METHOD 8082 POLYCHLORINATED BIPHENYLS (PCBs) BY GAS CHROMATOGRAPHY
4.0 APPARATUS AND MATERIALS
4.1 Gas chromatograph - An analytical system complete with gas chromatograph suitable for on-column and split-splitless injection and all required accessories including syringes, analytical columns, gases, electron capture detectors (ECD), and recorder/integrator or data system.
4.2 GC columns
This method describes procedures for both single-column and dual-column analyses. The single-column approach involves one analysis to determine that a compound is present, followed by a second analysis to confirm the identity of the compound (Sec. 8.4 describes how GC/MS confirmation techniques may be employed). The single-column approach may employ either narrow-bore (# 0.32 mm ID) columns or wide-bore (0.53 mm ID) columns. The dual-column approach involves a single injection that is split between two columns that are mounted in a single gas chromatograph. The dual-column approach employs only wide-bore (0.53 mm ID) columns. A third alternative is to employ dual columns mounted in a single GC, but with each column connected to a separate injector and a separate detector.
The columns listed in this section were the columns used to develop the method performance data. Listing these columns in this method is not intended to exclude the use of other columns that may be developed. Laboratories may use other capillary columns provided that they document method performance (e.g., chromatographic resolution, analyte breakdown, and MDLs) that equals or exceeds the performance specified in this method.
4.2.1 Narrow-bore columns for single-column analysis (use both columns to confirm compound identifications unless another confirmation technique such as GC/MS is employed). Narrow bore columns should be installed in split/splitless (Grob-type) injectors.
4.2.1.1 30 m x 0.25 or 0.32 mm ID fused silica capillary column chemically bonded with SE-54 (DB-5 or equivalent), 1 µm film thickness.
4.2.1.2 30 m x 0.25 mm ID fused silica capillary column chemically bonded with 35 percent phenyl methylpolysiloxane (DB-608, SPB-608, or equivalent), 2.5 µm coating thickness, 1 µm film thickness.
4.2.2 Wide-bore columns for single-column analysis (use two of the three columns listed to confirm compound identifications unless another confirmation technique such as GC/MS is employed). Wide-bore columns should be installed in 1/4 inch injectors, with deactivated liners designed specifically for use with these columns.
4.2.2.1 30 m x 0.53 mm ID fused silica capillary column chemically bonded with 35 percent phenyl methylpolysiloxane (DB-608, SPB-608, RTx-35, or equivalent), 0.5 µm or 0.83 µm film thickness.
4.2.2.2 30 m x 0.53 mm ID fused silica capillary column chemically bonded with 14% cyanopropylmethylpolysiloxane (DB-1701, or equivalent), 1.0 µm film thickness.
4.2.2.3 30 m x 0.53 mm ID fused silica capillary column chemically bonded with SE-54 (DB-5, SPB-5, RTx-5, or equivalent), 1.5 µm film thickness.
4.2.3 Wide-bore columns for dual-column analysis (choose one of the two pairs of columns listed below).
4.2.3.1 Column pair 1
30 m x 0.53 mm ID fused silica capillary column chemically bonded with SE-54 (DB-5, SPB-5, RTx-5, or equivalent), 1.5 µm film thickness.
30 m x 0.53 mm ID fused silica capillary column chemically bonded with 14% cyanopropylmethylpolysiloxane (DB-1701, or equivalent), 1.0 µm film thickness.
Column pair 1 is mounted in a press-fit Y-shaped glass 3-way union splitter (J&W Scientific, Catalog No. 705-0733) or a Y-shaped fused-silica connector (Restek, Catalog No. 20405), or equivalent.
4.2.3.2 Column pair 2
30 m x 0.53 mm ID fused silica capillary column chemically bonded with SE-54 (DB-5, SPB-5, RTx-5, or equivalent), 0.83 µm film thickness.
30 m x 0.53 mm ID fused silica capillary column chemically bonded with 14% cyanopropylmethylpolysiloxane (DB-1701, or equivalent), 1.0 µm film thickness.
Column pair 2 is mounted in an 8 in. deactivated glass injection tee (Supelco, Catalog No. 2-3665M), or equivalent.
4.3 Column rinsing kit - Bonded-phase column rinse kit (J&W Scientific, Catalog No. 430-3000), or equivalent.
4.4 Volumetric flasks - 10-mL and 25-mL, for preparation of standards.
