ASTM D4059 Test Method forAnalysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography
4. Summary of Test Method
4.1 The test specimen is diluted with a suitable solvent. The resulting solution is treated by a procedure to remove interfering substances after which a small portion of the resulting solution is injected into a gas chromatographic column. The components are separated as they pass through the column with carrier gas and their presence in the effluent is measured by an electron capture (EC) detector and recorded as a chromatogram. The test method is made quantitative by comparing the sample chromatogram with a chromatogram of a known quantity of one or more standard Aroclors, obtained under the same analytical conditions.

5. Significance and Use
5.1 United States governmental regulations mandate that electrical apparatus and electrical insulating fluids containing PCB be handled and disposed of through specific procedures. The procedure to be used for a particular apparatus or quantity of insulating fluid is determined by the PCB content of the fluid. The results of this analytical technique can be useful in selecting the appropriate handling and disposal procedure.

5.2 Quantification in this technique requires a peak-by-peak comparison of the chromatogram of an unknown specimen with that of standard Aroclor test specimens obtained under identical conditions. The amount of PCB producing each peak in the standard chromatogram shall be known independently.

5.3 The technique described is based on data for standard chromatograms of Aroclors 1242, 1254, and 1260 obtained using specific chromatographic column packing materials and operating conditions. Relevant chromatograms are reproduced in Fig. 1, Fig. 2, and Fig. 3, for isothermal packed columns and in Figs. X4.1 through X4.3) for temperature programmed mega-bore capillary columns. Each peak is identified by its retention time relative to that of a standard. The types and amounts of PCB associated with each peak have been determined by mass spectroscopy and are given in Table 1, Table 2, and Table 3. Other chromatographic operating conditions, and in particular, other column packing materials, may give different separations. The data given in the tables should not be used if chromatograms of the standards differ significantly from those shown in the figures. The peaks in such standard chromatograms shall be independently identified and quantified.

5.4 Different isomers of PCB with the same number of chlorine substituents can cause substantially different responses from EC detectors. Mixtures of PCB containing the same amount of PCB, but with a different ratio of isomers, can give quite different chromatograms. This technique is effective only when the standard PCB mixtures and those found in the unknown test specimen are closely related. Aroclors 1242, 1254, and 1260 are adequate standards because they have been found to be the most common PCB contaminant in electrical insulating oils.