Page:NIOSH Manual of Analytical Methods - 3514.pdf/2

ETHYLENIMINE: METHOD 3514, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

12.

13. 14.

15.

EQUIPMENT:

Chloroform with 1% ethanol as a preservative, UV grade. Hexane, UV grade. 2-Propanol, UV grade. Methanol, UV grade. Ethylenimine.* 1,2-Naphthoquinone-4-sulfonic acid, sodium salt. Deionized water. NaOH solution (0.1 M). Dissolve 1 g of NaOH in water to make 250 mL of solution. KH 2PO 4 solution (0.1 M). Dissolve 3.40 g of KH 2PO 4 in water to make 250 mL of solution. Buffer solution (pH = 7.7). Mix 100 mL of 0.1 M KH 2PO 4 with 93.4 mL of 0.1 M NaOH. Folin's reagent. Dissolve 0.40 g of 1,2naphthoquinone-4-sulfonic acid, sodium salt, in 100 mL of buffer solution. Dilute to 500 mL with water. Wrap flask with aluminum foil and refrigerate. Solution is stable for 5 days. Na 3PO 4 solution (0.5 M). Dissolve 19 g of Na 3PO 4·12H2O in water to make 100 mL of solution. 4-(1-Aziridinyl)-1,2-naphthoquinone. See Appendix. Calibration stock solution, 500 µg/mL. Dissolve 125 mg of 4-(1-aziridinyl)-1,2naphthoquinone in chloroform to make 250 mL of solution. Recovery stock solution, 10 mg/mL. Dissolve 2.50 g of ethylenimine in chloroform to make 250 mL of solution.

1. Sampler: midget bubbler, with 15 mL of Folin's reagent. 2. Personal sampling pump, 0.2 L/min, with flexible, connecting tubing. 3. High performance liquid chromatograph with column (page 1) and UV detector. 4. Syringes, 1-mL, readable to 10 µL. 5. Syringes, 100-µL, readable to 1 µL. 6. Syringes, 10-µL, readable to 0.1 µL. 7. Volumetric flasks, low actinic glass, 500-, 250, 100-, and 10-mL. 8. Graduated cylinders, 100- and 25-mL. 9. Separatory funnels with PTFE stopcocks. 10. Funnels, glass. 11. Beakers, 2-L and 50-mL. 12. Aluminum foil. 13. Filter paper. 14. pH paper. 15. Pipet bulb.

See SPECIAL PRECAUTIONS.

SPECIAL PRECAUTIONS: Ethylenimine is carcinogenic, very toxic, and extremely flammable [7]. This compound is strongly irritating to the eyes, skin, and mucous membranes. Handle only in a hood.

SAMPLING: 1. 2. 3.

4.

Calibrate the personal sampling pump with a representative sampler in line. Sample at 0.2 L/min for a sample size of 1 to 48 L. After sampling, use a pipet bulb to force air through the bubbler stem to dislodge ethylenimine derivative and recover sampling solution. Rinse the stem with 2 mL of chloroform, and add the wash to the bubbler. Seal the bubbler with a nonreactive stopper (PTFE or glass). Do not seal with rubber. Protect the sample from light, and ship at 5 °C.

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