ASTM D4059 Test Method forAnalysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography
7. Apparatus
7.1 Instruments:
7.1.1 Gas Chromatograph, equipped with oven temperature control reproducible to 1°C and with heated injection port.
7.1.2 Means to Record the Chromatogram, such as a pen recorder, preferably coupled to a digital integrator to determine peak areas. An automatic sample injector may be used.
7.1.3 Injector, stainless steel construction, equipped with suitable adapters to permit use of direct column injection, packed column injection, or split/splitless capillary injection. All metal surfaces shall be lined with glass.
7.1.3.1 Mega-bore capillary columns may be effectively utilized on a packed column injector by replacing the standard glass liner with a tapered capillary liner. While capillary conversion kits are commercially available, this specialized hardware will not routinely be necessary when working with mega-bore columns.
7.1.4 Detector - High-temperature Ni electron capture detector with sufficient sensitivity to allow 50 % full-scale recorder deflection with a sample containing 0.6 ng or less of phosphorothioic acid o-(2-chloro-4-nitrophenyl) o,o-dimethylester ("dicapthon"). The detector must be operated within its linear response range and the detector noise level should be less than 2 % of full scale.
NOTE 1 - Other detectors may be used. Refer to Appendix X1.
7.2 Column, made of glass or fused silica, packed with appropriate materials. A precolumn may be used to extend the analytical column's useful life.
7.2.1 A 1.83-m (6-ft) long, 6.35-mm (0.25-in.) outside diameter, 2 to 4-mm (0.08 to 0.16 in.) inside diameter glass column packed with 3 % OV1 on 80/100 mesh Chromosorb has been found useful. Other column lengths may be used, provided they give adequate separation of the PCB components. Packings OV101 and DC200 on Chromosorb WAW also give separations with which the data in Table 1, Table 2, and Table 3 may be used.
7.2.2 A fused silica wide-bore capillary column such as a 15-m mega-bore (0.53-mm ID) column having a 1.5-µm film of polydimethylsiloxane has been shown to approximate a packed column system and generate chromatograms with similar separations thus allowing the use of the Webb & McCall calibration data.
7.3 Volumetric Flasks and Pipettes, appropriate for making dilutions.
7.4 Precision Syringe, glass, graduated to 0.1 µL.
7.5 Vials, glass, with PTFE-lined aluminum caps.
7.6 Analytical Balance or Hydrometer, capable of measuring densities of approximately 0.9 g/mL.
