Page:NIOSH Manual of Analytical Methods - 9202.pdf/2

 CAP TAN and T HIOP HAN ATE -MET HYL: M ETH OD 9202, Issue 1, dated 1 5 Ma rch 2003 - Page 2 of 4 EQUIPMENT:

REAGENTS: 1. 2. 3. 4. 5.

Isop ropa nol, H PLC pesticide grade .* Aceton itrile, HPL C grade .* Triethylam ine (T EA).* Deionized water. Thiophanate-methyl* stock solution, 10 mg/m L. Prepare in acetonitrile. 6. Captan * stock s olution, 5 m g/m L. P repare in acetonitrile. 7. TEA-PO 4 Preservative. Dissolve 1.4 mL of TEA in 90 mL of deionized water in a 100 mL volumetric flask. Add phosphoric acid to lower pH to 7.0 +/- 0.1 as indicated by a calibrated pH m eter. B ring vo lum e to 100 m L with w ater. Keep tightly capped and refrigerated. Solution stable for 12 months. 8. Mobile phase A. Com bine 20 mL of npropanol and 2.8 mL triethylamine in a 1 L volumetric flask and bring to volume using deionized water. Adjust pH to 7.0 (+/- 0.1) with phosphoric acid using a pH m eter. Final concentrations: 2% n-propanol, 0.02 M TEAPO 4. Degas prior to use. 9. Mobile phase B. Transfer 20 mL of npropanol to a 1 L volumetric flask and adjust to volum e with a cetonitrile. Degas prior to use. 10. Ortho-p hos pho ric acid* >85 % by weight, ACS grade or better.

1. Sa m pler: 8" x 12" S ciencew are™ Re usable Heavyweight P olyethyle ne Bags, 4 m m wall thickness (B el-Art No. H1317 8-0812). 2. Co ntaine r: 250 m L sc rew-top c onta iner with PTF E liner. 3. High Performance Liquid Chromatograph (HPLC ) with UV detector. 4. Autosampler or injection valve capable of 5 µL injections. 5. An alytic al colum n: P henom enex® Synergi™ 4µ Hydro-RP 80A (250 x 2.00 mm ) or equ ivalent. 6. Vials, 2-mL with PTFE-lined caps. 7. Syringes, 50-:L, 1-mL, and 5-mL. 8. Volumetric flasks, 5-mL, 100-mL, and 1-L. 9. PTFE syringe filter, 4-mm, 0.45-µm pore. 10. pH m eter. 11. Graduated cylinders, 50-mL. 12. Pipettes, glass, disposable, 2-mL. 13. Bagge d refrigera nt.


 * See SPECIAL PRECAUTIONS

SPECIAL PRECAUTIONS: Th iophana te-m ethyl: Avo id inhaling vap ors or du st; avo id sk in con tact. W ear glo ves and suitab le cloth ing when handling pure m ate rial. So lvents: Avoid sk in contac t and open flam e. Us e in a h ood. Pho sph oric acid: Av oid sk in con tact. C apta n: Use in h ood. Avoid con tact w ith sk in, eyes, and clothing an d inge stion o r inhalation. Eye protection sho uld be worn. SAMPLING: 1. Pour 150 mL of isopropanol into the polyethylene bag. 2. Insert hand into bag. W rap the top of the bag securely around the forearm, several inches above the w rist. NOTE: Allergies to alcohol are extremely rare. Before conducting the handwash, check to see if the person has ever had a reaction to alcohols, or is taking medications that could react with the alcohol. Some skin conditions, such as cuts, abrasions, and eczema can be irritated by contact with alcohols. If the person’s hand seems “dried-out” after the handwash, hand lotion can be applied. 3. Shake hand in alcohol with constant back and forth motion for 30 seconds. Rem ove hand from bag and dry with paper tow el. 4. Transfer solution to glass ja r, cap securely. 5. Lab el and pac k fo r shipm ent. 6. For field blank, add 150 mL isopropanol to a clean bag, shake for 30 seconds, then transfer the solve nt to a g lass jar for shipm ent.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition