Page:NIOSH Manual of Analytical Methods - 2554.pdf/2

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GLY CO L ET HER S: ME TH OD 2554, Issue 1, dated 1 5Ma rch 2003 - Page 2 of 4 REAGENTS:

EQUIPMENT:

1. Propylene glycol m ono m ethyl ethe r, reag ent grad e.* 2. Dipropylene glycol monomethyl ether, reagent grad e.* 3. Propylene glycol monomethyl ether acetate, reag ent grade .* 4. Me thylene chloride, chrom atographic gra de.* 5. Me than ol, chrom atog raph ic grade.* 6. Desorbing solution, 15% m ethanol in 85% m ethylene chloride (V/V). 7. Propylene glycol monomethyl ether calibration stock solution, 46.2 mg/m L. Dilute 0.5 mL analyte to 10 mL with desorbing solution. 8. Dipropylene glycol monomethyl ether calibration stock solution, 47.5 mg/m L. Dilute 0.5 mL analyte to 10 mL with desorbing solution. 9. Propylene glycol m ono m ethyl ethe r ace tate calibra tion sto ck solution, 48.5 m g/m L. Dilute 0.5 mL nitrobenzene to 10 mL with desorbing solution. 10. Air, compressed, purified, and filtered. 11. Helium, purified and filtered. 12. Hydrogen, filtered.

1. Sam pler: glass tube, 7 cm long, 6-mm OD, 4mm ID, flame-sealed ends, containing two sections of Anasorb® 747 (140mg/70 mg) sep arate d by a 2 -m m ureth ane foam plug. A silylated glass wool plug precedes the front section. A urethane foam plug follows the back sectio n. T ubes are com m ercially available from SKC, Inc. 2. Personal sampling pump, 0.1 to 0.2 L/min, connected with flexible tubing. 3. Gas chrom atograph, FID, integrator, and 30-m Stabilwax-DA or equivalent capillary column (page 255 4-1). 4. Vials, autosampler, with PTFE-lined caps. 5. Syringes, 10-:L, 25-:L, and 1-mL. 6. Volumetric flasks, 10-mL. 7. Refrigerant packs for shipping.

  • See SPECIAL PRECAUTIONS

SPECIAL PRECAUTIONS: Methylene chloride is a carcinogen [3]. Methanol is very flamm able and toxic. Glycol ethers are irritants and hazardous compounds. W ear appropriate protective clothing and work with these compounds in a well-ventilated hood. SAMPLING: 1. Ca librate each pers ona l sam pling pum p with a represe ntative sam pler in line. 2. Break the ends of the sampler imm ediately prior to sampling. Attach sampler to personal sampling pump with flexible tubing. 3. Sam ple at an accurately known flow rate between 0.1 and 0.2 L/min for a total sample size of 10 L. 4. Cap the samplers with plastic (not rubber) caps and pack securely for shipment. Samples should be kept cold.

SAMPLE PREPARATION: 5. Place the front and back sorbent sections of the sampler tube in separate vials. Place the glass wool preceding the front section into the vial containing the front section. Discard the remaining foam plugs. 6. Ad d 1.0 m L of the desorbing solution into each vial. Attach crim p caps to each vial. 7. Plac e the sam ple vials in an u ltrasonic ba th for 3 0 m inutes .

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition