ACETIC ACID: METHOD 1603, Issue 2, dated 15 August 1994 - Page 3 of 4 9.
10.
Determine desorption efficiency (DE) at least once for each batch of charcoal 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 acetic acid 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 together with working standards (steps 11 and 12). e. Prepare a graph of DE vs. mg acetic acid recovered. Analyze three quality control blind spikes and three analyst spikes to insure 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 1603-1. 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 with formic acid, reanalyze and apply the appropriate dilution factor in calculations. Measure peak area. Divide the peak area of analyte by the peak area of internal standard on the same chromatogram.
CALCULATIONS: 13.
14.
Determine the mass, mg (corrected for DE) of acetic acid 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 acetic acid in the air volume sampled, V (L):
EVALUATION OF METHOD: Method S169 was issued on May 13, 1977 [3], and validated over the range 12.5 to 50 mg/m 3 at 22 °C and 767 mm Hg using a 173-L sample [1,4]. Overall precision, SˆrT, was 0.058 with an average recovery of 105.4%, representing a non-significant bias. The concentration of acetic acid was independently verified by a total hydrogen analyzer. Desorption efficiency was 0.96 in the range 2.1 to 8.4 mg per sample. Breakthrough (5% on back section) was never achieved and testing was discontinued after 4.6 hrs when 10.4 mg of acetic acid was collected without breakthrough for a 269-L sample at 90% RH. A user check gave an estimated LOD of 0.01 mg per sample and a desorption efficiency of 1.01 in the range 0.3 to 5 mg per sample [2].
REFERENCES: [1]
[2] [3]
Backup Data Report for Acetic Acid, prepared under NIOSH Contract No. 210-76-0123, available as "Ten NIOSH Analytical Methods," Order No. PB 275-834 from NTIS, Springfield, VA 22161. User check, UBTL, NIOSH Sequence #4213-K (unpublished, January 31, 1984). NIOSH Manual of Analytical Methods, 2nd ed., V. 4, S169, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 78-175 (1978). NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
