Page:NIOSH Manual of Analytical Methods - 1619.pdf/3

PHENYL GLYCIDYL ETHER: METHOD 1619, Issue 1, dated 15 August 1994 - Page 3 of 4 c. 9.

10.

Prepare calibration graph (phenyl glycidyl ether peak area vs. mg phenyl glycidyl ether per 0.5 mL). Determine desorption efficiency (DE) at least once for each lot of charcoal used for sampling in the range of interest. Prepare three tubes at each of five levels plus three medial blanks. a. Remove and discard back sorbent section of a media blank sampler. b. Inject known amount (1 to 20 µL) of phenyl glycidyl ether or standard solution of phenyl glycidyl ether in CS 2 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. mg phenyl glycidyl ether recovered. Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration graph and DE graph are in control.

MEASUREMENT: 11.

12.

Set gas chromatograph according to manufacturer's recommendations and to conditions given on page 1619-1. 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 an aliquot of the desorbed liquid with CS 2, reanalyze, and apply the appropriate dilution factor in calculations. Measure peak area.

CALCULATIONS: 13.

14.

Determine the mass, mg (corrected for DE) of phenyl glycidyl ether found in the sample front (W f) and back (W b) sorbent sections, and in the average media blank front (B f) and back (B b) sorbent sections. NOTE: If W b > W f/10, report breakthrough and possible sample loss. Calculate concentration, C, of phenyl glycidyl ether in the air volume sampled, V (L):

EVALUATION OF METHOD: S74 was issued on February 14, 1975 [2] and validated over the range 31 to 121 mg/m 3 for 50-L air samples from dynamically generated test atmospheres [1]. The average recoveries ranged from 91.2 to 93.7%. The phenyl glycidyl ether concentrations were independently measured by means of a total hydrocarbon analyzer. Breakthrough was not observed after sampling 220 L from a test atmosphere containing 112 mg/m 3 of phenyl glycidyl ether. The average desorption efficiency was 98% over the range of 1.5 to 6 mg per sample. Sample stability was not determined; however, refrigeration of the samples upon receipt by the labortory is recommended.

REFERENCES: [1]

[2]

Documentation of the NIOSH Validation Tests, S74, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-185 (1977). Available as GPO Stock #017-033-00231-2 from Superintendent of Documents, Washington, DC 20402. NIOSH Manual of Analytical Methods, 2nd ed., Vol. 2, S74, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-157-B (1977).

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