Page:NIOSH Manual of Analytical Methods - 5516.pdf/2

2,4- and 2,6-TOLUENEDIAMINE: METHOD 5516, Issue 2, dated 15 August 1994 - Page 2 of 5


 * 1) Toluene, reagent grade.
 * 2) 1-(2-Methoxyphenyl)piperazine, purified (seeAPPENDIX A).
 * 3) Sampling medium: 43 μg/mL 1-(2-methoxy-phenyl)piperazine in toluene.
 * 2,4-Toluenediamine*, reagent grade.
 * 2,6-Toluenediamine*, reagent grade.
 * 1) Acetic anhydride, reagent grade.
 * 2) Methanol, reagent grade.
 * 3) Mobile phase A: Dissolve 60 mg anhydroussodium acetate in 1 L of 12% acetonitrile indistilled water. Add 17% (V/V) aqueous aceticacid. Bring pH to 6.0.
 * 4) Mobile phase B: Acetonitrile, chromatographicquality.
 * 5) Water, distilled deionized.
 * 6) Sodium acetate, anhydrous.
 * 2,4-Bisacetamidotoluene, (see APPENDIX B).
 * 2,6-Bisacetamidotoluene, (see APPENDIX B).
 * 1) Calibration stock solution, 0.5 μg/μL. Dissolve 5mg each of 2,4- and 2,6-bisacetamidotoluenein methanol. Dilute to 10 mL.
 * 2) Nitrogen, prepurified.
 * 3) Pentane*, purified.


 * 1) Sampler: midget impinger, 25-mL.
 * 2) Personal sampling pump, 1 L/min, with flexibleconnecting tubing.
 * 3) Liquid chromatograph (HPLC) with 229-nmUV detector, recorder, integrator, and column(page 5516-1).
 * 4) Vials, 4-mL and 20-mL, glass, with PTFE-linedcaps.
 * 5) Pipets, pasteur, 14.6-cm, glass disposable.
 * 6) Volumetric flasks, 10-mL.
 * 7) Syringes, 10- and 100-μL.
 * 8) Pipets, 2-mL (graduated) and 15-mL, glass,with pipet bulb.
 * 9) Water bath.
 * 10) Hotplate, spark-free, 35 to 50 °C.
 * 11) Evaporator, Mini-Vap, six-port, or equivalent.
 * 12) pH meter.
 * 13) Beakers, 250-mL.
 * 14) Flask, filtration, 500-mL.
 * 15) Funnel, Buchner, fritted glass, 100-mL.
 * 16) Vacuum pump.
 * 17) Vacuum desiccator.
 * 18) Watchglass.


 * See SPECIAL PRECAUTIONS

2,4-Toluenediamine is a cancer suspect agent [13]; 2,6-toluenediamine may be mutagenic [14]. Handle these chemicals carefully in a hood or glove box, and avoid working-surface contamination which might occur by spillage or by dissipation of fine powder from opening of containers or making transfers. Pentane is highly volatile and flammable. Take adequate precautions while handling pentane.


 * 1) Calibrate each personal sampling pump with a representative sampler in line.


 * 1) Transfer 15.0 mL sampling medium to an impinger.


 * 1) Connect the assembled impinger to a sampling pump.

5. Transfer sample solution, including condensed water, to a 20-mL vial for shipment. Rinse impingerwith 1 to 2 mL toluene. Add rinsings to sample solution. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
 * 1) Sample 30 to 500 L of air at an accurately measured sampling rate of1 L/min. When it is necessary toadd solvent for proper impinger operation during sampling, add only toluene.NOTE: The reagent in the sampling medium reacts with isocyanates present to form ureas, thuspreventing reaction of the isocyanate with the toluenediamines.