Page:NIOSH Manual of Analytical Methods - 5014.pdf/2

 CHLORINATED TERPHENYL (60% CHLORINE): METHOD 5014, Issue 2, dated 15 August 1994 - Page 2 of 3

REAGENTS: 1. 2. 3. 4.

5.

EQUIPMENT:

Isooctane (2,2,4-trimethylpentane), distilled in glass.* Hexane, distilled in glass.* Chlorinated terphenyl (60% chlorine).* Calibration stock solution, 1 mg/mL. Dilute an accurately weighed 100-mg portion of chlorinated terphenyl to 100 mL with hexane. Nitrogen, 99.999%.



See SPECIAL PRECAUTIONS.

1. Sampler: 37-mm glass fiber filter (Gelman pad in a closed-face polystyrene cassette (Gelman #4338 or equivalent). 2. Personal sampling pump, 1 to 3 L/min, with flexible connecting tubing. 3. Gas chromatograph, 63Ni ECD, integrator and column (page 5014-1). 4. Tweezers, stainless steel. 5. Vials, glass, 5-mL, crimp seals or caps, silicone rubber septa lined with polyperfluoroethylene. 6. Pipets, 1-, 2- and 4-mL, with pipet bulb. 7. Ultrasonic bath. 8. Balance, readable to 0.1 mg. 9. Volumetric flasks, 5-, 10-, 25- and 100-mL. 10. Syringe, 10-µL.
 * 1) 64877 or equivalent) supported by a backup

SPECIAL PRECAUTIONS: Hexane (flash point = -22 °C) and isooctane (flash point = 4 °C) are highly flammable. Prepare samples and standards in well-ventilated hood. Chlorinated terphenyls may be similar to chlorinated biphenyls in toxicity. Use protective clothing to avoid skin contact.

SAMPLING: 1. 2.

Calibrate each personal sampling pump with a representative sampler in line. Sample at an accurately known flow rate between 1 and 3 L/min for a total sample size of 100 to 1500 L.

SAMPLE PREPARATION: 3. 4. 5.

Transfer filter to 5-mL vial using tweezers. Discard backup pad. Pipet 4.0 mL of isooctane into vial and seal immediately. Agitate vial in ultrasonic bath for 30 min to complete extraction.

CALIBRATION AND QUALITY CONTROL: 6.

7.

Calibrate daily with at least six working standards over the range 1 to 100 µg chlorinated terphenyl per sample. a. Add known amounts of calibration stock solution to hexane in 10-mL volumetric flasks and dilute to the mark. b. Analyze together with samples and blanks (steps 9 and 10). c. Prepare calibration graph (detector response vs. µg chlorinated terphenyl per sample). Prepare two control samples at each of two levels for checking analysis of field samples. a. For each control sample, inject calibration stock solution directly onto filter. Mount filter in cassette and draw ca. 30 L of analyte-free air through (to evaporate hexane). Seal cassette and store overnight. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94