GC Analysis of PCBs in Transformer Oil on SPB®-5 after SPE using Supelclean™ LC-Florisil® and LC-Si
Materials
analytical column
CONDITIONS
sample preparation
SPE (Solid Phase Extraction)
sample/matrix
used transormer oil containing 50 ppb Aroclor 1254.
SPE tube/cartridge
Supelclean LC-Florisil, 1.0 g/6 mL (57057)
SPE tube/cartridge
Supelclean LC-Si, 1.0 g/6 mL (57051)
condition
0.5 mL isooctane (Florisil tube)
sample addition
0.2 g transformer oil or 0.1 g waste oil
washing
5 x 2 mL isooctane
column
SPB-5, 30 m × 0.32 mm I.D., 0.25 μm film (24048)
oven
40 °C (4 min) to 300 °C at 10 °C/min, hold 5 min
detector
ECD
carrier gas
nitrogen
injection
1 μL, splitless (30 sec delay), then split (50:1)
Description
Application
Connect Supelclean LC-Si SPE tube (1 g/6 mL) in series to male luer outlet of Supelclean LC-Florisil SPE tube (1 g/6 mL) using an SPE Tube Adapter (57020-U). Apply up to 0.2 g transformer oil or 0.1 g waste oil to upper frit of Florisil SPE tube. Pass 5 x 2 mL isooctane through both Florisil and LC-Si SPE tubes. Oil interferences will be retained on SPE tubes whereas PCBs will elute with isooctane fractions. Collect and combine isooctane fractions using 10 mL volumetric flask. Analyze isooctane extract using GC-ECD.
Legal Information
Florisil is a registered trademark of U.S. Silica Company
SPB is a registered trademark of Merck KGaA, Darmstadt, Germany
Supelclean is a trademark of Sigma-Aldrich Co. LLC