ISOCYANAT ES, TOTA L (MAP): METHO D 5525, Issue 1, dated 15 March 2003 - Page 2 of 17 REAGENTS:
EQUIPMENT:
For Glass-fiber Filter (GFF) Sam pling and An alysis 1. 1-(9-anthracenylmethyl)piperazine (MAP) [5,6] impregnated filters. a. 37-m m : 1.1 mg M AP/filter. b. 25-m m : 0.5 mg M AP /filter. c. 13-m m : 0.13 mg MAP /filter. 2. Extracting solution: 1x10-4 M MAP in acetonitrile (2.76 mg MAP per 100 mL acetonitrile). 3. Acetic an hydride (HP LC grad e).* 4. Aceton itrile (HPLC grad e).*
1. Sam pler: Glass-fiber filter, Type A/E BinderFree, 13- or 37-m m (Gelm an or equivalent), coated with appropriate amount of MAP [5,6] (see Reagents) in an opaque cassette filter holder with cellulose bac kup; or 25-m m glass-fiber filter coated with MAP (see Reagents) in an IOM sampler with stainless steel cassette; or impinger. 2. Personal sampling pump, capable of sam pling at 1 to 2 L/m in with flexible connecting tubing. NO TE : Avoid leaching of plasticizer into solvent during impinger sampling. For impingers, Fluran TM tubing is acceptable, PVC tubing is not. 3. W ide-m outh glass jars (2 0-m L) with PT FE lined cap fo r extra ction a nd tra nsp ort. 4. Insulated shipping container with ice packs. 5. High performance liquid chromatograph (HPLC) with binary solvent and gradient capabilities, PEEK tubing, and post-column addition pump, interfaced with an autoinjection system, em ploying 150x 4.6-m m Ine rtsilTM C8, 5-:m column with titanium frits, in a column oven set to 30 °C (or a minimum of 5 degrees above ambient). Adaption of m eth od to a narrowe r bo re colum n is acc epta ble. 6. UV detector s et to 25 3 nm . 7. Fluorescence (FL) detector with either (a) Xenon source: excitation 368 nm, emission 409 nm; or (b) Deuterium source: excitation 254 nm, emission 409 nm. 8. Volumetric flasks, glass, various sizes. 9. Visiprep TM or equivalent solid phase extraction (SPE) manifold with drying attachment and disposable valve liners. 10. Supelclean TM LC-Si or equivalent SPE tubes (0.5g) with 6-mL reservoir. 11. Disposable 20-mL glass vials with PTFElined caps. 12. Microsyringes. 13. HPLC vials. 14. Pipets, disposable glass. 15. PTF E syringe filters (0.45-µm pore size). 16. Forceps for handling filters. 17. Sealing bands. 18. Top-loading balance , 2 to 3 decimal place. 19. Analytical balance, 5 place.
Fo r Im pinger Sam pling and Analysis 5. Impinger solution: 1x10 -4 M MAP [5,6 ] in butyl benzo ate (2.76 m g per 100 m L butyl benzoate). 6. Butyl benzoate: Purified by running through a silica gel column. 7. Methylene chloride (HP LC grad e).* 8. Acetonitrile (HPL C grade ). 9. Me than ol (HPLC grade ).* 10. 90:10 aceto nitrile-m eth anol. Chromatography 11. Phosp horic acid, 85% (99.9 99% ).* 12. Form ic acid (AC S reage nt gra de).* 13. Acetonitrile (HPL C grade ). 14. Triethylam ine (99.5% ).* 15. Hydroch loric ac id (conce ntrate d).* 16. 100 m M p hos pha te-form ate buffer, pH 6.0 and pH 1.6, and aceton itrile-buffer m obile phase s (APP END IX A). 17. Post-column phosphoric acid (4.4 N) and aceto nitrile-a cid post-colum n addition m obile phase (APPE ND IX B). 18. Monomer standards in acetonitrile: MAPderivatives, 2x10 -8 N to 3x10-5 N (NCO groups per liter). Synthesis of MAPderivatives (APPEN DIX C ). C
See SPECIAL PRECAUTIONS
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
