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TRIAZINE HERBICIDES and THEIR METABOLITES: METHOD 8315, Issue 1, dated 15 March 2003 - page 2 of 6 EQUIPMENT:

REAGENTS: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

Sodium bicarbonate, Certified grade. Ethyl ac etate, HP LC grad e.* Ethyl ether, Sp ectra nalyzed grad e.* Atrazine. Cyanazine. Propazine. Simazine. Desethyl atrazine. Desisopropyl atrazine. Internal standard solution, Phenanthrene-d 10, 100 :g/m L in me thanol. Store in refrigerator. Sodium sulfate, anhydrous, Certified ACS grade. Sodium chloride, reagent grade. Helium, zero grade. Nitrogen, zero grade. Me than ol, HP LC grad e.* Deionized water. A urine pool collected, frozen until use, and then thoroughly mixed

  • See SPECIAL PRECAUTIONS

1. Gas chrom atograph with m ass se lective detector,SPB-5 or equivalent capillary colum n and autos am pler (page 8315 -1). NOTE: If large batche s of sam ples are done, chilling the autosampler tray assures that there is no evaporation of the samples 2. Guard column, 1.5 meter x 0.4 mm ID, made of the same m aterial (or SPB-1) as the analytical colum n and joined by a capillary column butt connector and polyamide/graphite ferrule. NOTE: This guard column and the injection port liner should be changed after every 35-40 sam ples. . 3. Analytical balance. 4. Analytical eva pora tor/m anifold fed with nitrogen gas. 5. Centrifuge. 6. “Roto-torque” rotator. 7. Disposable screw-top culture tubes, 16x125 mm , with PTFE-lined caps. NOTE: Caps with rubber liners will not work. 8. Disposable volumetric pipets, 5-mL. 9. Disposable transfer pipets, both short and long. 10. Volumetric flask, 25-mL. 11. Beakers, 50-mL, 5-mL. 12. Dispos able cen trifuge tubes, 15-m L, with caps. 13. Autosampler vials with 100-:L polypropylene inserts and caps. 14. Syringes, 10-:L and 100-:L. 15. Polypropylene bottles, 30-mL and 250-mL. 16. Disposable filtration columns, 10-mL with 20 :m pore frit. 17. Metal scoopula. 18. Repipet dispenser bottles, 1-L.

SPECIAL PRECAUTIONS: Un iversal precautio ns should always be used when dealing with bodily fluids o r extra cts thereo f. Me than ol, ethyl ethe r, and ethyl acetate are a ll highly flam m able; handle with care and use in a hood. Reagents 4-10 come from the manufacturer with expiration dates on them. Be certain to heed these dates.

SAMPLING: 1. Collect the urine in a polyethylene bottle and cap. 2. Ship the s am ple in dry ice in an insulated conta iner, store at -80°C upo n arrival at lab. A rem inder: comm ercial shippers have special labeling requirements for packages containing dry ice.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

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