ALLYL CHLORIDE: METHOD 1000, Issue 2, dated 15 August 1994 - Page 3 of 3
c. Cap the tube. Allow to stand overnight. d. Desorb (steps 5 through 7) and analyze together with working standards (steps 11 and 12). e. Prepare a graph of DE vs. mg allyl chloride recovered. 10. Analyze three quality control blind spikes and three analyst spikes to insure that the calibration graph and DE graph are in control. MEASUREMENT: 11. Set gas chromatograph according to manufacturer’s recommendations and to conditions given on page 1000-1. Inject sample aliquot manually using solvent flush technique or with autosampler. NOTE: If peak area is above the linear range of the working standards, dilute with benzene, reanalyze and apply the appropriate dilution factor in calculations. 12. Measure peak area. CALCULATIONS: 13. Determine the mass, mg (corrected for DE) of allyl chloride found in the sample front ( ) and back ( ) sorbent sections, and in the average media blank front ( ) and back ( ) sorbent sections. NOTE: If > /10, report breakthrough and possible sample loss. 14. Calculate concentration, , of allyl chloride in the air volume sampled, (L): , mg/m³. EVALUATION OF METHOD: Method S116 was issued on May 9, 1975 [2], and validated over the range 1.8 to 7.2 mg/m³ at 25 °C and 759 mm Hg using a 100-L sample [1]. Overall precision, , was 0.071 with average recovery 105.5%, representing a nonsignificant bias. The concentration of allyl chloride was independently verified by direct gas chromatography. Desorption efficiency was 0.943 in the range 0.15 mg to 0.6 mg allyl chloride per sample. Breakthrough (5% on back section) occurred between 210 and 240 min when sampling an atmosphere containing 7.56 mg/m³ allyl chloride at 0.94 L/min at 0% RH. REFERENCES: [1] Documentation of the NIOSH Validation Tests, NIOSH, S116, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-185 (1977). [2] NIOSH Manual of Analytical Methods, 2nd ed., V. 2, S116, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-157-B (1977). METHOD REVISED BY: G. David Foley, NIOSH/DPSE; originally validated under NIOSH Contract CDC-99-74-45.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
