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TRIPHENYL PHOSPHATE: METHOD 5038, Issue 1, dated 15 August 1994 - Page 3 of 3

10. d. Prepare graph of recovery vs. µg triphenyl phosphate per sample.

Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration and recovery graphs are in control.

MEASUREMENT:

11. Set gas chromatograph according to manufacturer's recommendations and to conditions given on page 5038-1. Inject 5-µL sample aliquot using solvent flush technique or with autosampler. NOTE: If peak area is above the linear range of the calibration graph, dilute, reanalyze, and apply appropriate dilution factor in the calibration.

12. Measure peak area.

CALCULATIONS:

13. Determine mass, µg (corrected for recovery), of triphenyl phosphate found in the sample (W)and in the average media blank (B).

14. Calculate concentration (C) of triphenyl phosphate in the volume of air sampled, V (L):

EVALUATION OF METHOD:

This method was evaluated over the range of 1.25 to 6.99 mg/m 3 at an atmospheric temperature and pressure of 24 °C and 759 mm Hg, using a 100-L sample. Overall sampling and measurement precision, SrT, was 0.066, with average recovery of 99.1%, representing a non-significant bias. Recovery of triphenyl phosphate from filters was 99.3% for an air sample concentration of 7.0 mg/m 3 at 1.5 L/min for 66 minutes. [1,3]. A storage stability study was not conducted.

REFERENCES:

[1]NIOSH Manual of Analytical Methods, 2nd. ed., V. 3, S210, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) CDC-99-74-45 (1978).

[2] Occupational Health Guideline for Triphenyl Phosphate, U.S. Department of Health and Human Services (NIOSH) and U.S. Department of Labor (OSHA) (1978).

[3] Backup Data Report for Triphenyl Phosphate, prepared under NIOSH Contract CDC-99-74-45.

METHOD REVISED BY: Robert P. Streicher, NIOSH/DPSE.

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