Page:NIOSH Manual of Analytical Methods - 5025.pdf/3

 CHLORINATED DIPHENYL OXIDE: METHOD 5025, Issue 2, dated 15 August 1994 - Page 3 of 4 MEASUREMENT: 8.

9.

Set gas chromatograph according to manufacturer's recommendations and to conditions given on page 5025-1. Inject sample aliquot manually using solvent flush technique or with autosampler. Open the effluent vent to keep the solvent from passing into the detector. Close the effluent vent after the solvent peak has eluted. NOTE: Under conditions given, the solvent elutes in about 20 sec. The large quantity of solvent injected may cause malfunction of the conductivity cell, unless it is vented. Sum the areas of selected peaks. NOTE: Use a bulk sample if necessary to identify the appropriate chromatographic peaks.

CALCULATIONS: 10. 11.

Determine the mass, µg (corrected for R) of chlorinated diphenyl oxide found in the sample (W) and in the average media blank (B) from the calibration graph. Calculate concentration, C, of chlorinated diphenyl oxide in the air volume sampled, V (L):

EVALUATION OF METHOD: Method S119 was evaluated over the range 0.1 to 1 mg/m 3 hexachlorodiphenyl oxide at 22 °C and 767 mm Hg using 90-L samples [1]. Overall precision, SˆrT, was 0.070; no reference method was used. The test atmospheres were generated from solutions (0.25 to 0.5% w/v) of chlorinated diphenyl oxide (Chem Samples) in toluene, using a fluid aspirator, cyclone and an impactor. Sampling with two filters in series was conducted in an atmosphere containing 1 mg/m 3 chlorinated diphenyl oxide. Chlorinated diphenyl oxide was found only on the front filters (with LOD = 0.002 mg/m 3). Filters enriched with 100 µg chlorinated diphenyl oxide were analyzed after passing 100 L of air through them. The resulting recovery of the analyte was 99.75% with Sr = 0.017%. The recovery of chlorinated diphenyl oxide from enriched filters through which no air was drawn was 1.012 in the range 23 to 90 µg per sample. Storage stability of the sample was not tested.

REFERENCES: [1] Documentation of the NIOSH Validation Tests, S119, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-185 (1977), available as Stock No. PB 274-248 from NTIS, Springfield, VA 22161. [2] NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, S119, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-157-B (1977). [3] NIOSH/OSHA Occupational Health Guidelines for Chemical Hazards, U.S. Department of Health and Human Services, Publ. (NIOSH) 81-123 (1981), available as Stock #PB83-154609 from NTIS, Springfield, VA 22161. [4] Occupational Diseases, A Guide to Their Recognition, revised ed., 255-256, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-181 (1978). [5] Patty, F. A. Industrial Hygiene and Toxicology, 2nd ed, Vol. 2, 1706-1707, Interscience, New York (1963).

METHOD REVISED BY: James E. Arnold, NIOSH/DPSE; S119 originally developed under NIOSH Contract CDC-99-74-45.

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