Page:NIOSH Manual of Analytical Methods - 5512.pdf/2

 PENTACHLOROPHENOL: METHOD 5512, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3. 4. 5. 6.

EQUIPMENT:

Pentachlorophenol *, ACS reagent grade. Ethylene glycol, ACS reagent grade.* Methanol, distilled in glass. Isopropanol, distilled in glass. Water, deionized and distilled. Calibration stock solution, 5 mg/mL. Dissolve 50 mg pentachlorophenol in 10 mL isopropanol.



See Special Precautions

1. Sampler: 37-mm cellulose ester membrane filter (0.8-µm pore size) supported by stainless steel screen in three-piece filter holder followed by a 25-mL bubbler with 15 mL ethylene glycol. 2. Personal sampling pump, 0.5 to 1 mL/min, with flexible polyethylene or PTFE tubing. 3. PTFE plugs and/or tubing. 4. Vials, glass, 20-mL with PTFE-lined caps. 5. Liquid chromatograph with a UV detector, recorder, integrator and column (page 5512-1). 6. Tweezers. 7. Syringes, 50- and 100-µL. 8. Volumetric flasks, 25-mL. 9. Pipets, 10- and 15-mL glass, delivery, with pipet bulb. 10. Graduated cylinders, glass, 25-mL.

SPECIAL PRECAUTIONS: Pentachlorophenol can irritate the eyes, can be absorbed through the skin, and can cause liver damage [6]. Ethylene glycol is very toxic. It may be harmful or fatal if absorbed through the skin or swallowed, may cause kidney damage, and is a suspect reproductive hazard [7].

SAMPLING: 1. 2. 3. 4. 5.

6.

Calibrate each personal sampling pump with a representative sampler in line. Transfer 15 mL ethylene glycol to a bubbler. Attach outlet of filter holder to inlet arm of bubbler. Connect outlet arm of bubbler to a second empty bubbler and then to the sampling pump. Sample 48 to 480 L (15 L for STEL) of air at an accurately known rate between 0.5 and 1.0 L/min. Transfer filter carefully using tweezers to the bubbler. Seal bubbler for shipment in a suitable container in order to prevent damage during transit. Seal the inlet and outlet of the bubbler stem by connecting a piece of PTFE tubing between them or by inserting PTFE plugs in the inlet and outlet. Collect a bulk sample (ca. 1 g) in a glass vial and ship it separately.

SAMPLE PREPARATION: 7. 8.

9.

Transfer the liquid from the bubbler, quantitatively, to a graduated cylinder. Bring volume to 15 mL with ethylene glycol. (If volume is greater than 15 mL, as would be the case when H 2O is scrubbed from humid air, record the volume and make an appropriate correction in the final calculations). Just before analysis, add 10 mL methanol and mix gently but thoroughly.

CALIBRATION AND QUALITY CONTROL: 10.

Calibrate daily with at least six working standards in the range 8 to 270 µg/25 mL. a. Add appropriate aliquots of calibration stock solution to a 60/40 (v/v) mixture of ethylene glycol and methanol. b. Analyze working standards together with samples and blanks (steps 13 through 15). NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94