1-NITR OP YRE NE: M ETH OD 2560, Issue 1, dated 1 5 Ma rch 2003 - Page 2 of 5 REAGENTS:
EQUIPMENT:
1. To luene, HPLC or GC grade .* 2. NIST , SRM 1650, Diesel Particulate Matter. 3. 1-Nitropyrene Standard Solution, 5000 µg/mL in toluene. (A ccu Stan dard Inc., N ew H aven, CT , or equivalen t).* 4. 1-Nitropyrene Standard Solution, 1000 µg/mL in toluene. (A ccu Stan dard Inc., N ew H aven, CT , or equivalen t).*
1. Sam pler: Glass fiber filter (Type A/E) 1-:m pore size, 37-mm diameter (Gelman Sciences, A nn A rbor, MI, or equ ivalent), back ed by a cellulose support pad 37 -m m OD, in a two part, 37-mm cassette filter holder. 2. Spacer Ring, 37 mm (SKC, Eighty Four, PA or eq uivalen t). NOTE: For calibration and QC sam ples, filter space r rings are used instead of a sup port p ad. 3. Personal sampling pump capable of operatin g fo r 8 h r at 2 L/m in, w ith flexible connecting tube. 4. Lab qua ke Rotary Shaker or equ ivalent. 5. Vials, Autosampler, glass with PTFE-lined crimp top cap, 1.8 mL. 6. Micro volume inserts for autosampler vials. 7. Forceps. 8. Syringes, glass: 5-µL, 10-µL, 1-mL, other sizes as needed. 9. Syringe filter with tube tip, 4-mm , 0.45-µm, PVDF. 10. Syringe, disposable: 1-mL volume. 11. Gas Chrom atograph: HP-5890 with HP-7673 Au tos am pler (or eq uivalent), An tek Model 704E N itrogen Chem ilum inescence Detector (or equivalent). Restek Rtx-5-ms®, 30 m X 0.32 mm id., 1.0-:m film thickness (or equivalent).
- See SPECIAL PRECAUTIONS
SPECIAL PRECAUTIONS:1-Nitropyrene is a cancer suspect agent and mutagen. Toluene is a flamm able liquid, toxic. SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Sam ple at an accurately known flow rate of 1.0 to 2.0 L/min for a volume of 480 to 960 L. 3. After the sample is collected, place the plastic plugs in the tubing connector stubs on the sampling cassette.
SAMPLE PREPARATION: 4. Extract Filters: a. Rem ove the filter from the cass ette with a pair of forceps, discard the support pad, fold the filter and transfer to a G C autos am pler vial. b. Add 1 mL of toluene and cap the vial with a septum crimp top. c. Place the vial on the rotary shaker. Rotate the samples for a minimum of 12 hours. 5. Prepare the filter extract for analysis. a. Carefully remove the septum cap from the vial containing the extracted filter. b. Using a transfer pipette, remove a s m uch liquid extract from the extraction vial as possible and transfer to a 1 mL disposable syringe with a 4-mm syringe filter attached. c. Filter the extract into a micro volume insert in a GC autosampler vial. Cap the vial with a septum crim p ca p. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
