GLUTARALDEHYDE: METHOD 2532, Issue 1, dated 15 August 1994 - Page 2 of 4 EQUIPMENT:
REAGENTS: 1. Glutaraldehyde, 25% (w/v) solution in water (Aldrich D19,930-3 or equivalent).* 2. Water, distilled, deionized. 3. Acetonitrile, HPLC grade. 4. Sodium sulfite, 1.13 M. Prepare fresh immediately before use. 5. Sulfuric acid, 0.02 N. 6. Sodium hydroxide, 0.01N.
See SPECIAL PRECAUTIONS.
1. Sampler: Glass tube, 110 mm long, 6-mm OD, flame-sealed ends and plastic caps containing two sections of silica gel coated with 2,4-dinitrophenylhydrazine HCl. The front section contains 300 mg, the back 150 mg, and sections are retained and separated by small plugs of silanized glass wool. (SKC 226-119 or equivalent). NOTE: The hydrochloride salt provides an acid catalyst for the reaction of glutaraldehyde with the dinitrophenylhydrazine. Other acids may be used as catalyst. 2. Personal sampling pump, 0.05 to 0.5 L/min, with flexible connecting tubing. 3. High performance liquid chromatograph (HPLC), UV detector (365 nm), column, and integrator (page 2532-1). 4. Shaker, mechanical. 5. Syringe, 10-mL, disposable. 6. Vials, glass, scintillation, 20-mL, with PTFElined caps. 7. Syringes, microliter, readable to 0.1-µL. 8. Flasks, volumetric, various sizes. 9. Pipets, various sizes. 10. Burets, 50-mL. 11. Stirrer, magnetic. 12. pH meter. 13. Beakers, 50-mL. 14. File.
SPECIAL PRECAUTIONS: Glutaraldehyde can irritate the mucous membrane and act on the central nervous system [2]. Work with this compound only in a well-ventilated hood.
SAMPLING: 1. 2. 3.
4.
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 known flow rate between 0.05 and 0.5 L/min for a total sample size of 1 to 30 L. NOTE: Glutaraldehyde reacts with the 2,4-dinitrophenylhydrazine to form a hydrazone derivative which provides sample stability and UV chromophores for analysis. The hydro Immediately after sampling, cap the sample tubes, including blanks, and pack securely for shipment, include 10-20 unused tubes from the same lot to be used for standard preparation.
SAMPLE PREPARATION: 5. 6.
Score each sampler with a file in front of the front sorbent section and break the tube at the score line. Remove and place front glass wool plug and front sorbent section (300 mg) in a vial. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
