Gas Chromatography–Mass Spectrometry (GC-MS) provides a powerful and sensitive analytical technique for the determination of PAHs and PCBs in soils, sludges, and solid waste samples. Samples are typically extracted using solvent extraction or Soxhlet methods, followed by cleanup to remove interferences before injection into the GC-MS system. The gas chromatograph separates individual analytes based on their volatility and polarity, while the mass spectrometer detects and identifies them through their unique mass spectra, enabling both qualitative and quantitative analysis. Modern GC-MS systems equipped with selective ion monitoring (SIM), high-resolution columns, and automated sample introduction deliver excellent sensitivity, accuracy, and reproducibility. This technique ensures reliable detection of trace-level SVOCs in complex environmental samples, supporting regulatory and environmental monitoring programs.