Page:NIOSH Manual of Analytical Methods - 7903.pdf/4

 ACIDS, INORGANIC: METHOD 7903, Issue 2, dated 15 August 1994 - Page 4 of 6

EVALUATION OF METHOD: The method was evaluated for hydrochloric, hydrobromic, nitric, phosphoric and sulfuric acids by laboratory generation of mixed acids [1]. Data for the individual analytes are: Range Studied (mg/m ) 0.35 - 6 0.14 - 14 0.5 - 2 2 - 20 1 - 10 0.5 - 2

(%) 0.7 0.3 -0.9 2.0 2.0 2.4

Measurement Precision ( Sr ) 0.053 0.025 0.029 0.056 0.018 0.028

Accuracy (%) ±23.4 ±11.9 ±19.7 ±16.5 ±18.7 ±19.4

Estimated LOD [2] (µg per sample) 0.7 0.6 2.0 0.9 0.7 0.9

AL

Acid HF [8] HCl [9] H3PO4 [1] HBr [1] HNO3 [1] H2SO4 [1]

3

(µg/ sample) 0.5 - 200 0.5 - 200 3 - 100 3 - 960 3 - 500 3 - 100

Overall Precision ( SˆrT ) 0.116 0.059 0.096 0.074 0.085 0.087

IC

The method was field-evaluated at two electroplating facilities using side-by-side silica gel tubes and bubblers. The method was evaluated for hydrofluoric acid in 1983 using the silica gel tubes and impingers [8]. Recovery based on impinger collection was 106% with Sˆ of 0.116. The capacity of the rT silica gel sampler for HF was 820 µg. This is equivalent to an 8-h sample at two to three times the OSHA PEL. Samples were stable for at least 21 days at 25 °C. Updated analytical columns have been used by NIOSH for analytical sequences [2]. REFERENCES:

HI

ST OR

[1]	 Cassinelli, M. E. and D. G. Taylor. Airborne Inorganic Acids, ACS Symposium Series 149, 137-152 (1981). [2]	 DataChem, Inc. NIOSH Analytical Sequences #7546, #7357, and #7594 (unpublished, 1992). [3]	 DataChem Laboratories, NIOSH Sequence #7923-C,D (unpublished, Jan. 25, 1994). [4]	 Cassinelli, M.E. “Development of a Solid Sorbent Monitoring Method for Chlorine and Bromine in Air with Determination by Ion Chromatography.” Appl. Occup. Environ. Hyg. 6:215-226 (1991) [5]	 NIOSH Manual of Analytical Methods, 2nd. ed., V. 7, P&CAM 339, U.S. Department of Health and Human Services, (NIOSH) Publication No. 82-100 (1982). [6]	 NIOSH [1994] NIOSH Manual of analytical methods (NMAM). 4th ed. Eller P.M., Cassinelli, M. E., eds. Method NIOSH 7902, Cincinnati, OH: U.S. Department of Health and Human Services, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 94-113 [www.cdc.gov/niosh/nmam/]. [7]	 NIOSH Manual of Analytical Methods, 2nd. ed., V. 5, P&CAM 268, U.S. Department of Health and Human Services, (NIOSH) Publication No. 82-100 (1982). [8]	 Cassinelli, M. E. “Laboratory Evaluation of Silica Gel Sorbent Tubes for Sampling Hydrogen Fluoride,” Am. Ind. Hyg. Assoc. J., 47(4) :219-224 (1986). [9]	 Cassinelli, M. E. and P. M. Eller. Ion Chromatographic Determination of Hydrogen Chloride, Abstract No. 150, American Industrial Hygiene Conference, Chicago, IL (1979). METHOD WRITTEN BY: Mary Ellen Cassinelli, NIOSH/DPSE.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition