NAPHTHAS: METHOD 1550, Issue 2, dated 15 August 1994 - Page 3 of 5 b. c. 9.
10.
Analyze together with samples and blanks (steps 11 and 12). Prepare calibration graph (ratio of peak area of analyte to peak area of internal standard vs. mg naphtha). 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 naphtha bulk sample 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 naphtha 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 1550-1. Inject sample aliquot manually using solvent flush technique or with autosampler. NOTE 1: The columns and conditions given provide moderate to good separation of components. If less resolution is needed, use shorter, less efficient columns as were used in validation of Methods S86 [2], S380 [3] and S382 [4]. 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 analyte by the peak area of internal standard on the same chromatogram.
CALCULATIONS: 13.
14.
Determine the mass, mg (corrected for DE) of naphtha 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 naphtha in the air volume sampled, V (L):
EVALUATION OF METHOD: Methods S86 (Naphtha, Coal Tar), S380 (Petroleum distillate) and S382 (Stoddard Solvent) were issued on March 14, 1975 [2,3,4]. They were validated at 24 °C and approximately 755 mm Hg using 10-, 4and 3-L air samples, respectively, of 2-50-W Hi-Flash Solvent (Neville Chemical Co.; BP 154 to 195 °C; d 0.893 g/mL), VM&P Naphtha (Amsco Product 1101; BP 120 to 147 °C; d 0.743 g/mL) and Stoddard Solvent (Fisher Scientific Co.; BP 159 to 176 °C; d 0.774 g/mL) [1]. Overall precision and recovery were as shown below, representing a non-significant bias in each method. Breakthrough tests in dry air showed a capacity of 20 to 25 mg of each solvent tested. Capacity at high relative humidity was not determined.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94
