LINDANE: METHOD 5502, Issue 2, dated 15 August 1994 - Page 3 of 3 CALIBRATION AND QUALITY CONTROL: 9.
Calibrate daily with at least five solutions covering the range 3 to 135 µg Aldrin or Lindane per sample. a. Add calibration stock solution with a microliter syringe to 15 mL isooctane in a vial. b. Analyze the working standards together with samples and blanks (steps 10 through 13). c. Prepare calibration graph (peak area vs. µg Aldrin or Lindane). Analyze three additional quality control blind spikes and three analyst spikes to ensure that the calibration graph is in control.
MEASUREMENT: 10. 11. 12.
13.
Set gas chromatograph to manufacturer's specifications and to conditions given on page 5502-1. Mix the contents of the scintillation vial thoroughly. Inject 15 µL sample aliquot using solvent flush technique or autosampler. NOTE: Open vent valve for 20 sec, beginning with time of injection, to prevent the solvent peak from entering the furnace. Measure peak area.
CALCULATIONS: 14.
15.
Determine the mass, µg, of Aldrin or Lindane found in the sample (filter plus bubbler), W, and average media blank (filter plus bubbler), B, from the measured peak areas and the calibration graph. Calculate the concentration, C (mg/m 3), of Aldrin or Lindane in the air volume sampled, V (L):
EVALUATION OF METHOD: Methods S275 (Aldrin) and S290 (Lindane) were issued on February 27, 1976, and March 26, 1976, respectively [3]. The substances used to generate test atmospheres at 25 °C and 760 mm Hg in dry air were Aldrite emulsifiable concentrate (64% Aldrin) and Ortho-Lindane Borer and Leaf Miner Spray [2]. Collection efficiencies and analytical method recoveries were 1.00 for both substances in the range 22 to 90 µg per sample. Sample filters extracted in isooctane immediately and stored one week at ambient conditions gave recoveries of 103% and 102%, respectively. Overall precision, SˆrT, was 0.092 for Aldrin and 0.086 for Lindane. No significant bias was found for either substance.
REFERENCES: [1] [2] [3] [4]
Documentation of the NIOSH Validation Tests, S275 and S290, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-185 (1977). NIOSH Manual of Analytical Methods, V. 3, S275 and S290, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-157-C (1977). Hill, R.H. and J.E. Arnold. Arch. Environ . Contam . Toxicol., 8, 621-628 (1979). Criteria for a Recommended Standard...Occupational Exposure During the Manufacture and Formulation of Pesticides, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 78-174 (1978).
METHOD REVISED BY:
Gangadhar Choudhary, Ph.D., NIOSH/DPSE; S275 and S290 originally validated under NIOSH Contract CDC-99-74-45.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
