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 ETHYLENIMINE: METHOD 3514, Issue 2, dated 15 August 1994 - Page 4 of 4 (recovery = average found concentration divided by the taken concentration) ranged from 91 to 105% for six sets of samples at 0.16 to 21 mg/m 3; thus, bias for sampling and analysis was not significant. Collection efficiencies of samplers at 0.15 L/min were >99% at 21 and 204 mg/m 3. Average recoveries from 15-mL quantities of Folin's reagent (fortified with ethylenimine in chloroform) were 0.93 and 0.95 at the 1.67- and 16.7-µg levels of ethylenimine, respectively; the precision ( Sr) was 0.024 (12 samples, pooled). Samples at the 1.67- and 16.7-µg levels were stable in Folin's reagent during storage for 14 days at 5 °C in the dark. Methylamine, diethylamine, butylamine, ethanolamine, dihexylamine, dicyclohexylamine, benzylamine, dibenzylamine, and aniline do not interfere with measurement of ethylenimine. Propylenime and 2bromoethylamine interfere.

REFERENCES: [1] [2] [3] [4] [5] [6] [7]

Analytical Report for Ethylenimine, Sequence #3680. Unpubl., NIOSH (1982) Ruhe, R.L., NIOSH Health Hazard Evaluation Report, HETA 82-287-1240, NIOSH, Cincinnati, Ohio (1982). NIOSH Manual of Analytical Methods, 2nd ed., V. 5, P&CAM 300, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 79-141 (1979). Evans, D.J., R.J. Mayfield and I.M. Russell. J. Chromatogr ., 115, 391-395 (1975). Rosenblatt, D.H., P. Hlinka and J. Epstein. Anal. Chem., 27, 1290-1293 (1955). Crompton, T.R. Analyst (London), 90, 107-111 (1965). NIOSH/OSHA Occupational Health Guidelines for Chemical Hazards, U.S. Department of Health and Human Services, Publ. (NIOSH) 81-123 (1981), available as GPO Stock #17-033-00337-8 from Superintendent of Documents, Washington, D.C. 20402.

METHOD WRITTEN BY: Samuel P. Tucker, Ph.D., NIOSH/DPSE; P&CAM 300 developed under NIOSH contract.

APPENDIX SYNTHESIS OF 4-(1-AZIRIDINYL)-1,2-NAPHTHOQUINONE Place 2 g of 1,2-naphthoquinone-4-sulfonic acid, sodium salt, and 250 mL of water into a 1-L separatory funnel which is wrapped with aluminum foil. Add 25 mL of 0.5 M trisodium phosphate, and shake the mixture. Ascertain that the pH is between 10.5 and 11.5. Add 0.3 mL of ethylenimine and shake at intervals over 10 min. Extract the 4-(1-aziridinyl)-1,2-naphthoquinone with six 200-mL portions of chloroform. Combine extracts in a 2-L beaker wrapped with aluminum foil. Cover the beaker with aluminum foil which is punctured with three holes, and evaporate chloroform with a nitrogen purge. Transfer the dry residue to a 50-mL beaker wrapped with aluminum foil. Add 35 mL of methanol and 1 mL of chloroform to the residue. A portion of the residue will remain undissolved. Filter and cool the solution to 0 °C. Wash the crystallized product with 4 mL of chilled methanol, and dry the product with a nitrogen purge. Melting point = 173 to 175 °C.

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