Page:NIOSH Manual of Analytical Methods - 5018.pdf/2

 2,4,7-TRINITROFLUOREN-9-ONE: METHOD 5018, Issue 2, dated 15 August 1994 - Page 2 of 3 REAGENTS: 1. 2. 3. 4.

EQUIPMENT:

Isooctane, HPLC grade. Methylene chloride, HPLC grade. Toluene. Calibration stock solution, 0.05 mg/mL. Dissolve 0.5 mg 2,4,7-trinitrofluoren-9-one* (TNF)* in 10 mL toluene.


 * See SPECIAL PRECAUTIONS.

1. Sampler: PTFE filter, 0.5-µm pore size, 37-mm diameter, with backup pad and in polystyrene cassette. 2. Personal sampling pump, 1 to 3 L/min, with flexible connecting tube. 3. Liquid chromatograph with UV detector, recorder, integrator, autosampler or syringe, and column (page 5018-1) 4. Ultrasonic waterbath. 5. Centrifuge. 6. Test tubes, glass, 10-mL, screw-cap. 7. Pasteur pipets. 8. Volumetric flasks, 10-mL 9. Syringes or micropipets, 5- to 100-µL 10. Pipets, 2-mL, glass, delivery, with pipet bulb. 11. Tweezers

SPECIAL PRECAUTIONS: Trinitrofluorenone is a suspect carcinogen and mutagen.

SAMPLING: 1. 2. 3. 4.

Calibrate each personal sampling pump with a representative sampler in line. Remove cassette plugs and attach cassette to personal sampling pump with flexible tubing. Sample at an accurately known flow rate between 1 and 3 L/min for a total sample size of 100 to 500 L. Plug the inlet and outlet of the cassette. Pack securely for shipment.

SAMPLE PREPARATION: 5. 6. 7. 8. 9.

Remove filter from cassette. Fold or roll the filter and slide it to the bottom of a test tube with tweezers. Add 2.0 mL toluene to each test tube and seal. Suspend test tube with filter in an ultrasonic bath. Agitate for 5 min. Centrifuge sample at ca. 2500 rpm for 30 min. Transfer an aliquot of clear sample liquid to a clean test tube or autosampler vial.

CALIBRATION AND QUALITY CONTROL: 10.

Calibrate daily with at least six working standards over the range 0.04 to 4 µg TNF per sample. a. Add known amounts of calibration stock solution to toluene in 10-mL volumetric flasks and dilute to the mark to produce concentrations of 0.02 to 2 µg/mL. b. Analyze together with samples and blanks (steps 13 through 15). c. Prepare calibration graph (peak area vs. µg TNF).

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94