Page:NIOSH Manual of Analytical Methods - 5007.pdf/3

 ROTENONE: METHOD 5007, Issue 2, dated 15 August 1994 - Page 3 of 3 MEASUREMENT: 9.

10.

Set HPLC system according to manufacturer's recommendations and to conditions given on page 5007-1. Inject 10-µL sample. NOTE: If peak area is above linear range of calibration graph, dilute, reanalyze, and apply appropriate dilution factor in calculations. Measure peak area.

CALCULATIONS: 11. 12.

Read the mass, mg (corrected for recovery) of Rotenone found on the filter (W) and average media blank (B) from the calibration graph. Calculate the concentration, C (mg/m 3), of Rotenone in the air volume sampled, V (L):

EVALUATION OF METHOD: Method S300 [2] was issued on May 11, 1979, and validated over the range 1.16 to 11.1 mg/m 3 at 25°C and 760 mm, using 100-L samples [1, 5]. Overall precision, SˆrT, was 0.079 with average recovery 100.4%, representing a non-significant bias. The concentration of Rotenone (generated by Wright dust feeder using Ortho Rotenone Dust [1%; Chevron Chemical Co.] enriched to 10% Rotenone with analytical grade Rotenone [Aldrich Chemical Co.]) was independently verified by collection in dioxane and HPLC analysis. Recovery was 0.98 in the range 250 to 1000 µg Rotenone per sample. Collection efficiency of the PTFE filter was found to be greater than 99% and no detectable Rotenone (LOD = 4 µg) was found on Chromosorb 102 tubes placed behind the PTFE filters at 11.8 mg/m 3. No loss was seen from spiked filters stored in the dark at room temperature for seven days.

REFERENCES: [1] Backup Data Report prepared under NIOSH Contract 210-76-0123, available as Order No. PB 82-114729 from NTIS, Springfield, VA 22161. [2] NIOSH Manual of Analytical Methods, 2nd. ed., V. 5, S300, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 79-141 (1979). [3] Gunther, F. A., and R. G. Blinn. Analysis of Insecticides and Acaricides, 419-420, Interscience, NY (1955). [4] Bushway, R. J., B. S. Engdahl, B. M. Colvin, and A. R. Hanks. J. Assoc. Official Anal. Chemists , 58, 965 (1975). [5] NIOSH Research Report-Development and Validation of Methods for Sampling and Analysis of Workplace Toxic Substances, U.S. Department of Health and Human Services, Publ. (NIOSH) 80-133 (1980).

METHOD REVISED BY: Jerome Smith, Ph.D., NIOSH/DPSE; S300 originally validated under NIOSH Contract 210-76-0123.

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