Page:NIOSH Manual of Analytical Methods - 5017.pdf/3

 DIBUTYL PHOSPHATE: METHOD 5017, Issue 2, dated 15 August 1994 - Page 3 of 3

MEASUREMENT: 9.

10.

Set gas chromatograph according to manufacturer's recommendations and to conditions given on page 5017-1. Inject sample aliquot manually using solvent flush technique or with autosampler. NOTE 1: Under these conditions, approximate retention times are 4 min for dibutyl phosphate and 6 min for tributyl phosphate. NOTE 2: If peak area is above the linear range of the working standards, dilute with eluent, reanalyze, and apply the appropriate dilution factor in calculations. Measure peak area. Divide the peak area of dibutyl phosphate derivative by the peak area of internal standard on the same chromatogram.

CALCULATIONS: 11. 12.

Determine the mass, mg of dibutyl phosphate found in the sample (W), and in the average media blank (B). Calculate concentration, C (mg/m 3), of dibutyl phosphate in the air volume sampled, V (L):

EVALUATION OF METHOD: Method P&CAM 297 was issued on November 8, 1978 [2]. The substance used to generate test atmospheres at 25 °C and 760 mm Hg in dry air was technical grade dibutyl phosphate containing ca. 55% dibutyl phosphate and 45% monobutyl phosphate [1,4]. The collection efficiencies and measurement recoveries were 1.00 in the range 0.5 to 5 mg per sample. Sample filters stored one week at ambient conditions gave recovery of 106 ± 5%. Overall sampling and measurement precision, SˆrT, was 0.057. No independent method was available to estimate bias. REFERENCES: [1] Backup Data for P&CAM 297, prepared under NIOSH Contract 210-76-0123 (unpublished, November 8, 1978). [2] NIOSH Manual of Analytical Methods, 2nd ed., Vol. 5, P&CAM 297, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 79-141 (1979). [3] NIOSH/OSHA Occupational Health Guidelines for Chemical Hazards, U.S. Department of Health and Human Services, Publ. (NIOSH) 81-123, available as GPO Stock #017-033-00337-8 from Superintendent of Documents, Washington, DC 20402. [4] NIOSH Research Report - Development and Validation of Methods for Sampling and Analysis of Workplace Toxic Substances, U.S. Department of Health and Human Services, Publ. (NIOSH) 80-133 (1980).

METHOD REVISED BY: Gangadhar Choudhary, Ph.D., ATSDR. P&CAM 297 prepared under NIOSH Contract 210-76-0123.

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