National Institute for Occupational Safety and Health

Summary

National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Attach sampler to personal sampling pump with flexible tubing. Sample at an accurately known flow rate of 0.2 ±0.03 L/min for a total sample size of 6 to 30 L. Cap the samplers. Pack securely for shipment.
SPECIAL PRECAUTIONS: Carbon disulfide is toxic and a serious fire and explosion hazard (flash point = -30 °C) ; all work with it must be done in a hood away from ignition sources. Diazomethane is an explosive, insidious poison and a strong irritant which may cause delayed hypersensitivity and cancer [3] . Concentrated solutions may explode violently, especially if impurities are present.
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National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Determine desorption efficiency (DE) at least once for each lot of coated XAD-2 resin used for sampling in the calibration range (step 8) . Prepare three tubes at each of five levels plus three media blanks. a. Remove and discard back sorbent section of a media blank sampler. b. Inject a known amount of methyl octanoate directly onto front sorbent section with a microliter syringe. c. Cap the tube. Allow to stand overnight. d. Desorb (steps 5 through 7) and analyze with working standards (steps 11 and 12) . e. Prepare a graph of DE vs. μg methyl octanoate recovered.
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National Institute for Occupational Safety and Health NIOSH Manual of Analytical Methods… (1994)

Sample stability was not determined. The method does not meet the 10% bias criterion for a valid NIOSH method. Breakthrough of the front section of the coated XAD-2 tube was not observed after sampling 53 L of dry test atmosphere containing 0.83 mg/m 3 for 240 min at 0.22 L/min. Desorption efficiencies for samples spiked with methyl octanoate were 1.01 to 1.05. The collection efficiency and reaction of diazomethane with the octanoic acid-coated resin may be strongly dependent on sample flow rates; therefore, all samples must be collected at a flow rate of 0.2 L/min only.
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