GC Analysis of Semivolatiles on SLB^®-5ms after SPME using 60 μm Carbowax^® Fiber

sample/matrix

Base neutral analytes at 50 ppb and internal standards 25 ppb in 0.1M phosphate buffer, pH 11, with 25% NaCl, 9 mL in 10 mL screw cap vial

SPME fiber

60 μm Carbowax (PEG) (57354-U)

extraction

30 min. direct immersion with agitation using CombiPal autosampler

desorption process

2 min at 250°C, splitless for 0.75 min then opened

column

SLB-5ms, 30 m x 0.25 mm I.D., 0.5μm film

oven

50°C(2 min) to 130°C @ 12°C/min to 200°C @ 20°C/min to 260°C @ 15°C/min to 310°C @ 20°C/min (4 min)

inj. temp.

Splitless/split with 0.75mm ID liner and Merlin Microseal

detector

ITMS m/z=50-230 @ 0.65 μsec per scan, transfer line 310°C

carrier gas

Helium, 1mL/min constant flow, 8.7 psi