3 oxazolidine derivative
+
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/93
H 2O
